Di­methyl­phenyl­sulfonium tri­fluoro­methane­sulfonate and methyl­di­phenyl­sulfonium tri­fluoro­methane­sulfonate

The bonding geometry of sulfur in the cations of the title compounds, C₈H₁₁S⁺·CF₃SO₃^? and C₁₃H₁₃S⁺·CF₃SO₃^?, respectively, is similar and is independent of the ratio of the Me/Ph substituents. As expected, in both cations, the S—Ph bonds are somewhat shorter than the S—Me bonds. In both crystal structures, the interaction between cations and anions is similar.     

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.     

Betainium tri­fluoro­acetate

The title compound, C₅H₁₂NO₂⁺·C₂F₃O₂^? or BET⁺·CF₃COO^? [BET is tri­methyl­glycine (betaine); IUPAC: 1‐carboxy‐N,N,N‐tri­methyl­methanaminium inner salt], contains pairs of bet­ainium and tri­fluoro­acetate ions forming a dimer bridged by a strong hydrogen bond between the carboxyl and carboxyl­ate groups of the two ions. The molecular symmetry of the cation is close to C_s, with protonation occurring at the carboxy O atom positioned anti to the N atom. The tri­fluoro­acetate anions are disordered over two positions. In one, the conformation of the CF₃ group is staggered with respect to the carboxyl­ate group, in the other, it is close to an eclipsed conformation. The sole hydrogen bond present in the structure is the strong O—H?O bond between the anion and the cation.     

Sarcosinium tri­fluoro­acetate

The title compound, C₃H₈NO₂⁺·C₂F₃O₂^?, crystallizes in space group C2/c. The main N—C—COOH skeleton of the protonated sarcosine mol­ecule is almost perfectly planar. The tri­fluoro­acetate anion has a staggered conformation and typical bond distances and angles. The CF₃ group is probably slightly disordered. The structure is stabilized by an extensive network of strong O—H?O hydrogen bonds and weaker N—H?O bonds.     

Conformation of cationic N,N‐di­methyl­glycine in di­methyl­glycinium tri­fluoro­acetate

In the title compound, C₄H₁₀NO₂⁺·C₂F₃O₂^?, the main N—C—COOH skeleton of the protonated amino acid is nearly planar. The C=O/C—N and C=O/O—H bonds are syn and the two methyl groups are gauche to the methyl­ene H atoms. The conformation of the cation in the crystal is compared to that given by ab initio calculations (Hartree–Fock, self‐consistent field molecular‐orbital theory). The tri­fluoro­acetate anion has the typical staggered conformation with usual bond distances and angles. The cation and anion form dimers through a strong O—H?O hydrogen bond which are further interconnected in infinite zigzag chains running parallel to the a axis by N—H?O bonds. Weaker C—H?O interactions involving the methyl groups and the carboxy O atoms of the cation occur between the chains.     

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

The title compound, C₆HCl₃N₂O₄, is an intermediate in the synthesis of 1,3,5‐tri­chloro‐2,4,6‐tri­nitro­benzene. The crystal structure at 153 K shows no major deviations from the previously reported structure at 295 K other than the expected contraction of the a and c axes and, correspondingly, the β angle.     

(η5‐Cyclo­penta­dienyl)(p‐fluoro­phenoxo)(nitro­syl)(tri­methyl­silyl­methyl)­molybdenum(II)

The title complex, [Mo(C₅H₅)(C₆H₄FO)(C₄H₁₁Si)(NO)], is formed by reacting CpMo(NO)(CH₂SiMe₃)₂, where Cp is cyclo­penta­dienyl, with one equivalent of p‐FC₆H₄OH. The complex exhibits the expected piano‐stool molecular structure, with a linear nitro­syl ligand [Mo—N—O 168.2 (2)°] having Mo—N and N—O distances of 1.764 (2) and 1.207 (3) Å, respectively. The phenoxo Mo—O distance of 1.945 (2) Å is suggestive of some multiple‐bond character.     

The twinned structure of ferricenyl­tri­fluoro­borate

Crystals of the title compound, [Fe(C₅H₅)(C₅H₄BF₃)], are monoclinic and twinned. The twinning initially resulted in a misleading unit‐cell assignment. The formal oxi­dation state of Fe is 3+, and the crystal packing consists of intermolecular C—H...F and π–π interactions.     

Methyl­tri­phenyl­stibonium tetra­fluoro­borate

In the title compound, [Sb(CH₃)(C₆H₅)₃]BF₄, there are four independent cations and anions in the asymmetric unit. The geometry around the Sb atom is distorted tetrahedral, with Sb—C distances in the range 2.077 (4)–2.099 (10) Å and angles at the Sb atom in the range 103.3 (3)–119.0 (4)°.     

Rubidium bis­(tri­fluoro­methane­sulfonyl)­imidate dioxane disolvate

The bis­(tri­fluoro­methane­sulfonyl)­imidate anion crystallizes with Rb as the title dioxane 1:2 solvate, Rb⁺·CF₃SO₂NSO₂CF₃⁻·2C₄H₈O₂, with the anion in a transoid conformation, as opposed to the cisoid form typically seen when there are significant cation–anion interactions. The Rb^I cation is eight‐coordinate, interacting with one anion in a chelating fashion and with two other anions through the remaining sulfonyl O atoms. The latter interactions link ion pairs through the formation of Rb₂O₂ dimers about inversion centers at (0, , 0) and (, , 0), forming extended columns which run parallel to the a axis of the unit cell. Rb–dioxane bridges crosslink these salt columns in the (010), (001) and (011) directions, resulting in a three‐dimensional network solid. One dioxane solvent mol­ecule is disordered over two half‐occupancy sites.     

The centrosymmetric dimer of di­chloro­(tri­methyl­siloxy)­aluminium

The title mol­ecule is dimeric, i.e. di‐μ‐tri­methyl­siloxy‐bis­(di­chloro­aluminium), [Al₂Cl₄(C₃H₉Si)₂], and possesses exact crystallographic inversion symmetry. The O atoms of the tri­methyl­siloxy groups bridge the two Al atoms to form a four‐membered ring. The Si—O bond distance [1.711 (3) Å], the Al—O mean bond distance [1.806 (4) Å] and the mean Si—C bond distance [1.875 (6) Å] appear to agree well with standard data. Mean values for C—Si—C, O—Si—C, and Si—O—Al angles are 112.9 (3), 105.8 (2), and 131.8 (2)° repectively. The two ring angles O—Al—O and Al—O—Al are 84.43 (16) and 95.57 (16)°, respectively.     

1‐(4‐Chloro­phenyl­sulfanyl)‐2‐nitro‐4‐(tri­fluoro­methyl)­benzene and 1‐(4‐chloro­phenyl­sulfanyl)‐4‐nitro‐2‐(tri­fluoro­methyl)­benzene

Two chemical isomers of 3‐nitro­benzotrifluoride, namely 1‐(4‐chloro­phenyl­sulfanyl)‐2‐nitro‐4‐(tri­fluoro­methyl)­benzene, C₁₃H₇ClF₃NO₂S, (I), and 1‐(4‐chloro­phenyl­sulfanyl)‐4‐nitro‐2‐(tri­fluoro­methyl)­benzene, C₁₃H₇ClF₃NO₂S, (II), have been prepared and their crystal structures determined with the specific purpose of forming a cocrystal of the two. The two compounds display a similar conformation, with dihedral angles between the benzene rings of 83.1 (1) and 76.2 (1)°, respectively, but (I) packs in P while (II) packs in P2₁/c, with C—H⋯O interactions. No cocrystal could be formed, and it is suggested that the C—H⋯O associations in (II) prevent intermolecular mixing and promote phase separation.     

Complex of cobalt(II) bromide with hexa­methyl­phospho­ric tri­amide

The title compound, di­bromo­bis­[tris­(di­methyl­amino)­phos­phine oxide]­cobalt(II), [CoBr₂(C₆H₁₈N₃OP)₂], displays tetrahedral coordination about cobalt. The mol­ecule has twofold crystallographic site symmetry. The short P—N bonds and the planarity of the di­methyl­amino groups indicate the importance of dπ–pπ interactions. One of the NMe₂ groups has an irregular conformation about the P—N bond and deviates from planarity. It is ascribed to the steric hindrance induced by coordination at the O atom of hexa­methyl­phospho­ric tri­amide.     

Diacetatobis­(tri­methyl­ene­thio­urea)­zinc(II) monohydrate

In the title compound, [Zn(CH₃COO)₂(C₄H₈N₂S)₂]·H₂O, the Zn atom is tetrahedrally coordinated in the ZnO₂S₂ form. N—H?O and O—H?O intramolecular and intermolecular hydrogen bonds are formed by the four N atoms and the water mol­ecule. N—H?O intermolecular hydrogen bonds and C—H?S and C—H?O intermolecular interactions interconnect columns formed by the mol­ecules into layers. Adjacent layers are then linked by other N—H?O and O—H?O intermolecular hydrogen bonds to form a three‐dimensional framework throughout the structure. The orientations of the acetate planes are such that the Zn atom lies within them.     

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

The title compound, C₄₅H₅₅NO₆P₂, consists of an acyclic P=N—P(O) monophosphazene chain and five bulky 2,4,6‐tri­methyl­phenoxy side groups which predominantly determine the molecular shape. Although the P—N single [1.586 (3) Å] and P=N double [1.517 (3) Å] bonds are significantly different from each other, both are substantially shorter than the ideal P—N single bond. The P—N—P angle [146.0 (2)°] corresponds to the upper limit reported for acyclic phosphazene derivatives in the literature.     

The 1:1 complex of 4‐nitro­phenol and 4‐methyl­pyridine

4‐Nitro­phenol and 4‐methyl­pyridine form a 1:1 hydrogen‐bonded dimer, C₆H₅NO₃.C₆H₇N, with the mol­ecules linked by an O—H?N hydrogen bond [O?N 2.668 (2) Å]. The dihedral angle between the phenyl and pyridine ring is 57.8 (4)°. The dimers pack in a herring‐bone structure in the crystal lattice.     

Bis­[N,N′‐bis(2,4,6‐tri­methyl­phenyl)‐1,2‐ethanediyl­idenedi­amine]copper(I) tetra­fluoro­borate

In the title compound, [Cu(C₂₀H₂₄N₂)₂]BF₄, the complex cation adopts a distorted tetrahedral structure, the dihedral angle between the least‐squares planes of the chelating ligand backbones being 51.1 (2)°. This flattening of the tetrahedral coordination sphere may be driven by the presence of intramolecular π–π stacking interactions between mesityl groups on adjacent ligands.     

The effects of substitution on tetrakis­(substituted imidazole)­copper(II) tri­fluoro­methane­sulfonates

The organic ligands 4‐methyl‐1H‐imidazole and 2‐ethyl‐4‐methyl‐1H‐imidazole react with Cu(CF₃SO₃)₂·6H₂O to give tetrakis(5‐methyl‐1H‐imidazole‐κN³)­cop­per(II) bis­(tri­fluoro­methane­sulfonate), [Cu(C₄H₆N₂)₄](CF₃SO₃)₂, and aqua­tetrakis(2‐ethyl‐5‐methyl‐1H‐imidazole‐κN³)copper(II) bis(tri­ fluoro­methane­sulfonate), [Cu(C₆H₁₀N₂)₄(H₂O)](CF₃SO₃)₂. In the former, the Cu atom has an elongated octahedral coordination environment, with four imidazole rings in equatorial positions and two tri­fluoro­methane­sulfonate ions in axial positions. This conformation is similar to those in the analogous complexes tetrakis­(imidazole)­cop­per(II) tri­fluoro­methane­sulfonate and tetrakis(2‐methyl‐1H‐imidazole)­cop­per(II) tri­fluoro­methane­sulfonate. In the second of the title compounds, the ethyl groups block the central Cu atom, and a square‐pyramidal coordination environment is formed around the Cu atom, with the substituted imidazole rings in the basal positions and a water mol­ecule in the axial position.     

Bis­(iso­propyl­amino)­methyl­carbenium tetrakis­(penta­fluoro­phenyl)­gallate

The title compound, [MeC(NHⁱPr)₂][Ga(C₆F₅)₄] crystallizes as discrete ions forming interionic hydrogen bonds of the type N—H?F.     

2,2‐Di­methyl‐1‐(2,4,6‐tri­nitro­phenyl)­hydrazine

The title mol­ecule (DMPH‐H), C₈H₉N₅O₆, was investigated to provide comparison with 2,2‐di­phenyl‐1‐picryl­hydrazine, which unlike DMPH‐H is readily oxidizable to form a well known stable free radical (DPPH). The structure shows essential differences in the configuration of the hydrazine‐N atoms, the ortho‐nitro group orientations and the crystal packing. The bond angles of the di­methyl­amino N atom [107.90 (13), 108.96 (12) and 112.21 (13)°] are consistent with a tetrahedral N atom and sp³ hybridization.