[N,N′‐Bis­(salicyl­idene)‐2,2‐di­methyl‐1,3‐propane­diaminato]­nickel(II) and [N,N′‐bis­(salicyl­idene)‐2,2‐di­methyl‐1,3‐propane­diaminato]copper(II)

In the title compounds, {2,2′‐[2,2‐di­methyl‐1,3‐propane­diyl­bis­(nitrilo­methyl­idyne)]­diphenolato‐κ⁴N,N′,O,O′}nickel(II), [Ni(C₁₉H₂₀N₂O₂)], and {2,2′‐[2,2‐di­methyl‐1,3‐propane­diyl­bis­(nitrilo­methyl­idyne)]­diphenolato‐κ⁴N,N′,O,O′}copper(II), [Cu(C₁₉H₂₀N₂O₂)], the Ni^II and Cu^II atoms are coordinated by two iminic N and two phenolic O atoms of the N,N′‐bis­(salicyl­idene)‐2,2‐di­methyl‐1,3‐propane­diaminate (SALPD^2?, C₁₇H₁₆N₂O₂^2?) ligand. The geometry of the coordination sphere is planar in the case of the Ni^II complex and distorted towards tetrahedral for the Cu^II complex. Both complexes have a cis configuration imposed by the chelate ligand. The dihedral angles between the N/Ni/O and N/Cu/O coordination planes are 17.20 (6) and 35.13 (7)°, respectively.     

N,N′‐Bis­[1‐(pyrazin‐2‐yl)­ethyl­idene]­hydrazine

Molecules of the title compound, C₁₂H₁₂N₆, contain both a di­imine linkage and an N—N bond, and assume a planar structure. The compound lies about an inversion centre and there are three intramolecular C—H⋯N hydrogen bonds.     

[N,N′‐Bis­(salicyl­idene)‐1,2‐di­phenyl‐(RS,SR)‐1,2‐ethane­di­amin­ato]­nickel(II)

In crystals of the title compound, [Ni(C₂₈H₂₂N₂O₂)], the coordination geometry around the Ni atom is square planar with a slight tetrahedral distortion. The five‐membered N,N′‐chelate ring adopts a distorted gauche conformation with the two phenyl groups in axial and equatorial orientations.     

[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.     

exo‐[N,N′‐Bis(3‐tert‐butyl­salicyl­idene)‐1,2‐di­phenyl‐(RS,SR)‐1,2‐ethane­diyl­diaminato]­oxovanadium(IV)

The title mononuclear oxovanadium(IV) complex, [VO(C₃₆H₃₈N₂O₂)], has a distorted square‐pyramidal coordination. The complex was shown to be the exo isomer.     

Bis­[chloro­bis(1,10‐phenanthroline‐N,N′)(thio­urea‐S)­nickel(II)] chloride nitrate diethanol solvate

The crystal structure of the title compound, [NiCl(C₁₂H₈N₂)₂(CH₄N₂S)]₂(NO₃)­Cl·­2C₂H₆O, is formed by [Ni(phen)₂(thio­urea)Cl]⁺ cations (phen = 1,10‐phenanthroline), chloride and nitrate counter‐ions, and ethanol solvate mol­ecules. The Ni atom is octahedrally coordinated to two bidentate phen ligands, a monodentate thio­urea and a chloride ion. Both the chloride and nitrate anions, which provide charge balance, are located at special positions on a twofold symmetry axis. Hydro­gen bonds play a key role in the packing and conformation of the cation and create a three‐dimensional network.     

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.     

[N,N′‐Bis(5‐bromo­salicyl­idene)‐o‐phenylene­diaminato]copper(II)

In the title compound, {4,4′‐di­bromo‐2,2′‐[o‐phenyl­ene­bis­(nitrilo­methyl­idene)]­di­phen­ol­ato‐O,N,N′,O′}copper(II), [Cu(C₂₀H₁₂Br₂N₂O₂], the Cu^II ion shows a slightly distorted square‐planar geometry with the N₂O₂ atoms of the Schiff base imine–phenol tetradentate ligand.     

2‐(Phenyl­amino­methyl­idene)­cyclo­hexane‐1,3‐dione

In the title compound, C₁₃H₁₃NO₂, there is polarization of π‐electron density from the amine N atom to the acceptor carbonyl groups: as a result, the mol­ecule exists predominantly in an azomethino‐1,3‐diketone tautomeric form. There is crystallographic evidence that the phenyl ring, although roughly coplanar with the rest of the mol­ecule, is deconjugated with the adjacent π system of the mol­ecule. The cyclo­hexane ring adopts an unsymmetrical half‐chair conformation and converts between two inversion‐related conformers. The mol­ecule is stabilized by an intramolecular hydrogen bond, while the intermolecular packing is dominated by a number of short C—H⋯O contacts.     

{3,3′‐[2,2′‐(Ethylenedioxy)dibenzyl­idene]bis(S‐methyl dithiocarbazate)}­nickel(II)

The tetradentate N₂S₂ Schiff base ligand 3,3′‐[2,2′‐(ethyl­ene­di­oxy)di­benzyl­idene]­bis­(S‐methyl di­thio­car­ba­zate) (H₂L), prepared by the condensation of S‐methyl di­thio­carb­aza­te with 1,4‐bis(2‐formyl­phenyl)‐1,4‐dioxa­butane in a 1:2 molar ratio, reacts with nickel acetate to form the title neutral metal complex, [Ni(C₂₀H₂₀N₄O₂S₄)]. The X‐ray structure of the complex shows a distorted square‐planar geometry around the Ni atom. The monomeric units are weakly associated into dimers via a long Ni?S interaction [3.569 (1) Å]. These dimeric units are then linked by C—H?S intermolecular contacts to form a polymeric chain along the a axis.     

Bis­[tris­(ethyl­enedi­amine)­cobalt(III)] di­chloro­bis­[μ‐(1‐hydroxy­ethyl­idene)­di­phospho­nato(4–)]­di­ruthenium(II,­III)­(Ru–Ru) chloride trihydrate

In the title compound, [Co(C₂H₈N₂)₃]₂[Ru₂(C₂H₄O₇P₂)₂Cl₂]Cl·3H₂O, the building unit contains two crystallographically independent dinuclear [Ru₂(hedp)₂Cl₂]⁵⁻ anions, where hedp [viz. (1‐hydroxy­ethyl­idene)­di­phospho­nate] serves as a bis‐chelating bridging ligand, two types of [Co(en)₃]³⁺ cations, one uncoordinated Cl⁻ anion and five water mol­ecules of crystallization. The [Ru₂(hedp)₂Cl₂]⁵⁻ anions are connected to one another, forming one‐dimensional chains along the a axis. The [Co(en)₃]³⁺ cations are located between these chains and lie across inversion centres. An extensive series of hydrogen bonds lead to the formation of a three‐dimensional supramol­ecular network structure, with channels generated along the [100] direction. The uncoordinated water mol­ecules and Cl⁻ anions reside in these channels.     

trans‐Bis­(diethano­lamine)­bis­(iso­thio­cyanato)­nickel(II)

In the neutral title complex, trans‐bis(2,2′‐imino­di­ethanol‐N,O)­bis­(iso­thio­cyanato)­nickel(II), [Ni(NCS)₂(C₄H₁₁NO₂)₂], the iso­thio­cyanate ions and the di­ethanol­amine mol­ecules act as mono­dentate and bi­dentate ligands, respectively. The Ni^II ion exhibits a distorted octahedral configuration with crystallographically imposed inversion symmetry and N_NCS—Ni—N_amine and N_NCS—Ni—O_amine bond angles of 88.78 (10) and 89.44 (10)°, respectively. The Ni—N bond distances are in the range 2.069 (3)–2.096 (2) Å. The mol­ecules are linked by hydrogen bonds to form a three‐dimensional infinite lattice.     

Bis­(acetato‐O)­tetrakis­(imidazole‐N3)­nickel(II)

In the title compound, [Ni(C₂H₃O)₂(C₃H₄N₂)₄], the Ni atom is coordinated centrosymmetrically by four N and two O atoms in an octahedral coordination [Ni—N = 1.986 (3) and 2.054 (3) Å; Ni—O = 2.697 (3) Å]. The O atoms of the acetate anions form hydrogen bonds to adjacent imidazole moieties, with the free O atom forming a somewhat shorter bond [N?O = 2.679 (3) and 2.870 (4) Å]. The hydrogen bonds give rise to a two‐dimensional layer structure.     

An unexpected chelate conformation in trans‐[(R)‐N,N′‐bis(α‐phenyl­salicyl­idene)­propane‐1,2‐diaminato(2–)]­bis(1‐methyl‐1H‐imidazole‐κN3)­cobalt(III) perchlorate

The title compound, [Co(C₂₉H₂₄N₂O₂)(C₄H₆N₂)₂]ClO₄, contains an optically active tetradentate Schiff base ligand in an equatorial plane and two 1‐methyl­imidazole ligands at apical positions. The central N—C—C—N chelate ring of the Schiff base ligand has an envelope structure with a λ conformation, which is different from the solution structure predicted from circular dichroism and ¹H NMR spectra.     

trans‐Bis­[2,3‐di­amino‐(R,S)‐propion­ato‐N,N′]­di­aqua­copper(II) dihydrate

The title copper complex, [Cu(dl ‐DAP)₂(H₂O)₂]·2H₂O or [Cu(C₃H₇N₂O₂)₂(H₂O)₂]·2H₂O, prepared from the non‐protein amino acid dl ‐2,3‐di­amino­propionic acid (dl ‐HDAP), has a center of symmetry and a distorted octahedral coordination, with four N atoms in equatorial positions and two water mol­ecules in apical sites. The water mol­ecule of crystallization is hydrogen bonded to the deprotonated carboxyl­ate group of the ligand.     

Bis­[methyl­enebis­(di­phenyl­phosphine)‐P,P′]­nickel(II) diperchlorate

The title compound, [Ni(Ph₂PCH₂PPh₂)₂](ClO₄)₂, was synthesized and its structure determined crystallographically. The Ni atom lies on an inversion centre and is at the center of a square formed by four P atoms which are necessarily coplanar. The Ni—P distances are 2.2188 (5) and 2.2322 (5) Å, and the P—Ni—P angle is 73.12 (3)°. The unique perchlorate anion is not coordinated to the Ni atom.     

Bis­[tris(3‐cyclo­hexyl­pyrazol‐1‐yl)­hydridoborato]copper(II) di­chloro­methane disolvate

The title compound, [Cu(C₂₇H₄₀BN₆)₂]·2CH₂Cl₂, contains a four‐coordinate Cu^II ion lying on a crystallographic inversion centre, giving rise to a near‐regular square‐planar stereochemistry. There is an axial contact of 2.71 Å between the Cu ion and ligand B—H group, although this is unlikely to correspond to a significant `agostic' interaction.     

Bis­[N,N′‐diiso­propyl‐N‐(tri­methyl­silyl)­benzamidinium] di‐μ‐chloro‐bis­[tetra­chloro­zirconate(IV)] di­chloro­methane disolvate

The structure of the salt of the di‐μ‐chloro‐bis­[tetra­chloro­zirconate(IV)] anion and the N,N′‐iso­propyl‐N‐(tri­methyl­silyl)benzamidinium cation, (C₁₆H₂₉N₂Si)₂[Zr₂Cl₁₀]·2CH₂Cl₂, is reported. The anion lies about an inversion centre and shows a substantially octahedral coordination around Zr, while the structure of the cation is unequivocally assigned as that of a benzamidinium ion.     

Bis­[tris(1,2‐ethanedi­amine‐N,N′)nickel(II)] tetra­thio­antimonate(V) nitrate

The title double salt, [Ni(C₂H₈N₂)₃]₂(SbS₄)(NO₃), was crystallized under solvothermal conditions. Hydro­gen bonds between the SbS₄^3? anions (at four sites) and the [Ni(en)₃]²⁺ (en = ethyl­enedi­amine) cations (at two sites) form a three‐dimensional network. The NO₃^? anion is disordered over four sites. The cation lies on a twofold rotation axis and the SbS₄^3? anion on a axis.     

[1,2‐Di­phenyl‐N,N′‐bis­(salicyl­idene)‐(RR,SS)‐1,2‐ethane­diyl­diamin­ato]­nitrido­manganese(V)

The title compound, [MnN(C₂₈H₂₂N₂O₂)], has a distorted square‐pyramidal coordination with an Mn[triple‐bond]N bond length of 1.516 (2) Å at the apical position. The five‐membered chelate ring adopts a gauche conformation with the two phenyl groups in equatorial orientations.