Tetrakis­(tri­phenyl­phosphine)silver(I) tetra­phenyl­borate aceto­nitrile solvate

In the title compound, [Ag{P(C₆H₅)}₄][B{P(C₆H₅)}₄]·CH₃CN, the Ag ion resides on a crystallographic twofold rotation axis and is tetrahedrally coordinated. There is a disparity between the two independent Ag—P distances. This is due, in part, to the temperature differences (all previous determinations are at room temperature) but also to the packing effects of various anions.     

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.     

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.     

Triethyl­ammonium tetra­phenyl­borate di­chloro­methane solvate

The crystal structure of the title compound, C₆H₁₆N⁺·C₂₄H₂₀B⁻·CH₂Cl₂, displays an N—H⋯π interaction between the triethyl­ammonium cation and a phenyl ring of the tetra­phenyl­borate anion. The distance between the ammo­n­ium H atom and the edge of this phenyl ring is 2.40 (3) Å. The ammonium group and the aryl moiety are nearly perpendicular, forming an intramolecular dihedral angle of 90.4°. A C—H⋯π interaction between the disordered di­chloro­methane solvate mol­ecule and a phenyl ring of the tetra­phenyl­borate anion is also present.     

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.     

Triclinic polymorphs of tri­phenyl­phosphine and tri­phenyl­phosphine sulfide

New triclinic polymorphs of tri­phenyl­phosphine, (I), and tri­phenyl­phosphine sulfide, (II), were crystallized. For the structure of (I), it is obvious that the highest peaks in the final difference electron‐density map are located at the `lone‐pair regions' of P atoms. We have observed this effect in two further phosphorous‐containing structures.     

Aqua­bis­(benzo­nitrile)(o‐benzo­quin­one di­imine)(tri­phenyl­phosphine)­ruthenium(II) bis­(tetra­fluoro­borate) hydrate

The Ru atom in the title compound, [Ru(C₆H₅CN)₂{P(C₆H₅)₃}{C₆H₄(NH)₂}(H₂O)](BF₄)₂·H₂O, has six‐coordinate octahedral geometry, with a trans arrangement of the tri­phenyl­phosphine ligand and the water mol­ecule. The asymmetric unit contains one complex cation, two tetra­fluoro­borate anions and one solvent water mol­ecule, which is disordered over two sites (ratio of occupancies 0.70:0.30).     

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.     

2,3,4,5‐Tetrakis­[(2‐hydroxy­ethyl)­thio]­tetra­thia­fulvalene tetra­fluoro­borate

The title complex, C₁₄H₂₀O₄S₈^+.BF₄^?, is a charge‐transfer complex with typical charges for the donor and anion of +1 and ?1, respectively. Two centrosymmetrically related donors form a face‐to‐face π‐dimer with a strong intermolecular S?S interaction. These π‐dimers stack along the a axis to form a donor column. The structure is extensively hydrogen bonded.     

Ethyl­tri­phenyl­phospho­nium perrhenate and (iodo­methyl)­tri­phenyl­phospho­nium perrhenate

Ethyl­tri­phenyl­phospho­nium perrhenate, (C₂₀H₂₀P)[ReO₄], and (iodo­methyl)­tri­phenyl­phospho­nium perrhenate, (C₁₉H₁₇IP)[ReO₄], have been crystallized from 2‐propanol. Both crystal structures consist of phospho­nium cations and perrhenate anions. The cations show the typical propeller‐like geometry. In both crystals, the positions of the nearly tetrahedral anions are stabilized by weak C—H⋯O hydrogen bonds, and for the latter compound, I⋯π interactions also occur.     

Chloro­bis­(tri­phenyl­phosphine)­nickel(I) tetra­hydro­furan solvate and an unsolvated trigonal phase of chloro­tris­(tri­phenyl­phosphine)­nickel(I)

In [NiCl(C₁₈H₁₅P)₂]·C₄H₈O, the Ni atom is coordinated by three ligands in a distorted trigonal–planar configuration, with a P—Ni—P angle of 111.52 (2)°. In [NiCl(C₁₈H₁₅P)₃], there are three independent mol­ecules in the asymmetric unit, with each Ni—Cl bond on a crystallographic threefold rotation axis. Each Ni centre is tetrahedrally bound. The Ni atoms in both compounds have a d⁹ configuration and a formal oxidation state of Ni^I. A comparison is made between the form of [NiCl(PPh₃)₃] presented here and that of a known toluene solvate.     

Phase change in tetra­phenyl­phospho­nium perchlorate

The title compound, C₂₄H₂₀P⁺·ClO₄^?, undergoes a sudden reversible phase change in the region of 173–180 K which involves ordering of three quarters of the perchlorate anions.     

Orthorhombic modification of tri­phenyl­tin 3‐ureidopropionate

The Sn atom in catena‐poly­[tri­phenyl­tin(IV)‐μ‐(3‐ureidopropionato‐O¹:O³)], [Sn(C₆H₅)₃(C₄H₇N₂O₃)]_n, is five‐coordinate and has a trans‐C₃SnO₂ trigonal‐bipyrmidal geometry arising from bridging through the O atom of the ureido fragment of an adjacent carboxyl­ate group. Infinite chains propagate helically along the c axis and adjacent chains are linked by N—H?O [N?O 2.851 (4) Å] hydrogen bonds into layers.     

Tetra­phenyl­arsonium tetra­iodo­thallate(III)

The As and Tl atoms in title compound, (C₂₄H₂₀As)[TlI₄], sit on fourfold inversion centres, resulting in a [TlI₄]^? anion with D_2d symmetry and a Tl—I bond length of 2.7691 (3) Å. The tetrahedral anion is tetragonally distorted, being flattened in the direction of the c axis of the tetragonal unit cell, so that the two unique I—Tl—I angles differ by about 9°. In contrast, the cation has S₄ symmetry and the tetrahedral coordination geometry of the As atom is very slightly stretched in the direction of the c axis.     

Host–guest‐like thi­amine–anion complexation in thia­minium bis­(tetra­fluoro­borate)

In the title compound, 3‐[(4‐amino‐2‐methyl‐5‐pyrimidin‐1‐io)methyl]‐5‐(2‐hydroxy­ethyl)‐4‐methyl­thia­zolium(2+) bis(tetra­fluoro­borate), C₁₂H₁₈N₄OS²⁺·2BF₄^?, the divalent thia­mine cation (in the F conformation) is associated with BF₄^? anions via two characteristic bridging interactions between the thia­zolium and pyrimidinium rings, i.e. C—H?BF₄^??pyrimidinium and N—H?BF₄^??thia­zolium interactions. Thi­amine mol­ecules are linked by N—H?O hydrogen bonds to form a helical chain structure.     

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

The title compound, [Mn(CF₃COO)₂(H₂O)₄], crystallizes in the monoclinic space group C2/c. At about 215 K, it undergoes a reversible phase transition, which leads to crystal twinning. The crystal structure of the high‐temperature phase was determined at 220 K. The Mn²⁺ ion lies on a twofold axis and is octahedrally coordinated by two monodentate tri­fluoro­acetate ligands in apical positions and by four equatorial aqua ligands, two of which lie on the twofold axis. Hydro­gen‐bonding interactions connect the complex mol­ecules, generating a three–dimensional network.     

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.     

trans‐(2‐Methyl­thio­benzoato‐O)phenylbis­(tri­phenyl­phosphine)­palladium(II), two conformational isomers

The title compound, trans‐[Pd(C₆H₅)(C₈H₇O₂S)(C₁₈H₁₅P)₂], crystallizes in two modifications differing only in the orientation of the 2‐methyl­thio­benzoato ligand. In both cases, this ligand binds to the metal centre via one O atom in a monodentate fashion. The only significant difference is a rotation about the C(Ph)—COO bond, with O—C—C—C torsion angles having values of 6.3 (7) and 157.3 (3)° in the two isomeric forms.     

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.