(Aceto­nitrile‐N)(o‐benzo­quinone di­imine‐N,N′)­chloro‐trans‐bis­(tri­phenyl­phosphine‐P)­ruthenium(II) hexa­fluoro­phosphate 0.25‐hydrate

The Ru atom in the title compound, [RuCl(CH₃CN){P(C₆H₅)₃}₂{C₆H₄(NH)₂}]PF₆·0.25H₂O, has a six‐coordinate octahedral geometry, with a trans arrangement of the tri­phenyl­phosphine groups. The asymmetric unit contains two complex mol­ecules and a partially occupied water site. Principal dimensions include Ru—N 1.958 (4)–2.044 (5), Ru—P 2.3897 (16)–2.4092 (15), and Ru—Cl 2.4280 (15) and 2.4295 (16) Å     

Pentane and tetra­hydro­furan solvates of trans‐di­chloro­bis­[1,2‐ethane­diyl­bis­(di­phenyl­phos­phine)‐P,P′]­molybdenum(II)

trans‐[MoCl₂(dppe)₂] [dppe is 1,2‐ethane­diyl­bis­(di­phenyl­phos­phine), C₂₆H₂₄P₂] was obtained as a side product from the reaction of trans‐[Mo(dppe)₂(N₂)₂] with Cp*GeCl to give the germyl­yne complex trans‐[Cl(dppe)₂Mo[triple‐bond]Ge(η¹‐Cp*)]. The crystal structures of the hemi­pentane (0.5C₅H₁₂) and di­tetra­hydro­furan (2C₄H₈O) solvates of trans‐[MoCl₂(dppe)₂], (IIIa) and (IIIb), respectively, have been determined.     

Carbonyl­[di­hydro­bis­(pyrazol‐1‐yl‐κN2)­borato]­hydrido­bis­(tri‐p‐tolyl­phosphine‐κP)­ruthenium(II)

The title compound, [RuH(C₆H₈BN₄)(C₂₁H₂₁P)₂(CO)], possesses two trans‐disposed tri‐p‐tolyl­phosphines in axial positions and the remaining ligands in equatorial positions. The overall geometry of the Ru^II ion is a distorted octahedral structure. The P—Ru—P axis deviates from linearity by about 13°. This distortion arises mainly from the steric congestion between the bulky phosphine moieties and the tetrahedral di­hydro­bis­(pyrazol‐1‐yl)­borate ligands.     

trans‐Bis­(diethano­lamine)­bis­(iso­thio­cyanato)­nickel(II)

In the neutral title complex, trans‐bis(2,2′‐imino­di­ethanol‐N,O)­bis­(iso­thio­cyanato)­nickel(II), [Ni(NCS)₂(C₄H₁₁NO₂)₂], the iso­thio­cyanate ions and the di­ethanol­amine mol­ecules act as mono­dentate and bi­dentate ligands, respectively. The Ni^II ion exhibits a distorted octahedral configuration with crystallographically imposed inversion symmetry and N_NCS—Ni—N_amine and N_NCS—Ni—O_amine bond angles of 88.78 (10) and 89.44 (10)°, respectively. The Ni—N bond distances are in the range 2.069 (3)–2.096 (2) Å. The mol­ecules are linked by hydrogen bonds to form a three‐dimensional infinite lattice.     

trans‐Bis(3,5‐di­aza‐1‐azonia‐7‐phosphaadamantane‐κP)­bis­(thiocyanato‐κS)­palladium(II) bis­(thio­cyanate)

The crystal structure of the title compound, trans‐[Pd(NCS)₂(C₆H₁₃N₃P)₂](NCS)₂, is one of the few pal­ladium(II) complexes containing two protonated water‐soluble 1,3,5‐tri­aza‐7‐phos­pha­adamantane (PTA) ligands re­ported to date. The compound displays a distorted square‐planar geometry, with the Pd atom on an inversion centre and with the S atoms of the thio­cyanate counter‐ions occupying the axial positions above and below the equatorial plane described by the phosphine and thio­cyanate ligands. Geometric parameters for the formal coordination polyhedron include a Pd—P distance of 2.2940 (8) Å, a Pd—S distance of 2.3509 (8) Å and a P—Pd—S angle of 89.45 (3)°. The effective cone angle for the PTA ligands was calculated as 114.5°.     

Di­chloro­bis­(di­benzyl­amino)­bis­(tetra­hydro­furan)­zirconium(IV) toluene hemisolvate

The title complex, [ZrCl₂(C₄H₈O)₂(C₁₄H₁₄N)₂]·0.5C₇H₈, was prepared in an unusual manner by utilizing [Mg{N(CH₂Ph)₂}₂] as a ligand transfer reagent. The Zr atom lies in a distorted octahedral environment where steric repulsion from the large di­benzyl­amino ligands leads to a widening of the N—Zr—N angle [99.95 (9)°] and corresponding compression of other angles [Cl—Zr—Cl 160.95 (3)° and O—Zr—O 78.22 (7)°]. This distortion is compared with those found in the previously determined structures of the di­methyl­amino and diethyl­amino analogues.     

trans‐Di­chloro‐cis‐bis(3,6‐di­methyl­carbazolyl)‐cis‐bis­(tetra­hydro­furan)­zirconium(IV) benzene sesquisolvate

In the title compound, [ZrCl₂(C₁₄H₁₂N)₂(C₄H₈O)₂]·1.5C₆H₆, the Zr atom is pseudo‐octahedral, with two Cl atoms in trans positions and two tetra­hydro­furan mol­ecules in cis positions. The two 3,6‐di­methyl­carbazolyl ligands are in cis positions and are canted with respect to one another. The two Zr—N distances are 2.1148 (18) and 2.1236 (18) Å, and the N—Zr—N angle is 95.08 (7)°. The title compound crystallizes as the benzene solvate, with one of the benzene mol­ecules positioned on an inversion center.     

trans‐Chloro­(methyl)­bis­(tri­cyclo­hexyl­phosphine)­platinum(II)

The crystal structure of the title compound, [PtCl(CH₃)(C₁₈H₃₃P)₂], is isostructural with various platinum(II) and palladium(II) complexes containing two bulky tri­cyclo­hexyl­phosphine ligands in a trans orientation. The Pt atom resides on an inversion centre, resulting in a 50% statistical disorder in the chloro and methyl positions. The most significant geometrical parameters are Pt—P 2.3431 (8), Pt—­Cl 2.440 (4) and Pt—C1 2.179 (13) Å, and P—Pt—P 180, P—Pt—Cl 89.15 (12) and 90.85 (12), and C—Pt—Cl 172.7 (5)°. The effective and Tolman cone angles for the tricyclohexylphosphine ligands were calculated as 160 and 162°, respectively.     

trans‐Di­chloro­bis­(tri­phenyl­phosphine‐P)­platinum(II)

Two different crystals (A and B) were used to structurally characterize trans‐[PtCl₂(PPh₃)₂] and to study random and systematic errors in derived parameters. The compound is isomorphous with trans‐[PdCl₂(PPh₃)₂] and with one of the polymorphs of trans‐[PtMeCl(PPh₃)₂] reported previously. Half‐normal probability plot analyses based on A and B show realistic s.u.'s and negligible systematic errors. R.m.s. calculations give very good agreement between A and B, 0.0088 Å. Important geometrical parameters are Pt—P = 2.3163 (11) Å, Pt—Cl = 2.2997 (11) Å, P—Pt—Cl = 87.88 (4) and 92.12 (4)°. Half‐normal probability plots and r.m.s. calculations were also used to compare the title compound with the palladium analogue, showing small systematic differences between the compounds. The torsion angles around the Pt—P bond were found to be very similar to those reported for isomorphous complexes, as well as to the torsion angles around the Pt—As bond in trans‐[PtCl₂(AsPh₃)₂]. The NMR coupling constants for the title compound are similar to Pt—P coupling constants reported for analogous trans complexes.     

Chloro{2,2′‐[(1S,2S)‐1,2‐di­phenyl‐1,2‐ethanediyl­bis­(nitrilo­methyl­idyne)]­diphenolato‐κ4O,N,N′,O′}(ethanol‐κO)­manganese(III)

The crystal structure of the title compound, [MnCl(C₂₈H₂₂N₂O₂)(C₂H₆O)], has been determined at 173 (2) K in the non‐centrosymmetric space group P2₁2₁2₁. The asymmetric unit contains two molecular units. An intermolecular O—H⋯Cl hydrogen bond is formed between the OH group of an ethanol mol­ecule coordinated to the Mn atom and the coordinated Cl⁻ anion, and so polymeric chains of Mn‐containing fragments are formed [O—H⋯Cl = 3.1281 (16) and 3.1282 (15) Å]. The Mn atoms have a pseudo‐octahedral coordination sphere, with the four donor atoms of the Schiff base forming an equatorial plane [Mn—O distances are 1.8740 (13), 1.8717 (13), 1.8749 (13) and 1.8823 (13) Å, and Mn—N distances are 1.9868 (15), 1.9910 (14), 1.9828 (15) and 1.9979 (14) Å]. The axial positions are occupied by an ethanol mol­ecule [Mn—O distances of 2.3069 (15) and 2.3130 (15) Å] and a Cl⁻ ligand [Mn—Cl distances of 2.5732 (6) and 2.5509 (6) Å].     

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.     

Bis(μ‐hexa­methyl­enetetr­amine)­bis(aqua­di­bromo­cadmium)­di­aqua­di­bromo­cadmium dihydrate

The title compound, poly­[[di­aqua­di­bromo­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐aqua­cad­mium‐di‐μ‐bromo‐aqua­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐di‐μ‐bromo] dihydrate], [Cd₃­Br₆­(C₆­H₁₂­N₄)₂­(H₂O)₄]·­2H₂O, is made up of two‐dimensional neutral rectangular coordination layers. Each rectangular subunit is enclosed by a pair of Cd₃(μ₂‐Br)₆(H₂O)₃ fragments and a pair of (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragments as sides (hmt is hexa­methyl­enetetr­amine). The unique Cd^II atom in the Cd₂Br₂ ring in the Cd₃(μ₂‐Br)₆(H₂O)₃ fragment is in a slightly distorted octahedral CdNOBr₄ geometry, surrounded by one hmt ligand [2.433 (5) Å], one aqua ligand [2.273 (4) Å] and four Br atoms [2.6409 (11)–3.0270 (14) Å]. The Cd^II atom in the (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragment lies on an inversion center and is in a highly distorted octahedral CdN₂O₂Br₂ geometry, surrounded by two trans‐related N atoms of two hmt ligands [2.479 (5) Å], two trans‐related aqua ligands [2.294 (4) Å] and two trans‐related Br atoms [2.6755 (12) Å]. Adjacent two‐dimensional coordination sheets are connected into a three‐dimensional network by hydrogen bonds involving lattice water mol­ecules, and the aqua, bromo and hmt ligands belonging to different layers.     

(2,2′‐Bipyridyl‐κ2N,N′)­bis­(salicyl­ato‐κ2O,O′)­zinc(II)

The asymmetric unit of the title compound, [Zn(C₇H₅O₃)₂(C₁₀H₈N₂)], contains one monomeric zinc complex. The Zn atom is coordinated to one 2,2′‐bipyridyl ligand via both N atoms and to two salicyl­ate anions (Hsal⁻) in a bidentate chelating manner involving carboxyl­ate O‐atom coordination. The complex exhibits a distorted octahedral geometry about the Zn^II atom, with the `apical' positions occupied by one of the two N atoms of the bipyridyl ligand and an O atom from one Hsal<sup>−</sup> ligand; the Zn atom is 0.168 (1) Å out of the `basal' plane. Two intramolecular six‐membered hydrogen‐bonded rings are present, generated from interactions between the carboxyl and hydroxyl groups of the salicyl­ate ligands. The crystal packing is governed by weak C—H⋯O and C—H⋯π interactions.     

(Nitro‐κN)[2‐(phenyldiazenyl‐κN2)pyridine‐κN](2,2′:6′,2′′‐terpyridine‐κ3N)ruthenium(II) tetrafluoroborate

The Ru—N bond distances in the title complex, [Ru(NO₂)(C₁₁H₉N₃)(C₁₅H₁₁N₃)]BF₄ or [Ru(NO₂)(tpy)(azpy)]BF₄, [tpy is 2,2′:6′,2′′‐ter­pyridine and azpy is 2‐(phenyl­azo)­pyridine], are Ru—N_py 2.063 (4), Ru—N_azo 2.036 (4), Ru—N_nitro 2.066 (3) Å, and Ru—N_tpy 2.082 (4), 1.982 (3) and 2.074 (4) Å. The azo N atom is trans to the nitro group. The azo N=N bond length is 1.265 (5) Å, which is the shortest found in such complexes to date. This indicates a multiple bond between Ru and the N atom of the nitro group, and π‐­backbonding [dπ(Ru) π*(azo)] is decreased.     

trans‐Diaquabis(1H‐imidazole‐4,5‐di­carboxyl­ate‐κ2N3,O4)­manganese(II)

In the title compound, [Mn(C₅H₃N₂O₄)₂(H₂O)₂], the Mn^II atom lies on an inversion centre, is trans‐coordinated by two N,O‐bidentate 1H‐imidazole‐4,5‐di­carboxyl­ate monoanionic ligands [Mn—O = 2.202 (3) Å and Mn—N = 2.201 (4) Å] and two water mol­ecules [Mn—O = 2.197 (4) Å], and exhibits a distorted octahedral geometry, with adjacent cis angles of 76.45 (13), 86.09 (13) and 89.20 (13)°. The complete solid‐state structure can be described as a three‐dimensional supramol­ecular framework, stabilized by extensive hydrogen‐bonding interactions involving the coordinated water mol­ecules, the carboxy O atoms and the protonated imidazole N atoms of the imidazole‐4,5‐di­carboxyl­ate ligands.     

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].     

Di‐μ‐chloro‐bis­{bis­[2,5‐bis­(4‐methoxy­phenyl)‐1,3,4‐oxadiazole‐κ2C2′,N]iridium(III)] dichloro­methane disolvate

In the title compound, [Ir₂(C₁₆H₁₃N₂O₃)₄Cl₂]·2CH₂Cl₂, the two Ir atoms, 3.7075 (6) Å apart, are bridged by two Cl atoms which straddle a twofold axis of rotation through the two Ir atoms. Each Ir centre resides in a distorted octa­hedral environment completed by two chelating 2,5‐bis­(4‐methoxy­phenyl)‐1,3,4‐oxadiazole ligands, with trans‐N—N and cis‐C—C dispositions. In the stacking structure, there are two types of hydrogen bonds, involving the meth­oxy substitutent, an N atom of the oxadiazole ring and the dichloro­methane solvent mol­ecules.     

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).     

trans‐Bis­[ethane‐1,2‐di­thiol­ato(2–)‐S,S′]­bis(2‐mer­cap­to­pyri­dine‐S)­tin(IV)

The title compound, [Sn(C₅H₅NS)₂(C₂H₄S₂)₂], was obtained from a 1:2 mixture of bis­(ethane‐1,2‐di­thiol­ato)­tin(IV) and 2‐mercapto­pyridine. The mol­ecules are discrete monomeric trans‐octahedral units, with the Sn^IV atom at the centre of symmetry, planar 2‐mercapto­pyridine zwitterions and SnS₂C₂ groups in twist–envelope conformations. The 2‐mercapto­pyridine ligands are monodentate and are bonded through the S atoms. The S—Sn distances between the S atom of edt (edt is ethane‐1,2‐di­thiol­ate) and the Sn atom are 2.473 (1) and 2.505 (1) Å, which are slightly longer than the S—Sn distance in Sn(edt)₂ of 2.390 (1) Å. The bond between the 2‐mercapto­pyridine S atom and the Sn atom are, remarkably, weaker than the S—Sn bond involving edt.     

Tetrakis­[1‐(3‐chloro­propyl)‐1,2,4‐tri­azole‐κN4]­bis­(tetrafluoroborato‐κF)copper(II)

In the title complex, [Cu(BF₄)₂(1tpc)₄] [1tpc is 1‐(3‐chloro­propyl)‐1,2,4‐triazole, C₅H₈ClN₃], the copper(II) centres reside in a tetragonally distorted octahedral coordination environment. Four 1tpc ligands are coordinated to the metal atom via the N4 atom of the triazole rings in a square‐planar arrangement, with Cu—N bond lengths in the range 2.002 (2)–2.019 (2) Å. Two tetra­fluoro­borate anions, in the axial positions above and below the square plane, are weakly coordinated to the copper(II) centre, with Cu—F distances of 2.4009 (18) and 2.5096 (18) Å.