scholarly journals Crystal Structure of Novel Terephthalate Salt of Antiarrhythmic Drug Disopyramide

Crystals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 368
Author(s):  
Majid Ismail Tamboli ◽  
Yohei Utusmi ◽  
Takayuki Furuishi ◽  
Kaori Fukuzawa ◽  
Etsuo Yonemochi
Keyword(s):  
Hydrogen Bond ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Triclinic System ◽  
Acidic Proton ◽  
Salt Crystals ◽  
Tertiary Amino

1:1 salt of Disopyramide (DPA) with Terephthalic acid (TA) was obtained by the slow solvent evaporation and the slurry crystallization methods. X-ray single crystal diffraction of DPA:TA confirmed the formation of salt by the transfer of an acidic proton from one of the carboxylic acidic groups of TA to the tertiary amino group of the chain moiety (N3-nitrogen atom) of the DPA molecules. DPA:TA salt crystals crystalize in the triclinic system with space group P-1. The asymmetric unit, comprising one protonated DPA and one TA anion, are linked by a strong charge assisted N+–H∙∙∙O¯ hydrogen bond and a C–H∙∙∙O¯ hydrogen bond. Moreover, structural characterization of DPA:TA salt was carried out using Fourier transform infrared spectroscopy, differential scanning calorimeter, thermogravimetric analysis, and powder X-ray diffraction techniques

Synthesis and Structural Characterization of Diisopropylammonium Trifluoroacetate and Diisoproplyammonium Pentafluoropropionate

2010 ◽  
Vol 65 (4) ◽  
pp. 479-484 ◽  
Author(s):  
Guido J. Reiß ◽  
Michaela K. Meyer
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Van Der Waals Interactions ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Donor Acceptor ◽  
Double Hydrogen

Diisopropylammonium trifluoroacetate ({[iPr2NH2][CF3COO]}; dip tfa; 1) and diisopropylammonium pentafluoropropionate ({[iPr2NH2][C2F5COO]}; dip pfp; 2) have been synthesized and structurally characterized by X-ray diffraction and spectroscopic methods. Both compounds form hydrogen-bonded cyclic dimers (Etter symbol: R44 (12)) in the solid state. The asymmetric unit of 1 contains one trifluoroacetate anion and one dip cation in the centrosymmetric space group Pī. The asymmetric unit of 2 consists of two crystallographically independent pentafluoropropionate anions and two independent dip cations forming dimers in the form of rings, both lying around centers of symmetry in the space group Pī. In dip tfa and dip pfp the cations act as double hydrogen bond donors, and each of the two oxygen atoms of the carboxyl group are single hydrogen bond acceptors. The donor acceptor distances of the N-H...O hydrogen bonds are within the expected range for medium strong hydrogen bonds. The quasi-molecular cyclic dimers are connected with neighboring units only by van der Waals interactions.

Synthesis of ReItricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two ReIdinuclear structures bridged by S atoms

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith
Keyword(s):  
Hydrogen Bond ◽  
Intermolecular Hydrogen Bond ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Pyridine Ligand ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Mononuclear Complexes

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.

Structural characterization of p-benzosemiquinone radical in a solid state: the radical stabilization by a low-barrier hydrogen bond

2006 ◽  
Vol 62 (6) ◽  
pp. 1051-1060 ◽  
Author(s):  
Krešimir Molčanov ◽  
Biserka Kojić-Prodić ◽  
Mario Roboz
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Variable Temperature ◽  
Organic Radical ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Packings ◽  
Dynamical Disorder ◽  
Benzenoid Ring

Semiquinone (p-benzosemiquinone), a transient organic radical, was detected in the solid state by EPR spectroscopy revealing four symmetrically equivalent protons. A variable-temperature X-ray diffraction analysis (293 and 90 K) and EPR data support a dynamical disorder of the proton. A low-barrier O—H···O hydrogen bond stabilizes the radical. The C—O bond length is 1.297 (4) Å, corresponding to a bond order of ca 1.5. The geometry of the radical implies an electron delocalization throughout the benzenoid ring. Two polymorphs of semiquinone, monoclinic and triclinic, were observed and their structures determined. Their crystal packings were compared with those of quinhydrone polymorphs.

X-ray characterization of tripyridinium bis[tetrabromidoferrate(III)] bromide asymmetric unit in solution by Debye function analysis

2016 ◽  
Vol 30 (24) ◽  
pp. 1650174
Author(s):  
F. Baniasadi ◽  
N. Sahraei ◽  
M. B. Fathi ◽  
M. M. Tehranchi ◽  
N. Safari ◽  
...  
Keyword(s):  
Density Functional ◽  
Function Analysis ◽  
Dilute Solution ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Debye Function ◽  
Functional Theory ◽  
X Ray ◽  
Diluted Solution

Abundant asymmetric unit of the [FeBr4]2[py.H]3Br magnetic molecule in the acetonitrile solvent was characterized via Debye function analysis (DFA) of the X-ray powder diffraction pattern from dilute solution. A diluted solution of the material in acetonitrile solvent has been prepared to reduce, as far as possible, the interaction between the molecular units. The X-ray diffraction from the sample was measured and Debye function simulations of three out of ten chemically plausible molecular units were observed to suitably comply with the experimental results. These three configurations were further optimized with first-principles method in the framework of density functional theory (DFT) and the most stable structure according to the calculated total energy is presented.

Synthesis and Structural Characterization of Zn(II) Coordination Polymer Material

2011 ◽  
Vol 282-283 ◽  
pp. 100-103 ◽  
Author(s):  
Li Hua Wang
Keyword(s):  
Hydrogen Bond ◽  
Coordination Polymer ◽  
Chain Structure ◽  
Title Complex ◽  
Dimensional Chain ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
One Dimensional ◽  
X Ray

In order to synthesize a new catalysis material, the title complex, [Zn(2,2’-bipyridine)(H2O)2(SO4)]n, was prepared and determined by X-ray diffraction. The results shows that the compound was crystallized in the monoclinic system, space groupC2/c, witha= 15.4304(14) Å,b= 12.7150(11) Å,c= 6.7068(5) Å,β= 102.103(10)º,V= 1286.61(19) Å3,Z= 4. The geometry of Zn(II) is a distortedcis-ZnN2O4octahedron. In the structure of the title complex, a one-dimensional chain structure is formed by hydrogen-bond.

Three new amidophosphoric acid esters with a P(O)[OCH2C(CH3)2CH2O] segment: X-ray diffraction, DFT, AIM and Hirshfeld surface investigations of bi- and tri-furcated (three and four-center) hydrogen bond interactions

2020 ◽  
Vol 235 (3) ◽  
pp. 69-84 ◽  
Author(s):  
Marjan Sadat Bozorgvar ◽  
Atekeh Tarahhomi ◽  
Arie van der Lee
Keyword(s):  
Hydrogen Bond ◽  
Crystal Packing ◽  
Closed Shell ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Amidophosphoric Acid ◽  
Acid Esters

AbstractStructural and packing features of three new amidophosphoric acid esters having a common part XP(O)[OCH2C(CH3)2CH2O], with X = [(CH3)3CNH] (1), [(CH3)2HCNH] (2) and [C6H11(CH3)N] (3), are investigated by single crystal X-ray diffraction. The results illustrate that the compounds 1 and 3 crystallize with one independent molecule in the asymmetric unit; whereas, for 2, the compound crystallizes with three independent molecules in the asymmetric unit. The crystal structures are mostly stabilized via tri-furcated hydrogen bond interactions (C–H · · ·)2(N–H · · ·)O=P in 1 and (C–H · · ·)3O=P in 3, while the stability is given by bi-furcated hydrogen bond interactions (C–H · · ·)(N–H · · ·)O=P in 2. For a better understanding of the nature, strength and energetics associated with the formation of the quoted multi-center hydrogen bond interactions, the Natural Bond Order (NBO) method from Density Functional Theory (DFT) and a topological analysis by means of Atoms In Molecules (AIM) and Hirshfeld surface procedures were performed. These studies reveal that the studied multi-center hydrogen bond interactions of the type O · · · H are favoured in the crystal packing displaying enrichment ratios larger than unity. The detailed nature of the different interactions in these multi-center interactions is studied for the first time in such compounds. It is shown that the N–H · · · O interaction is rather non-covalent closed-shell whereas the C–H · · · O interaction is more van der Waals closed-shell. Stronger hydrogen bond interactions are observed for a lower multiple H-atom acceptor oxygen in three-center hydrogen bond interactions (C–H · · ·)(N–H · · ·)O=P of 2 than for four-center interactions in 1 [i.e. (C–H · · ·)2(N–H · · ·)O=P] and 3 [i.e. (C–H · · ·)3O=P]. The better H-atom acceptability of the O atom of P=O compared with the esteric O atom is explained by the richer s-character of the hybrid orbital of the O atom acceptor of P=O coupled with enhance of the polarization and charge. The obtained results are also confirmed by Molecular Electrostatic Potential (MEP).

Synthesis and Structural Characterization of a Cu(II) Coordination Polymer from N1,N2-Di(pyridin-4-yl)oxalamide

2014 ◽  
Vol 69 (9-10) ◽  
pp. 1045-1049
Author(s):  
Hai-Wei Kuai ◽  
Tao Hu ◽  
Ding-Yun Jiang ◽  
Yun-Hua Qian ◽  
Deng-Hao Li
Keyword(s):  
Hydrogen Bonding ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Chain Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Triclinic System ◽  
A Chain ◽  
2D Network

Abstract The reaction of Cu(NO3)2·3H2O with N1,N2-di(pyridin- 4-yl)oxalamide (L) and KSCN in the presence of DMF by the layering method gives rise to a new complex [Cu(L2)(SCN)2(DMF)2]n (1). Complex 1 has been characterized by single-crystal and powder X-ray diffraction, IR spectroscopy, and elemental and thermogravimetric analyses. It crystallizes in the triclinic system with space group P1̅ and shows a chain structure. Delicate N-H···O hydrogen bonding exists in individual units, and adjacent chains are linked by intermolecular interactions, resulting in an extended 2D network.

scholarly journals Absolute structure and absolute configuration

1999 ◽  
Vol 55 (5) ◽  
pp. 908-915 ◽  
Author(s):  
H. D. Flack ◽  
G. Bernardinelli
Keyword(s):  
Single Crystal ◽  
Absolute Configuration ◽  
Structure Determination ◽  
Diffraction Experiment ◽  
X Ray Diffraction ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Absolute Structure

Fundamental notions concerning absolute structure and absolute configuration, and their determination from single-crystal diffraction measurements, are presented and reviewed. A glossary of terms with definitions useful in this field is provided. For absolute structure and its determination, the separate but interacting influences of the structure and the inversion-distinguishing power of an X-ray diffraction experiment with dispersive scatterers are examined. Important experimental and algorithmic details of the current methods used for absolute-structure determination are provided. Characterization of crystals for absolute-structure determination and of molecules for absolute-configuration determination are treated. Attention is given to the analysis of absolute structure and absolute configuration in twinned crystals.

The Preparation and Crystal Structures of the 1 : 1 Adducts of 5-Nitrosalicylic Acid and 2-Chloro-3,5- dinitrobenzoic Acid with Triphenylphosphine Oxide

1998 ◽  
Vol 51 (5) ◽  
pp. 437 ◽  
Author(s):  
Graham Smith ◽  
Daniel E. Lynch ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Triphenylphosphine Oxide ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonding ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Phosphoryl Oxygen

The (1 : 1) adducts of 5-nitrosalicylic acid (5-nsa) and 2-chloro-3,5-dinitrobenzoic acid (cdnba) with triphenylphosphine oxide (tppo), [(5-nsa)(tppo)] (1) and [(cdnba)(tppo)] (2), have been prepared and their structures determined by X-ray diffraction and reffned to residuals R 0·045 (1) and 0·043 (2) for 2540 and 3265 observed reflections respectively. Crystals of both adducts are monoclinic, space group P21/c (1) and P21/a (2), with 4 dimer units in cells of dimensions a 16·217(1), b 7·6807(8), c 19·697(4) Å, β 113·357(8)° [for (1)] and a 16·009(5), b 8·687(1), c 17·640(5) Å, β 90·30(1)o [for (2)]. In both examples, the two molecules comprising the asymmetric unit are linked by a single hydrogen bond between the proton of the carboxylic acid and the phosphoryl oxygen of tppo [O- - -O, 2·524(3) Å (1); 2·72(3) Å (2)], while, in each case, the additional functional groups of the acid are not involved in any other intermolecular hydrogen-bonding interactions.

Exploring the complex map of insulin polymorphism: a novel crystalline form in the presence of m-cresol

2020 ◽  
Vol 76 (4) ◽  
pp. 366-374 ◽  
Author(s):  
Fotini Karavassili ◽  
Alexandros Valmas ◽  
Maria Dimarogona ◽  
Anastasia E. Giannopoulou ◽  
Stavroula Fili ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Form ◽  
Crystalline Form ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Potential Use

In this study, the first crystal structure of a novel crystal form of human insulin bound to meta-cresol in an acidic environment is reported. The combination of single-crystal and powder X-ray diffraction crystallography led to the detection of a previously unknown monoclinic phase (P21). The structure was identified from the powder patterns and was solved using single-crystal diffraction data at 2.2 Å resolution. The unit-cell parameters at pH 6.1 are a = 47.66, b = 70.36, c = 84.75 Å, β = 105.21°. The structure consists of two insulin hexamers per asymmetric unit. The potential use of this insulin form in microcrystalline drugs is discussed.

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