Powder study of propanthioamide dervative C8H6N2S2

The crystal structure of 2‐cyano‐3‐(2‐thienyl)prop‐2‐enethioamide (C₈H₆N₂S₂), a propanethioamide derivative was solved from high resolution laboratory X‐ray powder diffraction data collected at ambient conditions. Structure determination was performed by means of the global optimization method of simulated annealing at a resolution of 1.5 Å. Rietveld refinement yielded an R_WP value of 4.02% (P2₁/a, a = 15.8174(2) Å, b = 5.6502(1) Å, c = 11.0952(1) Å, β = 116.9923(7)°, V = 883.6(5) ų, Z = 4). The molecules are stacked in parallel layers and are stabilized by hydrogen bonds. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of the quaternary alloy CuTaInSe3

The crystal structure of the quaternary compound CuTaInSe₃ belonging to the system (CuInSe₂)_1‐x(TaSe)_x with x= 0.5, was analyzed using X‐ray powder diffraction data. This material is isostructural with the CuFeInSe₃ compound, and crystallize in the tetragonal space group P42c (Nº 112), Z = 1, with unit cell parameters a = 5.7831(1) Å, c = 11.6227(4) Å, V = 388.71(2) ų. The Rietveld refinement of 18 instrumental and structural variables led to R_p = 8.0%, R_wp = 9.5%, R_exp = 6.3% and χ² = 1.5 for 4501 step intensities and 144 independent reflections. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X‐ray powder diffraction study of the semiconducting alloy Cu2Cd0.5Mn0.5GeSe4

The structure of the semiconducting alloy Cu₂Cd_0.5Mn_0.5GeSe₄ was refined from an X‐ray powder diffraction pattern using the Rietveld method. The present alloy crystallizes in the wurtz‐stannite structure, space group Pmn2₁ (N^o 31), and unit cell parameters values of a = 8.0253(2) Å, b = 6.8591(2) Å, c = 6.5734(2) Å and V = 361.84(2) ų. The structure exhibits a three‐dimensional arrangement of slightly distorted CuSe₄, Cd(Mn)Se₄ and GeSe₄ tetrahedras connected by corners. © 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Synthesis,Structure and Characterizations of a Molybdenum Sulfide Complex with inorganic Cluster [Mo3S13]2‐ and Organic Amine Me4N+

The complex of (Me₄N)₂Mo₃S₁₃ ( I ) has been synthesized under mild hydrothermal condition. The crystal structure was determined by single crystal X‐ray diffraction at room temperature. Crystal data: M = 854.91, Trigonal, space group P3 (No. 143), a = 11.2351(8) Å, c = 5.8885(6) Å, and Z = 1, There is an inorganic [Mo₃S₁₃]^2‐ core composed of a Mo₃‐triangle, a μ₃‐S atom, three doubly bridging disulfide and three terminal disulfide. Two organic amine ions act as the positive charge to balance the [Mo₃S₁₃]^2‐ cluster.     

Synthesis,crystal structure and photophysical studies on a ruthenium(II) carbonyl hydrido compound based on 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid (H2bpdc)

A novel complex, namely [Ru^II(PPh₃)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H₂bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H₂bpdc with [Ru^II(PPh₃)₃(CO)(H)₂] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) ų, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature.     

Hydrothermal synthesis and structure of a 2D supramolecular framework with right‐ and left‐helices based on mixed ligands

An exploration of the cobalt‐OH‐BDC‐bpp system under hydrothermal conditions, has led to the isolation of a novel framework [Co(OH‐BDC)(bpp)_0.5(H₂O)]_n (OH‐BDC = 5‐hydroxyisophthalic acid, bpp = 1,3‐bi(4‐pyridyl)propane). Single‐crystal X‐ray analysis reveals that it crystallizes in the monoclinic space group P2₁/n. a = 10.235(8) Å, b =17.882(14) Å, c = 14.291(11) Å, β = 92.107(9)°.The cobalt ions are linked into an extended helical chain via OH‐BDC and mono‐coordinated bpp ligands through hydrogen‐bonding interactions. Further these helical chains are united together through the bridging bpp to form a 2D layer and the adjacent chains possess the opposite chirality. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a 3‐D supramolecular Cu/Mn complex with pydc

A supramolecular compound, {[CuMn(pydc)₂(H₂O)₅]·2H₂O} ( 1 ) (pydc = pyridine‐2,6‐dicarboxylate dianion), has been synthesized and characterized by single‐crystal X‐ray diffraction. Single‐crystal X‐ray analysis reveals that it crystallizes in the triclinic space group P‐1, a = 8.4763(17) Å, b = 9.7715(19) Å, c = 13.909(3) Å, α =101.234(3)°, β =102.520(3)°, γ= 97.375(4)°. Two mixed‐metal ions exhibit similar coordinated geometries with octahedron. 1 possesses a 3‐D unusual supramolecular network featuring 1D water tape. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of a new one‐dimensional cobalt complex with dicyanamide and 4‐picolyl choride bridges

The synthesis and structure of the 1D cobalt (II) complex, [Co( L )₂(dca)₂] ( 1 ) (dca = dicyanamide, C₂N₃^–, L = 4‐picolyl choride) is reported. Complex 1 crystallized in triclinic system, space group P ‐1, with cell dimensions of a = 7.291(2) Å, b = 7.481(2) Å, c = 9.007(3) Å, α =104.444(4)°, β = 96.971(4)°, γ =102.618(4)°, V = 456.1(2) ų, Z = 1, Dc = 1.624 Mg/m³. In complex 1 , Co (II) is 6‐coordinated by N atoms of four dca ligands and two L ligands. The centrosymmetric CoN6 chromophore is an axially elongated octahedron that has Co‐N distances ranging from 2.122(3) to 2.154(3) Å. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,structure and photoluminescence of a 3D pillared heterometallic coordination polymer containing 2D inorganic cadmium‐potassium‐oxide layer subunits

Self‐assembly of Cd(NO₃)₂ with o ‐phthalic acid monopotassium salt (KHphth) in the presence of ethylenediamine (en) produced a new heterometallic coordination polymer [CdK₂(phth)₂(en)_0.5(H₂O)]_n ( 1 ). Single‐crystal X‐ray analyses reveal that it crystallizes in a monoclinic space group P 2₁/c. a = 11.6707(6) Å, b = 8.1019(4) Å, c = 20.9503(11) Å, β = 94.6640(10)^o. The complex displays an en‐pillared 3D framework, which is constructed from 2D [CdK₂(phth)₂(H₂O)]_n layers featuring uncommon inorganic cadmium‐potassium‐oxide layers containing potassium‐oxide layers. In the solid state, complex 1 shows photoluminescence with the maximum emission intensities at 355 nm upon excitation at 312 nm. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and crystal structure of a 2D Cd(II) complex with a 4,4'‐diazenediyldiphthalic acid ligand

An exploration of the cadmium‐L system under hydrothermal condition, has led to the isolation of a novel framework {[Cd(L)_0.5(H₂O)₃]}_n ( 1 ) (H₄L = 4,4'‐diazenediyldiphthalic acid). Single‐crystal X‐ray analysis reveals that it crystallizes in the triclinic space group P‐1. a = 5.746(3) Å, b =6.526(4) Å, c = 14.701(8) Å, α=92.348(8), β = 99.622(6), γ=106.877(7)°. The Cd^II ions are linked into an extended 2‐D rectangle‐like structure via L ligands, which exhibits an attractive three‐connected honeycomb topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

X‐ray diffraction refinement of the crystal structure of anosovite prepared from leucoxene

The crystal structure of anosovite, (Ti_1.69Al_0.26Fe_0.05)³⁺(Ti_0.97Zr_0.03)⁴⁺O₅, prepared by carbothermal reduction of leucoxene under vacuum at 1450°C has been refined by Rietveld method using powder X‐ray diffraction data. It was found that it represents slightly monoclinically deformed pseudobrookite type structure with lattice parameters a = 9.8111 Å, b = 3.7509 Å, c = 9.9468 Å, β = 90.628°. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural study of the semimagnetic semiconductor Zn0.5Mn0.5In2Te4

The semimagnetic semiconductor alloy Zn_0.5Mn_0.5In₂Te₄ was refined from an X‐ray powder diffraction pattern using the Rietveld method. This compound crystallizes in the space group I42m (Nº 121), Z = 2, with unit cell parameters a = 6.1738(1) Å, c = 12.3572(4) Å, V = 471.00(2) Å3, c / a = 2.00. This material crystallizes in a stannite‐type structure. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and crystallographic characterization of crystalline modifications of 3,4:9,10‐perylenetetracarboxylic dianhydride at room temperature

3,4:9,10‐Perylenetetracarboxylic dianhydride (PTCDA) powder obtained from Sigma‐Aldrich was purified by three cycles of temperature gradient sublimation in an evacuated quartz glass tube providing variable conditions. By means of X‐ray diffraction (XRD) analysis, a crystallographic characterization of the powders obtained during the sublimation process and selected single crystals was carried out evidencing the presence of a major α‐ and a minor β‐PTCDA component in all samples. Lattice parameters of high precision were obtained for α‐PTCDA (a = 3.73283(4) Å, b = 12.0328(6) Å, c = 17.3998(4) Å, β = 98.689(2)°, V = 772.57(4) ų and d₁₀₂ = 3.219(3) Å) by whole‐X‐ray‐powder‐pattern‐fitting of the experimental XRD pattern using the Le Bail approach. Employing a (001) KCl wafer as substrate for the material purification results in formation of single phase α‐PTCDA accompanied by a decrease in the size of the crystallites which is attributed to the presumed lower temperature of the KCl wafers. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Interaction in the molten system Rb2O‐P2O5‐TiO2‐NiO. Crystal structure of the langbeinite‐related Rb2Ni0.5Ti1.5(PO4)3

The interaction in the molten system Rb₂O‐P₂O₅‐TiO₂‐NiO was investigated at different molar ratios Rb/P = 0.5‐1.3, fixed Ti/P = 0.15, Ti/Ni = 1.0 at temperature range 1073–953 K. The conditions of formation of complex phosphates RbTi₂(PO₄)₃, Rb₂Ni_0.5Ti_1.5(PO₄)₃ and RbNiPO₄ have been determined. The new phosphate Rb₂Ni_0.5Ti_1.5(PO₄)₃ (space group P2₁3, a = 9.9386(2) Å) has been obtained and investigated by the single crystal X‐ray diffraction and FTIR‐spectroscopy. It has langbeinite‐like structure, that is built up from mixed (Ni/Ti)O₆‐octahedra and РО₄‐tetrahedra. Rubidium atoms are located in closed cavities of 3D‐framework.     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,characterization and magnetic behaviour of a linear chain poly(oxomolybdophosphate) compound

A new linear chain compound, [Cu(en)₂][Cu(en)₂(H₂O)_1.5][Cu(en)₂(H₂O)₂]_0.5[{Cu(en)₂}₅{HP₂Mo₅O₂₃}₃] · 6.5H₂O ( 1 ) (en = ethylenediamine), has been synthesized under mild hydrothermal conditions, and characterized by elemental analysis, IR, thermogravimetric analyses, magnetic susceptibility measurements and single‐crystal X‐ray diffraction. The crystals are monoclinic, C2/c, a = 42.509(2) Å, b = 25.542(2) Å, c =22.1011(14) Å, β = 102.5940(10)º, V = 23419(3) ų, Z = 8. The crystal structure of 1 features Cu‐bearing cations that are both free as well as being coordinated to the poly(oxomolybdophosphate) groups formed a linear chain that runs along the b axis. Magnetic studies show that the complex is antiferromagnetic. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione

The crystal structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione (C₂₂H₂₀N₂OS) has been determined from three dimensional single crystal X‐ray diffraction data. The title compound crystallizes in the monoclinic space group P 2₁/c, with a = 10.6674(13), b = 10.1077(7), c = 17.9467(19) Å, β = 98.460(9)°, V = 1914.0(3) ų, D_calc = 1.251 g cm^–3, Z = 4. In the title compound, the allyl group shows positional disorder. Molecules are linked by C‐H···O, C‐H···N and C‐H···S intermolecular interactions forming two‐dimensional network. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Solvothermal syntheses and crystal structures of two 4‐heterocyclic acylpyrazolone complexes

Many explorations of transition metal (M)‐L system under solvothermal condition, have led to the syntheses of two new 4‐heterocyclic acylpyrazolone complexes [Co(L)₂(CH₃OH)₂] (HL = 1‐phenyl‐3‐methyl‐4‐(2‐furoyl)‐5‐pyrazolone) ( 1 ) and [Cr(L)₃] ( 2 ). Single‐crystal X‐ray analyses reveal that crystal structures of compound 1 and 2 are respectively orthorhombic, Pbca, a = 15.0378(6) Å, b = 9.8405(4) Å, c = 20.7321(8) Å, V = 3067.9(2) ų, Z = 8 and triclinic, P‐1, a = 10.7966(18) Å, b = 13.023(2) Å, c = 15.520(3) Å, α = 73.011(4)°, β = 84.884(4)°, γ = 70.267(4)°, V = 1964.3(6) ų, Z = 2. Complex 1 has a two‐dimensional (2D) network structure that is formed by O–H···N H‐bonding interactions. Complex 2 makes a one‐dimensional (1D) zigzag chain structure by intermolecular π···π interactions, which is further interlinked via C–H···N H‐bonding interactions to generate a 2D sheet, and then a three‐dimensional (3D) supramolecular network structure is further linked by intermolecular C–H···π interactions. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of the three‐dimensional coordination polymer [Ag3hmt3(μ3 ‐btc)]·5H2O

A new coordination polymer, [Ag₃hmt₃(μ₃ ‐btc)]·5H₂O (1) (hmt = hexamethylenetetramine, btc=1,3,5‐benzenetricarboxlic), has been successfully synthesized. Crystal data: P2₁/a, a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, β = 101.9820(14)°, V = 3455.40(7) ų, Z = 4, Dc = 2.002 Mg/m³. In the hexagonal structure of Ag‐hmt unit, each Ag‐hmt unit comprises three Ag atoms and three hmt ligands. The μ₃ ‐btc ligands bridge adjacent two‐dimensional honeycomb‐like Ag‐hmt layers to form three‐dimensional networks. Structure analysis show that hydrogen bonds play a key role for the stable structure in the compounds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)