Hemi[hexa­aqua­magnesium(II)] (μ‐2,6‐bis{[bis­(carboxyl­ato­methyl)­amino]­methyl}‐4‐chloro­phenolato)­bis­[di­aqua­magnesium(II)] decahydrate

The crystal structure of the title compound, [Mg(H₂O)₆]_0.5[Mg₂(C₁₆H₁₄ClN₂O₉)(H₂O)₄]·10H₂O, shows that this bi­nuclear complex consists of two Mg centres in distorted octahedral geometry, joined by an oxo bridge which is a derivative of the deprotoned hydroxy group of the phenolate in the ligand mol­ecule. In the anion, the coordination sphere of each Mg^II ion is completed by two carboxyl­ates, a tertiary N atom and two water mol­ecules. The inner coordination spheres for the Mg^II ions are very similar, both in ligand sets and in geometry. Each unit of the binuclear complex has one negative charge neutralized by a neighbouring hydrated cation, [Mg(H₂O)₆]²⁺, in which the Mg atom lies on an inversion centre. In each cell, there are 34 water mol­ecules and most of them participate in the formation of hydrogen bonds, which contribute greatly to the stability of the whole structure.     

Ethyl N‐[2‐(hydroxy­acetyl)­phenyl]­carbamate,ethyl N‐[2‐(hydroxy­acetyl)‐4‐iodo­phenyl]­carbamate and ethyl N‐[2‐(hydroxy­acetyl)‐4‐methyl­phenyl]­carbamate

In ethyl N‐[2‐(hydroxy­acetyl)phenyl]carbamate, C₁₁H₁₃NO₄, all of the non‐H atoms lie on a mirror plane in the space group Pnma; the mol­ecules are linked into simple chains by a single C—H⋯O hydrogen bond. The mol­ecules of ethyl N‐[2‐(hydroxy­acetyl)‐4‐iodo­phenyl]carbamate, C₁₁H₁₂INO₄, are linked into sheets by a combination of O—H⋯I and C—H⋯O hydrogen bonds and a dipolar I⋯O contact. Ethyl N‐­[2‐(hydroxy­acetyl)‐4‐methyl­phenyl]carbamate, C₁₂H₁₅NO₄, crystallizes with Z′ = 2 in the space group P; pairs of mol­ecules are weakly linked by an O—H⋯O hydrogen bond and these aggregates are linked into chains by two independent aromatic π–π stacking inter­actions.     

Bis{μ‐2‐[3‐(cyclo­hexyl­ammonio)­propyl­imino­methyl]­phenolato}bis­[di­chloro­copper(II)]

The title compound, [Cu₂(C₁₆H₂₄N₂O)₂Cl₄], is a dinuclear copper(II) complex with inversion symmetry. Each Cu^II atom is five‐coordinated by two O and one N atom from two Schiff base ligands, and by two Cl atoms, giving an approximately trigonal–bipyramidal coordination environment.     

Bis(μ‐hexa­methyl­enetetr­amine)­bis(aqua­di­bromo­cadmium)­di­aqua­di­bromo­cadmium dihydrate

The title compound, poly­[[di­aqua­di­bromo­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐aqua­cad­mium‐di‐μ‐bromo‐aqua­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐di‐μ‐bromo] dihydrate], [Cd₃­Br₆­(C₆­H₁₂­N₄)₂­(H₂O)₄]·­2H₂O, is made up of two‐dimensional neutral rectangular coordination layers. Each rectangular subunit is enclosed by a pair of Cd₃(μ₂‐Br)₆(H₂O)₃ fragments and a pair of (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragments as sides (hmt is hexa­methyl­enetetr­amine). The unique Cd^II atom in the Cd₂Br₂ ring in the Cd₃(μ₂‐Br)₆(H₂O)₃ fragment is in a slightly distorted octahedral CdNOBr₄ geometry, surrounded by one hmt ligand [2.433 (5) Å], one aqua ligand [2.273 (4) Å] and four Br atoms [2.6409 (11)–3.0270 (14) Å]. The Cd^II atom in the (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragment lies on an inversion center and is in a highly distorted octahedral CdN₂O₂Br₂ geometry, surrounded by two trans‐related N atoms of two hmt ligands [2.479 (5) Å], two trans‐related aqua ligands [2.294 (4) Å] and two trans‐related Br atoms [2.6755 (12) Å]. Adjacent two‐dimensional coordination sheets are connected into a three‐dimensional network by hydrogen bonds involving lattice water mol­ecules, and the aqua, bromo and hmt ligands belonging to different layers.     

2‐[Benzoyl­(hydroxy­imino)­methyl­amino]­benzoic acid

The structure of the title compound, C₁₅H₁₂N₂O₄, consists of a polymeric arrangement, around inversion centres, of mol­ecules linked through O—H⋯N and O—H⋯O hydrogen bonds; there are also intramolecular hydrogen bonds. All these hydrogen‐bond interactions result in the formation of infinite chains parallel to the [010] direction. The oxime group has an E conformation.     

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.     

Hexa­aqua­bis­(di­methyl sulfoxide)­yttrium(III) trichloride

The title compound, [Y(C₂H₆OS)₂(H₂O)₆]Cl₃, contains the cation [Y(H₂O)₆{(CH₃)₂SO}₂]³⁺ with a distorted square antiprismatic geometry of the eight coordinated O atoms. The six water mol­ecules are coordinated with an average Y—O distance of 2.38 (2) Å, ranging from 2.360 (3) to 2.404 (3) Å. Each water mol­ecule forms two hydrogen bonds to the chloride anions with O—Cl distances ranging from 3.068 (4) to 3.422 (4) Å. The two di­methyl­ sulfoxide ligands, situated in the cis position with the O—Y—O angle equal to 83.22 (11)°, have Y—O distances of 2.269 (3) and 2.278 (3) Å.     

Bis(μ‐ethyl pyridine‐2,6‐di­carboxyl­ato)­bis­[di­aqua­chloro­cadmium(II)] dihydrate

The reaction of cadmium chloride with pyridine‐2,6‐di­carboxylic acid (PDA) and 98% H₂SO₄ in ethanol led to the formation of the title compound, bis­[μ‐6‐(ethoxy­carbonyl)­pyridine‐2‐carboxyl­ato]‐1:2κ⁴O⁶,N,O²:O²;1:2κ⁴O²:O²,N,O⁶‐bis­[di­aqua­chloro­cadmium(II)] dihydrate, [Cd₂(C₉H₈NO₄)₂Cl₂(H₂O)₄]·2H₂O. PDA is esterified to monoethyl ­pyridine‐2,6‐di­carboxyl­ate (MEPD) by the catalysis of H₂SO₄ during the reaction. The dinuclear Cd^II complex lies about an inversion centre and the unique Cd atom has a pentagonal–bipyramidal geometry. The two Cd atoms are bridged by two carboxyl­ate O atoms, forming a planar Cd₂O₂ unit. Stair‐like chains are formed via O—H⋯Cl hydrogen bonds and these are further arranged into two‐dimensional layers via hydrogen bonds involving solvate water mol­ecules.     

[2‐(Anilino­methyl)­phenyl]­di­phenyl­phosphine and {2‐[(N‐methyl­anilino)­methyl]­phenyl}di­phenyl­phosphine

The title compounds, Ph₂PCH₂N(H)Ph or C₂₅H₂₂NP and Ph₂PCH₂N(CH₃)Ph or C₂₆H₂₄NP, respectively, are isomorphous, with calculated theoretical Tolman angles of 174 and 182°.     

Bis­[bis­(di­phenyl­phosphino­methyl)­phenyl­phosphine]­di­chloro­tetra­gold(I) bis­[chloro­tris­(penta­fluoro­phenyl)­aurate(III)]

The cation of the title compound, [Au₄(PPh₂CH₂PPhCH₂PPh₂)₂Cl₂][Au(C₆F₅)₃Cl]₂ or [Au₄Cl₂(C₃₂H₂₉P₃)₂][AuCl(C₆F₅)₃]₂, displays a rhomboidal geometry for the Au atoms, with short Au?Au distances of 3.104 (2) and 3.185 (1) Å; the linear coordination at the Au^I atoms is distorted: P—Au—P 164.7 (2)° and P—Au—Cl 170.67 (11)°. The anion shows the expected square‐planar geometry at Au^III, with the Au atom 0.022 (5) Å out of the plane of the four donor atoms.     

1‐(2‐Hydroxy‐4,6‐di­methyl­phenyl)­ethanone

In the crystal of the title compound, C₁₀H₁₂O₂, there are two symmetry‐independent mol­ecules, which are essentially superimposable. Each mol­ecule exhibits an intramolecular O—H?O hydrogen bond, with O?O separations of 2.483 (4) and 2.468 (4) Å.     

2‐[3‐Furyl­(hydroxy)­methyl]‐2,3‐di­methyl­cyclo­hexanone

In the mol­ecule of the title compound, C₁₃H₁₈O₃, there is a syn relationship between the two vicinal methyl groups. The six‐membered ring adopts a chair conformation, with one equatorial and two axial groups, and the furyl group is almost parallel to the ketone group. Intermolecular hydrogen bonds [O—H?O=C 2.814 (3) Å] form chains along [100].     

Secondary interactions in the iso­morphous compounds 2,6‐bis­(chloro­methyl)­pyridinium chloride and 2,6‐bis­(bromo­methyl)­pyridinium bromide

The title compounds, C₇H₈Cl₂N⁺·Cl⁻ and C₇H₈Br₂N⁺·Br⁻, are isomorphous. In the crystal packing, layers parallel to the ac plane are formed by a classical N⁺—H⋯X⁻ hydrogen bond (X = halogen) and two X⋯X contacts. A third X⋯X contact links the layers, and a fourth, which is however very long, completes a ladder‐like motif of halogen atoms. Hydro­gen bonds of the form C—H⋯X play at best a subordinate role in the packing.     

trans‐[1,3‐Bis(2,4‐di­methyl­phenyl)­imidazolidin‐2‐yl­idene]­di­chloro­(tri­phenyl­phosphine‐κP)­palladium(II)

The title complex, [PdCl₂(C₁₉H₂₂N₂)(C₁₈H₁₅P)], shows slightly distorted square‐planar coordination of the palladium(II) metal center. The Pd—C bond distance between the N‐heterocyclic ligand and the metal atom is 2.008 (3) Å. The dihedral angle between the two di­methyl­phenyl ring planes is 33.17 (13)°.     

Bis(μ‐6‐hydroxy­picolinato)‐μ‐oxo‐bis­[di­pyridine­manganese(III)] monohydrate

The title compound, [Mn₂(μ‐O)(C₆H₃NO₃)₂(C₅H₅N)₄]·H₂O, was isolated from the reaction of 2,6‐pyridine­di­carboxylic acid with [Mn₁₂O₁₂(CH₃COO)₁₆(H₂O)₄] in pyridine. The dimanganese complex has twofold symmetry; the Mn^III atoms are bridged by one oxo and two amidate ligands and show compressed octahedral Jahn–Teller distortion. The molecular packing comprises a three‐dimensional structure constructed by means of extensive intermolecular interactions, including three kinds of hydrogen bonds and π–π interactions.     

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.     

Bis­[N,N‐bis(2‐hydroxy­ethyl)­di­thio­carbamato]­di­methyl­tin(IV)

The title compound, [Sn(CH₃)₂(C₅H₁₀NO₂S₂)₂], has crystallographic mirror symmetry (C—Sn—C on mirror plane) and the coordination polyhedron around the Sn atom is a tetrahedron [C—Sn—C 139.3 (2)° and S—Sn—S 82.3 (1)°] distorted towards a skew‐trapezoidal bipyramid owing to an intramolecular Sn?S contact [3.0427 (6) Å]. The mol­ecules are linked into a linear chain by intermolecular O—H?O hydrogen bonds [O?O 2.646 (3) Å].     

Bis{μ‐[6‐(hydroxy­methyl)‐2‐pyridyl]­methano­lato‐κ3N,O:O}bis{[2,6‐bis­(hydroxy­methyl)­pyridine‐κ3O,N,O′]copper(II)} di­acetate

The title dinuclear Cu^II complex, [Cu₂(C₇H₈NO₂)₂(C₇H₉NO₂)₂](CH₃COO)₂, has been synthesized by the reaction of Cu(CH₃COO)₂·H₂O with pdmH₂ (pdmH₂ is pyridine‐2,6‐diyldi­methanol) in the presence of tetra­butyl­ammonium hydro­xide. The title complex contains a centrosymmetric Cu₂O₂ core and each Cu^II atom has distorted octahedral geometry. Molecular [Cu₂(pdmH)₂(pdmH₂)]²⁺ cations are connected by hydrogen bonds involving the CH₃COO⁻ anions, forming one‐dimensional chains along the a axis.     

2,4‐Di­hydroxy‐1,3‐bis­(methoxy­carbonyl­methoxy)­calix­[4]­arene and 1,3‐bis­(ethoxy­carbonyl­methoxy)‐2,4‐di­hydroxy­calix­[4]­arene chloro­form solvate

The two title calix­[4]­arene compounds, C₃₄H₃₂O₈, (I), and C₃₆H₃₆O₈·CH₃Cl, (II), respectively, which differ only in the size of the alkyl function on the pendant ester group, are compared. Compound (I) forms a novel supramolecular array, whilst (II) fails to do so due to accommodating a chloro­form guest molecule in the lower‐rim cavity.