Stabilizing, non-covalent interactions in the solid state structure of novel aryltin hydrides and halogenides

2014 ◽  
Vol 92 (6) ◽  
pp. 556-564 ◽  
Author(s):  
Cathrin Zeppek ◽  
Roland C. Fischer ◽  
Ana Torvisco ◽  
Frank Uhlig
Keyword(s):  
Solid State ◽  
Intermolecular Interactions ◽  
Structural Parameters ◽  
State Structure ◽  
X Ray Diffraction ◽  
Aromatic Substituent ◽  
X Ray ◽  
Π Interactions ◽  
Non Covalent Interactions ◽  
Covalent Interactions

A group of novel aryltin chlorides, bromides and hydrides (ArnSnY4-n) (Ar = o-tolyl, 2,6-xylyl, 1-naphthyl, 2-naphthyl, p-n-butylphenyl; Y = Cl, Br, H) have been synthesized and structurally characterized via X-ray diffraction. These compounds display noncovalent intermolecular interactions in the form of edge to face, π–π stacking and C–H···π interactions resulting in discrete arrangements in the solid state. The strength of these interactions and their effect on resulting structural parameters, as well as the consequence of the aromatic substituent on the type of interactions present, will be highlighted and discussed.

scholarly journals A Comparative Theoretical and Spectroscopic Study of Aminomethylbenzoic Acid Derivatives as Potential NLO Candidates

2020 ◽  
Vol 3 (1) ◽  
pp. 102
Author(s):  
Amani Direm ◽  
Koray Sayın
Keyword(s):  
Nmr Spectra ◽  
Close Agreement ◽  
Molecular Electrostatic Potential ◽  
Structural Parameters ◽  
13C Nmr Spectra ◽  
X Ray Diffraction ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Non Covalent Interactions ◽  
Covalent Interactions

Three aminomethylbenzoic acid derivatives were theoretically studied at M062X/6-311++G(d,p) level in a vacuum, namely 2-ammonio-5-methylcarboxybenzene perchlorate (1), 4-(ammoniomethyl) carboxybenzene nitrate (2) and 4-(ammoniomethyl)carboxybenze perchlorate (3). The compounds’ structures were fully optimized and compared with the single-crystal X-ray diffraction results, showing a very close agreement with the experimental structural parameters. Their IR, 1H- and 13C-NMR spectra were calculated and examined in detail. Furthermore, the molecular electrostatic potential (MEP) maps of the studied compounds were investigated and the strength of the non-covalent interactions evaluated. In addition to these results, the NLO properties of the three compounds were predicted.

Unprecedented Hexa- and Undecanuclear Frameworks of Two New Tin(IV) Oxo Clusters Resulting from Partial Debenzylation Reactions

2010 ◽  
Vol 65 (11) ◽  
pp. 1293-s1308 ◽  
Author(s):  
Laurent Plasseraud ◽  
Hélène Cattey ◽  
Philippe Richard
Keyword(s):  
Solid State ◽  
1H Nmr Spectroscopy ◽  
Trifluoromethanesulfonic Acid ◽  
Synthetic Route ◽  
State Structure ◽  
X Ray Diffraction ◽  
Neutral Cluster ◽  
Broad Resonance ◽  
X Ray ◽  
The Core

A new and facile synthetic route to the known neutral cluster ((PhCH2)2SnO)6[((PhCH2)2SnOH)2- (CO3)]2 (2) as well as its reactivity toward trifluoromethanesulfonic acid (HO3SCF3, TfOH) are reported. The solid-state structure of the new solvate 2·6C7H8 has been determined by single-crystal X-ray diffraction. The core of 2 can be described as a pair of coplanar pentanuclear [(PhCH2)2SnO]5 ladders bridged at their ends by two carbonate groups. Successive additions of TfOH to a suspension of 2 in CD3CN were monitored by 119Sn{1H} NMR spectroscopy showing the transformation of the fingerprint of 2 (δ = −244, −246, −306 ppm), via new upfield signals, to a final broad resonance located at δ = −474 ppm. Thereafter, two unprecedented ionic monobenzyltin(IV) oxo clusters, 3 and 4, resulting from a debenzylation reaction and exhibiting unusual hexa- and undecanuclear frameworks, respectively, have been isolated as single crystals.

scholarly journals Solid-State Structures and Photoluminescence of Lamellar Architectures of Cu(I) and Ag(I) Paddlewheel Clusters with Hydrogen-Bonded Polar Guests

Molecules ◽  
2021 ◽  
Vol 26 (21) ◽  
pp. 6731
Author(s):  
Haruki Inoue ◽  
Yuga Yamashita ◽  
Yoshiki Ozawa ◽  
Toshikazu Ono ◽  
Masaaki Abe
Keyword(s):  
Solid State ◽  
Diffuse Reflectance Spectroscopy ◽  
X Ray Diffraction ◽  
Uv Illumination ◽  
Near Ir ◽  
Carboxylic Groups ◽  
Dta Analysis ◽  
Non Covalent Interactions ◽  
Solid State Structures ◽  
Covalent Interactions

Two hexanuclear paddlewheel-like clusters appending six carboxylic-acid pendants have been isolated with the inclusion of polar solvent guests: [Cu6(Hmna)6]·7DMF (1·7DMF) and [Ag6(Hmna)6]·8DMSO (2·8DMSO), where H2mna = 2-mercaptonicotininc acid, DMF = N,N’-dimethylformamide, and DMSO = dimethyl sulfoxide. The solvated clusters, together with their fully desolvated forms 1 and 2, have been characterized by FTIR, UV–Vis diffuse reflectance spectroscopy, TG-DTA analysis, and DFT calculations. Crystal structures of two solvated clusters 1·7DMF and 2·8DMSO have been unambiguously determined by single-crystal X-ray diffraction analysis. Six carboxylic groups appended on the clusters trap solvent guests, DMF or DMSO, through H-bonds. As a result, alternately stacked lamellar architectures comprising of a paddlewheel cluster layer and H-bonded solvent layer are formed. Upon UV illumination (λex = 365 nm), the solvated hexasilver(I) cluster 2·8DMSO gives intense greenish-yellow photoluminescence in the solid state (λPL = 545 nm, ΦPL = 0.17 at 298 K), whereas the solvated hexacopper(I) cluster 1·7DMF displays PL in the near-IR region (λPL = 765 nm, ΦPL = 0.38 at 298 K). Upon complete desolvation, a substantial bleach in the PL intensity (ΦPL < 0.01) is observed. The desorption–sorption response was studied by the solid-state PL spectroscopy. Non-covalent interactions in the crystal including intermolecular H-bonds, CH···π interactions, and π···π stack were found to play decisive roles in the creation of the lamellar architectures, small-molecule trap-and-release behavior, and guest-induced luminescence enhancement.

scholarly journals Thermal solid-state Z/E isomerization of 2-alkylidene-4-oxothiazolidines: Effects of non-covalent interactions

2011 ◽  
Vol 76 (3) ◽  
pp. 317-328 ◽  
Author(s):  
Zdravko Dzambaski ◽  
Milovan Stojanovic ◽  
Marija Baranac-Stojanovic ◽  
Dragica Minic ◽  
Rade Markovic
Keyword(s):  
Solid State ◽  
1H Nmr Spectroscopy ◽  
Amorphous State ◽  
Intramolecular Hydrogen Bonding ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Configurational Isomerization ◽  
Non Covalent Interactions ◽  
Intramolecular Hydrogen ◽  
Covalent Interactions

Configurational isomerization of stereo-defined 5-substituted and unsubstituted 2-alkylidene-4-oxothiazolidines 1 in the solid state, giving the Z/E mixtures in various ratios, was investigated by 1H-NMR spectroscopy, X-ray powder crystallography and differential scanning calorimetry (DSC). The Z/E composition can be rationalized in terms of non-covalent interactions, involving intermolecular and intramolecular hydrogen bonding and directional non-bonded 1,5-type S...O interactions. X-Ray powder crystallography, using selected crystalline (Z)-4- oxothiazolidine substrates, revealed transformation to the amorphous state during the irreversible Z ? E process. A correlation between previous results on the Z/E isomerization in solution and now in the solid state was established.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

scholarly journals A variable-temperature X-ray diffraction and theoretical study of conformational polymorphism in a complex organic molecule (DTC)

RSC Advances ◽  
2018 ◽  
Vol 8 (67) ◽  
pp. 38445-38454 ◽  
Author(s):  
Andrea Gionda ◽  
Giovanni Macetti ◽  
Laura Loconte ◽  
Silvia Rizzato ◽  
Ahmed M. Orlando ◽  
...  
Keyword(s):  
Theoretical Study ◽  
Crystal Packing ◽  
Variable Temperature ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Complex Organic Molecule ◽  
Non Covalent Interactions ◽  
Complex Organic ◽  
Covalent Interactions

A small conformational change in the asymmetric unit has a significant effect on how non-covalent interactions determine (i) the crystal packing and (ii) the effect of T on the relative balance of electrostatics and dispersion–repulsions.

The two solid-state conformations of nefopam methiodide, a quaternary ammonium salt of the analgesic drug

1990 ◽  
Vol 68 (7) ◽  
pp. 1128-1134 ◽  
Author(s):  
Robert Glaser ◽  
André Michel ◽  
Marc Drouin
Keyword(s):  
Solid State ◽  
Ammonium Salt ◽  
Quaternary Ammonium ◽  
Quaternary Ammonium Salt ◽  
State Structure ◽  
X Ray Diffraction ◽  
Analgesic Drug ◽  
X Ray ◽  
Positional Disorder ◽  
X Ray Crystallography

The solid-state structure of nefopam methiodide, a quaternary ammonium salt of nefopam hydrochloride (a non-narcotic analgesic drug), has been determined by single crystal X-ray diffraction analysis. Nefopam methiodide gives crystals belonging to the monoclinic P21/c space group and, at 298 K, a = 10.001(1), b = 9.928(1), c = 17.598(1) Å, β = 94.41(1)°, V = 1742.2(2) Å3, Z = 4, R(F) = 0.086, and Rw(F) = 0.108. Due to disorder, the boat (flattened chair) and twist-chair (flattened chair) conformations of the 2,5-benzoxazocine eight-membered ring were both observed in the crystal with 55:45 occupancy, respectively. Positional disorder was also observed for the iodide counterion, which showed occupancies of 81:9.5:9.5. Keywords: nefopam, analgesic, X-ray crystallography, conformation.

Solid-state and solution 117Sn NMR study of C2O4(SnPh3)2: a revision

2011 ◽  
Vol 34 (5-6) ◽  
pp. 153-153
Author(s):  
Libasse Diop
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
State Structure ◽  
X Ray Diffraction ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Nmr Study ◽  
Tetrahedral Environment ◽  
Good Agreement

Abstract Solid-state and solution 117Sn nuclear magnetic resonance studies of C2O4(SnPh3)2 have been carried out and found to be in good agreement with the tetrahedral environment of the tin (IV) atom as found from the solid state structure, previously determined by a single crystal X-ray diffraction analysis.

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