Synthesis and X-ray diffraction study of (Cs0.5Ba0.25)[UO2(CH3COO)3] and Ba0.5[UO2(CH3COO)3]

Uranyl triacetate complexes (Cs_0.5Ba_0.25)[UO₂(CH₃COO)₃] (I) and Ba_0.5[UO₂(CH₃COO)₃] (II) are synthesized for the first time and their structures are determined by X-ray diffraction. Both compounds crystallize in the cubic crystal system. The crystal data are as follows: a = 17.3289(7) ?, V = 5203.7(4) ?³, space group I2₁3 and Z = 16 (I); a = 17.0515(8)?, V = 4957.8(4) ?³, space group I $ \bar 4 $ \bar 4 3d, and Z = 16 (II). In I and II, as in all uranyl triacetates studied earlier, the coordination polyhedron of the uranium atom is a hexagonal bipyramid whose vertices are occupied by the oxygen atoms of the uranyl and three acetate groups. The uranium-containing group belongs to the AB ₃⁰¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻) crystal chemical group of uranyl complexes. It was found that compound II is isostructural to the (Rb_0.50Ba_0.25)[UO₂(CH₃COO)₃] studied earlier.     

Crystal structure of R[UO2(CH3COO)3] (R = NH 4+ , K+, or Cs+)

The single crystal structure of NH₄[UO₂(CH₃COO)₃] (I), K[UO₂(CH₃COO)₃] (II), and Cs[UO₂(CH₃COO)₃] (III) is studied by X-ray diffraction. I and II crystallize in the tetragonal crystal system. The crystal data are as follows: a = 13.6985(3) and c = 27.5678(14) ?, V = 5173.1(3) ?³, space group I4₁/a, Z = 16, and R = 0.023 for I; a = 13.8890(5) and c = 26.0839(18) ?, V = 5031.7(4) ?³, space group I4₁/a, Z = 16, and R = 0.037 for II. Crystals III are orthorhombic, a = 18.176(2), b = 13.119(2), and c = 22.088(4) ?, V = 5267(1)?³, space group Pbca, Z = 16, and R = 0.0424. In structures I–III, the uranium-containing structural units are represented by discrete mononuclear [UO₂(CH₃COO)₃]⁻ groups, which belong to the AB ₃⁰¹ (A = UO₂²⁺, B ⁰¹=CH₃COO⁻) crystal chemical group of uranyl complexes.     

Crystal structure of PbUO2(CH3COO)4(H2O)3

Single crystals of PbUO₂(CH₃COO)₄(H₂O)₃ have been investigated by X-ray diffraction (R = 0.029 for 3175 reflections). The structure of this compound is formed by [Pb(CH₃COO)(H₂O)₃]⁺ chains, which are oriented along the [100] axis and limited by one-core complexes [UO2(CH₃COO)₃]⁻. The coordination numbers of the Pb(II) and U(VI) atoms are 8, and the coordination polyhedron of uranium is a hexagonal bipyramid whose vertices contain oxygen atoms of three bidentate cyclic acetate groups and the uranyl group. Taking into account the different crystallographic roles of acetate ions, the crystal-chemical formula of [PbUO₂(CH₃COO)₄(H₂O)₃] chains can be written as AA′B ²¹ B ¹¹(B ⁰¹)₂ M ₃¹, where A = Pb; A′ = UO₂²⁺; M ¹ = H₂O; and B ²¹, B ¹¹, and B ⁰¹ are CH₃COO⁻ groups.     

Crystal structure of M4[(UO2)2C2O4(SO4)2(NCS)2] ( M = K+, Rh+) and K4[(UO2)2C2O4(SeO4)2(NCS)2]

Three heteroacidoligand uranyl complexes M ₄[(UO₂)₂C₂O₄(SO₄)₂(NCS)₂] (M = K⁺ (I), Rb⁺ (II)) and K₄[(UO₂)₂C₂O₄(SeO₄)₂(NCS)₂] (III) have been synthesized and their crystal structure has been determined by X-ray diffraction analysis. The compounds I–III are isostructural and crystallized in the monoclinic system, sp. gr. P2₁/c, Z = 2, a = 11.5548(3) ?, b = 7.0847(1) ?, c = 13.5172(3) ?, β = 93.130(1)°, V = 1104.90(4), R = 0.015 (I); a = 11.5854(9) ?, b = 7.3841(6) ?, c = 13.9072(9) ?, β = 95.754(3)°, V = 1183.74(15), R = 0.0235 (II); a = 11.6715(3) ?, b = 7.1418(2) ?, c = 13.8546(1) ?, β = 93.539(1)°, V = 1152.66(5), R = 0.0126 (III). Basic structural units of these crystals are [(UO₂)₂C₂O₄(XO₄)₂(NCS)₂]⁴⁻ chains, which belong to the crystallochemical group A ₂ K ⁰² B ₂² M ₂¹ (A = UO₂²⁺, K ⁰² = C₂O₂₋⁴, B ² = SO₄²⁻ or SeO₄²⁻, M ¹ = NCS⁻) of uranyl complexes. Uranium-containing chains are connected into a 3D framework via a system of electrostatic interactions with potassium or rubidium cations from outer spheres. Original Russian Text ? I.V. Medrish, E.V. Peresypkina, A.V. Virovets, L.B. Serezhkina, 2008, published in Kristallografiya, 2008, Vol. 53, No. 3, pp. 495–498.     

Synthesis and X-ray structural investigation of K2(H5O2)[UO2(C2O4)2(HSeO3)]

The synthesis and X-ray diffraction analysis of K₂(H₅O₂)[UO₂(C₂O₄)₂(HSeO₃)] single crystals have been performed. This compound crystallizes in the triclinic system with the unit-cell parameters a = 6.7665(4) ?, b = 8.8850(4) ?, c = 12.3147(7) ?, α = 94.73°, β = 90.16°, γ = 92.11°, sp. gr. P[`1]P\bar 1, Z = 2, and R = 0.019. The basic structural units are island [UO₂(C₂O₄)₂(HSeO₃)]³⁻ groups, which belong to the AB ₂⁰¹ M ¹ crystallochemical group of uranyl complexes (A = UO₂²⁺, B ⁰¹ = C₂O₄²⁻, and M ₁ = HSeO₃⁻). Uraniumcontaining complexes are linked through K⁺ and H₅O₂⁺ ions and via a system of hydrogen bonds with the participation of oxonium hydrogen atoms in this structure.     

Synthesis, characterization and crystal structure of [Ni(DACH)2](H2O)2(CH3COO)2 (DACH = 1,4-diazacycloheptane): a three-dimensional (3-D) hydrogen-bonded network embodying 1-D water chains

The mononuclear complex [Ni(DACH)₂](H₂O)₂(CH₃COO)₂ (DACH = 1,4-diazacyclo-heptane) has been synthesized and characterized by IR, UV-Vis, elemental analysis and single crystal X-ray diffraction. The complex crystallizes in monoclinic system, P2₁/n space group with a=7.500(3) ?, b=8.788(3) ?, c=16.429(6) ?, β=93.395(5)°, D _c =1.269 g cm⁻³, μ=0.930 mm⁻¹, V=1080.9(6) ?³, Z=2. The central Ni^II atom is in a square-planar coordination geometry formed by four N atoms of two DACH chelated ligands. The notable feature of the title compound resides in the formation of a three-dimensional network through hydrogen bonds between the [Ni(DACH)₂]²⁺ cations, the CH₃COO⁻ counter anions and the guest water molecules trapped in the crystal lattice.     

Synthesis and structure of {NH2(C2H5)2}2[(UO2)2(C2O4)(CH3COO)4] · 2H2O

Single crystals of the compound {NH₂(C₂H₅)₂}₂[(UO₂)₂C₂O₄(CH₃COO)₄] · 2H₂O (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 9.210(2) ?, b = 14.321(3) ?, c = 12.659(3) ?, β = 105.465(13)°, V = 1609.2(6) ?³, space group P2₁/c, Z = 2, and R = 0.0198. The structural units of crystals I are binuclear groups of the composition [(UO₂)₂C₂O₄(CH₃COO)₄]²⁻ with an island structure, which belong to the crystal-chemical group A ₂ K ⁰² B ₄⁰¹ (A = UO₂²⁺, K ⁰² = C₂O₄²⁻, B ⁰¹ = CH₃COO⁻) of the uranyl complexes, diethylammonium cations, and water molecules. The uranium-containing groups are joined into a three-dimensional framework through electrostatic interactions with diethylammonium cations and a system of hydrogen bonds, which are formed with the participation of the atoms involved in the composition of the water molecules, oxalate ions, acetate ions, and diethylammonium cations. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 65–67.     

Synthesis and Crystal Structure of Copper II and Silver I Complex with 1,4-diazabicyclo[2.2.2]octane[Cu(CBC)2(Dabco)(H2O)] n (1) and [Ag2(HBC)2(Dabco)] n (2)

Two 1D polymeric complex, [Cu(CBC)₂(Dabco)(H₂O)] _n (1) and [Ag₂(HBC)₂(Dabco)] _n (2) have been synthesized and characterized by X-ray single crystal analysis, where CBCH is p-chlorobenzoic acid, HBCH 2 is 2-hydroxybenzoic acid and Dabco is 1,4-diazabicyclo[2.2.2]octane. Complex 1 has been obtained in high yield by hydrothermal synthesis from CuO and CBCH and Dabco, and complex 2 has been obtain by evaporation of the solvent from silver salicylate and Dabco, 1 crystallizes in the orthorhombic space group Pmn2 ₁ with a = 24.3310(5) ?, b = 6.9050(6) ?, c = 5.9980(5) ?, Z = 2, V = 1007.70(4) ?³ and Dx = 1.657 g cm⁻³, 2 crystallizes in the monoclinic space group P2 ₁ /m with a = 10.292(3) ?, b = 6.913(2) ?, c = 14.417(4) ?, β = 95.660(5), Z = 2, V = 1020.8(5) ?³ and Dx = 1.959 g cm⁻³. The final R value is 0.0302 for 1323 measured reflections for 1 and the final R value is 0.0684 for 1545 measured reflections for 2. The atomic arrangement is built by infinite one-dimensional polymeric chain in both complexes. These chains are cross-linked by hydrogen bonds involving the coordinated water molecules to form a two-dimensional framework in complex 1.     

Crystal structure of the UO2SO4 · 2SO(CH3)2 compound: A new type of uranyl sulfate ribbons and the UO2SO4 · 2SO (CH3)2-UO2SO4 · 2CO(NH2)2 morphotropic transition

Single crystals of bis(dimethyl sulfoxide) uranyl sulfate are prepared, and their crystal structure is determined using X-ray diffraction analysis. The crystals are monoclinic, space group P2₁/c, a = 12.9189(8) ?, b = 7.9008(5) ?, c = 12.1405(7) ?, β = 95.677(1)°, R ₁ = 0.0216, wR ₂ = 0.0468 for 2761 unique reflections with F > 2σ(F). The crystal structure of the UO₂SO₄ · 2Dmso compound (where Dmso is dimethyl sulfoxide) is built up of infinite uncharged ribbons of the composition [UO₂SO₄ · 2Dmso]_∞, in which the SO₄ tetrahedron is tridentately coordinated to two uranyl groups. The differences between the structures of the uranyl sulfate compounds formed upon replacement of dimethyl sulfoxide by other molecules are considered. Original Russian Text ? E.V. Alekseev, E.V. Suleĭmanov, E.V. Chuprunov, G.K. Fukin, E.V. Baranov, 2007, published in Kristallografiya, 2007, Vol. 52, No. 2, pp. 283–286.     

Synthesis and crystal structure of oxonitrate complexes Cs[VO2(NO3)2], Cs[MoO2(NO3)3], and MoO2(NO3)2

Cs[VO₂(NO₃)₂] (I), MoO₂(NO₃)₂ (II), and Cs[MoO₂(NO₃)₃] (III) complexes have been obtained by crystallization from nitric solutions and studied by single-crystal X-ray diffraction. Complexes I and II contain infinite zigzag chains of similar compositions, [VO₂(NO₃)₂]⁻ and [MoO₂(NO₃)₂], in which V and Mo atoms form, respectively, trigonal- and pentagonal-bipyramidal polyhedra. Each of these polyhedrons also contains one terminal and two bridge O atoms and two terminal NO₃ groups which are monodentate and bidentate in complexes I and II, respectively. Complex III has an island structure and consists of Cs⁺ cations and [MoO₂(NO₃)₃]⁻ anions, in which the Mo atom is surrounded by one bidentate NO₃ group and two monodentate NO₃ groups and two terminal O atoms in the cis-positions; oxygen atoms form a polyhedron in the form of distorted octahedron. According to the ab initio calculation of isolated MoO₂(NO₃)₂ molecules in the gas phase and solution, the coordination environment of the Mo atom, similarly to the Cr(VI) atom in CrO₂(NO₃)₂, is formed by two bidentate nitrate groups and two terminal O atoms (polyhedron- twisted trigonal prism).     

Solvent-controlled structures. Synthesis and characterization of complexes Cu(L)2(CH3COO)2 and [Cu2(μ-CH3COO)4(L)2](L)2 [L = N-(4′-methylaniline)-4-pyridinecarboxamide]

Two complexes Cu(L)₂(CH₃COO)₂ (1) and [Cu₂(μ-CH₃COO)₄(L)₂](L)₂ (2) (L = N-(4′-methylaniline)-4-pyridinecarboxamide) have been prepared and their crystal structures have been determined by single-crystal X-ray diffraction. The complexes are obtained by using the same raw materials and reaction conditions except solvents. The presence or absence of water controls the coordination mode to give rise to different structures. The structure of 1 has a triclinic space group P-1 with a = 8.381(3) ?, b = 8.545(4) ?, c = 11.357(5) ?, α = 110.654(6)°, β = 102.388(7)°, γ = 97.889(7)°, V = 722.9(5) ?³, and Z = 1. The structure of 2 has a triclinic space group P-1 with a = 9.121(3) ?, b = 9.454(3) ?, c = 17.233(5) ?, α = 77.374(5)°, β = 89.827(6)°, γ = 74.342(6)°, V = 1393.8(7) ?³, and Z = 1. Supramolecular assemblies have also been found via noncovalent bonds such as hydrogen bonds, π–π stacking interactions.     

Synthesis and structure of K2[(UO2)4(O)2(OH)2(C2O4)(CH3COO)2(H2O)2]·2H2O

Single crystals of the compound K₂[(UO₂)₄(O)₂(OH)₂(C₂O₄)(CH₃COO)₂(H₂O)₂]·2H₂O (I) are synthesized, and their structure is investigated using X-ray diffraction. Crystals of compound I belong to the triclinic system with the unit cell parameters a = 7.6777(6) ?, b = 7.9149(7) ?, c = 10.8729(9) ?, α = 72.379(2)°, β = 86.430(3)°, γ = 87.635(2)°, V = 628.33(9) ?³, space group P , Z = 1, and R ₁ = 0.0323. The main structural units of the crystals are [(UO₂)₄(O)₂(OH)₂(C₂O₄)(CH₃COO)₂(H₂O)₂]²⁻ chains, which belong to the crystal-chemical group A ₄ M ₂³ M ₂² K ⁰² B ₂⁰¹ M ₂¹ (A = UO₂²⁺, M ³ = O²⁻, M ² = OH⁻, K ⁰² = C₂O₄²⁻, B ⁰¹ = CH₃COO⁻, M ¹ = H₂O) of the uranyl complexes. The chains are formed by linking the centrosymmetric tetramers of the composition (UO₂)₄(O)₂(OH)₂(CH₃COO)₂(H₂O)₂ via tetradentate bridging oxalate ions. The uranium-containing groups are joined into a three-dimensional framework through the electrostatic interaction with potassium cations and a system of hydrogen bonds, which are formed with the participation of atoms involved in the composition of the water molecules, hydroxide ions, and uranyl ions. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 3, pp. 483–487.     

Crystal structure of bis[diethylenetriamine-N′-(3-propionato)-N, N′,N″,O,O′]dicopper(II) Diperchlorate, [Cu2(4-Dtmp)2](ClO4)2

A complex of copper(II) with the diethylenetriaminemonopripionate ligand [Cu₂(4-Dtmp)₂](ClO₄)₂ (I) is synthesized and characterized using X-ray diffraction. The crystals of compound I are monoclinic, a = 7.740(2) Å, b = 19.199(3) Å, c = 8.449(2) Å, β = 91.61(2)°, Z = 2, and space group P2₁/n. The structural units of crystal I are centrosymmetric dimeric cations and statistically disordered ClO ₄ ⁻ anions. In the cation, the copper atom is coordinated by three N atoms [mean Cu-N, 2.01(1) Å] and two O atoms [Cu-O, 2.134(6) Å and 1.958(7) Å] of the pentadentate bridging-chelate Dtmp ligand, which occupy vertices of the trigonal bipyramid. The binuclear cations are linked via centrosymmetric pairs of hydrogen bonds into ribbons aligned parallel to the a axis of the crystal. The ClO ₄ ⁻ anions form columns in the same direction. In the crystal, the cationic ribbons and anionic columns alternate in a chessboard fashion. __________ Translated from Kristallografiya, Vol. 50, No. 3, 2005, pp. 450–454. Original Russian Text Copyright ? 2005 by Antsyshkina, Sadikov, Poznyak, Sergienko.     

Reactions of triosmium clusters with indole: X-ray structures of [Os3(CO)10(μ-OH)(μ-OMeCO)] and [Os3(μ-H)(CO)10(μ-1, 2-η2-NC8H6)]

Treatment of [Os₃(CO)₁₂] with indole in presence of a methanolic solution of Me₃NO⋅2H₂O at 60^∘C afforded the previously reported compounds [(μ-H)Os₃(CO)₁₀(μ-OMe)] 2, [(μ-H)Os₃(CO)₁₀(μ-OH)] 3 and [Os₃(CO)₁₀(μ-OH)(μ-OMeCO)] 4 in 10, 5 and 20% yields, respectively. The reaction of [Os₃(CO)₁₀(MeCN)₂] with indole at room temperature gave [(μ-H)Os₃(CO)₁₀(μ-1,2-η²-NC₈H₆)] 5 in 40% yield. Compounds 4 and 5 have been characterized by single crystal X-ray diffraction studies. Compound 4 crystallizes in the monoclinic space group P2(1)/c with a = 23.1239(3), b = 9.8087(4), c = 16.9017(6) ?, β = 92.6998(14)^∘, Z = 8 and V = 3829.3(2) ?³ and 5 crystallizes in the monoclinic space group P2(1)/c with a = 9.009(3), b = 9.764(4), c = 24.906(6) ?, β = 93.452(14)^∘, Z = 4 and V = 2186.9(13) ?³. Compound 4 consists of an open cluster of three osmium atoms with the hydroxy and methoxycarbonyl ligands bridging the open Os–Os edge. Compound 5 consists of an isosceles triangle of osmium atoms with one elongated Os–Os edge which is bridged by the hydride and the indolyl ligands.     

Solvothermal Syntheses and Crystal Structures of Neodymium Thiostannates [Nd(dien)3]2[(Sn2S6)Cl2] and [Nd(dien)3]2[(Sn2S6)(SH)2]

Abstract  

Two neodymium thiostannates [Nd(dien)₃]₂[(Sn₂S₆)Cl₂] (1) and [Nd(dien)₃]₂[(Sn₂S₆)(SH)₂] (2) (dien = diethylenetriamine) were synthesized by the reaction of tin and sulfur in the presence of NdCl₃ and Nd₂O₃, respectively under solvothermal conditions. Compounds 1 and 2 crystallize in monoclinic space group P2₁/n. Crystallographic data for 1: a = 11.6722(16), b = 15.119(2), c = 14.1566(19) ?, β = 96.213(3)°, V = 2483.6(6) ?³, Z = 4. For 2: a = 11.7190(14), b = 15.2168(19), c = 14.2209(18) ?, β = 95.775(4)°, V = 2523.1(5) ?³, Z = 4. The nine-coordinate [Nd(trien)₃]³⁺ complex cation formed in situ acts as the counter ion to the [Sn₂S₆]⁴⁻ anion. The [Nd(dien)₃]³⁺, [Sn₂S₆]⁴⁻ and Cl^– (or SH^–) ions form a 3-dimensional network structure through the N–H···S and N–H···Cl hydrogen bonds.     

Synthesis and X-ray structural investigation of (C3N6H7)4(CN3H6)2[UO2(CrO4)4] · 4H2O and (H3O)6[UO2(CrO4)4]

Single crystals of the compounds (C₃N₆ H₇)₄(CN₃H₆)₂[UO₂(CrO₄)₄] · 4H₂O (I) and (H₃O)₆[UO₂(CrO₄)₄] (II) are synthesized, and their structures are investigated using X-ray diffraction. Compound I crystallizes in the triclinic system with the unit cell parameters a = 6.3951(8) ?, b = 10.8187(16) ?, c = 16.9709(18) ?, α = 93.674(4)°, β = 97.127(4)°, γ = 92.020(4)°, space group, P Z = 1, V = 1161.6(3) ?³, and R = 0.0470. Crystals of compound II belong to the monoclinic system with the unit cell parameters a = 14.3158(4) ?, b = 11.7477(3) ?, c = 13.1351(4) ?, β= 105.836(1)°, space group C2/c, Z = 4, V = 2125.2(1) ?³, and R = 0.0213. The uranium-containing structural units of crystals I and II are mononuclear anionic complexes of the composition [UO₂(CrO₄)₄]⁶⁻ with an island structure, which belong to the crystal-chemical group Am ₁⁴ (A = UO₂₊², M ¹ = CrO₂₋⁴) of the uranyl complexes. The [UO₂(CrO₄)₄]⁶⁻ anionic complexes are joined into a three-dimensional framework through the electrostatic interactions with outer-sphere cations and a system of hydrogen bonds. Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 284–290.     

Crystal structure and phase transitions in the new crystals of [(CH3)2NH2]2CuCl4[(CH3)2NH2]Cl

Crystals grown from a solution of dimethylammonium and copper chlorides are studied using electron paramagnetic resonance (EPR) and X-ray diffraction. The dielectric properties of the crystals grown are measured. It is established that the crystals have the composition [(CH₃)₂NH₂]₂CuCl₄[(CH₃)₂NH₂]Cl and, in phase I at room temperature, are described by the orthorhombic space group Pna2₁ with the unit cell parameters a = 11.338 Å, b = 9.981 Å, and c = 15.675 Å. At temperatures of 279 K and 253 K, the crystals undergo jumpwise phase transitions into the incommensurate modulated ferroelectric phase II and commensurate modulated phase III, respectively. __________ Translated from Kristallografiya, Vol. 49, No. 1, 2004, pp. 92–100. Original Russian Text Copyright ? 2004 by Kirpichnikova, Pietraszko, Bednarski, Waplak, Sheleg. Dedicated to the 80th Birthday of L.A. Shuvalov     

A Novel 1:1 Co-Crystal of Bis(1,10-Phenanthroline)(1,10-Phenanthroline-5,6-Dione)Nickel(II) Hexafluorophosphate and Tris(1,10-Phenanthroline)Nickel(II) Hexafluorophosphate Complexes, [Ni(phen)2(phen-dione)] [Ni(phen)3] (PF6)4

Abstract  

The purpose of this study was to investigate whether co-crystals form by simply mixing pure solutions of [Ni(phen)₃](PF₆)₂ and [Ni(phen)₂(phen-dione)](PF₆)₂ where phen is 1,10-phenanthroline and phen-dione is 1,10-phenanthroline-5,6-dione. The 1:1 cocrystal, [Ni(phen)₂(phen-dione)][Ni(phen)₃](PF₆)₄·CH₃CN has been characterized by elemental analysis, IR, paramagnetic NMR, and UV–vis spectroscopies, cyclic voltammetry, and single crystal X-ray structure analysis. The title complex crystallized in triclinic crystal system (z = 2) with space group of Pī, a = 13.201(2) ?, b = 14.782(3) ?, c = 22.294(4) ?, α = 81.575(15)^o, β = 88.756(15)^o, γ = 88.032(15)^o and V = 4300.1(14) ?³. A careful inspection of the packing pattern in the lattice reveals that non-covalent interactions of three different types, viz. C–H···F, C=O···H−C and C−H···π interactions, are active in the lattice. The coordination around the Ni(II) centers is a distorted octahedral, with bite angles of 78.3−79.8^o for the chelating phen and phen-dione ligands. Cyclic voltammetry of this co-crystal shows that the Ni(III/II) couple is quasi-reversible. The effective magnetic moment (μ_eff) of the co-crystal was measured to be 2.87 BM per Ni(II) ion by Evans method. The magnitude of μ_eff is consistent with magnetic moment for octahedral Ni(II) complexes.     

Synthesis and crystal structure of Cu3(Bipy)2(L1)2(L2)2? 4H2O(Bipy = 2,2′-bipyridine, L1 =1-((2-sulfonateethylimino)methyl)-2-naphthol), L2 = 2-hydroxy-1-naphthaldehyde)

The title compound, Cu₃(Bipy)₂(L¹)₂(L²)₂⋅4H₂O, was synthesized in the methanol solution of Bipy and Cu(II) in the presence of 1-((2-sulfonate-ethylimino)-methyl)-2-naphthol (L¹), which was condensation compound of taurine and 2-hydroxy-1-naphthaldehyde. This complex crystallized in the space group P-1 with a = 9.825(2) ?, b = 12.626(2) ?, c = 14.342(3) ?, α = 90.29(1)^∘, β = 100.67(1)^∘, γ = 101.67(2)^∘, and Z = 2. In the trinuclear Cu(II) complex, there are two type Cu atoms which have square and square pyramid geometries, respectively. The Cu–N distances vary from 1.965(3) to 2.000(4) ?, while the Cu–O distances are between 1.896(3) and 2.337(4) ?.     

A Novel Three Dimensional Organic–Inorganic Hybrid Based Porous Phase: Synthesis and Characterization of Reduced Oxovanadium pyromellitate, [VIV2O2(H2O)2(C6H2(COO)4)]

The hydrothermal reaction of a mixture of VOSO₄ · xH₂O, 1,2,4,5-benzenetetracarboxylic acid (pyromellitic acid) and 0.1 M H₂SO₄ for 72 h at 160 °C gives blue needle like crystals of [V^IV ₂O₂(H₂O)₂(C₆H₂(COO)₄)] in 30% yield. The compound has a porous 3-D extended network structure having a rigid architecture which is held together by the multidentate functionalities of 1,2,4,5-benzenetetracarboxylate ligand. Crystal data for the compound: monoclinic space group C 2/c (No:15), a = 11.756(5) ?, b = 9.645(3) ?, c = 11.822(7) ?, β = 107.10(4)°, Z = 8. The compound constitutes the first example of a fully reduced oxovanadium based solid incorporating the organic ligand. This article consists of synthesis, crystal structure and characterization of [V^IV ₂O₂(H₂O)₂(C₆H₂(COO)₄)].