NEt4OH·5H2O containing hydro­xide–water layers

In the title compound, tetraethyl­ammonium hydro­xide pentahydrate, C₈H₂₀N⁺·OH^?·5H₂O, layers of approximately hexagonally close‐packed NEt₄⁺ cations and anionic layers of hydro­xide and water mol­ecules are stacked alternately along the b axis. All hydro­xide and water H atoms are in ordered positions, giving rise to a network of hydrogen bonds [O?O 2.633 (1)–2.947 (2) Å] with four‐ and six‐membered rings. The hydro­xide ion accepts four hydrogen bonds from four water mol­ecules but does not act as a proton donor.     

Benzyl­tri­methyl­ammonium hydro­xide trihydrate containing hydro­xide–water layers

In the title compound, C₁₀H₁₆N⁺·OH⁻·3H₂O, two-dimensional bilayer-like arrays of organic cations and corrugated anionic hydro­xide–water layers are stacked alternately along the c axis. All hydro­xide and water H atoms are in ordered positions, giving rise to a network of hydrogen bonds [O⃛O 2.639 (2)–2.927 (2) Å for water donors and O⃛O 3.323 (2) Å for hydro­xide donors] with four- and six-membered rings.     

Dichloro(tetrahydrofuran‐O)[(trimethylsilyl)amido‐N]gallium(III)

The title compound, [GaCl₂(C₃H₁₀NSi)(C₄H₈O)], is the tetra­hydro­furan‐coordinated monomer of the previously structurally characterized dimer [GaN(H)SiMe₃Cl₂]₂. The title compound consists of discrete monomeric mol­ecules with two crystallographically independent mol­ecules within the unit cell. The crystal structure is composed of a Ga atom in a four‐coordinate tetrahedral arrangement, with Ga—N distances of 2.025 (3) and 2.026 (3) Å in the two independent mol­ecules.     

Poly[tetrasodium(I)‐tetra‐μ2‐bis(butane‐1,4‐diyldioxy)borato‐μ2‐1,4‐butane­diol]

In the title compound, [Na₄(C₈H₁₆BO₄)₄(C₄H₁₀O₂)]_n, there are two coordination types for the four independent Na⁺ cations: two Na⁺ cations bond to six diolate O atoms [Na—O = 2.305 (2)–2.609 (2) Å], while the other two are five‐coordinate via one 1,4‐butane­diol [2.289 (2) and 2.349 (3) Å] and four diolate O atoms [2.295 (2)–2.408 (2) Å]. Corresponding to this, there are three‐ and four‐coordinate diolate O atoms, the latter bridging Na atoms. The 1,4‐butane­diol mol­ecules lie on inversion centres. The boron stereochemistry shows minor local perturbations from its usual tetrahedral state [B—O = 1.457 (4)–1.503 (4) Å]. The resulting polymer packs as sheets parallel to the (10) plane crosslinked by the butane­diol mol­ecules. The structure was solved using data from a multiple crystal.     

Aquachlorobis[4,4,5,5‐tetramethyl‐2‐(2‐pyridyl)‐4,5‐dihydro‐1H‐imidazol‐1‐oxyl 3‐oxide‐κ2O1,N2]nickel(II) nitrate methanol disolvate monohydrate

The title complex, [NiCl(C₁₂H₁₆N₃O₂)₂(H₂O)]NO₃·2CH₄O·H₂O, was obtained from a methano­lic solution of Ni(NO₃)₂·6H₂O, 2‐pyridyl nitro­nyl nitro­xide (2‐NITpy) and (NEt₄)₂[CoCl₄]. The equatorial coordination sites of the octahedral Ni^II centre are occupied by two chelating radical ligands, with the axial positions occupied by the Cl^? and water ligands. The H₂O—Ni—Cl axis of the complex lies along a crystallographic twofold axis, so that only half the cation is present in the asymmetric unit. The Ni—Cl bond length [2.3614 (17) Å] is significantly shorter than distances typical of octahedral Ni^II centres [2.441 (5) Å]. However, with only one nitrate anion per formula unit, the oxidation state of the metal must be assigned as Ni^II. The 2‐NITpy ligands bend away from the equatorial plane, forming a hydro­phobic region around the Cl atoms. Conversely, the ligated water mol­ecule forms moderately strong hydrogen bonds with the disordered methanol solvent mol­ecules, which in turn form interactions with the water of crystallization and the disordered nitrate anion. These interactions combine to give hydro­philic regions throughout the crystal structure.     

trans‐Di­chloro‐cis‐bis(3,6‐di­methyl­carbazolyl)‐cis‐bis­(tetra­hydro­furan)­zirconium(IV) benzene sesquisolvate

In the title compound, [ZrCl₂(C₁₄H₁₂N)₂(C₄H₈O)₂]·1.5C₆H₆, the Zr atom is pseudo‐octahedral, with two Cl atoms in trans positions and two tetra­hydro­furan mol­ecules in cis positions. The two 3,6‐di­methyl­carbazolyl ligands are in cis positions and are canted with respect to one another. The two Zr—N distances are 2.1148 (18) and 2.1236 (18) Å, and the N—Zr—N angle is 95.08 (7)°. The title compound crystallizes as the benzene solvate, with one of the benzene mol­ecules positioned on an inversion center.     

Hydro­gen‐bond networks in tris(4‐hydroxy­phenyl)­methane and its 1:1 molecular complex with 4,4′‐bi­pyridine

In tris(4‐hydroxy­phenyl)­methane (or 4,4′,4′′‐methane­triyl­tri­phenol), C₁₉H₁₆O₃, mol­ecules are connected by O—H⃛O hydrogen bonds [O⃛O = 2.662 (2) and 2.648 (2) Å] into two‐dimensional square networks that are twofold interpenetrated. In tris(4‐hydroxy­phenyl)­methane–4,4′‐bi­pyridine (1/1), C₁₉H₁₆O₃·C₁₀H₈N₂, trisphenol mol­ecules form rectangular networks via O—H⃛O [O⃛O = 2.694 (3) Å] and C—H⃛O [C⃛O = 3.384 (3) Å] hydrogen bonds. Bi­pyridine mol­ecules hydrogen bonded to phenol moieties [O⃛N = 2.622 (3) and 2.764 (3) Å] fill the voids to complete the structure.     

A uranyl ion complex of N‐methyl‐p‐tert‐butyl­dihomo­ammonio­calix­[4]­arene with di­aqua­di­pyridine­lithium as counter‐ion

The title complex, di­aqua­di­pyridine­lithium (N‐methyl‐p‐tert‐butyl­dihomo­ammonio­calix­[4]­arene‐κ⁴O)­dioxouranium(VI) tri­pyridine solvate monohydrate, [Li(C₅H₅N)₂(H₂O)₂][UO₂(C₄₆H₅₈NO₄)]·3C₅H₅N·H₂O, contains an `internal' tetraphenoxide‐coordinated uranyl complex of the macrocycle, in which the protonated N atom is involved in an intramolecular hydrogen bond with the uranyl oxo group located in the cavity. The Li⁺ ion is in a tetrahedral environment and its two water ligands are involved in hydrogen bonds with two phenoxide O atoms, two pyridine mol­ecules and one water mol­ecule. This arrangement is compared with those obtained previously for other homo­aza­calixarenes and also for homo­oxa­calixarenes in the presence of alkali metal hydro­xides.     

N‐Cyclo­hexyl‐2‐[5‐(4‐pyridyl)‐4‐(p‐tolyl)‐4H‐1,2,4‐triazol‐3‐yl­sulfanyl]­acetamide dihydrate

In the title compound, C₂₂H₂₅N₅OS·2H₂O, the mol­ecules are stacked in columns running along the b axis. In this arrangemant, the mol­ecules are linked to each other by a combination of one two‐centre N—H⋯O hydrogen bond and four two‐centre O—H⋯O hydrogen bonds containing two types of ring motif, viz.R₄⁴(10) and R₃³(11). In the crystal structure, centrosymmetric π–π inter­actions between the triazole rings, with a distance of 3.691 (2) Å between the ring centroids, also affect the packing of the mol­ecules.     

Redetermination of fac‐tris­(benzo­hydrox­am­ato)­iron(III) tri­hydrate

Due to its importance as a model for naturally occurring iron(III) siderophores such as desferriox­amine B, the crystal structure of the title compound, [Fe(C₇H₆NO₂)₃]·3H₂O, which was reported previously (R = 0.12, one of water mol­ecules disordered), has been redetermined (R = 0.041 without disorder). The complex has pseudo‐octahedral geometry around the Fe^III atom, with Fe—O bond lengths ranging from 1.9689 (18) to 2.0585 (17) Å and O—Fe—O bond angles in the chelate rings of 78.01 (7), 78.83 (7) and 78.95 (7)°. There is extensive hydrogen bonding involving the water mol­ecules and the hydro­xamate ligands.     

Bis­[tris(2,2′‐bi­pyridine‐κ2N,N′)­ruthenium(II)] hexa­cyano­ferrate(III) chloride octahydrate

In the title compound, [Ru^II(C₁₀H₈N₂)₃]₂[Fe^III(CN)₆]Cl·8H₂O, the [Ru(bpy)₃]²⁺ (bpy is 2,2′‐bi­pyridine) cations and water mol­ecules afford intriguing microporous honeycomb layers, while the [Fe(CN)₆]³⁻ anions and the remainder of the water mol­ecules form anionic sheets based on extensive hydrogen‐bonding networks. The cationic and anionic layers alternate along the c axis. The Fe atom in [Fe(CN)₆]³⁻ lies on an inversion centre and the axial cyano ligands are hydrogen bonded to the water mol­ecules encapsulated within the micropores [N⋯O = 2.788 (5) Å], giving an unusual interpenetration between the cationic and anionic layers. On the other hand, the in‐plane cyano ligands are relatively weakly hydrogen bonded to the water mol­ecules [N⋯O = 2.855 (7) and 2.881 (8) Å] within the anionic sheets.     

The double-layered hydro­xide 3CaO·Al2O3·0.5CaBr2·0.5CaCl2·10H2O

The title compound, calcium oxide–dialuminium trioxide–calcium dibromide–calcium dichloride hydrate (3/1/0.5/0.5/10), also formulated as Ca₂Al(OH)₆Br_0.478Cl_0.522·2H₂O (dicalcium aluminium hydro­xide hemibromide hemichloride dihydrate), is a double-layered hydro­xide which belongs to the solid solution Ca₂Al(OH)₆Br_xCl_1−x·2H₂O, where x can vary from 0 to 1. Chloride and bromide anions of the negatively charged interlayer [Br_0.5Cl_0.5·2H₂O]⁻ share statistically the same crystallographic site. Al³⁺ and Ca²⁺ cations are coordinated by six and seven O atoms, respectively. All water mol­ecules are bonded to Ca²⁺ cations and assume the seventh coordination position. Anions in the interlayer are surrounded by ten H atoms. Br⁻ and Cl⁻ are therefore connected to the main layer by ten hydrogen bonds, six of 2.74 (2) Å and four of 2.52 (5) Å, where the donors are hydroxyl groups and water mol­ecules, respectively. Like the chloride equivalent, the title compound is a 6R polytype with trigonal space group Rc and lattice parameters a = 5.7537 (4) Å and c = 48.108 (4) Å.     

catena‐Poly­[[[(1,10‐phenanthroline‐κ2N,N′)­manganese(II)]‐μ‐l‐tartrato‐κ4O1,O2:O3,O4] hexahydrate]

The title compound, {[Mn(C₄H₄O₆)(C₁₂H₈N₂)]·6H₂O}_n, has a linear chain structure containing monomeric [Mn(C₄H₄O₆)(C₁₂H₈N₂)] repeat units. Each manganese ion is six‐coordinate, with the two phenanthroline N atoms [Mn—N = 2.229 (2) and 2.235 (2) Å] and four O atoms from two tartrate anions [Mn—O_COO = 2.1252 (19) and 2.1310 (19) Å, and Mn—O_OH = 2.2404 (19) and 2.2424 (19) Å] forming a seriously distorted octahedral coordination environment. Six water mol­ecules exist outside every repeat unit as solvate mol­ecules. Extensive hydrogen‐bonding interactions and π–π stacking of the phenanthroline moieties exist between the chains.     

7‐Carboxyl­ato‐8‐hydroxy‐2‐methyl­quinolinium monohydrate and 7‐carboxy‐8‐hydroxy‐2‐methyl­quinolinium chloride monohydrate at 100 K

Both 7‐carboxyl­ato‐8‐hydroxy‐2‐methyl­quinolinium monohydrate, C₁₁H₉NO₃·H₂O, (I), and 7‐carboxy‐8‐hydroxy‐2‐methyl­quinolinium chloride monohydrate, C₁₁H₁₀NO₃⁺·Cl⁻·H₂O, (II), crystallize in the centrosymmetric P space group. Both compounds display an intramolecular O—H⋯O hydrogen bond involving the hydroxy group; this hydrogen bond is stronger in (I) due to its zwitterionic character [O⋯O = 2.4449 (11) Å in (I) and 2.5881 (12) Å in (II)]. In both crystal structures, the HN⁺ group participates in the stabilization of the structure via intermolecular hydrogen bonds with water mol­ecules [N⋯O = 2.7450 (12) Å in (I) and 2.8025 (14) Å in (II)]. In compound (II), a hydrogen‐bond network connects the Cl⁻ anion to the carboxylic acid group [Cl⋯O = 2.9641 (11) Å] and to two water mol­ecules [Cl⋯O = 3.1485 (10) and 3.2744 (10) Å].     

catena‐Poly­[[di­aqua­(isonicotinato‐O,O′)­europium(III)]‐di‐μ‐isonicotin­ato‐O:O′]

The title complex, [Eu(C₆H₄O₂)₃(H₂O)₂], has a double carboxyl­ate‐bridged infinite‐chain structure, with one chelating carboxyl­ate group on each Eu ion centre, which also binds to two water mol­ecules to yield an eight‐coordinate square‐antiprismatic geometry, with Eu—O bond lengths in the range 2.338 (3)–2.594 (3) Å. The pyridine N atoms of the isonicotinate groups do not coordinate to the Eu ions; instead, they direct the formation of Eu^III coordination polymers via hydrogen bonding with coordinated water mol­ecules.     

Precursor of a β‐lactamase inhibitor: allyl (4S,8S,9R)‐10‐[(E)‐ethyl­idene]‐4‐methoxy‐11‐oxo‐1‐aza­tri­cyclo­[7.2.0.03,8]­undec‐2‐ene‐2‐carboxyl­ate

The molecular structure of the title tricyclic compound, C₁₇H₂₁NO₄, which is the immediate precursor of a potent synthetic inhibitor {Lek157: sodium (8S,9R)‐10‐[(E)‐ethyl­idene]‐4‐methoxy‐11‐oxo‐1‐aza­tri­cyclo­[7.2.0.0^3,8]­undec‐2‐ene‐2‐carboxyl­ate} with remarkable potency, provides experimental evidence for the previously modelled relative position of the fused cyclo­hexyl ring and the carbonyl group of the β‐lactam ring, which takes part in the formation of the initial tetrahedral acyl–enzyme complex. In this hydro­phobic mol­ecule, the overall geometry is influenced by C—H?O intramolecular hydrogen bonds [3.046 (4) and 3.538 (6) Å, with corresponding normalized H?O distances of 2.30 and 2.46 Å], whereas the mol­ecules are interconnected through intermolecular C—H?O hydrogen bonds [3.335 (4)–3.575 (5) Å].     

The solid dihydrate of N,N‐di­methyl‐n‐tetra­decyl­amine oxide

Crystalline N,N‐di­methyl‐n‐tetra­decyl­amine oxide has been prepared by reaction of liquid N,N‐di­methyl‐n‐tetra­decyl­amine with 70% H₂O₂ in the presence of CO₂ as catalyst. The resulting soft low‐melting solid was crystallized as the dihydrate, viz. C₁₆H₃₅NO·2H₂O. The extended hydro­carbon chains pack in a parallel fashion, with the N‐oxide ends of the mol­ecules forming hydrogen bonds with the water mol­ecules in hydro­philic layers. The N—O distance is 1.411 (3) Å.     

Berberine formate–succinic acid (1/1)

The title compound [systematic name: 9,10‐di­methoxy‐2,3‐methyl­ene­dioxy‐5,6‐di­hydro­dibenzo­[a,g]­quinolizinium form­ate–succinic acid (1/1)], C₂₀H₁₈NO₄⁺·CHO₂⁻·C₄H₆O₄, con­tains centrosymmetric pairs of almost planar berberine cations, and hydrogen‐bonded (C₄H₆O₄⋯HCOO⁻)₂ rings of succinic acid with formate anions, bonded by O—H⋯O hydrogen bonds with O⋯O distances of 2.4886 (15) and 2.5652 (16) Å. Pairs of cations and mol­ecules of succinic acid are connected by non‐conventional weak C—H⋯O hydrogen bonds, with C⋯O distances of 3.082 (2) and 3.178 (2) Å.     

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.     

1,3‐Dibenzoylimidazolidine‐2‐thione and 1,3‐dibenzo­yl‐3,4,5,6‐tetra­hydro­pyrimidine‐2(1H)‐thione

The title compounds, 1,3‐dibenzo­ylimidazolidine‐2‐thione, C₁₇H₁₄N₂O₂S, (I), and 1,3‐dibenzo­yl‐3,4,5,6‐tetra­hydro­pyrimidine‐2(1H)‐thione, C₁₈H₁₆N₂O₂S, (II), were obtained from the reactions of imidazolidine‐2‐thione and 1,4,5,6‐tetra­hydro­pyrimidine‐2‐thiol, respectively, with benzoyl chloride. Compounds (I) and (II) contain, respectively, imidazolidinethione [C=S = 1.6509 (14) Å] and ­pyrimidinethione [C=S = 1.6918 (19) Å] moieties bonded to two benzoyl rings. The mol­ecules of (I) exhibit C₂ symmetry, the C=S bond lying along the twofold rotation axis, while the mol­ecules of (II) have mirror symmetry (C_s). The imida­zolidine ring in (I) is essentially planar, while the pyrimidine ring in (II) adopts a boat conformation. Mol­ecules of (I) are linked by weak inter­molecular C—H⋯O inter­actions, while mol­ecules of (II) are held together by van der Waals inter­actions.