@article { ISI:000248376400006, title = {Unusual trisulphide linkage in bromine-thiourea reaction: crystal structure of formamidinium trisulphide complex with bromine}, journal = {Molecular Crystals and Liquid Crystals}, volume = {469}, year = {2007}, month = {SEP}, pages = {69+}, publisher = {TAYLOR \& FRANCIS LTD}, type = {Article}, address = {4 PARK SQUARE, MILTON PARK, ABINGDON OX14 4RN, OXON, ENGLAND}, abstract = {

{A new complex of formamidinium trisulphide with bromine has been synthesized. Single-crystal X-ray analysis of this compound revealed a novel trisulphide linkage in the formamidinium trisulphide moiety. The crystals belong to orthorhombic space group Fdd2 with a = 14.9119(15)

}, keywords = {bromine, crystal structure, formamidinium trisulphide, thiourea}, issn = {1542-1406}, doi = {10.1080/15421400701431265}, author = {Tol, Abhaya D. and Natu, Arun D. and Puranik, Vedavati G.} } @article { ISI:000261711400041, title = {Molecular association via halogen bonding and other weak interactions in the crystal structures of 11-bromo-12-oxo-5 beta-cholan derivatives}, journal = {Journal of Molecular Structure}, volume = {892}, number = {1-3}, year = {2008}, month = {DEC}, pages = {246-253}, publisher = {ELSEVIER SCIENCE BV}, type = {Article}, address = {PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS}, abstract = {

Methyl 3 alpha,7 alpha-diacetoxy-12-oxo-5 beta-cholan-24-oate 2, methyl 11 alpha-bromo-3 alpha,7 alpha-diacetoxy-12-oxo-5 beta-cholan-24-oate 3, methyl 11 beta-bromo-3 alpha,7 alpha-diacetoxy-12-oxo-5 beta-cholan-24-oate 4 and methyl 11,11-dibromo-3 alpha,7 alpha-diacetoxy-12-oxo-5 beta-cholan-24-oate 5 were synthesized. The crystal structures of these molecules were resolved to study the effect of bulky bromine atom in the steroid skeleton of cholic acid with different stereo-chemical orientations at C-11 on the two-dimensional arrangement of molecules and solid-state properties. All the molecules associate only via weak intermolecular interactions in their crystal structures, notable one being the Halogen Bonded assembly (C-Br center dot center dot center dot O) in 5. (C) 2008 Elsevier B.V. All rights reserved.

}, keywords = {11-Bromosteroids, Cholic acid, crystal structure, Halogen bonding}, issn = {0022-2860}, doi = {10.1016/j.molstruc.2008.05.051}, author = {Salunke, Deepak B. and Hazra, Braja G. and Gonnade, Rajesh G. and Pore, Vandana S. and Bhadbhade, Mohan M.} } @article { ISI:000269291500035, title = {Nanocrystalline Mn-Zn-ferrite by novel oxalato-hydrazinated complex method}, journal = {Materials Chemistry and Physics}, volume = {117}, number = {1}, year = {2009}, month = {SEP}, pages = {187-191}, publisher = {ELSEVIER SCIENCE SA}, address = {PO BOX 564, 1001 LAUSANNE, SWITZERLAND}, abstract = {

We report here for the first time the synthesis of technologically important ferrite, using a metal oxalato-hydrazinate (MOH) complex method. The MOH complex of iron-manganese-zinc was synthesized at room temperature using the precursors, ferrous ammonium sulphate, manganese acetate and zinc acetate. Thermo-gravimetric studies of MOH intermediate showed complete phase formation of MnZnFe(2)O(4) at 280 degrees C. XRD data showed the formation of single phase cubic spinel MnZnFe(2)O(4). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) demonstrate the spherical shape particle morphology. TEM images indicated the particle size of ferrite powder in the range of 20-36 nm. Magnetization of synthesized nano-sized Mn(0.69)Zn(.0.19)Fe(2.12)O(4) was observed coercive force (H(c)) at 127.82 Oe with a saturation magnetization (M(s)), 34.5 emu g(-1) using vibrating sample magnetometer (VSM) at room temperature. Mossbauer study of nano-sized ferrite powder showed super-paramagnteic behavior. (c) 2009 Elsevier B.V. All rights reserved.

}, keywords = {crystal structure, Magnetic materials, Mn-Zn-ferrite, Nanostructures, Optical properties}, issn = {0254-0584}, doi = {10.1016/j.matchemphys.2009.05.036}, author = {Kanade, K. G. and Amalnerkar, Dinesh P. and Potdar, H. S. and Kale, B. B.} } @article { ISI:000264717200003, title = {Structural phase transitions of syndiotactic polystyrene}, journal = {Progress in Polymer Science}, volume = {34}, number = {3}, year = {2009}, month = {MAR}, pages = {280-315}, publisher = {PERGAMON-ELSEVIER SCIENCE LTD}, address = {THE BOULEVARD, LANGFORD LANE, KIDLINGTON, OXFORD OX5 1GB, ENGLAND}, abstract = {

Syndiotactic polystyrene (sPS) exhibits four crystal modifications (alpha, beta, gamma, and delta), along with intermediate forms with different molecular conformations, as well as different chain-packing structures. The extensive literature on the crystal structures exhibited by sPS is reviewed herein, including, the mechanisms of phenomena such as solvent-induced crystallization, thermally induced crystallization and gelation, and the phase transitions among the various crystalline forms. The latter have been studied by static and dynamic wide-angle and small-angle X-ray scattering, infrared and Raman spectra, and neutron scattering, etc., in addition to computer simulations. (C) 2009 Elsevier Ltd. All rights reserved.

}, keywords = {crystal structure, Gelation, phase transition, polymorphism, Solvent-induced crystallization, Syndiotactic polystyrene}, issn = {0079-6700}, doi = {10.1016/j.progpolymsci.2008.11.002}, author = {Gowd, E. Bhoje and Tashiro, Kohji and Ramesh, C.} } @article { ISI:000281980600018, title = {Conformational polymorphism in racemic 2,4-Di-o-Benzoyl-6-o-Tosyl myo-Inositol 1,3,5-Orthoacetate}, journal = {Journal of Structural Chemistry}, volume = {51}, number = {4}, year = {2010}, month = {AUG}, pages = {725-730}, publisher = {SPRINGER}, address = {233 SPRING ST, NEW YORK, NY 10013 USA}, abstract = {

The title compound, C(29)H(26)O(10)S, yields two conformational polymorphs concomitantly from dichloromethane-methanol mixture; the major polymorph grows as plates (Form I, monoclinic, P2(1)/n) and the minor polymorph grows as needles (Form II, triclinic, P-1). The two forms differ mainly in orientation of the tosyl group. In Form I, sulfonyl oxygen of the tosyl group makes intermolecular C -HaEuro broken vertical bar O interactions, whereas the same group in Form II is involved in an intramolecular short dipolar S=OaEuro broken vertical bar C=O (sulfonyl-carbonyl) contact. The molecular organization and the influence of various weak non-covalent interactions that stabilize these conformers in the crystal lattices are discussed.

}, keywords = {Conformation, crystal structure, dipolar interactions, Inositol, non-covalent interactions, polymorphism, sulfonyl-carbonyl contact}, issn = {0022-4766}, doi = {10.1007/s10947-010-0107-y}, author = {Manoj, Kochunnoonny and Gonnade, Rajesh G. and Bhadbhade, Mohan M. and Shashidhar, M. S.} } @article { ISI:000288772300011, title = {Magnetic properties of thermal plasma synthesized nanocrystalline nickel ferrite (NiFe2O4)}, journal = {Journal of Alloys and Compounds}, volume = {509}, number = {12}, year = {2011}, month = {MAR}, pages = {4404-4413}, publisher = {ELSEVIER SCIENCE SA}, address = {PO BOX 564, 1001 LAUSANNE, SWITZERLAND}, abstract = {

A rapid synthesis method is reported for magnetic nanoparticles of nickel ferrite involving thermal plasma assisted vapor phase condensation process. The as-synthesized samples were characterized by X-ray Diffraction, Transmission Electron Microscopy, Vibrating Sample Magnetometer and X-ray Photoelectron Spectroscopy techniques. The average particle size was determined from the TEM micrographs and found to be around 30 nm. The effects of reactor parameters on the magnetic and structural properties have been evaluated, to find the optimized parameters so as to achieve the highest values of saturation magnetization and coercivity. Reasonably high saturation magnetization (48 emu/g) has been assigned to the high degree of crystallinity, achieved on account of high temperature during the growth, and the cation redistribution. The high value of coercivity (1150e) is explained on the basis of possible lattice defects arising from the cation redistribution. Detailed analysis of cation distribution using the XRD line intensity data leads to the conclusion that these samples are iron deficit and nickel rich. (C) 2011 Elsevier B.V. All rights reserved.

}, keywords = {crystal structure, Magnetic measurements, Magnetization, Nanostructured materials, TEM}, issn = {0925-8388}, doi = {10.1016/j.jallcom.2011.01.057}, author = {Nawale, Ashok B. and Kanhe, Nilesh S. and Patil, K. R. and Bhoraskar, S. V. and Mathe, Vikas L. and Das, A. K.} } @article { ISI:000294506200003, title = {Synthesis and structural characterization of a solvated dimorph of a hydrazonato-oxovanadium(v) complex with [OV(mu-O)VO] core}, journal = {Journal of the Indian Chemical Society}, volume = {88}, number = {7}, year = {2011}, month = {JUL}, pages = {937-941}, publisher = {SCIENTIFIC PUBL-INDIA}, address = {5-A, NEW PALI RD, PO BOX 91, NEAR HOTEL TAJ HARI MAHAL, JODHPUR, 342 003, INDIA}, abstract = {

In this paper we report the synthesis and structural characterization of a different monoclinic variety of the title complex [V2O3(L)(2)], incorporating the doubly deprotonated benzoyl hydrazone of 5-chloro-2-hydroxyacetophenone (H2L) with P2(1)/c space group that showed some differences in bonding patterns in the solid state with respect to its another monoclinic variety with C2/c space group reported earlier.

}, keywords = {crystal structure, dimorphism, hydrazone complex, Oxovanadium(v) complex}, issn = {0019-4522}, author = {Mondal, Bipul and Banerjee, Rahul and Ghosh, Tapas} } @article { ISI:000300076200019, title = {Synthesis and stereochemistry of highly crowded N-benzylpiperidones}, journal = {Journal of Molecular Structure}, volume = {1007}, year = {2012}, month = {JAN}, pages = {158-167}, publisher = {ELSEVIER SCIENCE BV}, address = {PO BOX 211, 1000 AE AMSTERDAM, NETHERLANDS}, abstract = {

A series of N-benzylated 3,5-diakyl-2,6-diarylpiperidin-4-ones 4-8 were conveniently synthesized in significant yields of 68-88\% by N-benzylation of the corresponding 2,6-diaryl-3,5-dimethylpiperidin-4-ones 1-3 using different benzyl bromides. Initially, the new piperidone 2,6-bis(4-ethoxypheny1)-3,5-dimethylpiperidin-4-one 3 was synthesized by the condensation of 1:1:2 M ratio of 3-pentanone, ammonium acetate and para-ethoxybenzaldehyde in ethanolic medium. All the synthesized new compounds 3-8 were characterized by their analytical and spectral (IR, H-1 and C-13 NMR) interpretations. The stereochemistry of the new piperidone 3 was elucidated as chair conformation with an equatorial orientation of all substituents, suggested by its vicinal couplings from H-1 NMR spectrum. To investigate the impact on piperidone stereochemistry as well as NMR chemical shifts, all the N-benzylated products 4-8 were compared with their corresponding precursors, and as a result, it is clearly established that all the synthesized N-benzyl piperidones exist in the chair conformation with an equatorial orientation of all the substituents at C-2, C-3, C-5, C-6 and N. Contrary to the probability all N-benzylated compounds retain the same conformation and configuration as their precursors, however, a remarkable change on the chemical shifts are observed. For the further unambiguous confirmation of stereochemistry, the 1-benzyl-3,5-dimethyl-2,6-diphenylpiperidin-4-one 4 was examined by single-crystal X-ray diffraction. The compound 4, C26H27NO, crystallized in a P-1 space group under triclinic system with unit cell dimensions a, b, c (angstrom) and alpha, beta, gamma (degrees) of 10.156(2), 11.002(2), 11.348(4) and 116.74(4), 100.81(3), 100.17(3), respectively. (C) 2011 Elsevier B.V. All rights reserved.

}, keywords = {Chair conformation, Configuration, crystal structure, N-benzylation, NMR, Piperidin-4-one}, issn = {0022-2860}, doi = {10.1016/j.molstruc.2011.10.037}, author = {Dindulkar, Someshwar D. and Parthiban, Paramasivam and Puranik, Vedavati G. and Jeong, Yeon Tae} } @article { ISI:000344793700010, title = {Correlation of the solid-state reactivities of racemic 2,4(6)-di-O-benzoyl-myo-inositol 1,3,5-orthoformate and its 4,4 {\textquoteleft}-bipyridine cocrystal with their crystal structures}, journal = {Acta Crystallographica Section C-Structural Chemistry}, volume = {70}, number = {11}, year = {2014}, month = {NOV}, pages = {1040+}, publisher = {WILEY-BLACKWELL}, type = {Article}, address = {111 RIVER ST, HOBOKEN 07030-5774, NJ USA}, abstract = {

Racemic 2,4(6)-di-O-benzoyl-myo-inositol 1,3,5-orthoformate, C21H18O8, (1), shows a very efficient intermolecular benzoyl-group migration reaction in its crystals. However, the presence of 4,4 {\textquoteleft}-bipyridine molecules in its cocrystal, C21H18O8 center dot C10H8N2, (1)center dot BP, inhibits the intermolecular benzoyl-group transfer reaction. In (1), molecules are assembled around the crystallographic twofold screw axis (b axis) to form a helical self-assembly through conventional O-H center dot center dot center dot O hydrogen-bonding interactions. This helical association places the reactive C6-O-benzoyl group (electrophile, El) and the C4-hydroxy group (nucleophile, Nu) in proximity, with a preorganized El center dot center dot center dot Nu geometry favourable for the acyl transfer reaction. In the cocrystal (1)center dot BP, the dibenzoate and bipyridine molecules are arranged alternately through OH center dot center dot center dot N interactions. The presence of the bipyridine molecules perturbs the regular helical assembly of the dibenzoate molecules and thus restricts the solid-state reactivity. Hence, unlike the parent dibenzoate crystals, the cocrystals do not exhibit benzoyl-transfer reactions. This approach is useful for increasing the stability of small molecules in the crystalline state and could find application in the design of functional solids.

}, keywords = {acyl transfer, cocrystal, crystal structure, design of functional solids, helical assembly, hydrogen bonding, myo-inositol, solid-state reactions}, issn = {0108-2701}, doi = {10.1107/S2053229614021834}, author = {Tamboli, Majid I. and Bahadur, Vir and Gonnade, Rajesh G. and Shashidhar, Mysore S.} } @article { ISI:000340149800003, title = {Synthesis, characterization, and crystal structure determination of palladacycles of para-substituted 2-thiobenzylazobenzenes}, journal = {Journal of Coordination Chemistry}, volume = {67}, number = {10}, year = {2014}, month = {JUN}, pages = {1702-1714}, publisher = {TAYLOR \& FRANCIS LTD}, address = {4 PARK SQUARE, MILTON PARK, ABINGDON OX14 4RN, OXON, ENGLAND}, abstract = {

Bichelated neutral palladacycles (1-3), [Pd(L)Cl], were synthesized from reaction of the new potential tridentate (C,N,S) ligands, 2-thiobenzylazobenzene (L-1), 4{\textquoteright}-methyl-2-thiobenzylazobenzene (L-2), and 4{\textquoteright}-chloro-2-thiobenzylazobenzene (L-3) with sodium tetrachloropalladate(II), Na-2[PdCl4], in ethanol. The compounds were characterized by elemental analysis, FT-IR, H-1 NMR, UV-visible, and thermogravimetric analysis. The crystal structures of L-2 and 1-3 were determined by single-crystal X-ray diffraction. In 1-3, the geometry around palladium remains almost square planar, coordinated to carbon, nitrogen, and sulfur of the ligand forming a bichelated cyclopalladate complex. The C-H center dot center dot center dot Cl type intermolecular hydrogen bonds, weak pi center dot center dot center dot pi, C-H center dot center dot center dot pi, and van der Waals interactions are believed to be the stabilizing forces for the crystal packing of these palladacycles.

}, keywords = {2-Thiobenzylazobenzene, CNS-donor ligand, crystal structure, Palladacycles, Thermogravimetric analysis}, issn = {0095-8972}, doi = {10.1080/00958972.2014.922683}, author = {Bhattacharjee, Tirtha and Kalita, Mukul and Chakravarty, Debamitra K. and Barman, Pranjit and Puranik, Vedavati G.} } @article { ISI:000364509100013, title = {Crystal structures of the pyrazinamide-p-aminobenzoic acid (1/1) cocrystal and the transamidation reaction product 4-(pyrazine-2-carboxamido)-benzoic acid in the molten state}, journal = {Acta Crystallographica Section C-Structural Chemistry}, volume = {71}, number = {11}, year = {2015}, month = {NOV}, pages = {1010-U276}, publisher = {INT UNION CRYSTALLOGRAPHY}, address = {2 ABBEY SQ, CHESTER, CH1 2HU, ENGLAND}, abstract = {

The synthesis of pharmaceutical cocrystals is a strategy to enhance the performance of active pharmaceutical ingredients (APIs) without affecting their therapeutic efficiency. The 1: 1 pharmaceutical cocrystal of the antituberculosis drug pyrazinamide (PZA) and the cocrystal former p-aminobenzoic acid (p-ABA), C7H7NO2- C5H5N3O, (1), was synthesized successfully and characterized by relevant solid-state characterization methods. The cocrystal crystallizes in the monoclinic space group P21/n containing one molecule of each component. Both molecules associate via intermolecular O-H center dot center dot center dot O and NH center dot center dot center dot O hydrogen bonds [O center dot center dot center dot O = 2.6102 (15)angstrom and O-H center dot center dot center dot O = 168.3 (19)degrees; N center dot center dot center dot O = 2.9259 (18) angstrom and N-H center dot center dot center dot O = 167.7 (16)degrees] to generate a dimeric acidamide synthon. Neighbouring dimers are linked centrosymmetrically through N-H center dot center dot center dot O interactions [N center dot center dot center dot O = 3.1201 (18) angstrom and N-H center dot center dot center dot O = 136.9 (14)degrees] to form a tetrameric assembly supplemented by C-H center dot center dot center dot N interactions [C center dot center dot center dot N = 3.5277 (19) angstrom and C-H center dot center dot center dot N = 147 degrees]. Linking of these tetrameric assemblies through N-H center dot center dot center dot O [N center dot center dot center dot O = 3.3026 (19) angstrom and N-H center dot center dot center dot O = 143.1 (17)degrees], NH center dot center dot center dot N [N center dot center dot center dot N = 3.221 (2) angstrom and N-H center dot center dot center dot N = 177.9 (17)degrees] and C-H center dot center dot center dot O [C center dot center dot center dot O = 3.5354 (18) angstrom and C-H center dot center dot center dot O = 152 degrees] interactions creates the twodimensional packing. Recrystallization of the cocrystals from the molten state revealed the formation of 4-(pyrazine-2-carboxamido) benzoic acid, C12H9N3O3, (2), through a transamidation reaction between PZA and p-ABA. Carboxamide (2) crystallizes in the triclinic space group P1 with one molecule in the asymmetric unit. Molecules of (2) form a centrosymmetric dimeric homosynthon through an acid-acid O-H center dot center dot center dot O hydrogen bond [O center dot center dot center dot O = 2.666 (3) angstrom and O-H center dot center dot center dot O = 178 (4) degrees]. Neighbouring assemblies are connected centrosymmetrically via a C-H center dot center dot center dot N interaction [C center dot center dot center dot N = 3.365 (3) angstrom and C-H center dot center dot center dot N = 142 degrees] engaging the pyrazine groups to generate a linear chain. Adjacent chains are connected loosely via C-H center dot center dot center dot O interactions [C center dot center dot center dot O = 3.212 (3) angstrom and CH center dot center dot center dot O = 149 degrees] to generate a two-dimensional sheet structure. Closely associated two-dimensional sheets in both compounds are stacked via aromatic pi-stacking interactions engaging the pyrazine and benzene rings to create a threedimensional multi-stack structure.

}, keywords = {acid-amide hetero-synthon, active pharmaceutical ingredient (API), cocrystal, crystal structure, hydrogen bonding, molten-state reaction, powder diffraction, transamidation reaction}, issn = {2053-2296}, doi = {10.1107/S2053229615019828}, author = {Thorat, Shridhar H. and Sahu, Sanjay Kumar and Gonnade, Rajesh G.} } @article { ISI:000368141200024, title = {Drug-drug molecular salt hydrate of an anticancer drug gefitinib and a loop diuretic drug furosemide: an alternative for multidrug treatment}, journal = {Journal of Pharmaceutical Sciences}, volume = {104}, number = {12}, year = {2015}, month = {DEC}, pages = {4207-4216}, publisher = {WILEY-BLACKWELL}, address = {111 RIVER ST, HOBOKEN 07030-5774, NJ USA}, abstract = {

A 1:1 monohydrate salt containing gefitinib, an orally administrated chemotherapy treatment for lung and breast cancers and furosemide, a loop diuretic drug, commonly used in the treatment of hypertension and edema, has been prepared. The molecular salt crystallized in triclinic P-1 space group. The CO bond lengths (similar to 1.26 angstrom) in the COOH group show that proton transfer has occurred from furosemide to morpholine moiety of the gefitinib suggesting cocrystal to be ionic. The morpholine moiety of the gefitinib showed significant conformational change because of its involvement in conformation dictating the strong N-H center dot center dot center dot O hydrogen bonding interaction. The strong hydrogen bonding interaction between gefitinib and furosemide places their benzene rings in stacking mode to facilitate the generation of pi-stack dimers. The neighboring dimers are bridged to each other via water molecule through N-H center dot center dot center dot O, C-H center dot center dot center dot O, O-H center dot center dot center dot N, and O-H center dot center dot center dot O interactions. The remarkable stability of the salt hydrate could be attributed to the strong hydrogen bonding interactions in the crystal structure. Interestingly, release of water from the lattice at 140 degrees C produced new anhydrous salt that has better solubility and dissolution rate than salt hydrate. The drug-drug molecular salt may have some bearing on the treatment of patient suffering from anticancer and hypertension. (C) 2015 Wiley Periodicals, Inc. and the American Pharmacists Association

}, keywords = {cancer chemotherapy, cocrystals, crystal engineering, crystal structure, dissolution rate, hydrate, phase transition, solubility, stability, thermal analysis}, issn = {0022-3549}, doi = {10.1002/jps.24651}, author = {Thorat, Shridhar H. and Sahu, Sanjay Kumar and Patwadkar, Manjusha V. and Badiger, Manohar V. and Gonnade, Rajesh G.} } @article { ISI:000367546300012, title = {Synthesis, crystal structure and in vitro DNA binding studies of combretastatin A-4 analogue}, journal = {Croatica Chemica Acta}, volume = {88}, number = {3}, year = {2015}, month = {DEC}, pages = {289-296}, publisher = {CROATIAN CHEMICAL SOC}, address = {MARULICEV TRG 19/II, 41001 ZAGREB, CROATIA}, abstract = {

Synthesis of a novel Combretastatin A-4 analogue using Schiff{\textquoteright}s reaction of benzil and 4-aminoantipyrine has been achieved under solvent free conditions. The structure of compound was examined spectroscopically and confirmed from single crystal diffraction studies. The synthesized Combretastatin A-4 analogue was investigated for its DNA binding ability as the plausible mechanism for its antitumor activity. The binding propensity of the synthesized compound with calf-thymus (CT) DNA was monitored with absorption and emission spectrophotometric titrations. The calculations predict a binding constant of 7.24 x 10(4) for the complex of the synthesized compound with CT DNA which is comparable in magnitude to that of DNA binding of bactericidal drug enoxacin and typical intercalation indicator ethidium bromide (EB). Competitive binding studies of the synthesized compound with EB using fluorescence titration reveal that it displaces the DNA-bound EB and binds in intercalative mode which was further supported by circular dichroism (CD) spectroscopy. The probable site and binding energy of the compound with DNA was further theoretically investigated by molecular docking studies. The significant DNA binding ability of the synthesized Combretastatin A4 analogue as revealed from this study could be related to the anticancer activity of the Combretastatin A4.

}, keywords = {benzil, bio-physical, combretastatin A-4, crystal structure, DNA binding, ethidium bromide, fluorescence, phenazones}, issn = {0011-1643}, doi = {10.5562/cca2662}, author = {Rizvi, Masood Ahmad and Dangat, Yuvraj B. and Yaseen, Zahid and Gupta, Vivek and Khan, Khaliquz Zaman} } @article {45705, title = {Synthesis, structure and DNA interaction studies of bisphosphoramides: theoretical and experimental insights}, journal = {Inorganica Chimica Acta}, volume = {461}, year = {2017}, month = {MAY }, pages = {84-91}, type = {Article}, abstract = {

New bisphosphoramides (having phenyl (EDAPOPh(2)) and ethoxy (EDADEP) substituents attached to phosphoryl groups bridged with ethylenediamine spacer) are synthesized and structurally characterized by spectroscopic techniques as well as elemental analysis. The molecular structure of EDAPOPh(2) was determined by single crystal X-ray diffraction technique. The interaction of these bisphosphoramides with calf thymus DNA (ct-DNA) is investigated using UV-Visible absorption and fluorescence spectral data as well as the DFT calculations. These studies reveal that EDAPOPh(2) and EDADEP interact with DNA in a partial intercalation mode. The intrinsic binding constants K-b of two different bisphosphoramides with ct-DNA were determined by fluorescence spectroscopy as 2.08 x 10(4) and 3.86 x 10(4) M-1 respectively. The results indicated that the two compounds bind to ct-DNA with different binding affinities, i.e. EDAPOPh(2) \> EDADEP. The binding mechanism of these bisphosphoramides to ct-DNA is also discussed. (C) 2017 Elsevier B.V. All rights reserved.

}, keywords = {Bisphosphoramides, crystal structure, DNA interaction, Molecular docking}, issn = {0020-1693}, doi = {10.1016/j.ica.2017.02.017}, author = {Goud, E. Veerashekhar and Sivaramakrishna, Akella and Vijayakrishna, Kari and Rao, C. V. S. Brahmmananda and Khedkar, Vijay M. and Jha, Prakash C.} } @article {46065, title = {Structural insights into the unique inhibitory mechanism of Kunitz type trypsin inhibitor from Cicer arietinum L. Vol. 37}, journal = {Journal of Biomolecular Structure \& Dynamics}, volume = {37}, year = {2019}, month = {JUL}, pages = {2669-2677}, type = {Article}, abstract = {

Kunitz-type trypsin inhibitors bind to the active pocket of trypsin causing its inhibition. Plant Kunitz-type inhibitors are thought to be important in defense, especially against insect pests. From sequence analysis of various Kunitz-type inhibitors from plants, we identified CaTI2 from chickpea as a unique variant lacking the functionally important arginine residue corresponding to the soybean trypsin inhibitor (STI) and having a distinct and unique inhibitory loop organization. To further explore the implications of these sequence variations, we obtained the crystal structure of recombinant CaTI2 at 2.8 angstrom resolution. It is evident from the structure that the variations in the inhibitory loop facilitates non-substrate like binding of CaTI2 to trypsin, while the canonical inhibitor STI binds to trypsin in substrate like manner. Our results establish the unique mechanism of trypsin inhibition by CaTI2, which warrant further research into its substrate spectrum.

}, keywords = {Chickpea, crystal structure, inhibitory loop, Kunitz trypsin inhibitor, Trypsin}, issn = {0739-1102}, doi = {10.1080/07391102.2018.1494633}, author = {Bendre, Ameya D. and Suresh, C. G. and Shanmugam, Dhanasekaran and Ramasamy, Sureshkumar} } @article {46909, title = {Influence of fluorine substitution on the molecular conformation of 3 {\textquoteleft}-deoxy-3 {\textquoteleft}-fluoro-5-methyluriaine}, journal = {Acta Crystallographica Section C-Structural Chemistry}, volume = {76}, year = {2020}, month = {APR}, pages = {346+}, type = {Article}, abstract = {

{Fluorine substitutions on the furanose ring of nucleosides are known to strongly influence the conformational properties of oligonucleotides. In order to assess the effect of fluorine on the conformation of 3{\textquoteright}-deoxy-3{\textquoteright}-fluoro-5-methyluridine (T-R(F)), C-10 H13FN2O5, we studied its stereochemistry in the crystalline state using X-ray crystallography. The compound crystallizes in the chiral orthorhombic space group P2(1)2(1)2(1) and contains two symmetry-independent molecules (A and B) in the asymmetric unit. The furanose ring in molecules A and B adopts conformations between envelope (E-2, 2{\textquoteright}-endo

}, keywords = {crystal structure, fluoro nucleoside, pseudorotation parameter, sugar puckering, uridine}, issn = {2053-2296}, doi = {10.1107/S2053229620003083}, author = {Aher, Manisha N. and Erande, Namrata D. and Kumar, Vaijayanti A. and Fernandes, Moneesha and Gonnade, Rajesh G.} } @article {47667, title = {Crystal structure analysis of highly efficient chiral resolution of (RS)-arginine-fumaric acid cocrystal under preferential enrichment conditions}, journal = {Journal of Molecular Structure}, volume = {1245}, year = {2021}, month = {DEC }, pages = {131073}, type = {Article}, abstract = {Two new hydrate cocrystals, (RS)-arginine-fumaric acid-H2O ( 2 ) and (S)-arginine-2 fumaric acid-H2O ( 3 ), were obtained by the slow evaporation of the saturated aqueous ethanol solution of a 1:1 mixture of S-enriched arginine (33\% ee) and fumaric acid or (S)-arginine and fumaric acid, respectively. Cocrystals 2 and 3 possess an isostructural molecular organization containing homochiral 1D chains of arginine sim-ilar to that of the anhydrous cocrystal of (RS)-arginine-fumaric acid ( 1 ). The latter showed an efficient {\textquoteleft}{\textquoteleft}preferential enrichment (PE){\textquoteright}{\textquoteright}, a unique spontaneous enantiomeric resolution phenomenon by simple recrystallization from the highly supersaturated solution. The formation of unstable cocrystals 2 and 3 seems to have played a crucial role in the enrichment of arginine in the mother liquor under PE crystal-lization conditions. (c) 2021 Elsevier B.V. All rights reserved.}, keywords = {Arginine, cocrystals, crystal structure, Enantiomeric resolution, preferential enrichment}, issn = {0022-2860}, doi = {10.1016/j.molstruc.2021.131073}, author = {Manoj, Kochunnoonny and Takahashi, Hiroki and Iwama, Sekai and Gonnade, G. Rajesh and Tsue, Hirohito and Tamura, Rui} } @article {48128, title = {Interplay of anion-pi(+) and pi(+)-pi(+) interactions in novel pyrido[2,1-a]isoquinolinium-based aiegens - substituent- and counterion-dependent fluorescence modulation and applications in live cell mitochondrial imaging}, journal = {Chemistry-A European Journal}, volume = {28}, year = {2022}, month = {JUL }, pages = {e202200632}, type = {Article}, abstract = {

Recently, the concept of anion-pi(+) interactions has witnessed unique applications in the field of AIEgen development. In this contribution, we disclose a consolidated study of a library of N-doped ionic AIEgens accessed through silver-mediated cyclization of pyridino-alkynes. A thorough photophysical, computational and crystallographic study has been conducted to rationalize the observed substituent- and counterion-dependent fluorescence properties of these luminogens. We further elucidate the prominent role of anion-pi(+) interactions, pi(+)-pi(+) interactions and other non-covalent interactions, in inhibiting the undesired ACQ effect. Finally, we have also demonstrated the application of selected AIEgens for imaging of mitochondria in live cells.

}, keywords = {1-a]isoquinolinium, AIEgens, anion-pi(+), crystal structure, mitochondrial imaging, pyrido[2}, issn = {0947-6539}, doi = {10.1002/chem.202200632}, author = {Mule, Ravindra D. and Roy, Rupam and Mandal, Koushik and Chopra, Deepak and Dutta, Tanoy and Sancheti, Shashank P. and Shinde, Popat S. and Banerjee, Somsuvra and Lal Koner, Apurba and Bhowal, Rohit and Senthilkumar, Beeran and Patil, Nitin T.} } @article {48136, title = {Synthesis, characterization and single crystal x-ray structures of trifluroacetylacetonate copper(ii) complexes}, journal = {Journal of Chemical Crystallography}, volume = {52}, year = {2022}, month = {DEC}, pages = {525-533}, type = {Article}, abstract = {

{Three Cu(II) complexes of 1,1,1-trifluoroacetylacetonate, viz. [Cu(TFACAC)(2)(MeOH)] (1), [Cu(TFACAC)(2)(py)] (2) and [Cu(TFACAC)(2)(DABCO)] (3) were synthesized and characterized by elemental analysis, IR, UV-Visible spectroscopy and cyclic voltammetry. Structures of complexes 1-3 were established by single crystal X-ray diffraction wherein 1 and 2 adapt square pyramidal geometry. Complex 1 crystallizes in triclinic space group P-(1), with a = 8.5059(6) angstrom

}, keywords = {Copper(II) complexes, crystal structure, cyclic voltammetry, DABCO, Pyridine, Trifluoroacetylacetone}, issn = {1074-1542}, doi = {10.1007/s10870-022-00937-1}, author = {Kumari, Neha and Bahadur, Vir and Butcher, Raymond J. and Kumbhar, Anupa A.} } @article {49953, title = {Transition metal complexes of Thiadiazole-Picolinic acid: Crystal structures, DFT insights and anticancer activity}, journal = {Journal of Molecular Structure}, volume = {1354}, year = {2026}, month = {MAR 5}, pages = {144763}, type = {Article}, abstract = {

Five novel transition metal complexes [Ni(H2aeth)2(Pic)2] (1), [Co(H2aeth)2(Pic)2] (2), [Ni(H2aeth)2(Pic)(HPic)] ClO4 (3), [Co(H2aeth)2(Pic)(HPic)]ClO4 (4) and [Zn(H2aeth)2 (Pic)(HPic)]ClO4 (5) were synthesized using a 2amino-5-ethylthio-1,3,4-thiadiazole (H2aeth) and picolinic acid (HPic) as co-ligands. These complexes were characterized by FT-IR, UV-Vis., X-ray photoelectron spectroscopy, TG-DTA, and single-crystal X-ray techniques. Crystallographic analysis confirmed distorted octahedral geometries around the metal centers with extensive hydrogen bonding networks promoting supramolecular assembly in the solid state. X-ray photoelectron spectroscopy (XPS), validated the +2 oxidation state of each metal center. Thermal studies indicated multistep decomposition processes resulting in the formation of metal oxides. Density functional theory (DFT) and timedependent DFT calculations were employed to explore electronic structures and predict UV-Vis. transitions, which showed good agreement with experimental data. Frontier molecular orbital (FMO) analysis revealed that Ni(II) complexes 1 and 3 are softer and more reactive, consistent with their observed biological activity. The anticancer potential of complexes 1-5 was evaluated in vitro using the MCF-7 human breast cancer cell line and the MTT assay. Complex 1 exhibited the strongest cytotoxicity (IC50 = 26.5 mu g/mL) followed by complexes 3 (34.9 mu g/mL), 4 (46.4 mu g/mL), 2 (81.1 mu g/mL), and 5 (103.3 mu g/mL). The observed activity trends correlate with metal identity and coordination environment, underlining the role of electronic and structural factors in modulating bioactivity. These findings suggest that thiadiazole-picolinate metal complexes, particularly those based on Ni (II), are promising scaffolds for anticancer drug development.

}, keywords = {Anti-cancer activity, crystal structure, DFT calculation, MCF-7 cell line, Picolinic acid, Thiadiazole complexes}, issn = {0022-2860}, doi = {10.1016/j.molstruc.2025.144763}, author = {Torambetov, Batirbay and Khojabaeva, Gulnaz and Bharty, M. K. and Gupta, Sushil K. and Kadirova, Shakhnoza and Pradeep, S. and Dastager, Syed G. and Gonnade, Rajesh G.} }