The crystal structure of triiodo (η5-methoxycarbonyl-cyclopentadienyl)-dicarbonylmolybdenum(IV)

Crystals of (C₅H₄COOMe)Mo(CO)₂I₃ are monoclinic, space-group P2₁/c, with a = 9.402(2), b = 10.675(3), c = 15.314(2) Å, = 106.79(1)°, and Z = 4. The coordination geometry is distorted octahedral with the ring centroid at one vertex and the iodide ligands defining a face.     

Crystal structure of the methanol solvate of (η5-cyclopentadienyl)[1,2-bis(diphenylphosphino)ethane] nitroruthunium(II) Ru(η5-C5H5)dppe)(NO2)·CH3OH

The title complex crystallizes in the centrosymmetric monoclinic space group C2/c (No. 15) withZ=8. The structure was refined toR=4.49% for those 2745 independent reflections with 2=5–50^o and |F |>6(F). Ruthenium-ligand distances are as follows: Ru-P=2.284(2) and 2.286(2) Å, Ru-NO₂=2.049(6) Å and Ru-C(Cp)=2.210(10)-2.246(9) Å. Bond lengths within the nitro ligand are N(1)-O(1)=1.226(10) Å and N(1)-O(2)=1.244(10) Å. The methanol of solvation is ordered but is subject to large thermal vibrational motions.     

Crystal structure of 2-pyridiniumferrocene tetrafluoroborate Fe(η5-C5H5)[(η5-C5H4)(2-C5H4NH+)](BF 4 − )

Protonation of Fe( ⁵-C₅H₅)[( ⁵-C₅H₄)(2-C₅H₄N)]1 in 98% H₂SO₄ followed by dilution with water and addition of NaBF₄ yields Fe( ⁵-C₅H₅)[( ⁵-C₅H₄)(2-C₅H₄NH⁺)](BF ₄ ^– )2 instead of a ferrocinium derivative. Complex2 crystallizes in the monoclinic system, P2₁ /a:a=7.984(1),b=9.981(2),c=18.220(4) Å,=102.31 (1)°,V=1418.5 ų,Z=4. The pyridinium ring makes a dihedral angle of 21.0(2)° with the cyclopentadienyl ring to which it is bound. One F atom of BF ₄ ^– is involved in short van der Walls contacts with the N (2.764(5) Å) and the H (2.08(6) Å) atoms of the NH⁺ moiety.     

X-ray structure of 3,3′-bis(4-methylthioquinolinyl) sulfide

The structure of the title compound has been solved by direct methods, and refined to anR value of 0.035 for 1613 reflections. Both methyl carbon atoms deviate from the plane of the pyridine ring by 1.505(3) Å in opposite directions. Both sulfur atoms S(1) and S(2) remain in short contact, at 3.247(1) Å. The two pyridine rings are inclined at 61.4(2)° to each other.Part XIV in the series of Azinyl Sulfides.     

Crystal structure of a (μ-bis(carbene))dimetal complex of tungsten

The (-bis(carbene))ditungsten complex, (CO)₅W{(C(OCH₂Ph)C(CH₂C₂H₃)(Me)CH₂CH₂C(OCH₂Ph)}W(CO)₅ (1) is only the fifth such complex to be crystallographically characterized. The steric demands of one side of the bis(carbene) ligand gives rise to small, but statistically significant differences in the bonding parameters to W. The W=C distances are 2.195(4) and 2.171(6)Å. The carbonyltrans to the longest W=C bond has the shortest of the ten W-CO separations (1.994(5)Å) and the longest CO bond length (1.156(6)Å). The planes defined by the two carbene groups have a dihedral angle of 44.5°.     

Crystal structure of phenyl bis(O-isopropylxanthato s,s′)arsenic(III)

The crystal structure of the title compound PhAs(S₂COPrⁱ)₂ has been determined by single crystal X-ray diffraction and refined by full matrix least squares analysis with anisotropic temperature factors. The crystal is monoclinic, space groupP2₁/c,a=8.889(6),b=16.174(19),c=13.506(14) Å,=102.02(7)°,V=1899.2 ų,Z=4,D _c=1.478 g cm^–3, monochromated Mo-K radiation, =0.71069 Å,=22.07 cm^–1.The geometry around the arsenic atom is square pyramidal. Each ligand is bonded to an arsenic atom through two unequal As-S bonds measuring 2.298 and 3.041 Å. The apical position is occupied by a phenyl group and a lone pair of electrons is presenttrans to the phenyl group.     

Crystal structure of octacalcium bis(hydrogenphosphate) tetrakis(phosphate)pentahydrate,Ca8(HP04)2(PO4)4·5H2O

The crystal structure of octacalcium bis(hydrogenphosphate) tetrakis(phosphate)pentahydrate, Ca₈(HPO₄)₂(PO₄)₄·5H₂O, has been refined toR=0.051 for 4502 reflections. The crystals are triclinic:P¯1,a=19.692(4),b=9.523(2),c=6.835(2) Å,=90.15(2),=92.54(2), and =108.65(1)°,Z=2. The structure can be considered to consist of two layers parallel to (100), an apatitic layer which corresponds very closely to that of hydroxyapatite and a hydrated layer which contains all the water molecules. Several atoms in the hydrated layer are probably disordered. Possibilities for the hydrogen-bonding arrangement are discussed.     

Crystal structure of chloro(dicarbonyl) bis(acetonitrile) (π-2-methallyl) molybdenum(II)

The title compound crystallizes in the monoclinic spacegroup P2₁/m with a = 6.796(9), b = 12.145(14), c = 7.749(8)Å, = 101.86(1)°, and Z = 2. The crystal structure consists of molecules of [MoCl(CO)₂(NCMe)₂(³-C₃H₄Me-2)] with crystallographically imposed C_s symmetry and has a pseudo-octahedral geometry, with the -allyl group trans- to the chloro group and the two cis-carbonyl and acetonitrile groups occupying the equatorial plane.     

Crystal structure and spectroscopic study of bis{1,3-bis[3-(5-amino-1,2,4-triazolyl)]triazenido-N′4,N2,N″4}nickel(II) tetrahydrate

The title compound [Ni(batt)₂]·4H₂O, in which Hbatt is 1,3-bis[3-(5-amino-1,2,4-triazolyl)]triazene, has been prepared and its crystal structure determined by X-ray diffraction methods. The compound crystallizes in the tetragonal space group I4/m (a = 10.5645(8) Å, c = 9.1336(6) Å, and Z = 2). The Ni(batt)₂ molecule has local 4¯ symmetry, but it is located on a crystallographic 4/m site and is disordered over the mirror plane. The ligand batt^– is tridentate with nitro-type coordination of the triazenido group and N⁴ coordination of the two outer triazolyl substituents. The complex has a distorted octahedral geometry with meridional configuration of the two nearly planar batt^– ligands. The geometry of the tridentate cavity is examined and a comparison is made with the Ni-terpyridyl system, which shows similar coordination around the nickel center. The FTIR, micro-Raman, and UV-vis spectra are analyzed in relation with the structure.     

Crystal structure and magnetic properties of bis(2,2′-bipyridine) azido copper(II) perchlorate

The title compound has been synthesized and its crystal structure has been solved at room temperature. It crystallizes in the triclinic system, space groupP, witha=7.853(1) Å,b=10.177(1) Å,c=13.651(4) Å,=74.57(1)°,=88.49(1)°, =80.675(4)°, andZ=2. The structure consists of isolated [Cu(bipy)₂N₃]⁺ cations (bipy=2,2-bipyridine) and perchlorate anions. The metallic cation environment has a distorted trigonal-bipyramidal geometry. The EPR spectrum is rhombic, which indicates that the distortion with respect to the perfect trigonal bipyramid is sufficiently pronounced to mixz ²- andx ²–y ²-type orbitals in the ground state. The temperature dependence of the molar magnetic susceptibility has been investigated in the 300-2.2 K temperature range.     

Crystal and molecular structure of μ-oxobis[bis(dipropyl dithiophosphato) oxomolybdenum(V)]

The title compound is triclinic, space group P¯1,a=10.670(5)b=13.053(3),c=8.944(5) Å,=100.18(3),=92.16(4),=80.88(3)°,Z=1,V=1210.4 ų, andR=0.043 for 2579 reflections. The molecule has two distorted octahedra sharing a corner occupied by an oxygen (bridging) atom, the Mo-O_b-Mo angle being 180°. The two molybdenum-oxygen bond lengths Mo-O_b (bridging) and Mo-O₁, (terminal) are 1.92 and 1.62 Å, respectively. Except the Mo-S bondtrans to the terminal oxygen atom which has a bond length 2.81 Å, all other Mo-S bonds have an average length of 2.50 Å.     

Crystal structure of N,N ′-bis(cyclohexyl)-1-(N,N-dihexylamino)perylene-3,4:9,10-bis(dicarboximide)

An asymmetric dialkylamino-substituted perylene bisimide (1), N,N′-bis(cyclohexyl)-1-(N,N-dihexylamino)perylene-3,4:9,10-bis(dicarboximide), was synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P–1, with a = 9.8924(6), b = 14.6338(10), c = 15.6221(10) Å, α= 105.098(3)°, β = 103.386(2)°, γ = 107.772(3)°, and Z = 2. The central perylene core of 1 is twisted with dihedral angles of 14.9(3)° and 11.6(3)°; this twist configuration induces the axial chirality in this family of perylene bisimide dyes. In the crystal structure, the intermolecular C–H···O interaction links a pair of molecules into a cyclic centrosymmetric dimer that is connected to one another via the intermolecular π–π stacking, so linking the molecules into a continuous one-dimensional framework along the [100] direction.     

Crystal structures of (η5-C5H4COMe)M(CO)3Me (M=Mo,W)

The crystal structures of ( ⁵-C₅H₄COMe)M(CO)₃Me (M=Mo,W) have been determined. They are not isostructural. M=Mo isP2₁/c,a=10.205(6),b=14.192(8),c=8.135(6) Å,=93.43(4)° andD(calc)=1.71 g cm^–3 forZ=4. M=WisP2₁/c,a=12.580(7),b=6.830(5),c=13.750(7) Å,=93.72(4)° andD(calc)=2.20 g cm^–3 forZ=4. Both have a four-legged piano stool geometry with the substituted carbon making the closest M-C( ⁵) approach. The methyl group in the M=W derivative is disordered between twotrans-ligand positions. The average bonding parameters for the more accurately determined Mo analog are: Mo-C()⁵)=2.34(3) Å, Mo-CO=1.98(2) Å, Mo-Me=2.304(4) Å.     

Crystal and molecular structure of aqua(2,2′-bipyridine)bis(betaine)copper(II) perchlorate monohydrate

A new monomeric copper(II) complex with 2,2-bipyridine (bpy) and betaine (bet), [Cu(byy)(bet)₂(H₂O)](ClO₄)₂ · H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space groupP-1 witha=8.859(2),b=11.191(2),c=14.850(3) Å, =91.41(1), =97.19(1), =91.97(1)°,V=1459.2(7) ų, andZ=2. The structure comprises discrete cations [Cu(bpy)(bet)₂(H₂O)]²⁺ in which the metal atom is coordinated in a distorted square-pyramidal environment by two oxygen atoms from a pair of monodentate carboxylato ligands [Cu–O=1.950(2) Å] and two nitrogen atoms of a bidentate bpy ligand [Cu–N=1.997(3)–2.005(3) Å] on the basal plane, and one aqua [Cu–O=2.267(3) Å] ligand at the apical position.     

Crystal structure of radical cation salt (BEDT-TTF)4(GaCl4)2 · C6H5CH3

A new radical cation salt based on bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) with the tetrahedral anion GaCl ₄ ^? , namely, (BEDT-TTF)₄(GaCl₄)₂ · C₆H₅CH₃, has been synthesized. The crystal structure of this salt is determined by X-ray diffraction analysis [a = 31.757(2) Å, b = 6.8063(3) Å, c = 34.879(2) Å, β = 90.453(4)°, V = 7538.8(7) ų, space group I2/c, and Z = 4]. In the structure, the radical cation layers alternate with the anion layers along the c-axis. The anion layers consist of the GaCl ₄ ^? tetrahedra and solvent molecules. The packing of BEDT-TTF molecules in the radical cation layer differs from that in the structure of the known salt (BEDT-TTF)₂GaCl₄, even though both compounds exhibit semiconductor properties.     

Crystal and molecular structure of [Pd(η5-C5H5) (bis-1,2-diphenylphosphinoethane)] [CF3SO3]

The crystal structure of the complex [Pd( ⁵-C₅ H₅) (PPh₂) CH₂CH₂PPh₂]⁺ [CF₃SO₃]^– has been determined from single crystal X-ray data and refined by least-squares methods toR=0.046. The monoclinic crystals have unit cell dimensionsa=9.832(3),b=12.104(4),c=13.765(4)Å,=111.22(3)°, space group P2₁, andz=2. In the cationic complex the palladium atom is coordinated to the ⁵-cyclopentadienyl moiety and to the phoshorus atoms of the chelating diphosphine. The arrangement of the two phosphorus atoms and the centroid of the cyclopentadienyl ring is approximately trigonal.     

Crystal structure of (3-aminopropionato)bis(ethylenediamine)cobalt(III) catena-di(μ-chloro)dichloroplumbate(II) monohydrate

Crystals of [Co(C₂H₈N₂)₂(C₃H₆NO₂)]PbCl₄ · H₂O [a = 7.627(1) Å, b = 11.238(1) Å, c = 11.444(1) Å, α = 99.125(1)°, β = 103.80(1)°, γ = 94.739(1)°, V = 933.09(1) ų, Z = 2, and space group $P\bar 1$ ] contain the octahedral PbCl₆ groups that share edges to form infinite [Cl₂Pb(μ-Cl)₂] _n ²ⁿ chains, in which the terminal Cl atoms occupy the cis positions. The Pb-Cl bond lengths are 2.763(1)–3.180(3) Å. In the discrete cationic complexes, the Co atom is coordinated by two ethylenediamine molecules and the 3-aminopropionate anion. In the enantiomeric complex with the Δ absolute configuration, the ethylenediamine rings have the λ and δ configurations and the aminopropionate ring has the λ configuration.     

Supramolecular structure of tetrakis-μ-(4-chloro-3-nitrobenzoato)-bis(methanol)dicopper(II)

The title compound, [Cu₂(II)(4-Cl-3-NO₂–C₆H₃CO₂)₄(CH₃OH)₂] or [Cu₂(4-chloro-3-nitrobenzoate)₄(MeOH)₂] has been prepared and its structure determined using X-ray crystallography. The complex crystallizes in the triclinic space group P-1 with a = 9.6887(9)Å, b = 10.6448(9)Å, c = 11.4194(10)Å, = 108.094(2), = 110.682(2), = 105.055(2), V = 952.691(15)ų, and Z = 1. The structure consists of centrosymmetric dimers in which the Cu(II) atoms display a square pyramidal CuO₅ coordination, with four carboxylate O atoms in the basal plane [CuO 1.951(2)–1.968(2)Å] and the methanol O atoms in the apical position [CuO 2.170(2)Å]. The Cu atoms are 2.614(1)Å apart and are bridged by four benzoate groups. The discrete dimers are extended into 1D chains that result from hydrogen bonding between the coordinated methanol on one Cu(II) dimer and the nitro substituent on an adjacent Cu(II) dimer. The chains are interdigited and held by – stacking interactions forming 3D supramolecular array.     

Crystal structures of [(η5-C5H4COOH)W(CO)3R] (R=Me,I)

The crystal structures of [(₅-C₅H₄COOH)W(CO)₃R] (R=Me, I) have been determined. They crystallize in two different monoclinic space groups. R=Me isP2₁/c,a=10.4833(6),b=8.0144(7),c=13.0731(6) , =93.147(4)°, andD(calc)=2.374 g-cm^–3 forZ=4. R=I isP2₁/n,a=7.814(2),b=13.075(4),c=11.097(4) , =91.75(2)°, andD(calc)=2.953 g-cm^–3 forZ=4. Both possess a four-legged piano stool geometry. The methyl ligand in the R=Me complex is disordered between two positions insyn oranti relative to the substituted carbon of the cyclopentadienyl ligand. The iodo ligand in the R=I complex is, however, exclusively insyn-position.     

The structure of (1,2:5, 6η-cyclononatetraene) (η-cyclopentadienyl)cobalt,CoC14H15

The title compound crystallizes in the monoclinic space groupP2₁/a,a=11.50(2),b=7.724(1),c=12.599(3) Å,=102.22(5)°,Z=4. The structure was solved by direct methods and refined by full-matrix least squares toR=0.049 for 1032 observed reflections. The cobalt atom is -bonded to the cyclopentadienyl ring, with a mean Co-C distance of 2.07(1) Å, and also -bonded to the cyclonoatetraene ring at C(2)-C(3) and at C(6)-C(7), with a mean Co-C distance of 2.00(1) Å.