Tri­benzyl­phosphine oxide

The title compound, (C₆H₅CH₂)₃PO, is an organic tertiary phosphine oxide. The mol­ecule has threefold symmetry, with the P—O bond along the threefold axis. Main dimensions include P—O 1.488 (4), P—C 1.823 (3) Å and O—P—C 114.7 (1)°. The crystals were accidentally obtained when preparing complexes of nickel(II) with di­benzyl­phosphine.     

Hexa­aqua­iron(II) dipicrate dihydrate

In the crystal structure of the title compound, [Fe(H₂O)₆](C₆H₂N₃O₇)₂·2H₂O, the centrosymmetric cationic iron com­plexes and picrate anions form separate stacks extending along the b axis. No picrate species ligate to the metal cation. Picrate ions are linked to one another in the stack via short intermolecular C⃛C contacts of 3.083 (4) and 3.055 (4) Å. Variable‐temperature X‐ray diffraction measurements per­formed between room temperature and 93 K showed a linear decrease of the lattice parameters, suggesting that there is no phase transition.     

Hexa­methyl­enetetraminium 2,4,6‐tri­nitro­phenolate

In the title complex, the 1:1 ionic adduct of hexa­methyl­enetetraminium and 2,4,6‐tri­nitro­phenolate, C₆H₁₃N₄⁺·­C₆H₂N₃O₇^?, the cation acts as a donor for bifurcated hydrogen bonds to the O atoms of the phenolate and one of the nitro groups of the 2,4,6‐tri­nitro­phenolate anion. The crystal structure is built from sheets of cations and anions, and is stabilized by intermolecular C—H?O and C—H?π interactions.     

Hexa­aqua­nickel(II) bis­(hypophosphite)

The structure of hexa­aqua­nickel(II) bis­(hypophosphite), [Ni(H₂O)₆](H₂PO₂)₂, has been determined. The crystals are prismatic. The packing of the Ni and P atoms (not the entire hypophosphite anions) is the same as in the structures of [Co(H₂O)₆](H₂PO₂)₂ and [Co_0.5Ni_0.5(H₂O)₆](H₂PO₂)₂. The Ni^II cations have a pseudo‐face‐centered cubic cell, with cell parameter a 10.216 Å and tetrahedral cavities occupied by P atoms. The Ni^II cation has crystallographically imposed twofold symmetry and has an octahedral coordination sphere consisting of six water O atoms, two of which also lie on the twofold axis. The planes of oppositely coordinated water mol­ecules are in a cross conformation. The geometry of the hypophosphite anion is close to point symmetry mm2. The hypophosphite anions are hydrogen bonded to the coordinated water molecules.     

Bis­(benzyl­ammonium) hexa­chloro­tin(IV)

The crystal structure of bis­(benzyl­ammonium) hexa­chloro­tin(IV), (C₇H₇NH₃)₂[SnCl₆], exhibits ionic layers separated by hydro­carbon layers. The hydro­carbon layer contains two crystallographically inequivalent benzyl groups and aromatic π–π stacking interactions are observed in this layer. In the inorganic layer, the ammonium groups interact with isolated tilted [SnCl₆]²⁻ octahedra through normal, bifurcated and trifurcated N—H⋯Cl hydrogen bonds.     

Hexa­aqua­cobalt(II) bis(4‐toluene­sulfonate)

The title compound, [Co(H₂O)₆](CH₃C₆H₄SO₃)₂, has a structure where the metal atom is surrounded by six mol­ecules of water forming the cation and the anion is deprotonated 4‐toluene­sulfonic acid. The Co atom is in a nearly regular octahedral coordination geometry, with Co—O distances between 2.0529 (14) and 2.0810 (16) Å, and angles ranging from 87.25 (9) to 92.75 (9)°. The supramolecular structure consists of parallel layers of cations and anions. The anions are arranged with their sulfonate groups directed towards the cation layer in an alternating fashion and form hydrogen bonds with the water mol­ecules of the cation.     

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.     

N‐(2,4‐Dimethoxy­benzyl­idene­amino)­guanidinium dihydrogenphosphate

In the asymmetric unit of the title compound, C₁₀H₁₅N₄O₂⁺·H₂PO₄⁻, there are two protonated amino­guanidinium cations and two dihydrogenphosphate anions. The positive charge on the protonated amidine group is delocalized over the three C—N bonds in a manner similar to that found in guanidinium salts. The amino­guanidinium cations are found to be the E‐isomer structures. Intra­molecular inter­actions of the N—H⋯N type are observed, leading to the formation of five‐membered rings. Extensive networks of O—H⋯O, N—H⋯O and C—H⋯O hydrogen bonds stabilize the three‐dimensional network. In the crystal structure, π–π inter­actions between the benzene rings, with a distance of 3.778 (2) Å between the ring centroids, also affect the packing of the mol­ecules.     

Hexa­aqua­nickel diorotate(1–) dihydrate at 150 K

In hexa­aqua­nickel bis(2,6‐di­oxo‐1,2,3,6‐tetrahydro­pyrimidine‐4‐carboxyl­ate) dihydrate, [Ni(H₂O)₆](C₅H₃N₂O₄)₂·2H₂O, the nickel cation is coordinated by six aqua ligands and only associated with the two orotate ions through hydrogen bonds. The structure is isotypic with the magnesium and zinc analogues. The metal cation sits on a crystallographic center of inversion that relates the water mol­ecules and the organic anions. The orotate moieties form an unbonded one‐dimensional chain mediated by a hydrogen‐bonded self‐recognition interaction. The hexa­aqua­nickel complex molecules bridge these chains laterally, acting as molecular clamps that bring neighboring layers nearer than expected. As a result of this three‐dimensional arrangement, a short contact of 3.166 (5) Å is observed between two C atoms of two adjacent ribbons.     

Three 1,2,4‐triazole derivatives containing subtituted benzyl and benzyl­amino groups

The title compounds, 4‐benzyl­amino‐3‐(4‐methyl­benzyl)‐1H‐1,2,4‐triazol‐5(4H)‐one, C₁₇H₁₈N₄O, (I), 3‐(4‐methyl­benzyl)‐4‐(4‐methyl­benzyl­amino)‐1H‐1,2,4‐tri­azol‐5(4H)‐one, C₁₈H₂₀N₄O, (II), and 3‐(4‐chloro­benzyl)‐4‐(4‐methyl­benzyl­amino)‐1H‐1,2,4‐triazol‐5(4H)‐one, C₁₇H₁₇ClN₄O, (III), were obtained from the corresponding Schiff base in the presence of diglyme and NaBH₄. Each compound contains a 1,2,4‐triazole ring and two benzene rings, which are essentially planar. The molecules are linked by a combination of intermolecular N—H⋯O and N—H⋯N hydrogen bonds. Additionally, there is a weak π–π stacking interaction in (I), involving the benzene ring of the amino­benzyl group and the partially aromatic 1,2,4‐triazole moiety, with a centroid–centroid distance of 3.7397 (10) Å.     

Hexa­aqua­dodeca‐μ‐bromo‐octahedro‐hexatantalum bromide chloride octahydrate

The title compound, [Ta₆Br₁₂(H₂O)₆](Br_0.4Cl_1.6)·8H₂O, crystallizes in space group P. The structure contains two crystallographically independent [Ta₆Br₁₂(H₂O)₆]²⁺ cluster cations forming distinct layers parallel to the ab plane. The compound is isoconfigurational with the double salts [Ta₆Br₁₂(H₂O)₆]X₂·trans‐[Ta₆Br₁₂(OH)₄(H₂O)₂]·18H₂O (X = Cl, Br).     

The effect of molecular planarity on crystal non‐centrosymmetry in benzyl­idene–aniline derivatives

In the title compound, N‐(2‐methoxy­phenyl)‐4‐nitro­benzyli­deneamine, C₁₄H₁₂N₂O₃, the two phenyl rings make a dihedral angle of 48.0 (2)° and the nitro group is at an angle of 6.5 (1)° with respect to its attached phenyl ring. In the crystal structure, mol­ecules are related as centrosymmetric pairs through π–π interactions and are further connected through strong C—H?O hydrogen bonds [C?O 3.4259 (17) Å and C—H?O 167°], forming molecular stacks along [100]. These stacks associate further through longer C—H?O interactions, forming two‐dimensional networks. In the c direction, there are only weak van der Waals interactions. The relationship between the molecular planarity and its centrosymmetry is also briefly described.     

2,3‐Bis(4‐nitro­benzyl­thio)­maleo­nitrile

The maleo­nitrile moiety of the title compound, (2Z)‐2,3‐bis­[(4‐nitro­benzyl)­sulfanyl]­but‐2‐ene­di­nitrile, C₁₈H₁₂N₄O₄S₂, is almost planar. The two benzene rings are nearly parallel to each other and perpendicular to the maleo­nitrile plane. Intermolecular S?S and π–π interactions are observed in the crystal structure.     

N‐(p‐Chloro­benzyl­idene)­phenyl­amine N‐oxide

The crystal structure of the title compound, C₁₃H₁₀ClNO, confirms that it exists as a nitro­ne. The geometry about C=N is Z. The relevant torsion angles indicate trans and cis conformations around the nitro­ne bond.     

Hexa­methyl­enetetra­mine–4‐nitro­catechol–water (1/2/1)

In the title adduct, 1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]dec­ane–4‐nitro­benzene‐1,2‐diol–water (1/2/1), C₆H₁₂N₄·2C₆H₅NO₄·H₂O, the hexa­methyl­ene­tetra­mine mol­ecule acts as an acceptor of intermolecular O—H?N hydrogen‐bonding interactions from the water mol­ecule and the hydroxy groups of one of the two symmetry‐independent 4‐nitro­catechol mol­ecules. The structure is built from molecular layers which are stabilized by three intermolecular O—H?O, two intermolecular O—H?N and four intermolecular C—H?O hydrogen bonds. The layers are further interconnected by one additional intermolecular O—H?N and two intermolecular C—H?O hydrogen bonds.     

Two Aromatic Ester Organoimido Derivatives of Hexa­molybdate: Syntheses,Crystal Structures,and Spectroscopic Studies

Two alkylimido derivatives of hexamolybdate, (Bu₄N)₂[Mo₆O₁₈(≡N‐o‐COOCH₃C₆H₄)] ( 1 ) and (Bu₄N)₂[Mo₆O₁₈(≡N‐o‐COOCH₂CH₃C₆H₄)] ( 2 ), were synthesized in high purity and good yields by the reaction of [(C₄H₉)₄N]₄[α‐Mo₈O₂₆] and methyl anthranilate or ethyl‐o‐aminobenzoate hydrochloride with N,N′‐dicyclohexylcarbodiimide (DCC) as a dehydrating agent in dry acetonitrile solution, which were characterized by elemental analyses, IR, UV/Vis, and ¹H NMR spectroscopy as well as ESI‐MS, and single‐crystal X‐ray diffraction study. Compound 1 crystallizes in the monoclinic space group P2₁/n with one‐dimensional chain structure via intramolecular hydrogen bond. Compound 2 also crystallizes in the monoclinic space group P2₁/n with dimer structure by intramolecular hydrogen bonds and π–π interactions between the pairs of cluster anions.     

N‐(4‐Nitro­benzyl­idene)‐N′‐phenyl­hydrazine

Molecules of the title compound (alternative name: p‐nitro­benz­aldehyde phenyl­hydrazone), C₁₃H₁₁N₃O₂, adopt an E configuration about the azomethine C=N double bond. Molecules are approximately planar and the dihedral angle between the planes of the phenyl rings is 11.62 (9)°. Hydro­gen bonding links mol­ecules related by 4₂ screw axes to form helices with a pitch of 7.7186 (8) Å.     

Four tri­fluoro­methyl­nitro­benzene analogues

The crystal structures of four tri­fluoro­methyl­nitro­benzene analogues (CF₃)C₆H₃(NO₂)[C₄H₈N₂]R (where C₄H₈N₂ is piperazinyl and R is ethyl carboxyl­ate, CO₂C₂H₅, or phenyl, C₆H₅), have been determined, and their conformations and packing arrangements are compared. The four compounds are ethyl 4‐[4‐nitro‐2‐(tri­fluoro­methyl)­phenyl]­piperazine‐1‐car­boxyl­ate, (I), and ethyl 4‐[2‐nitro‐4‐(tri­fluoro­methyl)­phen­yl]piper­azine‐1‐carboxyl­ate, (II), both C₁₄H₁₆F₃N₃O₄, and 1‐­[4‐nitro‐2‐(tri­fluoro­methyl)­phenyl]‐4‐phenyl­piperazine, (III), and 1‐[2‐nitro‐4‐(tri­fluoro­methyl)­phenyl]‐4‐phenyl­piperazine, (IV), both C₁₇H₁₆F₃N₃O₂. All mol­ecules adopt a rod‐like conformation, while the asymmetric units of (II) and (IV) contain two unique mol­ecules that pack as monodirectional pairs. All mol­ecules pack with C—H⋯O/F close contacts to all but one of the O atoms and to five of the 18 F atoms.     

6‐(4‐Methoxy­benzyl­amino)­purin‐3‐ium chloride

The title compound, C₁₃H₁₄N₅O⁺·Cl⁻, belongs to the group of aromatic cytokinins. These compounds affect a variety of important physiological processes in plants and animals as well as in bacteria, including cell division, differentiation and senescence. The structure consists of a 6‐(4‐methoxy­benzyl­amino)­purinium cation and a Cl⁻ anion. The cation moiety exists as the N3‐protonated N7 tautomer. The cation contains nearly planar benzene and purine ring systems, with a dihedral angle of 77.46 (5)°. The crystal structure is stabilized by N_amino—H⋯N_purine hydrogen bonds connecting two adjacent mol­ecules, thus forming centrosymmetric dimers.     

The antiestrogen [2‐(4‐benzyl­phenoxy)­ethyl]­diethyl­ammonium chloride

The crystal structure of the title compound, C₁₉H₂₆NO⁺·Cl^? (common name: N,N‐diethyl‐2‐[(4‐phenyl­methyl)phenoxy]‐ethan­amine hydro­chloride), contains one mol­ecule in the asymmetric unit. The planes through the two phenyl rings are roughly perpendicular. Protonation occurs at the N atom, to which the Cl^? ion is linked via an N—H?Cl hydrogen bond. The mol­ecule adopts an eclipsed rather than extended conformation.