Ca2CuTe4O10Cl2, a new synthetic tellurium(IV) oxochloride

Single crystals of dicalcium copper tetra­tellurium deca­oxide dichloride, Ca₂CuTe₄O₁₀Cl₂, were synthesized via a transport reaction in sealed evacuated quartz glass tubes. The building units of the structure are irregular CaO₇ polyhedra, centrosymmetric CuO₄Cl₂ octa­hedra and two crystallographically distinct TeO₄E distorted bipyramids (E being the 5s² lone pair of Te^IV). The TeO₄E and CuO₄Cl₂ polyhedra together form planes that are connected by the Ca atoms. The CuO₄Cl₂ octa­hedra are isolated from each other by the other building units.     

Sr2Cu2TeO6Br2: honeycomb layers of copper(II) ions

Single crystals of distrontium(II) dicopper(II) tellurium(VI) hexa­oxide dibromide, Sr₂Cu₂TeO₆Br₂, were synthesized via solid state/gas phase reactions in sealed evacuated silica tubes. The building units are irregular SrO₄Br₃ polyhedra (a new type of coordination polyhedron around Sr^II), CuO₅ square pyramids and TeO₆ octa­hedra. The CuO₅ square pyramids and the TeO₆ octa­hedra together form layers in the bc plane bridged by Sr atoms. The Cu atoms are arranged to form puckered honeycomb layers. The Te atom lies on an inversion centre.     

A synthetic zinc tellurium oxochloride,Zn2(TeO3)Cl2

Single crystals of dizinc tellurium dichloride trioxide, Zn₂(TeO₃)Cl₂, were synthesized via a transport reaction in sealed evacuated glass tubes. The compound has a layered structure in which the building units are [ZnO₄Cl] square pyramids, distorted [ZnO₂Cl₂] tetrahedra and [TeO₃E] tetrahedra (E is the 5s² lone pair of the Te^IV atom), joined through shared edges and corners to form charge‐neutral layers. Cl atoms and Te‐atom lone pairs protrude from the surfaces of each layer towards adjacent layers, and the layers are held together by dispersion forces only. The compound is isostructural with the synthetic compound CuZn(TeO₃)Cl₂ and the mineral sophiite, Zn₂(SeO₃)Cl₂.     

Monoclinic Cu3(SeO3)2Cl2: an oxo­halide with an unusual CuO4Cl trigonal–bipyramidal coordination

In single crystals of a new monoclinic (C2/m) form of tricopper(II) diselenium(IV) dichloride hexa­oxide, Cu₃(SeO₃)₂Cl₂, the Se atom is in the 4i position, while the two Cu atoms are in 2a and 4i positions. The structure is based on layers of CuO₄Cl trigonal bipyramids, CuO₄ square planes and SeO₃E tetra­hedra. The Cu polyhedra are connected by edge‐ and corner‐sharing to form [010] chains and these chains are bridged by the Se atoms to form (001) layers. The compound is isostructural with Cu₃(TeO₃)₂Br₂.     

Crystal structure and magnetic properties of the coupled spin dimer compound SrCu2(TeO3)2Cl2

Single crystals of the strontium copper tellurium oxochloride SrCu₂(TeO₃)₂Cl₂ were synthesized via solid-gas reactions in sealed evacuated silica tubes. The compound crystallizes in the monoclinic system, space group P2₁, a=7.215(2), b=7.2759(15), c=8.239(2) Å, β=96.56(4)°, Z=2. The building units are [SrO₆Cl₂] irregular polyhedra, [CuO₄] and [CuO₃Cl] square planes, [TeO₃E] tetrahedra and [TeO₃₊₁E] trigonal bipyramids; E being the 5s² lone pair of Te(IV). The Cu atoms can be regarded as forming a chain of weakly connected dimers. The magnetic susceptibility of the compound shows a broad maximum typical for antiferromagnetic spin fluctuations with a non-magnetic ground state. A Heisenberg spin model with coupled s=1/2 dimers leads to a satisfactory fitting of the experimental data.     

Indium tellurium trioxide chloride,InTeO3Cl

The new oxy­chloride InTeO₃Cl was synthesized from a mixture of In₂O₃, InCl₃ and TeO₂. Its structure has been determined from single‐crystal X‐ray diffraction data. The structure is composed of layers separated by a van der Waals gap. The layers consist of edge‐sharing chains of [InO₄Cl₂] octahedra linked through [TeO₃] trigonal pyramids. No free Cl atoms are located between the layers.     

Mg2Ru2Cl10O·16H2O

Mg₂Ru₂Cl₁₀O·16H₂O {dimagnesium μ‐oxo‐bis­[penta­chloro­ruthenate(IV)] hexa­deca­hydrate} crystallizes in the monoclinic system (space group P2₁/c). The structure consists of layers of [Ru₂Cl₁₀O]⁴⁻ anions, [Mg(H₂O)₆]²⁺ cations and water mol­ecules stacked along the a axis. Only the O atom bonded to Ru occupies the 2a site with symmetry. All the other atoms occupy general 4e sites. The crystal structure is stabilized by O—H⋯O and O—H⋯Cl inter­actions.     

Nickel vanadium tellurium oxide,NiV2Te2O10

Single crystals of nickel(II) divanadium(V) ditellurium(IV) decaoxide, NiV₂Te₂O₁₀, were synthesized via a transport reaction in sealed evacuated silica tubes. The compound crystallizes in the triclinic system (space group P). The Ni atoms are positioned in the 1c position on the inversion centre, while the V and Te atoms are in general positions 2i. The crystal structure is layered, the building units within a (010) layer being distorted VO₆ octahedra and NiO₆ octahedra. The metal–oxide layers are connected by distorted TeO₄E square pyramids (E being the 5s² lone electron pair of Te^IV) to form the framework. The structure contains corner‐sharing NiO₆ octahedra, corner‐ and edge‐sharing TeO₄E square pyramids, and corner‐ and edge‐sharing VO₆ octahedra. NiV₂Te₂O₁₀ is the first oxide containing all of the cations Ni^II, V^V and Te^IV.     

Two hydro­chlorides of 7‐methyl‐3,7,11,17‐tetra­aza­bi­cyclo­[11.3.1]­heptadeca‐1(17),13,15‐triene

The X‐ray structure determinations of the two title com­pounds, namely 7‐methyl‐7,17‐di­aza‐3,11‐diazo­niabi­cyclo[11.3.1]­hep­ta­deca‐1(17),13,15‐triene dichloride monohydrate, C₁₄H₂₆N₄²⁺·2Cl^?·H₂O, (I), and 7‐methyl‐17‐aza‐3,7,11‐triazo­niabi­cyclo­[11.3.1]­heptadeca‐1(17),13,15‐triene 2.826‐chloride 0.174‐nitrate, C₁₄H₂₇N₄³⁺·2.826Cl^?·0.174NO₃^?, (II), are re­ported. Protonation occurs at the secondary amine N atoms in (I) and at all three amine N atoms in (II) to which the Cl^? ions are linked via N—H?Cl hydrogen bonds. The macrocyclic hole is quite different in both structures, as is observed by comparing particularly the N3?N4 distances [2.976 (4) and 4.175 (4) Å for (I) and (II), respectively]. In (II), a Cl^? ion alternates with an NO₃^? ion in a disordered structure.     

μ‐Aqua‐penta­aqua­[μ‐3,6‐bis(6‐methyl‐2‐pyridyl)­pyridazine]­chloro­dinickel(II) trichloride trihydrate

The title compound, μ‐aqua‐1:2κ²O‐penta­aqua‐1κ²O,2κ³O‐μ‐3,6‐bis(6‐methyl‐2‐pyridyl)­pyridazine‐1κ²N¹,N⁶:2κ²N²,N³‐chloro‐1κCl‐dinickel(II) trichloride trihydrate, [Ni₂Cl(C₁₆H₁₄­N₄)(H₂O)₆]Cl₃·3H₂O, consists of two Ni^II atoms, a 3,6‐bis(6‐methyl‐2‐pyridyl)­pyridazine mol­ecule, four Cl atoms and nine water mol­ecules. The two Ni atoms are octahedrally coordinated by N and Cl atoms, and by water mol­ecules, and the three six‐membered rings, a pyridazine and two picolines, are planar to within 0.181 (3) Å. The crystal structure is stabilized by an intra‐ and intermolecular hydrogen‐bonding scheme involving water–water and water–chlorine interactions.     

The addition‐reaction product of 1,1,1,4,4,4‐hexa­chloro‐1,4‐disila­butane with N‐methyl­imidazole

The product of the addition reaction of 1,1,1,4,4,4‐hexa­chloro‐1,4‐disila­butane with N‐methyl­imidazole is μ‐ethyl­ene‐C¹:C²‐bis­[di­chloro­tris(1‐methyl­imidazole‐N³)­silicon(IV)] dichloride, C₂₆H₄₀Cl₄N₁₂Si₂²⁺·2Cl^?. Two of the six Cl atoms are replaced by aromatic nitro­gen bases and the coordination sphere of silicon is extended from four to six. The mol­ecule is located on a crystallographic centre of inversion. The environment around the Si atom can be described as a slightly distorted octahedron with the Cl atoms occupying axial positions and the three N‐methyl­imidazole ligands and the ethyl­ene bridge in the equatorial plane.     

Ag2Hg2(TeO4)3

Red single crystals of disilver(I) dimercury(II) tris­[tetra­oxo­tellurate(VI)], Ag₂Hg₂(TeO₄)₃, were obtained under hydro­thermal conditions at 523 K. The structure is built up of _∞¹[(TeO_2/1O_4/2)({TeO_2/1O_2/2}₂O_4/2)] chains, with an overall composition [TeO₄]²⁻, that run parallel to the crystallographic a axis. Distorted AgO₆ and HgO₆ polyhedra (the latter with two short and nearly collinear Hg—O bonds) link the tellurate chains into a three‐dimensional network. Except for one Te atom situated on an inversion center, all atoms occupy general positions.     

(2‐Hydroxy­ethyl)­hydrazinium(2+) dichloride

The crystal structure of the title compound, C₂H₁₀N₂O²⁺·2Cl⁻, is built up from one 2‐hydroxy­ethyl­hydrazinium(2+) cation and two Cl⁻ anions. The mol­ecular structure is stabilized by O—H⋯Cl and N—H⋯Cl hydrogen bonds. The crystal structure is stabilized by one N—H⋯O and three N—H⋯Cl inter­actions, and the three‐dimensional network of hydrogen bonds stabilizes the crystal packing. All five hydrazinium H atoms are involved in hydrogen bonds to Cl⁻ anions. The Cl⋯H contact distances range from 2.122 (15) to 2.809 (14) Å.     

Barium divanadium(V) tellurite(IV)

A new three‐dimensional bimetallic tellurite, BaV₂TeO₈, was synthesized by the hydro­thermal reaction of Ba(OH)₂, TeO₂ and V₂O₅, and characterized by single‐crystal X‐ray diffraction. The three‐dimensional framework is built up from anionic [V₂TeO₈]_n²ⁿ⁻ layers parallel to (101) and connected via Ba—O bonds. The anionic layers are formed by three types of polyhedra, namely VO₅ tetra­gonal pyramids, VO₄ tetra­hedra and TeO₄₊₂ `folded square' polyhedra.     

Chloro­di­methyl(N‐methyl­pyrrolidin­one)­tin(IV)‐μ‐chloro‐di­chloro­di­methyl­tin(IV)

The synthesis and the X‐ray structural analysis of the title compound, μ‐chloro‐1:2κ²Cl‐tri­chloro‐1κCl,2κ²Cl‐tetra­methyl‐1κ²C,2κ²C‐(N‐methyl­pyrrolidin‐2‐one)‐1κO‐ditin(IV), [Sn₂Cl₄(CH₃)₄(C₅H₉NO)], are described. The title compound is found to exhibit a distorted trigonal–bipyramidal geometry at both Sn^IV atoms. The Sn—Cl—Sn angle involving the bridging chlorine ligand is 135.56 (5)°, with the Sn—Cl bond lengths being 2.5704 (13) and 3.1159 (13) Å.     

A trichloro‐bridged binuclear ruthenium complex with 1,1,1‐tris(diphenylphosphinomethyl)ethane

The tri­chloro‐bridged dinuclear Ru^II complex tri‐μ‐chloro‐bis{[1,1,1‐tris­(di­phenyl­phosphino­methyl)­ethane‐κ³P,P′,P′′]ruthenium(II)} hexa­fluoro­phosphate ethanol solvate, [Ru₂Cl₃(tripod)₂]PF₆·C₂H₆O, containing the tripod [1,1,1‐tris­(di­phenyl­phosphino­methyl)­ethane, C₄₁H₃₉P₃] ligand, was unexpectedly obtained from the reaction of [Ru^IIICl₃(tripod)] with 1,4‐bis­(di­phenyl­phosphino)­butane (dppb), followed by pre­cipitation with NH₄PF₆. The magnetic moment of the compound at room temperature indicates that the dinuclear [Ru₂(μ‐Cl)₃(tripod)₂]⁺ cation is diamagnetic. A single‐crystal X‐ray structure determination revealed that the two Ru atoms are bridged by the three Cl atoms. The coordination sphere of each Ru atom is completed by the three P atoms of a tripod ligand. The two P₃Ru units are exactly eclipsed, while the bridging Cl atoms are staggered with respect to the six P atoms. The Ru⋯Ru distance is 3.3997 (7) Å and the mean Cl—Ru—Cl bond angle is 77.7°.     

Protonation products of pentaaminopentane as novel building blocks for hydrogen‐bonded networks

The structures of 3‐amino‐1,2R,4S,5‐tetra­ammoniopentane tetrachloride monohydrate, C₅H₂₁N₅⁴⁺·4Cl^?·H₂O, and 1,2R,3,4S,5‐penta­ammoniopentane tetra­chloro­zincate tri­chlor­ide monohydrate, (C₅H₂₂N₅)[ZnCl₄]Cl₃·H₂O, have been determined from single‐crystal X‐ray diffraction data. Both compounds show a complex network of N—H?O, O—H?Cl and N—H?Cl hydrogen bonds. There are a total of 14 H atoms of the tetra‐cation and 15 H atoms of the penta‐cation available for hydrogen bonding. However, due to the particular shape of the primary linear poly­ammonium cations, only a certain number of H atoms can be involved in hydrogen‐bond formation. It is further shown that hydrogen bonding has an influence on the conformation of such alkyl­ammonium cations.     

Bis­[hydrogen 1,1′‐bis­(di­phenyl­phos­phinato)­ferrocenium] octa­chloro­diantimony(III)

In the title compound, [Fe(C₃₄H₂₉O₂P₂)]₂[Sb₂Cl₈], the discrete centrosymmetric [Sb₂Cl₈]^2? anions are formed from two edge‐shared square pyramids of Cl atoms about each Sb atom. Within the cation, the two di­phenyl­phosphinate groups share one H atom and the ferrocene cyclo­penta­dienyl rings are in a staggered conformation, with the average value of the twist angle being 46°. In the crystal, each [Sb₂Cl₈]^2? anion is involved in eight C—H?Cl interactions with four surrounding cations and these interactions interconnect the ions to form molecular columns along the a direction.     

Bis(2,2‐bi­pyridine‐N,N′)tetra‐μ‐chloro‐tetracopper(I)

A novel centrosymmetric chair‐like dimer, bis(2,2′‐bi­pyridine)‐1κ²N,N′;3κ²N,N′‐tetra‐μ‐chloro‐1:2κ²Cl;­2:3κ²Cl;­3:4κ²Cl;1:4κ²Cl‐tetra­copper(I), [Cu₄Cl₄­(C₁₀­H₈­N₂)₂], has been solvothermally synthesized and structurally characterized. The complex self‐assembles into a three‐dimensional network via C—H?Cl hydrogen bonds, π–π stacking and weak Cu?Cl electrostatic interactions.     

Tetrameric indium trichloride,a new modification of a widely used compound

The title compound, hexa‐μ‐chloro‐1:2κ⁴Cl;2:3κ⁴Cl;3:4κ⁴Cl‐hexachloro‐1κ²Cl,2κCl,3κCl,4κ²Cl‐hexakis­(diethyl­amine)‐1κ²N,2κN,3κN,4κ²N‐tetraindium(III), [(InCl₃)₄(Et₂NH)₆] or [In₄Cl₁₂(C₄H₁₁N)₆], lies about an inversion centre and consists of four octahedrally coordinated In centres linked by bridging Cl atoms to form three four‐membered In₂Cl₂ rings.