The Synthesis and Structure of (1-(Diphenylphosphino)-1 - (Phenylthio)Ferrocene)Tricarbonyliron(O) (ptppf)Fe(CO)3

The complex (ptppf)Fe(CO)₃ has been prepared in high yield by the reaction of ptppf, l-(diphenyl-phosphino)-l'-(phenylthio)ferrocene, with (cis-cyclooctene)₂-Fe(CO)₃ in THF at ?60°C. The complex has been characterized by IR, ³¹P NMR, mass spectrometry and single-crystal X-ray diffraction. This compound is the first example of a ferrocenyl ligand having both sulfur and phosphorus donor atoms bound to a Fe(CO)₃ moiety. X-ray crystallography shows that the two cyclopentadienyl rings are approximately eclipsed, a rotation of 13° from exactly eclipsed conformation. The tricarbonyl iron center has a trigonal bipyramidal geometry with sulfur occupying the equatorial site and phosphorus the axial site. Crystals of (ptppf)Fe(CO)₃ are monoclinic, with a = 11.645(2), b = 14.304(1), c = 17.075(2) Å,β = 109.23(3)°, Z = 4, and space group P 2₁/n. The structure was solved according to the heavy-atom method and refined by full-matrix least-squares procedures to R = 0.037 for 2098 reflections with I ≥ 2.5σ(I).     

Characterization and Molecular Structure of Bis(Isopropyl Xanthate) Bis(1,10-Phenanthroline) Nickel(II): [Ni(phen)2(CH3)2CHOCSS](CH3)2CHOCSS

The crystal and molecular structure of the title compound, [Ni(phen)₂(CH₃)₂CHOCSS](CH₃)₂CHOCSS has been determined by X-ray diffraction. The brown crystal is triclinic of space group Pi, with parameters a = 11.790(2), b = 12.410(3), c = 12.680(3) Å, α = 92.49(3), β = 96.54(3), γ = 117.43(3)° and Z = 2. The compound contains a six-coordinate cation and an isopropyl xanthate anion (CH₃)₂CHOCSS^?, the central Ni atom is chelated by four nitrogen atoms of two phenanthroline ligands and two sulfur atoms of an isopropyl xanthate ligand. The TG data indicate that it decomposed completely at 734°C.     

Darstellung und Kristallstruktur von Tris(äthylendiamin)kobalt(III)-trichlorostannat(II)-dichlorid, [Co(en)3][SnCl3]Cl2

Preparation and Crystal Structure of Tris(ethylenediamine) cobalt(III)-trichlorostannate(II)-dichloride, [Co(en)₃] [SnCl₃]Cl₂ The title compound has been prepared from [Co(en)₃]Cl₃ and SnCl₂ · 2H₂O in aqueous HCl solution. It crystallizes in the orthorhombic space group Pbca, with a = 21.906(7), b = 10.607(3), c = 15.356(7) Å. The crystal structure has been determined from 1606 independent reflections by Patterson snd Fourier syntheses, and has been refined by least squares methods to R = 0.074. The [Co(en)₃]³⁺ ion is found to have the conformation of Λ(δδλ) resp. Δ(λλδ). The structure of the [SnCl₃]^? ion corresponds to a distorted tetrahedron, in which one site is occupied by the stereochemically active 5s electron pair. The following Sn? Cl distances have been found 2.493(7), 2.492(5), 2.479(7) Å, the distances of the two anionic Cl atoms from Sn are >4 Å.     

Deprotonierte Dithiocarbaminsäureester als Thiolat-S-Donor-Liganden. Strukturen von Ph(H)NC(S)SMe,Co(PhNC(S)SMe)3 und Cu6(PhNC(S)SMe)6

Deprotonated Dithiocarbamic Acid Esters as Thiolate S-Donor Ligands. Structures of Ph(H)NC(S)SMe, Co(PhNC(S)SMe)₃, and Cu₆(PhNC(S)SMe)₆ The reaction of N-phenyl-S-methyldithiocarbamate, PhN(H)C(?S)SMe, ( 1 ) with cobalt(II) and copper(II) salts yields the monomeric compound Co^III(PhNC(S)SMe)₃ ( 2 ) and the hexameric compound Cu₆^I(PhNC(S)SMe)₆ ( 3 ). These complexes contain the negatively charged imino-thiolate ligand PhN?C(? S)SMe, which has been formed by deprotonation of 1 . The crystal structures of 1 – 3 have been determined. 1 forms centrosymmetrical dimers through N? H …? S bridge bonds, the conformation in the solid state and in solution is Z,E′. Co^III shows in 2 a trigonal-antiprismatic coordination, with the ligands acting as N,S-chelates. 3 contains an octahedral Cu₆-core with Cu …? Cu-distances ranging from 276.3(5) to 305.7(4) pm. Each copper center is trigonally coordinated to one nitrogen and two sulfur atoms of three different ligands. Crystal data: 1 , triclinic, space group P1 , a = 590.5(6), b = 869.0(1), c = 968.5(9) pm, α = 67.29(8), β = 78.44(8), γ = 81.64(9)°, Z = 2, 1 775 reflections, R(R_w) = 0.0317(0.032). 2 , orthorhombic, space group Pbca, a = 978.0(2), b = 1 842.9(4), c = 3 059.7(6) pm, Z = 8, 1 129 reflections, R(R_w) = 0.0997(0.0886). 3 , monoclinic, space group P2₁/c, a = 1 363.1(3), b = 1 342.8(3), c = 1 671.9(3) pm, β = 103.48°, Z = 2, 1 374 reflections, R(R_w) = 0.0708(0.0617).     

Synthese und Struktur von Bis(3-diethylamino-5-phenyl-1,2,4-dithiazolium)-tetrachlorocobaltat(II)

Synthesis and Structure of Bis(3-diethylamino-5-phenyl-1,2,4-dithiazolium)-tetrachlorocobaltat(II) The title compound 1 was prepared by reaction of Tris(1,1-diethyl-3-benzoyl-thioureato)cobalt(III) with SOCl₂ in acetonitrile. 1 has been characterized by IR-spectroscopy and VIS-spectroscopy. The structure of 1 has been determined by an X-ray structure analysis. The compound crystallizes in the monoclin space group C2/c with a = 16.224; b = 11.257; c = 17.697 Å; β = 107,43° and Z = 4. The final R value was R = 0.027 for 2073 observed reflections. The cation of 1 is nearly plane with an extended delocalization of electrons. The CoCl₄^2? anion is tetrahedral with two different long Co? Cl pairs. Interionic contacts S …? Cl exists between the structural units of the cations and the anion.     

Investigations on crystal structure of a novel 3-((4,6-dimethylpyrimidin-2-yl)amino)isobenzofuran-1(3H)-one,and related theoretical studies

In this report, 3-((4,6-dimethylpyrimidin-2-yl)amino)isobenzofuran-1(3H)-one have been synthesized via reaction between phthalaldehydic acid and 2-amino-4,6-dimethylpyrimidine in 90% yields and characterized by Infrared (IR), Nuclear Magnetic Resonance (NMR), Ultraviolet–visible (UV–Vis), X-ray single crystal diffraction techniques. The single-crystal X-ray analysis shows that the title compound crystallizes in the triclinic space group P-1 with unit-cell parameters a = 7.9351(4) Å, b = 11.1687(6) Å, c = 16.1281(9) Å, α = 73.713(5)°, β = 80.362(5)°, γ = 72.882(4)° and Z = 4. A theoretical study with hybrid functional B3LYP 6-311G (d, p) basis set have been used in calculations. The structural and electronic properties have been detailed. The title compound was screened for its antioxidant activity by (1,1-diphenyl-2-picryl hydrazyl) free radical scavenging (DPPH), Ferric ion reducing antioxidant power (FRAP), total phenolic contents (TP) assays and its ferrous ions chelating property. Electronic absorption titration, thermal denaturation measurement and viscosity techniques were used to determine the interaction between double stranded DNA (dsDNA) and compound 1. In three techniques, the mode of binding of compound 1 to dsDNA is minor groove. The UV–Vis measurement results allowed the calculation of the binding constant showing the binding strength of compound 1 to dsDNA was calculated as 8.13 × 10⁴ ± 0.07 L mol⁻¹. Moreover, the molecular docking calculations have been performed to investigate the compound–DNA interactions, computationally. In molecular docking calculations, it was observed that for the title compound, the lowest energy docking pose takes place in the minor groove of DNA and in addition to minor groove binding, interactions between the compound and the consecutive base pairs of DNA which may cause a partial intercalation were also observed. Results showed that title compound – DNA complex is stabilized by several hydrogen bonds, and Pi-alkyl interactions also take part in the stabilization of the complex. Binding affinities of the lowest energy docking pose of the title compound was found to be −8.3 kcal/mol.     

Palladium(II) Complexes with the Mixed‐Donor Ligand CH3S‐(CH2)3‐PPh2 Crystal Structures of [PdCl2{CH3S‐(CH2)3‐PPh2}n](n = 1, 2)

The phosphorus‐sulfur ligand 1‐(methylthio)‐3‐(diphenylphosphino)‐propane (S‐P3) has been synthesized and characterized by ¹H NMR and ¹³C NMR. Reactions of S‐P3 with [PdCl₂(PhCN)₂] afforded the complexes [PdCl₂(S‐P3)] ( I ) and [PdCl₂(S‐P3)₂] ( II ), in which S‐P3 acts as a bidentate and monodentate ligand, respectively. Compound I crystallizes in monoclinic space group P2₁/n (No. 14) with cell dimensions: a = 8.589(3), b = 15.051(3), c = 17.100(3)Å, β = 102.91(2)°, V = 2154.7(9)ų, Z = 4. Likewise, compound II crystallizes in monoclinic space group P2₁/n (No. 14) with a = 9.993(5), b = 8.613(4), c = 18.721(5)Å, β = 90.18(3)°, V = 1611.3(12)ų, Z = 2. Compound II has a trans square planar configuration with only the P‐site of the ligand bonded to the palladium atom.     

The crystal structure of K2[Cu3ZnF(PO4)3], a new mixed zinc copper phosphate

The title compound has been prepared by hydrothermal synthesis and its crystal structure was determined by single crystal X-ray diffraction: space group P2₁/m, a = 4.8890(2), b = 14.3857(5), c = 7.9017(3) Å, β = 90.134(4)°, wR₂ = 0.123, R = 0.045. Cu²⁺ has two different coordination polyhedra: an elongated square pyramidal [CuFO₄] and square planar [CuO₄] coordination in a 2:1 ratio. Edge-sharing double-pyramids and [CuO₄] squares form zig-zag chains interconnected by [ZnO₄] and [PO₄] tetrahedra to form an open anionic framework structure whose channels are occupied by the K⁺ ions.     

[VCl3(NPPh3)(OPPh3)], ein Phosphaniminato-Komplex von Vanadium(IV)

[VCl₃(NPPh₃)(OPPh₃)], a Phosphorane Iminato Complex of Vanadium(IV) The title compound has been prepared from vanadium tetrachloride and Me₃SiNPPh₃ in the presence of OPPh₃ in CCl₄ solution, forming orange-red, moisture sensitive crystals, which were characterized by an X-ray structure determination. Space group Cc, Z = 4, 2 560 observed unique reflections, R = 0.049. Lattice dimensions at 0°C: a = 1 018(1), b = 1 826(2), c = 1 859(2) pm, β = 93.65(9)° [VCl₃(NPPh₃)(OPPh₃)] forms monomeric molecules, in which the vanadium atom is coordinated in a distorted square pyramidal fashion with the (NPPh₃)^? ligand in apical position. The three chlorine atoms and the oxygen atom of the OPPh₃ molecule occupy the basal positions. The phosphorane iminato group V?N?PPh₃ is nearly linear (bond angle VNP 161.4°), the bond lengths VN (169 pm) and PN (162 pm) correspond with double bonds.     

Synthesis and Characterization of (βDiketonate)(7-norbornadienyl acetate)Copper(l) Complexes,Single-Crystal Structure of (hfac)Cu(7-AcO-NBD)

Copper(I) complexes of general formula (β-diketonate)Cu(7-AcO-NBD), where 7-AcO-NBD = 7-norbornadienyl acetate and β-diketonate = 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate (1), 1,1,1-trifluoro-2,4-pentanedionate (2), 2,4-pentanedionate (3), 4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedionate (4), 4,4,4-trifluoro-1-phenyl-1,3-butanedionate (5), were prepared from reactions of CuCl with Na(β-diketonate) in the presence of 7-AcO-NBD. AH compounds were characterized by elemental analyses, ¹H, ¹³C, ¹⁹F NMR and IR spectra. Single-crystal strucutre of compound 1 was determined by X-ray diffraction analysis that showed a mononuclear copper species with coordination of a chelating β-diketonate ligand through two oxygen atoms and the 7-AcO-NBD through its C? C double bond and an oxygen atom in the solid state. For compound 1, the crystal data are: triclinic, space group $ {\rm P}\bar 1 $, a= 5.4519(14) Å, b= 11.852(3) Å, c= 13.304(3) Å, α = 74.721(20)° β = 80.220(20)°, γ= 76.848(19)°, Z = 2, R_F = 0.060 and R_w = 0.064. Hot-wall chemical vapor deposition experiments revealed that compound 1 is suitable as a precursor for deposition of copper films in the temperature range 170–260 °C.     

Saure Sulfate des Neodyms: Synthese und Kristallstruktur von (H5O2)(H3O)2Nd(SO4)3 und (H3O)2Nd(HSO4)3SO4

Acidic Sulfates of Neodymium: Synthesis and Crystal Structure of (H₅O₂)(H₃O)₂Nd(SO₄)₃ and (H₃O)₂Nd(HSO₄)₃SO₄ Light violett single crystals of (H₅O₂)(H₃O)₂ · Nd(SO₄)₃ are obtained by cooling of a solution prepared by dissolving neodymium oxalate in sulfuric acid (80%). According to X‐ray single crystal investigations there are H₃O⁺ ions and H₅O₂⁺ ions present in the monoclinic structure (P2₁/n, Z = 4, a = 1159.9(4), b = 710.9(3), c = 1594.7(6) pm, β = 96.75(4)°, R_all = 0.0260). Nd³⁺ is nine‐coordinate by oxygen atoms. The same coordination number is found for Nd³⁺ in the crystal structure of (H₃O)₂Nd(HSO₄)₃SO₄ (triclinic, P1, Z = 2, a = 910.0(1), b = 940.3(1), c = 952.6(1) pm, α = 100.14(1)°, β = 112.35(1)°, γ = 105.01(1)°, R_all = 0.0283). The compound has been prepared by the reaction of Nd₂O₃ with chlorosulfonic acid in the presence of air. In the crystal structure both sulfate and hydrogensulfate groups occur. In both compounds pronounced hydrogen bonding is observed.     

Polysilane derivatives of the transition metals II. The crystal and molecular structure of [tris(trimethylsilyl)silyl]pentacarbonylmanganese, (Me3Si)3SiMn(CO)5

The crystal and molecular structures of [tris(trimethylsilyl)silyl]pentacarbonylmanganese, (Me₃Si)₃SiMn(CO)₅, have been determined from three-dimensional X-ray data obtained by counter methods. The compound crystallizes in space group P$\text{1}$ of the triclinic system, with two molecules in a unit cell of dimensions: a = 9.002(2), b = 9.655(2), c = 15.639(3) Å, α = 83.66(1), β = 105.65(1), γ = 114.61(1)°.The observed and calculated densities are 1.20 (±0.03) and 1.23 g-cm^?3 respectively. Full-matrix least-squares refinement of the structure has led to a final value of the conventional R factor of 0.059 for the 818 independent reflections having F² > 3σ(F²).The coordination geometry about the manganese atom is approximately octahedral and, about the silicon atom bonded to the manganese atom, tetrahedral.The relative orientations of carbonyl and trimethylsilyl groups, when viewed down the MnSi bond, appear consistent with minimization of energy due to nonbonded interactions.Two of the equatorial carbonyl groups are displaced out of the equatorial plane towards the silicon ligand by 6°. The SiMn bond is 2.564(6) Å long and has no multiple character.     

Synthesis and structure of complex compound Rh(III) of (NH4)2[Rh(NO2)3(NH3)(µ-OH)]2 composition

The crystalline structure of a new compound Rh(III) of (NH₄)₂[Rh(NO₂)₃(NH₃)(μ-OH)]₂ composition has been determined. The crystallographic characteristics are H₁₆N₁₀O₁₄Rh₂: a = 6.3963(2) Å, b = 9.3701(4) Å, c = 13.6646(5) Å, β = 102.266(1)°, V = 800.28(5) ų, Z = 2, d _calc = 2.432 g/cm³. The distance Rh...Rh in the dimer is 3.200 Å. Original Russian Text Copyright ? 2006 by S. P. Khranenko, I. A. Baidina, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 2, pp. 380–384, March–April, 2006.     

SYNTHESIS AND STRUCTURE OF A NOVEL MONONUCLEAR TUNGSTEN (VI) CITRATO COMPLEX, (NH4)3[Li(H2O)3WO3(C6 H4O7)]

Abstract

The first mononuclear tungsten-citrato complex, (NH₄)₃[Li (H₂O)₃WO₃(C₆H₄O₇)] (1), has been prepared by the reaction of ammonium tetrathio tungstate and lithium citrate in CH₃OH-H₂O solution at pH 8.2. There are two crystallographically independent anions in the asymmetric crystallographic unit. The crystal structure of the title compound (triclinic, space group P1, a = 6.901(1), b = 15.136(3), c = 16.107(3) Å, α = 75.85(3), β = 89.89(3), γ = 89.97(3), V = 1631.4(6) ų, R = 0.068, R _W = 0.1674 for 3878 reflections with I > 2σ(I)), reveals that in the compound a tungsten atom is coordinated to a fully deprotonated citrate as a tridentate ligand and three terminal oxygen atoms to form a distorted coordination octahedron.     

Darstellung und Kristallstrukturen der ersten Alkalimetall‐hexacarbonatooxotetraberyllate: K6[Be4O(CO3)6] · 7 H2O und K6[Be4O(CO3)6]

Preparation and Crystal Structures of the first Alkalimetall‐hexacarbonato‐oxotetraberyllates: K₆[Be₄O(CO₃)₆] · 7 H₂O and K₆[Be₄O(CO₃)₆] K₆[Be₄O(CO₃)₆] · 7 H₂O has been prepared by dissolving freshly precipitated Be(OH)₂ in an aqueous KHCO₃ solution. After enriching the title compound by extraction with ethanol the heptahydrate crystallizes from the organic phase (triklin, P1¯ (No. 2) with a = 951, 01(11), b = 958, 45(12), c = 1601, 7(2) pm, α = 79, 253(13)°, β = 78, 943(12)°, γ = 65, 119(12)°, V_EZ = 1290, 6(3)·10⁶ pm³, Z = 2). Thermal decomposition forms rhombohedral crystals of the anhydrous compound (trigonal‐rhombohedric, R3¯ (No. 148) with a = 1416, 42(6), c = 1704, 5(1) pm, V_EZ = 2961, 4(3)·10⁶ pm³, Z = 6).     

Isolation,Purification, and Characterization of Antimicrobial Compound 6-[1,2-dimethyl-6-(2-methyl-allyloxy)-hexyl]-3-(2-methoxy-phenyl)-chromen-4-one from Penicillium sp. HT-28

A fungal culture (Penicillium sp., HT-28), isolated from soil has been evaluated for its bioactivity, which showed broad spectrum antimicrobial activity and was effective against methicillin-resistant Staphylococcus aureus (MRSA) also. Statistical optimization of the medium by response surface methodology (RSM) enhanced the antimicrobial activity up to 1.8-fold. Column chromatography was used to isolate the active compound (A), which was characterized to be 6-[1,2-dimethyl-6-(2-methyl-allyloxy)-hexyl]-3-(2-methoxy-phenyl)-chromen-4-one by various spectroscopic techniques such as infrared (IR), ¹H and ¹³C nuclear magnetic resonance (NMR) spectra, and mass spectroscopy. Minimum inhibitory concentration (MIC) of the active compound (A) ranged from 0.5 to 15 μg/mL. Viable cell count studies of the active compound (A) showed S. aureus, Escherichia coli, Staphylococcus epidermidis, and Salmonella typhimurium 1 to be the most sensitive. The compound retained its bioactivity after treating it at 100 °C for 1 h. Furthermore, the compound (A) when tested for its biosafety was found neither to be cytotoxic nor mutagenic. The study demonstrated that an apparently novel compound isolated from Penicillium sp. (HT-28) seems to be a stable and potent antimicrobial.     

[Yb3OBr4{N(SiMe3)2}3 (THF)3], ein Amido-Komplex des Ytterbiums mit clusterähnlichem Aufbau

[Yb₃OBr₄{N(SiMe₃)₂}₃(THF)₃], an Amido Complex of Ytterbium with a Clusterlike Structure The title compound has been prepared from YbBr₃ and NaN(SiMe₃)₂ in THF suspension, forming yellow single crystals from hexane solutions which were characterized by a crystal structure determination. Space group P1 , Z = 2, lattice dimensions at ?100°C: a = 1085.4(1), b = 1410.2(1), c = 1912.0(1) pm; α = 78.62(1)°, β = 80.61(1)°, γ = 73.45(1)°, R = 0.025. In the molecular structure of [Yb₃OBr₄{N(SiMe₃)₂}₃(THF)₃] the three ytterbium atoms together with the μ₃-oxygen atom and a μ₃-bromine atom form a distorted trigonal bipyramid. In addition, three μ₂-Br atoms coordinate the Yb atoms in the equatorial plane, whereas the THF molecules and the N(SiMe₃)₂^? ligands are terminally coordinated, thus forming a distorted octahedrally surrounding of the Yb atoms.     

Two polymorphic modifications of 1-(N-morpholiniomethyl)spirobi- (3-oxo-2,5-dioxa-1-silacyclopentan)- ate hydrate

The compound 1-(N-morpholiniomethyl)spirobi(3-oxo-2,5-dioxa-1-silacyclopentan)ate crystallizes from aqueous solution of γ-butyrolactone in the form of two crystal hydrate modifications: monoclinic (with D = 1.53 g/cm³, space group P 2₁/n) and triclinic (D = 1.45 g/cm³, space group P1^-). For the monoclinic form, an X-ray structural study at -100°C has been performed. For both structures the coordination polyhedron of the silicon atom is a trigonal bipyramid. In the crystal structures there are strong intermolecular hydrogen bonds of NH···O and OH···O types.     

Kristall- und MolekülStruktur von 2(C6H5)3AsO · H2SeO3

Crystal and Molecular Structure of 2(C₆H₅)₃AsO · H₂SeO₃ 2(C₆H₅)₃AsO · H₂SeO₃ crystallizes in the orthorhombic space group Fdd2—C_2v¹⁹, with a = 20.472(9), b = 32.747(1) and c = 10.008(8) Å and Z = 8; d (calc./obs.) = 1.52₇/1.52 g · cm^?3. The structure has been determined from 808 independent reflections by Patterson- and Fouriersyntheses, and has been refined by least squares methods to R = 0.056. In the compound two (C₆H₅)₃AsO-units and one selenite group are linked by short H-bonds [O …? H …? O-distance 2.48(4) resp. 2.35(4) Å]. The As? O-distances are 1.64(9), the Se? O-distances are 1.69(3), 1.83(3), resp. 1.76(3) Å.     

Die Kristallstruktur von Kalium-trithiowolframat-chlorid K3(WOS3)Cl

A recently prepared new thiotungstate has been characterized by three-dimensional X-ray structure analysis, to be a double salt, containing K₂WOS₃ and KCl in equimolar proportions: potassium trithiotungstate chloride, K₃(WOS₃)Cl. Space group: Pca2₁ with a = 12.507, b = 6.317, c = 12,371 Å, Z = 4. The compound represents a new structure type with stoichiometry M^I₂XY₄ · M^IZ. Besides isolated tetrahedral WOS₃^2- ions (bond lengths W–O 1.760 Å, W–S 2.208, 2.197, 2.196 Å) the structure contains Cl^? ions octahedrally co-ordinated by K⁺, the K⁺ ions having 5S + 10 + 2Cl as neighbours. The dimensions of the WOS₃^2? ions in this compound show that, as in other transition metal oxo-, thio- and selenoanions, strong π bonding is present, the W–S bonds taking part in the π bond system.