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1.
Jerry L. Atwood Anthony W. Coleman Hongming Zhang Simon G. Bott 《Journal of inclusion phenomena and macrocyclic chemistry》1989,7(2):203-211
The title calixarenes all exist in the solid state as bilayers of anionic calixarenes in the cone configuration. These layers alternate with inorganic regions which contain the cations and the water molecules. The overall structures bear a close resemblance to those found for clay minerals. The sodium salt crystallizes in the triclinic space groupP witha = 10.998(6),b = 13.582(5),c = 14.472(5) Å, = 74.01(3), = 89.09(4), = 86.50(4)°, andZ = 2 forD
calc
= 1.72 g cm–3. Refinement based on 4727 observed reflections led to a conventionalR = 0.050. The potassium salt crystallizes in the triclinic space groupP witha = 11.815(9),b = 13.636(6),c = 14.040(9) Å, = 100.24(5), = 111.86(9), = 95,14(9)°, andZ = 2 forD
calc
= 1.77 g cm–3. Refinement based on 2977 observed reflections led toR = 0.15. The rubidium and cesium salts are isostructural and crystallize in the monoclinic space groupP21/n with parameters for Rb[Cs]a = 11.603(5) [11.704(3)],b = 28.607(8) [29.747(9)],c = 12.512(5) [12.604(4)] Å, = 91.70(4) [91.63(2)°], andZ = 4 forD
calc
= 2.01 [2.24] g cm–3. Refinement based on 1750 [4257] observed reflections led toR = 0.108 [0.075]. Disorder of the cations was observed for the rubidium and cesium salts.
Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82074 (95 pages). 相似文献
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Cafeo G Kohnke FH White AJ Garozzo D Messina A 《Chemistry (Weinheim an der Bergstrasse, Germany)》2007,13(2):649-656
Calix[2]benzo[4]pyrrole m-6 and p-6, each containing two dipyrromethane moieties and two m-phenylene or p-phenylene units, respectively, were readily synthesised from pyrrole, 1,3- and 1,4-bis(1,1'-dimethylhydroxymethyl)benzene, (m-4 and p-4, respectively) and acetone. Macrocycles m-6 and p-6 were tested as receptors for a selection of anions, such as acetate, dihydrogenphosphate and fluoride. The X-ray structures of m-6 and p-6 and those of the complexes m-6F(-), m-6Cl(-) and m-6CH(3)COO(-) (with an nBu(4)N(+) counterion) were also determined. 相似文献
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Na2[Pr4O2]Cl9 and K2[Pr4O2]Cl9, the First Reduced Quaternary Praseodymium Chlorides with Anti-SiS2 Analogous [Pr4/2O] Chains The compounds A2[Pr4O2]Cl9 (A = Na, K) are the first reduced quaternary praseodymium chlorides with anti-SiS2 analogous [Pr4/2O] chains. Synthesis took place in the temperature range from 900 to 600°C in silica-jacketed niobium containers from Pr metal, PrCl3, PrOCl and NaCl (KCl) as starting materials. The X-ray structure analysis of a single crystal of Na2[Pr4O2]Cl9 (monoclinic, P21/m (No. 11), Z = 2, a = 812.2(2) pm, b = 1 134.1(2) pm, c = 937.6(2) pm, β = 106.51(2)°, R = 0.048, Rw = 0.037) exhibits trans-edge connected chains of [Pr4/2O] tetrahedra running along [001] which are connected by surrounding common chloride ions forming layers parallel to (001). These layers are connected by further chloride ions to a three-dimensional network. The sodium ions surrounded by a heavily distorted octahedron of chloride ions are placed between the layers. The X-ray structure analysis of a single crystal of the otherwise isotypic K2[Pr4O2]Cl9 (monoclinic, P21/m (No. 11), Z = 2, a = 820.6(2) pm, b = 1 133.2(4) pm, c = 949.2(3) pm, β = 103.94(2)°, R = 0.073, Rw = 0.054) shows that potassium is coordinated by nine chloride ions. 相似文献
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On the K4[Ag4O4] Relation Single crystals of mainly new oxides A4[M4O4] with M = Cu, A = Li? Rb and M = Ag, A = Na, Rb, Cs have been prepared by “reaction at the metallic substrate” (i.e. the wall) and the crystal structures were refined. For lattice constants and atomic parameters see text. The [M4O4]4? ring is planar only for the M4-part, the positions of the O2? particles deviate in a non systematic way from this plane. Only Li4[Cu4O4] contains an almost planar ring. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated. 相似文献
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K4[Ag404] Structure Type M4[Ag4O4] (M ? Li? Cs) and M4[Cu4O4] (M ? Li? Rb) have been prepared anew; as an example the crystal structure of K4[Ag4O4] has been revised. Contrary to our first report [2, 3] it crystallizes in the space-group I4 m2 with the “ring” [Ag4O4]4? which is not plane, however. Each two O2? (trans-arrangement) are rather (0.02 Å) above and below the plane of the “ring”, respectively. The new parameters are given in the text. The distances, for example d(Ag+·O2?) = 2.058 Å and the Madelung Part of Lattice Energy, MAPLE, are both in a very good agreement with the measurements and calculations, respectively, which have been done on other ternary oxides with silver. 相似文献
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The only dialkylated products obtained in the reaction of tetrahydroxyketocalixarene 2a with MeI/K(2)CO(3) or PhCH(2)Br/K(2)CO(3) are the corresponding proximal (i.e., 1,2) O,O'-dialkyl ethers, in contrast to the parent tetrahydroxycalix[4]arene 1a which affords the distal (1,3) dialkyl ether derivatives. Pairs of geminally alkylated phenoxy groups in the conformationally rigid dibenzylated and tetrabenzylated derivatives are oriented in an anti fashion. These results can be rationalized assuming that the 1,3-alternate arrangement of the rings preferred by 2a is adopted during all the intermediate stages of the alkylation. The NMR spectra (in CDCl(3)) of the monomethyl, dimethyl, trimethyl, and tetramethyl ether derivatives of 2a are in agreement with a 1,3-alternate conformation. 相似文献
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Na5[VO4][O] and Na4[VO4][OH] were obtained from reactions of V2O5 with Na2O and additional NaOH in the latter case, respectively, at 600‐700 °C in sealed Ag containers under Ar atmosphere. The crystal structures have been determined from X‐ray single crystal data. The structures contain isolated [VO4]3? complexes and non‐coordinating oxide and hydroxide anions, respectively. Raman and infrared data is compared for both compounds and hydrogen bonding is discussed for Na4[VO4][OH]. 相似文献
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Ting-Yan Lan Jian-Xin Chen Xiu-Qing Lü Yuan-Biao Huang Zhong-Shui Li Chun-Xia Wei Zhi-Chun Zhang 《Structural chemistry》2006,17(1):35-41
Two Keggin-type phosphododecamolybdate compounds [Cd(2,2′-bpy)3]2[PMoVMoVI
11O40] (1) and [H3PMo12O40]·3(4,4′-bpy)·4H2O (2) (bpy=bipyridine) were prepared by the hydrothermal method for the first time and characterized by elemental analyses, X-ray
single-crystal diffraction, ESR spectra, and IR spectra, showing that compound 1 consists of a mixed valence Keggin polyanion [PMoVMoVI
11O40]4− and two isolated coordinated cations [Cd(2,2′-bpy)3]2+, while compound 2 is an intermolecular compound based on organic substrate 4,4′-bpy and heteropoly acid unit H3PMo12O40. Furthermore, both the compounds show strong photoluminescence properties in the solid state at room temperature. The catalytic
activities of the two compounds were also determined by the oxidation of benzaldehyde to benzoic acid using H2O2 as oxidant in a liquid–solid triphase system. 相似文献
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B. Koji-Prodi
. Rui-Toro J. Kobe 《Acta Crystallographica. Section C, Structural Chemistry》1983,39(9):1248-1253
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Schleid T Strobel S Dorhout PK Nockemann P Binnemans K Hartenbach I 《Inorganic chemistry》2008,47(9):3728-3735
The halide derivatives of yttrium ortho-oxomolybdate YX[MoO 4] (X = F, Cl) both crystallize in the monoclinic system with four formula units per unit cell. YF[MoO 4] exhibits a primitive cell setting (space group P21/ c; a = 519.62(2) pm, b = 1225.14(7) pm, c = 663.30(3) pm, beta = 112.851(4) degrees ), whereas the lattice of YCl[MoO 4] shows face-centering (space group C2/m; a = 1019.02(5) pm, b = 720.67(4) pm, c = 681.50(3) pm, beta = 107.130(4) degrees ). The two compounds each contain crystallographically unique Y (3+) cations, which are found to have a coordination environment of six oxide and two halide anions. In the case of YF[MoO 4], the coordination environment is seen as square antiprisms, and for YCl[MoO 4], trigon-dodecahedra are found. The discrete tetrahedral [MoO 4] (2-) units of the fluoride derivative are exclusively bound by six terminal Y (3+) cations, while those of the chloride compound show a 5-fold coordination around the tetrahedra with one edge-bridging and four terminal Y (3+) cations. The halide anions in each compound exhibit a coordination number of two, building up isolated planar rhombus-shaped units according to [Y 2F 2] (4+) in YF[MoO 4] and [Y 2Cl 2] (4+) in YCl[MoO 4], respectively. Both compounds were synthesized at high temperatures using Y2O3, MoO3, and the corresponding yttrium trihalide in a molar ratio of 1:3:1. Single crystals of both are insensitive to moist air and are found to be coarse shaped and colorless with optical band gaps situated in the near UV around 3.78 eV for the fluoride and 3.82 eV for the chloride derivative. Furthermore, YF[MoO 4] seems to be a suitable material for doping to obtain luminescent materials because the Eu (3+)-doped compound shows an intense red luminescence, which has been spectroscopically investigated. 相似文献
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Three types of heteropolyvanadates, [(C2H5)4N]4[PdV6O18] (1), [(C2H5)4N]4[Cu2V8O24] (2), and [(C6H5)4P]4[Ni4V10O30(OH)2(H2O)6] (3), were synthesized through the reaction between the [VO3]- anion and metal template cations of Pd(II), Cu(II), and Ni(II). The X-ray crystal structures of 1 (a = 29.952(4) A, b = 12.911(2) A, and c = 13.678(2) A, orthorhombic, space group Pca2(1) with Z = 4), 2 (a = 13.740(1) A, b = 22.488(2) A, c = 18.505(2) A, and beta= 94.058(2) degrees , monoclinic, space group P2(1)/n with Z = 4), and 3 (a = 12.333(2) A, b = 16.208(4) A, c = 16.516(3) A, alpha = 112.438(3) degrees , beta = 94.735(3) degrees , and gamma = 104.749(3) degrees , triclinic, space group P with Z = 1) demonstrate that the metal cationic species induced cyclic [VO3](n-)n (n = 6, 8, 10) ring formation and the cations are incorporated in the rings themselves. In the metal inclusion products, the cyclic vanadates act as macrocyclic ligands, in which the metal cationic species act as the templates. The cyclic vanadate is composed of tetrahedral VO4 units that share corners and incorporates a metal cationic species in the center of the molecules. The bowl-shaped complex 1 includes a Pd2+ cation that is coordinated by the oxygen donors of a boatlike hexavanadate ring. The diamagnetic complex 1 was characterized via 51V and 17O NMR spectroscopy. Complex 2 involves an octavanadate ring and two Cu2+, which are located on both sides of the mean plane as defined by the eight oxygen atoms that bridge the vanadium atoms. In the case of complex 3, the di-mu-hydroxo-bridged Ni2+ dimer with capped Ni2+ aqua ions is formed by hydrolysis to form the decavanadate ring, in which two of the tetrahedral vanadate units are not bonded to the Ni2+ core but supported by hydrogen bonds through the aqua-ligand in the capped Ni2+ cation. Complexes 1-3 in solution were clearly identified by their characteristic isotope patterns using ESI-MS studies. 相似文献