Coordination chemistry of nitrile-functionalized mixed thia-aza macrocycles [9]aneN2S and [9]aneNS2 towards silver(I)
The coordination chemistry towards silver(I) of the small-ring macrocycles [9]aneN2S (1-thia-4,7-diazacyclononane) and [9]aneNS2 (1,4-dithia-7-azacyclononane) incorporating nitrile-functionalized pendant arms is considered both in the presence and the absence of exogenous bridging ligands. The aim is to understand the influence of the number and length of the pendant arms on the nuclearity and dimensionality of the resulting complexes. The X-ray crystal structures of the complexes bis[4,7-bis(cyanomethyl)-1-thia-4,7-diazacyclononane- κ 3N,N ′ ,S]silver(I) tetrafluoridoborate, [Ag(C10H16N4S)2]BF4 or [Ag(L1)2]BF4, [4,7-bi...
Source: Acta Crystallographica Section C - February 14, 2022 Category: Chemistry Authors: Blake, A.J. Lippolis, V. Schroder, M. Tags: macrocylic ligands silver(I) thiocyanate ligand nitrile derivatives crystal structure research papers Source Type: research
Synthesis, crystal structure and photocatalytic properties of a three-dimensional copper(II) metal – organic framework based on 1,3,5-tris(2-methylimidazol-1-yl)benzene
A three-dimensional metal – organic framework, namely, poly[[bis( μ 3-benzene-1,3,5-tricarboxylato)bis[ μ 3-1,3,5-tris(2-methylimidazol-1-yl)benzene]tricopper(II)] hexahydrate], {[Cu3(C9H3O6)2(C18H18N6)2] · 6H2O}n or {[Cu(BTC)2/3(TMIB)2/3] · 2H2O}n, (I) [TMIB is 1,3,5-tris(2-methylimidazol-1-yl)benzene and H3BTC is benzene-1,3,5-tricarboxylic acid], has been synthesized under solvothermal conditions and structurally characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction and thermogravimetric analysis (TGA). Compound (I) features an unusual three-dimensional (3,4)-connected 2-nodal net ...
Source: Acta Crystallographica Section C - February 9, 2022 Category: Chemistry Authors: Chen, H.-R. Tags: metal-organic framework MOF copper 2-nodal (3,4)-net crystal structure 1,3,5-tris(2-methylimidazol-1-yl)benzene benzene-1,3,5-tricarboxylic acid photocatalysis research papers Source Type: research
Syntheses and crystal structures of new naphthalene – and anthracene – vanadate salts and an unprecedented dimetallabis(anthracene) sandwich complex: [Na(tetrahydrofuran)3][V2(anthracene)2]
Reduction of bis(naphthalene)vanadium(0) by potassium naphthalene (KNp) in tetrahydrofuran (THF) provides a highly reactive, thermolabile, and so far unisolable brown substance, which affords the first reported derivatives of bis(naphthalene)vanadates. From these solutions, thermally stable (298 K) and structurally characterized compounds have been obtained, including dark-red rods of catena-poly[bis( μ 3- η 4: η 6: η 4-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium], [K2V(C4H8O)4(C10H8)2]n or [K(THF)2]2[V(C10H8)2] (3), and red plates of (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassiu...
Source: Acta Crystallographica Section C - February 9, 2022 Category: Chemistry Authors: Kucera, B.E. Young, V.G. Brennessel, W.W. Ellis, J.E. Tags: naphthalene anthracene bis(polyarene)vanadates dimetallabis(anthracene) sandwich complex crystal structure research papers Source Type: research
8-Furylimidazolo-2 ′ -deoxycytidine: crystal structure, packing, atropisomerism and fluorescence
8-Furylimidazolo-2 ′ -deoxycytidine (furImidC), C14H14N4O5, is a fluorescent analogue of 2 ′ -deoxycytidine, also displaying the same recognition face. As a constituent of DNA, furImidC forms extraordinarily strong silver-mediated self-pairs. Crystal structure determination revealed that furImidC adopts two types of disordered residues: the sugar unit and the furyl moiety. The disorder of the sugar residue amounts to an 87:13 split. The disorder of the furyl ring results from axial chirality at the C8 — C2 ′ ′ bond connecting the nucleobase to the heterocycle. The two atropisomers are present in unequal proportio...
Source: Acta Crystallographica Section C - February 9, 2022 Category: Chemistry Authors: Budow-Busse, S. Jana, S.K. Kondhare, D. Daniliuc, C. Seela, F. Tags: 8-furylimidazolo-2 ′ -deoxycytidine crystal structure atropisomerism crystal packing Hirshfeld surface analysis fluorescence research papers Source Type: research
Mirror-plane disorder in a nickel chloride Schiff base complex: a suitable case study for crystallographic instruction
The nickel chloride complex of the Schiff base N2,N2 ′ -propanediylbis(2,3-butanedione-2-imine-3-oxime), namely, chlorido(3,9-dimethylundeca-3,8-diene-2,10-dione 10-oxime 2-oximato- κ 4N,N ′ ,N ′ ′ ,N ′ ′ ′ )nickel(II), [NiCl(C11H19N4O2)], at 100 K crystallizes in the orthorhombic space group Cmce. The structure exhibits mirror disorder of the main molecule that is not present in the bromide analogue. The relatively small number of unique reflections in the data set and the disorder imposed by the crystallographic mirror plane present a challenging educational case study. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - February 8, 2022 Category: Chemistry Authors: Chang, H. Chen, W.-C. Shen, J.-S. Ong, T.-G. Wang, V.C.-C. Yap, G.P.A. Tags: Schiff base nickel complex case study disorder oxime crystal structure research papers Source Type: research
A new three-dimensional cadmium(II) coordination polymer based on bis[4-(2-methylimidazol-1-yl)phenyl]methanone: synthesis, structure and properties
A novel three-dimensional CdII coordination polymer, namely, poly[[( μ 3-benzene-1,4-diacetato)( μ 2-benzene-1,4-diacetato)bis{ μ 2-bis[4-(2-methylimidazol-1-yl)phenyl]methanone}dicadmium(II)] tetartohydrate], {[Cd(C10H8O4)(C21H18N4O)] · 0.25H2O}n or {[Cd(PBEA)(MIPMO)] · 0.25H2O}n, (I), was synthesized by the hydrothermal method using benzene-1,4-diacetic acid (H2PBEA), bis[4-(2-methylimidazol-1-yl)phenyl]methanone (MIPMO) and Cd(NO3)2 · 6H2O. The title compound was structurally characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy and thermogravimetric analysis, and exhibits a three-...
Source: Acta Crystallographica Section C - January 31, 2022 Category: Chemistry Authors: Sun, Y. Li, K. Xu, D.-N. Chen, J.-J. Wang, X.-Y. Xu, X.-J. Tao, J.-Q. Tags: coordination polymer bis[4-(2-methylimidazol-1-yl)phenyl]methanone benzene-1,4-diacetic acid luminescence sensing photocatalytic degradation crystal structure iron sensing research papers Source Type: research
Syntheses, crystal structures and Hirshfeld surface analysis of (Z)-3-[(3-acetyl-2-hydroxyphenyl)amino]-2-bromoprop-2-enal and a novel ZnII complex
A novel zero-dimensional dinuclear zinc complex, di- μ -acetato-1:2 κ 4O:O ′ -( μ -2-acetyl-6-{[(Z)-2-bromo-3-oxoprop-1-en-1-yl]azanidyl}phenolato-1 κ 2O1,O2:2 κ 3O1,N,O6)(N,N-dimethylacetamide-1 κ O)dizinc(II), [Zn2(C11H8BrNO3)(CH3COO)2(C4H9NO)] or [Zn2(L)(CH3COO)2(DMA)], 1, was synthesized using (Z)-3-[(3-acetyl-2-hydroxyphenyl)amino]-2-bromoprop-2-enal (H2L), which was synthesized from 1-(3-amino-2-hydroxyphenyl)ethanone and 2-bromomalonaldehyde. H2L and 1 were characterized by single-crystal X-ray diffraction, FT – IR spectroscopy and elemental analysis. Theoretical calculations of the bond orders and excited...
Source: Acta Crystallographica Section C - January 27, 2022 Category: Chemistry Authors: Jiang, T.-L. Li, W.-Z. Gao, Q.-F. Tan, D.-F. Pang, J.-Y. Zhang, S.-H. Tags: dinuclear zinc complex crystal structure Hirshfeld surface analysis prop-2-enal bond order research papers Source Type: research
A three-dimensional gadolinium organic framework based on a pyridinedicarboxylic acid organic linker with a paddle-wheel-type network structure
A new gadolinium(III) – pyridine-2,5-dicarboxylic acid (GdIII – 2,5-H2pdc)-based three-dimensional coordination polymer, namely, poly[dimethylazanium [bis( μ -pyridine-2,5-dicarboxylato)gadolinium(III)]], {[(CH3)2NH2][Gd(C7H3NO4)2]}n, CP-1, has been synthesized via a typical solvothermal method. The as-synthesized material was characterized in the solid state using single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetric analysis and FT – IR spectroscopy. During the synthesis of CP-1, the in situ dimethylformamide (DMF) promotes the formation of a dimeric unit and these act as secondary building...
Source: Acta Crystallographica Section C - January 27, 2022 Category: Chemistry Authors: Tiwari, R.K. Saini, M.K. Behera, J.N. Hussain, F. Tags: paddle-wheel structure helical structure Hirshfeld surface analysis 3D network magnetic properties crystal structure research papers Source Type: research
Crystallographic hallucinations
(Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - January 27, 2022 Category: Chemistry Authors: Toby, B.H. Tags: psilocybin Rietveld pharmaceutical psychedelic quantitative phase analysis scientific commentaries Source Type: research
Weak intermolecular interactions in a series of biologically active 4 ′ -methylthio-trans-stilbenes
The crystal structures of nine methoxy-substituted 4 ′ -methylthiostilbenes, which are potential inhibitors of human recombinant cytochrome P450 enzymes, were determined. These compounds included two mono-methoxy-substituted derivatives: 2-methoxy-4 ′ -methylthio-trans-stilbene {systematic name: 1-[(E)-2-(2-methoxyphenyl)ethenyl]-4-(methylsulfanyl)benzene} (1) and 3-methoxy-4 ′ -methylthio-trans-stilbene (2), both C16H16OS; four dimethoxy derivatives: 2,3-dimethoxy-4 ′ -methylthio-trans-stilbene (3), 2,5-dimethoxy-4 ′ -methylthio-trans-stilbene (4), 3,5-dimethoxy-4 ′ -methylthio-trans-stilbene (5) and 2,4-dimet...
Source: Acta Crystallographica Section C - January 25, 2022 Category: Chemistry Authors: Grze ś kiewicz, A.M. Stefa ń ski, T. Dutkiewicz, Z. Kubicki, M. Tags: stilbene conformation intermolecular interaction crystal structure docking study research papers Source Type: research
Cynarine monohydrate from synchrotron powder X-ray diffraction data
The crystal structure of cynarine monohydrate (systematic name: 1,3-bis{[(E)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy}-4,5-dihydroxycyclohexane-1-carboxylic acid monohydrate), C25H24O12 · H2O, has been solved and refined using synchrotron powder X-ray diffraction data, and optimized using density functional techniques. Despite being purchased as anhydrous, cynarine crystallizes as a monohydrate and the crystal structure is characterized by alternating layers of hydrocarbon and hydrogen-bonding interactions parallel to the bc plane. Hydrogen bonds are significant in the crystal structure. The carboxylic acid group forms a s...
Source: Acta Crystallographica Section C - January 25, 2022 Category: Chemistry Authors: Kaduk, J.A. Boaz, N.C. Markun, E.L. Gindhart, A.M. Blanton, T.N. Tags: powder diffraction cynarine 1,5-dicaffeoylquinic acid Rietveld refinement density functional theory crystal structure research papers Source Type: research
Coordination chemistry of polynitriles. Part 9. Decacyanoferrocene revisited: crystal and molecular structure of cis-[{C5(CN)5}2(MeCN)4Fe]
The reaction of Ag[C5(CN)5] with anhydrous FeCl2 in acetonitrile leads to colourless crystals of tetrakis(acetonitrile- κ N)bis(pentacyanocyclopentadienido- κ N)iron(II) acetonitrile 1.8-solvate, [Fe(C10N5)2(CH3CN)4] · 1.8CH3CN or cis-[{C5(CN)5}2(MeCN)4Fe] · 1.8MeCN. The compound crystallizes in the triclinic space group P\overline{1} as monomers, which exhibit weak C — H...N and π – π interactions. The crystals contain ca 20% solvent-accessible voids, which are nearly completely filled by two MeCN molecules. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - January 21, 2022 Category: Chemistry Authors: S ü nkel, K. Blockhaus, T. Tags: ferrocene pentacyanocyclopentadienide π – interactions weak interactions decacyanoferrocene crystal structure research papers Source Type: research
Coordination chemistry of polynitriles. Part 9. Decacyanoferrocene revisited. Crystal and molecular structure of cis-[{C5(CN)5}2(MeCN)4Fe]
The reaction of Ag[C5(CN)5] with anhydrous FeCl2 in acetonitrile leads to colourless crystals of tetrakis(acetonitrile- κ N)bis(pentacyanocyclopentadienido- κ N)iron(II) acetonitrile 1.8-solvate, [Fe(C10N5)2(CH3CN)4] · 1.8CH3CN or cis-[{C5(CN)5}2(MeCN)4Fe] · 1.8MeCN. The compound crystallizes in the triclinic space group P\overline{1} as monomers, which exhibit weak C — H...N and π – π interactions. The crystals contain ca 20% solvent-accessible voids, which are nearly completely filled by two MeCN molecules. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - January 21, 2022 Category: Chemistry Authors: S ü nkel, K. Blockhaus, T. Tags: ferrocene pentacyanocyclopentadienide π – interactions weak interactions decacyanoferrocene crystal structure research papers Source Type: research
Bis(2,6-diisopropylphenyl) tellurone: a well-defined monomeric diorganotellurone without cocrystallized solvents and without stabilizing intramolecular contacts
Only two crystal structures of diorganotellurones have been reported to date, both of which contain cocrystallized solvents and one of which is stabilized by intramolecular Te — N secondary bonding interactions. This work describes the crystal structure of bis(2,6-diisopropylphenyl) tellurone, (C12H17)2TeO2 or C24H34O2Te, the first well-defined diorganotellurone without cocrystallized solvents and without stabilizing intramolecular contacts. The molecule has crystallographic twofold symmetry, with half the molecule as the asymmetric unit. The molecular structure is compared to previously reported tellurones and those com...
Source: Acta Crystallographica Section C - January 18, 2022 Category: Chemistry Authors: Shibuya, Y. Koguchi, S. Oba, M. Tags: organotellurium compound crystal structure tellurone monomer hydrogen bond research papers Source Type: research
Trioxazolo[23]metacyclophane: synthesis, structural analysis, and optical properties
The synthesis and characterization of the conjugated macrocycle trioxazolo[23]metacyclophane, C27H15N3O3 (M), is reported. The macrocycle was synthesized in three steps by the multicomponent van Leusen reaction and consists of meta-linked phenylenes connected through positions 4 and 5 of an oxazole heterocyclic ring. The molecular structure was investigated by NMR spectroscopy, mass spectrometry, gel permeation chromatography (GPC), and single-crystal X-ray crystallography. X-ray diffraction (XRD) analysis shows that M possesses a twisted saddle-like shape and interacts with nearby molecules by various π – π interactio...
Source: Acta Crystallographica Section C - January 18, 2022 Category: Chemistry Authors: Yu, H. Gray, D.L. Woods, T.J. Moore, J.S. Tags: metacyclophane conjugated macrocycle van Leusen reaction gel permeation chromatography van Leusen MCRs crystal structure research papers Source Type: research
