Structure and properties of double complex salts [Co(NH3)6][Fe(CN)6] and [Co(NH3)6]2[Cu(C2O4)2]3

Double complex salts (DCSs) [Co(NH₃)₆][Fe(CN)₆] (I) and [Co(NH₃)₆]₂[Cu(C₂O₄)₂]₃ (II) and complex [Co(NH₃)₆]₂(C₂O₄)₃·4H₂O (III) are synthesized and investigated by single crystal XRD, crystal optics, and elemental analysis. The crystalline phases of I, II, and III (R-3, P2₁/c, and Pnnm space groups respectively) have the following crystallographic characteristics: a = 10.9804(2) ?, b = 10.9804(2) ?, c = 10.8224(3) ?, V = 1130.03(4) ?³, Z = 3, d _x = 1.65 g/cm³ (I); a = 9.6370(2) ?, b = 10.2452(2) ?, c = 13.2108(3) ?, V = 1932.90(9) ?³, Z = 2, d _x= 1.97 g/cm³ (II), and a = 11.7658(3) ?, b = 11.7254(3) ?, c = 14.1913(4) ?, V = 1304.34(5) ?³, Z = 2, d _x = 1.68 g/cm³ (III). This paper investigates the products of DCS thermolysis in a hydrogen atmosphere: the intermetallic compound CoFe with the bcc parameter a = 2.852 ? for I and a heterogeneous mixture of Co and Cu in the decomposition of II. The coordinated CN⁻ and C₂O₄²⁻ groups then turn into NH₃, hydrocarbons, and CO₂. The dominant hydrocarbon is methane.     

Mononuclear eight-coordinate (NH4)3[YIII(Nta)2] and one-dimensional unlimited zigzag type nine-coordinate {K[YIII(Egta) · 4H2O}n complexes: Syntheses and structural determination

The title complexes (NH₄)₃[Y^III(Nta)₂] (I) (H₃Nta = nitrilotriacetic acid) and {K[Y^III(Egta)] · 4H₂O} _n (II) (H₄Egta = ethyleneglycol-bis-(2-aminoethylether)-N,N,N′,N′-tetraacetic acid) were prepared, and their molecular and crystal structures were determined by single-crystal X-ray diffraction techniques. Complex I crystallizes in the rhombohedral crystal system with R $ \bar 3 $ \bar 3 c space group. The central Y³⁺ ion is eight-coordinated by two nitrogen and six oxygen atoms, which come from two tetradentate Nta ligands. The crystal data are as follows: a = 7.9340(14) ?, c = 54.611(15) ?, V = 2977.1(11) ?³, Z = 6, ρ_calcd = 1.738 mg/cm³, μ = 3.011 mm⁻¹, F(000) = 1596, R = 0.0234 and wR = 0.0641 for 686 observed reflections with I ≥ 2σ(I). The {K[Y^III(Egta)] · 4H₂O} _n is nine-coordinated by two nitrogen and seven oxygen atoms and produces a 1D unlimited zigzag-type chain through a bridging carboxylic group. {K[Y^III(Egta)] · 4H₂O} _n crystallizes in the monoclinic crystal system with C2/c space group. The crystal data are as follows: a = 37.588(5) ?, b = 13.7101(19) ?, c = 8.6070(12) ?, β = 99.929(2)°, V = 4369.0(11) ?³, Z = 8, ρ_calcd = 1.753 mg/cm³, μ = 2.934 mm⁻¹, F(000) = 2368, R = 0.0385 and wR = 0.0800 for 4082 observed reflections with I ≥ 2σ(I).     

Crystal structure of [Cu(NH3)4](ReO4)2

At T = 150 K, the crystal structure of [Cu(NH₃)₄](ReO₄)₂ is studied: a = 6.5167(3) ?, b = 6.7790(3) ?, c = 7.4627(3) ?, α = 67.336(1)°, β = 80.004(1)°, γ = 70.687(1)°, V = 286.70(2) ?³, P-1 space group, Z = 1, d _x = 3.661 g/cm³. We analyze the packing of ions using the translation sublattice isolation technique.     

Double complex salts [Pd(NH3)4]3[Rh(NO2)6]2, [Pd(NH3)4]3[Rh(NO2)6]2·H2O as promising precursors to prepare Pd-Rh nanoalloys

Two new double complex salts [Pd(NH₃)₄]₃[Rh(NO₂)₆]₂ (I) and [Pd(NH₃)₄]₃[Rh(NO₂)₆]₂·H₂O (II) are synthesized and characterized. The techniques to produce one-phase residues of the salts are developed. The crystallographic data for I: a = 18.915(2) ?, V = 6767.4 ?³, F-43c space group, Z = 8, d _x = 2.548 g/cm³; II: a = 21.160(6) ?, b = 8.085(7) ?, c = 21.363(4) ?, β = 91.71(4)°, V = 3661.1(6) ?³, P2₁/c space group, d _x = 2.357 g/cm³. Thermal properties of the obtained compounds in the hydrogen and helium atmosphere are studied. It is shown that the final product of their decomposition both in the inert and reducing atmosphere is a powder consisting of bimetallic nanosized particles (nanoalloy) of Pd_0.59Rh_0.41 (Fm-3m space group, a = 3.856(2) ?, crystallite size of 8–11 nm).     

Synthesis and vibrational spectra of copper(II) and erbium(III) complexes with 2-[2′-(oxymethyldiphenylphosphinyl)phenyldiazenyl]-4- tert -butylphenol (HL) [CuL2] · 2H2O and Er(NO3)2 · 2 HL · 2H2O. Crystal structure of [CuL2] · 2H2O

The syntheses of the complex copper salt CuL₂ · 2H₂O (I) and the erbium nitrate complex Er(NO₃)₃ · 2HL · 2H₂O (II) (HL is 2-[2′-(oxymethyldiphenylphosphinyl)phenyldiazenyl]-4-tert-butylphenol) have been described. Basic vibrational frequencies in the IR spectra of I and II have been interpreted. The crystal structure of I has been determined by X-ray crystallography: the crystals are monoclinic, a = 15.157(3) ?, b = 17.080(2) ?, c = 22.451(9) ?, β = 106.09(3)°, V = 5584(3) ?³, Z = 4, space group C2/c, R = 0.0546 (for 1152 reflections with I > 2σ(I)). The coordination polyhedron of the copper atom (symmetry C ₂) can be described as a symmetrically elongated square bipyramid (4+2). The basic square of the Cu polyhedron is formed by the oxygen atom of the substituted phenol and one of the nitrogen atoms of the azo group of each of the two deprotonated ligands L⁻ (Cu-N, 1.969(6) ?; Cu-O, 1.899(5) ?). The angles between the opposite O and N atoms are 157.6°, and the other equatorial angles are in the range 90.6°–95.9°. The axial positions are occupied by the anisole O(2) and O(2A) atoms (Cu-O, 2.737(6) ?, the O(2)Cu(1)O(2A) angle, 132.3°). In the crystal of I, complex molecules and water molecules of crystallization are combined by a system of hydrogen bonds. IR spectra show that, in complex II, as distinct from compound I, the HL ligand is coordinated to the erbium atom through the phosphoryl oxygen atom. Original Russian Text ? A.Yu. Tsivadze, L.Kh. Minacheva, I.S. Ivanova, V.E. Baulin, E.N. Pyatova, V.S. Sergienko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 4, pp. 601–607.     

Two novel organic amine templated lanthanide sulfates: Layer H3DETA · [Nd(H2O)(SO4)3] and chain-like H3DETA · [Ho(H2O)2(SO4)3]

Two novel organic amine templated lanthanide sulfates, layer (H₃DETA)[Nd(H₂O)(SO₄)₃] (I) and chain-like (H₃DETA)[Ho(H₂O)₂(SO₄)₃] (II), are hydrothermally synthesized by using diethylenetriamine (DETA) as template, and are structurally characterized by ICP, elemental analysis, X-ray single-crystal diffraction, X-ray powder diffraction, IR, and TG. Compound I is monoclinic with space group P2₁ and data of unit cell: a = 6.6518(13), b = 10.373(2), c = 11.091(2) ?, β = 93.61(3)°, V = 763.7(3) ?³, ρ _c = 2.421 g/cm³, μ(MoK _α) = 3.885 mm⁻¹, Z = 2, R ₁ = 0.0194 for 3312 reflections with F _o > 2σ(F _o). The Nd ions are nine-coordinated by one oxygen atom of coordinated water and eight oxygen atoms of sulfates. Compound I displays the layer structure constructed by linking Nd ions with three-linkage SO₄ tetrahedra as the bridge (affording one coordinated vertex and coordinated edge). Compound II crystallizes in the monoclinic space group P2₁/c with unit cell data: a = 6.594(13) ?, b = 14.783(3) ?, c = 16.599(3) ?, β = 93.47(3)°, V = 1614.2(6) ?³, ρ _c = 2.454 g/cm³, μ(MoK _α) = 5.37 mm⁻¹, Z = 4, R ₁ = 0.0259 for 1815 reflections with F _o > 2σ(F _o). The Ho ions are eight-coordinated by two oxygen atoms of coordinated water and six oxygen atoms of sulfates. The straight chain-like structure of II is attained by alternatively arranging HoO₈ polyhedra and two-linkage SO₄ tetrahedra (affording two coordinated vertices). The TG results indicate that the two compounds experience three weight losses and lead to distinct residues: Nd₂O₃ for I and HoO(SO₄)_0.5 for II.     

New π ligand N,N,N,N′,N′,N′-hexaallylethylenediaminium (L2+): Synthesis and crystal structures of LBr2 · 2H2O and its cuprocomplexes L[CuII(Br0.45Cl3.55)], L[Cu 4I (Br4.55Cl1.45)], and L[Cu 4I Br6]

The alkylation of ethylenediamine with allyl bromide in the presence of a fourfold (with respect to ethylenediamine) molar amount of NaHCO₃ in acetone with an ethanol admixture (15: 1) affords LBr₂ · 2H₂O (I), where L²⁺ is the N,N,N,N′,N′,N′-hexaallylethylenediaminium cation. Single crystals of complexes L[Cu^II(Br_0.45Cl_3.55)] (II), L[Cu₄^I(Br_4.55Cl_1.45)] (III), and L[Cu₄^IBr₆] (IV) are prepared by ac electrochemical synthesis from an ethanolic solution of LBr₂ · 2H₂O, CuCl₂ · 2H₂O (or CuBr₂) at copper wire electrodes. The crystal structures of compounds I–IV are determined by X-ray diffraction analysis. The crystals of complex I are monoclinic: space group P2₁/n, a = 8.544(3), b = 10.404(3), c = 13.350(4) ?, β = 97.29(3)°, V = 1177.2(6) ?³, Z = 2. The bromine anions in compound I are bonded to the L²⁺ cations and water molecules through hydrogen contacts (E)H…Br (E = O, C) of 2.57(3)–2.86(3) ?. The crystals of compounds II–IV are triclinic: space group P . For II: a = 8.762(4), b = 9.163(4), c = 16.500(6) ?, α = 95.62(4)°, β = 96.39(4)°, γ = 111.46(4)°, V = 1211.4(9) ?³, Z = 2; for III: a = 9.074(4), b = 9.435(4), c = 9.829(5) ?, α = 116.12(4)°, β = 104.14(4)°, γ = 100.22(4)°, V = 692.3(6) ?³, Z = 1; for IV isostructural III: a = 9.084(4), b = 9.404(4), c = 9.869(4) ?, α = 116.31(3)°, β = 104.00(3)°, γ = 100.37(3)°, V = 692.1(5) ?³, Z = 1. Unlike the isolated tetrahedral CuX₄²⁻ anion in structure II, an original chain anion (Cu₄X₆²⁻) _n is observed in the structures of π complexes III and IV. Original Russian Text ? M.M. Monchak, A.V. Pavlyuk, V.V. Kinzhibalo, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya, 2009, Vol. 35, No. 6, pp. 414–419.     

Two New Octahedral Cd(II) Complexes [Cd(L)2] and {[Cd(LH)2(SCN)2]H2O} [L = C6H5C(OH)NN = C(CH3)C5H4N]: Synthesis and Structural Studies

Two new octahedral Cd(II) complexes [Cd(L)₂] (1) and {[Cd(LH)₂(SCN)₂]H₂O} (2) [where LH = C₁₄H₁₃N₃O] are synthesized using a tridentate hydrazone ligand (LH) and they are characterized by elemental analysis, IR spectra, NMR spectra, thermal studies and finally the structures have been determined by single crystal X-ray diffraction. Complex 1 crystallizes in monoclinic system, space group C2/c with a = 22.565(6) ?, b = 10.252(3) ?, c = 12.187(4) ?, β = 118.851(2)^∘, and Z = 4. Complex 2 also crystallizes in the monoclinic system, space group P2₁/c with a = 9.257(9)?, b = 17.809(2)?, c = 9.548(9)?, β = 107.439(4)^∘, and Z = 2. In 1 the ligand binds the Cd(II) ion in tridentate fashion, whereas in 2 it acts as a bidentate ligand.     

Preparation, Structure, and Thermal Decomposition of Co(II) Complexeswith 2,3- and 2,5-Dichlorobenzoic Acid and Imidazole

Summary.  The reaction products of Co(II)-2,3- and -2,5-dichlorobenzoate with imidazole (1, 2; CoL ₂⋯2imdċ2H₂O, L=C₇H₃Cl₂O, imd=imidazole) were characterized by their spectroscopic and thermochemical properties. The compounds crystallize in the monoclonic system with space group = P2₁/c, a=13.848(3), b=12.841(3) ?, c= 7.064(2) ?, β=98.12 °, V=1243.5(4) ?³, Z=2 for 1 and space group =P2₁/n, a=13.293(3), b= 6.964(2), c=13.800(3) ?, β=108.92(3) °, V=1208.6(4) ?³, Z=2 for 2. The complexes lose their crystal water in one step at 333 K and subsequently decompose to CoO with intermediate formation of Co₃O₄. Received August 9, 1999. Accepted (revised) February 11, 2000     

Tetrahedral complexes of zinc(II) chloride with N- and O-containing organic ligands: Synthesis and crystal structures of [ZnCl2(C12H12N2O)] and [ZnCl2(H2O)2](Me4Pyz)2

New complex chlorides [ZnCl₂(ODA)] (I) (ODA=oxydianiline, C₁₂H₁₂N₂O) and [ZnCl₂(H₂O)₂](Me₄Pyz)₂ (II) (Me₄Pyz = 2,3,5,6-tetramethylpyrazine) were synthesized and crystallographically characterized. Crystals of I are monoclinic, space group C2/c, a = 22.682(2) ?, b = 12.646(1) ?, c = 9.951(1) ?, β = 93.23(2)°, V = 2849.7(5) ?³, ρ_calc = 1.569 g/cm³, Z = 8. Structure I contains cyclic fragments consisting of two tetrahedral complexes (ZnCl₂N₂) and two coordinated bridging oxydianiline ligands. Crystals of II are monoclinic, space group P2(1)/c, a = 8.972(2) ?, b = 13.862(3) ?, c = 17.528(4) ?, β = 101.72(3)°, V = 2134.5(7) ?³, ρ_calc = 1.384 g/cm³, Z = 4. In structure II, supramolecular pseudo-metallocycles are formed due to formation of hydrogen bonds O(w)-H…N between coordinated water molecules and noncoordinated nitrogen atoms of tetramethylpyrazine molecules.     

Preparation, Structure, and Thermal Decomposition of Co(II) Complexeswith 2,3- and 2,5-Dichlorobenzoic Acid and Imidazole

 The reaction products of Co(II)-2,3- and -2,5-dichlorobenzoate with imidazole (1, 2; CoL ₂⋯2imdċ2H₂O, L=C₇H₃Cl₂O, imd=imidazole) were characterized by their spectroscopic and thermochemical properties. The compounds crystallize in the monoclonic system with space group = P2₁/c, a=13.848(3), b=12.841(3) ?, c= 7.064(2) ?, β=98.12 °, V=1243.5(4) ?³, Z=2 for 1 and space group =P2₁/n, a=13.293(3), b= 6.964(2), c=13.800(3) ?, β=108.92(3) °, V=1208.6(4) ?³, Z=2 for 2. The complexes lose their crystal water in one step at 333 K and subsequently decompose to CoO with intermediate formation of Co₃O₄.     

Synthesis and structures of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O

Single crystals of Cs₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 4H₂O (I) and (NH₄)₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 6H₂O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂]⁴⁻ chains belonging to the crystal-chemical group A₂K⁰²B₂²M₂¹ (A = UO₂²⁺, K⁰² = C₂O₄²⁻, B² = SO₄²⁻, M¹ = NCS⁻) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions. Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120.     

Coordination polymers based on [Re6Se8(CN)6]4? cluster anion, lanthanide cations, and tetraatomic alcohol erythritol

By the interaction of aqueous solutions of salts of the [Re₆Se₈(CN)₆]⁴⁻ cluster anion with salts of Nd(III), Tb(III), and Yb(III) lanthanides in the presence of tetraatomic alcohol erythritol (butane-1,2R,3S,4-tetraol) three new compounds are obtained: K[Nd(C₄H₁₀O₄)(H₂O)₄{Re₆Se₈(CN)₆}]·4H₂O (P $ \bar 1 $ \bar 1 space group, a = 11.544 ?, b = 13.643 ?, c = 13.838 ?, α = 111.97°, β = 108.08°, γ = 90.08°) (1); [{Yb₂(C₄H₉O₄)₂ × (H₂O)₂}{Re₆Se₈(CN)₆}]·5H₂O (P $ \bar 1 $ \bar 1 space group, a = 10.308 ?, b = 10.505 ?, c = 11.154 ?, α = 88.21°, β = 81.83°, γ = 78.50°) (2); [{Tb₂(C₄H₉O₄)₂(C₄H₁₀O₄)}{Re₆Se₈(CN)₆}]·4H₂O (P $ \bar 1 $ \bar 1 space group, a = 10.002 ?, b = 10.276 ?, c = 11.762 ?, α = 91.32°, β = 104.01°, γ = 106.02°) (3). The structures of these compounds are the coordination polymers (chain (2) and grids (1 and 3)) with different coordination modes of erythritol to the lanthanide cations.     

Synthesis and crystal structure of inclusion compounds: Trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid with boric acid and tetrabutylammonium salt

Two new inclusion compounds (n-C₄H₉)₄N⁺C₁₈-H₁₃O₄ ⁻·B(OH)₃ (1) and (n-C₄H₉)₄N⁺C₁₈H₁₃O₄ ⁻ (2) were prepared and characterized by X-ray crystallography. Crystal data: compound 1, monoclinic P2(1)/c, a = 1.569 9(1) nm, b = 0.995 5(6) nm, c = 2.293 3(1) nm, β = 109.962(3)°, Z = 4, and R ₁ = 0.0434, wR = 0.075 9; compound 2, monoclinic C2/c, a = 1.400 5(3) nm, b = 1,282 1(2) nm, c = 1.765 7(3) nm, β = 100.388(1)°, Z = 4, and R ₁ = 0.0584, wR = 0.096 6. In the crystal structure of 1, the tetramers formed by two trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (EADA) anions and two boric acid molecules were connected through O—H⋯O hydrogen bonds to generate a channel type host lattice. The tetra-n-butylammonium cations were stacked to give two columns within each channel with cross-sectional size of about 2.30 nm × 0.93 nm. In the crystal structure of 2, similar honeycomb host lattices with big size were also formed along the [101] direction by three-dimensional accumulation of EADA anions. The tetra-n-butylammonium cations were accommodated in a zigzag fashion within each channel. Translated from Acta Chimica Sinica, 2006, 64(18): 1904–1910 [译自: 化学学报]     

Crystal structure of the reaction product of copper(II) nitrate with α-(3,3-Dimethyl-3,4-dihydro-1-isoquinolyl)hydroxy-iminoacetonitrile [Cu3(μ3-OH)(μ-L)3(NO3)2(H2O)] · 2H2O

The coordination compound [Cu₃(μ₃-OH)(μ-L)₃(NO₃)₂(H₂O)] · 2H₂O (I), where L is the α-(3,3-dimethyl-3,4-dihydro-1-isoquinolyl)hydroxyiminoacetonitrile anion, has been synthesized. The crystal and molecular structure of I was determined by X-ray diffraction (Enraf-Nonius CAD4, MoK _α radiation, graphite monochromator, ω-scan mode, 2θ_max = 49.96°, 7673 unique reflections, a = 12.745(3) ?, b = 13.726(3) ?, c = 28.835(6) ?, β = 93.44(3)°, V = 5035.2(17) ?³, Z = 4, space group P2₁/c). In the trimer complex I, the copper atoms are combined by a bridging hydroxy group. The copper atoms are additionally linked pairswise by three tridentate chelating bridging organic anions coordinated to the Cu(II) atoms by the N and O atoms of the deprotonated oxime group and by the N atom of the dihydroisoquinoline moiety. Original Russian Text ? V.I. Sokol, V.V. Davydov, N. Yu. Merkur’eva, E.I. Polyakova, Yu.V. Shklyaev, V.S. Sergienko, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 10, pp. 1643–1652.     

One-and two-dimensional silver-tetramethylpyrazine coordination polymers with uncoordinated anions: Synthesis and structure of [Ag(Me4Pyz)]PF6 and [Ag2(Me4Pyz)3](BF4)2·H2O

Coordination polymers [Ag(Me₄Pyz)] PF₆(I) and [Ag₂(Me₄Pyz)₃](BF₄)₂·H₂O (II) have been synthesized, and their structures have been determined. The crystals of I are monoclinic, space group C2/c, a = 9.440(2) ?, b = 10.587(2) ?, c = 13.165(3) ?, β= 107.19(3)°, V = 1257.0(5) ?³, d = 2.056 g/cm³, Z = 4. The crystals of II are monoclinic, space group P2₁/n, a = 13.062(3) ?, b = 12.259(2) ?, c = 18.996(4) ?, β = 97.73(3)°, V = 3014.1(11)?³, ρ = 1.798 g/cm³, Z = 4. The structure of I is built of linear polymeric cations [Ag(C₈H₁₂N₂)] _∞ ⁺ and octahedral anions [PF₆]⁻. Upon the interaction of tetramethylpyrazine molecule with Ag⁺ ions, intersecting polymeric chains [Ag(C₈H₁₂)] _∞ ⁺ (1D polymer) are formed extending in mutually perpendicular diagonal directions. The structure of II consists of layers (2D polymers) formed by fused sixmembered rings. These rings consist of Ag⁺ ions linked by bridging ligands Me₄Pyz. Original Russian Text ? Yu.V. Kokunov, Yu.E. Gorbunova, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 5, pp. 743–750.     

Mixed-ligand complexes [Cd(DMSO)5(NCS)][Cr(NH3)2(NCS)4] · 3DMSO and [Mn(DMSO)4(H2O)2][Cr(NH3)2(NCS)4]2 · 6DMSO · 2H2O: Syntheses and crystal structures

New mixed-ligand coordination compounds[Cd(DMSO)₅(NCS)][Cr(NH₃)₂(NCS)₄] · 3DMSO (I) and [Mn(DMSO)₄(H₂O)₂][Cr(NH₃)₂(NCS)₄]₂ · 6DMSO · 2H₂O (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction analysis. The crystals of compound I are monoclinic, a = 14.5275(7), b = 23.1692(11), c = 14.6969(6) ?, β = 97.057(2)°, V = 4909.4(4) ?³, space group P2₁/c, Z = 4, ρ_calcd = 1.507 g/cm³, R = 0.0556. The crystals of compound II are triclinic, a = 11.7784(3), b = 12.1760(3), c = 13.1922(2) ?, α = 85.5420(10)°, β = 87.9000(10)°, γ = 70.3680(10)°, V = 1776.46(7) ?³, space group P , Z = 1, ρ_calcd = 1.444 g/cm³, R = 0.0350. Original Russian Text ? E.A. Gerasimova, T.V. Utkina, E.V. Peresypkina, A.V. Virovets, T.G. Cherkasova, 2009, published in Zhurnal Neorganicheskoi Khimii, 2009, Vol. 54, No. 5, pp. 751–755.     

A ladder-like 4d–4f complex constructed from edge-sharing rhombus and square of Mo2Yb2 based on [Mo(CN)8]4? and Yb3+ ions as building Blocks

A novel 4d-4f complex, {Cs[Yb(MeOH)₃(DMF)(H₂O)Mo(CN)₈] · H₂O} _n (1) (DMF = N,N′-dimethylformamide) has been synthesized and structurally characterized. The complex 1 is a one-dimensional (1D) infinite chain, which adopts a 1D ladder-like structure motif assembled from an edge-sharing rhombus and square of Mo₂Yb₂ based on the [Mo(CN)₈]⁴⁻ and Yb³⁺ as building blocks. The complex 1 crystallizes in triclinic, space group P1 with a = 9.841(2) b = 10.226(2) ?, c = 13.404(3) ?, α = 82.02(3)°, β = 86.86(3)°, γ = 65.10(3)°, V = 1211.7(4) ?³ and Z = 2.     

Crystal structures of 4-(oxiran-2-ylmethoxy) benzoic acid and 4-acetoxybenzoic acid

Compounds 4-(oxiran-2-ylmethoxy)benzoic acid (2) and 4-acetoxybenzoic acid (4) are synthesized by a new synthetic route and studied by X-ray crystallography. Compound 2 crystallizes in the monoclinic system, P2₁/n space group, a = 5.1209(2) ?, b = 30.3429(16) ?, c = 5.9153(3) ?, β = 96.725(3)°, V = 912.81(8) ?³, Z = 4. Compound 4 crystallizes in the triclinic system, P-1 space group, a = 7.3400(4) ?, b = 8.0819(3) ?, c = 15.6548(9) ?, α = 85.754(3)°, β = 84.268(2)°, γ = 70.023(3)°, V = 867.63(8) ?³, Z = 4. The crystal structure of 2 comprises two crystallographically independent molecules of the compound. In the crystal structures of 2 and 4, pairs of molecules form carboxyl dimers.     

Crystal structure of a new mononuclear complex of Mn(II) with a bbbi ligand (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene)

A new mononuclear complex Mn(bbbi)₂(H₂O)₄(ClO₄)₂·(bbbi)₂·(H₂O)₂ 1 (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene) is synthesized under hydrothermal conditions and characterized by IR spectroscopy, elemental analysis, and single crystal X-ray structural analysis. Crystal data for 1: triclinic, , a = 8.8478(7) ?, b = 15.0550(11) ?, c = 16.4310(12) ?, α = 108.657(7)°, β = 104.044(7)°, Γ = 99.317(7)°, V = 1942.2(3) ?³, Z = 1, final R = 0.0621. Each manganese atom is octahedrally coordinated by four aqua ligands and two nitrogen atoms of two distinct bbbi ligands. The molecule is stabilized by hydrogen bonding and π…π interactions.