Synthesis and Characterization of Monomeric and Dimeric Structures of Calix[4]arenes Containing Amidoferrocene

Abstract The reaction of 1,1′-bis(chlorocarbonyl)ferrocene with bis-aminobenzylcalix[4]arene gave amidoferrocene calix[4]arene monomer 1. Compound 1 crystallized in the monoclinic system P21/c with a = 11.196(6) ?, b = 14.971(11) ?, c = 32.007(2) ?, β = 96.413(4)° and V = 5330.9(6) ?³. X-ray diffraction analyses of 1 showed that the calix[4]arene scaffold was in cone conformation in which the intramolecular hydrogen bonding were formed through OH groups at the lower rim to stabilize the structure. Moreover, the intramolecular hydrogen bond between the amide groups of the amidoferrocene unit also presented in the crystal structure. On the other hand, the condensation of 1,1′-bis(chlorocarbonyl)ferrocene with p-tert-bis-aminobenzylcalix[4]arene resulted in the monomeric 2 and [2 + 2] dimeric compounds 3. ¹H-NMR studies signified that the calix[4]arene building block in compounds 2 and 3 adopted the cone conformation. Index Abstract Synthesis and Characterization of Monomeric and Dimeric Structures of Calix[4]arenes Containing Amidoferrocene Chomchai Suksai*, Pannee Leeladee, Colin Jennings, Thawatchai Tuntulani*, Palangpon Kongsaeree The condensation of 1,1′-bis(chlorocarbonyl)ferrocene with p-tert-bis-aminobenzylcalix[4]arene resulted in the monomeric and [2 + 2] dimeric compounds.      

Separation of (<Emphasis Type="Italic">S</Emphasis>)-(−)-3-Methyl-2-pyrrolidinone as an Inclusion Complex with (<Emphasis Type="Italic">R</Emphasis>)-(+)-4,4′,6,6′-Tetrachloro-2,2′-bis(hydroxydiphenylmethyl)-1,1′-biphenyl Host and its X-ray Structural Study

Abstract By inclusion complexation with the chiral host compound (R)-(+)-4,4′,6,6′-tetrachloro-2,2′-bis(hydroxydiphenylmethyl)-1,1′-biphenyl, racemic 3-methyl-2-pyrrolidinone was resolved and its (S)-(−)-enantiomer was isolated as a 1:1 inclusion complex, which crystallises in the orthorhombic crystal system in the space group P2₁2₁2₁ (a = 14.1163(2) ?, b = 14.7140(3) ?, c = 17.2025(3) ?). By the inclusion complexation, the keto–enol equilibrium of the guest was frozen and the keto-form was isolated in a pure form. By X-ray structural study of the complex, the guest molecule included was elucidated to be the keto-form and its absolute configuration was determined to be (S). Index Abstract By inclusion complexation with (R)-(+)-4,4′,6,6′-tetrachloro-2,2′-bis (hydroxydiphenylmethyl)-biphenyl, racemic 3-methyl-2-pyrrolidinone was resolved and its (S)-(−)-enantiomer isolated and in addition the keto–enol equilibrium of the guest was frozen and the keto-form isolated. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and Crystal Structure of Nitrogen-rich Compound: 2,5,2′-triazido-1,1′-azo-1,3,4-triazole

Abstract  The title compound 2,5,2′-triazido-1,1′-azo-1,3,4-triazole(2) has been synthesized by the reaction of 2,5,2′-trichloro-1,1′-azo-1,3,4-triazole(1) with sodium azide. Its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P−1 with a = 6.6604(13) ?, b = 6.7035(13) ?, c = 12.916 (3) ?, α = 98.13(3)°, β = 95.56(3)°, γ = 106.48° V = 541.68(18) ?³, Z = 2, C₄HN₁₇, Mr = 287.22, D _c  = 1.761 g cm⁻³, F(000) = 288 and μ(MoKa) = 0.140 mm⁻¹, the final R = 0.0553 and wR = 0.1541. X-ray analysis indicates a stronger delocalization of the azo π bond along the hypothetical N₄ moiety within the title compound than those in(E)-1,2-bis(2,6-diazido-9- azabicyclo[3.3.1]nonan-9-yl)diazene. Index abstract  The title compound 2,5,2′-triazido-1,1′-azo-1,3,4-triazole has been synthesized by the reaction of 2,5,2′-trichloro-1,1′-azo-1,3,4-triazole with sodium azide. Its crystal structure was determined by single-crystal X-ray diffraction. X-ray analysis indicates a stronger delocalization of the azo π bond along the hypothetical N4 moiety within the title compound than those in(E)-1,2-bis(2,6-diazido-9-azabicyclo[3.3.1] nonan-9-yl)diazene.      

Synthesis and Crystal Structure of New <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis[1-(4-methoxyphenyl)-5-methyl-1<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazole-4-carbonyl]hydrazide

Abstract  The N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide 6 was synthesized from aryl triazole acids and its structure is established by MS, IR, and ¹H NMR spectral data. Compound 6, C₂₂H₂₂N₈O₄, Mr = 462.48, crystallizes in the monoclinic space group P2(1)/c with unit cell parameters a = 15.3451(8), b = 8.6486(4), c = 16.8502(9) ?, α = 90.00, β = 95.731(2), γ = 90.00o, V = 2225.1(2) ?³, Z = 4, and Dx = 1.381 mg m⁻³. The final R was 0.0450. The four aromatic rings are close to linear because of N···H–N hydrogen bonds. Index Abstract  Synthesis and crystal structures of N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide Heng-Shan Dong, Yan-Fei, Wang, Hong-Ru Dong, Bin, Wang, Bin Quan N,N′-Bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide was synthesized.      

Synthesis and Crystal Structure of 4,6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde

Abstract The title compound, 3, 6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]- benzene-1,3-dicarbaldehyde was synthesized by Vilslmeier reaction from resveratrol (trans-3,4′,5-trihydroxystilbene). Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with crystallographic parameters: a = 7.2950(15) ?, b = 14.781(3) ?, c = 12.202(2) ?, β = 96.57(3)°, μ = 0.108 mm⁻¹, V = 1307.1(5) ?, Z = 4, Dx = 1.445 g/cm³, F(000) = 592, T = 293(2) K, 2.17°≤ θ ≤ 26.00°. The X-ray results demonstrated that the Vilslmeier reaction of resveratrol with DMF, POCl₃ and CH₃CN yielded 4,6-dhydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde. Graphical Abstract In this article, a resveratrol derivative was prepared and structurally characterized by single crystal X-ray diffraction.      

Synthesis and Structure of a New Coordination Polymer [Cd(pzdc)(bpy)]<Subscript>n</Subscript> (H<Subscript>2</Subscript>pzdc = Pyrazine-2,3-dicarboxylic Acid,bpy = 2,2′-Bipyridine)

Abstract A new 3D coordination polymer, [Cd(pzdc)(bpy)]_n (1) (pzdc = pyrazine-2,3-dicarboxylic acid, bpy = 2,2′-bipyridine), has been hydrothermally synthesized and characterized by the elemental analyses, IR spectrum and single crystal X-ray diffraction. X-ray diffraction analysis reveals that 1 (C₁₆H₁₀CdN₄O₄) crystallizes in monoclinic space group P2₁/c, features an interesting 3D zipper-like networks constructed by 2D layers via strong π–π packing interactions. Cell unit parameter for 1: a = 9.767(1), b = 14.022(2), c = 13.719(2) ?, β = 100.86(1)^o, and Z = 4. Graphical Abstract A new 3D coordination polymer, [Cd(pzdc)(bpy)]_n (pzdc = pyrazine-2,3-dicarboxylic acid, bpy = 2,2′-bipyridine), has been hydrothermally synthesized and characterized by the elemental analyses, IR spectrum and single crystal X-ray diffraction. X-ray diffraction analysis reveals that [Cd(pzdc)(bpy)]_n features an interesting 3D zipper-like networks constructed by 2D layers via strong π–π packing interactions.      

Synthesis,Crystal Structure and Bioactivities of <Emphasis Type="Italic">N</Emphasis>-(2,6-Difluorobenzoyl)-<Emphasis Type="Italic">N</Emphasis>′-[5-(Pyrid-4-yl)-1,3,4-Thiadiazol-2-yl]Urea

Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea, 3, has been synthesized by reaction of 2-amino-5-(pyrid-4-yl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate, and its structure was characterized with X-ray crystallographic, NMR, MS and IR techniques. It crystallizes in the triclinic space group P − 1, with a = 7.0821(9) ?, b = 9.4896(13) ?, c = 11.6594(15) ?, α = 82.311(2)°, β = 82.328(2)°, and γ = 87.641(2)°. In the title compound, the urea scaffold in each molecule is essentially planar due to the presence of intramolecular N–H···O hydrogen bond. The molecules are linked by intermolecular complementary N–H···O hydrogen bonds into centrosymmetric R ₂²(8) dimers. Intermolecular π–π stacking interactions are also present. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria. Index Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea has been synthesized and characterized with X-ray crystallographic, NMR, MS and IR techniques. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities.      

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.      

Synthesis, Crystal Structure of a New Co(II) Complex with Pyrazine-2,3,5,6-tetracarboxylic Acid

Abstract A new complex [Co(H₂pztc)(bpy)H₂O] (H₄pztc = pyrazine-2,3,5,6-tetracarboxylic acid, bpy = 2,2′-bipyridine) has been synthesized by hydrothermal reactions of Co(NO₃)₂ · 6H₂O with H₄pztc and bpy and characterized by IR and X-ray diffraction single crystal structure analysis. It belongs to monoclinic system, P2₁/c space group with a = 13.454(2) ?, b = 12.939(2) ?, c = 11.4993(19) ?, α = 90°, β = 111.640(3)°, γ = 90°. This complex is assembled into 3D supramolecular architecture by hydrogen bonds (O–H···O, C–H···O). Index Abstract A new complex of cobalt(II) with pyrazine-2,3,5,6-tetracarboxylic acid and 2,2′-bipyridine is assembled by intermolecular hydrogen bonds forming 2D layer and 3D supramolecular network.      

Synthesis of 7,4′-Bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone and Crystal Structure of its Ester

Abstract 7,4′-bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone (I) and its ester were synthesized and examined by IR, element analysis and ¹H NMR. The crystal of 7,4′-bis-(acetyl oxide)-8,3′,5′-tris-(acetoxymethyl)isoflavone (II) was studied by X-ray diffraction. (II) crystallizes in the monoclinic with space group P2 ₁ /c. a = 17.987(3) ?, b = 17.972(3) ?, c = 8.4087(11) ?, β = 97.703(3)°, V = 2693.7(6) ?³ and Z = 4. The molecular structure of the ester consists of a benzopyranone moiety, a phenyl moiety, two acetyl oxides and three acetoxymethyl groups. Hydrogen bonds and aromatic stacking interactions link the ester into a two-dimensional structure. Index Abstract 7,4′-bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone and its ester were synthesized and examined by IR, element analysis and ¹H NMR. The result of the ester’s crystal structure showed that hydrogen bonding and aromatic π–π stacking assemble the ester into a two-dimensional networking structure.      

Synthesis and Crystal Structure a Two-Dimensional Coordination Polymer: [Cd( μ -N3)( μ -HL)(H2O)]n [HL?=?Monodeprotonated 2,2′-bypyridine-3,3′-diol]

Abstract  Hydrated cadmium perchlorate reacted with sodium azide and 2,2′-bypyridine-3,3′-diol (H₂L) in ethanol solution and resulted in the formation of a two-dimensional coordination polymer: [Cd(μ-N₃)(μ-HL)(H₂O)]_n. The complex has been characterized by elemental analysis and IR spectrum, and its crystal structure determined by X-ray crystallography and the complex crystallizes in the monoclinic system with space group P2₁/c and a = 7.2849(14), b = 9.9568(19), c = 17.058(3) Ǻ, β = 102.254(2)°. In the complex both azide anion and monodepronated 2,2′-bypyridine-3,3′-diol anion (HL) act as bridge ligands and led to the formation of a two-dimensional sheet structure on (100) plane, and the O–H⋯N hydrogen bond made the sheets pile up along [100] direction, which forms a supramolecular three-dimensional structure. Graphical Abstract  The title two-dimensional Cd(II) coordination polymer was synthesized by cadmium perchlorate, sodium azide and 2,2′-bypyridine-3,3′-diol and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the two-dimensional coordination polymer was fabricated with azide anion and monodeprotonated 2,2′-bypyridine-3,3′-diol as mixed bridge ligands.      

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.     

Two Isostructural Complexes Constructed from Mixed Ligands of Dipyrido[3,2-d:2′,3′-f]quinoxaline and Phthalate with Novel Oxygen Clusters

Abstract Two isostructural dinuclear complexes [M₂(Dpq)₂(phth)₂(H₂O)₄] · 2H₂O [M = Zn(1), Ni(2), Dpq = dipyrido[3,2-d:2′,3′-f]quinoxaline, phth = phthalate] have been synthesized and characterized. Crystal data: (1), Mr = 1031.55, monoclinic, C2/c, a = 27.7948(11), b = 10.5196(4), c = 15.0390(5) ?, β = 110.818(1), Z = 4, V = 4110.2 ?³, R ₁ = 0.0277, wR ₂ = 0.0718 [I > 2σ(I)]; (2), Mr = 1018.19, monoclinic, C2/c, a = 27.675(4), b = 10.3601(15), c = 15.082(2) ?, β = 110.954(2), Z = 4, V = 4038.3 ?³, R ₁ = 0.0248, wR ₂ = 0.0668 [I > 2σ(I)]. The dinuclear units are connected into 2-D supramolecular net through O–H···O hydrogen bonding. Moreover, the 2-D networks are ultimately packed into a 3-D supramolecular structure via interlayer π···π stacking interaction between the aromatic rings of Dpq ligands. Furthermore, the photoluminescence property of compound 1 is also studied. Graphical Abstract Two isostructural dinuclear complexes [M₂(Dpq)₂(phth)₂(H₂O)₄] · 2H₂O [M = Zn(1), Ni(2), Dpq = dipyrido[3,2-d:2′,3′-f]quinoxaline, phth = phthalate] have been synthesized, and the structure study reveals that each dinuclear complex is connected with six other dinuclear units through the O–H···O hydrogen bonding to form 2-D supramolecular networks.      

Intermolecular Hydrogen Bonds and the Supramolecular Structure of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(<Emphasis Type="Italic">p</Emphasis>-tolylsulfonyl)diethylenetriamine

Abstract  The title compound N,N′-bis(p-tolylsulfonyl)diethylenetriamine (1) was synthesized and its crystal structure determined by X-ray diffraction. Adjacent molecules of 1, symmetrically related through a c-glide, are linked by alternating hydrogen bonds that form molecular chains along [0 0 1]. Two molecular chains occur in each unit cell and pack to form alternating layers in a three-dimensional supramolecular structure. The compound crystallizes in the Pca2₁ space group stabilized by the inclusion of solvent dichloromethane molecules in structural voids between molecules of 1. The dichloromethane molecules are related through a twofold screw rotation axis and are not disordered. Index Abstract  Intermolecular hydrogen bonds involving sulfonamide moieties of title compound afford a supramoleular structure that accommodates the inclusion of dichloromethane in alternating layers.      

Crystal and Molecular Structure of 6,6′-Dimethoxy-gossypol:Acetic acid (1:1)

Abstract By crystallization from dilute solutions of acetic acid (2–4%) in diethyl ether, acetone, or methyl ethyl ketone, 6,6′-dimethoxy-gossypol forms a solvate with acetic acid in a one-to-one molar ratio. The compound crystallizes in the triclinic P space group and has unit cell dimensions of a = 7.5793(10) ?, b = 14.7211(19) ? and c = 14.740(2) ?, α = 106.260(3)°, β = 102.310(3)°, γ = 95.975(3)°, Z = 2. The structure was solved by direct methods and refined to an R1 value of 0.0394 on 4252 observed reflections. Enantiomeric pairs of dimethoxy-gossypol molecules form centrosymmetic dimers that are characterized by a pair of intermolecular hydrogen bonds and by hydrophobic stacking between pairs of naphthalene rings. The acetic acid molecule accepts a hydrogen bond from a gossypol hydroxyl group and donates to a hydrogen bond with one of the aldehyde groups of an adjacent gossypol molecule. Although there is less hydrogen bonding in this structure than in the gossypol:acetic acid (1:1) structure, the molecular packing of the two compounds is similar. Graphical abstract Crystal and molecular structure of 6,6′-dimethoxy-gossypol:acetic acid (1:1) Michael K. Dowd and Edwin D. Stevens The molecular structure of the acetic acid solvate of 6,6′-dimethoxy-gossypol is presented.      

Crystal and Molecular Structures of Tris(1-Methylimidazol-2-yl)Phosphine,Tris(4-Methylthiazol-2-yl)Phosphine and its Sulfide

Abstract  Two crystal structures of tris(azolyl)phosphines, PR₃ [R′ = 1-methylimidazol-2-yl (1) or R′′ = 4-methylthiazol-2-yl (2)], and the crystal structure of the sulfurisation product of 2, R′′₃PS (3), were determined. All compounds crystallise in polar space groups, 1 in the orthorhombic space group Pna2₁ with cell parameters a = 13.9779(15) ?, b = 9.2492(10) ? and c = 10.2439(11) ?; 2 in the trigonal space group, R3c, with a = 15.2383(10) ? and c = 10.5882(13) ? and 3 in the orthorhombic space group, Cmc2₁, with a = 13.466(3) ?, b = 9.308(2) ? and c = 12.207(3) ?. Graphical Abstract  This article presents two crystal structures of tris(azolyl)phosphines and one of a tris(thiazolyl)phosphine sulfide, a compound which show potential for wide application in coordination chemistry due to their multidentate nature.      

Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium Perchlorate Dihydrate

Abstract The crystal structure of 4,4′-bipyridin-1-ium perchlorate dihydrate, [C₁₀H₉N₂](ClO₄) · 2H₂O, is determined by room temperature X-ray diffraction. The compound crystallizes in the triclinic space group P-1 with a = 8.122(3) ?, b = 9.726(3) ?, c = 17.648(6) ?, α = 78.181(4)°, β = 82.797(5)°, γ = 67.439(4)°, Z = 2, V = 1258.4(7) ?³. In the compound, monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds in a head-to-tail fashion. The chains are stacked via π–π stacking interactions to create two-dimensional sheets. The interlayer space is occupied by the hydrogen-bonded water chains that are linked to the organic sheets via C–H···O interactions and the perchlorate anions that are linked to the water chains and the organic sheets via O–H···O and C–H···O hydrogen bonds, respectively, thus generating a three-dimensional supramolecular architecture. Index Abstract Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium perchlorate dihydrate Jian-Yong Zhang, Ai-Ling Cheng and En-Qing Gao* Monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds, and these chains are stacked via π–π stacking and hydrogen bond interactions involving water molecules and perchlorate anions.      

Hydrogen-bonded Multicomponent Behavior in Tetra-<Emphasis Type="Italic">iso</Emphasis>-butyl-resorcin[4]arene–1,4-Bis(pyridyl)ethane–Methanol–Water (1/2/0.5/1)

Abstract  Co-crystallization of the tetra-iso-butyl-resorcin[4]arene (1) with 1,4-bis-(pyridyl)ethane (bpe) obtained from methanol yields a molecular solid of the multicomponent host–guest complex 1 · 2(bpe) · 0.5MeOH · H₂O (2) in which 1 assemblies with water molecules to form a hydrogen-bonded dimer. The bpe ligands in both cis- and trans-stereo configurations exist in the complex 2, of which trans-bpe moieties as guests are encapsulated in the capsules constructed by two pairs of opposition bowls of resorcinarenes. Graphical Abstract  The 1,4-bis(pyridyl)ethane (bpe) ligands in both cis- and trans-stereo configurations exist in a multicomponent molecular solid, of which trans-bpe moieties as guests are encapsulated in the capsules constructed by two pairs of opposition bowls of resorcinarenes.      

Crystal Structure of Antitubercular Complex: <Emphasis Type="Italic">cis</Emphasis>-(chloro)-[<Emphasis Type="Italic">N,N</Emphasis>′-<Emphasis Type="Italic">bis</Emphasis>-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) Monohydrate

Abstract  Diethyl-2,2′-bipyridine-3,3′-dicarboxylate (3 or L) reacts with RuCl₃ · 3H₂O to give cis-(Cl)-[Ru(L)₂Cl₂] · H₂O (4) and structure of the complex was determined by spectral (IR, ¹H-NMR), and mass spectroscopic data, elemental analyses and X-ray crystallography. The structure is solved in triclinic, space group p-1 with a = 10.658 (2), b = 12.446 (3), c = 14.186 (5) ?, α = 104.856 (3), β = 108.704 (3), γ = 94.973 (2)°, V = 1693.2 (8) ?³, Z = 2 with final R = 0.012. The geometry of the complex is shown to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes with Ru–N distance as 2.021 (2)−2.071 (3) ?. The cis-position is occupied by two chloride atoms with Ru–Cl distance as 2.4156 (12) and 2.4167 (13) ?. The trans-axial Cl2–Ru1–N and Cl1–Ru1–N4 angles are respectively, 172.42 (7) and 174.12 (7)°. A weak hydrogen bonding is observed between the two chlorides and hydrogens of neighbouring molecule [C–H···Cl distance as 2.72, 2.77 (4) ?]. A second type of weak hydrogen bonding is also observed between the oxygens of carboxylate groups and hydrogens of a neighbouring molecule [C–H···O distance as 2.53, 2.56 and 2.34 (4) ?]. Graphical Abstract  The structure of anti-tubercular precursor complexes, cis-(chloro)-[N,N′-bis-(diethyl-2,2′-bipyridine-3,3′-dicarboxylate)]ruthenium(II) monohydrate is solved by single crystal X-ray diffraction analysis which reveals geometry of the complex to be a distorted octahedral with four nitrogens of two 2,2′-bipyridyl ligands in two different planes. The cis-position is occupied by two chloride atoms.      

Solid State Structure of 6,7-Dihydro-1,4-Di(2′-Pyridyl)-5<Emphasis Type="Italic">H</Emphasis>-Cyclopenta[d]Pyridazine

Abstract  The X-ray structure of 6,7-dihydro-1,4-di(2′-pyridyl)-5H-cyclopenta[d]pyridazine ligand (5-dppn) shows the existence of a trans/trans conformation. The 5-dppn crystallizes in a triclinic space group P-1 with a = 7.1048(15) ?; b = 9.008(2) ?; c = 10.986(3) ?; α = 88.279(16)°; β = 85.454(15)°; γ = 69.104(12)°; V = 654.7(3) ?³ and Z = 2. The analysis of 5-dppn crystal structure demonstrates the presence of edge-edge Ar–H···N and face-face Aliph-H···N centrosymmetric dimer interactions. The unit cell packing arrangement confirmed the presence of two molecules opposite to each other. Index Abstract  The X-ray structure of 6,7-dihydro-1,4-di(2′-pyridyl)-5H-cyclopenta[d]pyridazine ligand (5-dppn) shows the existence of a trans/trans conformation.