Crystal Structure Analysis of {[μ‐N,N′‐Bis(salicylidene)‐2,2′‐dimethyl‐1,3‐propanediaminato](dimethylformamide) zinc(II)}diiodomercury(II)

The title compound, a hetero‐dinuclear complex with Zn^II and Hg^II ions, forms crystals which belong to the monoclinic system, space group P2₁/n, with unit cell dimensions a = 11.2217(12), b = 17.7493(11), c = 13.9293(13) Å, β = 94.830(3)°, V = 2764.5(4) ų. The cell contains four molecules. The Zn…Hg distance is 3.5362(15) Å.     

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)     

Microstructures of Mg–Zn–Nd alloy including small quasicrystalline grains

Two kinds of Mg-rich and low neodymium Mg–Zn–Nd alloys including icosahedral quasicrystal phase (I-phase) were prepared under conventional casting conditions. The microstructures and phases of Mg–Zn–Nd quasicrystal alloys were investigated by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and transmission electron microscopy (TEM). The results indicate that the I-phase in Mg–Zn–Nd quasicrystal alloy is a simple icosahedral quasicrystal with quasi-lattice of a_R = 0.525 nm. It has been proved that the as-cast Mg_70.8Zn₂₈Nd_1.2 quasicrystal alloy mainly consisted of I-phase and Mg₇Zn₃ matrix phase. While the as-cast Mg_70.5Zn_28.5Nd₁ alloy mainly consisted of I-phase, Mg₇Zn₃ matrix phase, dendrite α-Mg phase and a new rod-like hexagonal phase.     

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)     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 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)     

The crystal and molecular structure of bis(tetramethylammonium) hexamolybdate(VI)

The crystal structure of the title compound, C₈H₂₄N₂Mo₆O₁₉ was determined by single crystal X‐ray diffraction technique. The crystals are trigonals, space group P‐3c1, with a = b = 10.0176(11) Å, c = 14.089(2) Å, γ = 120°, V = 1224.4(3) Å₃, Z = 2. The structure was solved by direct methods and refined by least‐squares methods to a Final R = 0.0316 for 1114 observed reflections with I > 2σ(I). In hexamolybdate anion, six MoO₆ distorted octahedra are fused together so that they all share a common vertex. O atoms are of three types: central, terminal and bridging, bonded to six, one and two Mo atoms, respectively. The crystallographic data of the structure was deposited with the Cambridge Data Center as No. CCDC 199679. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal and molecular structure of trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II)

Trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II), [Ni(sac)₂(pypr)₂], where sac and pypr are the saccharinate anion and the 2‐pyridinepropanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 8.1981(8), b = 9.9680(10), c = 10.4956(10) Å, α = 90.740(3)° β = 108.142(3)°, γ = 111.025(3)°, Z = 1, V = 1.537 ų. The structure of the nickel(II) complex consists of neutral molecules in which the nickel(II) ion sits on a center of symmetry and is octahedrally coordinated by two sac ligands, and two neutral pypr ligands. The pypr acts as a bidentate N‐ and O‐donor ligand forming a seven‐membered chelate ring, while sac behaves as a monodentate O‐donor ligand via the carbonyl O atom. The Ni‐N bond distance is 2.1016(15) Å, whereas the Ni‐O_pypr and Ni‐O_sac bond distances are 2.1280(12) and 2.0792(11) Å, respectively. The individual molecules are held together with a strong hydrogen bond between the hydroxyl O atom of pypr and N atom of sac and the C‐H…O type weak hydrogen bonds between some ring hydrogen atoms of pypr and sac, and the carbonyl and sulfonyl O atoms of sac in the neighbouring molecules. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,Crystal and Molecular Structure of 2‐Pyridylethanolbis(saccharinato)mercury(II)

2‐Pyridylethanolbis(saccharinato)mercury(II), [Hg(sac)2(pyet)], where sac and pyet are the saccharinate anion and the 2‐pyridylethanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 10.4518(6), b = 11.3796(6) (5), c = 19.9945(12) Å, a = 102.758(3)° b = 98.146(3)°, g = 104.751(3)°, Z = 4, V = 2193.0(2) ų. The unit cell contains two crystallographically independent [Hg(sac)2(pyet)] units in which the mercury(II) ion is tetrahedrally coordinated by two nitrogen atoms of two sac ligands, and one nitrogen and one oxygen atoms of one neutral pyet ligands. The pyet acts as a bidentate N‐ and O‐donor ligand forming a six‐membered chelate ring, while sac behaves as a monodentate N‐donor ligand. The average bite angle of the pyet ligand is 75.8(5)°. The Hg‐N_sac bond distances are in the range 2.0874(18) and 2.1931(18) Å, whereas the Hg‐N_pyet and Hg‐O_pyet bond distances are 2.2452(19)‐2.3202(19) and 2.6036(17)‐2.5902(16) Å, respectively. The crystal exhibits two strong hydrogen bonds between the hydroxyl O atom of pyet and sulfonyl O atoms of sac and the C‐H…O type weak hydrogen bonds between H atoms of the aromatic rings of the pyet and the sulfonyl O atoms of the sac ligands. Furthermore, packing of the molecules in the solid‐state results in aromatic π‐π interactions associated with the aromatic rings of sac‐sac and py‐py.     

Crystal structure analysis of {bis‐2,6‐(3,5‐dimethylprazolyl) pyridine‐dicyanato}copper(II)monohydrate

A mononuclear copper(II) complex, [Cu(dmpp)(OCN)₂(H₂O)], was synthesized using 2,6‐bis (3,5‐dimethylpyrazolyl) pyridine (dmpp) and cyanate anion (OCN), and characterized by single crystal X‐ray diffraction. The coordination around the Cu atom is a distorted square‐pyramid involving three N atoms from the dmpp ligand and one N atom from OCN at the basal plane. The O atom of the OCN group is located at the apical position. The Cu atom is located 0.2782(1) Å above the basal plane. The Cu atom is coordinated by different donor atoms of the OCN groups. The complex crystalizes in monoclinic space group P2₁/n, with unit cell dimensions a= 12.4413(12), b=11.1457(13), c=14.2203(12) Å, β=108.817(3)°, V= 1866.5(3) ų. The cell containes 4 molecules. In the crystal, there are three intermolcular and three intramolecular hydrogen bonds interactions. The Cu atom and crystal water O interactions is 5.574 Å. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Structure and optical properties of Mg‐doped ZnO nanoparticles by polyacrylamide method

Mg‐doped ZnO (Mg_xZn_1‐xO) nanoparticles with precise stoichiometry are synthesized through polyacrylamide polymer method. Calcination of the polymer precursor at 650 °C gives particles of the homogeneous solid solution of the (Mg_xZn_1‐xO) system in the composition range (x < 0.15). ZnO doping with Mg causes shrinkage of lattice parameter c. The synthesized Mg_xZn_1‐xO nanoparticles are typically with the diameter of 70–85 nm. Blue shift of band gap with the Mg‐content is demonstrated, and photoluminescence (PL) from ZnO has been found to be tunable in a wide range from green to blue through Mg doping. The blue‐related PL therefore appeared to be caused by energetic shifts of the valence band and/or the conduction band of ZnO. Mg_xZn_1‐xO nanoparticles synthesized by polyacrylamide‐gel method after modified by polyethylene glycol surfactant have a remarkable improvement of stability in the ethanol solvent, indicating that these MZO nanoparticles could be considered as the candidate for the application of solution–processed technologies for optoelectronics at ambient temperature conditions.     

Synthesis and crystal structure determination of two dispiro compounds from laboratory x‐ray powder diffraction data

The crystal structures of the dispiro compounds 1,3,4,8,10,11‐Hexaphenyl‐13‐methyl‐1,2,8,9,13‐pentaazadispiro[4.1.4.3]tetradeca‐2,9‐dien‐6‐one ( 3a ) and 4,11‐Bis(4‐methoxyphenyl)‐13‐methyl‐1,3,8,10‐tetraphenyl‐1,2,8,9,13‐pentaazadispiro‐[4.1.4.3]tetradeca‐2,9‐dien‐6‐one ( 3b ) have been determined at room temperature from X‐ray powder diffraction data using the method of simulated annealing as implemented in the programs DASH and TOPAS. Subsequent Rietveld refinements using the data collected to 1.5 Å resolution yielded R‐Bragg values of 2.2% for ( 3a ) and 3.7% for ( 3b ). It was found, that both compounds crystallize in the monoclinc space group P 2₁/n with lattice parameters of a = 17.1656(5) Å, b =13.8128(3) Å, c = 16.1016(5) Å, and β = 103.7330(2)° for ( 3a ) and a = 17.2529(8) Å, b = 13.8729(5) Å, c =16.1287(10) Å, and β = 103.6910(3)° for ( 3b ). Both compounds exhibit a distorted hexagonal close type of packing (hcp) of the molecular centers of gravity. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure refinement of the ternary compound Cu2SnTe3 by X‐ray powder diffraction

The ternary compound Cu₂SnTe₃ crystallizes in the Imm2 (Nº 44) space group, Z = 2, with a = 12.833(4) Å, b = 4.274(1) Å, c = 6.043(1) Å, V = 331.5(1) ų. Its structure was refined from X‐ray powder diffraction data using the Rietveld method. The refinement of 25 instrumental and structural variables led to R_p = 10.2%, R_wp = 11.8%, R_exp = 7.7%, R_B = 10.6%, S = 1.6 and χ² = 2.6, for 5501 step intensities and 163 independent reflections. This compound is isostructural with Cu₂GeSe₃, and consists of a three‐dimensional arrangement of slightly distorted CuTe₄ and SnTe₄ tetrahedra connected by common corners. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural analysis of bis{(N,N′–dimethylformamide) (μ‐formato)[μ‐bis(salicylidene)–1,3‐propanediaminato] nickel(II)} copper(II) and zinc(II) monohydrate hetero‐trinuclear complexes

The two linear hetero‐trinuclear metallic complexes with Cu²⁺, Ni²⁺ and Zn²⁺ ions, [CuNi₂ {(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(I) and [ZnNi₂{(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(II), form crystals which belong to the monoclinic system, space group P2₁/c, with unit cell dimensions a=10.537(4), b=16.612(5), c=13.837(3) Å, β=111.09(5)°, V=2259.8(12) ų in (I) and a=10.525(4), b=16.658(5), c=13.826(3) Å, β=111.11(5) °, V=2261.4(8) ų in (II), respectively. The coordinations around the M (Ni²⁺, Cu²⁺, Zn²⁺) ions in the title complexes are distorted octahedrals. The stereochemistries of the bridge ligands, linking to the metal ions each other, are changed between Ni…M (Cu²⁺, Zn²⁺) distances. The Ni…M (Cu²⁺, Zn²⁺) distances are 3.0469(13) and 3.0645(14), respectively. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The crystal structure of α‐SrGaBO4

A new compound α‐SrGaBO₄ has been synthesized by solid state reaction at high temperatures, and its structure has been solved by direct methods from powder X‐ray diffraction. α‐SrGaBO₄ has an orthorhombic system, Pccn space group, with lattice parameters a = 15.3154(7) Å, b = 8.9186(4) Å, c = 5.8130(3) Å, and Z = 8. The structure consists of infinite chains run parallel to the c axis and built up of GaO₄ tetrahedral and BO₃ triangles. The basic unit of these chains is a six ‐ membered Ga₂BO₈ ring formed by two GaO₄ tetrahedra and one BO₃ triangles. The Sr atom is bonded to eight oxygen atoms. The strontium atoms serve to hold the chains together through co‐ordination with oxygen atoms. DTA curve of noncrystalline glassy SrGaBO₄ was discussed. The XRD results show no phase transition occurs between ‐173 °C and 127 °C. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Crystal Structure Analysis of One Dimensional Supramolecular [Cd (Glu) (Tu)2]n

The complex of [Cd (C₅H₆O₄) (CH₄N₂S)₂]_n ( I ) has been synthesized and its X‐ray crystal structure determined at room temperature, M = 394.74, monoclinic, space group Pc (No. 7), with lattice parameters a = 7.683(3), b = 11.566, c = 16.00(1) Å, β = 100.32 (4)°, and Z = 4. There are two different Cd sites in this complex. Cd (1) coordinates to four oxygen atoms from Glutaric anion and two sulfide atoms from thiourea. Cd (2) coordinates to three oxygen and two sulfide atoms. The Cd atoms are linked by glutaric anion to form one‐dimensional chains. The adjacent chains are held together by hydrogen bonds to form a three dimensional network.     

On the anharmonic vibrations in crystalline silicon

Using a total of 1052 Bragg reflections of silicon, an X-ray investigation has been carried out to deduce the anharmonic thermal parameter β, apart from the estimation of the harmonic contribution of the thermal vibration at room temperature. Reflections of type h + k + l = 4n, and 4n ± 1 were used to estimate these parameters using MoK α radiation and a Nonius CAD-4 X-ray diffractometer. We obtain B_si, = 0.451(0.008) Ų and β_si = 0.279(2.630) eV Å⁻³ with R = 3.12%. The present B and β values are in very good agreement with the earlier studies.     

Synthesis and crystal structure of binuclear molecule Ho<Subscript>2</Subscript>(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COO)<Subscript>6</Subscript>⋅4H<Subscript>2</Subscript>O

The complex Ho₂(2-FC₆H₄COO)₆?4H₂O has been synthesized and structurally characterized by single crystal X-ray diffraction methods. The complex crystallizes in the triclinic system with space group P \(\bar 1\), lattice parameters a = 9.293(8) Å, b = 9.845(8) Å, c = 12.703(11) Å, α = 85.470(14)^°, β = 87.537(12)^°, γ = 62.485(11)^°, V = 1027.5(15) ų, Z = 1, D_calc = 1.998 Mg/m³. The Ho³⁺ ion is in distorted monocapped square-antiprism coordination environment and is coordinated by nine oxygen atoms, seven from five 2-FC₆H₄COO^2? groups, two from two water molecules. Two Ho³⁺ ions are linked together by four bridging carboxylate groups to form a binuclear molecule with inversion center.     

Rh(I) and Pd(II) complexes of methoxy functionalized heterocyclic carbene: Synthesis and characterization

A new methoxy functionalized 2‐(trichloromethyl)‐1,3‐diarylimidazolidin (6) was synthesized as the precursor for N‐heterocyclic carbene complexes of Pd(II) and Rh(I) by the condensation of N,N'‐bis(2,4‐dimethoxyphenyl)‐1,2‐diaminoethane with chloral. The structures of all compounds have been elucidated by a combination of multinuclear NMR spectroscopy, elemental analysis and in one instance, by single crystal X‐ray diffraction. Compound 8, C₂₇H₃₄N₂O₄ClRh, crystallizes in the triclinic space group P‐1 with cell dimensions a = 9.7642(12)Å, b = 11.1914(11)Å, c = 13.0102(14)Å, α = 104.034(9)°, β = 106.658(9)°, γ = 99.658(9)° with Z = 2. The molecular structure of 8 shows the geometry around the Rh metal to be a slightly distorted square planar. The crystal structure shows the formation of centrosymmetric dimers via intermolecular C‐H...Cl hydrogen bonds. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure and conformation of a nickel complex: {2‐Hydroxo‐3‐piperidine‐1‐yl‐methyl‐N,N′(bis‐5‐bromobenzylpropylenediimine)nickel(II)perchlorate}

The title compound, a nickel complex [C₂₃H₂₆N₃O₂Br₂Ni.(ClO₄)] (CCDC 199520) crystallizes in triclinic space group P with the cell parameters a = 10.2560(4), b = 10.8231(4), c = 12.0888(5)Å, α = 99.404(1), β = 99.780(1), γ = 92.252(1)° and V = 1301.49(9)ų. The structure was solved by Patterson method and refined by full‐matrix least‐squares procedures to a final R = 0.0497 using 6287 observed reflections. In the complex, the piperidine ring takes chair conformation and the geometry around the Ni ion is slightly distorted square planar. The dihedral angle between the planes [N‐Ni‐N and O‐Ni‐O] is 9.4(1)°. The chelate ring containing both the nitrogen atoms adopts twisted boat conformation. The molecules in the crystal are stabilized by N‐H…O and C‐H…O types of hydrogen bonds in addition to a C‐H…π interaction. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)