Molecular Structure of Quinolin-1-(2-quinolyl)-2-one mesitylimine: An Unusual Amination Product of 2,4,6-Trimethylaniline and 2-Chloroquinoline

Abstract  The molecular structure of quinolin-1-(2-quinolyl)-2-one mesitylimine has been determined. The Buchwald-Hartwig amination of mesitylaniline with two equivalents of 2-chloroquinoline results in dearomatization of one quinoline heterocycle, forming an imine with the mesitylaniline nitrogen and aminating the second 2-chloroquinoline via the cyclic nitrogen. The mesityl and quinoline moieties are nearly perpendicular to the plane of the central quinolyl structure. Rationalization of the imine formation is found by a consideration of the relative stability of the syn and anti conformations of the reaction intermediate. Crystal data: space group P2₁/c, a = 12.609(3), b = 15.010(3), c = 12.456(3) ?, β = 112.68(3)°; V = 2,175.3(8) ?³, Z = 4, R = 0.0649, wR₂ = 0.1498. Graphical Abstract  The amination of mesitylaniline with two equivalents of 2-chloroquinoline results in dearomatization of one quinoline heterocycle, forming an imine with the mesitylaniline nitrogen and aminating the second 2-chloroquinoline via the cyclic nitrogen.      

Crystal Structure of N-(tert-Butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)cyclohexane Carboxamide

Abstract  The crystal structure of N-(tert-butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)-cyclohexane-carboxamide 1 has been determined. The title compound crystallized in the orthorhombic space group pbca with cell parameters, a = 10.6556(6) ?, b = 18.0132(11) ?, c = 19.5513(12) ?, v = 3752.7(4) ?³, Z = 8, D _cal = 1.269 Mg/m³ at T = 120 K. The structure refined by full-matrix least-squares procedures to find R ₁ = 0.0463 and wR ₂ = 0.0937 for 3059 reflections. The soxazole ring isn’t coplanar with the phenyl ring. Index Abstract  The crystal structure of N-(tert-butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)-cyclohexane-carboxamide 1 has been studied.      

Crystal Structure of the Tunnel-like Supramolecular Complex: Methylviologen(2+) Octaaquaoxalatodiiron(II) Disulfate

Abstract  The 3D supramolecular complex, (C₁₂H₁₄N₂)[Fe(II)₂(C₂O₄)(OH₂)₈] · 2(SO₄)²⁻, is monoclinic, P2₁/n, with the following cell parameters: a = 8.0413(16) ?, b = 17.272(4) ?, c = 9.806(2) ?, β = 106.25(3)°, V = 1307.6(5) ?³, Z = 2, R ₁ = 0.0344, and wR ₂ = 0.0763. X-ray crystallography revealed that the structure can be regarded as a hydrogen-bonded tunnel-like supramolecule with the methylviologen lying in the tunnel as the charge compensating cation. The multiple intermolecular hydrogen bonds between the octaaquaoxalatodiiron cations and the isolated sulfate ions link the supramolecular complex into a quasi-three-dimensional open-framework structure. Graphical Abstract  Crystal Structure of the Tunnel-like Supramolecular Complex: Methylviologen(2+) Octaaquaoxalatodiiron(II) Disulfate Xin Yang, Jiang Li, Shenyi Shi, Yawei Hou and Yongkui Shan A hydrogen-bonded tunnel-like supramolecular structure with the methylviologen lying in the tunnel as the charge compensating cation has been synthesized for the first time.      

Crystal of Tetrakis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II)

Abstract  A new complex [Cu(NCS)₄ (N-Eim)₄] [Cu(NCS)₂ (N-Eim)₂] (where N-Eim = N-ethylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Triclinic space group P−1 with the parameters: a = 8.7707(18) ?, b = 10.712(2) ?, c = 13.511(3) ?, α = 104.73(3)°, β = 104.84(3)°, γ = 102.52(3)°, V = 1131.54(3) ?³, with Z = 1 formula units. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments; one is coordinated by four N-ethyl-imidazole ligands and two axial SCN groups, and another by two SCN groups and two N-ethyl-imidazole ligands. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim)₄] units. Index Abstract  The title compound, tetrakis(1-ethyl-1H-imidazole)diisothio cyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim) 4] units.      

The Preparation, Characterization and X-ray Structural Analysis of Tetrakis[1-Methyl-3-(2-Propyl)-2(3H)-Imidazolethione]Cadmium(II) Hexafluorophosphate

Abstract  A new compound, [Cd(mipit)₄][PF₆]₂ has been synthesized and characterized via standard solid and solution state methods including single crystal X-ray crystallography (mipit = 1-methyl-3-(2-propyl)-2(3H)-imidazolethione). The title compound crystallizes in tetragonal space group I4 ₁ /a with a = 12.478(2) ?, b = 12.478(2) ?, c = 28.806(6) ?, and Z = 4. The complex is a high melting, colorless solid that has a distorted tetrahedral CdS₄ coordination geometry. Thermogravimetric analysis results for the title compound as well as for another potential CdS synthon and two potential CdSe synthons are reported. Graphical Abstract  The synthesis and characterization of the title compound, a new ionic homoleptic cadmium complex, tetrakis[1-methyl-3-(2-propyl)-2(3H)-imidazolethione]cadmium(II) hexafluorophosphate is reported. The results of a single crystal X-ray diffraction analysis reveal a distorted tetrahedral CdS₄ coordination sphere about the cadmium. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal and Molecular Structure of the 1:2 Salt Formed Between 1,2-(4-Pyridyl)Ethane and 2-(4-Hydroxyphenylazo)Benzoic Acid

Abstract  Proton transfer occurred during co-crystallization of 1,2-(4-pyridyl)ethane with 2-(4-hydroxyphenylazo)benzoic acid to yield a salt comprising a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions. Centrosymmetrically related anions associate by charge-assisted O–H···O hydrogen bonds to form 24-membered {···OC₃N₂C₄OH}₂ synthons. These are connected into a supramolecular polymer via charge-assisted N–H···O hydrogen bonds involving the 1,2-bis(4-pyridinium)ethane dications. The compound crystallizes in the triclinic space group P−1 with a = 8.517(4) ?, b = 9.110(5) ?, c = 10.477(5) ?, α = 96.850(13)°, β = 94.446(12)°, γ = 104.946(10)° and Z = 1 {two anions and a dication}. Index Abstract  Supramolecular chains mediated by charge-assisted O–H···O and N–H···O hydrogen bonding are found in the salt containing a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions.      

Crystal Structure of bis(18-Crown-6)-bis(formato-O) dicaesium dihydrate

Abstract  The crystal structure of the title compound, [2Cs⁺(C₁₂H₂₄O₆)₂(CHO₂ ⁻)₂(H₂O)₂], was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁ /n with cell parameters a = 10.4278(7) ?, b = 10.0183(5) ?, c = 18.2383(12) ?, β = 93.723(5)°, V = 1910.3(2) ?³ and Z = 2. The Cs cations are bonded to each of the six O atoms of a crown ether ring, two water molecules, and one O atom of a formato anion. As a result of that, a centrosymmetric dimeric dinuclear complex is formed. The two halves of the dimer are connected by a ring of formato anions and water molecules which are linked by O–H···O hydrogen bonds. Index Abstract  The title compound, bis(18-crown-6)-bis(formato-O), caesium dihydrate, features a centrosymmetric dimeric dinuclear complex where two Cs cations are coordinated by six O atoms of a crown ether ring. The two halves of this complex are held together by a ring of formato anions and water molecules which are linked by hydrogen bonds.      

Synthesis and Structure of a CdI<Subscript>2</Subscript> Coordination Polymer with 1,4-Bis(benzimidazole-1-yl-methylene)benzene (bbmb)

Abstract  In this paper, solution reaction of cadmium iodide with organic multifunctional ligand 1,4-bis(benzimidazole-1-yl-methylene)benzene generated a 1D polymer [CdI₂ (bbmb). (DMF) (CH₃CN)]_n 1, and the crystal structure has been determined (C₂₇H₂₈CdI₂N₆O), Mr = 818.75, a  = 14.929(1) ?, b = 17.381(2) ?, c = 15.850(1) ?, β = 114.8190(10)°, space group C2/c, Z = 4, and V = 3733.3(6) ?³. In 1 the tetrahedral coordination of Cd(II) and the conformation of the bbmb ligand make it a wave-shaped structure.

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Graphical Abstract  Synthesis and structure of a CdI2 coordination polymer with 1,4-bis(benzimidazole-1-yl-methylene)benzene(bbmb) Xiucun Liu, Xiaoling Guo, Yunyin Niu, Qingli Wang, Qian Cui, Hongwei Hou, Xiaorui Lv, SeikWeng Ng Solution reaction of cadmium iodide with organic multifunctional ligand 1,4-bis(benzimidazole-1-yl-methylene)benzene (bbmb) generated a 1D polymer [CdI₂ (bbmb) (DMF)(CH₃CN)]_n, in which the tetrahedral coordination of Cd(II) and the conformation of bbmb ligand make it a wave-shaped structure.

     

Synthesis and Crystal Structure of a New Coordination Polymer from Cadmium and V-Shape Ligand Bis(imidazol-1-yl) methane

Abstract  The new coordination polymer, [Cd(BIM)₂(NO₃)₂]_n, has been prepared from the reaction of bis(imidazol-1-yl) methane (BIM) with Cd(NO₃)₂ in methanol and water. The compound were characterized by single crystal X-ray diffraction and IR spectroscopy, it crystallizes in the monoclinic space group C2/m with a = 14.400(3) ?, b = 9.3894(18) ?, c = 8.6926(17) ?, β = 123.499(2)°, V = 980.1(3) ?³, Z = 2. The Cd atoms are coordinated to four nitrogen atoms from four different BIM ligands and two nitrates to form a slightly distorted octahedral geometry. Further, the BIM ligands act as a bridged ligand to form 1D infinite cationic double chain with a 16-membered macrometallacyclic tetragonal box structure. Graphical Abstract   Synthesis and Crystal Structure of a New Coordination Polymer from Cadmium and V-Shape Ligand Bis(imidazol-1-yl) methane Chuan-Ming Jin*, Ling-Yan Wu, Zhen-Xing Zhong A new coordination polymer with 1D infinite cationic double chain with a 16-membered macrometallacyclic tetragonal box structure has been prepared from the reaction of bis(imidazol-1-yl) methane (BIM) and Cd(NO₃)₂.      

Spectroscopic Studies and Crystal Structure of 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl) methyl] Thiourea

Abstract  A new mannich base 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl)methyl] thiourea formed by the direct condensation of thiourea, succinimide and benzaldehyde has been synthesized. The structure of this mannich base has been elucidated on the basis of micro elemental analysis, IR, ¹H NMR, ¹³C NMR, Mass and UV–Visible Techniques. The crystal structure of the title compound C₁₂ H₁₃ N₃ O₂ S was determined. It crystallizes in the monoclinic system, space group P2₁/c with a = 10.8234 (7) ?, b = 6.0355 (5) ?, c = 19.3692 (14) ?, β = 100.540(3)°, Z = 4 and V = 1243.94 (16) ?³. The structure was solved by the full-matrix least squares on F ² and had a refined R value of 0.0465 for 1,964 observed reflections. The crystal structure is stabilized by strong intramolecular C–H···O, C–H···S interactions and inter molecular N–H···O and S···S interactions. Graphical Abstract  This paper describes the spectroscopic and crystallographic studies of the title compound which is essential in ascertaining the structure of this new compound.      

Crystal Structure of 2-{1-[(1-(2-Pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate,the Product of Template Condensation in the Presence of Cr(III)

Abstract  In an attempt to synthesize a Cr(III) complex of 2′-[1-(2-pyridinyl)ethylidene]oxamohydrazide an azine product 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate was obtained by an electrophilic acyl substitution catalyzed by Cr(III). Its structure was determined by X-ray crystal analysis and showed significant changes in comparison to the corresponding unprotonated compound. The 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate crystallizes in the space group P2₁/n of the monoclinic crystal system with unit cell parameters a = 14.3809(3) ?, b = 24.1516(5) ?, c = 15.4471(3) ?, β = 99.930(2)°, V = 5284.74(19) ?³ and Z = 12, i.e. three molecules per asymmetric unit. Graphical Abstract  In the template condensation of the 2′-[1-(2-pyridinyl)ethylidene]oxamohydrazide in presence of the chromium(III) ion the 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate was obtained and characterized by NMR spectroscopy and X-ray crystallography. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis,Characterization and Crystal Structure of Bis(isothiocyanato)-bis(pyridine) Zinc(II) Crystal

Abstract  Bis(isothiocyanato)-bis(pyridine) zinc(II) crystal has been prepared at room temperature and characterized by elemental analysis, IR spectrum and X-ray single crystal determination. The complex crystallizes in monoclinic space group P2₁/m with unit cell parameters: a = 5.5786(3), b = 11.0587(5), c = 12.1616(6) ?, β = 96.776(3)°, V = 745.03(6) ?³, Z = 2, D _x  = 1.514 g cm⁻³. The X-ray structure determination has revealed that the crystal is centered-symmetrical and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation. Index Abstract  The title compound, bis(isothiocyanato)-bis(pyridine) zinc(II), was synthesized by zinc compound, KSCN and C₅H₅N (pyridine) and its crystal structure was determined. Single crystal X-ray structure determination reveals that the crystal is centered-symmetrical, and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation.      

A Unusual Bridging Mode of Diphenylhydantoin in Pentaaquabis[(5,5-Diphenylhydantoinato)Potassium]

Abstract  A new complex of diphenylhydantoin, pentaaquabis[(5,5-diphenylhydantoinato)potassium], has been synthesized and the structure has been solved by X-ray diffraction. The crystals are monoclinic, space group C2/c, with a = 34.959(5) ?, b = 8.273(4) ?, c = 11.692(2) ?, β = 109.069(13)°, M _r = 670.80, V = 3196.0(17) ?³, Z = 4 and R = 0.050. The potassium cations are assembled in dimers bridged through the carbonyl O atoms of the anions. The metal atom is in a distorted octahedral coordination environment. Index Abstract  In pentaaquabis[(5,5-diphenylhydantoinato)potassium] the potassium cations are coupled in dimers through the carbonyl O atoms of the anions.      

The Synthesis and Crystal Structure of New Bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol

Abstract  The title compound bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol 8 has been synthesized and established by H NMR, IR and MS spectra and X-ray diffraction crystallography. Compound 8, C₂₃H₂₉Cl₂N₃O, Mr = 424.31, crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 14.5402(6) ?, b = 12.5888(5) ?, c = 11.6510(5) ?, α = 90o, β = 100.183o(2), γ = 90o, V = 2099.05(15) ?³, D_x = 1.343 mg m⁻³ and Z = 4. The final R was 0.0514. The molecular conformation and packing is stabilized by interactions of intermolecular O1–H1···N3′. Index Abstract  The structure of bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol by the reaction of compound 4 and Grignard regent is studied.      

Crystallographic and Conformational Analysis of [(Z)-2-ethoxy-6-[(2-hydroxyphenylamino)methylene]cyclohexa-2,4-dienone]

Abstract  The single crystal X-ray diffraction analysis of the title compound, C₁₅H₁₅NO₃, shows that the structure is adopted to its NH tautomeric form and crystallizes in the orthorhombic space group P bcn with a = 21.2424(15) ?, b = 12.7696(9) ?, c = 9.3605(10) ?, Z = 8, V = 2539.1(4) ?³, D _c  = 1.346 g/cm³. The molecular conformation in the crystal is stabilized by an intramolecular H-bond and the crystal structure is stabilized by the bifurcated O–H···O type intermolecular H-bonds. In order to understand the effects on conformational flexibility of the title molecule, molecular energy profile was calculated as a function of the selected torsion angle by means of AM1 semi-empirical method. Index Abstract  Molecular and crystal structure of [(Z)-2-ethoxy-6-[(2-hydroxyphenylamino)methylene]cyclohexa-2,4-dienone], C₁₅H₁₅NO₃, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect to the selected torsion angle has been achieved by AM1 semi-empirical calculations.      

High Temperature Ionic Liquids: Thermal Properties and Dimorphism in [1-(Methoxycarbonyl) Ethyl] Triphenylphosphonium <Emphasis Type="Italic">p</Emphasis>-Toluenesulfonate

Abstract  Investigation of the thermal properties of triphenylphosphonium p-toluenesulfonates, which are high temperature ionic liquids, reveals that they solidify to a noncrystalline material on fast cooling from the melt. During the study, a second crystalline form of [1-(methoxycarbonyl) ethyl] triphenylphosphonium p-toluenesulfonate (form II) has been obtained. Form II is monoclinic P2₁/c, with a = 11.002(5)?, b = 12.793(5)?, c = 18.805(5)?, and β = 102.498(5)°. Comparison with form I reveals the existence of a common robust structural feature involving interactions between cations and anions. Graphical Abstract  Investigation of thermal properties of ionic liquids has revealed a second crystalline form of [1-(methoxycarbonyl) ethyl] triphenylphosphonium p-toluenesulfonate.      

Spectroscopic Studies and Crystal Structure of (<Emphasis Type="Italic">Z</Emphasis>)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone

Abstract  The Schiff base (Z)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone has been synthesized from the reaction of 2-aminophenol with 2-hydroxy-3-methoxybenzaldehyde. The title compound has been characterized by elemental analysis, FT-IR, ¹H-NMR, ¹³C-NMR and UV–Visible techniques. The structure of the title compound also was determined crystallographically. The crystal structure has been solved by direct methods and refined by full-matrix least squares. The title compound crystallize in the monoclinic space group P2₁/c with a = 10.438(1), b = 8.851(1), c = 12.746(1) ?, β = 95.72(1)°, V = 1171.7(2) ?³, D _x  = 1.379 g cm⁻³, respectively (R1 = 0.0522 and wR2 = 0.126 for 1442 reflections [I > 2σ(I)]). Index Abstract   N-salicylideneaniline derivatives have been shown to exist as tautomeric forms due to intramolecular proton shifts between the phenol-oxygen and the imine-nitrogen, via intramolecular hydrogen bonding O–H···N or O···H–N.      

An X-Ray Crystallographic Study of the Novel Aminal bis-(<Emphasis Type="Italic">p</Emphasis>-Ethoxycarbonylphenylamino-)methane

Abstract  The crystal structure of bis-(p-Ethoxycarbonylphenylamino-)methane (1) has been determined by single crystal X-ray diffraction analysis. The bis-aminal (1) molecule is V-shaped and situated on a twofold axis passing through C1 with the phenyl rings forming a dihedral angle of 70.2(1)°. The carboxylate and phenyl groups are coplanar. The crystal structure of 1 is compared with the structure of the closely related aminals, 2–5. Crystal data: 1 C₁₉H₂₂N₂O₄, tetragonal, space group I4 ₁ cd (N.110), a = 20.4760(7) Ǻ, b = 20.4760(7) Ǻ, c = 8.2984(3) ?, and V = 3477.7(2) ?³, for Ζ = 8. Index Abstract  The crystal structure of bis-(p-ethoxycarbonylphenylamino-)methane (1) has been determined by single crystal X-ray diffraction analysis.      

Synthesis and Crystal Structure of a Mixed-Ligand Cobalt(II) Complex with 2-Aminobenzimidazole

Abstract  The cobalt(II) complex, [Co(abz)₂(SCN)₂] 1, has been synthesized by the reaction of cobalt(II) nitrate with ammonium thiocyanate and abz ligands (abz = 2-aminobenzimidazole), and was fully structurally characterized by elemental analysis, IR spectra, X-ray diffraction and thermogravimetric experiments. It crystallizes in the triclinic P-1 space group with a = 8.6316(10), b = 9.3426(10), c = 13.254(2) ?, α = 95.793(2), β = 95.870(2), γ = 115.7380(10), V = 945.1(2) ?³, and Z = 2. The central cobalt(II) atom is four-coordinated to nitrogen donors from two neutral abz ligands and two isothiocyanate anions respectively, adopting a slightly distorted tetrahedral geometry. In addition, the intermolecular N–H···N and N–H···S hydrogen bonds interactions link the discrete mononuclear units into infinite three-dimensional networks. Index Abstract  The essence sentence of the paper: In the mixed-ligand mononuclear complex, [Co(abz)₂(SCN)₂], the four coordinated cobalt(II) atom exhibits a slightly distort tetrahedron, which is further assembled into 3D infinite network by intermolecular hydrogen interactions.      

The Synthesis and Crystal Structure of 5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl Acid

Abstract  5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl acid 3 was synthesized from 1-aminonaphthalene. The yielded product 3 was investigated with X-ray crystallographic, NMR, MS and IR techniques. Compound 3, C₁₄H₁₁N₃O₂, Mr = 253.26, crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 10.068(2), b = 12.353(2), c = 20.102(4) ?, V = 2500.1(8) ?³, Z = 8, Dx = 1.346 Mgm^-3. The final R was 0.0474. The molecular packing is stabilized by intermolecular O–H···N interactions. Index Abstract  5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl acid 3 was synthesized from 1-aminonaphthalene. The yielded product 3 was investigated with X-ray crystallographic, NMR, MS and IR techniques. Compound 3, C₁₄H₁₁N₃O₂, Mr = 253.26, crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 10.068(2), b = 12.353(2), c = 20.102(4) ?, α = β = γ = 90.00o. V = 2,500.1(8) ?³, Z = 8, Dx = 1.346 Mgm⁻³. The final R was 0.0474. The molecular packing is stabilized by intermolecular O–H···N interactions.