scholarly journals Crystal and molecular structures of a binuclear mixed ligand complex of silver(I) with thiocyanate and 1H-1,2,4-triazole-5(4H)-thione

2020 ◽  
Vol 76 (1) ◽  
pp. 42-47
Author(s):  
Janjira Kreaunakpan ◽  
Kittipong Chainok ◽  
Nathan R. Halcovitch ◽  
Edward R. T. Tiekink ◽  
Teerapong Pirojsirikul ◽  
...  
Keyword(s):  
Mixed Ligand Complex ◽  
Three Dimensional ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Ligand Complex ◽  
Face To Face ◽  
Crystal And Molecular Structures ◽  
Hirshfeld Surfaces ◽  
Thiocyanate Ligand

The complete molecule of the binuclear title complex, bis[μ-1H-1,2,4-triazole-5(4H)-thione-κ2 S:S]bis{(thiocyanato-κS)[1H-1,2,4-triazole-5(4H)-thione-κS]silver(I)}, [Ag2(SCN)2(C2H3N3S)4], is generated by crystallographic inversion symmetry. The independent triazole-3-thione ligands employ the exocyclic-S atoms exclusively in coordination. One acts as a terminal S-ligand and the other in a bidentate (μ2) bridging mode to provide a link between two AgI centres. Each AgI atom is also coordinated by a terminal S-bound thiocyanate ligand, resulting in a distorted AgS4 tetrahedral coordination geometry. An intramolecular N—H...S(thiocyanate) hydrogen bond is noted. In the crystal, amine-N—H...S(thione), N—H...N(triazolyl) and N—H...N(thiocyanate) hydrogen bonds give rise to a three-dimensional architecture. The packing is consolidated by triazolyl-C—H...S(thiocyanate), triazolyl-C—H...N(thiocyanate) and S...S [3.2463 (9) Å] interactions as well as face-to-face π–π stacking between the independent triazolyl rings [inter-centroid separation = 3.4444 (15) Å]. An analysis of the calculated Hirshfeld surfaces shows the three major contributors are due to N...H/H...N, S...H/H...S and C...H/H...C contacts, at 35.8, 19.4 and 12.7%, respectively; H...H contacts contribute only 7.6% to the overall surface.

scholarly journals Steric control of supramolecular association in structures of Zn(S2COR)2 with N,N′-bis(pyridin-4-ylmethyl)oxalamide

2019 ◽  
Vol 234 (3) ◽  
pp. 165-175 ◽  
Author(s):  
Yee Seng Tan ◽  
Hao Zhe Chun ◽  
Mukesh M. Jotani ◽  
Edward R.T. Tiekink
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Hirshfeld Surfaces ◽  
Binuclear Molecule ◽  
Supramolecular Chain ◽  
The One ◽  
Distorted Tetrahedral Coordination ◽  
Cyclohexyl Group

Abstract The crystal and molecular structures of the one-dimensional coordination polymer [Zn(S2COEt)2(4LH2)]n (1) and binuclear [Zn(S2COCy)2]2(4LH2) (2) are described, where 4LH2 is N,N′-bis(pyridin-4-ylmethyl)ethanediamide. In 1, the Zn(S2COEt)2 entities are linked by bidentate bridging 4LH2 ligands through the pyridyl-N atoms to generate a twisted supramolecular chain. As a result of monodentate xanthate ligands, the N2S4 donor set defines a distorted tetrahedral coordination geometry and, crucially, allows the participation of the non-coordinating sulfur atoms in supramolecular association. Thus, in the crystal amide-N–H···O(amide) and amide-N–H···S(thione) hydrogen bonds link chains into a three-dimensional architecture. The substitution of the ethyl group in the xanthate ligand with a cyclohexyl group results in very different structural outcomes. In 2, a binuclear molecule is observed with the coordination geometry for zinc being defined by chelating xanthate ligands and a pyridyl-N atom with the NS4 donor set defining a highly distorted geometry. In the molecular packing, amide-N–H···S(thione) hydrogen bonds stabilise a supramolecular chain along the a-axis and these are connected into a three-dimensional arrangement by methylene-C–H···O and methylene-C–H···π(pyridyl) interactions. The relative importance of the specified intermolecular interactions and weaker, contributing contacts has been revealed by an analysis of the calculated Hirshfeld surfaces of 1 and 2.

scholarly journals The 1:2 co-crystal formed between N,N′-bis(pyridin-4-ylmethyl)ethanediamide and benzoic acid: crystal structure, Hirshfeld surface analysis and computational study

2020 ◽  
Vol 76 (1) ◽  
pp. 102-110 ◽  
Author(s):  
Sang Loon Tan ◽  
Edward R. T. Tiekink
Keyword(s):  
Hydrogen Bonds ◽  
Benzoic Acid ◽  
Computational Study ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Molecular Structures ◽  
Amide Hydrogen ◽  
Title 1 ◽  
Crystal And Molecular Structures ◽  
Hirshfeld Surfaces

The crystal and molecular structures of the title 1:2 co-crystal, C14H14N4O2·2C7H6O2, are described. The oxalamide molecule has a (+)-antiperiplanar conformation with the 4-pyridyl residues lying to either side of the central, almost planar C2N2O2 chromophore (r.m.s. deviation = 0.0555 Å). The benzoic acid molecules have equivalent, close to planar conformations [C6/CO2 dihedral angle = 6.33 (14) and 3.43 (10)°]. The formation of hydroxy-O—H...N(pyridyl) hydrogen bonds between the benzoic acid molecules and the pyridyl residues of the diamide leads to a three-molecule aggregate. Centrosymmetrically related aggregates assemble into a six-molecule aggregate via amide-N—H...O(amide) hydrogen bonds through a 10-membered {...HNC2O}2 synthon. These are linked into a supramolecular tape via amide-N—H...O(carbonyl) hydrogen bonds and 22-membered {...HOCO...NC4NH}2 synthons. The contacts between tapes to consolidate the three-dimensional architecture are of the type methylene-C—H...O(amide) and pyridyl-C—H...O(carbonyl). These interactions are largely electrostatic in nature. Additional non-covalent contacts are identified from an analysis of the calculated Hirshfeld surfaces.

scholarly journals Bis[2-(4,5-diphenyl-1H-imidazol-2-yl)-4-nitrophenolato]copper(II) dihydrate: crystal structure and Hirshfeld surface analysis

2019 ◽  
Vol 75 (11) ◽  
pp. 1664-1671 ◽  
Author(s):  
Sailesh Chettri ◽  
Dhiraj Brahman ◽  
Biswajit Sinha ◽  
Mukesh M. Jotani ◽  
Edward R. T. Tiekink
Keyword(s):  
Chelate Ring ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Bidentate Ligands ◽  
Metal Centre ◽  
Hirshfeld Surfaces ◽  
Square Planar ◽  
Intermolecular Contacts

The crystal and molecular structures of the title CuII complex, isolated as a dihydrate, [Cu(C21H14N3O3)2]·2H2O, reveals a highly distorted coordination geometry intermediate between square-planar and tetrahedral defined by an N2O2 donor set derived from two mono-anionic bidentate ligands. Furthermore, each six-membered chelate ring adopts an envelope conformation with the Cu atom being the flap. In the crystal, imidazolyl-amine-N—H...O(water), water-O—H...O(coordinated, nitro and water), phenyl-C—H...O(nitro) and π(imidazolyl)–π(nitrobenzene) [inter-centroid distances = 3.7452 (14) and 3.6647 (13) Å] contacts link the components into a supramolecular layer lying parallel to (101). The connections between layers forming a three-dimensional architecture are of the types nitrobenzene-C—H...O(nitro) and phenyl-C—H...π(phenyl). The distorted coordination geometry for the CuII atom is highlighted in an analysis of the Hirshfeld surface calculated for the metal centre alone. The significance of the intermolecular contacts is also revealed in a study of the calculated Hirshfeld surfaces; the dominant contacts in the crystal are H...H (41.0%), O...H/H...O (27.1%) and C...H/H...C (19.6%).

scholarly journals Some chalcones derived from thiophene-3-carbaldehyde: synthesis and crystal structures

2019 ◽  
Vol 75 (7) ◽  
pp. 957-963 ◽  
Author(s):  
Trung Vu Quoc ◽  
Duong Tran Thi Thuy ◽  
Thuan Dang Thanh ◽  
Thanh Phung Ngoc ◽  
Vuong Nguyen Thien ◽  
...  
Keyword(s):  
Potassium Hydroxide ◽  
Thiophene Ring ◽  
Three Dimensional ◽  
Ethanol Solution ◽  
Molecular Structures ◽  
Chain Formation ◽  
Axis Direction ◽  
Crystal And Molecular Structures ◽  
Phenyl Rings ◽  
Thiophene Derivatives

The synthesis, spectroscopic data and crystal and molecular structures of four 3-(3-phenylprop-1-ene-3-one-1-yl)thiophene derivatives, namely 1-(4-hydroxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C13H10O2S, (1), 1-(4-methoxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C14H12O2S, (2), 1-(4-ethoxyphenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C15H14O2S, (3), and 1-(4-bromophenyl)-3-(thiophen-3-yl)prop-1-en-3-one, C13H9BrOS, (4), are described. The four chalcones have been synthesized by reaction of thiophene-3-carbaldehyde with an acetophenone derivative in an absolute ethanol solution containing potassium hydroxide, and differ in the substituent at the para position of the phenyl ring: –OH for 1, –OCH3 for 2, –OCH2CH3 for 3 and –Br for 4. The thiophene ring in 4 was found to be disordered over two orientations with occupancies 0.702 (4) and 0.298 (4). The configuration about the C=C bond is E. The thiophene and phenyl rings are inclined by 4.73 (12) for 1, 12.36 (11) for 2, 17.44 (11) for 3 and 46.1 (6) and 48.6 (6)° for 4, indicating that the –OH derivative is almost planar and the –Br derivative deviates the most from planarity. However, the substituent has no real influence on the bond distances in the α,β-unsaturated carbonyl moiety. The molecular packing of 1 features chain formation in the a-axis direction by O—H...O contacts. In the case of 2 and 3, the packing is characterized by dimer formation through C—H...O interactions. In addition, C—H...π(thiophene) interactions in 2 and C—H...S(thiophene) interactions in 3 contribute to the three-dimensional architecture. The presence of C—H...π(thiophene) contacts in the crystal of 4 results in chain formation in the c-axis direction. The Hirshfeld surface analysis shows that for all four derivatives, the highest contribution to surface contacts arises from contacts in which H atoms are involved.

Crystal and molecular structures of boldenone and four boldenone steroid esters

2019 ◽  
Vol 234 (10) ◽  
pp. 671-683 ◽  
Author(s):  
Alexandru Turza ◽  
Maria O. Miclăuș ◽  
Aurel Pop ◽  
Gheorghe Borodi
Keyword(s):  
Crystal Structures ◽  
High Throughput ◽  
High Throughput Screening ◽  
Molecular Structures ◽  
Anabolic Androgenic Steroid ◽  
Crystal And Molecular Structures ◽  
Hirshfeld Surfaces ◽  
Intermolecular Contacts ◽  
Lattice Energies ◽  
Steroid Skeleton

Abstract Androsta-1,4-dien-17β-ol-3-one, also known as boldenone, is an anabolic-androgenic steroid derived from testosterone. The crystal structures of boldenone base, boldenone acetate, boldenone propionate, boldenone cypionate and a boldenone acetate polymorph obtained by high throughput screening were investigated. Hirshfeld surfaces and fingerprint plots breakdown revealed that the molecular packing in the crystals are driven by dominant H⋯H intermolecular contacts, followed by O⋯H/H⋯O contacts and to a lesser degree C⋯H/H⋯C contacts. The steroid skeleton rings, for all the reported compounds, adopt the following conformation: planar in A, chair in B and C, whereas C(13) envelope conformations are found for the five-membered D rings. The total lattice energies were calculated as a sum of four terms (Coulombic, polarization, dispersion, repulsion).

One-dimensional CuIand AgIladder-like coordination polymers supported by 2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole

2013 ◽  
Vol 69 (9) ◽  
pp. 1017-1021
Author(s):  
Liu-cheng Gui ◽  
Guang-ming Liang ◽  
Hua-hong Zou ◽  
Zhong Hou
Keyword(s):  
Hydrogen Bonds ◽  
Metal Ion ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Asymmetric Unit ◽  
Counter Anion ◽  
One Dimensional ◽  
Solvent Molecules ◽  
Distorted Tetrahedral Coordination

The title complexes, poly[[bis[μ2-2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole-κ2N1:N3]copper(I)] tetrafluoroborate acetonitrile monosolvate], {[Cu(C15H15N3)2]BF4·CH3CN}n, (I), and poly[[bis[μ2-2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole-κ2N1:N3]silver(I)] perchlorate methanol monosolvate], {[Ag(C15H15N3)2]ClO4·CH3OH}n, (II), are isostructural and exhibit one-dimensional ladder-like structures in which each asymmetric unit contains one metal ion (Cu+or Ag+), two 2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole (bep) ligands, one counter-anion (tetrafluoroborate or perchlorate) and one interstitial molecule (acetonitrile or methanol). Each metal ion exhibits a distorted tetrahedral coordination geometry consisting of two pyridyl and two benzimidazole N atoms from four distinct ligands. Two metal ions are linked by two bep ligands to form a centrosymmetric 18-memberedM2(bep)2metallacycle, while adjacentM2(bep)2metallacycles are further interlinked by another two bep ligands resulting in a ladder-like array. In the extended structure, four adjacent ladder-like arrays are connected together through C—H...F, O—H...O and C—H...O hydrogen bonds between bep ligands, solvent molecules and counter-anions into a three-dimensional supramolecular structure.

Kupfer(I)-Komplexe mit ungesättigten Stickstoffliganden, V / Kupfer(I)-Komplexe mit Diazadienen als Chelate und Brücken: Röntgenstrukturenuntersuchungen an (DAD)Cu(μ-Cl)2Cu(DAD), [(DAD)2Cu]⁺ (CuCl2)-, (DAD)CuCl, [μ-(DAD)2Cu5Cl5]n und [μ-(DAD)Cu(OTf)]n (DAD = Diazadien) / Copper(I) Complexes with Unsaturated Nitrogen Ligands, V Copper(I) Complexes with Chelating and Bridging Diazadienes: X-Ray Diffraction Studies of (DAD)Cu(μ-Cl)2Cu(DAD), [(DAD)2Cu]+ (CuCl2)-, (DAD)CuCl, [μ-(DAD)2Cu5Cl5]n and [μ-(DAD)Cu(OTf)]n (DAD = Diazadiene)

1990 ◽  
Vol 45 (10) ◽  
pp. 1369-1382 ◽  
Author(s):  
Heindirk tom Dieck ◽  
Lutz Stamp
Keyword(s):  
Coordination Polymer ◽  
Molecular Complexes ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Halide Ions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nitrogen Ligands ◽  
Crystal And Molecular Structures ◽  
Irregular Geometries

Diazadienes RN = CR′-CR′ = NR (DAD) form molecular complexes with copper(I) halides of composition (DAD)CuX, the structures of which vary from [(DAD)2Cu]+(CuCl2)⁻ with a non-tetrahedral bis(chelated) cation, over [(DAD)CuCl]2 with asymmetrically bridging chloro ligands to planar three-coordinate (DAD)CuCl. The composition of the isolated complexes depends on the relative concentrations or on the solvent. The “soft” coordination geometry of copper is underlined by the structure of the coordination polymer of composition (DAD)2Cu5Cl5, in which Cu atoms of coordination number 2, 3 and 4 and very irregular geometries are encountered and where the DAD ligands are exclusively bridging. Halide ions and sp2-nitrogen donors are very competitive. Bridging DAD ligands are also encountered in (DAD)Cu-Y with the less nucleophilic anions trifluoromethane-sulphonate or perchlorate. Crystal and molecular structures are established for all these coordination geometries and the causes are discussed for the coordination flexibility of copper(I)

Synthesis and Structural Characterization of the Mixed Ligand Complex [Cu(Hml)2(Phen)] · 2 H2O (H2ml = 2-Methyllactic Acid)

2003 ◽  
Vol 58 (1) ◽  
pp. 151-154 ◽  
Author(s):  
Rosa Carballo ◽  
Berta Covelo ◽  
Ezequiel M. Vázquez-Lópeza ◽  
Alfonso Castiñeiras ◽  
Juan Niclós
Keyword(s):  
Magnetic Measurements ◽  
Mixed Ligand Complex ◽  
Three Dimensional ◽  
Mixed Ligand ◽  
Water Molecules ◽  
Ligand Complex ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral

Abstract A new mixed-ligand complex of copper(II) with 1,10-phenanthroline and 2-methyllactate was prepared. [Cu(HmL)2(phen)] ·2H2O (where HmL = monodeprotonated 2-methyllactic acid) was characterized by elemental analysis, IR, electronic and EPR spectroscopy, magnetic measurements at room temperature, thermogravimetric analysis and X-ray diffractometry. The copper atom is in a tetragonally distorted octahedral environment and the 2-methyllactato ligand is bidentately chelating. The presence of lattice water molecules mediates the formation of a three-dimensional network.

THE CRYSTAL AND MOLECULAR STRUCTURES OF m-DINITROBENZENE AND p-DINITROBENZENE

1961 ◽  
Vol 39 (8) ◽  
pp. 1638-1644 ◽  
Author(s):  
J. Trotter
Keyword(s):  
Three Dimensional ◽  
Molecular Structures ◽  
Steric Effects ◽  
Crystal And Molecular Structures

The structures of m-dinitrobenzene and p-dinitrobenzene have been refined by three-dimensional (Fo—Fc) syntheses. The results indicate that both nitro groups in each molecule are twisted 11° out of the aromatic plane, about the C—N bonds, in contrast to nitrobenzene, where the whole molecule is completely planar. These molecular configurations are shown to be in accord with those which might be expected from intramolecular steric effects. The dimensions of the three molecules have also been compared.

Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XL. X-Ray Crystal Structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru, Os)

1995 ◽  
Vol 48 (11) ◽  
pp. 1887 ◽  
Author(s):  
MI Bruce ◽  
PJ Low ◽  
BW Skelton ◽  
ERT Tiekink ◽  
A Werth ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Chloro Complexes ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru and Os) have been determined. A revised synthesis of the bromo osmium complex is given. The coordination geometry about the metal atom is based on a distorted octahedron with one face being occupied by the cyclopentadienyl group [average Ru -C(Cp) 2.214(3), Os-C(Cp) 2.177(3)Ǻ] and the other by the bromide [ Ru -Br 2.5683(8), Os-Br 2.5438(9)Ǻ] and the two phosphorus atoms [ Ru -P 2.323(2), 2.329(1); Os-P 2.290(2), 2.297(2)Ǻ]. Structural parameters are compared with those of the corresponding chloro complexes and differ only minimally. Crystals of MBr (PPh3)2(η-C5H5).CH2Cl2 are triclinic, space group Pī , with unit cell dimensions ( Ru [Os]): a 14.374(5) [14.276(4)], b 14.057(4) [13.959(3)], c 10.012(5) [9.903(3)]Ǻ, α 99.43(3) [99.79(2)], β 105.60(3) [105.74(2)], γ 100.42(3) [100.39(2)]°, V 1868(1) [1817.7(9)] Ǻ3, Z 2. The structures were refined by a full-matrix least-squares procedure to R 0.050 [0.036] for 7365 [5108] reflections with I ≥ 3σ(I).

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