Synthesis of tetrahalide dianions directed by crystal engineering
CrystEngComm 17(35), 6641-6645(2015). doi:10.1039/C5CE01288K
N-(6-Methylpyridin-2-yl)mesitylenesulfonamide and acetic acid--a salt, a cocrystal or both?
In the solid obtained fromN-(6-methylpyridin-2-yl)mesitylenesulfonamide and acetic acid, the constituents interactviatwo N—H...O hydrogen bonds. The H atom situated in one of these short contacts is disordered over two positions: one of these positions is formally associated with an adduct of the neutral sulfonamide molecule and the neutral acetic acid molecule, and corresponds to a cocrystal, while the alternative site is associated with salt formation between a protonated sulfonamide molecule and deprotonated acetic acid molecule. Site-occupancy refinements and electron densities from difference Fourier maps suggest a trend with temperature, albeit of limited significance; the cocrystal i…
Diphenyltin(IV) complexes of the 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-olates: Synthesis and multinuclear NMR, 119Sn Mössbauer, electrospray ionization MS, X-ray characterization and assessment of in vitro cytotoxicity
Abstract A series of cis-bis{5-[(E)-2-(aryl)-1-diazenyl]quinolinolato}diphenyltin(IV) complexes have been synthesized and characterized by 1H, 13C, 119Sn NMR, ESI-MS, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analysis. The structures of a ligand L6H (i.e., 5-[(E)-2-(4-ethoxyphenyl)-1-diazenyl]quinolin-8-ol) and three diphenyltin(IV) complexes, viz., Ph2Sn(L1)2 · (CH3)2CO (1), Ph2Sn(L4)2 (4) and Ph2Sn(L5)2 (5) (L = 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-ol: aryl = phenyl – (L1H); 4′-methylphenyl – (L4H) and 4′-bromophenyl – (L5H)) were determined by single crystal X-ray diffraction. In general, the complexes were found to adopt a distorted cis-octahedral a…
Di-n-octyltin(IV) complexes with 5-[(E)-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acid: Syntheses and assessment of solid state structures by 119Sn Mössbauer and X-ray diffraction and further insight into the solution structures using electrospray ionization MS, 119Sn NMR and variable temperature NMR spectroscopy
Abstract Reactions of 5-[( E )-2-(aryl)-1-diazenyl]-2-hydroxybenzoic acids (LHH′, where the aryl group is an R-substituted phenyl ring such that for L 1 HH′: X = H; L 2 HH′: X=2′-OCH 3 ; L 3 HH′: X = 3′-CH 3 ; L 4 HH′: X = 4′-CH 3 ; L 5 HH′:X = 4′-Cl) with n Oct 2 SnO in 2:1 and 1:1 molar ratios have been investigated. Two types of complexes, n Oct 2 Sn(LH) 2 and {[ n Oct 2 Sn(LH)] 2 O} 2 , were isolated and they have been characterized by 1 H, 13 C, 119 Sn NMR, ESI-MS, IR and 119m Sn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of n Oct 2 Sn(L 1 H) 2 ( 1 ), {[ n Oct 2 Sn(L 2 H)] 2 O} 2 ( 3 ) and {[ n Oct 2 Sn(L 3 H)] 2 O} 2 ( 4 ) were de…
Synthesis, photophysical properties and structures of organotin-Schiff bases utilizing aromatic amino acid from the chiral pool and evaluation of the biological perspective of a triphenyltin compound
Abstract Five new organotin(IV) complexes of compositions [Me 2 SnL 1 ] ( 1 ), [Me 2 SnL 2 ] n ( 2 ), [Me 2 SnL 3 ] ( 3 ), [Ph 3 SnL 1 H] n ( 4 ) and [Ph 3 SnL 3 H] ( 5 ) (where L 1 = (2 S )-2-(( E )-(( Z )-4-hydroxypent-3-en-2-ylidene)amino)-3-(1 H -indol-3-yl)propanoate, L 2 = (2 S )-( E )-2-((2-hydroxybenzylidene)amino)-3-(1 H -indol-3-yl)propanoate and L 3 = (2 S )-( E )-2-((1-(2-hydroxyphenyl)ethylidene)amino)-3-(1 H -indol-3-yl)propanoate were synthesized and spectroscopically characterized. The crystal structures of 1 – 4 were determined. For the dimethyltin derivative 2 , a polymeric chain structure was observed as a result of a long Sn∙∙∙O contact involving the exocyclic carbony…
Organotin(IV) complexes ofN-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine
Organotin(IV) derivatives of N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycine have been synthesized and characterized by 1H, 13C, 119Sn NMR, 119Sn Mossbauer, and IR spectroscopy along with elemental analyses. The di- and triorganotin(IV) complexes were readily obtained from the reactions of organotin halides and sodium/potassium N-[(2Z)-3-hydroxy-1-methyl-2-butenylidene]glycinate. The diorganotin compound reacted with Ph3SnCl in refluxing benzene to give the mixed organotin dinuclear complex of composition Ph2Sn(2-OC(CH3)-C(H)C(CH3)NCH2COO)·Ph3SnCl, which was characterized by single crystal X-ray structure determination. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:149–154, 2003; Publ…
Molecular basis of the interaction of novel tributyltin(IV) 2/4-[(E)-2-(aryl)-1-diazenyl] benzoates endowed with an improved cytotoxic profile: Synthesis, structure, biological efficacy and QSAR studies
A series of tributyltin(IV) complexes based on 2/4-[(E)-2-(aryl)-1-diazenyl]benzoate ligands was synthesized, wherein the position of the carboxylate and aryl substituents (methyl, tert-butyl and hydroxyl) varies. The complexes, Bu(3)SnL(1-4)H (1-4), have been structurally characterized by elemental analysis and IR, NMR ((1)H, (13)C, and (119)Sn) and (119)Sn Mossbauer spectroscopy. All have a tetrahedral geometry in solution and a trigonal bipyramidal geometry in the solid-state, except for Bu(3)SnL(4)H (4) that was ascertained to have tetrahedral coordination by X-ray crystallography. Cytotoxicity studies were carried out on human tumor cell lines A498 (renal cancer), EVSA-T (mammary cance…
Re-visiting of 5-[(E)-2-(aryl)-1-diazenyl]-quinolin-8-ol with tweaking of Sn–Ph groups: Synthesis, spectroscopic characterization and X-ray crystallography
Abstract Reactions of sodium 5-[(E)-2-(aryl)-1-diazenyl]quinolin-8-olates (LH, where the aryl group is an R-substituted phenyl ring such that for L1H: R = H; L2H: R = 2′-CH3; L3H: R = 3′-CH3; L4H: R = 4′-CH3; L5H: R = 4′-OCH3 and L6H: R = 4′-OC2H5) with Ph3SnCl in a 1:1 molar ratio yielded complexes of composition Ph3SnL. The complexes have been characterized by 1H, 13C, 119Sn NMR, IR and 119mSn Mossbauer spectroscopic techniques in combination with elemental analyses. The crystal structures of Ph3SnL1 · 0.5C6H6 (1), Ph3SnL2 (2), Ph3SnL5 · C6H6 (5) and Ph3SnL6 · 0.5C6H6 (6) were determined. The results of the X-ray studies indicated that the benzene solvated compounds 1, 5 and 6 are distort…
An in vitro comparative assessment with a series of new triphenyltin(IV) 2-/4-[(E)-2-(aryl)-1-diazenyl]benzoates endowed with anticancer activities: Structural modifications, analysis of efficacy and cytotoxicity involving human tumor cell lines
Four new triphenyltin(IV) complexes of composition Ph 3SnLH (where LH = 2-/4-[(E)-2-(aryl)-1-diazenyl]benzoate) (1-4) were synthesized and characterized by spectroscopic ( 1H, 13C and 119Sn NMR, IR, 119Sn Mössbauer) techniques in combination with elemental analysis. The 119Sn NMR spectroscopic data indicate a tetrahedral coordination geometry in non-coordinating solvents. The crystal structures of three complexes, Ph 3SnL 1H (1), Ph 3SnL 3H (3), Ph 3SnL 4H (4), were determined. All display an essentially tetrahedral geometry with angles ranging from 93.50(8) to 124.5(2)°; 119Sn Mössbauer spectral data support this assignment. The cytotoxicity studies were performed with complexes 1-4, along…
CCDC 1431712: Experimental Crystal Structure Determination
Related Article: Tushar S. Basu Baul, Pelesakuo Kehie, Andrew Duthie, Nikhil Guchhait, Nune Raviprakash, Raveendra B. Mokhamatam, Sunil K. Manna, Nerina Armata, Michelangelo Scopelliti, f, Ruimin Wang, Ulli Englert|2017|J.Inorg.Biochem.|168|76|doi:10.1016/j.jinorgbio.2016.12.001
CCDC 1431713: Experimental Crystal Structure Determination
Related Article: Tushar S. Basu Baul, Pelesakuo Kehie, Andrew Duthie, Nikhil Guchhait, Nune Raviprakash, Raveendra B. Mokhamatam, Sunil K. Manna, Nerina Armata, Michelangelo Scopelliti, f, Ruimin Wang, Ulli Englert|2017|J.Inorg.Biochem.|168|76|doi:10.1016/j.jinorgbio.2016.12.001
CCDC 1431715: Experimental Crystal Structure Determination
Related Article: Tushar S. Basu Baul, Pelesakuo Kehie, Andrew Duthie, Nikhil Guchhait, Nune Raviprakash, Raveendra B. Mokhamatam, Sunil K. Manna, Nerina Armata, Michelangelo Scopelliti, f, Ruimin Wang, Ulli Englert|2017|J.Inorg.Biochem.|168|76|doi:10.1016/j.jinorgbio.2016.12.001
CCDC 1431714: Experimental Crystal Structure Determination
Related Article: Tushar S. Basu Baul, Pelesakuo Kehie, Andrew Duthie, Nikhil Guchhait, Nune Raviprakash, Raveendra B. Mokhamatam, Sunil K. Manna, Nerina Armata, Michelangelo Scopelliti, f, Ruimin Wang, Ulli Englert|2017|J.Inorg.Biochem.|168|76|doi:10.1016/j.jinorgbio.2016.12.001