scholarly journals Structural diversity in copper(I) iodide complexes with 6-thioxopiperidin-2-one, piperidine-2,6-dithione and isoindoline-1,3-dithione ligands

2020 ◽  
Vol 76 (8) ◽  
pp. 1336-1344
Author(s):  
Amelia M. Wheaton ◽  
Ilia A. Guzei ◽  
John F. Berry
Keyword(s):  
Three Dimensional ◽  
Structural Diversity ◽  
Structural Features ◽  
Acta Cryst ◽  
Bridging Ligands ◽  
Hydrogen Bonding Interactions ◽  
Scattering Effects ◽  
Internuclear Distances ◽  
Solvent Molecules ◽  
The Given

Copper(I) iodide complexes are well known for displaying a diverse array of structural features even when only small changes in ligand design are made. This structural diversity is well displayed by five copper(I) iodide compounds reported here with closely related piperidine-2,6-dithione (SNS), isoindoline-1,3-dithione (SNS6), and 6-thioxopiperidin-2-one (SNO) ligands: di-μ-iodido-bis[(acetonitrile-κN)(6-sulfanylidenepiperidin-2-one-κS)copper(I)], [Cu2I2(CH3CN)2(C5H7NOS)2] (I), bis(acetonitrile-κN)tetra-μ3-iodido-bis(6-sulfanylidenepiperidin-2-one-κS)-tetrahedro-tetracopper(I), [Cu4I4(CH3CN)4(C5H7NOS)4] (II), catena-poly[[(μ-6-sulfanylidenepiperidin-2-one-κ2 O:S)copper(I)]-μ3-iodido], [CuI(C5H7NOS)] n (III), poly[[(piperidine-2,6-dithione-κS)copper(I)]-μ3-iodido], [CuI(C5H7NS2)] n (IV), and poly[[(μ-isoindoline-1,3-dithione-κ2 S:S)copper(I)]-μ3-iodido], [CuI(C8H5NS2)] n (V). Compounds I and II crystallize as discrete dimeric and tetrameric complexes, whereas III, IV, and V crystallize as polymeric two-dimensional sheets. To the best of our knowledge, compound III is the first instance of an extended hexagonal [Cu3I3] structure that is not supported by bridging ligands. Structures I, II, and IV display weak to moderately strong Cu...Cu cuprophilic interactions [Cu...Cu internuclear distances range between 2.5803 (10) and 2.8485 (14) Å]. All structures except III display weak hydrogen-bonding interactions between the N—H of the ligand and the μ2 and μ3-I− atoms. Structure III contains classical N–H...O interactions between the SNO ligands that connect the molecules in a three-dimensional framework. Complex V features π–π stacking interactions between the aryl rings of the SNS6 ligands within the same polymeric sheet. In structure IV, there were three partially occupied solvent molecules of dichloromethane and one partially occupied molecule of acetonitrile present in the asymmetric unit. The SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18] was used to correct the diffraction data for diffuse scattering effects and to identify the solvent molecules. The given chemical formula and other crystal data do not take into account the solvent molecules.

scholarly journals Crystal structure of an unknown tetrahydrofuran solvate of tetrakis(μ3-cyanato-κ3N:N:N)tetrakis[(triphenylphosphane-κP)silver(I)]

2015 ◽  
Vol 71 (10) ◽  
pp. 1262-1265
Author(s):  
Peter Frenzel ◽  
Dieter Schaarschmidt ◽  
Alexander Jakob ◽  
Heinrich Lang
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Acta Cryst ◽  
Compound C ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Solvent Molecules ◽  
Set Up ◽  
The Given ◽  
Triphenylphosphine Ligand

In the title compound, [{[(C6H5)3P]Ag}4{NCO}4], a distorted Ag4N4-heterocubane core is set up by four AgIions being coordinated by the N atoms of the cyanato anions in aμ3-bridging mode. In addition, a triphenylphosphine ligand is datively bonded to each of the AgIions. Intramolecular Ag...Ag distances as short as 3.133 (9) Å suggest the presence of argentophilic (d10...d10) interactions. Five moderate-to-weak C—H...O hydrogen-bonding interactions are observed in the crystal structure, spanning a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst.C71, 9–18] following unsuccessful attempts to model it as being part of disordered tetrahydrofuran solvent molecules. The given chemical formula and other crystal data do not take into account these solvent molecules.

scholarly journals Crystal structure of 3-(4-chlorophenoxy)-4-(2-nitrophenyl)azetidin-2-one with an unknown solvate

2015 ◽  
Vol 71 (1) ◽  
pp. o8-o9
Author(s):  
Sevim Türktekin Çelikesir ◽  
Mehmet Akkurt ◽  
Aliasghar Jarrahpour ◽  
Habib Allah Shafie ◽  
Ömer Çelik
Keyword(s):  
Three Dimensional ◽  
Dihedral Angles ◽  
Maximum Deviation ◽  
Acta Cryst ◽  
Compound C ◽  
Dimensional Network ◽  
Lactam Ring ◽  
The Mean ◽  
Solvent Molecules ◽  
The Given

In the title compound, C15H11ClN2O4, the central β-lactam ring is approximately planar [maximum deviation = 0.044 (2) Å for the N atom from the mean plane] and subtends dihedral angles of 61.17 (11) and 40.21 (12) °, respectively, with the nitro and chlorobenzene rings. Both substituents lie to the same side of the β-lactam core. In the crystal, N—H...O hydrogen bonds link the molecules intoC(4) chains propagating in [010]. The chains are cross-linked by C—H...O and weak C—H...π interactions, generating a three-dimensional network. The solvent molecules were found to be highly disordered and their contribution to the scattering was removed with the SQUEEZE procedure inPLATON[Spek (2009).Acta Cryst.D65, 148–155], which indicated a solvent cavity of volume 318 Å3containing approximately 114 electrons. These solvent molecules are not considered in the given chemical formula and other crystal data.

scholarly journals Crystal structure of fac-{5-[(hexylazaniumyl)methyl]-2-(pyridin-2-yl)phenyl-κ2 N,C 1}bis[2-(pyridin-2-yl)phenyl-κ2 N,C 1]iridium(III) chloride

2018 ◽  
Vol 74 (10) ◽  
pp. 1439-1443
Author(s):  
Sureemas Meksawangwong ◽  
Suwadee Jiajaroen ◽  
Kittipong Chainok ◽  
Waraporn Pinyo ◽  
Filip Kielar
Keyword(s):  
Crystal Structure ◽  
Complex Molecule ◽  
Three Dimensional ◽  
Crystal Data ◽  
Chemical Formula ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Coordination Environment ◽  
Solvent Molecules ◽  
The Given

The asymmetric unit of the title compound, fac-[Ir(C11H8N)2(C18H24N2)]Cl or fac-[Ir(ppy)2(Hppy-NC6)]Cl, contains two [Ir(ppy)2(ppy-NC6)](H+) cations, two Cl− anions and disordered solvent. In each complex molecule, the IrIII ion is coordinated by two C,N-bidentate 2-(pyridin-2-yl)phenyl ligands and one C,N-bidentate N-[4-(pyridin-2-yl)benzyl]hexan-1-aminium ligand, leading to a distorted fac-octahedral coordination environment. In the crystal, the molecules are linked by N—H...Cl, C—H...π and π–π interactions, forming a three-dimensional supramolecular structure. The hexyl group of one molecule is disordered over two orientations with a refined occupancy ratio of 0.412 (13):0.588 (13). The acetone and hexane solvent molecules were found to be highly disordered and their contribution to the scattering was masked using the solvent-masking routine smtbx.mask in OLEX2 [Rees et al. (2005). Acta Cryst. D61, 1299–1301]. These solvent molecules are not considered in the given chemical formula and other crystal data.

scholarly journals Three-Dimensional Structures of Carbohydrates and Where to Find Them

2020 ◽  
Vol 21 (20) ◽  
pp. 7702 ◽  
Author(s):  
Sofya I. Scherbinina ◽  
Philip V. Toukach
Keyword(s):  
Experimental Data ◽  
Molecular Modeling ◽  
Computational Methods ◽  
Three Dimensional ◽  
Structural Diversity ◽  
Structural Data ◽  
Structural Features ◽  
Data Validation ◽  
Data Generation ◽  
Efficient Treatment

Analysis and systematization of accumulated data on carbohydrate structural diversity is a subject of great interest for structural glycobiology. Despite being a challenging task, development of computational methods for efficient treatment and management of spatial (3D) structural features of carbohydrates breaks new ground in modern glycoscience. This review is dedicated to approaches of chemo- and glyco-informatics towards 3D structural data generation, deposition and processing in regard to carbohydrates and their derivatives. Databases, molecular modeling and experimental data validation services, and structure visualization facilities developed for last five years are reviewed.

scholarly journals Crystal structures of three 4-substituted-2,2′-bipyridines synthesized by Sonogashira and Suzuki–Miyaura cross-coupling reactions

2017 ◽  
Vol 73 (4) ◽  
pp. 610-615
Author(s):  
Thuy Luong Thi Thu ◽  
Ngan Nguyen Bich ◽  
Hien Nguyen ◽  
Luc Van Meervelt
Keyword(s):  
Cross Coupling ◽  
Coupling Reactions ◽  
Acta Cryst ◽  
X Ray ◽  
Π Interactions ◽  
Cross Coupling Reactions ◽  
Synthetic Routes ◽  
Solvent Molecules ◽  
The Given ◽  
Crystal Packings

Facile synthetic routes for three 4-substituted 2,2′-bipyridine derivatives, 4-[2-(4-methylphenyl)ethynyl]-2,2′-bipyridine, C19H14N2, (I), 4-[2-(pyridin-3-yl)ethynyl]-2,2′-bipyridine, C17H11N3, (II), and 4-(indol-4-yl)-2,2′-bipyridine, C18H13N3, (III),viaSonogashira and Suzuki–Miyaura cross-coupling reactions, respectively, are described. As indicated by X-ray analysis, the 2,2′-bipyridine core, the ethylene linkage and the substituents of (I) and (II) are almost planar [dihedral angles between the two ring systems: 8.98 (5) and 9.90 (6)° for the two molecules of (I) in the asymmetric unit and 2.66 (14)° for (II)], allowing π-conjugation. On the contrary, in (III), the indole substituent ring is rotated significantly out of the bipyridine plane [dihedral angle = 55.82 (3)°], due to steric hindrance. The crystal packings of (I) and (II) are dominated by π–π interactions, resulting in layers of molecules parallel to (30-2) in (I) and columns of molecules along theaaxis in (II). The packing of (III) exhibits zigzag chains of molecules along thecaxis interacting through N—H...N hydrogen bonds and π–π interactions. The contributions of unknown disordered solvent molecules to the diffraction intensities in (II) were removed with the SQUEEZE [Spek (2015).Acta Cryst.C71, 9–18] algorithm ofPLATON. The given chemical formula and other crystal data do not take into account these solvent molecules.

scholarly journals (η6-Benzene)(carbonato-κ2O,O′)[dicyclohexyl(naphthalen-1-ylmethyl)phosphane-κP]ruthenium(II) chloroform trisolvate

2014 ◽  
Vol 70 (7) ◽  
pp. m272-m273
Author(s):  
Saravanan Gowrisankar ◽  
Helfried Neumann ◽  
Anke Spannenberg ◽  
Matthias Beller
Keyword(s):  
Hydrogen Bonding ◽  
Metal Complex ◽  
Room Temperature ◽  
Crystal Packing ◽  
The Other ◽  
Asymmetric Unit ◽  
Carbonate Group ◽  
Acta Cryst ◽  
Hydrogen Bonding Interactions ◽  
Solvent Molecules

The title compound, [Ru(CO3)(η6-C6H6){(C6H11)2P(CH2C10H7)}]·3CHCl3, was synthesized by carbonation of [RuCl2(η6-C6H6){(C6H11)2P(CH2C10H7)}] with NaHCO3in methanol at room temperature. The RuIIatom is surrounded by a benzene ligand, a chelating carbonate group and a phosphane ligand in a piano-stool configuration. The crystal packing is consolidated by C—H...O and C—H...Cl hydrogen-bonding interactions between adjacent metal complexes and between the complexes and the solvent molecules. The asymmetric unit contains one metal complex and three chloroform solvent molecules of which only one was modelled. The estimated diffraction contributions of the other two strongly disordered chloroform solvent molecules were substracted from the observed diffraction data using the SQUEEZE procedure inPLATON[Spek (2009).Acta Cryst.D65, 148–155].

scholarly journals Crystal structure of bis[cis-diaquabis(phenanthroline)cobalt(II)] bis(citrato)germanate(IV) dinitrate

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Olha Buchko ◽  
Viktoriya Dyakonenko ◽  
Elena Martsinko ◽  
Elena Chebanenko
Keyword(s):  
Crystal Structure ◽  
Solvent Molecule ◽  
Crystal Data ◽  
Chemical Formula ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
Water Oxygen ◽  
Solvent Molecules ◽  
The Given ◽  
Oxygen Atoms

The asymmetric unit of the title compound, [Co(C12H8N2)2(H2O)2]2[Ge(C6H5O7)2](NO3)2, features two complex [(C12H8N2)2(H2O)2Co]2+ cations, two NO3 − anions as well as one centrosymmetric [(C6H5O7)2Ge]2− anion. Two HCit ligands (Cit = citrate, C6H4O7) each coordinate via three different oxygen atoms (hydroxylate, α-carboxylate, β-carboxylate) to the Ge atom, forming a slightly distorted octahedron. The coordination polyhedron of the Co atom is also octahedral, formed by coordination of four nitrogen atoms from two phenanthroline molecules and two water oxygen atoms. In the crystal, the cations and anions are linked by hydrogen bonds and form layers parallel to the bc plane. The structure exhibits disorder of the NO3 − anion [disorder ratio 0.688 (9) to 0.312 (9)]. There are also highly disordered solvent molecules (presumably water and/or ethanol) in the crystal structure; explicit refinement of these molecules was not possible, and the content of the voids was instead taken into account using reverse Fourier transform methods [SQUEEZE procedure in PLATON; Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Crystal structure of an unknown solvate of {2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato-κ4O,N,N′,O′}(N-ferrocenylisonicotinamide-κN1)cobalt(II): a CoII–salen complex that forms hydrogen-bonded dimers

2015 ◽  
Vol 71 (9) ◽  
pp. 1100-1104
Author(s):  
Bryan Brautigam ◽  
Chelsea Herholdt ◽  
William Farnsworth ◽  
Ellen Brudi ◽  
Eric McDonald ◽  
...  
Keyword(s):  
Ring Structure ◽  
X Ray Diffraction ◽  
Acta Cryst ◽  
X Ray ◽  
Pyramidal Geometry ◽  
Salen Complex ◽  
Hydrogen Bonding Interactions ◽  
Solvent Molecules ◽  
Square Pyramidal Geometry ◽  
Hydrogen Bonded

The title compound, [CoFe(C5H5)(C16H14N2O2)(C11H9N2O)], was prepared as an air-stable red–brown solid by mixing equimolar amounts of {2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato}cobalt(II) andN-ferrocenylisonicotinamide in dry dichloromethane under nitrogen and was characterized by ESI–MS, IR, and single-crystal X-ray diffraction. The structure at 100 K has triclinic (P-1) symmetry and indicates that the complex crystallizes as a mixture of λ and δ conformers. It exhibits the expected square pyramidal geometry about Co, and forms hydrogen-bonded dimers through amide N—H groups and phenolate O atoms on an adjacent molecule. The involvement of only half of the salen ring structure in hydrogen-bonding interactions results in slight folding of the salen ring away from the pyridine coordination site in the δ conformer with an inter-salicylidene fold angle of 9.9 (7)°. In contrast, the λ conformer is nearly planar. The dimers pack into an open structure containing channels filled with highly disordered solvent molecules. These solvent molecules' contributions to the intensity data were removed with the SQUEEZE procedure [Spek (2015).Acta Cryst.C71, 9–18] available inPLATON.

scholarly journals Tetracarbonyl[N-(diphenylphosphanyl-κP)-N,N′-diisopropyl-P-phenylphosphorus diamide-κP]molybdenum(0) with an unknown solvent

IUCrData ◽  
2018 ◽  
Vol 3 (6) ◽  
Author(s):  
Martha Höhne ◽  
Marc Gongoll ◽  
Anke Spannenberg ◽  
Bernd H. Müller ◽  
Normen Peulecke ◽  
...  
Keyword(s):  
Solvent Molecule ◽  
Coordination Geometry ◽  
Crystal Data ◽  
Chemical Formula ◽  
Acta Cryst ◽  
Carbonyl Ligands ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Solvent Molecules ◽  
The Given

The title complex, [Mo(C24H30N2P2)(CO)4], contains a molybdenum centre bearing a P,P′-cis-chelating Ph2PN( i Pr)P(Ph)NH( i Pr) and four carbonyl ligands in a distorted octahedral coordination geometry. This results in a nearly planar four-membered metallacycle. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds to form layers parallel to the ac plane. For the final refinement, the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

scholarly journals Crystal structure of an unknown solvate of bis(tetra-n-butylammonium) [N,N′-(4-trifluoromethyl-1,2-phenylene)bis(oxamato)-κ4O,N,N′,O′]nickelate(II)

2015 ◽  
Vol 71 (6) ◽  
pp. 578-581
Author(s):  
François Eya'ane Meva ◽  
Dieter Schaarschmidt ◽  
Tobias Rüffer
Keyword(s):  
Rotation Axis ◽  
Point Group ◽  
Solvent Molecule ◽  
Three Dimensional ◽  
Group Symmetry ◽  
Acta Cryst ◽  
Coordination Environment ◽  
Dimensional Network ◽  
Square Planar ◽  
The Given

In the title compound, [N(C4H9)4]2[Ni(C11H3F3N2O6)] or [N(n-Bu)4]2[Ni(topbo)] [n-Bu =n-butyl and topbo = 4-trifluoromethyl-1,2-phenylenebis(oxamate)], the Ni2+cation is coordinated by two deprotonated amido N atoms and two carboxylate O atoms, setting up a slightly distorted square-planar coordination environment. The [Ni(topbo]2−anion lies on a twofold rotation axis. Due to an incompatibility with the point-group symmetry of the complete molecule, orientational disorder of the CF3group is observed. The tetrahedral ammonium cations and the anion are linked by weak intermolecular C—H...O and C—H...F hydrogen-bonding interactions into a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s). The given chemical formula and other crystal data do not take into account the unknown solvent molecule.

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