scholarly journals Hydrogen-Bonded Networks Based on Cobalt(II), Nickel(II), and Zinc(II) Complexes of N,N'-Diethylurea

2010 ◽  
Vol 2010 ◽  
pp. 1-12 ◽  
Author(s):  
Labrini Drakopoulou ◽  
Catherine P. Raptopoulou ◽  
Aris Terzis ◽  
Giannis S. Papaefstathiou
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Vibrational Spectroscopy ◽  
Supramolecular Structures ◽  
Counter Ion ◽  
Structure Determinations ◽  
Hydrogen Bonded

N,N'-diethylurea (DEU) was employed as a ligand to form the octahedral complexes[M(DEU)6]2+(M=Co, Ni and Zn). Compounds[Co(DEU)6](BF4)2(1),[Co(DEU)6](CIO4)2(2),[Ni(DEU)6](CIO4)2(3), and[Zn(DMU)6](CIO4)2(4) have been prepared from the reactions of DEU and the appropriate hydrated metal(II) salts in EtOH in the presence of 2,2-dimethoxypropane. Crystal structure determinations demonstrate the existence of[M(DEU)6]2+cations andCIO4-(in2–4) orBF4-(in1) counterions. The[M(DEU)6]2+cations in the solid state are stabilized by apseudochelateeffect due to the existence of six strong intracationicN-H⋯O(DEU)hydrogen bonds. The[M(DEU)6]2+cations and counterions self-assemble to form hydrogen-bonded 2D architectures in2–4that conform to thekgd(kagome dual) network, and a 3D hydrogen-bondedrtl(rutile) network in1. The nature of the resulting supramolecular structures is influenced by the nature of the counter-ion. The complexes were also characterized by vibrational spectroscopy (IR).

The Hexakis(N,N'-Dimethylurea)Cobalt(Ii) Cation: A Flexible Building Block for the Construction of Hydrogen Bonded Networks

2003 ◽  
Vol 58 (1) ◽  
pp. 74-84 ◽  
Author(s):  
Giannis S. Papaefstathiou ◽  
Robby Keuleers ◽  
Constantinos J. Milios ◽  
Catherine P. Raptopoulou ◽  
Aris Terzis ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Spectroscopic Data ◽  
Low Frequency ◽  
Great Stability ◽  
Structure Determinations ◽  
Interionic Hydrogen ◽  
Hydrogen Bonded

AbstractThe ligand N.N'-dimethylurea (DMU) is used to propagate the octahedral coordination geom- etry of [Co(DMU)6]2+ into 1D and 2D assemblies via a combination of coordinative bonds and interionic hydrogen-bonding. Compounds [Co(DMU)6](ClO4)2 (1), [Co(DMU)6](BF4)2 (2) and [Co(DMU)6](NO3)2 (3) have been prepared from the reactions of DMU and the appropriate hydrated cobalt(II) salts in EtOH. MeCN or Me2CO (only for 1) in the presence of 2,2-di- methoxypropane. Crystal structure determinations demonstrate the existence of [Co(DMU)6]2+ cations and CIO4- , BF4- or NO3- counterions. The great stability of the [Co(DMU)6]2+ cation in the solid state is attributed to a pseudochelate effect which arises from the existence of strong intracationic N-H···O(DMU) hydrogen bonds. The [Co(DMU)6]2+ cations and counterions self- assemble to form a hydrogen-bonded ID architecture in 1, and different 2D hydrogen-bonded networks in 2 and 3. The precise nature of the resulting supramolecular structure is influenced by the nature of the counterion. Two main motifs of intermolecular (interionic) hydrogen bonds have been observed: N-H ···O(ClO4-, NO3-) or N-H ··· F(BF4-) and weak C-H F(BF4- ) or C-H-O(NO3- ) hydrogen bonds. The complexes were also characterized by vibrational spec- troscopy (IR, far-IR. low-frequency Raman). The spectroscopic data are discussed in terms of the nature of bonding and the know;n structures.

Temperature- and solvate-dependent disorder in the crystal structure of [PNP]+[HSO4]−

2019 ◽  
Vol 74 (4) ◽  
pp. 373-379
Author(s):  
Carsten Jenne ◽  
Marc C. Nierstenhöfer
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystals ◽  
Vibrational Spectroscopy ◽  
Diethyl Ether ◽  
Water Yield ◽  
Decomposition Products ◽  
Partial Decomposition

AbstractMetathesis reactions of [PNP]Cl ([PNP]+ ≡ bis(triphenyl-λ5-phosphanylidene)ammonium) with Na2[SO4] or K[HSO4] in water yield [PNP]2[SO4] and [PNP][HSO4], respectively, as colorless solids. Reactions under basic conditions lead to a partial decomposition of the weakly coordinating [PNP]+ cation. N-Diphenylphosphine-triphenylphosphazene, triphenylphosphinimine, and benzene were identified as decomposition products by NMR spectroscopy. The compounds [PNP]2[SO4] and [PNP][HSO4] were characterized by multinuclear NMR and vibrational spectroscopy. [PNP][HSO4] could be crystallized from acetonitrile-diethyl ether giving single crystals with and without additional acetonitrile solvate molecules. The [HSO4]− anions form dimers in the solid state in both structures, which are held together by O–H⋯O hydrogen bonds. At T = 127 K the [HSO4]− anions in the crystal structure of solvate free [PNP][HSO4] are ordered, while at T = 300 K and in the structure containing additional acetonitrile solvate molecules a disorder of the [HSO4]− anions over two positions is observed, for the latter even at 150 K.

Heterocyclic Tautomerism. IV. The Solution and Crystal Structures of 1-Aryl-3-phenyl-1,2,4-triazol-5-ones

1988 ◽  
Vol 41 (4) ◽  
pp. 419 ◽  
Author(s):  
AD Rae ◽  
CG Ramsay ◽  
PJ Steel
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Crystal Structures ◽  
Complex Network ◽  
Water Molecules ◽  
X Ray ◽  
Structure Determinations ◽  
Hydrogen Bonded

The title compounds are shown to exist in solution and in the solid state as 4H-tautomers. X-Ray crystal structure determinations show that 1,3-diphenyl-1,2,4-triazol-5-one exists as a dimeric pair of strongly hydrogen-bonded molecules and that 3-phenyl-1-(2-pyridyl)-1,2,4- triazol-5-one exists as the 4H-tautomer stabilized by a complex network of hydrogen bonding to water molecules.

Model compounds of aromatic nylons. 3. The conformation of the 4T Nylon, poly(tetramethylene terephthalamide), using X-ray diffraction, solid-state 13C nmr spectroscopy and ir spectroscopy

1989 ◽  
Vol 67 (5) ◽  
pp. 840-849 ◽  
Author(s):  
Josée Brisson ◽  
Johanne Gagné ◽  
François Brisse
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Solid State Nmr ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Model Compounds ◽  
X Ray ◽  
Structure Determinations

Three model compounds of poly(tetramethylene terephthalamide) or 4T Nylon have been synthesized and characterized using single crystal X-ray diffractometry, infrared spectroscopy, and 13CCP/MAS nmr spectroscopy. The model compounds are the para-substituted N,N′-tetramethylene dibenzamides, where the substituents are the—OMe, —tBu, —CN, and —CH3 groups. The crystal structure determinations reveal three distinct conformations for the CO—NH—(CH2)4—NH—CO sequence of atoms. The conformation is all trans for OMe, tgtttg−t for the tBu substituent, and tsttts−t for the CN substituent ([Formula: see text], [Formula: see text], and [Formula: see text]). In all three derivatives, the dihedral angle between the aromatic ring and the amide plane is around 30°. The OMe and tBu para-substituted molecules are interconnected by nearly linear hydrogen bonds of normal N … O distances. However, for the CN derivative the N … O distance is exceptionally short, 2.402(4) Å. On the basis of its infrared and solid state nmr spectra, it is proposed that N,N′-tetramethylene di-para-methyl benzamide has a crystal structure comparable to that of its unsubstituted analog. The methylenic sequence of the parent polyamide, 4T Nylon, has the tgtttg−t conformation. Furthermore, the polyamide chains form sheets within which the chains, parallel to one another, are connected through hydrogen bonds. Keywords: polyamide, crystal structure, solid-state nmr.

scholarly journals Organotin(IV) selenate derivatives – Crystal structure of [{(Ph3Sn)2SeO4} ⋅ CH3OH] n

2021 ◽  
Vol 44 (1) ◽  
pp. 213-217
Author(s):  
Waly Diallo ◽  
Hélène Cattey ◽  
Laurent Plasseraud
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Point Of View ◽  
Intermolecular Hydrogen Bonds

Abstract Crystallization of [(Ph3Sn)2SeO4] ⋅ 1.5H2O in methanol leads to the formation of [{(Ph3Sn)2SeO4} ⋅ CH3OH] n (1) which constitutes a new specimen of organotin(IV) selenate derivatives. In the solid state, complex 1 is arranged in polymeric zig-zag chains, composed of alternating Ph3Sn and SeO4 groups. In addition, pendant Ph3Sn ⋅ CH3OH moieties are branched along chains according to a syndiotactic organization and via Sn-O-Se connections. From a supramolecular point of view, intermolecular hydrogen bonds established between the selenate groups (uncoordinated oxygen) and the hydroxyl functions (CH3OH) of the pendant groups link the chains together.

scholarly journals Spectroscopic, X-ray Diffraction and Density Functional Theory Study of Intra- and Intermolecular Hydrogen Bonds in Ortho-(4-tolylsulfonamido)benzamides

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 926
Author(s):  
Malose J. Mphahlele ◽  
Eugene E. Onwu ◽  
Marole M. Maluleka
Keyword(s):  
Density Functional Theory ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Density Functional ◽  
Tetrahedral Geometry ◽  
Hindered Rotation ◽  
Hydrogen Bond Acceptor ◽  
Functional Theory ◽  
Vis Spectroscopy ◽  
Hydrogen Bonded

The conformations of the title compounds were determined in solution (NMR and UV-Vis spectroscopy) and in the solid state (FT-IR and XRD), complemented with density functional theory (DFT) in the gas phase. The nonequivalence of the amide protons of these compounds due to the hindered rotation of the C(O)–NH2 single bond resulted in two distinct resonances of different chemical shift values in the aromatic region of their 1H-NMR spectra. Intramolecular hydrogen bonding interactions between the carbonyl oxygen and the sulfonamide hydrogen atom were observed in the solution phase and solid state. XRD confirmed the ability of the amide moiety of this class of compounds to function as a hydrogen bond acceptor to form a six-membered hydrogen bonded ring and a donor simultaneously to form intermolecular hydrogen bonded complexes of the type N–H···O=S. The distorted tetrahedral geometry of the sulfur atom resulted in a deviation of the sulfonamide moiety from co-planarity of the anthranilamide scaffold, and this geometry enabled oxygen atoms to form hydrogen bonds in higher dimensions.

scholarly journals 1,1′,3,3′-Tetramesitylquinobis(imidazole)-2,2′-dithione

IUCrData ◽  
2019 ◽  
Vol 4 (9) ◽  
Author(s):  
Jayaraman Selvakumar ◽  
Kuppuswamy Arumugam
Keyword(s):  
Crystal Structure ◽  
Molecular Weight ◽  
Solid State ◽  
Structural Analysis ◽  
Hydrogen Bonds ◽  
Cell Volume ◽  
Title Compound ◽  
Unit Cell Volume ◽  
Density Peaks ◽  
Solvent Molecules

The solid-state structural analysis of the title compound [systematic name: 5,11-disulfanylidene-4,6,10,12-tetrakis(2,4,6-trimethylphenyl)-4,6,10,12-tetraazatricyclo[7.3.0.03,7]dodeca-1(9),3(7)-diene-2,8-dione], C44H44N4O2S2 [+solvent], reveals that the molecule crystallizes in a highly symmetric cubic space group so that one quarter of the molecule is crystallographically unique, the molecule lying on special positions (two mirror planes, two twofold axes and a center of inversion). The crystal structure exhibits large cavities of 193 Å3 accounting for 7.3% of the total unit-cell volume. These cavities contain residual density peaks but it was not possible to unambiguously identify the solvent therein. The contribution of the disordered solvent molecules to the scattering was removed using a solvent mask and is not included in the reported molecular weight. No classical hydrogen bonds are observed between the main molecules.

scholarly journals 6-Methyl-2-oxo-N-(quinolin-6-yl)-2H-chromene-3-carboxamide: crystal structure and Hirshfeld surface analysis

2016 ◽  
Vol 72 (8) ◽  
pp. 1121-1125
Author(s):  
Lígia R. Gomes ◽  
John Nicolson Low ◽  
André Fonseca ◽  
Maria João Matos ◽  
Fernanda Borges
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Dihedral Angle ◽  
Surface Analysis ◽  
Coumarin Derivative ◽  
Hirshfeld Surface ◽  
Supramolecular Structures ◽  
Hirshfeld Surface Analysis ◽  
Quinoline Ring ◽  
Π Interactions

The title coumarin derivative, C20H14N2O3, displays intramolecular N—H...O and weak C—H...O hydrogen bonds, which probably contribute to the approximate planarity of the molecule [dihedral angle between the coumarin and quinoline ring systems = 6.08 (6)°]. The supramolecular structures feature C—H...O hydrogen bonds and π–π interactions, as confirmed by Hirshfeld surface analyses.

scholarly journals Crystal structure and Hirshfeld surface analysis of 2,4-diamino-6-phenyl-1,3,5-triazin-1-ium 4-methylbenzenesulfonate

2018 ◽  
Vol 74 (8) ◽  
pp. 1159-1162
Author(s):  
Ramalingam Sangeetha ◽  
Kasthuri Balasubramani ◽  
Kaliyaperumal Thanigaimani ◽  
Savaridasson Jose Kavitha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Intermolecular Interactions ◽  
Hirshfeld Surface ◽  
Amino Group ◽  
Asymmetric Unit ◽  
Graph Set ◽  
Molecular Salt ◽  
Sulfonate Anion ◽  
Hydrogen Bonded

In the title molecular salt, C9H10N5 +·C7H7O3S−, the asymmetric unit consists of a 2,4-diamino-6-phenyl-1,3,5-triazin-1-ium cation and a 4-methylbenzenesulfonate anion. The cation is protonated at the N atom lying between the amine and phenyl substituents. The protonated N and amino-group N atoms are involved in hydrogen bonding with the sulfonate O atoms through a pair of intermolecular N—H...O hydrogen bonds, giving rise to a hydrogen-bonded cyclic motif with R 2 2(8) graph-set notation. The inversion-related molecules are further linked by four N—H...O intermolecular interactions to produce a complementary DDAA (D = donor, A = acceptor) hydrogen-bonded array, forming R 2 2(8), R 4 2(8) and R 2 2(8) ring motifs. The centrosymmetrically paired cations form R 2 2(8) ring motifs through base-pairing via N—H...N hydrogen bonds. In addition, another R 3 3(10) motif is formed between centrosymetrically paired cations and a sulfonate anion via N—H...O hydrogen bonds. The crystal structure also features weak S=O...π and π–π interactions. Hirshfeld surface and fingerprint plots were employed in order to further study the intermolecular interactions.

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