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1.  A dimer of bis­(N-heterocyclic carbene)rhodium(I) centres spanned by a dibenzo-18-crown-6 bridge from synchrotron radiation 
The compound (μ-3,3′,3′′,3′′′-{[2,5,8,15,18,21-hexa­oxatricyclo­[20.4.0.09,14]hexa­cosa-1(22),9,11,13,23,25-hexa­ene-11,12,24,25-tetra­yl]tetra­kis­(methyl­ene)}tetra­kis­(1-methyl-1H-imidazol-2-yl))bis­[(η4-cyclo­octa-1,4-diene)rhodium(I)] bis­(hexa­fluoridophosphate) acetonitrile sesquisolvate dihydrate, [Rh2(C8H12)2(C40H42N8O6)](PF6)2·1.5CH3CN·2H2O, crystallized from acetonitrile under an atmosphere of diethyl ether. In the crystal structure, the complex cation exhibits two square-planar RhI centres, each bound by a cyclo­octa­diene (COD) ligand and by two adjacent imidazolyl­idene N-heterocyclic carbene (NHC) donors from the same phen­oxy ring of the {[dibenzo-18-crown-6-11,12,24,25-tetra­yl]tetra­kis­(methyl­ene)}tetra­kis­(1-methyl-1H-imidazol-2-yl) (L) ligand. The dibenzo-crown ether bridge of L spans the Rh centres and forms hydrogen bonds with water mol­ecules. One water mol­ecule with half occupancy bridges adjacent macrocycles in the lattice. Another water with full occupancy forms weak hydrogen bonds to the crown ether O atoms and is, in turn, part hydrogen bonded by a lattice water with half occupancy. The latter water is within hydrogen-bonding distance of a fourth water also with partial occupancy. The result of these inter­actions is the formation of a layer in the ab plane. Two PF6 − ions, one of which is twofold disordered, and one ordered and one twofold disordered (with 0.5 occupancy) lattice acetonitrile mol­ecules complete the crystal structure.
doi:10.1107/S160053681204901X
PMCID: PMC3588264  PMID: 23476343
2.  [μ-3,3′-Diisopropyl-1,1′-(propane-1,3-di­yl)bis­(1,3-diazinan-2-yl­idene)]bis­[bromido­(η4-cyclo­octa-1,5-diene)rhodium(I)] 
The title compound, [Rh2Br2(C8H12)2(C17H32N4)], was obtained by the reaction of 3,3′-(propane-1,3-di­yl)bis­(1-isopropyl-3,4,5,6-tetra­hydro­pyrimidin-1-ium) bromide and [{Rh(cod)Cl}2] (cod is cyclo­octa-1,5-diene) in tetra­hydro­furan. The two RhI atoms each have a distorted square-planar coordination environment, defined by a bidentate cod ligand, a bromide anion and one C atom of the bridging bidentate bis-N-heterocyclcic carbene (NHC) ligand. The average Rh—CNHC distance is 2.038 (7) Å, suggesting that the bond has a major σ contribution with very little back donation. The distances between the cod ligands and the RhI atoms vary between 2.104 (4) and 2.210 (4) Å.
doi:10.1107/S1600536814001135
PMCID: PMC3998270  PMID: 24764831
3.  Bis[1,2-bis­(dimethyl­phosphino)ethane-κ2 P,P′]rhodium(I) dichlorido[(1,2,5,6-η)-1,5-cyclo­octa­diene]rhodium(I) 
In the title complex, [Rh(C6H16P2)2][RhCl2(C8H12)], the asymmetric unit contains two [Rh(dmpe)2] [dmpe = 1,2-bis­(dimethyl­phosphino)ethane] half-cations, lying on inversion centers, and an [RhCl2(cod)]− (cod = 1,5-cyclo­octa­diene) anion, wherein Rh is coordinated by two chloride ligands and two olefinic π-bonds of the cyclo­octa­diene ligand. The Rh atoms in the cations and anion exhibit square-planar coordination and are separated without any unusual inter­actions.
doi:10.1107/S1600536808032509
PMCID: PMC2959718  PMID: 21580855
4.  (N-Benzoyl-N′-phenyl­thio­urea-κS)chlorido(η4-1,5-cyclo­octa­diene)rhodium(I) 
The title compound, [RhCl(C8H12)(C14H12N2OS)], is a rhodium(I) derivative with a functionalized thio­urea ligand. Despite the presence of several heteroatoms, the thio­urea ligand coordinates only in a monodentate fashion via the S atom. The geometry of the coordination sphere is approximately square planar about the RhI atom, with two bonds to the π-electrons of the 1,5-cyclo­octa­diene ligand, one bond to the Cl− ligand and one bond to the S atom of the thio­urea ligand. The mol­ecular structure is stabilized by intra­molecular N—H⋯O and N—H⋯Cl hydrogen bonding. Inter­molecular N—H⋯O hydrogen-bonding inter­actions lead to the formation of layers extending parallel to (011).
doi:10.1107/S1600536810029740
PMCID: PMC3007502  PMID: 21588103
5.  Dichlorido(η4-cyclo­octa-1,5-diene)bis­(triphenyl­phosphine)osmium(II) 
The OsII atom in the title compound, [OsCl2(C8H12)(C18H15P)2], is located on a crystallographic twofold axis and adopts a distorted octa­hedral coordination geometry. The two triphenyl­phosphine ligands are trans to each other, while the two chlorine ligands are cis-disposed. The coordination is completed by the cyclo­octa­diene (COD) ligand with bonding to the two olefin double bonds. The C=C bond has a length of 1.403 (6) Å, which is significntly longer than a free olefinic double bond (≃1.34 Å).
doi:10.1107/S1600536809037817
PMCID: PMC2970349  PMID: 21577759
6.  (N-Benzoyl-N′,N′-diphenyl­thio­ureato-κ2 S,O)(η4-cyclo­octa-1,5-diene)rhodium(I) 
The title complex, [Rh(C20H15N2OS)(C8H12)], exhibits an essentially square-planar coordination environment around the RhI atom, which bears a bidentate cyclo­octa­diene ligand as well as a monoanionic bidentate benzoyl­thio­ureate ligand. The RhI atom, the S- and O-donor atoms and the alkene centroids of the cyclo­octa­diene ligand do not deviate by more than 0.031 Å from their least mean-squares plane.
doi:10.1107/S1600536812029753
PMCID: PMC3414120  PMID: 22904727
7.  (18-Crown-6)potassium [(1,2,5,6-η)-cyclo­octa-1,5-diene][(1,2,3,4-η)-naph­tha­lene]­ferrate(−I) 
The title salt, [K(C12H24O6)][Fe(C8H12)(C10H8)], is the only known naphthalene complex containing iron in a formally negative oxidation state. Each (naphthalene)(1,5-cod)ferrate(−I) anion is in contact with one (18-crown-6)potassium cation via K⋯C contacts to the outer four carbon atoms of the naphthalene ligand (cod = 1,5-cyclo­octa­diene, 18-crown-6 = 1,4,7,10,13,16-hexa­oxacyclo­octa­deca­ne). When using the midpoints of the coordinating olefin bonds, the overall geometry of the coordination sphere around iron can be best described as distorted tetra­hedral. The naphthalene fold angle between the plane of the iron-coordinating butadiene unit and the plane containing the exo-benzene moiety is 19.2 (1)°.
doi:10.1107/S160053681203704X
PMCID: PMC3470125  PMID: 23125569
8.  Chlorido(η 4-cyclo­octa-1,5-diene)(N,N′-diethyl­thio­urea-κS)rhodium(I) 
In the title rhodium(I) complex, [RhCl(C8H12)(C5H12N2S)], N,N′-diethyl­thio­urea acts as a monodenate S-donor ligand. The rhodium(I) coordination sphere is completed by the Cl atom and the COD [= 1,5-cyclo­octa­diene] ligand inter­acting through the π-electrons of the double bonds. If the midpoints of these two bonds are taken into account, the Rh atom exhibits a distorted square-planar coordination. The syn conformation of the N,N′-diethyl­thio­urea ligand with respect to the Cl atom is stabilized by an intra­molecular N—H⋯Cl hydrogen bond. A weak inter­molecular N—H⋯Cl inter­action links mol­ecules along the a axis.
doi:10.1107/S1600536810039644
PMCID: PMC3009226  PMID: 21588809
9.  μ-Oxido-bis­[hydridotris(tri­methyl­phosphane-κP)iridium(III)](Ir—Ir) bis­(tetra­fluorido­borate) dihydrate 
The title compound, [Ir2H2O(C3H9P)6](BF4)2·2H2O, was isolated from the reaction between [Ir(COD)(PMe3)3]BF4 and H2 in water (COD is cyclo­octa-1,5-diene). The asymmetric unit consists of one IrIII atom bonded to three PMe3 groups, one hydride ligand and half an oxide ligand, in addition to a BF4 − counter-ion and one water molecule of hydration. The single oxide ligand bridging two IrIII atoms is disordered across an inversion center with each O atom having a 50% site occupancy. Each IrIII atom has three PMe3 groups occupying facial positions, with the half-occupancy O atoms, a hydride ligand and an Ir—Ir bond completing the coordination sphere. The Ir—Ir distance is 2.8614 (12) Å, comparable to other iridium(III) metal–metal bonds. Two water mol­ecules hydrogen bond to two BF4 − anions in the unit cell.
doi:10.1107/S160053681400453X
PMCID: PMC3998581  PMID: 24826089
10.  trans-Carbonyl­chloridobis(tri-p-tolyl­phosphine)rhodium(I) acetone solvate 
The title compound, [RhCl(C21H21P)2(CO)]·C3H6O, was precipitated in trace yield from a reaction of RhCl(cod)(THP) with P(p-tol)3 in a 1:1 acetone-d 6/CD3OD solution under a hydrogen atmosphere [p-tol = p-tolyl, THP = tris­(hydroxy­meth­yl)phosphine, P(CH2OH)3, and cod = 1,5-cyclo­octa­diene]. The complex displays a square-planar geometry around the RhI atom. The complex mol­ecules and the acetone mol­ecules are linked into a chain along the a axis by inter­molecular C—H⋯Cl and C—H⋯O hydrogen bonds.
doi:10.1107/S1600536808003528
PMCID: PMC2960764  PMID: 21201856
11.  Chloridotris[tris­(4-fluoro­phen­yl)phosphine]rhodium(I) methanol solvate 
In the title compound, [RhCl{P(p-FC6H4)3}3]·CH3OH, the Rh atom adopts a distorted square-planar geometry. Rh, Cl and one P atom lie on a mirror plane, as does the solvent molecule. There are two inter­molecular hydrogen bonds, one between the methanol O atom and an aryl H atom (2.51 Å), and one between the Cl atom and the hydr­oxy H atom of methanol [2.34 (3) Å]. The complex precipitates in trace amounts from a reaction between RhCl(cod)(thp) [cod is 1,5-cyclo­octa­diene and thp is tris­(hydroxy­meth­yl)phos­phine] and P(p-FC6H4)3 under argon in CD3OD. Two C6H4-F units are disordered over two positions; for one the site occupancy factors are ca. 0.53 and 0.47, for the other the values are ca. 0.64 and 0.36. The methyl H atoms of the solvent molecule are disordered across the mirror plane.
doi:10.1107/S1600536808005485
PMCID: PMC2960913  PMID: 21201983
12.  (+)-{1,2-Bis[(2R,5R)-2,5-dimethyl­phospho­lan-1-yl]ethane-κ2 P,P′}(η4-cyclo­octa-1,5-diene)rhodium(I) tetra­fluorido­borate 
The title compound, [Rh(C8H12)(C14H28P2)]BF4, exhibits a rhodium(I) complex cation with a bidentate bis­phosphine ligand and a bidentate η2,η2-coordinated cyclo­octa-1,5-diene. Together the ligands create a slightly distorted square-planar cordination environment for the Rh(I) atom. There are three mol­ecules in the asymmetric unit and intra­molecular P—Rh—P bite angles of 82.78 (5), 82.97 (6) and 83.09 (5)° are observed. The dihedral angles between the P—Rh—P and the X—Rh—X planes (X is the centroid of a double bond) are 14.7 (1), 14.8 (1) and 15.3 (1)°. The structure exhibits disorder of one cyclo­octa­diene ligand as well as one BF4 anion.
doi:10.1107/S1600536810019859
PMCID: PMC2979608  PMID: 21579351
13.  Chlorido(η4-1,5-cyclo­octa­diene)[(penta­fluoro­eth­yl)diphenyl­phosphane]iridium(I) 
The title structure,[IrCl(C8H12)(C14H10F5P)], reveals that (C2F5)PPh2 (penta­fluoro­ethyl­diphenyl­phosphane or pfepp) disrupts the iridium dimer [(cod)IrCl]2 (cod = cyclo­octa-1,5-diene) by rupturing the bridging chloride ligands and binding in the open coordination site to form (cod)Ir(pfepp)Cl with the IrI atom in a distorted square-planar coordination environment. The structure deviates very little from the IrI–triphenyl­phosphine analog, although a significantly (∼20σ) shorter Ir—P bond is noted for the title compound.
doi:10.1107/S160053681005141X
PMCID: PMC3050217  PMID: 21522590
14.  Synthesis, Characterization and Molecular Structures of some Bismuth(III) Complexes with Thiosemicarbazones and Dithiocarbazonic Acid Methylester Derivatives with Activity against Helicobacter Pylori 
Metal-Based Drugs  1995;2(5):271-292.
The reactions of bismuth(III) nitrate pentahydrate and bismuth(III) chloride with heterocyclic thiosemicarbazones and derivatives of dithiocarbazonic acid methylester were used to synthesize the respective bismuth(III) complexes, which could be divided into five groups D-H because of their stoichiometrical properties and their molecular structures. The molecular structure and the near coordination sphere of the bismuth(III) central atom of four representative compounds were determined by single-crystal X-ray studies. Bis[1-azepanyl-4-(2-pyridyl)-2,3-diazapenta-1,3-diene-1-thiolato-N′,N3,S]bismuth(III) nitrate (5) belongs to group D. The two tridentate ligands and the nitrate ion surround the bismuth atom. The best description of the coordination sphere appears to be that of a distorted trigonal dodecahedron with one position occupied by the lone pair of the bismuth atom. Bis[1-azepanyl-4-(2-thienyl)-2,3-diazapenta-1,3-diene-1-thiolato-N3,S]bismuth(III) nitrate (9) is assigned to complex type E. Here, two deprotonated ligand molecules are coordinated to the bismuth(III) central atom as bidentate ligands. The structure of this complex can best be described as a distorted trigonal antiprism with a five-coordinated central atom. The two triangular faces are formed by the atoms S(4), N(6), O(11) and S(3), N(4) and the lone pair of the central atom. The two chelate rings are almost perpendicular to each other. Complex molecules of group F form dimeric units with bichloro-bridged bismuth atoms. The structure of di-μ-chlorobis[1-azepanyl-4-(2-pyridyl)-2,3-diazapenta-1,3-diene-1-thiolato-N′,N3,S-chloro]dibismuth(III) (15) can be described as two six-coordinated bismuth atoms, which are bound together via two bridging chlorine atoms. The two bismuth atoms Bi(1) and Bi(1a) and the two bridging chlorine atoms Cl(2) and Cl(2a) form the Bi2Cl2 plane. The two tridentate ligand molecules coordinate via the same atoms as shown in complex 5. In addition, they form two parallel planes, which are perpendicular to the Bi2Cl2 plane. With regard to the center of the Bi(1)-Bi(2) axis they are central point symmetrical, i.e. one pyridine ring lies above and the other beneath the Bi2Cl2 plane. Bismuth(III) chloride and pyridine-2-carboxaldehydethiosemicarbazone 1 b or 2-acetylpyridine-thiosemicarbazone 1 c form complexes of group G. Three chlorine atoms and a bidentate ligand are coordinated to the bismuth(III) central atom. The bidentate ligand bound to the central atom through the N(3) atom and the sulfur atom of the thioketo group. The structure of 18 is completely different from the structures of the bismuth(III) complexes discussed so far and was therefore assigned to group H. The bismuth central atom is coordinated with two ligands, which are bound in different ways. One of them is deprotonated. This ligand is bound to the central atom via the sulfur atom S(3) of the thiolate group and the N(5) atom. An interaction between the sulfur atom of the thiophene ring and the bismuth atom is not possible.The other ligand molecule is not deprotonated. This ligand is bound to the bismuth(III) cation merely via the sulfur atom S(1) of the thioketo group. The best description of the coordination sphere of the bismuth atom is that of a distorted square bipyramidal polyhedron. The square face is formed by the atoms S(3), N(5), Cl(1), the lone pair and the bismuth atom within. The axial positions are occupied by the atoms S(1) and Cl(2). The bond angle between S(1), Bi(1) and Cl(2) differs by about eight degrees from the value determined for a regular square bipyramidal polyhedron of 180 degrees.
Some of the newly synthesized bismuth complexes and three ligands have been tested against several strains of Helicobacter pylori bacteria in an agar dilution test. Almost all of the listed bismuth complexes show excellent inhibitory properties with regard to growth of H. pylori already at low concentrations.
doi:10.1155/MBD.1995.271
PMCID: PMC2364985  PMID: 18472778
15.  {2-[Bis(2,4-di-tert-butyl­phen­oxy)phosphan­yloxy-κP]-3,5-di-tert-butyl­phenyl-κC 1}[(1,2,5,6-η)-cyclo­octa-1,5-diene]rhodium(I) toluene monosolvate 
The reaction of (η3-all­yl)[(1,2,5,6-η)-cyclo­octa-1,5-diene]rhodium(I) with tris­(2,4-di-tert-butyl­phen­yl)phosphite in toluene produces the title compound, [Rh(C42H62O3P)(C8H12)]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite mol­ecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent mol­ecule is disordered over two different orientations, with site-occupation factors of 0.810 (2) and 0.190 (2).
doi:10.1107/S1600536812002851
PMCID: PMC3274931  PMID: 22346878
16.  (μ1-Methano­lato-κ1 O)-μ1-methoxo-κ1 O-(μ2-2-amino-1-methyl-5H-imidazol-4-one-κ2 N:N′)-hexa­carbonyl­dirhenium(I) 
In the title compound, [Re2(CH3O)2(CO)6(C4H6N3O)], the two ReI atoms are linked by a methoxo and methanolato bridge, as well as by a creatinine ligand that coordinates in a bidentate fashion. Three fac-carbonyl ligands occupy the rest of the slightly distorted octa­hedral geometry around each ReI atom. The bridging methanolato and methoxo ligands are bent out of the Re2O2 plane by 49.2 (4) and 47.8 (3)° respectively. This is normally associated with a methanolato-bridging-type coordination rather that the more planar methoxo-type bridging. Furthermore, the creatinine bridging molecule is very slightly distorted from the Re2N2C plane, indicating that the pyrazolo N atom bonded to the RhI atom is not protonated. Charge balance can thus only be attained if one assumes a positional disorder for the methanolato/methoxo H atom. All attempts to locate disordered protons around these O atoms were unsuccessful. Four hydrogen bonds, one N—H⋯O and three C—H⋯O, are observed in the structure. The mol­ecules pack in a head-to-head and tail-to-tail fashion when viewed along the c axis, in alternating columns.
doi:10.1107/S1600536812041700
PMCID: PMC3515115  PMID: 23284342
17.  {Bis[2-(dicyclo­hexyl­phosphino)phen­yl]methyl­silyl-κ3 P,Si,P′}chloridoplatinum(II) 
In the title compound, [Pt(C37H55P2Si)Cl], prepared from MeSiH[(cy)2PC6H4]2 and [Pt(cod)Cl2] (cy = cyclo­hexyl; cod = cyclo­octa-1,5-diene), the PtII atom is coordinated by two P atoms, one Si atom and one Cl atom in a distorted square-planar geometry. The two P atoms are in a trans arrangement and the four cyclo­hexane rings adopt a chair conformation.
doi:10.1107/S1600536808028857
PMCID: PMC2959269  PMID: 21201023
18.  Di-μ-oxido-bis­({2-[(R,R)-(−)-(2-amino­cyclo­hexyl)imino­meth­yl]-4-nitro­phenolato-κ3 N,N′,O}oxidovanadium(V)) dimethyl sulfoxide disolvate 
The title compound, [V2(C13H16N3O3)2O4]·2C2H6OS, is a centrosymmetric dimeric complex solvated by two dimethyl sulfoxide mol­ecules. Each VV atom is six-coordinated by one oxide group, two N atoms and one O atom from the tridentate Schiff base ligand, and by two additional bridging O atoms in a distorted octa­hedral coordination geometry. Three atoms of the cyclo­hexane ring are each disordered over two sites, with occupancy factors of 0.501 (10) and 0.499 (10). C—H⋯O and N—H⋯O hydrogen bonds link the dimers and solvent mol­ecules into a supra­molecular network.
doi:10.1107/S1600536808038762
PMCID: PMC2967873  PMID: 21581499
19.  Chemistry of a novel zerovalent ruthenium π-acidic alkene complex, Ru (η6-1,3,5-cyclooctatriene)(η2-dimethyl fumarate)2 
A novel zerovalent ruthenium complex with a π-acidic ligand, Ru(η6-cyclooctatriene)(η2-dimethyl fumarate)2 (1), was prepared from Ru(η4-cyclooctadiene)(η6-cyclooctatriene) [Ru(cod)(cot)]. Complex 1 or Ru(cod)(cot) catalyzes various new carbon-carbon bond-forming reactions that include the [2 + 2] cycloaddition of alkenes and alkynes via ruthenacycles, the creation of a new hydrocarbon, pentacyclo[6.6.0.02,6.03,13.010,14]tetradeca-4,11-diene [PCTD], by dimerization of 2,5-norbornadiene via C-C bond cleavage, and the codimerization of alkynes and/or alkenes. Complex 1 was shown to be an excellent mother complex for various zerovalent ruthenium complexes. Complex 1 reacts with amines, phosphines or water to give new zerovalent ruthenium complexes with the ligands. The resulting aqua complexes have a water ligand with an oxygen atom that is a chiral center, i.e., ruthenium complexes with a ‘chiral water’ ligand were prepared and fully characterized.
PMCID: PMC3756878  PMID: 24019585
zerovalent ruthenium complex; [2 + 2] cycloaddition; ruthenacycle; codimerization; aqua complex; chiral water
20.  catena-Poly[[[bis­(N,N-dimethyl­formamide)iron(II)]-{μ-2,2′-bis­(diphenyl­phosphino­yl)-N,N′-[(1R,2R)-cyclo­hexane-1,2-di­yl]dibenzamide}] bis­(perchlorate) N,N-dimethyl­formamide disolvate] 
The title extended solid coordination compound, {[Fe(C44H40N2O4P2)(C3H7NO)2](ClO4)2·2C3H7NO}n, was crystallized un­ex­pectedly from the reaction mixture containing the Trost ligand (1R,2R)-(+)-1,2-diamino­cyclo­hexane-N,N′-bis­(2′-di­phenyl­phosphinobenzo­yl) and Fe(ClO4)2·6H2O in a 1:1 ratio in dimethyl­formamide (DMF) under reflux conditions. The polymeric complex is characterized by FeII metal centers that are coordinated by two oxidized Trost ligands, each coordinated in a bidentate fashion in a square plane, along with two DMF mol­ecules above and below the plane [average Fe—ODMF = 2.086 (4) Å], forming an overall pseudo-octa­hedral geometry. The Trost ligand binds adjacent FeII centers, each FeII being bound through the O atom of one of the phosphine oxides [average Fe—OPPh2 = 2.115 (4) Å] and the carbonyl O atom of the adjacent amide [average Fe—Oamide = 2.192 (3) Å]. Disorder is observed in the co-solvated solvent: there are two DMF mol­ecules per FeII centre, which were modeled as one DMF mol­ecule with complete occupancy and the other being modeled in two positions with equal occupancy. Disorder was also observed with one of the perchlorate anions, which was modeled in two positions with 0.75:0.25 occupancy.
doi:10.1107/S1600536809045188
PMCID: PMC2971940  PMID: 21578561
21.  Tetra­aqua­tetra­kis{μ3-3,3′-[(E,E)-ethane-1,2-diylbis(nitrilo­methyl­idyne)]benzene-1,2-diolato}octa­zinc(II) N,N-dimethyl­formamide hexa­solvate 
The asymmetric unit of the title compound [Zn8(C16H12N2O4)4(H2O)4]·6C3H7NO, consists of eight ZnII cations, four tetra­valent anionic ligands, L 4− (L 4− = 3,3′-(1E,1′E)-(ethane-1,2-diylbis(azan-1-yl-1-yl­idene))bis­(methan-1-yl-1-yl­idene)dibenzene-1,2-bis­(olate), four coordinated water mol­ecules and six N,N-dimethyl­formamide solvate mol­ecules. The coordination complex comprises an octa­nuclear ZnII unit with its ZnII centers coordinated in two discrete distorted square-pyramidal geometries. Four ZnII atoms each coordinate to two nitro­gen atoms and two phenolate oxygen atoms from an individual L 4− ligand and one coordinated water mol­ecule. The other four ZnII atoms each bind to five phenolate oxygen atoms from three different L 4− ligands. In the crystal structure, the ZnII complex unit, coordinated water mol­ecules and dimethyl­formamide solvate mol­ecules are linked via O—H⋯O and C—H⋯O hydrogen bonds. Mol­ecules are connected by additional inter­molecular O—H⋯O and C—H⋯O hydrogen bonds, forming an extensive three dimensional framework.
doi:10.1107/S1600536809046923
PMCID: PMC2972079  PMID: 21578596
22.  (Benzoyl­acetonato-κ2 O,O′)dicarbonyl­rhodium(I) 
In the title compound, [Rh(C10H9O2)(CO)2], a distorted square-planar coordination geometry is observed around the RhI atom, formed by the O atoms of the bidentate ligand and two C atoms from the carbonyl ligands. The RhI atom is displaced from the plane through the surrounding atoms by 0.017 Å. In the crystal, C—H⋯O inter­action is observed between a methyl group of the bidentate ligand and a carbonyl O atom. Metallophilic inter­actions [3.308 (3) and 3.461 (3) Å] between neighbouring RhI atoms are encountered in the crystal, resulting in the formation of a metal chain along the b-axis direction.
doi:10.1107/S1600536812044893
PMCID: PMC3588716  PMID: 23468681
23.  ([2.2.2]Cryptand-κ6 O)potassium (η4-cyclo­octa­diene)bis­(η2-pyrene)cobaltate(1−) pentane hemisolvate  
The cation, anion, and solvent in the title compound, [K(C18H36N2O6)][Co(C8H12)(C16H10)2]·0.5C5H12, are well separated. The pentane solvent mol­ecules are found in channels along [100] and were modeled as disordered over crystallographic inversion centers. Using the mid-points of the coordinated olefins, the angle between the Cpy/Cpy–Co–Cpy/Cpy and the Ccod/Ccod–Co–Ccod/Ccod planes (py is pyrene and cod is cyclo­octa­diene) is 67.6 (2)°. Thus, the overall geometry of the coordination sphere around cobalt is best described as distorted tetra­hedral.
doi:10.1107/S1600536812029078
PMCID: PMC3393249  PMID: 22807709
24.  A tetra­nuclear chlorido-bridged manganese(II) cluster with imidazole ligands 
The crystal structure of di-μ3-chlorido-tetra-μ2-chlorido-dichloridoocta­(imidazole-κN)tetra­manganese(II) ethanol 1.234 solvate, [Mn4Cl8(C3H4N2)8]·1.234C2H5O or [Mn4Cl8(Him)8]·1.234EtOH, where Him is imidazole (C3H4N2), is based upon two Mn4Cl4 cubes which share one face, and which each lack one manganese vertex, giving a Mn4Cl6 unit. This contains two different octa­hedral coordination environments for the Mn atoms. Mn1 is coordinated by four bridging chlorido ligands and two imidazole N atoms, whereas Mn2 is coordinated by three bridging and one terminal Cl and two imidazole N atoms. The remaining two Mn centres are generated by inversion symmetry. A partial occupancy solvent mol­ecule (ethanol) is present. The crystal structure displays several N—H⋯Cl and N—H⋯O hydrogen bonds.
doi:10.1107/S1600536808029139
PMCID: PMC2959378  PMID: 21201026
25.  [(1,2,5,6-η)-Cyclo­octa-1,5-diene]bis­(4-methyl­phen­yl)platinum(II) 
In the mononuclear title complex, [Pt(C7H7)2(C8H12)], the PtII ion exhibits a square-planar coordination geometry defined by two methyl­phenyl ligands and the mid-points of the two π-coordinated double bonds of cyclo­octa-1,5-diene. The two methyl­phenyl groups have a cis relationship with a C—Pt—C bond angle of 88.54 (18)° and a dihedral angle between the mean planes of the benzene rings of 83.87 (1)°. Each complex mol­ecule links to four symmetry-related ones through inter­molecular C—H⋯π inter­actions, forming a layer almost parallel to the bc plane.
doi:10.1107/S1600536810049664
PMCID: PMC3050351  PMID: 21522559

Results 1-25 (544834)