Na₂Fe(CN)₅(NO)·2D₂O at 11 and 293 K by X-ray, and at 15 K by neutron diffraction

Precise X-ray and neutron structural determinations of Na₂Fe(CN)₅(NO)·2D₂O performed at very low temperatures are presented. The X-ray and neutron diffraction positional and atomic displacement parameters agree very well. The [Fe(CN)₅(NO)]²⁻ anion has approximate octahedral stereochemistry.

Bismuth(V) iron(III) tris­(phosphate) oxide

Bi^V_0.4Fe^III₃O(PO₄)₃ exists as a branched polymeric chain of Fe atoms singly or doubly bridged by oxo and phosphate O atoms, in between which are found Bi sites.

Sodium trivanadium(III) bis­(sulfate) hexa­hydroxide

In the title compound, octahedrally coordinated vanadium and tetrahedral sulfate ions share corners to form layers that are held together by hydrogen bonds and by sodium ions, which are located between the layers.

Bis­(di-tert-butyl­thio­phosphinic iso­propyl­amidato-N,S)­nickel(II)

Di­chloro­bis­[2-(o-tolyl­iminio­methyl)­phenolato-O]­zinc(II)

Tetrameric indium trichloride, a new modification of a widely used compound

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

Polymeric di­aqua­tetra-μ-thio­cyanato-manganese(II)­mercury(II) bis­(N,N-di­methyl­acet­amide) solvate

(Ethanol-O)­tris­(nitrato-O,O′)­bis­(tri­phenyl­phosphine oxide-O)­cerium(III)

High-temperature phase of trans-tetra­aqua­bis­(tri­fluoro­acetato-O)­manganese(II)

Bis­(acridine-N)(nitrato-O,O′)silver(I)

Bis(1,5-di­aza­cyclo­octane-N,N′)nickel(II) dibromide

(Benzoxazole-2-thiol­ato-S)(benzoxazole-2-thione-S)­bis­(tri­phenylphosphine)copper(I)

Bis­[N-phenyl­(di­cyclo­hexyl­thiophos­phinoyl)­thio­methan­amido-S,S′]copper(II)

Intra- and intermolecular C—H⋯π interactions in bis­[benzyl 3-(fluoren-9-yl­idene)­dithio­carb­azato-N³,S]­nickel(II)

Two isostructural triboluminescent lanthanide complexes

Tri­azido­cobalt(III) complexes with tridentate amine ligands

Tris(2,6-di-tert-butyl-4-methyl­phenol­ato-O)(tri­phenyl­phosphine oxide-O)samarium(III)

cis-Di­chloro(di­methyl sulfoxide-S)(2-methoxypyridine-N)platinum(II)

4,5-Di­azafluoren-9-ol

Terephthal­aldehyde bis­(thio­semi­carba­zone) bis­(di­methyl­form­amide) solvate

Diels–Alder adducts of maleic anhydride and dienes: new compounds by crystallization

Tetracycline hydrochloride: a synchrotron microcrystal study

Ethyl methyl 1,4-di­hydro-4-(3-nitro­phenyl)-2,6-bis­(1-piperidylmethyl)­pyridine-3,5-di­carboxylate

3-Hydroxy­benz­aldehyde

Tetra­kis­(di­ethyl­amino)­phospho­nium bromide hemihydrate

Tris(2-methylphenyl)phosphonium tetra­chloroborate

4-Ethynyl-4-hydroxycyclohexan-1-one and 4-ethynyl-4-hy­droxy-2,3,5,6-tetra­methylcyclohexa-2,5-dien-1-one

Racemic 1,2-di­phenylbut-3-yn-2-ol

Disappearance of intramolecular stacking due to one-atom movement or increment of a `propyl­ene linker' in pyrazolo­[3,4-d]­pyrimidine-based flexible models

4-Vinyl­benzoic acid and 9-vinyl­anthracene

Benzo­[i]­naphtho­[c,d]­bicyclo­[5.4.1]dodecan-12-one

25,27-(6-Tosyl-3,9-dioxa-6-aza­undecane-1,11-diyldi­oxy)-26,28-(3,6,9-trioxaun­decane-1,11-diyldi­oxy)­calix­[4]­arene

Norfloxacin dihydrate

Marchantin M tri­methyl ether

A norbornenyl derivative with through-space ketone π-interaction

Unexpected dipivaloyl­ation of 9-li­thia­ted fluorene: formation of 1-(fluoren-9-yl­idene)-2,2-di­methyl­propyl pivalate

(1S,2R,2′S)- and (1S,2S,2′S)-1-phenyl-2-phenyl­thio-2-(tetra­hydro­pyran-2′-yl­thio)­ethanol diastereoisomers at 193 K

N-Propionyl-1,2-benzisoselenazol-3(2H)-one

1,21-Heni­cosanediol

Racemic and chiral 1-[N-(chloro­acetyl)carbamoylamino]-2,3-di­hydro-1H-inden-2-yl chloro­acetate

Phase change in tetra­phenyl­phospho­nium perchlorate

1D-3,4-Di-O-(di­phenyl­methylphos­pho­nio)-1,2,5,6-tetra-O-methyl-chiro-inositol diiodide

7,8-Di­phenyl-9-di­methyl­sulfido-10,11-μ-hydro-7,8-dicarba-nido-undecaborane(9)

2,3-Di­hydro-3-methyl-2-nitrimino-1,3-thiazole

N-[Bis(2,4,6-tri­methyl­phen­oxy)­phos­phinoyl]-P,P,P-tris­(2,4,6-tri­methyl­phen­oxy)phosphazene

Intermolecular O—H⋯O hydrogen bonding in the three independent molecules of (2S)-3-(4-hydroxyphenyl)-2-(1-oxoisoindolin-2-yl)­propanoic acid

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

The cation of the title compound displays a rhomboidal geometry for the Au atoms, with short Au⋯Au distances of 3.104 (2) and 3.185 (1) Å. 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.

Tetra­aqua(5-fluoro­uracil-1-acetato-O)copper(II) tetra­hydrate

In the title complex, the Cu atom, which is located on an inversion centre, is in the centre of a distorted octahedral geometry, with six O atoms provided by two monodentate carboxyl­ate groups and four water mol­ecules. Intra- and intermolecular hydrogen bonds make up a three-dimensional network.

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

The previously reported title compound (R = 0.12, one of water mol­ecules disordered) has been redetermined (R = 0.041, no disorder). The complex has pseudo-octahedral geometry around the Fe^III atom. There is extensive hydrogen bonding involving the water mol­ecules and the hydro­xamate ligands.

cis-μ-Chloro-μ-p-toluene­thiol­ato-bis­[chloro­(tri­ethyl­phos­phine)­palladium]

The title compound, prepared in the course of synthetic studies of organochalcogenide compounds of Pd^II, has bridging chloro and aryl­thiol­ato groups, with the phosphines being trans to the bridging chloro group. The four-membered metallocyclic Pd₂ClS ring is unexpectedly non-planar, with a dihedral angle of 133.8 (1)° between the PdCl₂SP coordination planes.

Di­thio­cyanatobis­[4,4,5,5-tetra­methyl-2-(4-pyridyl-κN)-1H-imidazoline-1-oxyl]­zinc(II)

The preparation and crystal structure of the title complex are described. The Zn^II ion adopts a distorted tetrahedral coordination. It is bonded to two thio­cyanate and two pyridyl N atoms.

trans-Tetra­chloro­bis­(4-methyl­pyridine)­germanium(IV)

The structure of the title compound is the first example of an addition compound of GeCl₄ with two aromatic nitro­gen bases. The environment around the Ge atom can be described as a slightly distorted octahedron with the 4-methyl­pyridine ligands occupying axial positions and the four chloro ligands in the equatorial plane. The structure of the title compound is isomorphous with the corresponding silicon halides.

Complexes of germanium bromides with 4-picoline and 3,4-lutidine

The reactions of GeBr₄ with 4-methyl­pyridine and 3,4-di­methyl­pyridine lead to tetra­bromo­bis(4-methyl­pyridine)­germanium, (I>), and tetra­bromo­bis(3,4-di­methyl­pyridine)­germanium, (II>), respectively. These structures show the same features as the corresponding silicon complexes.

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

The title copper complex has a center of symmetry and a distorted octahedral coordination, with four N atoms in equatorial positions and water mol­ecules in the apical sites. The water mol­ecule of crystallization is hydrogen bonded to the deprotonated carboxyl­ate group of the ligand.

A three-dimensional open-framework zinc arsenate, (C₄H₁₂N₂)₂[Zn₇(AsO₄)₆­(H₂O)₂]

The title compound is a new open-framework zinc arsenate, which is isostructural with the zinc phosphate UiO-17. The open three-dimensional anionic framework, made up of vertex-sharing AsO₄ tetrahedra, ZnO₄ tetrahedra and ZnO₅ trigonal bipyramids, contains a two-dimensional eight-ring channel system in which diprotonated piperazinium cations reside.

Aqua­bis­(crotonato)­bis­(pyridine)­copper(II)

The title compound crystallizes as a monomer, with the copper ion in a pentacoordinated square-pyramidal environment, bisected by a twofold axis passing through the metal atom and the apex. The mol­ecules organise in chains connected by hydrogen bonds running along the unique b axis.

Fumaric acid–trans-cinnamamide (1/2)

In the title adduct, fumaric acid has a centre of symmetry and is connected to two trans-cinnam­amide mol­ecules through cyclic hydrogen bonds. A single-crystal photoirradiation promoted the conformational disorder of the fumaric acid.

4,5-Di­chloro­phthalic acid–trans-cinnam­amide (1/2) and 3,4,5,6-tetra­chloro­phthalic acid–trans-cinnam­amide (1/2)

In the two title adducts, (I>) and (II>), respectively, the di­carboxyl­ic acid is connected to two cinnam­amide mol­ecules through cyclic hydrogen bonds. The arrangement of the C=C bonds of neighbouring cinnam­amide mol­ecules is twisted.

Benzene-1,2,4,5-tetra­carboxylic acid–trans-cinnam­amide (1/2)

In the title adduct, a hydrogen-bonded unit of the acid and two cinnam­amide mol­ecules has a crystallographic twofold axis parallel to b, and the acid molecules are linked by cyclic hydrogen bonds to form a flat zigzag along c.

3α-Tosyl­oxy­methyl­tropane(N⁸–B)borane

In the title compound, the tosyl­oxy­methyl substituent is in an endo position; the BH₃ group is equatorial and the (N-bonded) methyl group is axial, relative to the six-membered heterocycle. The N—B bond of 1.649 (8) Å is one of the longest known.

A ter­phenyl halide series: 2,6-Trip₂­H₃C₆X (Trip = 2,4,6-triiso­propyl­phenyl; X = Cl, Br, I)

The three title sterically encumbered ter­phenyl halides are isomorphous and isostructural with a plane of symmetry through the centre of the mol­ecule. The C—X bond distances are 1.745 (3) [X = Cl, (I)], 1.910 (4) [X = Br, (II)] and 2.102 (6) Å [X = I, (III)].

Redetermination of ternifoline-C at 150 K

The relative molecular stereochemistry and crystal packing of the diterpenoid ternifoline-C at 150 K are similar to the results of a previous study probably using room-temperature data.

5-Fluoro-1-octanoyl­uracil

The 5-fluoro­pyrimidine-2,4(1H,3H)-dione moiety of the title compound is similar to the known structure of 1-acetyl-5-fluoro­uracil. The 1-octanoyl group and the 5-fluoro­uracil moiety are essentially coplanar with the acyl carbonyl group, which is oriented towards the ring C—H group and away from the nearer ring carbonyl group.

N-(4-Methyl­phenyl)-N-(5-nitro­furfuryl)-N-prop-2-ynyl­amine

In the title compound, the furan ring is inclined at an angle of 84.35 (4)° to the phenyl ring. The crystal structure is dominated by van der Waals forces.

meso-2,2′-Di­phenyl-3,3′,4,4′-tetra­hydro-2,2′-bi­furan-5,5′(2H,2′H)-dione

The crystal structure of the title compound contains a crystallographic inversion center. The C—C bond linking the two halves of the mol­ecule is slightly elongated at 1.577 (3) Å.

Tetra­kis­(3,5-di­methyl­pyridine)­dihydrido­silicon dibromide bis­(aceto­nitrile) solvate and 3,5-di­methylpyridinium bromide

In the course of an attempt to synthesize tetrakis(3,5-di­methyl­pyridine)­dihydridosilicon dibromide, crystals of its aceto­nitrile disolvate, (I>), and of 3,5-di­methyl­pyridinium bromide, (II), were obtained in the same reaction flask. They have both been structurally characterized.

Methyl 2-methyl-6-methyl­thio-1,3-dioxo-4-[(2,3,4,6-tetra-O-acetyl-β-D-gluco­pyran­osyl)­amino]-2,3-di­hydro-1H-pyrrolo­[3,4-c]­pyridine-7-carboxyl­ate

The title compound has peripheral acetyl and carbo­methoxy groups which show disorder. The absolute structure, known from the starting materials, was confirmed by the analysis.

2,4,6-Tri­methyl­phenol

A one-dimensional connectivity of strong hydrogen bonds in this simple structure results in a b axis which is very short compared with a and c. This provides a perfect example for the concept of periodic bond-chain vectors.

1,3,5-Tri-p-tolyl­biuret

In the title compound, the biuret moiety is nearly planar and an intramolecular hydrogen bond completes a six-membered ring. Each phenyl ring of the p-tolyl groups is twisted by approximately 60–80° with respect to the others.

Hydrogen bonding in N,N,N′,N′-tetra­methyl­ethyl­ene­diammonium bis­(benzene­selenol­ate)

The title crystal structure reveals hydrogen bonding between the benzene­seleno­late anions and the tetra­methyl­ethyl­enedi­ammonium cations.

Redetermination of 1,3,5-tri­chloro-2,4-di­nitro­benzene

The crystal structure at 153 K of the title compound, an intermediate in the synthesis of 1,3,5-tri­chloro-2,4,6-tri­nitro­benzene, shows no major deviations from the previously reported structure at 295 K other than the expected contraction of the cell volume.

2,4,6-Tris­[2-(tri­methyl­silyl)­ethynyl]-1,3,5-triazene: a novel precursor to C–N two-dimensional structures

The title structure consists of separate mol­ecules arranged in sheets parallel to the ab plane. In each mol­ecule, the central (CN)₃ ring, the ethynyl units, and the Si atoms lie in the same plane. Typical C—C and C—N bond distances are 1.197 (5) and 1.42 (4) Å, respectively. The angles inside the (CN)₃ ring range from 114 (3) to 125 (3)° and the acetyl­enic branches are nearly linear.

2-Amino-6-chloro-4-(1-phenyl­ethyl­amino)­pyrimidine

The structure of the title compound comprises a racemic mixture of chiral mol­ecules associated by N—H⋯N hydrogen-bonding interactions. The dihedral angle between the two rings is 77.90 (6)°.

4-Anilino-3-nitro­pyridine

The structure of the title compound comprises two unique mol­ecules that separately form hydrogen-bonded polymer chains via N—H⋯N interactions. Molecular independence arises due to a difference in the dihedral angles between the linked rings, i.e. 52.19 (4) and 46.17 (5)°.

4,6-Di­chloro-2-(methyl­thio)­pyrimidine

The structure of the title compound comprises six symmetry unique mol­ecules that vary only slightly in their N—C—S—C torsion angle. All the mol­ecules are planar to within less than 3.1°.

2-Chloro-3-morpholino-1,4-naphtho­quinone

The structure of the title compound comprises essentially planar mol­ecules stacked parallel to the a axis. C—H⋯O hydrogen-bonding interactions exist to both naphtho­quinone O atoms and the Cl atom, but not to the morpholine O atom.

24(R)-Acetyl­oxy-1α,2α-ep­oxy­cholesta-4,6-dien-3-one hydrate. Erratum

Erratum to Acta Cryst. (2000), C56, e307–308.