Bis(benzo-15-crown-5-κ5 O)strontium bis­(triiodide)

The title compound, [Sr(C14H20O5)2](I3)2, obtained by slow evaporation of an ethanol/dichloro­methane solution (1:1) of SrCl2, benzo-15-crown-5 and I2, is built of sandwich-like [Sr(benzo-15-crown-5)2]2+ cations and isolated linear I3 − anions which are arranged in alternating layers parallel to (010). The triiodide anions are located in general positions, whereas the cations are located on centres of inversion

Transition-Metal(II)-Crown-Ether-Polyiodides

The crown-ethers 12-crown-4 (12c4) and benzo-12-crown-4 (b12c4) encapsulate divalent manganese, iron, cobalt, and nickel cations building large sandwich-type dications with square-antiprismatic coordination polyhedra; benzo-15-crown-5 (b15c5) forms in-cavity complexes with six-plus-one coordinate Mn(11) and Co(II). The anions are a variety of polyiodides, I-3(-), I-5(-), I-7(-), I-12(2-), I-16(2-), and I-18(4-). The crystal. structures of 12 new compounds have been determined, 8 of which contain 12-crown-4: [Mn(12c4)(2)](I-3)(2)(12c4) (1) and [Co(12c4)(2)](I-3)(2)(12c4) (2) are isotypic (monoclinic, C2/c, No. IS) and contain isolated triiodide anions. Isotypic [Mn(12c4)(2)](I-5)(2) (3) and [Ni(12c4)(2)] (I-5)(2) (4) (monoclinic, Cm, No. 8) feature V/L-shaped I-5(-) anions which are connected to zigzag chains. The hexadecaiodides, built of nonaiodide and heptaiodide subunits, in the isotypic compounds [Mn(12c4)(2)](I-16) (5), [Fe(12c4)(2)](I-16) (6), [Co(12c4)(2))(I-16) (7) (orthorhombic, Pna2(1), No. 33) exhibit a new structural motif for I-16(2-) anions. The elusive octadecaiodide I-18(4-) in [Co(12c4)(2)](2)(I-18) (8) (monoclinic, C2/c, No 15) consists of a linear pentaiodide to which iodine and triiodide are attached Analogous reactions with benzo-12-crown-4 yielded the pentaiodides [Mn(b12c4)(2)](I-5)(2) (9) and [Co(b12c4)(2)](I-5)(2) ( 10). 9 features a trans-pentaiodide,chain to which an additional pentaiodide is connected; it also contains an isolated pentaiodide anion. The crystal structure of 10 contains isolated V/L-shaped pentaiodide anions exclusively. The anionic parts in [Co(b15c5)(2)(MeCN)(H2O)] (I-7)(2) (11) (monoclinic, Cc, No. 9) and [Mn(b15c5)(2)(H2O)(2)](I-12) (12) (monoclinic, P2(1)/c, No. 14) are determined by polymeric pyramidal heptaiodides in 11 and by a two-dimensional network of dodecaiodide anions with twisted sawhorse geometry in 12

Iodine Molecules Included in the Structure of Dibenzo-24-Crown-8, (I-2)@(db24c8)

A reaction of YI3, dibenzo-24-crown-8 and iodine in ethanol yielded, as a by-product, red single crystals of (I-2)@(db24c8). In the triclinic crystal, P-1, a = 485.0(1), b = 1203.7(3), c = 1280.4(2) pm, alpha = 64.56(2)degrees, beta = 86.82(2)degrees, gamma = 83.89(2)degrees, V = 671.1(2) x 10(6) pm(3), Z = 1, R-1= 0.0301 for 1965 reflections with I-0 > 2 sigma(I-0), iodine molecules with an I-I distance of 268.39(7) pm, slightly longer than in the gas phase, are included in a matrix of db24c8 molecules

Redetermination of tantalum pentabromide, (TaBr5)(2)

Crystals of di-mu-bromido-bis[tetrabromidotantalum(+V)], (+TaBr5)(2), were obtained by recrystallization at 773 K. A first crystal structure study of (+TaBr5)(2) was reported by Rolsten [J. Am. Chem. Soc. (1958), 80, 2952-2953], who analysed the powder diffraction pattern and came to the conclusion that it crystallizes isotypically with (NbBr5)(2) in a primitive orthorhombic cell. These findings are not in agreement with our current results of a monoclinic C-centred structure. (TaBr5)(2) is isotypic with alpha-(+NbCl5)(2). The crystal structure contains [TaBr6] octahedra sharing common edges forming [TaBr5](2) dimers. Two crystallographically independent dimers with symmetries m and 2/m and Ta center dot center dot center dot Ta distances of 4.1574 (11) and 4.1551 (15) angstrom, respectively, are present in the structure

Ru11Lu20, a New Intermetallic Compound with Eight- to Ten-Coordinate Ruthenium Atoms

The new intermetallic compound Ru11Lu20 was obtained as black single crystals during an attempted comproportionation reaction of lutetium(III) chloride, LuCl3, with metallic lutetium in the presence of ruthenium metal at 950 °C. Ru11Lu20 crystallizes with the trigonal space group R-3, Z = 6, a = 1255.1(1), c = 2973.0(4) pm, R1 for all data: 0.0380. Ruthenium atoms center eight-, nine- and ten-vertex polyhedra of lutetium atoms which are connected in a complicated manner to a three-dimensional network

Silver Compounds in Synthetic Chemistry. Part 8. Complexes of Perfluoroorgano Silver(I) Derivatives with 4-Dimethylaminopyridine (DMAP)

Attempted syntheses of AgRf center dot DMAP were performed using the established route starting from AgF and Me3SiRf (R-f = CF3, C2F5, C6F5) followed by the addition of DMAP. Unexpectedly, reactions with perfluoroalkylsilver(I) derivatives yielded products, which underwent known equilibria, while exclusively the pentafluorophenyl derivative exhibits its zwitterionic nature in solution and in the solid state. Moreover, both perfluoroalkyl derivatives investigated decomposed slowly but more or less selectively even at -20 degrees C in solution: AgC2F5 center dot DMAP mainly into AgOCOCF3 (probably under the influence of moisture) and AgCF3 center dot DMAP mainly into the unprecedented derivative 3-trifluoromethyl-4-dimethylaminopyridine. The molecular structure of AgC6F5 center dot DMAP was elucidated showing a twist arrangement of the aromatic rings quite unusual for linear coordinated species

The First Rare-Earth Metal Telluride Chlorides, RTeCl (R = La, Ce, Pr, Nd)

The first rare-earth metal telluride chlorides, RTeCl with R = La, Ce, Pr, Nd, were obtained as single crystals and/or powder samples by the reaction of anhydrous rare-earth trichlorides, RCl3, with the respective rare-earth metals R and elemental tellurium (Te) in sealed tantalum containers at temperatures as high as 1050 degrees C. All four telluride-chlorides crystallize with the so-called tetragonal PbFCl type of structure but according to RTeCl = PbClF, with, for the example of LaTeCl-I, a = 451.7(1), c = 827.4(2) pm, V-E/Z = 84.5(1) angstrom(3), tetragonal, P4/nnm (No. 129). LaTeCl and CeTeCl are dimorphic, the second modification crystallizes with the PbCl2 type of structure with, for LaTeCl-II, a = 795.2(1), b = 450.8(1), c = 940.4(1) pm, V-E/Z = 84.3(1) angstrom(3), orthorhombic, Pnma (No. 62). In both structures, La3+ is nine-coordinate, [LaTe5Cl4], with similar mean La-Te and La-Cl distances in both modifications, 333.2 vs. 333.1 pm and 302.9 vs. 301.8 pm, respectively

A New 3D Coordination Polymer of Bismuth with Nicotinic Acid N-Oxide

The new three-dimensional coordination polymer {[Bi(NNO)2(NO3)]·1.5H2O}n (1, NNO− = nicotinate N-oxide) was synthesized and characterized by elemental analysis, IR and 1H-NMR spectroscopy, as well as single-crystal X-ray diffraction analysis. 1 crystallizes in the monoclinic space group C2/c. The crystal structure consists of a rectangular-shaped grid constructed with NNO linkers. Cavities of a diameter of 7.9–8.3 Å2 are filled with disordered water molecules. The thermal stability of the compound was evaluated by thermogravimetric analysis

The hexadecaiodide ion I₁₆²⁻. Synthesis and crystal structure of [Na(15c5)]₂I₁₆

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