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Syntheses and X-ray crystal structures of four 4-(4-methoxyphenyl)piperazin-1-ium (MeOPP) salts, with 2,2,2-trifluoroacetate, C11H17N2O+πC2F3O2- (I), 2,3,4,5,6-pentafluorobenzoate, C11H17N2O+πC7F5O2-πH2O (II), 4-iodobenzoate C11H17N2O+πC7H4IO2-πH2O (III), and 4-methylbenzoate, C11H17N2O+π- C8H7O2-πH2O (IV) anions are presented. The salts form directly from equimolar quantities of N-(4-methoxyphenyl)piperazine and the corresponding organic acid in methanol and crystallize from 1:1 methanol/ethyl acetate. Salt I is anhydrous whereas II, III, and IVare all monohydrates. In all cases, the MeOPP cation conformation is determined by the torsion about the N--C bond between the piperazinium and 4-methoxybenzene rings. Crystal packing in each structure is largely dictated by N--Hπ π πO and (in II, III, and IV) O--Hπ π πO hydrogen bonds, although each also features weak C--Hπ π πO-type hydrogen bonds. Salt II also has π-π-stacking interactions between cation and anion arene rings, and III exhibits Iπ π πI close contacts. [ABSTRACT FROM AUTHOR]

The title compound, C6H15N2O+·C6H2N3O7-·H2O, was synthesized via slow evaporation of an aqueous solution of picric acid with the substituted morpholine base and crystallized with one cation (C6H15N2O)+, one anion (C6H2N3O7)- and a water molecule in the asymmetric unit. The morpholine ring in the cation adopts a chair conformation. The structure is stabilized by C--H...O, O--H...O, O--H...N and N--H...O hydrogen-bonding interactions and π-π stacking. The intermolecular interactions of the synthesized compound were quantified by Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]

The synthesis and crystal structures of the molecular salts of 4-(4-nitrophenyl) piperazine with trifluoroacetate, namely, 4-(4-nitrophenyl)piperazin-1-ium trifluoroacetate, C10H14N3O2+·C2F3O2- (I), and with trichloroacetate, namely, 4-(4-nitrophenyl)piperazin-1-ium trichloroacetate, C10H14N3O2+·C2Cl3O2-, (II), are reported and compared. A partial positional disorder of the anions was found. In both structures, the piperazine rings adopt a chair conformation, whereas the positions of the nitrophenyl group on the piperazine ring differ from bisectional in (I) to equatorial in (II). In both structures, the supramolecular assemblies are mono-periodic on the basis of the chain-of-rings motifs supported by aromatic π-π interactions. Hirshfeld surface analysis was used to explore the intermolecular close contacts in both crystals. The most dominant contacts of the Hirshfeld surface of the cation-anion pairs of the asymmetric units are O...H/H...O, and those with a contribution of halogen atoms: F...H/H...F in (I) and Cl...H/H...Cl in (II), respectively. [ABSTRACT FROM AUTHOR]

Eleven (4-phenyl)piperazinium salts containing organic anions have been prepared and structurally characterized, namely, 4-phenylpiperazin-1-ium f4l-uorobenzoate monohydrate, C10H15N2+-C7H4FO2-H2O, 1; 4-phenylpiperazin-1-ium 4-bromobenzoate monohydrate, C10H15N2+-C7H4NO2-H2O, 3; 4-phenylpiperazin-1-ium 4-iodobenzoate, C10H15N2+-C7H4IO2_, 4; 4-phenylpiperazin-1-ium 4-nitrobenzoate, C10H15N2+-C7H4NO4_, 5; 4-phenylpiperazin-1-ium 3,5-dinitrosalicylate, C10H15N2+-C7H3N2O7_, 6; 4-phenylpiperazin-1-ium 3d,i5n-itrobenzoate, C10H15N2+-C7H3N2O6_, 7; 4-phenylpiperazin-1-ium picrate, C10H15N2+-C6H2N3O7_, 8; 4-phenylpiperazin-1-ium benzoate monohydrate, C10H15N2+-C7H5O2_-H2O, 9; 4-phenylpiperazin-1-ium p-toluenesulfonate, C10H15N2+-C7H7O3S_, 10; 4-phenylpiperazin-1-ium tartarate monohydrate, C10H15N2+-C4H5O6~-H2O, 11; and 4-phenylpiperazin-1-ium fumarate, C10H15N2+-C4H3O4_, 12. Compounds 1 and 3-12 are all 1:1 salts with the acid proton transferred to the phenylpiperaizine basic N atom (the secondary amine) with the exception of 3 where there is disorder in the proton position with it being 68% attached to the base and 32% attached to the acid. Of the structures with similar stoichiometries only 3 and 9 are isomorphous. The 4-phenyl substituent in all cases occupies an equatorial position except for 12 where it is in an axial position. The crystal chosen for structure 7 was refined as a nonmerohedral twin. There is disorder in 5, 6, 10 and 11. For both 5 and 6, a nitro group is disordered and was modeled with two equivalent orientations with occupancies of 0.62 (3)/0.38 (3) and 0.690 (11)/0.310 (11), respectively. For 6,10 and 11, this disorder is associated with the phenyl ring of the phenylpiperazinium cation with occupancies of 0.687 (10)/0.313 (10), 0.51 (7)/0.49 (7) and 0.611 (13)/389 (13), respectively. For all salts, the packing is dominated by the N--H--O hydrogen bonds formed by the cation and anion. In addition, several structures contain C--H--Ä (1, 3, 4, 8, 9,10, and 12) and aromatic ä-ä stacking interactions (6 and 8) and one structure (5) contains a -NO2"-x interaction. For all structures, the Hirshfeld surface fingerprint plots show the expected prominent spikes as a result of the N--H--O and O--H--O hydrogen bonds. [ABSTRACT FROM AUTHOR]

2-(3-Hydroxypropyl)-1H-benzimidazole, C10H12N2O, which has potential biological activity, can be used as a ligand for complexation with metals. This compound is an electron donor, due to the lone pair of the nitrogen atom in the imidazole ring. This nitrogen atom also acts as a proton acceptor. In the crystalline phase, the nitrate salt, namely, 2-(3-hydroxypropyl)-1H-benzimidazol-3-ium nitrate, C10H13N2O+·NO3-, has been studied. The protonation of the 2-(3-hydroxypropyl)benzimidazole unit results in significant delocalization of the electron density within the imidazole ring. The salt formation leads to variations in the intermolecular interactions, which were studied by analysis of the Hirshfeld surfaces and two-dimensional fingerprint plots. [ABSTRACT FROM AUTHOR]

A new 0D organic--inorganic hybrid material bis[1-(prop-2-en-1-yl)-1Himidazol- 3-ium] hexachloridostannate(IV), (C6H9N2)2[SnCl6], has been prepared and characterized by single-crystal X-ray diffraction, Hirshfeld surface analysis and UV--visible spectroscopy. The structure consists of isolated [SnCl6]2 octahedral anions separated by layers of organic 1-(prop-2-en-1-yl)- 1H-imidazol-3-ium cations. The 1-(prop-2-en-1-yl) fragment in the organic cation exhibits disorder over two sets of atomic sites having occupancies of 0.512 (9) and 0.488 (9). The crystal packing of the title compound is established by intermolecular N/C--H Cl hydrogen bond and п-п stacking interactions. Hirshfeld surface analysis employing three-dimensional molecular surface contours and two-dimensional fingerprint plots has been used to analyse the intermolecular interactions present in the structure. The optical properties of the crystal were studied using UV--visible absorption spectroscopy, showing one intense band at 208 nm, which is attributed to п-п transitions in the cations. [ABSTRACT FROM AUTHOR]

In the title molecular salt, (C5H7N2)2[SnCl6], the cation is protonated at the pyridine N atom and the complete dianion is generated by a crystallographic centre of symmetry. In the crystal, N—HCl hydrogen bonds link the components into a three-dimensional network built up from the stacking of alternate cationic and anionic layers. The nature of the intermolecular interactions has been analysed in terms of the Hirshfeld surfaces of the cations and the anions. The thermal behaviour and the Raman spectrum of the title compound are reported. [ABSTRACT FROM AUTHOR]

In the title molecular salt, 1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-9- ium aquatrichloridozincate(II), (C7H9N4O2)[ZnCl3(H2O)], the fused ring system of the cation is close to planar, with the largest deviation from the mean plane being 0.037 (3) A ° . In the complex anion, the ZnII cation is coordinated by three chloride ions and one oxygen atom from the water ligand in a distorted tetrahedral geometry. In the crystal, inversion dimers between pairs of cations linked by pairwise N--H…O hydrogen bonds generate R2 2(10) rings. The anions are linked into dimers by pairs of O--H…Cl hydrogen bonds and the respective dimers are linked by O--H…O and N--H…Cl hydrogen bonds. Together, these generate a three-dimensional supramolecular network. Hirshfeld surfaces were generated to gain further insight into the packing. [ABSTRACT FROM AUTHOR]

Charge-assisted hydrogen bonding plays a significant role in the crystal structures of solvates of ionic com­pounds, especially when the cation or cations are primary ammonium salts. We report the crystal structures of four ammonium salts of molybdenum halide cluster solvates where we observe significant hydrogen bonding between the solvent molecules and cations. The crystal structures of bis(anilinium) octa-μ3-chlorido-hexa­chlorido-octa­hedro-hexa­molybdate N,N-di­­methyl­formamide tetra­solvate, (C6H8N)2[Mo6Cl8Cl6]·4C3H7NO, (I), p-phenyl­enedi­ammonium octa-μ3-chlorido-hexa­chlorido-octa­hedro-hexa­mol­yb­date N,N-di­methyl­formamide hexa­solvate, (C6H10N2)[Mo6Cl8Cl6]·6C3H7NO, (II), N,N′-(1,4-phenyl­ene)bis­(propan-2-iminium) octa-μ3-chlorido-hexa­chlo­rido-octa­hedro-hexa­molybdate acetone tris­olvate, (C12H18N2)[Mo6Cl8Cl6]·3C3H6O, (III), and 1,1′-dimethyl-4,4′-bipyridinium octa-μ3-chlo­rido-hexa­chlorido-octa­hedro-hexa­molybdate N,N-di­methyl­formamide tetra­solvate, (C12H14N2)[Mo6Cl8Cl6]·4C3H7NO, (IV), are reported and described. In (I), the anilinium cations and N,N-di­methyl­formamide (DMF) solvent mol­ecules form a cyclic R4²(8) hydrogen-bonded motif centered on a crystallographic inversion center with an additional DMF mol­ecule forming a D(2) inter­action. The p-phenyl­enedi­ammonium cation in (II) forms three D(2) inter­actions between the three N—H bonds and three independent N,N-di­methyl­formamide mol­ecules. The dication in (III) is a protonated Schiff base solvated by acetone mol­ecules. Compound (IV) contains a methyl viologen dication with N,N-di­methyl­formamide mol­ecules forming close contacts with both aromatic and methyl H atoms. [ABSTRACT FROM AUTHOR]

The reaction of 2-methylthio-5-amino-1,3,4-thiadiazole (Me-SNTD; C3H5N3S2) with copper(II) acetate monohydrate [Cu(OAc)2·H2O; C4H8CuO5] resulted in the formation of the title binuclear compound, [Cu2(C2H3O2)4(C3H5N3S2)2] or [Cu2(OAc)4(Me-SNTD)2]. The structure has triclinic (P 1) symmetry with a crystallographic inversion centre located at the midpoint of the line connecting the Cu atoms in the dimer. These two Cu atoms of the dimer [Cu···Cu = 2.6727(6)Å] are held together by four carboxylate groups. Each Cu atom is further coordinated to the N atom of an Me-SNTD molecule and exhibits a Jahn-Teller-distorted octahedral geometry. The dimers are connected into infinite chains by hydrogen bonds between the NH (Me-SNTD) and the carboxylate groups of neighbouring molecules, generating an R²2(12) ring motif. The molecules are further linked by C--H···π interactions between the thiadiazole rings and the methyl groups of the acetate units. [ABSTRACT FROM AUTHOR]

In the title compound, C18H12O3S2, synthesized by the Claisen-Schmidt condensation method, the essentially planar chalcone unit adopts an s-cis configuration with respect to the carbonyl group within the ethyl­enic bridge. In the crystal, weak C--H...π inter­actions connect the mol­ecules into zigzag chains along the b-axis direction. The mol­ecular structure was optimized geometrically using Density Functional Theory (DFT) calculations at the B3LYP/6-311 G++(d,p) basis set level and compared with the experimental values. Mol­ecular orbital calculations providing electron-density plots of HOMO and LUMO mol­ecular orbitals and mol­ecular electrostatic potentials (MEP) were also computed both with the DFT/B3LYP/6-311 G++(d,p) basis set. The experimental energy gap is 3.18 eV, whereas the theoretical HOMO-LUMO energy gap value is 2.73 eV. Hirshfeld surface analysis was used to further investigate the weak inter­actions present. [ABSTRACT FROM AUTHOR]

In the title mol­ecular salt, (C5H8N3)2[CoCl4], the cations are protonated at their pyridine N atoms and the anion is an almost regular tetra­hedron. The crystal structure consists of alternating inorganic layers, built from tetra­chlorido­cobaltate anions, and organic layers formed by protonated cations of 2,6-di­amino­pyridinium. The crystal packing is governed by C/N—HCl hydrogen-bonding inter­actions between the organic and the inorganic ions and ClCl inter­actions. Moreover, the cations show a π–π stacking inter­action [inter­centroid distance = 3.763 (2) Å]. The prevalence of these inter­actions is illustrated by an analysis of the three-dimensional Hirshfeld surface and by two-dimensional fingerprint plots. [ABSTRACT FROM AUTHOR]

The synthesis and the crystal structure of a new halide-bridged polymer, namely catena-poly[bis­(1,2,3-benzotriazolium) [[tetra­chlorido­bis­muth(III)]-μ-chlorido] dihydrate], {(C6H6N3)2[BiCl5]·2H2O}n are reported. The structure comprises polyanionic zigzag chains of formula [(BiCl5)2−]n running along the c-axis direction. The 1,2,3-benzotriazolium cations are linked between these polymer chains, via the water mol­ecules, giving rise to left- and right-handed helical chains. Hirshfeld surface analysis and fingerprint plots were used to decode the inter­molecular inter­actions in the crystal network and determine the contribution of the component units for the construction of the three-dimensional architecture. [ABSTRACT FROM AUTHOR]

The synthesis of 4-azaniumyl-2,2,6,6-tetramethylpiperidin-1-ium diperchlorate, C9H22N22+⋅2ClO4-, was carried out from an aqueous reaction of perchloric acid with 4-amino-2,2,6,6-tetramethylpiperidine. This compound was characterized by TGA--DSC analysis and single-crystal X-ray diffraction. The piperidine ring of the dication adopts a chair conformation and the orientation of the C--H3 bond is equatorial. One of the two crystallographically independent perchlorate anions exhibits disorder [occupancies 0.625 (7) and 0.375 (7)]. The crystal packing is constituted by a succession of mixed layers parallel to the (-102) plane, made up of C9H22N22+ dications and ClO4- anions. These ions are linked by normal and bifurcated N--H⋯O hydrogen bonds with R44(12) graph-set motifs, generating a two-dimensional network. The intermolecular interactions in the crystal structure were quantified and analysed using Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]

Imidazole-containing compounds exhibit a myriad of pharmacological activities. Two tetrachloridozincate salts of 4-carboxy-1H-imidazol-3-ium, ImHCO2H+, are reported. Bis(4-carboxy-1H-imidazol-3-ium) tetrachloridozincate monohydrate, (C4H5N2O2)2[ZnCl4]·H2O, (I), crystallizes as a monohydrate salt, while bis(4-carboxy-1H-imidazol-3-ium) tetrachloridozincate bis(1H-imidazol-3-ium-4-carboxylato) monohydrate, (C4H5N2O2)2[ZnCl4]·2C4H4N2O2·H2O, (II), is a co-crystal salt with six residues: two ImHCO2H+ cations, two formula units of the zwitterionic 1H-imidazol-3-ium-4-carboxylate, ImHCO2, one tetrachloridozincate anion and one water molecule disordered over two sites in a 0.60 (4):0.40 (4) ratio. The geometric parameters of the ImHCO2H+ and the ImHCO2 moieties are the same within the standard uncertainties of the measurements. Both compounds exhibit extensive hydrogen bonding, including involvement of the tetrachloridozincate anion, resulting in interconnected chains of anions joined by water molecules. [ABSTRACT FROM AUTHOR]

The asymmetric unit of the title salt, [p-FC6H4CH2NH3]+⋅H2PO4-, contains one 4-fluorobenzylammonium cation and one dihydrogen phosphate anion. In the crystal, the H2PO4- anions are linked by O--H⋯O hydrogen bonds to build corrugated layers extending parallel to the ab plane. The FC6H4CH2NH3+ cations lie between these anionic layers to maximize the electrostatic interactions and are linked to the H2PO4- anions through N--H⋯O hydrogen bonds, forming a three-dimensional supramolecular network. Two hydrogen atoms belonging to the dihydrogen phosphate anion are statistically occupied due to disorder along the OH⋯HO direction. [ABSTRACT FROM AUTHOR]

The crystal structure of the title compound, (C6H16N2O)[CdCl1.90I2.10], a new organic-inorganic hybrid salt synthesized in the form of single crystals, consists of discrete statistically distributed dichloridodiiodidocadmate/chloridotriiodidocadmate anions (occupancy ratio 0.90:0.10) and 4-(2-ammonioethyl)morpholin- 4-ium cations, [NH3(CH2)2NH(CH2)4O]2+. The cations are linked by intermolecular N--H...O hydrogen bonds, forming corrugated chains extending parallel to the c axis. The [CdCl1.90I2.10]2- tetrahalidocadmate anions lie between the chains to maximize the electrostatic interactions and are connected with the organic cations via N--H...Cl and C--H...Cl(I) hydrogen bonds developing in the ab plane and leading to the formation of a three-dimensional network structure. The tetracoordinate CdII atom has a distorted tetrahedral conformation, with a τ4 index of 0.87. [ABSTRACT FROM AUTHOR]

The structure of the title non-centrosymmetric organic-inorganic hybrid salt, (C8H12NO)2[ZnCl4], consists of two 4-methoxybenzylammonium cations sandwiched between anionic layers, formed by isolated tetrachloridozincate tetrahedra. The double layers extend parallel to the ac plane. The crystal packing is assured by Coulombic interactions and by a complex N--H...Cl and C--H...Cl hydrogen-bonding system mostly involving the positively charged ammonium groups and the chloride ligands of the isolated tetrahedral [ZnCl4]2 units. One of the methyleneammonium groups is disordered over two sets of sites in a 0.48 (2):0.52 (2) ratio. The crystal investigated was twinned by nonmerohedry with a twin component ratio of 0.738 (2):0.262 (2). [ABSTRACT FROM AUTHOR]

The title organic-inorganic hybrid salt, (C7H11N2)2[V(C2O4)2O(H2O)]?2H2O, shows a distorted octahedral coordination environment for the vanadium(IV) atom in the anion (point group symmetry 2), with four O atoms from two symmetry-related chelating oxalate dianions and two O atoms in trans configuration from a coordinating water molecule and a terminal vanadyl O atom. In the crystal, (001) layers of cations and anions alternate along [001]. The anionic layers are built up by intermolecular O--H⋯O hydrogen bonds involving the coordinating and solvent water molecules. The cationic layers are linked to the anionic layers via N--H⋯O hydrogen bonds between the pyridinium group and the non-coordinating O atoms of the oxalate group. The 4-(dimethylamino)pyridinium cations are also engaged in &#960-π stacking with their antiparallel neighbours [centroid-to-centroid distance = 3.686 (2) Å]. Considering all supramolecular features, a three-dimensional network structure is accomplished. [ABSTRACT FROM AUTHOR]

The asymmetric unit of the title compound, 2C6H9N2+•HPO42-, comprises two 2-amino¬anilinium cations and one hydrogen phosphate dianion. In the crystal, the HPO42- dianions are linked by O--H⋯O hydrogen bonds into chains along [100]. The inorganic anionic chains and organic cations are linked by N--H⋯O and N--H⋯N hydrogen bonds, forming a two-dimensional supra¬molecular network extending parallel to (001). [ABSTRACT FROM AUTHOR]