Syntheses, characterization, and X-ray crystal structures of diorganotin(IV) derivatives of 2-pyridinethiolato-N-oxide

2003 ◽  
Vol 81 (10) ◽  
pp. 1070-1075 ◽  
Author(s):  
Chunlin Ma ◽  
Junhong Zhang ◽  
Rufen Zhang
Keyword(s):  
Crystal Structure ◽  
Stacking Interactions ◽  
X Ray ◽  
X Ray Crystallography ◽  
Nmr Data ◽  
Π Stacking ◽  
Oxide Crystal ◽  
Distorted Trigonal Bipyramid ◽  
Π Stacking Interaction ◽  
Derivatives Of

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. The tin environment is a distorted trigonal bipyramid with the Cl and oxygen atoms in apical positions. Both complexes exhibit strong π–π stacking interactions. Key words: diorganotin, π–π stacking interaction, 2-pyridinethiolato-N-oxide, crystal structure.

2,2'-Bipyridine Mercury(II) Complexes [Hg(bpy)(NO2)X] (X = NO2 –, SCN– , CH3COO–); Π-Π Stacking In The Crystal Structure Of [Hg(bpy)(NO2)2]

2005 ◽  
Vol 60 (3) ◽  
pp. 289-293 ◽  
Author(s):  
Ali Ramazani ◽  
Ali Morsali ◽  
Leila Dolatyari ◽  
Bijan Ganjeie
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Aromatic Rings ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Coordinate Geometry ◽  
C Nmr

The mercury(II) complexes of 2,2′-bipyridine (bpy), [Hg(bpy)(NO2)2], [Hg(bpy)(NO2) (CH3COO)], and [Hg(bpy)(NO2)(NCS)] have been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The structure of [Hg(bpy)(NO2)2] has been confirmed by X-ray crystallography. The complex is a monomer and the Hg atom has an unsymmetrical six-coordinate geometry, formed by two nitrogen atoms of the bpy ligand and four oxygen atoms of the two nitrite anions. There is a short intermolecular π-π stacking interaction between parallel aromatic rings

X-ray Crystal Structure of Gallium Tris- (8-hydroxyquinoline):  Intermolecular π−π Stacking Interactions in the Solid State

1999 ◽  
Vol 11 (3) ◽  
pp. 530-532 ◽  
Author(s):  
Yue Wang ◽  
Weixing Zhang ◽  
Yanqin Li ◽  
Ling Ye ◽  
Guangdi Yang
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Stacking Interactions ◽  
X Ray ◽  
Π Stacking

Synthesis and characterization of a linked, π-π stacked organotin compound of 2-mercapto-6-nitrobenzothiazolyl diphenyltin chloride with 2-ethoxyl-6-nitrobenzothiazole

2003 ◽  
Vol 81 (7) ◽  
pp. 825-831 ◽  
Author(s):  
Chunlin Ma ◽  
Qin Jiang ◽  
Rufen Zhang
Keyword(s):  
Title Compound ◽  
Organotin Compound ◽  
X Ray Diffraction ◽  
X Ray ◽  
Stacking Interaction ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Molecular Components

The new organotin compound, Ph2Sn(Cl)[S(C7H3N2O2S)]·[(C7H3N2O2S)OEt], assembled by an intermolecular aromatic benzothiazole–benzothiazole π-π stacking interaction, has been synthesized by the reaction of diphenyltin dichloride with 2-mercapto-6-nitrobenzothiazole. The title compound was characterized by elemental, IR, 1H NMR, and X-ray crystallography analyses. Single-crystal X-ray diffraction data reveals that the title compound has two different molecular components. The component Ph2Sn(Cl)[S(C7H3N2O2S)] has a pentacoordinate tin, which further forms an infinite one-dimensional chain by intermolecular non-bonded Cl···S interactions, resulting in an intercalation lattice that holds (C7H3N2O2S)OEt molecules. The formation of the molecule (C7H3N2O2S)OEt as well as its intercalated mechanism has also been discussed.Key words: organotin, assemble, π-π stacking interaction, 2-mercapto-6-nitrobenzothiazole, non-bonded interaction, crystal structure.

Triazene derivatives of (1,x-)diazacycloalkanes. Part VI. 3-({5,5-Dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines — Synthesis, characterization, and X-ray crystal structure

2006 ◽  
Vol 84 (10) ◽  
pp. 1294-1300 ◽  
Author(s):  
Keith Vaughan ◽  
Shasta Lee Moser ◽  
Reid Tingley ◽  
M Brad Peori ◽  
Valerio Bertolasi
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Ion Trapping ◽  
Published Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diazonium Ion ◽  
Derivatives Of ◽  
C Nmr

Reaction of a series of diazonium salts with a mixture of formaldehyde and 1,2-diamino-2-methylpropane affords the 3-({5,5-dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines (1a–1f) in excellent yield. The products have been characterized by IR and NMR spectroscopic analysis, elemental analysis, and X-ray crystallography. The X-ray crystal structure of the p-methoxycarbonyl derivative (1c) establishes without question the connectivity of these novel molecules, which can be described as linear bicyclic oligomers with two imidazolidinyl groups linked together by a one-carbon spacer. This is indeed a rare molecular building block. The molecular structure is corroborated by 1H and 13C NMR data, which correlates with the previously published data of compounds of types 5 and 6 derived from 1,3-propanediamine. The triazene moieties in the crystal of 1c display significant π conjugation, which gives the N—N bond a significant degree of double-bond character. This in turn causes restricted rotation around the N—N bond, which leads to considerable broadening of signals in both the 1H and 13C NMR spectra. The molecular ion of the p-cyanophenyl derivative (1b) was observed using electrospray mass spectrometry (ES + Na). The mechanism of formation of molecules of type 1 is proposed to involve diazonium ion trapping of the previously unreported bisimidazolidinyl methane (13).Key words: triazene, bistriazene, imidazolidine, synthesis, X-ray crystallography, NMR spectroscopy.

scholarly journals Noncovalent Interactions between 1,3,5-Trifluoro-2,4,6-triiodobenzene and a Series of 1,10-Phenanthroline Derivatives: A Combined Theoretical and Experimental Study

Crystals ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 140 ◽  
Author(s):  
Yu Zhang ◽  
Jian-Ge Wang ◽  
Weizhou Wang
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Quantum Chemical ◽  
Halogen Bond ◽  
Noncovalent Interactions ◽  
Stacking Interactions ◽  
Halogen Bonds ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Structural Competition

How many strong C−I⋯N halogen bonds can one 1,3,5-trifluoro-2,4,6-triiodobenzene molecule form in a crystal structure? To answer this question, we investigated in detail the noncovalent interactions between 1,3,5-trifluoro-2,4,6-triiodobenzene and a series of 1,10-phenanthroline derivatives by employing a combined theoretical and experimental method. The results of the quantum chemical calculations and crystallographic experiments clearly show that there is a structural competition between a C−I⋯N halogen bond and π⋯π stacking interaction. For example, when there are much stronger π⋯π stacking interactions between two 1,10-phenanthroline derivative molecules or between two 1,3,5-trifluoro-2,4,6-triiodobenzene molecules in the crystal structures, then one 1,3,5-trifluoro-2,4,6-triiodobenzene molecule forms only one C−I⋯N halogen bond with one 1,10-phenanthroline derivative molecule. Another example is when π⋯π stacking interactions in the crystal structures are not much stronger, one 1,3,5-trifluoro-2,4,6-triiodobenzene molecule can form two C−I⋯N halogen bonds with two 1,10-phenanthroline derivative molecules.

Synthesis and crystal structure of a novel prochiral ketoimine: (E)-acetophenoneO-diphenylphosphoryl oxime

2015 ◽  
Vol 71 (3) ◽  
pp. 181-184
Author(s):  
Sean H. Majer ◽  
Joseph M. Tanski
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Stacking Interactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Face To Face ◽  
Π Stacking

A novel activated prochiral ketoimine, (E)-acetophenoneO-diphenylphosphoryl oxime, C20H18NO2P, with an electron-withdrawing substituent on the imine N atom similar to other prochiral ketoimines, has been synthesized and the X-ray crystal stucture determined. The molecules pack together in the solid stateviaweak intermolecular C—H...O interactions and both face-to-face and edge-to-face π-stacking interactions.

scholarly journals Synthesis, characterization and crystal structure of platinum(II) complexes with thiourea derivative ligands

2018 ◽  
Vol 9 (4) ◽  
pp. 360-368
Author(s):  
Ebru Keskin ◽  
Ummuhan Solmaz ◽  
Gun Binzet ◽  
Ilkay Gumus ◽  
Hakan Arslan
Keyword(s):  
Single Crystal ◽  
Weak Interactions ◽  
Platinum Complexes ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Thiourea Derivatives ◽  
X Ray ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
In Cis

Thiourea derivatives [N-(di-n-propylcarbamothioyl)-4-fluorobenzamide (HL1) and N-(di-n-propylcarbamothioyl)-4-bromobenzamide (HL2)] and their platinum complexes have been successfully synthesized and structurally characterized by spectroscopic 1H NMR, 13C NMR, COSY, HMQC, and FT-IR techniques. The structure of both complexes was also confirmed by single crystal X-ray diffraction studies. The study of X-ray single crystal diffraction shows that the supramolecular aggregation of the complexes is stabilized via weak interactions as well as stacking interactions such as C-H···π and π···π. The cis-[Pt(L1-S,O)2 showed C–H···π and π···π stacking interactions, whereas only C–H···π stacking interaction was observed in cis-[Pt(L2-S,O)2]. In addition, the strong classical and non-classical intermolecular hydrogen bonds are not found in the prepared complexes. Therefore, it can be said that the C–H···π and π···π stacking interactions play an important role in the formation of supramolecular structures of the complexes.

scholarly journals Sildenafil–Resorcinol Cocrystal: XRPD Structure and DFT Calculations

Crystals ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1126
Author(s):  
Rafael Barbas ◽  
Vineet Kumar ◽  
Oriol Vallcorba ◽  
Rafel Prohens ◽  
Antonio Frontera
Keyword(s):  
Crystal Structure ◽  
Dft Calculations ◽  
Density Functional ◽  
Molecular Electrostatic Potential ◽  
Noncovalent Interaction ◽  
Functional Theory ◽  
X Ray ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Interaction Plot

Herein, the X-ray powder diffraction (XRPD) crystal structure of a new Sildenafil cocrystal is reported, where resorcinol has been used as the coformer. The crystal structure has been solved by means of direct space methods used in combination with density functional theory (DFT) calculations. In the structure, the Sildenafil and resorcinol molecules form cooperative hydrogen bond (HB) and π-stacking interactions that have been analyzed using DFT calculations, the molecular electrostatic potential (MEP) surface, and noncovalent interaction plot (NCI plot). The formation of O–H⋯N H-bonds between resorcinol and Sildenafil increases the dipole moment and enhances the antiparallel π-stacking interaction.

scholarly journals Synthetic Studies on Potent Marine Drugs: Synthesis and the Crystal Structure of 6-tert-butyl-4-phenyl-4H-chromene-2-carboxylic Acid

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Hui-Jing Li ◽  
Jun-Li Wang ◽  
Rui Wang ◽  
Dong-Hui Luo ◽  
Yan-Chao Wu
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Carboxylic Acid ◽  
Methyl Ester ◽  
Crystallographic Analysis ◽  
Antitumor Antibiotic ◽  
Stacking Interactions ◽  
X Ray ◽  
Structural Activity Relationship ◽  
Derivatives Of

4H-Chromene-2-carboxylic acid ester derivatives of renieramycin M might be of use for the structural-activity relationship studies of antitumor antibiotic tetrahydroisoquinoline natural products. Accordingly, 6-tert-butyl-4-phenyl-4H-chromene-2-carboxylic acid, one key intermediate, was synthesized via the condensation of (3E)-2-oxo-4-phenylbut-3-enoate methyl ester with 4-tert-butylphenol in the presence of AuCl3/3AgOTf (5 mol%), followed by cyclodehydration and aqueous hydrolysis. The product was unambiguously shown to the 4H-chromene-2-carboxylic acid by spectroscopy and X-ray crystallographic analysis. A packing diagram of the crystal structure shows that aromaticπ-stacking interactions and O–H⋯O hydrogen bond stabilize the structure in the solid.

Dimethyltellurium(IV) derivatives with mixed 1,1-dithio ligands. Crystal structures of Me2Te[S2CNMe2][S2COEt] and Me2Te[S2CNEt2][S2COMe]

1999 ◽  
Vol 77 (7) ◽  
pp. 1262-1273 ◽  
Author(s):  
John E Drake ◽  
Layla N Khasrou ◽  
Anil G Mislankar ◽  
Raju Ratnani
Keyword(s):  
Lone Pair ◽  
Mixed Ligand ◽  
Equatorial Position ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Secondary Interactions ◽  
Infrared And Raman Spectroscopy ◽  
Distorted Trigonal Bipyramid ◽  
Derivatives Of

Mixed ligand derivatives of Me2TeLL'2, where L = N,N-dialkyl dithiocarbamate or O,O-alkylene dithiophosphate and L' = O-alkyl dithiocarbonate, have been synthesized and characterized by elemental analysis, 1H, 13C, 31P, and 125Te NMR spectroscopy and infrared and Raman spectroscopy, and X-ray crystallography. Me2Te[S2CNMe2][S2COEt], 8: P[Formula: see text] (no. 2), with cell parameters a = 10.073(3) Å, b = 10.139(2) Å, c = 9.108(2) Å, α = 92.36(2)°, β = 115.55(2)°, γ = 111.19(2)°, V = 760.7(4) Å3, Z = 2, R = 0.0343, Rw = 0.0296. Me2Te[S2CNEt2][S2COMe], 9: P21/c (no. 14) with cell parameters a = 9.881(4) Å, b = 17.671(3) Å, c = 10.149(4) Å, β = 113.65(3)°, V = 1623.3(10) Å3, Z = 4, R = 0.0567, Rw = 0.0514. The immediate environment about tellurium in both molecules is essentially that of a saw-horse structure in which the lone pair is apparently stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. The S-Te-S angles in the two molecules are 166.87(6)° and 162.0(1)° for 8 and 9, respectively. In both molecules, the Te—S bonds to the dithiocarbamate groups are slightly shorter than those to dithiocarbonates. The dithiocarbamate groups are oriented to give secondary interactions involving the apparently terminal sulfur atoms resulting in Te—S distances of 3.205(2) and 3.277(4) Å, respectively, in 8 and 9. However, only in 9 is there a similar Te—S distance of 3.346(5) Å involving the S2COMe group because in 8, the OEt group of S2COEt, rather than the terminal S atom, is oriented toward Te. Key words: structure, tellurium, methyl, dithiocarbamates, dithiocarbonates, dithiophosphates.

Sign in / Sign up

Export Citation Format

Share Document