1,3‐Propane­di­ammonium tetra­thio­tungstate and N,N,N′,N′‐tetra­methyl­ethyl­enedi­ammonium tetra­thio­tungstate

The title complexes, (C₃H₁₂N₂)[WS₄] and (C₆H₁₈N₂)[WS₄], contain tetrahedral [WS₄]²⁻ dianions, which accept a complex series of hydrogen bonds from the organic dications. The strength and number of these hydrogen bonds affect the W—S distances.     

[Benzyl­bis­(di­methyl­amino)­methyl­silyl‐κ2C,N](N,N,N′,N′‐tetra­methyl­ethyl­ene­di­amine‐κ2N,N)­lithium(I)

The title compound, [Li(C₁₂H₂₁NSi)(C₆H₁₆N₂)], is an intermediate in the synthesis of the corresponding organometallic compounds. The mol­ecule has an unusual C—Si—N—Li four‐membered heterocycle which adopts a folded conformation, with the coordination around the Li, N, C and Si atoms being distorted tetrahedral. Its structure is strongly supported by ¹H NMR, ¹³C NMR and ¹³C–¹H correlation spectra. The compound has potential for application in the synthesis of other novel organometallic compounds.     

Layered zincoarsenate templated by N,N,N′,N′‐tetra­methyl­ethyl­ene‐di­amine mol­ecules

The title compound, N,N,N′,N′‐tetra­methyl­ethyl­enedi­ammon­ium di­aqua­(arsenate)­(hydrogen arsenate)­dizinc(II), (C₆H₁₈N₂)_0.5[Zn₂(AsO₄)(HAsO₄)(H₂O)₂], is a new zincoarsenate obtained by hydro­thermal synthesis. The structure consists of infinite two‐dimensional anionic layers alternating with planes containing centrosymmetric organic diprotonated template N,N,N′,N′‐tetra­methyl­ethyl­enedi­ammonium cations, [H₃N­C₆H₁₂NH₃]²⁺. The latter are interconnected to the framework through hydrogen bonds.     

N,N,N′,N′‐Tetra­methyl­ethyl­enedi­ammonium dichloride

The structure of the title compound, C₆H₁₈N₂²⁺.2Cl^?, has been determined and has a centre of symmetry. The mol­ecule has strong intermolecular hydrogen bonding between each Cl^? and an N—H bond [Cl?N = 3.012 (3) Å].     

Hydro­gen bonding in ethyl­ene­di­ammonium bis­(hydrogen malonate) mono­hydrate

In the title compound, C₂H₁₀N₂²⁺·2C₃H₃O₄^?·H₂O, the hydrogen malonate anion has an intramolecular O—H?O hydrogen bond of 2.430 (2) Å. The water mol­ecule lies on a twofold axis and connects the anions into pairs through hydrogen bonds of 2.734 (1) Å. The ethyl­enedi­ammonium cation lies across an inversion centre. Each of the ammonium protons is involved in hydrogen bonding to an anion or a water mol­ecule [N?O 2.815 (2)–2.875 (2) Å].     

Bis­[N,N′‐bis­(di­phenyl­methyl­ene)ethyl­enedi­amine‐κ2N,N′]copper(I) di­chloro­cuprate(I)

The 1:1 adduct of N,N′‐bis­(di­phenyl­methyl­ene)­ethyl­enedi­amine (bz₂en) with copper(I) chloride, viz. [Cu(C₂₈H₂₄N₂)₂][CuCl₂], has been synthesized. The structure contains cationic moieties of Cu^I ions (Cu on a twofold axis) coordinated to four N atoms of two bz₂en mol­ecules (in a distorted tetrahedron) and linear di­chloro­cuprate(I) anions (with Cu on an inversion centre). These cations and anions are packed in columns along b. The packing of the cation and anion columns involves a significant C—H⋯Cl interaction and four short intermolecular C—H⋯π contacts, two of which are between cation columns.     

Ammonium di­chloro­bis­(di­methyl­glyoximato‐N,N′)­iridate(III)

In the title compound, (NH₄)[IrCl₂(C₄H₇N₂O₂)₂], (I), the Ir atom is octahedrally coordinated by two trans Cl^? and two di­methyl­glyoximate chelate ligands in the equatorial plane. A two‐dimensional hydrogen‐bond network between ammonium cations NH₄⁺ and anionic [IrCl₂(C₄H₇N₂O₂)₂]^? complexes is extended along the bc plane.     

N,N,N′,N′‐Tetra­methyl­ethyl­ene­diammonium–succinate–succinic acid (1/1/1)

In the title compound, C₆H₁₈N₂²⁺·C₄H₄O₄²⁻·C₄H₆O₄, the components lie on centres of symmetry in space group , such that the asymmetric unit contains three half‐mol­ecules. Despite the different mode (with respect to other di­carboxylic acids) adopted by the intermolecular self‐interaction of succinic acid derivatives, the overall structure of the title compound consists of anionic layers that are typical of the packing structures exhibited by other di­carboxylic acid analogues.     

trans‐Di­aqua(C‐meso‐5,12‐di­methyl‐1,4,8,11‐tetra­aza­cyclo­tetra­decane‐N,N′,N′′,N′′′)copper(II) dichloride dihydrate

The crystal structure of the title complex, [Cu(C₁₂H₂₈N₄)(H₂O)₂]Cl₂·2H₂O, has been determined. The Cu^II atom is octahedrally coordinated by the four N atoms of the tetradentate macrocyclic ligand in equatorial positions and by the O atoms of two water mol­ecules in axial positions. The crystal structure is stabilized by a three‐dimensional network of hydrogen bonds.     

trans‐Bis­[N‐(2‐hydroxy­ethyl)­ethyl­ene­di­amine‐κ2N,N′]­bis­(iso­thio­cyanato‐κN)­nickel(II)

The crystal structure of the title compound, [Ni(NCS)₂(C₄H₁₂N₂O)₂], has two crystallographically independent half‐mol­ecules in the asymmetric unit, with each Ni atom residing on a centre of symmetry. The two mol­ecules exhibit similar coordination geometry but display differences with regard to other structural features. Each Ni^II centre is octahedrally coordinated by two mutually trans chelating hydroxy­ethyl­ethyl­ene­di­amine ligands and two mutually trans iso­thio­cyanate ions. The two independent mol­ecules form chains through different types of non‐covalent interactions. In the case of one of the mol­ecules, only NCS and free OH groups participate in hydrogen bonding, while in the chain based on the second mol­ecule, the NCS, NH, NH₂ and free OH groups are involved in intermolecular hydrogen bonding. The two chains interact with one another through hydrogen bonding, forming planar sheets. The third packing direction is mediated only by van der Waals interactions.     

Bis­(acetone‐κO)­bis(N,N′‐di­methyl­ethyl­enedi­amine‐κ2N,N′)copper(II) diperchlorate

The title compound, [Cu(C₄H₁₂N₂)₂(C₃H₆O)₂](ClO₄)₂, is the first structurally characterized Cu^II complex having acetone as axial ligands. The complex adopts an elongated octahedral trans‐[CuN₄O₂] coordination geometry, with the Cu atom having 222 site symmetry. The axial Cu—O(acetone) and in‐plane Cu—N bond lengths are 2.507 (5) and 2.041 (3) Å, respectively.     

Layered (ethyl­ene­di­amine‐κ2N,N′)cobalt(II) molybdate(VI)

The structure of poly­[[(ethyl­enedi­amine‐κ²N,N′)­cobalt(II)]‐μ‐tetra­oxo­molyb­dato(VI)], [Co(C₂H₈N₂)MoO₄]_n or [CoMoO₄(C₂H₈N₂)]_n, is composed of puckered layers constructed from MoO₄ tetrahedra and CoN₂O₄ octahedra, with the ethyl­enedi­amine ligand coordinated to the Co atom in a cis fashion. Each pair of cobalt sites forms a binu­clear edge‐sharing unit through a {Co₂O₂} interaction. The binuclear octahedral units are interconnected through the bridging MoO₄ tetrahedra into a layer structure.     

N,N′,N′′,N′′′‐Tetraethylterephthalamidinium bis(tetrazolate)

The crystal structure of the title 2:1 salt of tetrazole and a substituted terephthal­amidine, C₁₆H₂₈N₄²⁺·2CHN₄^?, contains an infinite network of hydrogen bonds, with short N?N distances of 2.820 (2) and 2.8585 (19) Å between the tetrazolate anion and the amidinium cation. Involvement of the lateral N atoms of the tetrazole in the hydrogen bonding appears to be a typical binding pattern for the tetrazolate anion.     

(12‐Hydro­xy­methyl‐5,5,7,12,14‐penta­methyl‐1,4,8,11‐tetra­aza­cyclo­tetra­decane‐N‐acetato‐N,N′,N′′,N′′′,O,O′)cobalt(III) chloride perchlorate monohydrate

In the title compound, [Co(C₁₈H₃₇N₄O₃)](ClO₄)Cl·H₂O, the Co^III ion has a distorted octahedral geometry, with four N atoms and two O atoms constituting the coordination sphere. The crystal structure is stabilized by a three‐dimensional network of hydrogen bonds.     

μ‐{N,N′‐Bis[2‐(dimethyl­amino)ethyl]oxamidato(2–)}‐1κ2O,O′:2κ4N,N′,N′′,N′′′‐bis­(4,4′‐dimethyl‐2,2′‐bipyridine‐1κ2N,N′)dinickel(II) bis­(perchlorate)

In the crystal structure of the title complex, [Ni₂(C₁₀H₂₀N₄O₂)(C₁₂H₁₂N₂)₂](ClO₄)₂ or [Ni(dmaeoxd)Ni(dmbp)₂](ClO₄)₂ {H₂dmaeoxd is N,N′‐bis­[2‐(dimethyl­amino)ethyl]oxamide and dmbp is 4,4′‐dimethyl‐2,2′‐bipyridine}, the deprotonated dmaeoxd²⁻ ligand is in a cis conformation and bridges two Ni^II atoms, one of which is located in a slightly distorted square‐planar environment, while the other is in an irregular octa­hedral environment. The cation is located on a twofold symmetry axis running through both Ni atoms. The dmaeoxd²⁻ ligands inter­act with each other via C—H⋯O hydrogen bonds and π–π inter­actions, which results in an extended chain along the c axis.     

(Acetonitrile‐κN){2‐[bis­(2‐pyridylethyl)­amino]ethanol‐κ4N,N′,N′′,O}zinc(II) bis­(perchlorate) monohydrate

In the title compound, [Zn(C₂H₃N)(C₁₆H₂₁N₃O)](ClO₄)₂·H₂O, the Zn^II ion is coordinated by two pyridyl N atoms, one amine N atom, and an ethanol O atom from the N,N′,N′′,O‐tetra­dentate 2‐[bis­(2‐pyridylethyl)amino]­ethanol donor ligand. The fifth coordination site is filled by an acetonitrile N atom, and there is one solvent water mol­ecule in the asymmetric unit. The 2+ charge of the cationic portion of the complex is balanced by two perchlorate counter‐anions.     

3‐(4‐Chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine and 3‐(2,4‐di­chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine

In both of the title compounds, C₂₃H₁₉ClN₂O, (I), and C₂₃H₁₈Cl₂N₂O, (II), the molecular packing is influenced by weak intermolecular C—H⋯O and C—H⋯π interactions, but despite the chemical similarity of the compounds, the packing in (II) is entirely different from that observed in (I).     

The diprotonated 2,2‐(propane‐1,3‐di­yl)bis­(1,1,3,3‐tetra­methyl­guanidinium) cation: packing and conformational changes

Subject to packing with different anions, the title cation undergoes various conformational changes with significantly different N—C—C—C torsion angles, as well as different angles between the NCN₂ guanidine planes. The 2,2‐(propane‐1,3‐di­yl)bis­(1,1,3,3‐tetra­methyl­guanidinium) salts reported here, viz. the dibromide, C₁₃H₃₂N₆²⁺·2Br⁻, the tetra­phenyl­borate chloride, C₁₃H₃₂N₆²⁺·C₂₄H₂₀B⁻·Cl⁻, the tetra­chloro­mercurate, (C₁₃H₃₂N₆)[HgCl₄], and the bis­(trifluoro­methanesulfonate), C₁₃H₃₂N₆²⁺·2CF₃SO₃⁻, are dominated by strong inter­molecular N—H⋯X hydrogen bonds, which form different packing patterns.     

Tetra­ethyl­ammonium bis­(N,N‐diethyl­dithio­carbamato‐κ2S,S′)iodo­cadmate(II)

The title compound, (C₈H₂₀N)[Cd(C₅H₁₀NS₂)₂I], containing a heteroleptic five‐coordinate mononuclear anionic cadmium complex, crystallizes in ortho­rhom­bic form in the space group Pnma. Both anion and cation lie about mirror planes. Unlike other known [Cd(dtc)₂X]‐type complexes (where dtc is dithio­carbamate and X is a halogen or pseudohalogen), the central CdS₄I core shows a square‐pyramidal configuration, with a basal plane defined by four S atoms from two chelating dithio­carbamate ligands related by a symmetry plane. The central Cd atom is displaced from the basal S₄ plane towards the apical I atom of the square pyramid.     

Polymorphism in bipodal O,O′‐dimeth­yl N,N′‐(m‐phenyl­ene­di­carbonyl)bis(thio­carbamate)

The title compound, C₁₂H₁₂N₂O₄S₂, crystallizes in white and yellow polymeric forms as a result of inter­esting anti–anti and syn–anti conformational isomerism of the thio­carbon­yl and carbon­yl moieties relative to one another. This work is the first reported X‐ray crystallographic structure determination of isomers of this class of bipodal ligand. The white form, anti–anti, (I), crystallizes with the benzene ring lying about a twofold rotation axis, resulting in both of the thio­carbon­yl and carbon­yl moieties being anti relative to each other. The yellow modification crystallizes as syn–anti, (II), with one thio­carbon­yl moiety syn and the other anti relative to the respective carbon­yl groups. The individual mol­ecules of both (I) and (II) are extensively linked through inter­molecular hydrogen bonds. Inter­molecular hydrogen bonding in (II) includes a network of bifurcated N—H⋯O and N—H⋯S hydrogen bonds, while mol­ecules of (I) include bifurcated C—H⋯O hydrogen bonds.