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.      

[KCl<Subscript>3</Subscript>{H<Subscript>2</Subscript>dabco}]: A Unique 3-D Charge-Assisted Hydrogen-Bonded Hybrid Network of Anionic KCl<Subscript>3</Subscript> Chains and Organic Cations

Abstract  The 3-D hybrid network [KCl₃{H₂dabco}] resulted from the assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O. The compound crystallizes in the trigonal space group R-3c with a = b = 16.0437(2) Å, and c = 22.3094(2) Å. The structure consists in polymeric chains of anionic {KCl₃}²⁻ linked to {H₂dabco}²⁺ units by hydrogen bonds. Each organic cation establishes such charge-assisted H···Cl interactions with two inorganic arrays leading to a 3-D network. Index Abstract  Assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O resulted in a 3-D hybrid network of inorganic {KCl₃}²⁻ chains H-bonded to bridging organic cations.      

Supramolecular Aggregation in the 1:1 Co-crystal Formed Between Merocyanine Dye and 3-Nitrophenol,Characterized as a Hydrate

Abstract  The title organic salt comprises a (E)-4-[2-(4-hydroxyphenyl)vinyl]-1-methylpyridinium cation, a 3-nitro-phenoxide anion and a solvent water molecule of crystallisation. The anions and water molecules aggregate to form supramolecular chains facilitated by charge-assisted O–H···O hydrogen bonds and these form layers which are interspersed by layers of cations. Interactions between layers include O–H···O hydrogen bonding, as well as C–H···O and C–H···π contacts; π···π and C–H···O contacts are found within layers of cations. The compound crystallizes in the monoclinic space group P2₁/n with a = 15.018(7) ?, b = 7.328(2) ?, c = 17.571(7) ?, β = 112.342(15)°, and Z = 4. Index Abstract  A layer structure comprising alternating anions/water molecules and cations associated via charge-assisted O–H···O hydrogen bonding as well as C–H···O, C–H···π and π···π contacts is found in (II) .     

Synthesis and Crystal Structure of a Fe(III) Complex with an Isonicotinyl Hydrazone Ligand, [Fe(N-Isonicotinamidosalicylaldimine)Cl<Subscript>2</Subscript>]

Abstract  

A new complex [Fe(N-isonicotinamidosalicylaldimine)Cl₂] has been synthesized by template reaction at room temperature and structurally characterized by X-ray single-crystal analysis. The complex crystallizes in triclinic crystal system, Pī space group, a = 7.273(6) ?, b = 10.015(8) ?, c = 10.479(8) ?, α = 71.067(10)°, β = 89.964(11)°, γ = 75.528(10)°, V = 696.4(9) ?³ and Z = 2. The coordination geometry around the Fe(III) ion is a distorted trigonal bipyramid with a O₂N₁Cl₂ donor set. In the crystal structure, N–H···Cl, C–H···O and C–H···Cl hydrogen bonds and π···π stacking interactions involving aromatic and unclosed π-systems link the molecules to form supramolecular double layers.     

Inter- and Intra-Molecular Hydrogen Bonding in Bis(2-amino-5-fluoro-3-methylphenyl)disulfide

Abstract  Bis(2-amino-5-fluoro-3-methylphenyl)disulfide was obtained by oxidation of 2-amino-5-fluoro-3-methylbenzenethiol and was characterized by elemental analysis, IR and ¹H-NMR spectroscopy. The X-ray structure was determined. Crystal data: C₁₄H₁₄N₂F₂S₂: Monoclinic, P2₁ /n, a = 11.8268(3), b = 9.5770(3), c = 12.3977(3) ?, β = 98.079(2)°, V = 1390.29(7) ?, Z = 4. The supramolecular structure arises because the NH₂ groups form three center S···H···F hydrogen bonds and two center N–H···F and N–H···S hydrogen bonds. Index Abstract  Inter- and Intra-Molecular Hydrogen Bonding in Bis(2-amino-5-fluoro-3-methylphenyl)disulfide J. E. Drake¹, M. B. Hursthouse², M. E. Light², R. Maheshwari³, K.G. Ojha³, R. Ratnani^3* Bis(2-amino-5-fluoro-3-methylphenyl)disulfide is linked into a three-dimensional frame work by a combination of intermolecular N–H···F and N–H···N and intramolecular N–H···S hydrogen bonds. The supramolecular structure arises because the NH₂ groups form three center S···H···F hydrogen bonds and two center N–H···F and N–H···S hydrogen bonds.      

Synthesis and Crystal Structure of Heptyl 3-(3,4-dihydroxyphenyl)-2-propenoate

Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds. Index Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure is in E isomer and its packing is stabilized by hydrogen bonds.      

Synthesis and Structure of [Fe<Subscript>3</Subscript>O(O<Subscript>2</Subscript>CCH<Subscript>2</Subscript>OMe)<Subscript>6</Subscript>(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][FeCl<Subscript>4</Subscript>]

Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined. The three iron atoms and the μ₃-oxo are coplanar. Each carboxylic ligand is bidentate and links two iron atoms in the cluster. The clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration. The [FeCl₄]⁻ anion is intercalated between the hydrogen-bonded sheets. Crystal data: space group P2₁/n, a = 10.276(2), b = 22.793(5), c = 17.091(3) ?, β = 96.66(3)°, V = 3976(1) ?³, Z = 4, R = 0.0837, wR ₂ = 0.1836. Graphical Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined in which the clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration.      

Crystallographic and Conformational Analysis of [(<Emphasis Type="Italic">E</Emphasis>)-2-[(3-Chlorophenylimino)methy])-4-methoxyphenol]

Abstract  The crystal structure of C₁₄H₁₂ClNO₂ was determined by X-ray analysis. It crystallizes in the triclinic space group Pc with a = 12.5346(10) ?, b = 4.5101(3) ?, c = 12.0534(11) ?, α = 90.00o, β = 113.669(6)o, γ = 90.00o, Z = 2, Dx = 1.393 mg/m³, μ (MoK_α) = 0.298 mm⁻¹. The title compound is photochromic and molecule is non-planar. It adopts a phenol–imine tautomeric form with a strong intramolecular O–H···N hydrogen bond and a strong intermolecular C–H···O hydrogen bond. Minimum energy conformations AM1 were calculated as a function of the three torsion angles θ1(C10–C9–N1–C8), θ2(C9–N1–C8–C1) and θ3(N1–C8–C1–C6), varied every 10°. As in the X-ray experiment results, molecule has an angle that makes it non-planar between two aromatic rings in AM1 optimized geometry. Graphical Abstract  Molecular and crystal structure of [(E)-2-[(3-chlorophenylimino)methy])-4-methoxyphenol], C₁₄H₁₂ClNO₂, 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.      

The Synthesis and Structure of Two Novel <Emphasis Type="Italic">N</Emphasis>-(Benzothiazol-2-yl)benzamides

Abstract  Two novel benzothiazoles 2-chloro-N-(benzothiazol-2-yl)benzamide (1) and 2-chloro-N-(6-cyanobenzothiazol-2-yl)benzamide (2) were obtained in multistep synthesis. They were characterised by means of IR, ¹H- and ¹³C-NMR spectroscopy and also by single-crystal X-ray diffraction. The compound 1 crystallises with triclinic space group P , a = 9.5923(8) ?, b = 9.8583(8) ?, c = 13.8962(10) ?, α = 89.162(6)°, β = 77.741(7)°, γ = 80.064(7)°, V = 1264.5(2) ?³, Z = 4 and compound 2 crystallises as methanol solvate with monoclinic space group P 2₁/n, a = 7.5093(9) ?, b = 13.0211(14) ?, c = 16.032(2) ?, β = 92.717(10)°, V = 1565.9(3) ?³, Z = 4. Both crystal structures consist of discrete dimers connected into a three-dimensional network by intermolecular C–H···O and C–H···X (X = Cl or S) hydrogen bonds and by face-to-face π–π stacking interactions. Index Abstract  The synthesis and structure of two novel N-(benzothiazol-2-yl)benzamides. Irena Ćaleta, Dominik Cinčić, GraceKarminski-Zamola and Branko Kaitner. Hydrogen bonds and π–π interactions in N-(benzothiazol-2-yl)benzamides N-(benzothiazol-2-yl)benzamides.      

Synthesis and Structure of Ba<Subscript>5</Subscript>(V<Subscript>2</Subscript>O<Subscript>7</Subscript>)<Subscript>2</Subscript>Cl<Subscript>2</Subscript>

Abstract  A new barium chlorovanadate, Ba₅(V₂O₇)₂Cl₂, was isolated by a high-temperature (850 °C) reaction employing a CsCl/RbCl flux. The structure was determined by single crystal X-ray diffraction methods. This compound crystallizes in an orthorhombic crystal system, Pmmn (No. 59), with a = 11.558(2) ?, b = 15.164(3) ?, c = 10.023(2) ?, Z = 4 and V = 1756.7(6) ?³. The structure of Ba₅(V₂O₇)₂Cl₂ was determined by full-matrix, least-squares methods with R ₁ = 0.0398, wR ₂ = 0.1069 and GOF = 1.048 for all data. This new structure can be described as a composite lattice made up of mixed covalent and ionic moities. The extended framework is orchestrated by stacked [Ba(V₂O₇)Cl]³⁻ slabs that are interconnected by Ba²⁺ cations through Ba–O bonds to the [V₂O₇] units. The Ba²⁺ and Cl^- ions form BN-type “[BaCl]” sheets with pseudo-hexagonal windows that are centered by [V₂O₇]⁴⁻ pyrovanadate units. Graphical Abstract  The structure of a new chlorovanadate, Ba₅(V₂O₇)₂Cl₂, exhibits an interesting BN-type salt lattice that consists of an extended [BaCl] sheet containing pseudo-hexagonal windows that are centered by [V₂O₇] pyrovanadate units.      

Synthesis,Characterization and Crystal Structure of (<Emphasis Type="Italic">S</Emphasis>)-2-(2-Hydroxynaphthalen-6-yl)-<Emphasis Type="Italic">N</Emphasis>-((pyridin-4-yl)methyl) Propanamide

Abstract  

The synthesis, characterization and crystal structure of the title compound, (S)-2-(2-hydroxynaphthalen-6-yl)-N-((pyridin-4-yl)methyl) propanamide, is described. The salt is enantiomerically pure and crystallize in the orthorhombic P2₁2₁2₁ chiral space group with a = 7.9174(13) ?, b = 11.1583(18) ?, c = 11.2600(18) ?. Each molecule is linked to four neighboring molecules through the O–H···O and N–H···N hydrogen bonds into a supramolecular helical chain. The O–H···O and N–H···N hydrogen bonds lead to 24-membered open rings. Chains are further connected into layers via extensive interchain H···O and H···C short contacts.     

Synthesis and Structure of Bis(3-dimethylammonium-1-propyne)pentachlorobismuthate(III) (C<Subscript>5</Subscript>H<Subscript>10</Subscript>N)<Subscript>2</Subscript>BiCl<Subscript>5</Subscript>

Abstract  

The synthesis and crystal structure are given for the bis(3-dimethylammonium-1-propyne)pentachlorobismuthate(III) salt. An X-ray investigation has shown that the title compound crystallizes at 298 K in a centrosymmetric monoclinic system, space group C2/c with the following lattice parameters a = 12.6215(4) ?, b = 18.9228(5) ?, c = 8.3134(2) ?, β = 104.100(2)°, V = 1925.70(9) ?³. The structure was solved from 7,716 independent reflections with R ₁ = 0.0457 and wR ₂ = 0.0906, and refined with 85 parameters. The structure consists of disordered 3-dimethylammonium-1-propyne, C₅H₉NH⁺ cations and polynuclear anions in which slightly distorted (BiCl₅)²⁻ anions, sharing an apex are interconnected in chains. These chains are themselves interconnected by means of N–H···Cl originating from the C₅H₉NH⁺ entities, forming a three-dimensional network.     

Hydrogen Bonded Channel Formation in a Molecular Complex: <Emphasis Type="Italic">cis-</Emphasis>1-Chloro-2-ammonium-1-trimethylsilylcycloheptane Picrate

Abstract  The crystal and molecular structure of cis-1-chloro-2-amino-1-trimethylsilylcycloheptane picrate (cis-CATP) is determined and discussed along with its spectroscopy. The crystal structure of this compound (C₁₀H₂₃SiClN⁺ C₆H₂N₃O₇⁻) consists of ammonium cycloheptane cation and picrate anion stabilized by interionic N–H···O and C–H···O interactions leading to extended hydrogen bonded network structure. Apart from the less common syn addition of nitrosylchloride to 1-trimethylsilylcycloheptene ring, an interesting and unexpected reversal of regiochemistry of addition is revealed. Index Abstract  The preparation of cis-1-chloro-2-ammonium-1-trimethylsilylcycloheptane picrate is described and its crystal structure is determined and discussed.      

Synthesis and Crystal Structure of a Novel Double-Chain Coordination Polymer [Zn<Subscript>2</Subscript>(bipy)<Subscript>2</Subscript>(btec)(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>]<Subscript>n</Subscript> (bipy = 2,2′-bipyridine; btec = 1,2,4,5-benzenetetracarboxylate)

Abstract  A novel aromatic polycarboxylate polymer, [Zn₂(bipy)₂(btec)(H₂O)₂]_n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. Compound 1 belongs to the triclinic crystal system, space group P-1; a = 7.7449(6) ?, b = 8.9286(8) ?, c = 10.7422(8) ?, α = 80.95(1)°, β = 70.21(1)°, γ = 78.14(1)°, V = 680.93(10) ?³, Z = 2. The coordination geometry of Zn(II) atom is distorted trigonal bipyramidal with two nitrogen atoms of one 2,2′-bipy group, two oxygen atoms from two different btec ligands, and one water. The 16-membered rings are alternately arranged forming an infinite 1-D double-chain structure. A 3-D network was constructed by interlayer C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state. Graphical Abstract  A 1-D double-chain aromatic polycarboxylate polymer, [Zn₂(bipy)₂(btec)(H₂O)₂]_n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. A 3-D network was constructed by intermolecular C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.      

Desynchronization of Pedal Motion: Crystallographic and Theoretical Study of (<Emphasis Type="Italic">E</Emphasis>)-4-[(4-ethylphenyl)diazenyl]-2-methylphenol

Abstract  The single crystal X-ray diffraction analysis of the title compound, C₁₅H₁₆N₂O, reveals that its molecules exhibit whole-molecule disorder at both crystal lattice sites due to pedal motion in solid state. The compound crystallizes in the monoclinic space group P 2₁/c with a = 20.5504(14) ?, b = 10.8887(5) ?, c = 12.0191(8) ? and β = 96.927(5)°. While major pedal conformers of the compound in solid state are stabilized by intermolecular O–H···N type hydrogen bonds leading to the formation of C(7) chains at Site 1 and C(8) chains at Site 2 along [0 1 0] axis, C–H···π type intermolecular interactions between major and minor conformers also serve to stabilize minor pedal conformers. An interesting feature about the crystal structure is that pedal conformers at Site 1 have two different occupancy factors arising from desynchronization of pedal motion along [2 1 0] direction in crystal phase. Quantum chemical calculations at the B3LYP/6-31++G** level suggest that the desynchronization of pedal motions make more unstable pedal conformers at Site 1 than those at Site 2. Index Abstract  Molecular and crystal structure of (E)-4-[(4-ethylphenyl)diazenyl]-2-methylphenol, C₁₆H₁₈N₂O, indicate desynchronization of pedal motion and the quantum chemical calculations at level of B3LYP/6-31++G** suggest that desynchronization of pedal motions make more unstable pedal conformers.      

Synthesis and Crystal Structure of a Polymorph of the DMF Solvate of the Dicoppertetracarboxylate Paddlewheel Complex Cu<Subscript>2</Subscript>(p-aminobenzoate)<Subscript>4</Subscript>(DMF)<Subscript>2</Subscript>

Abstract  Reaction between p-aminobenzoic acid (HpABA) and Cu(NO₃)₂ · 2.5H₂O in basic MeOH/DMF affords green crystals of the dicopper paddlewheel complex, Cu₂(pABA)₄(DMF)₂ · 2DMF, 1, identified by single crystal X-ray crystallography: triclinic P-1, with a = 10.3728(2) ?, b = 10.617(2) ?, c = 11.128(2) ?, α = 81.705(3)°, β = 79.984(2)°, γ = 65.965(2)° and Z = 2. The crystal structure of 1 reveals that it is the second polymorph of Cu₂(pABA)₄(DMF)₂ · 2DMF and experiments on the stability of 1 indicate that it can be converted to Form I through desolvation followed by exposure to DMF. Graphical Abstract  Crystal structure of a polymorphic discrete dicoppertetracarboxylate is investigated for the conversion between the two forms influenced by hydrogen bonds.      

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.      

<Emphasis Type="Italic">Trans-</Emphasis>dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO<Subscript>2</Subscript>Cl<Subscript>2</Subscript>[OP(OPh)<Subscript>3</Subscript>]<Subscript>2</Subscript>

Abstract  The molecular structure of trans-dichlorodioxobis(triphenylphosphate) molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ has been determined. Crystal data: Monoclinic, Pn, a = 11.767(2), b = 10.341(2), c = 15.682(3) ?, β = 92.27(3)°, V = 1906.8(7) ?⁻³, Z = 2. Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI) was obtained by the reaction of molybdenum oxide, HCl and triphenylphosphate and was characterized by elemental analysis, IR, and ¹H-NMR spectroscopy. Index Abstract   Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ V. Huch¹, R. Kumar², S. Mathur¹, R. Ratnani² The immediate environment around Mo is distorted octahedral with two cis-oxygen atoms and two trans-chlorine atoms along with two triphenylphosphate moieties.      

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.      

Complementary Supramolecular Aggregation via O–H···O Hydrogen-bonding and Hg···S Interactions in Bis[N,N′-di(2-hydroxyethyl)-dithiocarbamato-S,S′]mercury(II): Hg[S2CN(CH2CH2OH)2]2

Abstract  The central mercury atom in Hg[S₂CN(CH₂CH₂OH)₂]₂ is asymmetrically chelated by two dithiocarbamate ligands leading to a distorted square planar geometry. Molecules aggregate into supramolecular chains via Hg···S interactions that are connected into a three dimensional array by extensive hydrogen bonding interactions. The compound crystallizes in the orthorhombic space group Pna2₁ with a = 13.8173(7) ?, b = 4.5307(1) ?, c = 26.0261(12) ?, and Z = 4. Index Abstract  Molecules associate into supramolecular chains via Hg···S interactions and these are connected into a three dimensional architecture by O–H···O hydrogen-bonding interactions.