Tetra­aqua(2,2′‐bi­pyridine)­nickel(II) terephthalate

The reaction of nickel(II) nitrate with terephthalic acid and 2,2′‐bi­pyridine in di­methyl­form­amide solution gives the title complex, [Ni(C₁₀H₈N₂)(H₂O)₄](C₈H₄O₄). The Ni^II ion is octahedrally coordinated to one 2,2′‐bi­pyridine and four water mol­ecules and does not coordinate to the terephthalate anion. Hydro­gen bonds between the terephthalate anions and the [Ni(2,2′‐bipy)(H₂O)₄]²⁺ cations produce a two‐dimensional hydrogen‐bonding architecture with double sheets.     

Di­aqua(2,2′‐bi­pyridine)­malonato­manganese(II)

In the crystal structure of the title compound, [Mn(C₃H₂O₄)(C₁₀H₈N₂)(H₂O)₂], the Mn^II atom demonstrates a distorted octahedral geometry, being coordinated by two N atoms of a 2,2′‐bi­pyridine ligand, two O atoms from the carboxyl­ate groups of the chelating malonate dianion and two O atoms of two cis water mol­ecules. The complex mol­ecules are linked to form a three‐dimensional supramolecular array by both hydrogen‐bonding interactions between coordinated water and the carboxyl­ate groups of neighboring mol­ecules and aromatic π–π‐stacking interactions of the bi­pyridine rings.     

Packing effects in 4,4′‐bis(4‐hydroxy­butyl)‐2,2′‐bi­pyridine and 4,4′‐bis(4‐bromo­butyl)‐2,2′‐bi­pyridine

Structure analyses of 4,4′‐bis(4‐hydroxy­butyl)‐2,2′‐bi­pyridine, C₁₈H₂₄N₂O₂, (I), and 4,4′‐bis(4‐bromo­butyl)‐2,2′‐bi­pyridine, C₁₈H₂₂Br₂N₂, (II), reveal intermolecular hydrogen bonding in both compounds. For (I), O—H·N intermolecular hydrogen bonding leads to the formation of an infinite two‐dimensional polymer, and π stacking interactions are also observed. For (II), C—H·N intermolecular hydrogen bonding leads to the formation of a zigzag polymer. The two compounds crystallize in different crystal systems, but both mol­ecules possess C_i symmetry, with one half mol­ecule in the asymmetric unit.     

Tetra­carbonyl­(di­phenyl­di­thio­phosphinato‐S,S′)­rhenium(I)

The title compound consists of [Re(C₁₂H₁₀PS₂)(CO)₄] mol­ecules in which the Re atom is octahedrally coordinated by four carbonyl groups and two di­thio­phosphinate S atoms. The main coordination distortion is imposed by the ligand bite angle of 78.29 (4)°. The bidentate coordination of the di­thio­phosphinate ligand involves almost equal Re—S [2.5366 (15) and 2.5535 (14) Å] and P—S distances [2.0100 (19) and 2.0212 (19) Å].     

(R)‐(+)‐2,2′‐Bis­(di­phenyl­phosphinoyl)‐1,1′‐bi­naphthyl

The title compound, BINAP oxide, C₄₄H₃₂O₂P₂, (I), was synthesized by direct oxidation of (R)‐(+)‐2,2′‐bis­(di­phenyl­phosphino)‐1,1′‐bi­naphthyl (BINAP) with tert‐butyl hydro­peroxide in toluene solution. The angle between the naphthyl planes of the bi­naphthyl group is 94.17 (3)°.     

4,4′‐Bis(N,N‐diethyl­amino)‐2,2′‐bi­pyridine

The title compound, C₁₈H₂₆N₄, contains two almost identical independent mol­ecules that lie about inversion centres. Each mol­ecule has a planar bi­pyridine nucleus and two terminal diethyl­amine groups oriented at almost right angles to the core. These diethyl­amine branches act as spacers, producing a very open structure with one of the lowest densities reported among related compounds. The most important intermolecular interactions are of the C—H⋯π type, which connect non‐equivalent moieties.     

2,2′,4,4′,6,6′‐Hexa­methyl‐4,4′‐bi­[4H‐pyran­yl]

The title mol­ecule, C₁₆H₂₂O₂, reveals C_i point symmetry in the crystal structure. The structure was disordered. The pyran ring is not planar; the O atom lies significantly out of the least‐squares plane (ten times the r.m.s. deviation of all six atoms).     

Di‐μ‐sulfito‐bis­[(4,4′‐di­methyl‐2,2′‐bi­pyridine)­zinc(II)] dihydrate and poly­[[aqua(1,10‐phenanthroline)­zinc(II)]‐μ3‐sulfito‐zinc(II)‐μ3‐sulfito]

Two different zinc sulfite compounds have been prepared through the decomposition of pyrosulfite–­di­thionite ions in aqueous solution, viz. a dimeric complex, di‐μ‐sulfito‐κ³O,O′:O′′;κ³O:O′,O′′‐bis­[(4,4′‐di­methyl‐2,2′‐bi­pyridine‐κ²N,N′)­zinc(II)] dihydrate, [Zn₂(SO₃)₂(C₁₂H₁₂N₂)₂]·2H₂O, (I), which was solved and refined from a twinned sample, and an extended polymer, poly­[[aqua(1,10‐phenanthroline‐κ²N,N′)­zinc(II)]‐μ₃‐sulfito‐κ²O:O′:O′′‐zinc(II)‐μ₃‐sulfito‐κ³O:O:O′], [Zn₂(SO₃)₂(C₁₂H₁₀N₂)(H₂O)]_n, (II). In (I), the dinuclear Zn^II complex has a center of symmetry. The cation is five‐coordinate in a square‐pyramidal arrangement, the anion fulfilling a bridging chelating role. Compound (II) comprises two different zinc units, one being five‐coordinate (square pyramidal) and the other four‐coordinate (trigonal pyramidal), and two independent sulfite groups with different binding modes to the cationic centers.     

Bis(2,4,7‐tri­methyl­indenyl)­cobalt(II) and rac‐2,2′,4,4′,7,7′‐hexamethyl‐1,1′‐biindene

The crystal and molecular structures of bis(η⁵‐2,4,7‐tri­methyl­indenyl)­cobalt(II), [Co(C₁₂H₁₃)₂], (I), and rac‐2,2′,4,4′,7,7′‐hexamethyl‐1,1′‐biindene, C₂₄H₂₆, (II), are reported. In the crystal structure of (I), the Co atom lies on an inversion centre and the structure represents the first example of a bis(indenyl)cobalt complex exhibiting an eclipsed indenyl conformation. The (1R,1′R) and (1S,1′S) enantiomers of the three possible stereoisomers of (II), which form as by‐products in the synthesis of (I), cocrystallize in the monoclinic space group P2₁/c. In the unit cell of (II), alternating (1R,1′R) and (1S,1′S) enantiomers pack in non‐bonded rows along the a axis, with the planes of the indenyl groups parallel to each other and separated by 3.62 and 3.69 Å.     

(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.     

Tri­phenyl(3,4,5‐tri­iodo­phenyl)­methane

The crystal structure of the title compound, alternatively called 1,2,3‐triiodo‐5‐(triphenylmethyl)benzene, C₂₅H₁₇I₃, is analysed in terms of I⋯I and I⋯π interactions and the herring‐bone T motif between phenyl groups. There are two mol­ecules in the asymmetric unit, denoted A and B. Inversion‐related A mol­ecules are connected via an I⋯π interaction (3.641 Å, to a C—C bond mid‐point) to form an I⋯π dimer, and these dimers are connected through symmetry‐independent B mol­ecules via I⋯I [3.5571 (15) Å] and I⋯π (3.561 Å, to a C—C bond mid‐point) interactions.     

trans‐[1,3‐Bis(2,4‐di­methyl­phenyl)­imidazolidin‐2‐yl­idene]­di­chloro­(tri­phenyl­phosphine‐κP)­palladium(II)

The title complex, [PdCl₂(C₁₉H₂₂N₂)(C₁₈H₁₅P)], shows slightly distorted square‐planar coordination of the palladium(II) metal center. The Pd—C bond distance between the N‐heterocyclic ligand and the metal atom is 2.008 (3) Å. The dihedral angle between the two di­methyl­phenyl ring planes is 33.17 (13)°.     

Trigonal–planar silver coordination in (3,5‐di­nitro­benzoato)­bis­(tri­phenyl­phosphine)­silver(I)

The three‐coordinate Ag atom in the title compound, [Ag(C₇H₃N₂O₆)(C₁₈H₁₅P)₂], shows trigonal–planar coordination [P—Ag—P = 147.1 (1)° and Σ_Ag = 359.0 (3)°]. Adjacent mol­ecules are linked through the O atoms of adjacent nitro groups [Ag?O = 3.205 (3) and 3.302 (4) Å] into a zigzag chain running parallel to the c axis.     

[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.     

Polymeric di­aqua­bis­[μ4‐1,3,5‐benzenetri­carboxyl­ato(3–)](μ‐4,4′‐bi­pyridine)­trizinc(II)

The solvothermal reaction of zinc(II) acetate with 1,3,5‐benzene­tri­carboxyl­ic acid and 4,4′‐bi­pyridine in 1‐butanol and acetic acid solution gives the title complex, [Zn₃(C₉H₃O₆)₂(C₁₀H₈N₂)(H₂O)₂]_n. There are two different coordination environments for the Zn atom, namely ZnNO₂(H₂O) and ZnO₄; in the latter case, the Zn atom lies on a twofold symmetry axis. Carboxyl­ate‐bridged Zn₃(O₂C)₆ clusters are connected through 1,3,5‐benzene­tri­carboxyl­ate and 4,4′‐bi­pyridine ligands (which lie about inversion centers), yielding a three‐dimensional framework.     

Tetra‐μ‐chloro‐1:2κ4Cl;1:3κ4Cl‐bis(4,4′‐di­methyl‐2,2′‐bi­pyridine)‐2κ2N,3κ2N‐lithium(I)­dipalladium(II) tetrakis­(penta­fluoro­phenyl)­borate di­chloro­methane 1.196‐solvate

In the crystal structure of the title compound, [LiPd₂Cl₄(C₁₂H₁₂N₂)₂](C₂₄F₂₀B)·1.196CD₂Cl₂ or [{(Me₂bipy)PdCl₂}₂(μ‐Li)]⁺·B(C₆F₅)₄⁻·1.196CD₂Cl₂ (Me₂bipy is 4,4′‐di­methyl‐2,2′‐bi­pyridine), an Li⁺ cation is stabilized by complexation with two (Me₂bipy)PdCl₂ units through weak Li—Cl interactions. This compound is thus a rare example of a complex that exhibits an arrested Cl⁻ abstraction.     

Poly­[[di­aqua­tris(μ6‐benzene‐1,2,4,5‐tetra­carboxyl­ato)­tris(μ2‐4,4′‐bi­pyridine)­hexacopper(II)] dihydrate]

The hydro­thermal reaction of an aqueous solution of Cu(CH₃COO)₂·H₂O, 1,2,4,5‐benzene­tetra­carboxylic acid and 4,4′‐bi­pyridine gave rise to the interesting title three‐dimensional polymer {[Cu₆(btec)₃(4,4′‐bpy)₃(H₂O)₂]·2H₂O}_n (btec is 1,2,4,5‐benzene­tetra­carboxyl­ate, C₁₀H₂O₈⁴⁻, and 4,4′‐bpy is 4,4′‐bi­pyridine, C₁₀H₈N₂), in which each btec ligand links six copper(II) cations into a lamellar [Cu₆(btec)₃(H₂O)₂]_n sub­polymer framework. There are two distinct diamine units and two distinct carboxylate units, with one of each lying across an inversion centre.     

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.     

μ‐Bi­phenyl‐2,2′‐di­thiol­ato‐κ2S:S′‐bis­[(tri­phenyl­phosphine‐κP)­gold(I)]

The reaction of ClAuPPh₃ and 1,1′‐bi­phenyl‐2,2′‐di­thiol in the presence of tri­methyl­benzyl­ammonium chloride and K₂CO₃ in a tetra­hydro­furan/methanol solution gives the title complex, [Au₂(C₁₂H₈S₂)(C₁₈H₁₅P)₂]. The mol­ecule contains P—Au—S units which `cross' with torsion angles of ∼90° [P—Au—Au—P = 86.23 (5)° and S—Au—Au—S = 95.62 (5)°]. The intra‐ and intermolecular Au⋯Au distances [3.9064 (3) and 6.3797 (5) Å, respectively] are outside the range for typical Au⋯Au interactions. However, the Au atoms appear to be drawn together, leading to a significant bending of the P—Au—S angles [170.24 (5) and 169.52 (5)°].     

Intermolecular contacts in the crystal packing of 2,2′‐(N,N′‐oxalyldiimino)­bis(3‐phenyl­propanamide) di­methyl sulfoxide solvate

In the title compound, C₂₀H₂₂N₄O₄·C₂H₆OS, two distinct hydrogen‐bond systems connect oxal­amide groups in one pattern and primary amide groups in the other to form a two‐dimensional network perpendicular to the c axis. These hydro­philic layers are joined to the three‐dimensional structure through C—H?π interactions. The hydrogen‐bonded waved layers shape holes which are occupied by disordered di­methyl sulfoxide solvent mol­ecules.