fac‐Tri­carbonyl(4,4′‐di­methyl‐2,2′‐bi­pyridine)­tri­phenyl­tin(II)­rhenium(I)

The title organometallic compound, fac‐tri­carbonyl‐2κ³C‐(4,4′‐di­methyl‐2,2′‐bi­pyridine)‐2κ²N,N′‐tri­phenyl‐1κ³C¹‐tin(II)­rhenium(I)(Sn—Re), [ReSn(C₆H₅)₃(C₁₂H₁₂N₂)(CO)₃], con­tains three unique π–π stacking interactions. The result is an infinite chain of uninterrupted alternating intra‐ and intermolecular offset π–π stacking interactions throughout the crystal lattice. This extended π–π stacking arrangement, and an additional isolated intramolecular π–π interaction between the remaining 4,4′‐di­methyl‐2,2′‐bi­pyridine ring and a second phenyl group, impose geometric constraints on the Re and Sn atoms, yielding distorted octahedral and tetrahedral coordinations, respectively, for the metal centers.     

Bis­(di‐μ‐acetato‐aqua{2‐[N‐ethyl‐N‐(2‐hydroxy‐4‐methyl­benzyl)­amino­methyl]‐1‐methyl­benz­imid­az­ole}­nickel)­nickel(II) tetra­hy­drate

The previously unknown title compound, tetra‐μ‐ace­tato‐1:2κ²O;1:2κ²O:O′;­2:3κ²O;­2:3κ²O:O′‐di­aqua‐1κO,3κO‐bis­(μ‐2‐{[N‐ethyl‐N‐(2‐hy­droxy‐5‐methylbenzyl)­am­ino]­methyl}‐1‐methyl‐1H‐benz­imid­az­ole)‐1κ³N³,N,O:2κO;3κ³N³,N,O:2κO‐tri­nickel(II) tetra­hy­drate, [Ni₃(C₁₈H₂₂N₃O)₂(C₂H₃O₂)₄(H₂O)₂]·­4H₂O, (I), is a centrosymmetric linear trinuclear nickel(II) complex, where the Ni atoms are in an octahedral coordination and the ligand heteroatoms act so as to model amino acid residues.     

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.     

Di­aqua­bis(4,5‐di­hydro‐1,2,4‐triazolo[1,5‐a]­pyrimidin‐5‐one‐N3)bis­(thiocyanato‐N)­nickel(II)

The title compound, [Ni(NCS)₂(C₅H₄N₄O)₂(H₂O)₂], crystallizes in the triclinic space group P. The molecular unit contains two neutral mol­ecules of 4,5‐di­hydro‐1,2,4‐triazolo[1,5‐a]­pyrimidin‐5‐one (5HtpO) coordinated through the N atom in position 3, two thio­cyanate ligands coordinated through their N atoms and two water mol­ecules completing an octahedral environment around the Ni^II ion, which lies on a centre of inversion. The structure is stabilized by hydrogen bonding. Distances in the coordination sphere are Ni—N3(5HtpO) 2.132 (2), Ni—O(water) 2.085 (2) and Ni—N(thio­cyanato) 2.040 (2) Å.     

A zigzag‐type one‐dimensional coordination polymer formed by (2,2‐di­methyl‐1,3‐propane­di­amine)­bis­(iso­nico­tin­ato)­platinum(II) and copper nitrate

The title compound, catena‐poly­[[[tri­aqua‐2κ³O‐(2,2‐dimethyl‐1,3‐propane­di­am­ine)‐1κ²N,N′‐μ‐isonicotinato‐1:2κ²N:O‐copper(II)­plati­num(II)]‐μ‐isonicotinato‐2:1′κ²O:N] dinitrate], {[CuPt(C₆H₄NO₂)₂(C₅H₁₄N₂)(H₂O)₃](NO₃)₂}_n, obtain­ed from equimolar (dmpda)Pt^II(isonic)₂ (where dmpda is 2,2‐di­methyl‐1,3‐propane­di­amine and isonic is isonicotinate) and copper(II) nitrate, has been found to be a one‐dimensional coordination polymer of the zigzag‐type.     

Polymeric μ‐cyano‐di­cyano­nickelate(II)‐μ‐cyano‐trans‐bis­[N‐(2‐hydroxyethyl)ethyl­enedi­amine]­cadmium(II)

The title compound, catena‐poly­[[μ‐cyano‐1:2κ²C:N‐di­cyano‐1κ²C‐trans‐bis­[N‐(2‐hydroxy­ethyl)­ethane‐1,2‐di­amine‐2κ²N,N′]­cadmium(II)­nickel(II)]‐μ‐cyano‐1:2′κ²C:N], [CdNi(CN)₄(C₄H₁₂N₂O)₂], consists of alternating square‐planar Ni(CN)₄ fragments, formally dianionic, and Cd(hydet‐en)₂ moieties [hydet‐en is N‐(2‐hydroxy­ethyl)­ethyl­ene­di­amine], with the two bridging cyanide ligands in a mutually trans disposition at the Ni atom and cis at the Cd atom. The resulting one‐dimensional zigzag chain structure has the Ni atom on an inversion center, while the distorted octahedron centered on the Cd atom lies on a twofold axis. The polymer chains are connected into undulating sheets by weak interchain N—H⋯N, N—H⋯O and O—H⋯N hydrogen bonds, which are also present between successive sheets.     

cis‐[1,4‐Bis(di­phenyl­phosphino)­butane](μ‐tetra­thio­tungstato)­palladium(II) N,N′‐di­methyl­form­amide hemisolvate hemihydrate

In the title compound, [1,4‐bis(di­phenyl­phosphino)­butane‐2κ²P,P′]­di‐μ‐thio‐1:2κ⁴S‐di­thio‐1κ²S‐palladium(II)­tung­sten(VI) N,N′‐di­methyl­form­amide hemisolvate hemihydrate, [PdWS₄­(C₂₈H₂₈P₂)]·0.5C₃H₇NO·0.5H₂O, the Pd atom is coordinated by two S atoms from the distorted‐tetrahedral [WS₄]²⁻ anion and two P atoms from the dppb mol­ecule [dppb is 1,4‐bis(di­phenyl­phos­phino)­butane] in an approximately square‐planar configuration. A puckered seven‐membered ring is formed by the Pd atom and the dppb ligand.     

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.     

catena‐Poly­[[tetrakis­[μ‐(3‐methoxy­phenyl)­acetato‐O:O′]­dicopper(II)]‐μ‐2‐aminopyrimidine‐N1:N3]

The structure of the title compound, [Cu₂(C₉H₉O₃)₄(C₄H₅N₃)], comprises a zigzag polymer of alternating tetrakis­(carboxyl­ato‐O:O′)­dicopper(II) and 2‐amino­pyrimidine units linked by axial Cu—N bonds, and the non‐centrosymmetric structure has four unique (3‐methoxy­phenyl)­acetate moieties.     

Bis­(tetra‐n‐butyl­ammonium) bis[(mandelato)­oxo­(peroxo)­vanadate(V)] mandelic acid solvate

The crystal structure of the title complex, bis­(tetra‐n‐butyl­ammonium) bis(‐‐hydroxy­benzene­acetato)‐1κ²O¹,O²:2κO²;1κO²:2κ²O¹,­O²‐bis­[oxo­(peroxo)­vanadium(V)] α‐hydroxy­benzene­acetic acid solvate, (C₁₆H₃₆N)₂­[V₂O₂(O₂)₂(C₈H₆O₃)₂]·C₈H₈O₃, consists of dimeric anions with twofold rotation symmetry, cations and mol­ecules of mandelic acid. Deprotonated hydroxyl O atoms of the mandelate dianion ligands bridge the V atoms to give a non‐planar V₂O₂ ring. Each V atom has distorted pentagonal pyramidal coordination geometry, with an oxo ligand in the axial position. The mandelic acid mol­ecule is disordered and coordinates weakly to the second axial site of each V atom through a carboxyl­ate O atom.     

Penta­chloro‐1,3,6‐tris­(diethyl­phenyl­phosphino)­dirhenium(II,III)

The title complex [systematic name: penta­chloro‐1κ³Cl,2κ²Cl‐tris(diethylphenylphosphino)‐1κP,2κ²P‐dirhenium(II,III)(Re—Re)], 1,3,6‐Re₂Cl₅(PEt₂Ph)₃ or [Re₂Cl₅(C₁₀H₁₅P)₃], consists of dirhenium mol­ecules with eclipsed structures similar to those of previously characterized 1,3,6‐Re₂Cl₅(PR₃)₃ compounds. The Re—Re bond distance is 2.2262 (3) Å and the metal–metal bond order is 3.5.     

A novel Na–O–Ni–O–Ni bridging complex of Cl‐HXTA,where Cl‐HXTA is 2,6‐bis{[bis­(carboxyl­ato­methyl)­amino]­methyl}‐4‐chloro­phenolate

In the structure of the title compound, hepta­aqua‐1κ³O,2κ²O,3κ²O‐(μ₃‐2,6‐bis{[bis­(carboxyl­ato­methyl)­amino]methyl}‐4‐chloro­phenolato‐1κO;2κ⁴O,O′,N,O¹;3κ⁴O¹N′,O′′,O′′′)dinickel(II)­sodium(I) pentahydrate, [NaNi₂(C₁₆H₁₄ClN₂O₉)(H₂O)₇]·5H₂O or [Ni₂(Cl‐HXTA)(H₂O)₄{Na(H₂O)₃}]·5H₂O, the trinuclear complex unit consists of two distorted NiNO₅ octahedra bridged by a phenolate O atom and an NaO₄ tetrahedron bridged to one of the Ni octahedra by a carboxylate O atom. There are four intramolecular hydrogen bonds forming four six‐membered rings in the complex and the complex mol­ecules are connected to each other by a very complicated hydrogen‐bond network.     

20‐Di­cyano­methyl­ene‐5,8,11,14‐tetraoxa‐2,17‐di­thia­bi­cyclo­[16.4.1]­tricosa‐1(23),18,21‐triene and its mercury(II) dichloride complex

The structures of the title compound, C₂₀H₂₄N₂O₄S₂, and its mercury(II) dichloride complex, dichloro{20‐di­cyano­methyl­ene‐5,8,11,14‐tetraoxa‐2,17‐di­thia­bi­cyclo­[16.4.1]­tricosa‐1(23),18,­21‐tri­ene‐κ⁴O,κS¹⁷}mercury(II), [HgCl₂(C₂₀­H₂₄­N₂­O₄­S₂)], have been determined by X‐ray crystallographic analyses. The mercury(II) dichloride complex has two independent mol­ecules of [HgCl₂(C₂₀H₂₄N₂O₄S₂)] in the lattice. The mercury(II) ion has pentagonal bipyramidal coordination which involves one S atom, four O atoms and two Cl^? ions.     

1,2‐Di­cyano‐1,2‐bis­(imidazolidine‐2‐thione)­digold(I) and 2,2‐di­cyano‐1,1‐bis­(di­methyl­thio­urea)­digold(I)

Gold(I) cyanide forms complexes with imidazolidine‐2‐thione (etu) and di­methyl­thio­urea (dmtu) with the formula [Au₂(CN)₂L₂], i.e. the title complexes di­cyano‐1κC,2κC‐bis(imidazolidine‐2‐thione)‐1κS,2κS‐digold(I)(Au—Au), [Au₂(CN)₂(C₃H₆N₂S)₂], and di­cyano‐1κ²C‐bis(N,N′‐di­methyl­thio­urea)‐2κ²S‐digold(I)(Au—Au), [Au₂(CN)₂(C₃H₈N₂S)₂]. In the etu complex, two approximately linear (etu)AuCN groups are held together by a weak homopolar Au—Au bond [3.117 (1) Å], with a torsion angle of 61 (3)° between the two groups. In the dmtu complex, an approximately linear Au(dmtu)₂ group is bound to an approximately linear Au(CN)₂ group by a weak heteropolar Au—Au bond [3.091 (1) Å], with a torsion angle of 83 (5)° between the two groups.     

Azido­[1,1′‐bis­(di­phenyl­phosphino)­ferrocene](penta­methyl­cyclo­penta­dienyl)­rhodium(III) hexa­fluoro­phosphate

In the title compound, azido‐2κN‐bis­[μ‐(1η⁵:2κP)‐di­phenyl­phosphino­cyclo­penta­dienyl][2(η⁵)‐penta­methyl­cyclo­penta­di­enyl]­iron(III)­rhodium(III) hexa­fluoro­phosphate, [{Rh(C₁₀H₁₅)(N₃)}{Fe(μ‐C₁₇H₁₄P)₂}]PF₆ or [FeRh(C₁₀H₁₅)(μ‐C₁₇H₁₄P)₂(N₃)]PF₆, the coordination sphere of Rh^III can be described as pseudo‐tetrahedral, composed of two P atoms from a 1,1′‐bis­(di­phenyl­phosphino)­ferrocene (dppf) ligand, an azido N atom and the centroid of the ring of a C₅Me₅ (Cp*) ligand. The two cyclo­penta­dienyl rings in the dppf moiety adopt an eclipsed conformation. The Rh⋯Fe distance is 4.340 (2) Å.     

A chloro(2‐pyridinecarboxaldehyde)(2,2′:6′,2′′‐ter­pyridine)­ruthenium(II) complex

The aldehyde moiety in the title complex, chloro(2‐pyridinecarboxaldehyde‐N,O)(2,2′:6′,2′′‐terpyridine‐κ³N)ruthenium(II)–chloro­(2‐pyridine­carboxyl­ic acid‐N,O)(2,2′:6′,2′′‐ter­pyridine‐κ³N)­ruthenium(II)–perchlorate–chloro­form–water (1.8/0.2/2/1/1), [RuCl­(C₆H₅NO)­(C₁₅H₁₁N₃)]_1.8[RuCl­(C₆H₅­NO₂)(C₁₅H₁₁N₃)]_0.2­(ClO₄)₂·­CHCl₃·­H₂O, is a structural model of substrate coordination to a transfer hydrogenation catalyst. The title complex features two independent Ru^II complex cations that display very similar distorted octahedral coordination provided by the three N atoms of the 2,2′:6′,2′′‐ter­pyridine ligand, the N and O atoms of the 2‐pyridine­carbox­aldehyde (pyCHO) ligand and a chloride ligand. One of the cation sites is disordered such that the aldehyde group is replaced by a 20 (1)% contribution from a carboxyl­ic acid group (aldehyde H replaced by carboxyl O—H). Notable dimensions in the non‐disordered complex cation are Ru—N 2.034 (2) Å and Ru—O 2.079 (2) Å to the pyCHO ligand and O—C 1.239 (4) Å for the pyCHO carbonyl group.     

Di‐μ‐sulfito‐bis­[(4,4′‐di­methyl‐2,2′‐bi­pyridine)­zinc(II)] dihydrate and poly­[[aqua(1,10‐phenanthroline)­zinc(II)]‐μ3‐sulfito‐zinc(II)‐μ3‐sulfito]

Two different zinc sulfite compounds have been prepared through the decomposition of pyrosulfite–­di­thionite ions in aqueous solution, viz. a dimeric complex, di‐μ‐sulfito‐κ³O,O′:O′′;κ³O:O′,O′′‐bis­[(4,4′‐di­methyl‐2,2′‐bi­pyridine‐κ²N,N′)­zinc(II)] dihydrate, [Zn₂(SO₃)₂(C₁₂H₁₂N₂)₂]·2H₂O, (I), which was solved and refined from a twinned sample, and an extended polymer, poly­[[aqua(1,10‐phenanthroline‐κ²N,N′)­zinc(II)]‐μ₃‐sulfito‐κ²O:O′:O′′‐zinc(II)‐μ₃‐sulfito‐κ³O:O:O′], [Zn₂(SO₃)₂(C₁₂H₁₀N₂)(H₂O)]_n, (II). In (I), the dinuclear Zn^II complex has a center of symmetry. The cation is five‐coordinate in a square‐pyramidal arrangement, the anion fulfilling a bridging chelating role. Compound (II) comprises two different zinc units, one being five‐coordinate (square pyramidal) and the other four‐coordinate (trigonal pyramidal), and two independent sulfite groups with different binding modes to the cationic centers.     

[N,N′‐Bis(5‐bromo­salicyl­idene)‐1,3‐di­amino­propane]­nickel(II) and [N,N′‐­bis(5‐chloro­salicyl­idene)‐1,3‐­di­amino­propane]copper(II)

The title compounds, {4,4′‐di­bromo‐2,2′‐[1,3‐propane­diyl­bis(nitrilo­methyl­idyne‐N)]­diphenolato‐O,O′}nickel(II), [Ni(C₁₇­H₁₄­Br₂­N₂O₂)], and {4,4′‐di­chloro‐2,2′‐[1,3‐pro­pane­diyl­bis­(ni­trilo­methyl­idyne‐N)]­di­phen­ol­ato‐O,O′}­copper(II), [Cu­(C₁₇­H₁₄­Cl₂­N₂O₂)], lie on crystallographic twofold axes. In both structures, the metal coordination sphere is a tetrahedrally distorted square plane formed by the four‐coordinate N₂O₂ donor set of the Schiff base imine–phenol ligands. In the Ni compound, the Ni—O and Ni—N distances are 1.908 (3) and 1.959 (4) Å, respectively, while in the Cu compound, the Cu—O and Cu—N distances are 1.907 (2) and 1.960 (2) Å, respectively. The two Schiff base moieties, which themselves are nearly planar, are inclined at an angle of 29.26 (7)° for the Ni compound and 29.26 (5)° for the Cu compound.     

Bis­[1‐(p‐chloro­phenyl)‐5‐iso­propyl­biguanide‐κ2N2,N4]­nickel(II) dichloride di­methyl­form­amide solvate

The asymmetric unit of the title compound, [Ni(C₁₁H₁₆ClN₅)₂]Cl₂·C₃H₇NO, contains one monomeric nickel(II) com­plex cation, two Cl⁻ anions and one di­methyl­form­amide sol­vent mol­ecule. The Ni atom is coordinated to each of two 1‐­(p‐chloro­phenyl)‐5‐iso­propyl­biguanide (proguanil) ligands via two N atoms. The complex exhibits a square‐planar coordination, with the Ni atom lying 0.021 (2) Å out of the basal plane. The crystal packing is characterized by several hydrogen bonds.     

Adducts of nickel(II) acetylacetonate chelating with heterocyclic bases: 3‐­cyanopyridine and 4‐cyanopyridine

In both title compounds, (acetyl­acetonato‐O,O′)­bis(3‐cyano­pyridine‐N)­nickel(II), (I), and (acetyl­acetonato‐O,O′)­bis(4‐cyanopyridine‐N)­nickel(II), (II), both [Ni(C₅­H₇O₂)₂(C₆H₄N₂)₂], the Ni^II atom, which is situated on a centre of symmetry, is octahedrally coordinated. Distances and angles for (I) and (II), respectively, are: Ni—O 2.009 (2)/2.016 (2) and 2.0110 (16)/2.0238 (18) Å, Ni—N 2.116 (3) and 2.179 (2) Å, O—Ni—O 91.86 (10) and 90.19 (7)°, and O—Ni—N 91.27 (11)/90.19 (11) and 89.65 (8)/90.79 (7)°.