Synthesis, properties, and molecular and crystal structure of hexaaquacopper(IV) bis(diaquacuprato-μ3-trihydroxyglutarato)germanate(IV) dihydrate [Cu(H2O)6][Ge(μ3-Thgl)2{Cu(H2O)2}2] · 2H2O

A procedure for the synthesis of the heteropolymetallic germanium(IV) and copper(II) complex with trihydroxyglutaric acid (H₅Thgl) [Cu(H₂O)₆][Ge(μ₃-Thgl)₂{Cu(H₂O)₂}₂] · 2H₂O (I) was developed and the complex was isolated for the first time in the solid state. The product was characterized by elemental analysis, powder X-ray diffraction, thermogravimetry, and IR spectroscopy. Compound I was studied by X-ray crystallography. The crystals are monoclinic, a = 10.216(2)?, b = 12.272(3)?, c = 10.679(2)?, β = 93.13(3)°, V = 1336.9(5)?³, Z = 2, space group P2₁/n, R1 = 0.0261 for 3616 reflections with I > 2σ(I). Compound I is composed of bimetallic [Ge(μ₃-Thgl)₂{Cu(H₂O)₂}₂]²⁻ anions, [Cu(H₂O)₆]²⁺ cations, and water molecules of crystallization. In the centrosymmetric trinuclear complex anion, the Ge(1) atom is bound by two fully deprotonated bridging ligands to two Cu atoms. The Ge(1) atom is coordinated at distorted octahedron vertices by six hydroxyl oxygen atoms of two Thgl⁵⁻ ligands (average Ge(1)-O distance is 1.8874(13)?). The Cu coordination polyhedron in the anion is an extended square pyramid (4 + 1) formed by the bridging hydroxyl oxygen atom (Cu(1)-O(3), 2.0039(12) ?), two carboxyl oxygen atoms (average CU(1)-O distance is 1.9674(14)?) of two Thgl⁵⁻ ligands, and two water oxygen atoms in equatorial and axial positions (Cu(1)-O, 1.9761(13) and 2.3643(14)?, respectively). In the centrosymmetric cation, the Cu coordination polyhedron is an extended square bipyramid (4 + 2). The equatorial Cu-O bond length is 1.9428(14) ? (average), the axial Cu-O bond is elongated to 2.5151(14)?. The cations and anions are combined by H-bonds.     

Crystal structure of metal-organic coordination polymers [Cu(bpy)2(H2O)2](NO3)2·4.5C2H5OH and [Cu2(bpy)(H2O)(L-pha)2](NO3)2·H2O

Two metal-organic coordination polymers [Cu(bpy)₂(H₂O)₂](NO₃)₂·4.5C₂H₅OH (1) and [Cu₂(bpy)(H₂O)(L-pha) ₂](NO₃)₂·H₂O (2) (L-Hpha = L-phenylalanine, bpy = 4,4′-bipyridyl) are prepared by slow evaporation of an aqueous alcoholic solution of copper nitrate, L-phenylalanine, and 4,4′-bipyridyl. The structure and composition of the obtained compounds are determined by single crystal XRD. The framework of compound 1 is positively charged and forms two types of intersecting channels. Compound 2 is a homochiral metal-organic coordination polymer whose structure contains L-phenylalanine anions.     

Crystal and Molecular Structures of Barium cis(NO2)-trans(N)-Bis(glycinato)dinitrocobaltate(III) Hydrate [Ba(H2O)4][Co(Gly)2(NO2)2]2 · 1.43H2O

Crystals of [Ba(H₂O)₄][Co(Gly)₂(NO₂)₂]₂ · 1.43H₂O (a=8.1917(6) , b=8.4440(4) , c=19.444(1) , =98.189(9)°, Z=2, space group P2/n) contain infinite strips of alternating axially symmetric [Ba(H₂O)₄]²⁺ fragments and two dinitro-bis(glycinato)cobaltate(III) ions. In addition to four oxygen atoms of water molecules, the nearest environment of Ba includes six oxygen atoms of the carboxyl groups of four anions, two of which are also coordinated by the cobalt atoms (Ba-O, 2.77–3.01 ). The nitrite ions do not interact with the Ba²⁺ ions.__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 5, 2005, pp. 329–332.Original Russian Text Copyright © 2005 by Zabel, Poznyak, Pawlowski.     

X-ray structure of KCs[Pd(NO3)4]·0.5H2O

A new Pd nitrate complex KCs[Pd(NO₃)₄]·0.5H₂O is synthetized. Its crystal structure contains isolated complex anions [Pd(NO₃)₄]²⁻, cations K⁺, Cs⁺, and crystallization water. Square-planar coordination around Pd is achieved by oxygen atoms of monodentate nitrate ligands. The coordinated nitrate ligands are all oriented in the same way, in a “basket”-like arrangement. The coordination around Pd is completed to 4+1 by forming Pd...Pd contacts of 3.564 ?. Original Russian Text Copyright ? 2009 by S. P. Khranenko, I. A. Baidina, N. V. Kuratieva, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 173–176, January–February, 2009.     

Hydrothermal synthesis and crystal structure of [Zn(pytpy)2][NO3]2·2H2O

The title compound, [Zn(pytpy)₂][NO₃]₂·2H₂O (pytpy = 4′-(4-pyridyl)-2,2′: 6′,2″-terpyridine), has been synthesized by the reaction of Zn(NO₃)₂·6H₂O with pytpy, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to tetragonal space group P4₃ with a = 0.90873(8) nm, b = 0.90873(8) nm, c = 4.4741(6) nm, V = 3.6946(7) nm³, Z = 4, D _c = 1.521 g/cm⁻³, μ = 0.736 mm⁻¹, F(000) = 1744, R = 0.0871, wR = 0.1302 for 5553 observed reflections with I > 2σ(I). X-ray analysis has revealed that the Zn^II ion is surrounded by six N atoms from two pytpy ligands leading to a distorted octahedral geometry. In the crystal structure there are numerous strong intermolecular and intramolecular H-bonds and π-π interactions.     

Synthesis and structures of nine-coordinate K[SmIII (Edta)(H2O)3] · 2H2O and Ten-Coordinate K2[SmIII(Pdta)(H2O)2]2 · 4.5H2O complexes

The title complexes, K[Sm^III(Edta)(H₂O)₃] · 2H₂O(I)(H₄Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid) and K₂[Sm^III(Pdta)(H₂O)₂]₂ · 4.5H₂O (II) (H₄Pdta = propylenediamine-N,N,N′,N′-tetraacetic acid), were prepared and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. Complex I has a mononuclear structure, and the Sm³⁺ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.84(5), b = 35.58(9), c = 12.15(3) ?, V = 8580(38) ?³, Z = 16, ρ _c = 1.925 g/cm³, μ = 3.010 mm⁻¹, F(000) = 4976, R = 0.0252, and wR = 0.0560 for 3510 observed reflections with I ≥ 2σ(I). Complex II has a binuclear structure and the Sm³⁺ ion is ten-coordinated by a Pdta ligand, two oxygen atoms from a carboxylic group of adjacent Pdta ligand and two water molecules, yielding a distorted bicapped square antiprismatic prism. The complex crystallizes in the triclinic crystal system with space group P $ \bar 1 $ \bar 1 . The crystal data are as follows: a = 8.9523(15), b = 10.7106(15), c = 11.6900(19) ?, α = 80.613(5)°, β = 80.397(5)°, γ = 76.530(4)°, V = 1065.7(3) ?³, Z = 1, ρc = 1.970 g/cm³, μ = 2.532 mm⁻¹, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I).     

Synthesis and crystal structure of [Fe4O2(H2O)10(C5H5NCOO)4](NO3)8 · 2H2O

Crystals of the tetranuclear complex [Fe₄O₂(H₂O)₁₀(C₅H₅NCOO)₄](NO₃)₈ · 2H₂O are obtained by the slow evaporation of an aqueous solution of iron(III) nitrate and isonicotinic acid. According to the X-ray diffraction data, four metal atoms lie in the same plane and together with two μ₃-O oxygen atoms form the fragment [Fe₄(μ₃-O)₂]¹⁰⁺. The [Fe₄O₂(H₂O)₁₀(C₅H₅NCOO)₄]⁸⁺ cation has been obtained and structurally characterized for the first time.     

Heat capacity and thermodynamical properties of the crystal of [RE2(Glu)2(H2O)8](ClO4)4·H2O (RE = Nd, Eu, Dy)

Thermodynamical data of rare earth complexes with amino acid are important for engineering chemistry and fundamental chemistry. However, they have rarely been reported. In this work, a series of crystalline complexes of rare earth perchlorate coordinated with glutamic acid have been synthesized in water medium, and their thermodynamical data, including the heat capacity in low temperature range and the standard enthalpy of formation, were determined. These complexes were identified to be [RE₂(Glu)₂(H₂O)₈](ClO₄)₄·H₂O (RE = Nd, Eu, Dy) by using thermogravimetric analysis (TG), differential thermal analysis (DTA), and chemical and elementary analyses. Their purity has been determined. No melting points were observed for all the three complexes. The heat capacity of the complexes was measured by an adiabatic calorimeter from 79 to 370 K. Abnormal heat capacity values were detected for two of the complexes and the decomposition range of one complex was found. The temperature, enthalpy change and entropy change of the decomposition processes of the three complexes were calculated. The polynomial equations of heat capacity in the experimental temperature range have been obtained by least squares fitting. The standard enthalpy of formation was determined by an isoperibol reaction calorimeter at 298.15 K. Supported by the Research Fund of Beijing Institute of Petro-Chemical Technology (N06-06)     

trans-dinitro- and trans-dinitratoruthenium complexes [RuNO(NH3)2(NO2)2(OH)] and [RuNO(NH3)2(H2O)(NO3)2]NO3·H2O

Methods for the synthesis of trans-diammino complexes [RuNO(NH₃)₂(NO₂)₂(OH)] (I) and [RuNO(NH₃)₂(H₂O)(NO₃)₂](NO₃)·H₂O (II) are suggested. The compounds were studied by IR spectroscopy and X-ray phase and X-ray structural analyses. Crystal data: space group P-1; a = 6.2328(2) ?, b = 11.0488(3) ?, c = 11.0981(4) ?, α = 71.942(1)°, β = 83.291(1)°, γ = 86.877(1)° (I); space group P2₁; a = 6.6290(2) ?, b = 13.4389(5) ?, c = 7.0180(2) ?, β 114.281(1)° (II). Complex II readily lost some part of crystal water on storage in open air. Original Russian Text Copyright ? 2009 by M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, and V. A. Vorob’yov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 341–348, March–April, 2009.     

Formation of Co nanoparticles in the process of thermal decomposition of the cobalt complex with hexamethylenetetramine (NO3)2Co(H2O)6(HMTA)2 · 4(H2O)

The thermal decomposition of the cobalt complex with hexamethylenetetramine (NO₃)₂Co(H₂O)₆(HMTA)₂ · 4(H₂O) was studied by the methods of differential thermal analysis, thermogravimetry, mass spectrometry, X-ray diffraction analysis, and by the magnetic method. It was established that the thermal decomposition of the complex in a current of an inert gas is accompanied by a pronounced exothermic process and formation of Co nanoparticles. It was shown that the kinetics of this process and the chemical nature of the decomposition products depend on the initial density of the sample under study.     

Structural determination of new eight-coordinate NH4[EuIII(Cydta)(H2O)2]·4.5H2O and K2[Eu 2III (pdta)2(H2O)2]·6H2O complexes

The NH₄[Eu^III(Cydta)(H₂O)₂]·4.5H₂O (I) (H₄Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K₂[Eu₂^III(pdta)₂(H₂O)₂]·6H₂O (II) (H₄pdta = propylenediamine-N,N,N′,N′-tetraacetic acid) complexes are prepared by heat-refluxing and acidity-adjusting methods respectively, and their composition and structures are determined by elemental analyses and single crystal X-ray diffraction techniques. The complex I has a mononuclear structure, crystallizes in the triclinic crystal system with the P[`1]P\bar 1 space group; the central Eu^III ion is eight-coordinated by a hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.653(4) ?, b = 10.041(4) ?, c = 14.405(6) ?, α = 88.469(6)°, β = 74.892(6)°, γ = 88.256(7)°, V = 1207.5(9) ?³, Z = 1, D _c = 1.731 g/cm³, μ = 2.669 mm⁻¹, F(000) = 638, R = 0.0257, and wR = 0.0667 for 3807 observed reflections with I ≥ 2σ(I). The EuN₂O₆ part in the [Eu^III(Cydta)(H₂O)₂]⁻ complex anion forms a pseudo-square antiprismatic polyhedron. The complex II is eight-coordinate as well; it is a binuclear structure that crystallizes in the monoclinic crystal system with the C ₂/c space group; half of the central Eu^III ion is coordinated by two nitrogen atoms from one hexadentate pdta ligand and six oxygen atoms from the same pdta ligand, one water molecule and carboxylic group from the neighboring pdta ligand respectively. The crystal data are as follows: a = 19.866(3) ?, b = 9.1017(12) ?, c = 21.010(3) ?, β = 104.972(2)°, V = 3670.1(9) ?³, Z = 8, D _c = 2.046 g/cm³, μ = 3.710 mm⁻¹, F(000) = 2240, R = 0.0213 and wR = 0.0460 for 4183 observed reflections with I ≥ 2σ(I). Otherwise, the two EuN₂O₆ parts in the [Eu₂^III(pdta)₂(H₂O)₂]²⁻ complex anion form a pseudo-square antiprismatic polyhedron.     

Hydrothermal synthesis and crystal structures of new uranyl oxalate hydroxides: α- and β-[(UO2)2(C2O4)(OH)2(H2O)2] and [(UO2)2(C2O4)(OH)2(H2O)2]·H2O

Two modifications of the new uranyl oxalate hydroxide dihydrate [UO₂)₂(C₂O₄)(OH)₂(H₂O)₂] (1 and 2) and one form of the new uranyl oxalate hydroxide trihydrate [(UO₂)₂(C₂O₄)(OH)₂(H₂O)₂]·H₂O (3) were synthesized by hydrothermal methods and their structures determined from single-crystal X-ray diffraction data. The crystal structures were refined by full-matrix least-squares methods to agreement indices R(wR)=0.0372(0.0842) and 0.0267(0.0671) calculated for 1096 and 1167 unique observed reflections (I>2σ(I)), for α (1) and β (2) forms, respectively and to R(wR)=0.0301(0.0737) calculated for 2471 unique observed reflections (I>2σ(I)), for 3. The α-form of the dihydrate is triclinic, space group , Z=1, a=6.097(2), b=5.548(2), , α=89.353(5), β=94.387(5), γ=97.646(5)°, , β-form is monoclinic, space group C2/c, Z=4, a=12.180(3), b=8.223(2), , β=95.817(4), . The trihydrate is monoclinic, space group P2₁/c, Z=4, a=5.5095(12), b=15.195(3), , β=93.927(3), . In the three structures, the coordination of uranium atom is a pentagonal bipyramid composed of dioxo UO₂²⁺ cation perpendicular to five equatorial oxygen atoms belonging to one bidentate oxalate ion, one water molecule and two hydroxyl ions in trans configuration in 2 and in cis configuration in 1 and 3. The UO₇ polyhedra are linked through hydroxyl oxygen atoms to form different structural building units, dimers [U₂O₁₀] obtained by edge-sharing in 1, chains [UO₆]_∞ and tetramers [U₄O₂₆] built by corner-sharing in 2 and 3, respectively. These units are further connected by oxalate entities that act as bis-bidentate to form one-dimensional chains in 1 and bi-dimensional network in 2 and 3. These chains or layers are connected in frameworks by hydrogen-bond arrays.     

Synthesis, crystal structure and electrochemistry properties of [Cd(phen)(H2O)4](ClO4)Cl · H2O

A new inorganic-organic hybrid solid, [Cd(phen)(H₂O)₄](ClO₄)Cl · H₂O (phen = 1,10-Phenanthroline), has been synthesized under reflux conditions and characterized by single-crystal X-ray diffractions, ICP analysis, elemental analysis and electrical analysis. The compound crystallizes in the orthorhombic, space group a = 0.88361(10) ?, b = 1.8492(2) ?, c = 2.2157(2) nm, Z = 8, Dc = 1.899 g cm⁻³. Furthermore, electrical studies for complex have also been reported in this article.     

Synthesis and crystal structure of one-dimensional heterotrimetallic coordination polymer {[(Dipic)2Cu]4 · Mg(H2O)2Na4(H2O)14}n · nNa2(H2O)10 · 2nCH3OH

A novel heterotrimetallic complex {[(Dipic)₂Cu]₄ · Mg(H₂O)₂Na₄(H₂O)_{14 n} · nNa₂(H₂O)₁₀ · 2nCH₃OH (H₂Dipic = pyridine-2,6-dicarboxylic acid) has been synthesized and structurally determined by X-ray diffraction method. The compound crystallizes in the triclinic system, space group P [`1]\bar 1, with a = 13.5523(13), b = 14.1859(13), c = 14.3213(14) ?, α = 62.6160(10)°, β = 68.2540(10)°, γ = 89.7110(10)°, V = 2224.7(4)?³, F(000) = 1144, M _r = 2237.70, Z = 1, ρ _c = 1.670 g cm⁻³, μ = 1.095 mm⁻¹, final R = 0.0507, wR = 0.1418 for 8042 independent reflections with R _int = 0.0228. According to the structure determination, the complex is composed of novel one-dimensional (1D) alternating chains, dinuclear Na(I) units, and lattice methanol molecules. The infinite 1D chain structure is built up with many of polymeric [(Dipic)₂Cu]₄ · Mg(H₂O)₂Na₄(H₂O)₁₄ units, which consists of four six-coordinated Cu²⁺ ions, one six-coordinated Mg²⁺ ion, two five-coordinated Na⁺ ions, and two six-coordinated Na⁺ ions. The 1D alternating chains are linked with another dinuclear Na(I) units by extensive hydrogen bonds to form a three-dimensional (3D) supramolecular structure in which uncoordinated methanol molecules act as space filling particles.     

Conformational rearrangement of 18-crown-6 upon the formation of aquanitratouranyl complexes: The refinement of crystal and molecular structures for [UO2(NO3)2(H2O)2] · 2H2O · 18C6

Comparing the geometry of [UO₂(NO₃)₂(H₂O)₂] · 2H₂O · 18C6 (18C6 = C₁₂H₂₄O₆) and IR spectroscopic data, we propose correlations between the conformation of an ethylene oxide unit of 18-crown-6 and the conformation-sensitive frequency in the IR spectrum. Spectral conformational analysis verifies the composition of the 18-crown-6 conformer in the [UO₂(NO₃)₂(H₂O)₂] · 18C6 complex whose structure is known. The distribution character of hydrogen bonds that retain crown ether molecules in aquanitratouranyl complexes is shown to influence the conformational uniformity of ethylene oxide units of the macrocycle.     

Structure and synthesis of nitrosoruthenium trans -diammines [Ru(NO)(NH3)2Cl3] and [Ru(NO)(NH3)2(H2O)Cl2]Cl·H2O

A DTA study of thermal decomposition of (NH₄)₂[Ru(NO)Cl₅] in helium atmosphere has been carried out, a synthetic procedure for preparation of the trans-diammine complex mer-[Ru(NO)(NH₃)₂Cl₃] (I) with yield ∼70% has been developed. On re-crystallization of I from aqueous solution a trans-aquanitroso complex [Ru(NO)(NH₃)₂Cl₂(H2O)]Cl·H₂O (II) has been isolated. The structures of the compounds have been determined by single crystal X-ray diffraction: space group Pbcn, a = 6.607(1) ? b = 11.255(2) ? c = 9.878(2) ? (I) and space group Ima2, a = 8.3032(3) ?, b = 8.0890(2) ?, c = 15.9192(5) ? II). Original Russian Text Copyright ? 2008 by M. A. Il’in, V. A. Emel’yanov, and I. A. Baidina __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 6, pp. 1128–1136, November–December, 2008.     

X-ray study of M(Aet)2·8H2O (M = Sr, Ba) and the crystal structure of [Sr(Aet)(OH2)5](Aet)·3H2O

An X-ray phase and X-ray structural analysis of M(Aet)₂-8H₂O compounds, where M(II) = Sr and Ba; (Aet)^- = (C₁₀H₁₁N₄O₂S₂) is the sulfaethiodole (2-(para-aminobenzene-sulfamido)-5-ethyl-1,3,4-thiadiazole) anion is carried out. Symmetry and unit cell parameters of Sr(Aet)₂•8H₂O and Ba(Aet)₂-8H₂O are found: P2₁/c, Z= 4, a = 10.390(2) ?, b= 14.609(3) ?, c = 21.931(5) ?, β = 92.42(2)°, R = 0.041; and P2₁/c, Z= 4, a = 9.793(2) ?, b = 15.408(4) ?, c = 22.553(6) ?, β = 94.98(2)° respectively. The considered compounds are isostructural. The structure of Sr(Aet)₂-8H₂O is fully studied; the crystals of the compound are composed of the complex centrosymmetric dimeric [(H₂O)5Sr(Aet)₂Sr(OH₂)₅]²⁺ cations, (Aet)^- anions, and water molecules; the independent part of the structural formula of the compound is [Sr(Aet)(OH₂)₅](Aet)•3H₂O. The sulfaethiodole anion is coordinated to the complexing metal atom by oxygen and nitrogen atoms with the formation of a four-membered ring.     

Crystal and molecular structure of tetraaquabarium Di-μ-tartrato-di-μ-hydroxodigermanate(IV) pentahydrate [Ba(H2O)4][Ge2(μ-Tart)2(μ-OH)2] · 5H2O

A new heteronuclear germanium barium complex with D-tartaric acid [Ba(H₂O)₄][Ge₂(μ-Tart)₂(μ-OH)₂]·5H₂O (I) (H₄Tart is tartaric acid) was synthesized. The identity of compound I and its com- position were determined by elemental analysis and X-ray diffraction. The thermal stability of the compound was studied; the coordination centers of the ligand were found from IR spectroscopy. The structure of I was determined by X-ray crystallography. Crystals I are tetragonal: a = 8.5033(2) ?, c = 30.9393(11) ?, V = 2237.10(11) ?³, Z = 4, space group P4₁, R1 = 0.0301 based on 4215 reflections with I > 2σ(I). In crystals I, neutral [Ge₂(μ-Tart)₂] dimers are linked in pairs by double hydroxyl bridges to form {[Ge₂(μ-Tart)₂(μ-OH)₂]²⁻}_∞ polymeric chains. Hydrated Ba²⁺ cations and crystal water molecules are in between the anionic chains. Polymeric complex anions, hydrated barium cations, and H₂O molecules are bound by a system of hydrogen bonds to form a framework.     

Synthesis and crystal structure of [Na2(μ-H2O)(H2O)CB[5]]Cl2 · 6H2O, [Na3(μ-H2O)4(H2O)4(CNPy@CB[6])]Cl3 · 8H2O, and [Rb2(μ-H2O)2(CNPy@CB[6])]Cl · 8H2O

The chain coordination polymers [Na₂(μ-H₂O)(H₂O)CB[5]]Cl₂ · 6H₂O (I), [Na₃(μ-H₂O)₄(H₂O)₄(CNPy@CB[6])]Cl₃ · 8H₂O (II), and [Rb₂(μ-H₂O)₂(CNPy@CB[6])]Cl₂ · 8H₂O (III) were prepared by heating (110°C) of a mixture of sodium or rubidium chloride, cucurbit[n]uril (CB[n], where n = 5, 6), 4-cyanopyridine, and water. According to X-ray diffraction data, binding of polynuclear cations with CB[n] in I–III occurs through coordination of the oxygen atoms of the cucurbit[n]uril portals to alkali metal atoms. Complexes I–III of the above composition isolated to the solid phase as supramolecular compounds with CB[n] were structurally characterized for the first time.