Synthesis and crystal structure of hexakis(isothiocyanato)erbium(III) thiocyanate bis(18-crown-6)dipotassium bis[(18-crown-6)ethanolpotassium]

A new complex compound, [K₂(18-crown-6)₂[K(18-crown-6)(EtOH)]₂[Er(NCS)₆](SCN) (I), was synthesized and its crystal structure was studied by X-ray diffraction. In this work, the synthes and X-ray difraction stady of the crystals of a new complex, hexakis (isothiocyanato) erbiu(III) thiocyanate bis(18-crown-6) dipotassium bis(18-crown-6) ethanolpotassium], [K₂(18-crown-6)₂][K(18-crown-6)(ETON)]₂[Er(NCS)₆(SCN)(I)] are described. In crystal I, the alternating [Er(NCS)₆]^3? anions and binuclear complex cation [K(18-crown-6)₂]²⁺ from infinite chains via the F-S bonds, while two complex cations [K(18-crown-6)(ETON)]⁺ and the statistically disordered SCN^? anion between them are linked by the hydragen bonds O-H…S and O-H…N. Complex I contains the host-guest complex cations [K₂(18-crown-6)₂)]²⁺ and [K(18-crown-6)(ETON)]⁺ [1]. The alternating octabedral [Er(NCS)₆]^3? anions and binuclear complex cations [K₂(18-crown-6)₂]²⁺of crystal I form infinite chains via the K-S bonds, while two complex cations [K(18-crown-6)(EtOH)]⁺ and the statistically disordered SCN^? anion lying between them are linked by interionic hydrogen bonds O-H…S and O-H…N. Complex I contains the host-guest complex cations [K₂(18-crown-6)₂]²⁺ and [K(18-crown-6)(EtOH)]⁺ [1].     

Synthesis and crystal structure of bis[(18-crown-6)oxonium]tetrabromomanganese(II)

A new complex compound, bis[(18-crown-6)oxonium]tetrabromomanganese(II), 2[(H₃O)⁺(18-crown-6)]·[MnBr₄]^2–, was prepared and studied by X-ray diffraction to reveal its unusual cubic crystal structure, space group Fd $ \bar 3 A new complex compound, bis[(18-crown-6)oxonium]tetrabromomanganese(II), 2[(H₃O)⁺(18-crown-6)]·[MnBr₄]^2–, was prepared and studied by X-ray diffraction to reveal its unusual cubic crystal structure, space group Fd, a 20.424 ?, and Z 8. In this crystal structure, the complex cation [(H₃O)⁺(18-crown-6)] the point symmetry position and the anion [MnBr₄]²⁻ with the point symmetry 23. The complex cation [(H₃O)⁺(18-crown-6)] has a guest-host structure, and, unlike metal complexes by hydrogen bonds between H₃O⁺ hydrogens and 18-crown-6 oxygens, rather than by coordination bonds. The pyramidal cation H₃O⁺ in this crystal structure is statistically disordered, and the tetrahedral anion [MnBr₄]²⁻ is reorientationally disordered. Original Russian Text ? A.N. Chekhlov, 2008, published in Zhurnal Obshchei Khimii, 2008, vol. 78, No. 10, pp. 1622–1626.     

Tetrakis(isothiocyanato)manganese(II) bis[aqua(18-crown-6)potassium] (18-crown-6)(thiocyanato)potassium

A new complex compound, i.e., tetrakis(isothiocyanato)manganese(II) bis[aqua(18-crown-6)potassium] (18-crown-6)(thiocyanato)potassium, was synthesized and its crystal structure was studied by X-ray diffraction (space group P2₁/m, a = 13.377, b = 14.690, c = 17.499 Å, β = 108.96°, Z = 2) and refined by the least-squares method in anisotropic approximation to R = 0.060 for 4715 independent reflections (CAD-4 automated diffractometer, λMoK _α). In the crystal, infinite chains are formed through the coordination bonds between its components. The monomer fragment of a chain [Mn(NCS)₅K₃(18-crown-6)₃(H₂O)₂] lies in plane m; three of the five SCN^? ligands and one of the two water molecules behave as bridges. The [Mn(NCS)₄]^2? anion has the tetrahedral structure. The coordination polyhedron of each of the three K⁺ cations is a distorted hexagonal bipyramid with six O atom of the corresponding crown ligand in a base. Three 18-crown-6 ligands have standard crown conformation.     

Synthesis and crystal structure of triaqua(18-crown-6)calcium bis(perchlorate) 18-crown-6 monohydrate

A complex [Ca(18C6)(H₂O)₃]²⁺(ClO ₄ ^? · 18C6 · H₂O is synthesized and studied by X-ray diffraction analysis. The structure (space group P2₁/n, a = 11.570 Å, b = 16.024 Å, c = 22.225 Å, β = 98.89°, Z = 4) is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.075 for 5305 independent reflections (CAD4 automated diffractometer, λMoK _α radiation). In the complex cation of the host-guest type, the Ca²⁺ cation lies in the cavity of the 18-crown-6 ligand and is coordinated by all the six O atoms and three O atoms of three water molecules. In a crystal, the alternating complex anions, 18C6 molecules, and water molecules are joined by hydrogen bonds into broad infinite chains along the y axis. The disordered ClO ₄ ^? anions are bonded to these chains on the side through hydrogen bonds.     

Self-assembly of supramolecular complexes of cyanine dyes containing terminal ammonium groups with bis(18-crown-6)stilbene

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双羟甲基-18-冠-6及其衍生物的合成

报道了双羟甲基-18-冠-6及其正丁基、烯丙基、酯基、羧酸基衍生物的合成。所合成的八种新冠醚化合物的结构已经IR、MS、NMR、元素分析证实。     

Synthesis and crystal structure of ammonium (picrate) (dibenzo-18-crown-6)

NH₄(Pic)(DB18C6) (Pic=picrate and DB18C6=dibenzo-18-crown-6), (C₂₆H₃₀N₄O₁₃) FW 606.56, arthorhombic,Pmn2₁,a=26.045(5),b=12.055(3),c=8.982(3) Å,V=2820(1) ų,Z=4,D _c =1.429 g/cm³, CuK, =1.54184 Å, (CuK)=9.5 cm^–1,F(000)=1272,T=298 K. The structure has been refined toR=0.0475 for 2617 unique observed reflections. In the lattice the 1:1 complex exists as a 2:2 dimer in which the crown are coupled through the Pic anions and NH₄ ⁺ cations. The asymmetric unit consists of two independent half crown ethers of which two opposite O atoms are on the mirror plane, two half ammonium cations of which the N and two H atoms are also on the mirror plane while the Pic anion is in a general position. Relative to each other, the corwn ethers are shifted by about 7.3 Å alongb and 1 Å alongc. The 1:1 sandwich of NH₄ with DB18C6 and Pic on dimerisation becomes a club pseudo-sandwich with three phenyl rings on either side of the mirror plane, thus forming a nearly parallel stack with a 3.6 Å inter-ring distance. The NH₄ ions hold the structure; two H atoms on the mirror plane are hydrogen-bonded to the opposite oxygens of the crown located on the purely aliphatic part of the ring (2.10(1), 2.06(3) and 2.26(3), 2.05(1) Å) for the two independent crowns, respectively, while the other two H atoms form mirror-related bifurcated hydrogen bonds with the phenoxide oxygen (1.99(1) and 2.01(1) Å) and theo-nitrogen oxygen (2.44(2) and 2.34(1) Å) of the picrates. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82037 (29 pages)     

Crystal Structure of 1,10-Diazonia-18-crown-6 Bis(hydrogen oxalate) and 1,10-Diazonia-18-crown-6 Oxalate Dihydrate

An X-ray diffraction study has been performed to study the crystal structure of 1,10-diazonia-18-crown-6 bis(hydrogen oxalate) [H₂DA18C6]²⁺·2C₂HO ₄ ^- (I) and 1,10-diazonia-18-crown-6 oxalate dihydrate [H₂DA18C6]²⁺·2C₂O ₄ ^- ·2H₂O (II). Crystals I are triclinic: space group , a = 7.825, b = 7.861, c = 9.349 , = 97.28, = 110.22, = 99.12°, Z = 1. Crystals II are monoclinic: space group P2 ₁ /n, a = 8.783, b = 10.640, c = 10.225 , = 97.04°, Z = 2. The structures of I and II were solved by direct methods and refined by the full-matrix least-squares procedure anisotropically to R = 0.036 (I) and 0.042 (II) for all 2206 (I) and 1990 (II) unique reflections measured (CAD-4 automatic diffractometer, CuK ). In the crystal structures, the ionic complexes (salts) I and II are not individual guest–host complex molecules but are parts of complex (infinite in two directions) three-dimensional layers of H-bonded molecular anions and DA18C6 dications (and water molecules in II). In structures I and II, the centrosymmetric DA18C6 dications have different conformations: two-angle in I and four-angle in II. The unusual four-angle conformation of the DA18C6 dication was found for the first time.     

Bis[(18-crown-6)potassium] tetrakis(isothiocyanato)zinc(II): synthesis and crystal structure

A new complex, bis[(18-crown-6)potassium] tetrakis(isothiocyanato)zinc(II) [[K(18-crown-6)₂] [Zn(NCS)₄]] (I), is synthesized. Its crystal structure is studied using X-ray diffraction analysis (space group Pna2₁, a = 17.604 Å, b = 14.190 Å, c = 17.625 Å, Z = 4) by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.099 for all 3994 measured independent reflections (CAD4 automated diffractiometer, λMoK _α radiation).     

Preparation and disordered crystal structure of (18-crown-6)ammonium isothiocyanate hemihydrate

A crystalline complex salt, (18-crown-6)ammonium isothiocyanate hemihydrate [NH ₄ ⁺ (18C6)]·SCN^?·0.5H₂O, was prepared and studied by single-crystal X-ray diffraction. The crystal structure of this salt is highly disordered: Almost all the constituents (except the water molecule) are disordered over two different orientations: major and less occupied or weakly occupied. The geometric parameters (bond lengths, bond angles, etc.) of the molecular and ionic constituents of the salt were determined with reasonable accuracy, and the crystal packing was elucidated. The sale forms in the crystal a complex tetrahedral supramolecular hydrogen-bonded structure consisting of one water molecule, two complex cations [NH ₄ ⁺ (18C6)], and two SCN^? anions.