(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.     

Low‐dimensional compounds containing cyano groups. I. catena‐Poly[[[dicyanoargentato(I)‐κN]bis(4‐methylpyridine‐κN)copper(II)]‐μ‐dicyanoargentato(I)‐κ2N:N′]

The structure of the title compound, [Cu(C₆H₇N)₂{Ag(CN)₂}₂]_n, is made up of neutral zigzag chains of [–NC–Ag–CN–Cu(4‐Mepy)₂{Ag(CN)₂}–NC–Ag–CN–] (4‐Mepy is 4‐methyl­pyridine). Neighbouring chains are linked by weak argentophilic interactions, with Ag?Ag distances of 3.2322 (12) Å. The Cu atom, which lies on a twofold rotation axis, is pentacoordinated by one monodentate Ag(CN)₂^? anion [Cu—N 1.985 (3) Å], the atoms of which lie on the same rotation axis, and by bridging di­cyano­argentate anions [2 × Cu—N 2.0827 (19) Å], with Ag atoms on inversion centres. The coordination polyhedron is completed by two 4‐Mepy mol­ecules [2 × Cu—N 2.038 (2) Å], which occupy the axial positions of a distorted trigonal bipyramid.     

catena‐Poly­[[(di‐2‐pyridyl­amine)­silver(I)]‐μ‐nicotinato] and catena‐poly­[[(di‐2‐pyridyl­amine)silver(I)]‐μ‐2,6‐di­hydroxy­benzoato]

In catena‐poly­[[(di‐2‐pyridyl­amine‐κ²N,N′)silver(I)]‐μ‐nico­tinato‐κ²N:O], [Ag(C₆H₄NO₂)(C₁₀H₉N₃)]_n, the Ag^I atom is tetracoordinated by two N atoms from the di‐2‐pyridyl­amine (BPA) ligand [Ag—N = 2.3785 (18) and 2.3298 (18) Å] and by one N atom and one carboxyl­ate O atom from nicotinate ligands [Ag—N = 2.2827 (15) Å and Ag—O = 2.3636 (14) Å]. Bridging by nicotinate N and O atoms generates a polymeric chain structure, which extends along [100]. The carboxyl O atom not bonded to the Ag atom takes part in an intrachain C—H⋯O hydrogen bond, further stabilizing the chain. Pairs of chains are linked by N—H⋯O hydrogen bonds to generate ribbons. There are no π–π interactions in this complex. In catena‐poly­[[(di‐2‐pyridyl­amine‐κ²N,N′)silver(I)]‐μ‐2,6‐di­hydroxy­benzoato‐κ²O¹:O²], [Ag(C₇H₅O₄)(C₁₀H₉N₃)]_n, the Ag^I atom has a distorted tetrahedral coordination, with three strong bonds to two pyridine N atoms from the BPA ligand [Ag—N = 2.286 (5) and 2.320 (5) Å] and to one carboxyl­ate O atom from the 2,6‐di­hydroxy­benzoate ligand [Ag—O = 2.222 (4) Å]; the fourth, weaker, Ag‐atom coordination is to one of the phenol O atoms [Ag⋯O = 2.703 (4) Å] of an adjacent moiety, and this interaction generates a polymeric chain along [100]. Pairs of chains are linked about inversion centers by N—H⋯O hydrogen bonds to form ribbons, within which there are π–π interactions. The ribbons are linked about inversion centers by pairs of C—H⋯O hydrogen bonds and additional π–π interactions between inversion‐related pairs of 2,6‐di­hydroxy­benzoate ligands to generate a three‐dimensional network.     

catena‐Poly[[(N,N‐dimethyl­formamide‐κO)(nitrato‐κO)silver(I)]‐μ‐1,2‐bis­(diphenyl­phosphino)ethane‐κ2P:P′] at 100 and 293 K: temperature effects on the volume of the solvent pocket

In the title chain compound, [Ag(NO₃)(C₃H₇NO)(C₂₆H₂₄P₂)]_n, the bis­(diphenyl­phosphino)ethane (dppe) components lie across centres of inversion. The dppe units link the Ag⁺ ions into chains along [100]. A nitrate anion is coordinated to the Ag atom, together with one mol­ecule of N,N‐dimethyl­formamide (DMF) solvent. At room temperature, the coordinated DMF shows a long Ag—O distance [2.620 (3) Å] and relatively large thermal motion, while at 100 K the Ag—O distance is shorter [2.5588 (19) Å] and the thermal motion is similar to that of the rest of the complex. The behaviour of the DMF mol­ecule is related to the size of the solvent pocket, viz. 146 ų at 293 K and 131 ų at 100 K.     

[Bis(2‐diphenylphosphinoethyl) sulfide‐κ3P,S,P′](triphenylphosphine‐κP)platinum(II) diperchlorate acetone solvate

In the title compound, [Pt(C₁₈H₁₅P)(C₂₈H₂₈P₂S)]­(ClO₄)₂·­C₃H₆O or [Pt(PPh₃)(PSP)](ClO₄)₂·CH₃COCH₃, where PSP is the potentially tridentate chelate ligand bis(2‐di­phenyl­phosphinoethyl) sulfide, all three donor groups of the PSP ligand are coordinated to the central Pt atom, with Pt—P = 2.310 (1) Å and Pt—S = 2.343 (1) Å. The fourth coordination site is occupied by the P donor of the tri­phenyl­phosphine ligand [Pt—P = 2.289 (1) Å]. The complex cation has exact mirror symmetry, with the S atom, the Pt atom and the P atom of the PPh₃ ligand in the mirror plane. The Pt atom has a distorted square‐planar coordination geometry. A π–π interaction is present between the phenyl rings of the PPh₃ ligand and the terminal –PPh₂ group of the PSP chelate.     

Bis(4‐aminopyridine)silver(I) nitrate and tris(2,6‐diaminopyridine)silver(I) nitrate

The bis(4‐aminopyridine)silver(I) cation in [Ag(C₅H₆N₂)₂]NO₃ has the Ag atom on a twofold axis and displays an N—Ag—N angle of 174.43 (15)° and an Ag—N distance of 2.122 (3) Å. The two ligands are planar and the angle between the two ligand planes is 79.45 (9)°. The pyridine rings are stacked in piles with an interplanar distance of 3.614 (5) Å, a distance that strongly suggests that pyridine π–π interactions have an appreciable importance with respect to the non‐bonded crystal organization. The tris(2,6‐diaminopyridine)­silver(I) cation in [Ag(C₅H₇N₃)₃]NO₃ has Ag—N distances of 2.243 (2), 2.2613 (17) and 2.4278 (18) Å, and N—Ag—N angles of 114.33 (7), 134.91 (7) and 114.33 (7)°. The Ag⁺ ion is situated 0.1531 (2) Å from the plane defined by the three pyridine N atoms.     

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.     

Tetrakis­(tetra­hydro­furan‐κO)­lithium mer‐tris­(carbazolyl‐κN)‐trans‐di­chloro(tetra­hydro­furan‐κO)­zirconate

In the title compound, [Li(C₄H₈O)₄][ZrCl₂(C₁₂H₈N)₃(C₄H₈O)], the environment of the Zr atom is pseudo‐octahedral, with the three carbazolyl ligands in a mer configuration. The counter‐ion of the zirconium complex is composed of an Li atom surrounded by four tetra­hydro­furan (THF) mol­ecules. The THF mol­ecule attached to the Zr atom is disordered over two sites, as are two of the THF mol­ecules in the lithium moiety. All bond distances and angles are consistent with those in complexes with similar structural entities. The Zr—N bond distances are 2.2185 (18) and 2.167 (3) Å.     

Polymeric (3‐amino‐2‐chloropyridine)nitratosilver(I)

In the title compound {alternative name: poly­[silver(I)‐μ‐(3‐­amino‐2‐chloro­pyridine)‐μ‐nitr­ato]}, [Ag(NO₃)(C₅H₅ClN₂)]_n the Ag^I atom is in an irregular AgN₂O₃ geometry, surrounded by one pyridyl N atom [Ag—N 2.283 (5) Å], one amine N atom [Ag—N 2.364 (6) Å] and three O atoms from different nitrate ions [Ag—O 2.510 (6)–2.707 (6) Å]. The Ag ions are bridged by the 3‐amino‐2‐chloro­pyridine ligands into helical chains. Adjacent uniform chiral chains are further interlinked through the NO₃ bridges into an interesting two‐dimensional coordination network in the solid.     

Aqua­chloro(1,10‐phenanthroline‐κ2N,N′)(p‐toluenesulfonato‐κO)copper(II)

In the title compound, [CuCl(C₇H₇O₃S)(C₁₂H₈N₂)(H₂O)], the central Cu atom is coordinated by a water mol­ecule, a chloride ion, an O‐monodentate p‐toluene­sulfonate anion and an N,N′‐bidentate 1,10‐phenanthroline ligand. The copper environment is best described as a slightly distorted square pyramid, with bond distances Cu—Cl 2.2282 (9) Å, Cu—OW 1.984 (3) Å, and Cu—N 2.006 (3) and 2.028 (3) Å; the apical Cu—O distance is 2.281 (2) Å. In the supramolecular structure, π–π‐stacking stabilization is observed, and classical and non‐classical hydrogen bonds also play an important role.     

(2‐Methyl­quinolin‐8‐olato)­iron(III) and ‐copper(II) complexes

The crystal structures of tris(2‐methyl­quinolin‐8‐olato‐N,O)­iron(III), [Fe­(C₁₀­H₈­NO)₃], (I), and aqua­bis(2‐methyl­quinolin‐8‐olato‐N,O)­copper(II), [Cu­(C₁₀­H₈NO)₂­(H₂O)], (II), have been determined. Compound (I) has a distorted octahedral configuration, in which the central Fe atom is coordinated by three N atoms and three O atoms from three 2‐methylquinolin‐8‐olate ligands. The three Fe—O bond distances are in the range 1.934 (2)–1.947 (2) Å, while the three Fe—N bond distances range from 2.204 (2) to 2.405 (2) Å. In compound (II), the central Cu^II atom and H₂O group lie on the crystallographic twofold axis and the coordination geometry of the Cu^II atom is close to trigonal bipyramidal, with the three O atoms in the basal plane and the two N atoms in apical positions. The Cu—N bond length is 2.018 (5) Å. The Cu—O bond length in the basal positions is 1.991 (4) Å, while the Cu—O bond length in the apical position is 2.273 (6) Å. There is an intermolecular OW—H?O hydrogen bond which links the mol­ecules into a linear chain along the b axis.     

7‐{Di­phenyl­[(tri­phenyl­phos­phine)­aurio]­phos­phine(1+)‐P}‐8‐methyl‐7,8‐dicarba‐nido‐undecaborate(1–) dichloro­methane hemi­solvate

The title compound, 7‐[(Ph₂P)Au(PPh₃)]‐8‐(CH₃)‐7,8‐nido‐C₂B₉H₁₀]·­0.5CH₂Cl₂ or [Au(C₁₅H₂₃B₉P)­(C₁₈H₁₅P)]·­0.5CH₂Cl₂, is the first reported gold derivative of the ligand [7‐­(Ph₂P)‐8‐(CH₃)‐7,8‐nido‐C₂B₉H₁₀]^?. It has a mono­nuclear structure with the gold centre in an essentially linear coordination [P—Au—P 174.041 (15)°]. The open C₂B₃ face contains one H atom that is strongly bonded to the central B atom and semi‐bridging to a neighbouring B atom [B—H distances 1.070 (16) and 1.45 (3) Å].     

Hexa‐μ2‐chloro‐μ4‐oxo‐tetrakis[(2‐ethyl­tetrazole‐κN4)copper(II)]

In the title molecular complex, [Cu₄Cl₆O(2‐EtTz)₄], where 2‐EtTz is 2‐ethyl­tetrazole (C₃H₆N₄), the central O atom is located on the symmetry site and is tetrahedrally coordinated to four Cu atoms, with Cu—O distances of 1.8966 (4) Å. A very slight distortion of Cu₄O from a regular tetrahedron is observed [two Cu—O—Cu angles are 108.76 (3)° and four others are 109.828 (13)°]. Each Cu atom is connected to three others via the Cl atoms, forming a slightly distorted Cl octahedron around the O atom, with O⋯Cl distances of 2.9265 (7) Å for Cl atoms lying on the twofold axis and 2.9441 (13) Å for those in general positions. The Cu atom has a distorted trigonal–bipyramidal environment, with three Cl atoms in the equatorial plane, and with the N atom of the 2‐ethyl­tetrazole ligand and the μ₄‐O atom in axial positions. The Cu atom is displaced out of the equatorial plane by ca 0.91 Å towards the coordinated N atom of the 2‐­ethyl­tetrazole ligand.     

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.     

Bis{μ‐2‐[(2,3‐dichloro­phenyl)­amino]­benzoato‐κO}di‐μ2‐ethoxo‐octa­methyl­di‐μ3‐oxo‐tetra­tin(IV)

The title compound, [Sn₄(CH₃)₈(C₁₃H₈Cl₂NO₂)₂(C₂H₅O)₂O₂], is a centrosymmetric dimer, with three linearly fused four‐membered Sn—O—Sn—O rings. The coordination poly­hedron of the Sn atom bonded to the carboxyl­ate can be described as trigonal–bipyramidal distorted toward square‐pyramidal. That of the second Sn atom is similar, but the distortion towards square‐pyramidal geometry is greater. The Sn—O and Sn—C distances are 2.020 (2)–2.226 (2) and 2.096 (4)–2.114 (4) Å, respectively. The benzene rings of the 2‐[(2,3‐dichloro­phenyl)­amino]benzoate ligand subtend an angle of 50.49 (17)°; the conformation of the ligand is stabilized by intra­molecular N—H⋯Cl and N—H⋯O hydrogen bonds. The structure is assembled viaπ–π stacking inter­actions to form chains parallel to [10].     

Bis(3,5‐di­methyl­pyrazole‐κN2)silver(I) nitrate

The two independent bis(3,5‐di­methyl­pyrazole)silver(I) cations in crystalline [Ag(C₅H₇N₂)₂]NO₃ display N—Ag—N angles of 175.51 (14) and 174.44 (13)°, and an average Ag—N distance of 2.124 (5) Å. The nitrate anion is situated between [Ag(C₅H₇N₂)₂]⁺ units and interacts via hydrogen bonds with the NH groups. The two 3,5‐di­methyl­pyrazole ligands are trans about the silver center. Only a small deviation from linearity is observed in the coordination around silver.     

trans‐Bis[3‐(2‐fluorophenyl)‐1‐(4‐nitrophenyl)triazenido‐κN3]bis(pyridine‐κN)palladium(II)

In the title complex, [Pd(C₁₂H₈FN₄O₂)₂(C₅H₅N)₂] or trans‐[Pd(FC₆H₄N=N—NC₆H₄NO₂)(C₅H₅N)₂], the Pd atom lies on a centre of inversion in space group P. The coordination geometry about the Pd²⁺ ion is square planar, with two deprotonated 3‐(2‐fluoro­phenyl)‐1‐(4‐nitro­phenyl)­triazenide ions, FC₆H₄N=N—NC₆H₄NO₂^?, acting as monodentate ligands (two‐electron donors), while two neutral pyridine mol­ecules complete the metal coordination sphere. The whole triazenide ligand is not planar, with the largest interplanar angle being 16.8 (5)° between the phenyl ring of the 2‐­fluorophenyl group and the plane defined by the N=N—N moiety. The Pd—N(triazenide) and Pd—N(pyridine) distances are 2.021 (3) and 2.039 (3) Å, respectively.     

cis‐[1,2‐Bis(diisopropylphosphino‐κP)‐1,2‐dicarba‐closo‐dodecaborane]dichloroplatinum(II) dichloromethane hemisolvate

The asymmetric unit of the title complex, [PtCl₂(C₁₄H₃₈B₁₀P₂)]·0.5CH₂Cl₂ or cis‐[PtCl₂{1,2‐(PⁱPr₂)₂‐1,2‐C₂B₁₀H₁₀}]·0.5CH₂Cl₂, contains one disordered solvent mol­ecule and two mol­ecules of the complex, in which each Pt^II atom displays slightly distorted square‐planar coordination geometry. The P atoms connected to the cage C atoms are coordinated to the Pt^II atom. The Pt—P distances vary slightly [2.215 (3) and 2.235 (4) Å] and the Pt—Cl distances are equal [2.348 (3) and 2.353 (5) Å].     

Di­cyclo­hexyl­ammonium 2,4‐di­chloro­phenoxy­acetate and (2,4‐di­chloro­phenoxy­acetato‐O,O′)bis­(tri­phenylphosphine‐P)silver(I)

The monoclinic cell of di­cyclo­hexyl­ammonium 2,4‐di­chloro­phenoxy­acetate contains four C₁₂H₂₄N⁺·C₅H₈Cl₂O₃^? ion pairs. The ammonium N atom is hydrogen bonded to the oxy­gen ends of two carboxyl groups to form a 12‐membered O—C—O?HNH?O—C—O?HNH ring. In (2,4‐di­chloro­phenoxy­lacetato)­bis­(tri­phenyl­phosphine)silver(I), [Ag(C₈H₅Cl₂O₃)(C₁₈H₁₅P)₂], the carboxyl CO₂ unit chelates to the Ag atom in an anisobidentate manner [Ag—O = 2.436 (2) and 2.517 (2) Å]; the Ag atom shows distorted tetrahedral geometry.     

[2,2′‐(1,3,5,8,10,12‐Hexaazacyclotetradecane‐3,10‐diyl)diethanol‐κ4N1,N5,N8,N12]bis(thiocyanato‐κS)copper(II)

In the crystal structure of the title compound, [Cu(NCS)₂(C₁₂H₃₀N₆O₂)], the Cu atom lies on an inversion centre and has an elongated octahedral coordination, with Cu—N distances of 2.004 (2) and 2.015 (2) Å, and a Cu—S distance of 2.9696 (10) Å. The 2,2′‐ethanol chains are axially oriented. The mol­ecules are linked to form a three‐dimensional network via O—H?N, N—H?O and N—H?S hydrogen bonds.