Synthesis, spectroscopy, and X-ray structures of fac-(CO)3(dppe)MnSC(S)H, fac-(CO)3(dppe)ReSC(S)H, fac-(CO)3(dppp)ReSC(S)H, and fac-(CO)3(dppb)ReSC(S)H

The monodentate dithioformato complexes, fac-(CO)₃(dppe)MnSC(S)H (1), fac- (CO)₃(dppe)ReSC(S)H (2), fac-(CO)₃(dppp)ReSC(S)H (3), and fac-(CO)₃ (dppb)ReSC(S)H (4), where dppe is 1,2-bis(diphenylphosphino)ethane, dppp is 1,3-bis(diphenylphosphino)propane, and dppb is 1,4-bis(diphenylphosphino)butane, were synthesized from the treatment of the corresponding hydrides, fac-(CO)₃ (P-P)MSC(S)H with CS₂. Compounds 1–4 crystallize in the monoclinic crystal system: for 1, space group = P2₁/c, a = 15.3139(3) Å, b = 9.7297(4) Å, c = 19.0991(6) Å, = 105.928(1), V = 2736.5 ų, Z = 4; for 2, space group = P2₁/c, a = 15.6395(8) Å, b = 9.8182(5) Å, c = 19.4153(11) Å, = 106.741(1), V = 2854.9(3) ų, Z = 4; for 3, space group = P2₁/n, a = 11.3570(10) Å, b = 19.465(2) Å, c = 15.5702(14) Å, = 104.776(2), V = 3328.3(5) ų, Z = 4; and for 4, space group = C2/c, a = 32.078(2) Å, b = 10.4741(6) Å, c = 19.0608(9) Å, = 94.315(2), V = 6386.1(6) ų, Z = 8.     

Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

The crystal and molecular structures oftrans-[PtCl₂(C₂H₄)(4-MeC₅H₄N)] (I) andtrans-[PtCl₂(C₂H₄)(2,4,6-Me₃C₅H₂N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP2₁/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl₂(C₂H₄) moiety.     

X-ray crystal structures ofcis-bis(diphenylphosphinamide)tetracarbonylmolybdenum(0) andtrans-bis(N-methyl diphenylphosphinamide)tetracarbonylmolybdenum(0)

The X-ray crystal structures ofcis-Mo(CO)₄(Ph₂PNH₂)₂,I, andtrans-Mo(CO)₄(Ph₂PNHMe)₂,II, are presented. ComplexI crystallizes in the monoclinic space groupP2₁/c(a=13.433(1),b=12.2719(8),c=17.318(2)Å;=109.79(1)°;V=2686.1(8)ų;Z=4). ComplexII crystallizes in the triclinic space groupP¯1 (a=6.9986(8),b=10.328(1),c=11.241(2)Å,=107.58(1)°,=91.76(1)°, =101.28(1)°,V=756.1(4)ų,Z=1). The molybdenum coordination geometry in each complex is a slightly distorted octahedron. The molybdenum-carbon bond lengths for the carbonyls trans to phosphorus in complexI are shorter than those the carbonyls trans to other carbonyls. The average molybdenum-phosphorus distance inI (2.525(5)Å) is similar to those in other diphenylphosphinamide complexes and longer than the molybdenum-phosphorus distance inII in 2.4585(7)Å). The distance between two nitrogen atoms incis Mo(CO)₄(Ph₂PNH₂)₂ (3.74(3)Å) is significantly larger than the sum of their van der Waals radii (3.10 Å) indicating that the two nitrogens are not hydrogen bonded.     

Crystal structure of triphenylphosphine-(1-(di(trifluoromethyl)-hydroxymethyl)-cyclopentadienyl)-(1,2-di(carboxymethyl) ethylene-1-yl) ruthenium (0)

The structure of triphenylphosphine — (1 — (di(trifluoromethyl) — hydroxymethyl) — cyclopentadienyl) — (1,2 — di(carboxymethyl)ethylene — 1 — yl) — ruthenium (0) has been studied by single-crystal X-ray diffraction techniques. This compound, [C₅ H₄(CF₃)2 COH] Ru(PPh₃)C2(CO₂Me)₂H, crystallizes in the triclinic space groupP¯1 witha =10.131,b= 15.107,c= 10.798 Å, = 102.14, = 107.04, = 89.64° andZ = 2. The structure was refined by block-diagonal least-squares methods to a finalR value of 0.042, including hydrogen atoms. The compound contains a dicarboxymethylethylene ligand coordinated to ruthenium both through a ketonic oxygen and through a metal--carbon -bond. An intramolecular hydrogen bond is observed. Details of the structure are reported, and the structures of several Ru(0) complexes are compared.     

Crystal Structure of Decakis(μ-chloro)-tetrakis(1,2,4-triphenylcyclopentadienyl)-hexakis(tetrahydrofuran)-di-potassium-tetra-neodymium(III) Tetrahydrofuran Trisolvate

Journal of Chemical Crystallography - The crystal structure of decakis(μ-chloro)-tetrakis(1,2,4-triphenylcyclopentadienyl)-hexakis(tetrahydrofuran)-di-potassium-tetra-neodymium(III)...     

Structure of (chloranilato)bis(tri-n-butylphosphine)palladium(II)

(Chloranilato)bis(tri-n-butylphosphine)palladium(II), [Pd(C₆Cl₂O₄){P(C₄H₉)₃}₂] (chloranilic acid=2,5-dichloro-3,6-dihydroxy-p-benzoquinone): FW=718.02,P2₁/c,a=21.729(6),b=17.293(5),c=21.010(9) Å,=112.62(3)°,V=7287.42 ų,Z=8,D _c=1.309mg m^–3, Mo, =0.710730 Å,=0.76 mm^–1,F(000)=3008, finalR=0.087, 2594 observed reflections. Palladium is ligated by a distorted square planar P₂O₂ coordination sphere in the title compound. The two molecules per asymmetric unit differ in the arrangement of phosphine n-butyl chains, yielding two unique metal centers.     

Structure of (N-(2-hydroxyphenyl)-salicylaldiminopiperidino) Ni(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂O₂Ni, has been determined by direct methods. The compound crystallizes in the monoclinic crystal system witha=22.973(1),b=5.212(1),c=27.076(1)Å, β=106.46(1)°, space groupC2/c,V=3109.1(6)ų, Z=8, andD _x=1.51g cm^?3. The nickel atom is in a slightly distorted square-planar environment of two oxygens [Ni(1)?O(1) 1.824(3) and Ni(1)?O(2) 1.856(3)Å] and two nitrogens [Ni(1)?N(1) 1.849(3) and Ni(1)?N(2) 1.932(3)Å] with O?Ni?N angles between 85.7(1) and 97.1(1)°. The nickel atom is 0.006 Å out of the plane of its ligands.     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.     

Crystal of catena-(μ2-terephthalato)-bis (N-methylimidazole)-copper(II)

A new one-dimensional chain complex [Cu(ta) (N-MeIm)₂]n (where ta = terephthalic acid dianion,N-MeIm =N-methylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Monoclinic space groupP2₁/c with the parameters:a = 5.2930(11)Å,b = 14.679(3)Å,c = 11.007(3)Å, β = 104.84(3)^°,V = 826.7(3)ų, withZ = 4 formula units. In the structure, each Cu atom is coordinated by a pair ofN-methylimidazole ligands and a pair of monodentate carboxylate groups, affording a square planar N₂O₂ geometry. Both carboxylate groups of the terephthalate dianion coordinate in a monodentate mode bridging two Cu(II) ions with formation of 1D zigzag chain along thec axis. This supramolecular compound exhibits a three-dimensional solid state structure constituted by hydrogen bonds and C–H–π stacking interactions.     

Crystal of Tetrakis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II)

Abstract  A new complex [Cu(NCS)₄ (N-Eim)₄] [Cu(NCS)₂ (N-Eim)₂] (where N-Eim = N-ethylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Triclinic space group P−1 with the parameters: a = 8.7707(18) ?, b = 10.712(2) ?, c = 13.511(3) ?, α = 104.73(3)°, β = 104.84(3)°, γ = 102.52(3)°, V = 1131.54(3) ?³, with Z = 1 formula units. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments; one is coordinated by four N-ethyl-imidazole ligands and two axial SCN groups, and another by two SCN groups and two N-ethyl-imidazole ligands. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim)₄] units. Index Abstract  The title compound, tetrakis(1-ethyl-1H-imidazole)diisothio cyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim) 4] units.      

Crystal and molecular structures of trans-bis(acetonitrile)bis(bipyridine)ruthenium(II) perchlorate and trans-diamminebis(bipyridine)ruthenium(II) perchlorate

The structures of trans-[(MeCN)₂(bpy)₂Ru](ClO₄)₂(I) andtrans-[(NH₃)₂(bpy)₂Ru](ClO₄)₂(II) have been determined by single crystal X-ray diffraction methods. (I) forms monoclinic crystals in the space groupP2₁/c witha=8.399(2),b=10.406(2),c=15.590(3) Å,=93.78(2)° andZ=2 atT=293 K. The final refinement gaveR=0.040 for 2448 reflections withF _o ² >3(F _o ² ). (II) crystallizes in the triclinic space groupP¯1 witha=1.702(1),b=8.439(2),c=10.525(2) Å,=107.56(2),=104.63(1), =100.89(2)° andZ=1 atT=293 K. Refinement using 1878 reflections withF _o ² >3(F _o ² ) produced a finalR value of 0.036. Both of these structures have the ruthenium atom located on a crystallographic inversion center. The bipyridine ligands in both structures are in the bowed conformation as a means of circumventing the steric problems associated with the trans arrangement of the bipyridine ligands. The Ru-N(monodentate) distance is longer for the ammonia complex (2.106(3) Å) than for the acetonitrile complex (2.008(4) Å); there are no significant differences in the distances and angles of the two Ru(bpy)₂ frameworks.     

Synthesis and X-ray structure of dichlorobis(8-(diphenylphosphinyl)quinoline)nickel(II)

Dichlorobis(8-(diphenylphosphinyl)quinoline)nickel(II) was formed in the reaction of 8-(diphenylphosphino)quinoline with nickel chloride in air. The title complex crystallized in P1 with the following cell dimensions: a = 8.5685(3) Å, b = 10.7736(2) Å, c = 13.4391(5) Å, and = 110.447(2)°, = 94.577(2)°; = 111.138(2)°, giving a volume of 1053.75(6) ų. The trans-dichlorobis(8-(diphenylphosphinyl)quinoline) nickel(II) adapts a central symmetric distorted octahedron. The structure is compared to other nickel(II) cation complexes, and possible reasons for the bonding states are discussed.     

Synthesis and structure of tetrakis(2,6-dichlorophenoxide) bis(THF) uranium(IV)

The reaction of UCl₄ with KO-2,6-Cl₂C₆H₃ in tetrahydrofuran results in the preparation of the title compound. The six-coordinate complex possesses pseudo-octahedral geometry about uranium, with U-O(phenoxide) bond lengths in the range 2.161(11) to 2.178(10) Å and U-O(THF) bond lengths of 2.467(10) and 2.475(11) Å. This complex crystallizes in the monoclinic space group P2₁/n (a = 11.169(2), b = 11.588(2), c = 35.119(5) Å, = 92.11(1)°, V = 4542.2(13) ų, and Z = 4).     

X-ray crystal structure of trans-bis(monoethanolamine) bis(saccharinato)nickel(II)

The crystal structure of trans-bis(monoethanolamine)bis(saccharinato)nickel(II), [Ni(C₇H₄NO₃S)₂(C₂H₇NO)₂], has been determined from X-ray diffraction data. The metal complex is monoclinic, with a = 11.0555(5), b = 8.9103(4), c = 11.3890(5) Å, = 105.0230(10)°, Z = 2, and space group P2_1/c . The structure consists of individual molecules. Two monoethanolamine molecules and two saccharinate anions coordinate the nickel atom forming a distorted octahedron. The monoethanolamine molecules act as a bidentate ligand and form five-membered trans chelate rings, which constitute the plane of the coordination octahedron, while two saccharinate ions behave as a monodentate ligand occupying the axial positions. Intermolecular hydrogen bonds link the molecules to form a three-dimensional infinite structure.     

Crystal structure of bis(4-dimethylaminopyridinium) tribromocuprate(I) and bis(4-dimethylaminopyridinium) tetrabromocuprate(II)

The synthesis and crystal structures of two copper bromide salts of the 4-dimethylaminopyridinium (4DMAP⁺) cation are reported. The Cu(I) salt, (4DMAP)₂CuBr₃, crystallizes in the monoclinic space group C2/c, with a = 11.724(2), b = 11.055(3), c = 15.763(3) Å, = 107.64(3)°, and Z = 4. It contains isolated planar 4DMAP⁺ cations and trigonal planar CuBr₃ ^2– anions. Small distortions from idealized D _3h symmetry are observed for the anion. For the Cu(II) salt, (4DMAP)₂CuBr₄, a triclinic cell is observed with a = 8.2373(2), b = 9.2428(2), c = 14.4391(1) Å, = 93.760(1), = 94.576(1), = 105.249(1)°, and Z = 2. This compound contains discrete planar 4DMAP⁺ cations and flattened tetrahedral CuBr₄ ^2– anions. Small distortions are observed for ideal D _2d symmetry.     

Growth and characterization of diaquatetrakis (thiocyanato) cobalt (II) mercury (II) N-methyl-2-pyrolidone (CMTWMP) single crystals

Single crystals of diaquatetrakis (thiocyanato) cobalt (II) mercury (II) N-methyl-2-pyrolidone, (CoHg(SCN)₄·(H₂O)₂·2(C₃H₆CONCH₃) (abbreviated as CMTWMP) were grown using slow solvent evaporation technique. The structure of the grown crystals was confirmed by single-crystal X-ray diffraction (XRD) technique. The optical properties of the crystals were investigated by Fourier transform infrared (FTIR) and UV–Vis–NIR transmission spectra. The grown crystals of CMTWMP were also subjected to dielectric, photoconductivity, thermal and microhardness studies. The photoconductivity study of CMTWMP confirms the electrochromism behaviour in the sample. The SHG efficiency of the sample was measured by Kurtz and Perry powder technique and its value is almost comparable with KDP.     

Reaction of bis(dimethoxyphosphino)dimethylhydrazine (dmpdmh) with PhCCo3(CO)9: synthesis and X-ray characterization of the dmpdmh-bridged polymorphs of PhCCo3(CO)7[(MeO)2PN(Me)N(Me)P(OMe)2]

The tricobalt cluster PhCCo₃(CO)₉ reacts with the bis(phosphanyl)hydrazine ligand bis(dimethoxyphosphino)dimethylhydrazine (dmpdmh) to give the monosubstituted cluster [PhCCo₃(CO)₈]₂(dmpdmh) and the disubstituted cluster PhCCo₃(CO)₇(dmpdmh) as the major products. This latter cluster contains a bridging dmpdmh ligand. Both IR and NMR spectroscopies (³¹P and ¹H) have been employed in the solution characterization of these two clusters. The solid-state structure of PhCCo₃(CO)₇(dmpdmh) was unequivocally established by X-ray diffraction analysis, which has revealed the presence of two different polymorphs for this particular cluster. The first polymorph crystallizes in the monoclinic space group P2₁/n, a = 9.7127(7) Å, b = 17.025(2) Å,c = 16.894(1) Å, = 96.245(5)°, V = 2777.0(4) ų, Z = 4, and d _calc = 1.689 g/cm³; while the second polymorph crystallizes in the orthorhombic space group Pbca, a = 16.925(2) Å, b = 16.208(2) Å, c = 20.541(3) Å, V = 5635(1) ų, Z = 8, and d _calc = 1.665 g/cm³.     

Structure of chlorohydroxonitrosyl(terpyridine)ruthenium(II) hexafluorophosphate

The title complex has the NO grouptrans to the hydroxyl ligand and the chloride ion in the plane of the tripyridyl ligand. The Ru?O and Ru?N(O) distances are 1.939(5) Å and 1.764(6) Å, respectively; the Ru?N?O bond angle is 171.7(6)⁰. These values are consistent with previously reported shortening of Ru?O distances whentrans to a linear NO ligand. The space group of the structure isP2₁/c, witha=9.7213(9) Å,b=13.9318(11) Å,c=14.523(4) Å, and β=105.820(13)⁰.     

Structure of trans-aqua-bis(pyridine)dibenzoatocopper(II)

Crystals oftrans-aqua-bis(pyridine)dibenzoatocopper(II), Cu(NC₅H₅)₂(C₇H₅O₂)₂(H₂O), are monoclinic,P2₁/n, witha=5.9847(10),b=18.874(5),c=19.728(10)A,=92.97(4)°,Z=4, andV=2225.5(13)A³. The full-matrix least-squares refinement used 3030 reflections withI> 2.5(I) and converged toR=0.067. The benzoate ions bond as monodentate ligands in this five-coordinate complex. The copper ion is in a square pyrimidal environment with trans pyridine groups and benzoate ions in a slightly distorted square planar arrangement and a water ligand in the axial position. The Cu-O distance to the water molecule is significantly longer (2.273(4) Å) than the distances to the O atoms of the carboxyl groups (1.934(3) and 1.930(4)Å).     

EPR spectra of (L-aspartate)di(2-pyridyl)aminezinc(II) hydrate substitutionally copper(II) doped complex

The [(L-aspartate)di(2-pyridyl)aminezinc(II)]hydrate doped with traces of copper was prepared. Electron paramagnetic resonance spectra of the polycrystalline sample were recorded at room temperature by using the X-band of the EPR spectrometer. The observedg factors for the complex areg _‖=2.258 andg _⊥=2.066. TheA _‖ value is 165.10⁻⁴ cm⁻¹. The crystal and molecular structure of the complex are also reported. The complex crystallizes in the monoclinic system; space groupP2₁ witha=7.2053(11),b=10.447(2),c=10.812(2) Å, β=108.489(14)° andZ=2. The structure can be described in the crystal lattice as polymeric chains.