Di‐μ‐phenyl­thio‐bis­[bis(η5‐methyl­cyclo­penta­dienyl)(tetra­hydro­furan)lanthanum(III)] bis­(tetra­hydro­furan) solvate

The title complex, [La₂(C₆H₇)₄(C₆H₅S)₂(C₄H₈O)₂]·2C₄H₈O, is a centrosymmetric dimer bridged through the S atoms of the benzene­thiolate ligands. The bridging La₂S₂ unit is completely planar, while the geometry around the nine‐coordinate La atom is that of a distorted trigonal bipyramid. The La—S—La and S—La—S angles are 117.51 (4) and 62.5 (1)°, respectively, and the average La—S bond length is 2.9759 Å. The crystals contain two tetra­hydro­furan solvate mol­ecules for every complex mol­ecule.     

The first compound with an unusual type of anion, [Li(SR)2]–: bis­(μ2‐aqua‐d2)tetra­kis(aqua‐d2)dilithium(I) bis­[bis­(tri‐tert‐butoxy­silanethiol­ato‐κ2O,S)lithate(I)] dihydrate‐d2

The title complex, [Li₂(D₂O)₆][Li(C₉H₂₇SSiO₃)₂]₂·2D₂O, is the first compound with an S—M bond (M = alkali metal) within an unusual type of lithate anion, [Li(SR)₂]⁻ {where R is Si[OC(CH₃)₃]₃}. There is a centre of symmetry located in the middle of the Li₂O₂ ring of the cation. All Li atoms are four‐coordinate, with LiO₄ (cations) and LiO₂S₂ (anions) cores. The singly charged [Li(SR)₂]⁻ anions are well separated from the doubly charged [Li₂(D₂O)₆]²⁺ cations; the distance between Li atoms from differently charged ions is greater than 5 Å. Both ion types are held within an extended network of O—D⋯O and O—D⋯S hydrogen bonds.     

catena‐Poly[bis­(tert‐butyl­ammonium) [plumbate(II)‐tri‐μ‐iodo] iodide dihydrate]

The title compound, {(C₄H₁₂N)₂[PbI₃]I·2H₂O}_n, crystallizes as an organic–inorganic hybrid. The six‐coordinate Pb atom lies on a centre of inversion and all the I atoms lie on mirror planes; the two independent cations both lie across mirror planes. The structure contains anionic chains along [100] of fused [PbI₃]⁻ units forming face‐sharing octa­hedra. Four cations enclose channels occupied by isolated iodide ions and water mol­ecules of hydration.     

Tri‐μ2‐chloro‐tetra­chloro‐μ3‐oxo‐hexakis­(tetra­hydro­furan‐κO)­dititanium(III)­samarium(III): a novel trinuclear Sm–Ti mixed species

In the title compound, [SmTi₂Cl₇O(C₄H₈O)₆], the metal ions are linked by a central μ₃‐oxo ion and by three μ₂‐chloro ions, giving a planar moiety containing a binary crystallographic axis. The coordination spheres are completed by terminal chloro ligands and tetra­hydro­furan mol­ecules, with resulting pentagonal bipyramidal and octahedral environments for the Sm and Ti atoms, respectively.     

catena‐Poly[[aqua­barium(II)]‐μ‐aqua‐bis­(μ‐2′‐carboxy­biphenyl‐2‐carboxyl­ato)]

In the title compound, [Ba{HOOC(C₆H₄)₂CO₂}₂(H₂O)₂] or [Ba(C₁₄H₉O₄)₂(H₂O)₂], the Ba atoms are coordinated by nine O atoms, six from two 2′‐carboxy­biphenyl‐2‐carboxyl­ate (Hbpdc⁻) ligands and three from three coordinated water mol­ecules, resulting in the formation of face‐sharing distorted monocapped square anti­prisms. The Hbpdc⁻ ligands bridge the Ba atoms to form a one‐dimensional helical polymer, with a Ba⋯Ba distance across the chain of 4.1386 (17) Å. Adjacent chains are parallel to each other. The two independent ligands are tetra­dentate and have the same coordination mode, exhibiting μ‐oxo bridges and η⁸‐chelation. The crystal structure is further stabilized by hydrogen bonds within each chain.     

(Tetra­hydro­furan)­potassium mer‐trans‐tris­(carbazolyl)­di­chloro(tetra­hydro­furan)­zirconate

In the title compound, [K(C₄H₈O)][ZrCl₂(C₁₂H₈N)₃(C₄H₈O)], the Zr atom is pseudo‐octahedral, with two Cl ligands in trans positions. There is extensive interaction between the potassium cation and two of the aromatic carbazolyl ligands in η⁶ [C⃛K = 3.167 (3)–3.331 (3) Å] and η² [C⃛K = 3.147 (3)–3.268 (2) Å] fashions.     

Poly[diaqua­(μ‐4,4′‐bipyridine)tetra­kis­(μ‐ferro­cenecarboxyl­ato)bis­(ferro­cenecarboxyl­ato)­tri­man­ganese(II)]

The title compound, [Mn₃Fe₆(C₅H₅)₆(C₆H₄O₂)₆(C₁₀H₈N₂)(H₂O)₂]_n, consists of two crystallographically unique Mn^II centers. One is situated on an inversion center and is octa­hedrally coordinated by two N atoms from two bridging 4,4′‐bipyridine (4,4′‐bipy) ligands and four O atoms, two from different bridging ferrocenecarboxyl­ate (μ₂‐FcCOO⁻; Fc is ferrocene) units and two from aqua ligands. The two halves of each 4,4′‐bipy ligand are related by a center of symmetry. The second Mn^II center is in a strongly distorted tetra­gonal–pyramidal geometry, coordinated by five O atoms, three from three μ₂‐FcCOO⁻ units and two from a fourth, chelating, η²‐FcCOO⁻ unit. The FcCOO⁻ units function as bridging ligands to adjacent Mn^II centers, leading to the formation of linear ⋯Mn1Mn2Mn2Mn1⋯ chains. Adjacent chains are further bridged by 4,4′‐bipy ligands, resulting in a two‐dimensional layered polymer.     

Di­chloro­bis­(di­benzyl­amino)­bis­(tetra­hydro­furan)­zirconium(IV) toluene hemisolvate

The title complex, [ZrCl₂(C₄H₈O)₂(C₁₄H₁₄N)₂]·0.5C₇H₈, was prepared in an unusual manner by utilizing [Mg{N(CH₂Ph)₂}₂] as a ligand transfer reagent. The Zr atom lies in a distorted octahedral environment where steric repulsion from the large di­benzyl­amino ligands leads to a widening of the N—Zr—N angle [99.95 (9)°] and corresponding compression of other angles [Cl—Zr—Cl 160.95 (3)° and O—Zr—O 78.22 (7)°]. This distortion is compared with those found in the previously determined structures of the di­methyl­amino and diethyl­amino analogues.     

catena‐Poly[[tetra­aqua­manganese(II)]‐μ‐4‐(carboxyl­ato­methyl­sulfanyl)­phenoxy­acetato]

The title compound, [Mn(C₁₀H₈O₅S)(H₂O)₄]_n, a one‐dimensional manganese(II) complex comprising helical chains bridged by 4‐(carboxylatomethylsulfanyl)phenoxyacetate ligands has been characterized by single‐crystal X‐ray diffraction analysis. Hydrogen‐bonding inter­actions between adjacent chains extend the complex into a three‐dimensional supra­molecular architecture.     

μ‐Oxo‐bis­[(2,3,12,13‐tetra­bromo‐5,10,15,20‐tetra­phenyl­porphyrinato)­iron(III)] bis­(di­chloro­methane) solvate

The precise structure of the title compound, [Fe₂O(C₄₄H₂₄Br₄N₄)₂]·2CH₂Cl₂, is reported. The Fe—N distances are non‐equivalent in pairs because of the asymmetric peripheral substitution; the values are 2.098 Å to the brominated rings and 2.041 Å to the other two rings. The Fe—O bond distance is 1.7583 (4) Å. The mol­ecule has required twofold symmetry so that there is one unique porphyrin macrocycle and one Fe—O bond length in contrast to a previous report on the same species.     

One‐dimensional structure of catena‐poly[tetra­ethyl­ammonium [tetra­cyano­iron(III)‐μ‐cyano‐[bis­(ethyl­ene­diamine)­cadmium(II)]‐μ‐cyano] tetra­hydrate]

The title compound, {(C₈H₂₀N)[CdFe(CN)₆(C₂H₈N₂)₂]·4H₂O}_n, was isolated from the aqueous system Cd²⁺/ethyl­ene­diamine (en)/[Fe(CN)₆]³⁻ in the presence of [Et₄N]Br. The crystal structure is dominated by a one‐dimensional motif, viz. a negatively charged 2,2‐CT (cis–trans) [–Cd(en)₂—NC—Fe(CN)₄—CN–]_nⁿ⁻ chain. The Cd and Fe atoms of the anion and the N atom of the cation all lie on twofold axes. The ethyl groups of the cation are equally disordered over two orientations. The cationic building block of the chain consists of a Cd^II atom coordinated by two chelating en ligands, and the distorted octa­hedral coordination is completed by two bridging cyano ligands in cis positions. The anionic building block is an [Fe(CN)₆]³⁻ anion in which the Fe^III atom is octa­hedrally coordinated by six cyano ligands; two of the cyano ligands, in trans positions, are bridging. The uncoordinated water mol­ecules link neighbouring chains through O—H⋯N and N—H⋯O hydrogen bonds.     

catena‐Poly[bis­[(1,10‐phenanthro­line)nickel(II)]‐μ‐3,6‐dicarboxy­cyclo­hexane‐1,2,4,5‐tetra­carboxyl­ato]

In the title compound, [Ni₂(C₁₂H₈O₁₂)(C₁₂H₈N₂)₂]_n, the 3,6‐dicarboxy­cyclo­hexane‐1,2,4,5‐tetra­carboxyl­ate (H₂chhc⁴⁻) anion has crystallographically imposed C₂ symmetry and bridges the six‐coordinate Ni atoms to generate polymeric [Ni₂(H₂chhc)_2/2(C₁₂H₈N₂)₂] chains extending in the [010] direction. The coordination polymer chains are linked into a three‐dimensional framework by O—H⋯O and C—H⋯O hydrogen bonds.     

catena‐Poly[sodium(I)‐μ‐tetra­ethoxy­borato]

The title compound, [Na(C₈H₂₀BO₄)]_n, has twofold crystallographic symmetry, with the Na⁺ cations bound by four O atoms [Na—O = 2.251 (3) Å]. The tetra­ethoxy­borate anion acts as a bridging ligand to form one‐dimensional polymers running along the twofold crystal axis. The crystal was treated as a racemic twin.     

Di­bromo­tetra‐μ3‐methoxo‐di‐μ2‐methoxo‐hexakis­(tetra­hydro­furan‐d8)­tetramagnesium

The crystal structure of the title compound, [Mg₄Br₂(CH₃O)₆(C₄D₈O)₆], consists of discrete mol­ecules with imposed symmetry C_i. The tetranuclear compound exhibits two crystallographically independent Mg atoms having distorted octahedral and trigonal–bipyramidal ­coordination spheres. The Mg atoms are bridged by two μ₃‐OMe and four μ₂‐OMe ligands, and their coordination is completed by two terminal Br and six tetra­hydro­furan ligands.     

Bis(μ‐2‐amino­pyridine)­bis­[(tri­fluoro­acetato)silver(I)]

The title compound, [Ag₂(C₂F₃O₂)₂(C₅H₆N₂)₂], is a dinuclear Ag^I complex with inversion symmetry. Each Ag atom is three‐coordinated by two N atoms from two different 2‐amino­pyridine ligands and by one O atom from a tri­fluoro­acetate anion, giving an approximately trigonal coordination environment. In the crystal packing, mol­ecules are connected by N—H⋯O and N—H⋯F hydrogen bonds, forming layers parallel to the (001) plane.     

Chloro­(μ‐6‐methyl­pyridine‐2‐carboxyl­ato)bis­(6‐methyl­pyridine‐2‐carboxyl­ato)triphenyl­chromium(III)­tin(IV) chloro­triphenyl­tin(IV)

The title compound, [CrSn(C₆H₅)₃(C₇H₆NO₂)₃Cl][Sn(C₆H₅)₃Cl(CH₄O)], was obtained from the reaction of Ph₃SnCl with the complex [Cr(C₇H₆NO₂)₃] in methanol. The structure contains [Ph₃SnCl(MeOH)] (A) and [Ph₃SnClCr(C₇H₆NO₂)₃] (B) mol­ecules. In mol­ecule A, the Sn atom of Ph₃SnCl is coordinated by one methanol mol­ecule. In mol­ecule B, the Sn atom of Ph₃SnCl is coordinated by one carboxyl­ate O atom of [Cr(C₇H₆NO₂)₃]. Mol­ecules A and B are connected through an O—H⋯O hydrogen bond between a carboxyl­ate O atom and the methanol OH group. Weak C—H⋯Cl inter­actions and O—H⋯O hydrogen bonds extend the components of (I) into a two‐dimensional network.     

Di‐μ‐benzoato‐bis­[di­carbonyl­(pyri­dine)­ruthenium(I)] (new polymorph) and di‐μ‐tri­fluoro­acetato‐bis­[di­carbonyl­(pyridine)­ruthenium(I)]

The syntheses and crystal structure determinations of a pair of `sawhorse' dimers are reported, viz. [Ru₂(C₆H₅CO₂)₂(C₅H₅N)₂(CO)₄] [a new polymorph, cf. Kepert, Deacon, Spiccia, Fallon, Skelton & White (2000). J. Chem. Soc. Dalton Trans. pp. 2867–2874] and [Ru₂(CF₃CO₂)₂(C₅H₅N)₂(CO)₄]. The Ru⋯Ru distances are 2.6724 (2) and 2.7122 (5) Å, respectively.     

catena‐Poly­[[bis­(nitrato)(pyrimidine)­copper(II)]‐μ‐pyrimidine‐N:N′]

The title compound, [Cu(NO₃)₂(C₄H₄N₂)₂]_n, crystallizes as a linear polymeric compound with one pyrimidine ligand bridging between two Cu^II atoms and a second pyrimidine ligand coordinated in a monodentate manner. The distorted octahedral geometry around the Cu^II atom consists of two pyrimidine N atoms at distances of 2.033 (4) and 2.025 (4) Å, and two nitrate O atoms at distances at 1.987 (3) and 1.973 (3) Å. The apical positions are occupied by an N atom of a bridging pyrimidine ligand [2.291 (4) Å] and a nitrate O atom at a long distance of 2.781 (3) Å. The basal plane is almost planar, with trans angles of 176.23 (14) and 165.34 (15)°.     

Poly[tetra­aquadi‐μ3‐malonato‐cobalt(II)­calcium(II)]

The structure of the polymeric title compound, [CaCo(C₃H₂O₄)₂(H₂O)₄]_n, consists of CaO₈ and CoO₆ polyhedra linked together by malonate groups. The Co atom lies on a centre of symmetry in an octa­hedral arrangement, and is coordinated by four malonate O atoms in a planar arrangement and two water mol­ecules in a trans conformation. The geometry around the Ca atom, which lies on a twofold axis, may be described as a distorted square anti­prism, which involves two water mol­ecules and six malonate O atoms. The Co—O and Ca—O bond lengths are in the ranges 2.0711 (12)–2.1004 (14) and 2.3775 (12)–2.6329 (12) Å, respectively.