Dinuclear Complexes and a One-dimensional Chain Involving Difunctional Ligands Containing the Acetylacetonate Functionality

Abstract Systems containing two acetylacetonate (acac) ligands separated by an aromatic spacer (1–3) react with Cu(II) in the presence of bidentate nitrogen ligands to form crystalline, capped, dinuclear (zero-dimensional) structures (6–8). Noncovalent interactions between stacked aromatic ligands on adjacent molecules in 7 and 8 produce one-dimensional chains in the crystal. Molecules 1–3 fail to produce crystalline, one-dimensional chains with covalent metal-organic bonding on reaction with Cu(II) alone. System 5, which contains a single acac ligand and a pyridyl nitrogen, forms a crystalline, one-dimensional chain on reaction with Cu(II) in the presence of a bidentate nitrogen ligand (9). The covalent bonding ribbon of the chain passes from acac to Cu(II) to the pyridyl nitrogen and back to acac. The phenanthroline ligands in 9 provide noncovalent bonding with adjacent chains in the crystal to produce a two-dimensional layered structure. Graphical abstract Dinuclear Complexes and a One-dimensional Chain Involving Difunctional Ligands Containing the Acetylacetonate Functionality Joseph B. Lambert and Zhongqiang Liu Two acetylacetonate ligands separated by an aromatic spacer react with Cu(II) in the presence of bidentate nitrogen ligands to form crystalline, capped, dinuclear (zero-dimensional) structures, whereas acetylacetonate linked to pyridine forms a crystalline, one-dimensional chain on reaction with Cu(II) with phenanthroline ligands on adjacent chains noncovalently bonded to form a two-dimensional layered structure in the crystal. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Inclusion Compounds of the Host 9-(4-Methylphenyl)-9<Emphasis Type="Italic">H</Emphasis>-xanthen-9-ol with a Series of Organic Guests

Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). For those guest molecules possessing electron acceptor atoms/functionalities hydrogen bonding with the host is the prominent mode of interaction and presents itself in the form of (Host)–OH···O(Guest) linkages. The cyclohexane and benzene guests however, occupy voids created by neighbouring host molecules which form hydrogen bonded dimers of the form (Host)–OH···O(Host). The structures of the inclusion compounds were investigated and their thermal stabilities determined. Selectivity experiments were also conducted. Graphical Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). Crystal structures and thermal stabilities were determined. The host selectivity was also investigated.      

Crystal and Molecular Structures of Benzyl-(2-chloro-6-methylpyrimidin-4-yl)amine and Benzyl-(4-chloro-6-methylpyrimidin-2-yl)amine: Confirmation of Computationally Predicted Restricted Rotation

Abstract Crystal structures for the isomeric compounds benzyl-(2-chloro-6-methylpyrimidin-4-yl)amine (1), as its hemi-hydrate, and benzyl-(4-chloro-6-methylpyrimidin-2-yl)amine (2) have been determined. Conformational differences lead to multiple molecules, i.e. two and three, in their respective structures. Layers feature in each of the crystal structures and are stabilized by substantial hydrogen-bonding interactions. Compound (1) crystallizes as a hemi-hydrate in the triclinic space group P-1 with a = 8.667(5) ?, b = 11.421(7) ?, c = 12.954(8) ?, α = 78.330(10)°, β = 84.553(10)°, γ = 75.510(9)°, and Z = 4. Compound (2) crystallizes in the monoclinic space group P2₁/c with a = 10.740(3) ?, b = 21.487(6) ?, c = 14.914(4) ?, β = 95.014(5)°, and Z = 12. Index Abstract Substantial hydrogen-bonding interactions leading to layer structures feature in each of the crystal structures of the isomeric title compounds. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

Synthesis and Crystal Structure of 2,13-Bis(acetamido)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0<Superscript>1.18</Superscript>,0<Superscript>7.12</Superscript>]docosane Tetrachlorocobalt(II)dihydrate

Abstract The novel ionic compound [H₂bdtd][CoCl₄] · 2H₂O (1) was prepared by the reaction between CoCl₂ and 2,13-bis(acetamido)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12]docosane (bdtd) in adjusted to pH 3.0 by 1.0 M HCl and structurally characterized. The crystals are monoclinic C2/c with a = 18.7777(9), b = 9.7356(4), c = 20.0884(9) ?, β = 109.6340(10)°, V = 3458.9(3) ?³, Z = 4. The dication H₂bdtd occupies a special position about an inversion center. The cobalt(II) atom in the anion is in a distorted tetrahedral environment with four chloride ligands. The crystal structure is stabilized by a variety of hydrogen-bonding contacts involving the dication, chloride anions and solvent water molecules. Cyclic voltammetry of [CoCl₄]²⁻ anion in 1 undergoes irreversible one-electron reduction to the Co^II/Co^I. Graphical abstract The crystal structure of the ionic compound [H₂bdtd][CoCl₄] · 2H₂O (1) consists of [H₂bdtd]²⁺ cation, [CoCl₄]²⁻ anion and water molecules joined together by ionic interaction and hydrogen bonds. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

The Crystal and Molecular Structure of a Polymorph and a Pseudo-Polymorph of Droperidol

Abstract Crystals of two crystal modifications of droperidol: a hemihydrate (1) and the z polymorph (2), have been isolated and their structure determined using X-ray diffraction methods. Droperidol hemihydrate crystallized in the triclinic space group P − 1, with unit cell parameters a = 6.2842(15), b = 10.1473(8), c = 16.1850(2) ?; α = 102.554(9); β = 91.917(14); γ = 99.316(12)°; V = 991.6(3) ?³, and Z = 2. The droperidol z polymorph crystallized in the monoclinic space group P2₁/c, with unit cell parameters a = 20.0406(8), b = 7.4955(4), c = 12.9733(5) ?; β = 98.089(2)°; V = 1929.39(15) ?³, and Z = 4. In 1 and 2 two molecules of droperidol are joined by two N–H···O hydrogen bonds. The structure of 1 shows a possible additional hydrogen bond linking the two droperidol molecules via the water molecule. Graphical Abstract The crystal and molecular structure of a polymorph and a pseudo-polymorph of droperidol A. Actins, R. Arajs, S. Belakovs, L. Orola, and M. V. Veidis Crystals of two crystal modifications of droperidol: a hemihydrate and the z polymorph have been isolated and their structure determined using single crystal X-ray diffraction methods. 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 1-Phenyl-3-methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5

Abstract A new compound 1-phenyl-3-methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5 (PMPeP-SHZ) has been synthesized and characterized by elemental analysis, IR spectrum, MS and single crystal X-ray diffraction. The compound crystallizes in a monoclinic, space group P2(1)/c with cell parameters: a = 10.8275(19) ?, b = 24.689(4) ?, c = 9.7167(16) ? and β = 95.127(4)°, Z = 4, S = 1.097. In the crystal structure, the compound presents in the diketo form. The structure exhibits both intra- and intermolecular hydrogen bonding and the molecules are interlinked through hydrogen bonds forming an infinite 2D network. The fluorescent result shows blue emission at room temperature in solid state. Graphical Abstract Synthesis, Characterization and Crystal Structure of 1-Phenyl-3- methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5 Li Zhang, Guan-Cheng Xu, Lang Liu, Guang-Fei Liu, and Dian-Zeng Jia* Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and Structure of Di-μ-oxo-bistripyrazolylborato Dioxo Vanadium (V) Complex with Lattice of Diacetonitrile

Abstract A novel oxovanadium complex was obtained by the reaction of VOSO₄ · 3H₂O with tripyrazolylborate sodium in MeOH. The complex (1) was characterized by element analysis, IR spectroscopy, ¹HNMR and its crystal for X-ray diffraction recrystallized from saturated CH₃CN solution. The compound crystallizes in the monoclinic, space group Pbca, with cell dimensions of a = 15.531(2) ?; b = 18.007(2) ?; c = 10.725(2) ?; V = 2,999.4(8) ?³ and D _calc = 1.533 g/cm³ for Z = 4. The structure was solved by direct methods and refined to an R-value of 0.0401. Structure analysis show that it is a di-μ-oxo-bistripyrazolylborato dioxo vanadium (V) complex with lattice of diacetonitrile. In addition, the electronic structure and the bonding characters of the complex were analyzed with ab initio calculations. Index Abstract Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and crystal structure of a copper coordination polymer [(Cu(btapo)2BrCH3OH)+Br−]n (btapo=1,3-bis(benzotriazol-1-yl) propan-2-ol)

A new coordination polymer [(Cu(btapo)₂BrCH₃OH)⁺Br⁻]_n (btapo = 1,3-bis(benzotria- zol-1-yl) propan-2-ol) was synthesized by the reaction of CuBr₂ and btapo, a new ligand synthesized in our laboratory, in THF. Its structure was determined by single-crystal X-ray crystallography. It crystallizes in tetragonal I4(1)/a space group with the crystal cell parameters of a=11.987(9) ?, c=54.24(4) ?, V=7794(10) ?³, and Z=8. The crystal X-ray analysis shows that each copper atom is five-coordinated with a bromine atom and four nitrogen atoms from four ligands to form a slightly distorted square pyramid. Each ligand bridges two copper atoms to form a two-strand helical chain. The chains are further extended to a three-dimensional network by the hydrogen bonds between the hydroxyl groups and the bromine anions. Supplementary material Crystallographic data for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Center as supplementary publication no. CCDC 600471. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (Fax;(+44) 1223–336-033; e-mail: deposit@ccdc.cam.ac.uk).     

Synthesis,Spectroscopy, In Vitro Biological Activity and X-ray Structure of (4-Methylpiperidine-dithiocarbamato-<Emphasis Type="Italic">S</Emphasis>,<Emphasis Type="Italic">S</Emphasis>′)triphenyltin(IV)

Abstract (4-Methylpiperidine-dithiocarbamato-S,S′)triphenyltin(IV) derivative of 4-methyl-1-piperidine carbodithioic acid (4-MePCDTA) have been synthesized and characterized by elemental, IR, multinuclear NMR (¹H and ¹³C) and mass spectrometric studies. The crystal structure of the complex has been determined by X-ray single crystal analysis, which shows unsymmetrical nature of the ligand towards coordination to tin. It crystallizes in monoclinic P21/c space group with the crystal cell parameters: a = 10.1863(10) ?, b = 21.200(2) ?, c = 11.7332(11) ?, β = 111.2020(10)°, Z = 4 and V = 2,362.2(4) ?³. The tin atom is coordinated to the two sulfur atoms of the dithiocarbamate ligand and three carbon atoms of the phenyl groups are in distorted trigonal bipyramid geometry. This complex was tested for its antimicrobial activity against six different plant and human pathogens. The screening results show that the complex exhibit higher antibacterial and antifungal activity than the free ligand. Index abstract Synthesis, Spectroscopy, in vitro Biological Activity and X-Ray Structure of (4-Methylpiperidine-dithiocarbamato-S,S′)triphenyltin(IV) Saira Shahzadi, Saqib Ali and Mohammmed Fettouhi 4-Methyl-1-piperidine carbodithioic acid behaves as anisobidentate ligand and chelates the tin atom by means of sulfur atoms giving cis-trigonal bipyramid geometry around the tin atom. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

The crystal and molecular structures of rac-threo-ifenprodil and two other 4-benzylpiperidinyl derivatives

The crystal structures of threo-ifenprodil [threo-2-(4-benzyl-piperidin-1-yl)-1-(4-hydroxyphenyl)-propan-1-ol] (1), potent NMDA receptor antagonist, and two related, biologically active compounds: threo-2-(4-benzyl-piperidin-1-yl)-1-(4-fluorophenyl)-propan-1-ol (2) and 4-benzyl-1-phenethyl-piperidinium chloride (3) have been determined by X-ray structure analysis of single crystals. Compound 1 crystallizes in an orthorhombic system, with a space group Pna2₁ (a = 34.843(3) Å, b = 6.0261(13) Å, c = 8.9343(9) Å), compound 2 – in a monoclinic space group P2₁/c (a = 14.194(1) Å, b = 6.2831(6) Å, c = 20.948(1) Å, = 101.762(6)), and compound 3 – in an orthorhombic space group Pbca (a = 10.4627(8) Å, b = 11.2166(6) Å, c = 31.669(2) Å). The piperidine rings are close to ideal chair conformations, the substituents are in equatorial positions. Overall shapes of the molecules, defined by the dihedral angles between the terminal aromatic rings, are very similar in all three cases. In 1 and 3 the crystal packing is mainly determined by the hydrogen bonds, while in case of 2 – by weak van der Waals interactions. The molecules of 1 and 3 are disordered, and the disorder is caused by a rotation around the N–C bond.     

Synthesis,Crystal Structure,and Properties of Two Zinc Tubular Coordination Polymers Based on Fluconazole

Two Zn(II)-containing complexes based on fluconazole, {[Zn(HFlu)₂(IPA)]·9H₂O}_n (1), {[Zn(HFlu)₂(OH-BDC)]·8H₂O}_n (2) (HFlu = fluconazole; 2-(2,4-difluoro- phenyl)-1,3-bis(1,2,4-triazol-1-yl)-propan-2-ol; H₂IPA = isophthalic acid; OH-H₂BDC = 5-hydroxyisophthalic acid) have been synthesized and structurally characterized. Complex 1 and 2 are both a one-dimensional (1D) tubular structure with the distorted dinuclear zinc rectangular-shaped cavity, and large free water molecules involved in strong O?H···O and O?H···N hydrogen bonds are accommodated in the 1D tubular structure. The thermal stabilities and photoluminescent properties of the coordination polymers have also been investigated.     

Dimer Formation in 4-Benzyl-5-Methoxymethyl-3-Methyl-1<Emphasis Type="Italic">H</Emphasis>-Pyrrole-2-Carboxylic Acid Benzyl Ester

Abstract A new substituted pyrrole, a precursor of meso-free-porphyrins, has been synthesised and characterised by single-crystal X-ray diffraction: monoclinic, P2₁/c with a = 14.607(9) ?, b = 5.136(2) ?, c = 25.832(17) ?, β = 108.14(5)°, Mr = 349.41, V = 1841.6(18) ?³, Z = 4. The molecules are assembled in centrosymmetric dimers via strong N–H...O hydrogen bonds. The dimers are gathered into chains via C–H...π intermolecular interactions. Graphical abstract The molecules in 4-benzyl-5-methoxymethyl-3-methyl-1H-pyrrole-2-carboxylic acid benzyl ester are joined in dimmers by strong hydrogen bonds. The dimmers are aggregated in chains running along the b axis through C-H...?€ intermoleculear interactions. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal and Molecular Structure of <Emphasis Type="Italic">trans</Emphasis>-1,2-bis(2-benzothiazolyl)ethene

Abstract The crystal and molecular structure of trans-1,2-bis(2-benzothiazolyl)ethene is reported. Crystal data for 1: monoclinic, space group C 2/c, a = 24.926(3) ?, b = 4.843(1) ?, c = 11.164(1) ?, β = 105.274(5) °, V = 1300.0(3) ?³, and D _c = 1.50 g/cm³ for Z = 4 and R = 0.028. The molecule crystallizes in the form of a colorless plate and forms one-dimensional slipped π-stacks. Graphical Abstract The title compound crystallizes to form 1D slipped π-stacks in the solid state. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal and Molecular Structures of C6H5CH2SOCH2CONHCH2C6H5 and C6H5SOCH2CON(iC3H7)2

Abstract  The crystal structures for two of the ligands C₆H₅CH₂SOCH₂CONHCH₂C₆H₅ (1) and C₆H₅SOCH₂CON(ⁱC₃H₇)₂ (2) have been determined by X-ray diffraction. These compounds crystallize in orthorhombic system with space groups and cell parameters, Pca21(no. 29), a = 8.4600(5) ?, b = 5.3534(5) ?, c = 32.136(2) ?, V = 1455.42(15) ?³ and Pna21(no. 33) a = 17.5563(11) ?, b = 5.7902(4) ?, c = 14.2866(9) ?, V = 1452.30(16) ?³, respectively. These molecules are stabilized in solid state by various intra and intermolecular hydrogen bonding interactions to give polymeric structures. The reported IR spectra of these compounds in solid state could be explained on the basis of the observed intermolecular hydrogen bonding interactions. Index Abstract  The title compounds C₆H₅CH₂SOCH₂CONHCH₂C₆H₅ (1) and C₆H₅SOCH₂CON(ⁱC₃H₇)₂ (2) were prepared by the oxidation of corresponding sulfides with H₂O₂/SeO₂ in methanol and their structures were determined. The structures show that the SO and CO groups are having “anti” configuration in 1 and “syn” configuration in 2. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

3D Solid-State Network from Hierarchical Supramolecular Self-Assembly of Transition Metal Complexes of Pyridine Based Ligand

Abstract  The crystal structures of [Cu(py)₄(ClO₄)](ClO₄) (1), [V(pic)₂(OH)](NO₃)₂ · H₂O (2) and [Ni(H₂O)₆][Ni(dpa)₂] · 2H₂O (3) [py = Pyridine, picH = Pyridine-2-carboxylic acid, dpaH₂ = Pyridine-2,6-dicarboxylic acid] was determined by single-crystal X-ray diffraction techniques. Solid-state structural analysis shows that all these complexes from extensive 3D network structure via supramolecular self-assembly. The crystal structures are stabilized by extended hydrogen bonding interactions. The complex 2 forms orange V₂O₅ micro spheroids when heated at ~400 °C for 6 h. Graphical Abstract  Hierarchical supramolecular self-assembly of transition metal complexes of pyridine based ligands in crystal. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis,Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl<Subscript>2</Subscript> · 3.5H<Subscript>2</Subscript>O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane)

Abstract The reaction of the potentially tetradentate ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl₂(CH₃CN)₂] yields a mixture of complexes, where the ligand acts as bidentate SS, or tetradentate 2NS or NSSN. This mixture of complexes SS, 2NS, and NSSN was crystallized with dichloromethane/n-pentane (1:1) and crystals of [Pt(bddn)]Cl₂ (isomer NSSN) were obtained. The complex has been characterized by elemental analyses, mass spectrometry, conductivity, IR, ¹H, ¹³C{¹H}, ¹H{¹⁹⁵Pt}, ¹⁹⁵Pt{¹H}NMR, HSQC and NOESY spectroscopies, and X-ray diffraction. Compound [PtCl₂(bddn)] · 3.5H₂O crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 15.430(7) ?, b = 17.405(4) ?, c = 18.887(7) ?, β = 91.24(2)°, V = 5071(3) ?³, Z = 4, R ₁ = 0.0354, wR₂ = 0.1034. This compound consist of discrete cations [Pt(bddn)]²⁺, Cl⁻ anions and water molecules of crystallization. The platinum(II) is tetracoordinated by two azine nitrogen atoms and two sulfur atoms of the thioether-pyrazole ligand, in a distorted square planar geometry. Graphical Abstract Synthesis, Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl ₂ · 3.5H ₂ O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane) Antonio de Leon, Josefina Pons*, Jordi García-Antón, Xavier Solans, Mercè Font-Bardia, Josep Ros* Reaction of the ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl₂(CH₃CN)₂], yields a mixture of complexes. The mixture was crystallized with dichloromethane/pentane (1:1) and crystals of [Pt(bddn)]Cl₂ · 3.5 H₂O was obtained. Electronic supplementary material The online version of this article contains supplementary material, which is available to authorized users.     

Supramolecular Cobalt(II), Copper(II) and Cadmium(II) Complexes Obtained from a Proton Transfer Compound including Pyridine-2,6-dicarboxylate and Propane-1,3-diaminium Ions; Synthesis,Characterization and Crystal Structure

Abstract The three complexes (pnH₂)[Co(pydc)₂]·4H₂O 1, (pnH₂)[Cu(pydc)₂]·4H₂O 2, and (pnH₂)[Cd(pydc)₂]·3.5H₂O 3 (pn: propane-1,3-diamine, pydc: pyridine-2,6-dicarboxylate) were prepared using a proton transfer compound (pnH₂)(pydc)·(pydcH₂)·2.5H₂O, LH ₂ and corresponding metallic salts. The characterization was carried out using elemental analysis, IR and NMR spectroscopy, and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in space group P , but complex 3 crystallizes in space group P2/c. Cell parameters of the complexes are a = 8.449(1) ?, b = 11.668(1) ?, c = 12.801(1) ?, α = 115.748(2)°, β = 93.038(2)°, γ = 97.867(2)° for 1; a = 7.973(2) ?, b = 16.632(2) ?, c = 25.280(5) ?, α = 94.178(6)°, β = 95.186(6)°, γ = 91.603(5)° for 2 and a = 20.055(1) ?, b = 13.8161(9) ?, c = 8.2418(5) ?, β = 100.086(1)° for 3. The three crystal structures illustrate that the metal ion is six-coordinated by two pydc’s. In structures of 2 and 3, it can be seen that propane-1,3-diaminium fragments have different conformations. The complexes have ion-pairing interactions, O–H···O, N–H···O and C–H···O hydrogen bonds, π–π stacking as well as van der Waals forces as the main factors in formation of their supramolecular structures. Index Abstract Supramolecular Cobalt(II), Copper(II) and Cadmium(II) Complexes Obtained from a Proton Transfer Compound including Pyridine-2,6-dicarboxylate and Propane-1,3-diaminium Ions; Synthesis, Characterization and Crystal Structure Hossein Aghabozorg, Mohammad Ghadermazi,Bahar Nakhjavan, Faranak Manteghi The synthesis, characterization, crystal structure and non-covalent interactions of three supramolecular complexes of Co(II), Cu(II) and Cd(II) obtained by the reaction of a proton transfer compound i.e. (pnH₂)(pydc)·(pydcH₂)·2.5H₂O with the corresponding metallic salts are reported. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Supramolecular Association in the Structure of 2,9-<Emphasis Type="Italic">C</Emphasis>-<Emphasis Type="Italic">meso</Emphasis>-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-diazoniacyclotetradecane as its Bis(nitrate) and Bis(acetate) Trihydrate

Abstract In the crystal structure of the nitrate salt, columns of di-cationic macrocycles, each disposed about a center of inversion, are interspersed by pairs of nitrate anions that form charged-assisted N–H···O hydrogen-bonding interactions, reinforced by C–H···O contacts. The topology of the resulting supramolecular architecture is that of a linear chain and these associate via further weak C–H···O contacts. In the structure of the acetate trihydrate, di-cationic macrocycles are circumscribed by 32-membered rings defined by O–H···O interactions, involving the acetate anions and solvent water molecules. Systematic variations in the geometric parameters in the molecular structures are correlated with the influence of intermolecular interactions. The nitrate crystallizes in the monoclinic space group P2₁/n with a = 8.3524(11) ?, b = 12.5497(16) ?, c = 11.1208(16) ?, β = 103.180(3)°, and Z = 2. The acetate trihydrate also crystallizes in the monoclinic space group P2₁/n with a = 9.6679(15) ?, b = 15.278(2) ?, c = 9.8376(18) ?, β = 106.068(5)°, and Z = 2. Index Abstract Supramolecular Association in the Structure of 2,9- C-meso -2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11- diazoniacyclotetradecane as its Bis(nitrate) and Bis(acetate) Trihydrate Saroj K. S. Hazari, ⁽¹⁾ Tapashi G. Roy, ^(1)* Kanak K. Barua ⁽¹⁾ and Edward R. T. Tiekink ^(2)* A linear supramolecular chain stabilized by charge-assisted N–H···O hydrogen-bonding interactions is found in the nitrate salt. In the acetate trihydrate, di-cationic macrocycles are circumscribed by 32-membered rings constructed by O–H···O hydrogen-bonds. Supramolecular Association in the Structure of 2,9- C-meso -2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11- diazoniacyclotetradecane as its Bis(nitrate) and Bis(acetate) Trihydrate Saroj K. S. Hazari, ⁽¹⁾ Tapashi G. Roy, ^(1)* Kanak K. Barua ⁽¹⁾ and Edward R. T. Tiekink ^{(2)* (1)}Department of Chemistry, University of Chittagong, Chittagong-4331, Bangladesh ⁽²⁾Department of Chemistry, The University of Texas at San Antonio, One UTSA Circle, San Antonio, Texas 78249-0698 Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt<Subscript>2</Subscript>(μ<Subscript>2</Subscript>-S)<Subscript>2</Subscript>] Core Structures

Abstract Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were synthesized from mononuclear starting materials, and characterized. Complex [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] has phospine ligands arranged trans and presents a planar [Pt₂(μ₂-S)₂] core structure, imposed by symmetry. In contrast, the almost isoformular complex [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)] revealed to be a butterfly molecule with phosphine ligands in a cis configuration. In both complexes, two pentafluorobenzenethiolate ligands bridge metal centers in an anti conformation. Both compounds have been X-ray characterized. Trans complex: a = 11.8576(13) ?, b = 12.3237(14) ?, c = 13.4644(16) ?, α = 90.528(9)°, β = 113.866(9)°, γ = 107.698(9)°, ; cis complex: a = 24.368(2) ?, b = 15.043(2) ?, c = 37.596(7) ?, β = 93.69(1)°, C2/c. Index Abstract Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt ₂ (μ ₂ -S ) ₂ ] Core Structures Sylvain Bernès, Luis Villanueva & Hugo Torrens Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were X-ray characterized, [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] and [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)]. The [Pt₂(μ₂-S)₂] core is constrained by symmetry to be planar in the former complex, affording a trans arrangement for non-bridging ligands, whereas the latter is a butterfly molecule with a cis configuration. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

The Preparation,Characterization and X-ray Structural Analysis of Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone]cadmium(II) Hexafluorophosphate

Abstract A new compound, [Cd(dmise)₄][PF₆]₂, has been synthesized and characterized via standard solid and solution state methods including single crystal X-ray crystallography (dmise = 1,3-dimethyl-2(3H)-imidazoleselone). The title compounds crystallizes in orthorhombic space group P bcn with a = 12.783(3), b = 22.206(4), c = 13.153(3) ?, V = 3733.8(13) ?³, Z = 4. The complex is a high melting, yellow water soluble 2:1 electrolyte solid that state has a flattened tetrahedral CdSe₄ coordination geometry. To date this is the only structural study reported for a homoleptic selenourea complex of cadmium. Graphical abstract The Preparation, characterization and X-ray structural analysis of Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone]cadmium(II) hexafluorophosphate Daniel J. Williams, Bradley J. McKinney, Ben Baker, Kevin P. Gwaltney and Donald VanDerveer Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone][PF₆]₂ is prepared in 82% yield by direct combination of cadmium acetate dihydrate, ammonium hexafluorophosphate, and the ligand in boiling acetonitrile. X-ray crystallography shows a structure with a distorted tetrahedral coordination sphere around the cadmium. This is the first report of a structural characterization of a homoleptic cadmium selenourea complex. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.