scholarly journals Synthesis and X-Ray Structure of (1Z,2Z)-1,2-Bis(2-(phenylsulfonyl)-1-(4-tolyl)ethylidene)hydrazine

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Hatem A. Abdel-Aziz ◽  
Hazem A. Ghabbour ◽  
Khalid A. Al-Rashood ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Closed Vessel ◽  
X Ray ◽  
H Nmr ◽  
Dimensional Network ◽  
Intramolecular Hydrogen ◽  
Single Crystal Analysis

The title compound (1Z,2Z)-1,2-bis(2-(phenylsulfonyl)-1-(4-tolyl)ethylidene)hydrazine (5) was prepared, in 78% yield, by the reaction of 2-(phenylsulfonyl)-1-(4-tolyl)ethan-1-one (3) with hydrazine hydrate in acetic acid at 90°C under microwave irradiation in a closed vessel with power 100 W for 3 min. The structure of the newly synthesized compound was established under the basis of its IR, mass,1H NMR, and X-ray single crystal analysis. The crystal of5belongs to monoclinic space group,P21/c, witha=5.2944(3) Å,b=17.5748(9) Å,c=15.4701(8) Å,β=105.767(4)°,Z=2,V=1385.30(13) Å3,Dc=1.306 Mg m−3,μ=2.05 mm−1,F(000)=572,R=0.075, andwR=0.224for 1419 observed reflections withI>2σ(I). The asymmetric unit of compound5contains one molecule withZconfiguration about the C7=N1 and C7A=N1A double bond. ThisZconfiguration of5is stabilized by intramolecular hydrogen bonds C1–H1A⋯N1 and C1A–H1AA⋯N1A. The molecular packing in the crystal structure of5is stabilized by intermolecular interactions forming a three-dimensional network.

Crystal Structure and Tautomerism of 1-[N-(4-Iodophenyl)]aminomethylidene-2(1H)naphthalenone

2001 ◽  
Vol 56 (10) ◽  
pp. 1003-1008 ◽  
Author(s):  
H. Ünver ◽  
M. Kabak ◽  
D. M. Zengin ◽  
T. N. Durlu
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Quantum Mechanical ◽  
Monoclinic Space Group ◽  
Quantum Mechanical Calculations ◽  
X Ray ◽  
H Nmr ◽  
Mechanical Methods ◽  
Intramolecular Hydrogen ◽  
Semi Empirical

1-[N-(4-Iodophenyl)]aminomethylidene-2(1H)naphthalenone (1) (C17H12NOI) has been studied by X-ray analysis, IR, 1H NMR, UV and AM1 semi-empirical quantum mechanical methods. It crystallises in the monoclinic space group P21/n with a = 4.844(3), b = 21.428(2), c = 13.726(2) Å, ß = 93.07(2)° (R1 =0.032 for 4132 reflections [I > 2σ(I)]). The title compound is not planar and an intramolecular hydrogen bond connects O1 and N1 [2.530(4) Å]. Complementary IR, 1H NMR and UV measurements out. Tautomerism and conformations of the title semi-empirical quantum mechanical calculations and the results are compared with the X-ray data.

Two polymorphs ofN-(2-methoxyphenyl)-4-oxo-4H-chromone-3-carboxamide

2013 ◽  
Vol 69 (8) ◽  
pp. 927-933 ◽  
Author(s):  
Ligia R. Gomes ◽  
John Nicolson Low ◽  
Fernanda Borges ◽  
Fernando Cagide
Keyword(s):  
Hydrogen Bonds ◽  
Molecular Conformation ◽  
Three Dimensional ◽  
Amide Group ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Intramolecular Hydrogen Bonds ◽  
Compound C ◽  
Dimensional Network ◽  
Intramolecular Hydrogen

The title compound, C17H13NO4, crystallizes in two polymorphic forms, each with two molecules in the asymmetric unit and in the monoclinic space groupP21/c. All of the molecules have intramolecular hydrogen bonds involving the amide group. The amide N atoms act as donors to the carbonyl group of the pyrone and also to the methoxy group of the benzene ring. The carbonyl O atom of the amide group acts as an acceptor of the β and β′ C atoms belonging to the aromatic rings. These intramolecular hydrogen bonds have a profound effect on the molecular conformation. In one polymorph, the molecules in the asymmetric unit are linked to form dimers by weak C—H...O interactions. In the other, the molecules in the asymmetric unit are linked by a single weak C—H...O hydrogen bond. Two of these units are linked to form centrosymmetric tetramers by a second weak C—H...O interaction. Further interactions of this type link the molecules into chains, so forming a three-dimensional network. These interactions in both polymorphs are supplemented by π–π interactions between the chromone rings and between the chromone and methoxyphenyl rings.

scholarly journals A New 3D Coordination Polymer of Bismuth with Nicotinic AcidN-Oxide

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Farzin Marandi ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Crystal Structure ◽  
Thermal Stability ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Thermal Stability Of

The new three-dimensional coordination polymer {[Bi(NNO)2(NO3)]·1.5H2O}n(1, NNO−= nicotinateN-oxide) was synthesized and characterized by elemental analysis, IR and1H-NMR spectroscopy, as well as single-crystal X-ray diffraction analysis.1crystallizes in the monoclinic space group C2/c. The crystal structure consists of a rectangular-shaped grid constructed with NNO linkers. Cavities of a diameter of 7.9–8.3 Å2are filled with disordered water molecules. The thermal stability of the compound was evaluated by thermogravimetric analysis.

scholarly journals Crystal structure of 3,14-dimethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.07,12]docosane tetrachloride tetrahydrate from synchrotron X-ray data

2018 ◽  
Vol 74 (8) ◽  
pp. 1039-1041
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Synchrotron Radiation ◽  
Three Dimensional ◽  
Water Molecules ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Dimensional Network

The crystal structure of the title salt, C20H44N4 4+·4Cl−·4H2O, has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at all four amine N atoms. The asymmetric unit contains one half-cation (completed by crystallographic inversion symmetry), two chloride anions and two water molecules. There are two molecules in the unit cell. The Cl− anions and hydrate molecules are involved in hydrogen bonding. The crystal structure is stabilized by intermolecular hydrogen bonds involving the macrocycle N—H groups and water O—H groups as donors and the O atoms of the water molecules and the Cl− anions as acceptors, giving rise to a three-dimensional network.

scholarly journals Crystal structure of 3,14-diethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.07,12]docosane tetrachloride tetrahydrate from synchrotron X-ray data

2021 ◽  
Vol 77 (2) ◽  
pp. 213-216
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Synchrotron Radiation ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Water Molecules ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Dimensional Network

The crystal structure of the hydrated title salt, C22H48N4 4+·4Cl−·4H2O (C22H48N4 = H4 L = 3,14-diethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.07,12]docosane), has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at all four amine N atoms. The asymmetric unit comprises one half of the macrocyclic cation (completed by crystallographic inversion symmetry), two chloride anions and two water molecules. The macrocyclic ring of the tetracation adopts an exodentate (3,4,3,4)-D conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the macrocycle N—H groups and water O—H groups as donors, and the O atoms of the water molecules and chloride anions as acceptors, giving rise to a three-dimensional network.

Synthesis, crystal structure and topological analysis of a three-dimensional polymeric network based on zinc(II), potassium and 5-sulfobenzene-1,3-dicarboxylate (SIP)

2018 ◽  
Vol 74 (8) ◽  
pp. 981-985
Author(s):  
Flávia H. Silva ◽  
Chris H. J. Franco ◽  
Charlane C. Corrêa ◽  
Renata Diniz
Keyword(s):  
Crystal Structure ◽  
Topological Analysis ◽  
Three Dimensional ◽  
Strong Interactions ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Rigidity ◽  
Dimensional Network ◽  
Point Symbol

Aromatic polycarboxylate linkers provide structural rigidity and strong interactions among the metal centre and the carboxylate O atoms. A new three-dimensional coordination polymer namely, catena-poly[potassium [tetraaqua(μ-5-sulfobenzene-1,3-dicarboxylato)zinc(II)]], {K[Zn(C8H3O7S)(H2O)4]} n or {K[Zn(SIP)(H2O)4]} n , where SIP is 5-sulfobenzene-1,3-dicarboxylate or 5-sulfoisophthalate, was obtained and characterized by elemental analysis and IR vibrational spectroscopy, and the single-crystal structure was determined by X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/n with Z = 4. Topological analysis revealed that K—O interactions form a two-dimensional network, which is uninodal 4-connected and can be described with a point symbol (44.62), and this plane network is classified as sql/Shubnikov. The layers are connected by Zn2+ ions coordinated to the SIP linker, forming a three-dimensional network. This net is a trinodal (3,5,6)-connected system with point symbol (3.44.52.62.73.83).(3.44.52.62.7).(3.72).

Determination of the structure of p-methylbenzamidinium formate monohydrate

1988 ◽  
Vol 53 (12) ◽  
pp. 3131-3137
Author(s):  
Bohumil Kratochvíl ◽  
Jan Ondráček ◽  
Jindřich Hašek ◽  
László Csordás
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Intermolecular Hydrogen Bonds ◽  
Dimensional Network ◽  
Intramolecular Hydrogen

The molecular and crystal structure of p-methylbenzamidinium formate monohydrate, C9H14N2O3, was solved by direct methods. The positions of all the atoms were localized and the structure was refined anisotropically. The final value of the R factor equalled 0·043 for 1 150 observed reflections (I > 1·96σ(I)). The substance crystallizes in the P21/c monoclinic space group with lattice parameters a = 1 038·9(4), b = 1 146·1(5), c = 912·4(3) pm, β = 94·77(3)0, Z = 4. The molecule contains an amidinium-carboxylate bond, formed by two intramolecular hydrogen bridges of the N-H···O type. Intermolecular hydrogen bonds are formed by the side hydrogen atoms of the amidine and the hydrogen atoms of the water molecule and are of the N-H···O and O-H···O types; they form a three-dimensional network in the crystal structure. In this, the structure of p-methylbenzamidinium formate monohydrate differs from the related structures of benzamidinium pyruvate and benzamidinium bromoacetate, characterized by infinite intermolecular chains formed through hydrogen bonding.

scholarly journals Crystal structure of bis(4-benzoylpyridine-κN)bis(methanol-κO)bis(thiocyanato-κN)nickel(II) methanol monosolvate

2019 ◽  
Vol 75 (2) ◽  
pp. 299-303 ◽  
Author(s):  
Carsten Wellm ◽  
Christian Näther
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Three Dimensional ◽  
Asymmetric Unit ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network ◽  
Pure Phase

The asymmetric unit of the title compound, [Ni(NCS)2(C12H9NO)2(CH3OH)2]·CH3OH, comprises one NiII cation, two thiocyanate anions, two 4-benzoylpyridine coligands, two coordinating, as well as one non-coordinating methanol molecule. The NiII cation is coordinated by two terminally N-bonded thiocyanate anions, the N atoms of two 4-benzoylpyridine coligands and the O atoms of two methanol ligands within a slightly distorted octahedron. Individual complexes are linked by intermolecular O—H...S hydrogen bonding into chains parallel to [010] that are further connected into layers parallel to (10\overline{1}) by C—H...S hydrogen bonds. Additional C—H...O hydrogen-bonding interactions lead to the formation of a three-dimensional network that limits channels extending parallel to [010] in which the non-coordinating methanol molecules are located. They are hydrogen-bonded to the coordinating methanol molecules. X-ray powder diffraction revealed that the compound could not be prepared as a pure phase.

scholarly journals Crystal structure of 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane bis(perchlorate) dichloride from synchrotron X-ray data

2020 ◽  
Vol 76 (3) ◽  
pp. 324-327 ◽  
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Chloride Anion ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Dimensional Network

The crystal structure of title salt, C14H36N4 4+·2ClO4 −·2Cl−, has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at all four amine N atoms. The asymmetric unit contains one half-cation (completed by crystallographic inversion symmetry), one perchlorate anion and one chloride anion. A distortion of the perchlorate anion is due to its involvement in hydrogen-bonding interactions with the cations. The crystal structure is consolidated by intermolecular hydrogen bonds involving the 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane N—H and C—H groups as donor groups, and the O atoms of the perchlorate and chloride anion as acceptor groups, giving rise to a three-dimensional network.

scholarly journals Crystal structure of bis[(oxalato-κ2O1,O2)(1,4,8,11-tetraazacyclotetradecane-κ4N)chromium(III)] dichromate octahydrate from synchrotron X-ray data

2017 ◽  
Vol 73 (3) ◽  
pp. 403-406 ◽  
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Distorted Octahedral Geometry ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Dimensional Network ◽  
Oxalate Ligand ◽  
Distorted Octahedral

The asymmetric unit of the title compound, [Cr(C2O4)(C10H24N4)]2[Cr2O7]·8H2O (C10H24N4= 1,4,8,11-tetraazacyclotetradecane, cyclam; C2O4= oxalate, ox) contains one [Cr(ox)(cyclam)]+cation, one half of a dichromate anion that lies about an inversion centre so that the bridging O atom is equally disordered over two positions, and four water molecules. The terminal O atoms of the dichromate anion are also disordered over two positions with a refined occupancy ratio 0.586 (6):0.414 (6). The CrIIIion is coordinated by the four N atoms of the cyclam ligand and one bidentate oxalato ligand in acisarrangement, resulting in a distorted octahedral geometry. The Cr—N(cyclam) bond lengths are in the range 2.069 (2)–2.086 (2) Å, while the average Cr—O(ox) bond length is 1.936 Å. The macrocyclic cyclam moiety adopts thecis-V conformation. The dichromate anion has a staggered conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups and water O—H groups as donors, and the O atoms of oxalate ligand, water molecules and the Cr2O72−anion as acceptors, giving rise to a three-dimensional network.

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