3,5‐Di­methyl‐4‐(2,4,6‐tri­methyl­phenyl­diazenyl)­phenol

In the title compound, C₁₇H₂₀N₂O, (I), the dihedral angle between the two phenyl rings is 15.69 (6)°. An intermolecular hydrogen‐bonding association exists between the hydroxy group and one of the azo N atoms.     

2,6‐Di­methyl‐4‐(phenyl­diazenyl)­phenol

The crystal structure of the title compound, C₁₄H₁₄N₂O, determined at 293 K, shows that the mol­ecule is approximately planar in the solid state and that the aromatic rings have a trans configuration with respect to the azo double bond, as found for other diazene derivatives. The packing can be described as a polymeric arrangement of mol­ecules linked through O—H⋯N and C—H⋯O hydrogen bonds and close contacts. These intermolecular interactions result in the formation of infinite chains parallel to the b axis.     

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.     

(N,N‐Di­iso­propyl­di­thio­carbamato‐S,S′)­bis­(tri­phenyl­phosphine‐P)­gold(I) butane solvate

In the crystal structure of the title complex, [Au(C₇H₁₄NS₂)(C₁₈H₁₅P)₂]·C₄H₁₀, the Au atom is in a distorted tetra­hedral environment consisting of the two P atoms of the tri­phenyl­phosphine ligands and the two S atoms of the diiso­propyl­thio­carbamate ligand. The molecular structure and packing are stablized by van der Waals interactions.     

Chloro(1‐{3‐[2‐(di­phenyl­phos­phanyl‐κP)­ethyl]‐η6‐benzyl}‐3,5‐di­methyl‐1H‐pyrazole‐κN2)­ruthenium(II) tri­fluoro­methane­sulfonate

To address the question of the role of chirality at the metal in enantioselective catalysis, a pseudo‐tetrahedral three‐legged piano‐stool complex has been prepared, i.e. [RuCl(C₂₆H₂₇N₂P)](CF₃SO₃). Anchoring a phosphine and a pyrazole tether to an arene (PArN) yields, after η⁶:η¹:η¹ coordination to ruthenium, [{η⁶:η¹:η¹‐(PArN)}RuCl]⁺ as a 1:1 mixture of enantiomers. Unfortunately, all attempts to resolve the enantiomers failed. The structure solution revealed the presence of racemic crystals.     

[N,N‐Bis(2‐hydroxy­ethyl)­di­thio­car­bamato‐S]­bis­(tri­phenyl­phosphine‐P)­copper(I) tri­phenyl­phosphine solvate

In the title compound, [Cu(C₅H₁₀NO₂S₂)(C₁₈H₁₅P)₂]·C₁₈H₁₅P, the Cu atom is in a distorted tetrahedral coordination, with two tri­phenyl­phosphine P atoms and two S atoms from an N,N‐bis(2‐hydroxy­ethyl)­di­thio­carbamate ligand occupying the vertices. The crystal structure is characterized by alternate layers of complex and tri­phenyl­phosphine mol­ecules.     

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

In the title compound, C₁₆H₂₅B₉S, there are two crystallographically independent mol­ecules, and the conformations of the phenyl and SMe₂ substituents indicate some intramolecular steric crowding. The bridging H atom is asymmetrically disposed. The title compound is a precursor to a crowded vertex‐labelled nido carborane ligand important in establishing the mechanism of isomerization of icosahedral heteroboranes.     

(Acetonitrile){2,6‐bis­[1‐(2‐ethyl‐6‐methyl­phenyl­imino)­ethyl]­pyridine}­dichloro­ruthenium(II) dichloro­methane hemisolvate: a chain of edge‐fused R66(24) rings

In the title compound, [RuCl₂(C₂H₃N)(C₂₇H₃₁N₃)]·0.5CH₂Cl₂, the Ru^II ion is six‐coordinated in a distorted octa­hedral arrangement, with the two Cl atoms located in the apical positions, and the pyridine (py) N atom, the two imino N atoms and the acetonitrile N atom located in the basal plane. The dichloromethane solvent mol­ecule lies on a twofold axis. The two equatorial Ru—N_imino distances are almost equal (mean 2.089 Å) and are substantially longer than the equatorial Ru—N_py bond [1.914 (4) Å]. It is observed that the N_imino—M—N_py bond angle for the five‐membered chelate rings of pyridine‐2,6‐diimine complexes is inversely related to the magnitude of the M—N_py bond. The title structure is stabilized by intra‐ and inter­molecular C—H⋯Cl hydrogen bonds. The inter­molecular hydrogen bonds form an R₆⁶(24) ring and a chain of edge‐fused rings running parallel to the [001] direction.     

cis‐Di­phenyl­bis(1,3,5‐tri­aza‐7‐phospha­adamantane‐κP)platinum(II)

The structure of the title compound, [Pt(C₆H₅)₂(C₆H₁₂N₃P)₂] or [Pt(Ph)₂(PTA)₂] (where Ph is phenyl and PTA is 1,3,5‐tri­aza‐7‐phosphaadamantane), is discussed. Selected geom­etric parameters are: Pt—P = 2.2888 (16) and 2.2944 (17) Å, Pt—C = 2.052 (5) and 2.064 (6) Å, C—Pt—C = 84.6 (2)° and P—Pt—P = 99.28 (6)°. The effective cone angle for the PTA ligands was calculated as 113°.     

cis‐Di­chloro­(di­methyl­aminomethyl­ene)­(tri­phenyl­phosphine)palladium(II) acetone solvate

The synthesis and X‐ray structural analysis of the title compound, [PdCl₂(C₃H₇N)(C₁₈H₁₅P)]·C₃H₆O, are described. The crystal structure contains discrete monomeric mol­ecules of the carbene complex and solvent mol­ecules separated by normal van der Waals distances. The Pd atom is four‐coordinate in an essentially square‐planar environment, with the chlorine ligands mutually cis; Pd—P = 2.2495 (7), Pd—Cl = 2.3508 (7) and 2.3600 (7), Pd—C 1.948 (2) and N—C(carbene) 1.274 (3) Å.     

(o‐Benzo­quinone di­imine‐N,N′)dichlorobis(tri­phenyl­phosphine‐P)ruthenium(II) 1.33‐methanol 0.33‐di­chloro­methane solvate

The Ru atom in the title compound, [RuCl₂{P(C₆H₅)₃}₂{C₆H₄(NH)₂}]·1.33CH₃OH·0.33CH₂Cl₂, shows a six‐coordinate octahedral geometry, with a trans arrangement of the tri­phenyl­phosphine groups. One and a half mol­ecules of complex, two mol­ecules of methanol and a half mol­ecule of di­chloro­methane form the asymmetric unit, with crystallographic twofold rotation symmetry for the complex mol­ecule in a special position.     

trans‐Di­iodo­bis(1,3,5‐tri­aza‐7‐phosphaadamantane)­platinum(II)

The crystal structure of the title compound, trans‐[PtI₂(C₆H₁₂N₃P)₂], describes one of the few platinum(II) complexes containing two of the water‐soluble 1,3,5‐tri­aza‐7‐phosphaadamantane ligands reported to date. The complex crystallizes on an inversion centre with the most important bond lengths and angles being Pt—P 2.3128 (12) Å, Pt—I 2.6022 (6) Å, P—Pt—I 90.94 (3)° and P′—Pt—I 89.06 (3)°.     

[2‐(Anilino­methyl)­phenyl]­di­phenyl­phosphine and {2‐[(N‐methyl­anilino)­methyl]­phenyl}di­phenyl­phosphine

The title compounds, Ph₂PCH₂N(H)Ph or C₂₅H₂₂NP and Ph₂PCH₂N(CH₃)Ph or C₂₆H₂₄NP, respectively, are isomorphous, with calculated theoretical Tolman angles of 174 and 182°.     

Di­bromo­[(–)‐sparteine‐κ2N,N′]­zinc(II)

In the title compound, di­bromo­[(6R,7S,8S,14S)‐1,3,4,7,7a,8,9,10,11,13,14,14a‐dodeca­hydro‐7,14‐methano‐2H,6H‐dipyrido­[1,2‐a:1′,2′‐e][1,5]­diazo­cine‐κ²N,N′]­zinc(II), [ZnBr₂(C₁₅H₂₆N₂)], the chiral nitro­gen‐chelating alkaloid (?)‐l ‐sparteine acts as a bidentate ligand, with two bromide ligands occupying the remaining coordination sites, producing a slightly distorted tetrahedral structure. The dihedral angle between the N—Zn—N and Br—Zn—Br planes is 82.4 (1)°. The distortion of the tetrahedral coordination is demonstrated by the fact that the midpoint of the N?N line does not lie in the Br—Zn—Br plane, but is tilted towards one of the N atoms by 0.164 Å. Similarly, the midpoint of the Br?Br line is tilted towards one of the Br atoms by 0.117 Å.     

μ‐Oxo‐bis­[(2,3,12,13‐tetra­bromo‐5,10,15,20‐tetra­phenyl­porphyrinato)­iron(III)] bis­(di­chloro­methane) solvate

The precise structure of the title compound, [Fe₂O(C₄₄H₂₄Br₄N₄)₂]·2CH₂Cl₂, is reported. The Fe—N distances are non‐equivalent in pairs because of the asymmetric peripheral substitution; the values are 2.098 Å to the brominated rings and 2.041 Å to the other two rings. The Fe—O bond distance is 1.7583 (4) Å. The mol­ecule has required twofold symmetry so that there is one unique porphyrin macrocycle and one Fe—O bond length in contrast to a previous report on the same species.     

[2‐(1H‐Inden‐3‐yl)­ethyl]­di­phenyl­phos­phine–borane

The title compound, C₂₃H₂₄BP, crystallizes in the centrosymmetric space group P2₁/c, with one mol­ecule in the asymmetric unit. The indene moiety is essentially planar. The P—B bond length is 1.923 (3) Å, which is within the expected range.     

Di­cyano{[(1S)‐(1‐phenyl­ethyl)­aziridin‐2‐yl]­methano­lato‐κ2N,O}boron

In the title compound, C₁₃H₁₄BN₃O, the aziridine ring is an almost equilateral triangle, the C—C distance being slightly shorter than the C—N distances, probably because of the dative B—N bond. The five‐membered ring, composed of two C atoms and N, B and O atoms, is fused with the aziridine ring to form a six‐membered ring with a chair conformation.     

(p‐Nitro­benzoato)­tri­phenyl­tin at 298 K

The structure at 298 K described here, [Sn(C₆H₅)₃(C₇H₄NO₄)], completely confirms the results at 173 K obtained previously [Weng, Das & Robinson (1990), Malays. J. Sci. 12 , 57]. In both structures, weak interaction between Sn and the carbonyl O atom of the benzoate group provides a distorted trigonal‐pyramidal environment at the Sn atom derived from its pseudo‐tetrahedral primary coordination in both mol­ecules of the asymmetric unit.     

Di­chloro­bis(1,2‐phenyl­enedi­amine)­nickel(II)

The title compound, [NiCl₂(C₆H₈N₂)₂], contains centrosymmetric mol­ecules with two phenyl­ene­di­amine ligands coordinated in a bidentate fashion. The Ni—N distances are 2.088 (1) and 2.096 (1) Å, and the Ni—Cl distance of 2.4635 (4) Å. The plane of each phenyl­enedi­amine mol­ecule makes a dihedral angle of 26.53 (7)° with the NiN₄ plane. Extensive hydrogen bonding leads to distinct cleavage in the bc plane.     

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.