The structure of solvate [Cu2(DfH)4(4,4′-Bipy)] · 2DMF

The crystal structure of [Cu₂(DfH)₄(4,4′-Bipy)] · 2DMF prepared by the reaction of copper(II) acetate with diphenylglyoxime (DfH₂) and 4,4′-bipyridine (4,4′-Bipy) was established by X-ray diffraction. The crystals are monoclinic; a = 15.5192(9) Å, b = 16.2427(11) Å, c = 14.0753(7) Å, β = 101.36(3)°, V = 3478.5(5) ų, Z = 2, and sp. gr. P2₁/c. The crystal structure is composed of discrete dinuclear molecules [Cu₂(DfH)₄(4,4′-Bipy)] and dimethylformamide (DMF) molecules. The coordination polyhedron of the Cu atom (the coordination number is 5) is a tetragonal bipyramid formed by the nitrogen atoms of two monodeprotonated bidentate oxime groups and the bidentate bridging 4,4′-Bipy ligand. The DMF molecules occupy the cavities formed by the dinuclear molecules [Cu₂(DfH)₄(4,4′-Bipy)]. The compound was characterized by IR and NMR spectroscopy.     

Synthesis and crystal structure of bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl)copper(II)

The title compound, bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl) copper(II), [Cu(C₁₇H₁₁NOCl)₂] (1) was synthesized and its crystal structure was determined. The Compound 1 is monoclinic, space group P2 ₁/c with a = 9.146(3) Å, b = 18.724(3) Å, c = 16.230(2) Å, β = 96.46(1)°, V = 2761.8(11) ų, Z = 4, D _c = 1.503 g cm^?3, μ(Mo Kα) = 1.020 mm^?1, R = 0.0606 for 2361 reflections [I > 2σ(I)]. In the title compound, the Cu atom is coordinated by an N₂O₂ donor set from the imine-phenol ligand in a slightly distorted square planar coordination geometry, with the two phenolate O atoms being deprotonated. The Cu–O bond lengths are 1.878(4) and 1.889(4) Å, the Cu–N bond lengths are 1.980(5) and 1.985(5) Å. The angles O1–Cu–N1 and O2–Cu–N2 are 90.96(19) and 90.72(19)°, respectively.     

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)     

Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

Crystal and molecular structure of bis(diphenylmethyl) ether

Bis(diphenyl methyl)ether, C₂₆H₂₂O, crystallizes in the monoclinic system:a = 9.823(2),b = 22.638(5),c = 9.275(2) Å, β = 104.89(1) °,Z = 4,P2₁/n. The structure has been determined by direct methods, using CuKα photographic data, and refined by full-matrix least squares toR = 0.058 with Cu Kα diffractometer data for 1974 observed reflections. The molecules are held together entirely by van der Waals' forces. There is a marked difference in the molecular conformation, as defined by dihedral angles, on each side of the central oxygen atom.     

Crystal structure of catena-poly[diaqua(μ-iminodiacetato-N,O,O′: O″)cobalt(II)]

The crystal structure of the [Co(C₄H₅NO₄)(H₂O)₂] complex has been determined by X-ray diffraction analysis (λMo, R = 0.0237 for 768 reflections). The crystals are orthorhombic, a = 14.345(1) Å, b = 5.234(1) Å, c = 9.780(1) Å, Z = 4, d _calcd = 2.045 g cm^?3, and space group Pca2₁. The donor atoms (one N and two O atoms) of the iminodiacetate ion (Ida) are located on the same octahedron face around the Co atom [Co-N, 2.120(3) Å; Co-O, 2.063(3) and 2.151(3) Å]. The O atoms of two water molecules are in the trans positions relative to the O atoms of the carboxylate groups [Co-O, 2.126(3) and 2.157(3) Å]. The sixth coordination site is occupied by the O atom of the adjacent Ida ion [Co-O, 2.054(3) Å], which results in the formation of infinite chains in the structure.     

Crystal Structure of bis(18-Crown-6)-bis(formato-O) dicaesium dihydrate

Abstract  The crystal structure of the title compound, [2Cs⁺(C₁₂H₂₄O₆)₂(CHO₂ ⁻)₂(H₂O)₂], was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁ /n with cell parameters a = 10.4278(7) ?, b = 10.0183(5) ?, c = 18.2383(12) ?, β = 93.723(5)°, V = 1910.3(2) ?³ and Z = 2. The Cs cations are bonded to each of the six O atoms of a crown ether ring, two water molecules, and one O atom of a formato anion. As a result of that, a centrosymmetric dimeric dinuclear complex is formed. The two halves of the dimer are connected by a ring of formato anions and water molecules which are linked by O–H···O hydrogen bonds. Index Abstract  The title compound, bis(18-crown-6)-bis(formato-O), caesium dihydrate, features a centrosymmetric dimeric dinuclear complex where two Cs cations are coordinated by six O atoms of a crown ether ring. The two halves of this complex are held together by a ring of formato anions and water molecules which are linked by hydrogen bonds.      

Synthesis Characterization and Crystal Structure of 2-(3,4,5-trimethoxyphenyl)-1-(4-fluorophenyl)-4,5-diphenyl-1H-imidazole

The title compound, C₃₀H₂₅FN₂O₃, was prepared from the four-component one-pot condensation reaction and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-Visible, and single-crystal X-ray diffraction. The compound crystallizes in the triclinic crystal system with the space group Pī, with unit cell parameters a = 10.286(2) Å, b = 11.795(2) Å, c = 21.331(4) Å, α = 100.270(3)°, β = 90.093(3)°, γ = 90.062(3)°, and Z = 4. The crystal and molecular structure of the title molecule is stabilized by intra-molecular interactions of types C–H···N and C–H···O.     

The Crystal and Molecular Structure of the Complex Diaquatetrakis(imidazole)copper(II) Terephthalate Crystal Structure Containing Cu(II) Him and TA

The title compound has been synthesized and its crystals structure determined at room temperature. MW = 536.01, monoclinic, space group C2/c, Z = 4, a = 22.193(5) Å, b = 8.038(2) Å, c = 15.699(4) Å, β = 119.64(2)°. The crystal structure consists of repeated [Cu(Him)₄(H₂O)₂] (Him = imidazole) cations and non-coordinated terephthalato dianions. The copper(II) ion displays an elongated octahedral coordination being linked to the four nitrogen atoms of the four imidazole ligands and to the two oxygen atoms of the two water molecules. The terephthalato dianions are hydrogen bonded to the four water molecules and four imidazole groups.     

Crystal structure of an unusual four-coordinated copper(II) complex containing 1,10-o-phenanthroline and salicyclic acid crystal structure containing Cu(II) o-phen and salicyclic acid

We have synthesized a multi-ligand chelate copper(II) complex [Cu · (C₇H₅O₃] · (C₁₂H₈N₂) · H₂O₁ · (C₇H₆O₃)· NO₃, and determined its structure by X-ray diffraction method. The space group of the title compound is P2₁/a. It is monoclinic, with a = 14.227(4), b = 9.627(4), c = 19.008(7) Å, β = 102.06(3)·, Z = 4. The two salicyclic acid molecules in the cell are in different environments, one inner, the other outer. The geometry around Cu(II) is a four-coordinated distorted plane square. The two coordinating atoms are two nitrogen atoms from phenanthroline, one oxygen atom from salicyclic acid, one oxygen atom from water.     

Crystal structure of zdenekite NaPbCu5(AsO4)4Cl · 5H2O

The crystal structure of the mineral zdenekite NaPbCu₅(AsO₄)₄Cl · 5H₂O was established (Bruker SMART CCD diffractometer, synchrotron radiation, λ = 0.6843Å, R = 0.096 for 1356 reflections). Single-crystal X-ray diffraction study demonstrated that zdenekite belongs to the monoclinic system with the unit-cell parameters a = 10.023(7) Å, b = 19.55(1) Å, c = 10.023(6) Å, β = 90.02(1)°, sp. gr. P2₁/n, Z = 4. The structure consists of polyhedral layers parallel to the (010) plane. These layers are formed by Cu? polyhedra φ = O, Cl, H₂O) and AsO₄ tetrahedra. Distorted Na octahedra and Pb 7-vertex polyhedra and H₂O molecules coordinated to these metal atoms are located between the layers.     

Crystal structure of (2,2′-bipyrimidine)-dinitratopalladium(II) acetone solvate

(2,2′-bipyrimidine)dinitratopalladium(II) forms a triclinic crystal in space groupP?1 witha=7.605(5) Å,b=8.791(4) Å,c=12.632(5) Å, α=85.11(3)⁰, β=78.79(4)⁰, γ=77.45(4)⁰,V=807.7(7) ų, andZ=2. The Pd atom exhibits square planar coordination geometry with mean Pd?O=2.206(7) Å, Pd?N=1.990(5) Å, O?Pd?O=92.0(2)⁰, and N?Pd?N=81.0(2)⁰. The complexes associate across an inversion center with Pd...Pd=3.190(2) Å. The bipyrimidine ligand is bowed with a 5.9(2)⁰ dihedral angle between the C₄N₂ rings. The nitrate ions are on the same side of the N₂O₂ donor atoms plane and make 60.4(2)⁰ and 66.6(2)⁰ dihedral angles with that plane.     

The crystal and molecular structure of bis(tetramethylammonium) pentachlorooxomolybdate(V)‐acetonitrile(1:1)

The crystal structure of the title compound, C₁₀H₂₇Cl₅MoN₃O was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/m, with a= 29.075(8) Å, b= 11.843(4) Å, c= 13.252(4) Å, β=117.049(7)°, V = 4064(2) ų, Z=8. The structure was solved by direct methods and refined by least‐squares methods to a final R = 0.0307 for 5095 observed reflections with I>2σ(I). In the pentachlorooxomolybdate anion, the planar chlorines are bent away from the axial oxygen ligand. The Mo‐O bond length is 1.6620(18) Å that indicates significant double bond character. The oxygen trans Mo‐Cl bond is significantly longer than all of the planar Mo‐Cl bonds. These differences can be attributed to a trans influence of the oxygen atom. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of di-μ-bromobromopentakis(benzimidazole)dicopper(II) monobromide tetrahydrate [Cu2Br3(C7H6N2)5]Br·4H2O

A new complex compound. [Cu₂Br₃(C₇H₆N₂)₅]Br·4H₂O, has been synthesized and its crystal structure investigated by single-crystal X-ray methods. The crystals are isostructural with those of the [Cu₂Cl₃(C₇H₆N₂)₅]Cl·4H₂O salt. They are orthorombic, space group Pnma with 4 formula units in a cell of dimensions:a+19.923(1),b+17.555(2),c+12.0523(4)Å. The structure was refined by full-matrix least-squares to giveR+0.047 andR _w+0.053 for 3569 intensities above 3σ(I). As in the chloride compound, the complex cation consists of pairs of distorted trigonal bipyramidal Cu(II) centers which share an edge by two equatorial bromide ions. The Cu...Cu nonbonding distance in the complex in 3.4894(7)Å. The two Cu?Br?Cu bridges are not equivalent and their geometry is slightly different from that in the chloride complex. Comparison of the investigated structure to other binulear bis(μ-halide) bridged copper(II) complexes of similar structure has been made.     

Synthesis and structural characterization of dihexamethylenetetraminetetraaquocobalt(II) hexaaquocobalt(II) sulfate hexahydrate

The synthesis and crystal structure of a new three dimensional cobalt(II) complex [Co(C₆H₁₂N₄)₂(H₂O)₄Co(H₂O)₆][SO₄]₂.6H₂O are reported. It crystallizes in the triclinic space group P-1 with a = 13.394(3), b = 16.077(3), c = 9.282(2) Å, = 89.71(2), = 90.42(2), = 114.02(2)°, V = 1825.6(7)ų and Z = 2. The structure is comprised of [Co(C₆H₁₂N₄)₂ (H₂O)₄Co(H₂O)₆][SO₄]₂ units and H₂O molecules. Two molecules of ligand and four molecules of water chelate one type of Co^II in an octahedral fashion through two N and four O atoms: the four O atoms form the equatorial plane and the two N atoms occupy the apical positions. The other type of Co^II cation is chelated by six water molecules.     

Crystal structure of 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl]benzamide : <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-dimethylformamide (1 : 1)

The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C₁₅H₁₁N₃O₂S₂ · C₃H₇NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2₁/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.     

A dinuclear cyano-bridged complex based on hexacyanoferrate(III) and samarium(III) nitrate: synthesis and crystal structure

A new complex, [Sm(DMF)₄(H₂O)₄Fe(CN)₆]·H₂O (DMF = N, N-dimethylformamide), has been synthesized and characterized by X-ray single crystal structure and thermogravimetric analyses. The complex crystallizes in the P2₁/n space group, with lattice parameters a = 17.583(4) Å, b = 8.870(2) Å, c = 19.845(6) Å, = 95.98(3)°, V = 3078(1) ų, D _x = 1.679 Mg m^–3, D _m = 1.65(1) Mg m^–3, Z = 4. The molecular structure shows that a cyano-bridged bimetallic structure is obtained. The Sm atom is coordinated by eight oxygen atoms of four water molecules and four DMF molecules and one nitrogen atom of the bridging cyanide ligand. The iron atom assumes approximately an octahedral environment surrounded by six CN ligands. The hydrate water molecule is hydrogen-bonded to one of the O atoms bound to Sm. Each terminal CN ligand of the Fe(CN) ₆ ^3– entity is hydrogen-bonded to some O atoms of water molecules. An infrared spectrum is also reported.     

Synthesis and structure of (NH4)4[(DMF)2Mo8O26]· 2CH3CH2OH·2H2O (DMF= N , N -dimethylformamide)

A new organic-inorganic hybrid γ-octamolybdate complex, (NH₄)₄[(C₃H₇NO)₂Mo₈O₂₆]·2CH₃CH₂OH·2H₂O was synthesized from the mixture of ethanol, DMF, 4-aminobenzoic acid, (NH₄)₆Mo₇O₂₄·4H₂O, HCl and H₂O. The structure was determined by X-ray crystallography. It crystallizes in monoclinic P2₁/n space group with the crystal cell parameters of a = 8.8825(4), b = 21.1608(10), c = 11.1343(6) ?, β = 104.7720(10)°, V = 2023.64(17) ?³ and Z = 2. The crystal X-ray analysis shows that two DMF molecules are bound to γ-octamolybdate anion. The molecular structure is stabilized by the complex hydrogen bonding.     

X-ray structure analysis of 3β-hydroxy-4-(1,4-oxazin-4-yl)-androstane (C31H54NO2)

The crystal structure of 3β-hydroxy-4-(1,4-oxazin-4-yl)-androstane (C₃₁H₅₄NO₂) has been determined by X-ray crystallographic techniques. The compound crystallizes in the orthorhombic space group P2₁2₁2 with the following unit-cell parameters: a = 7.124(1) Å, b = 10.127(1) Å, c = 40.660(1) Å, V = 2933.4(1) ų, and Z = 4. The structure has been solved by direct methods and refined to an R factor of 0.067. Three six-membered rings, A, C, and E, exist in the chair conformation, while the ring B adopts a distorted half-chair conformation. The five-membered ring, D, has a distorted envelope conformation. The crystal structure is stabilized by strong intermolecular O-H...O hydrogen bonds.     

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)