Syntheses, Crystal Structures, and Reactivity of [enH]4[Sn2Se6]·en, [enH]4[Sn2Te6]·en and [enH]4[Sn2S6]: Known Anions within Novel Coordination Spheres obtained by Novel Synthesis Routes

Author(s):  
Stefanie Dehnen ◽  
Christian Zimmermann
1994 ◽  
Vol 49 (6) ◽  
pp. 770-772 ◽  
Author(s):  
Klaus Schulbert ◽  
Rainer Mattes

The reactions of N-substituted dithiocarbamic acid esters and nickel acetate yield, by partial degradation of the esters, the polynuclear nickel thiolato complexes cyclo-[(μ-SMe)2Ni]6, 1 and [(μ-SMe)2(Ni(MeNHCS2))2, 2. Their crystal structures have been determined. The Ni coordination spheres are comprised of four sulfur atoms in a planar arrangement. 1 is a second, highly symmetrical modification of the already known cyclic hexamer Ni6(SMe)12. In 2 two Ni(PhNHCS2) moieties are bridged to dimers by thiolato groups. Two of these dimers are connected to a tetramer by weak axial Ni-S interactions. Crystal data for 1: monoclinic, space group P21/n, a = 986.1(2), b = 1308.1(3), c = 1228.6(2) pm, β = 96.07(3)°, Z = 2, R = 0.072, Rw = 0.062, 3797 reflections. 2: orthorhombic, space group Pnma, a = 1790.0(4), b = 1806.7(4), c = 934.4(2) pm. Z = 4, R = 0.061, Rw = 0.051, 2079 reflections


Author(s):  
Joseph S. Merola ◽  
Marion A. Franks

The crystal structures of two solvates offac-trichloridotris(trimethylphosphane-κP)rhodium(III) are reported,i.e.one with water in the crystal lattice,fac-[RhCl3(Me3P)3]·H2O, and one with methanol in the crystal lattice,fac-[RhCl3(Me3P)3]·0.5CH3OH. These rhodium compounds exhibit distorted octahedral coordination spheres at the metal and are isotypic with the analogous iridium compounds previously reported by us [Merolaet al.(2013).Polyhedron,54, 67–73]. Comparison is made between the rhodium and iridium compounds, highlighting their isostructural relationships.


Author(s):  
Bo Zhang ◽  
R. Carlson ◽  
E. N. Pederson ◽  
B. Witholt ◽  
F. Srienc

2002 ◽  
Vol 58 (2) ◽  
pp. 198-218 ◽  
Author(s):  
G. D. Ilyushin ◽  
V. A. Blatov

The first attempt is undertaken to consider systematically topological structures of zirconosilicates and their analogs (60 minerals and 34 synthetic phases), where the simplest structure units are MO6 octahedra and TO4 tetrahedra united by vertices ([TO4]:[MO6] = 1:1–6:1). A method of analysis and classification of mixed three-dimensional MT frameworks by topological types with coordination sequences {N k } is developed, which is based on the representation of crystal structure as a finite `reduced' graph. The method is optimized for the frameworks of any composition and complexity and implemented within the TOPOS3.2 program package. A procedure of hierarchical analysis of MT-framework structure organization is proposed, which is based on the concept of polyhedral microensemble (PME) being a geometrical interpretation of coordination sequences of M and T nodes. All 12 theoretically possible PMEs of MT 6 polyhedral composition are considered where T is a separate and/or connected tetrahedron. Using this methodology the MT frameworks in crystal structures of zirconosilicates and their analogs were analyzed within the first 12 coordination spheres of M and T nodes and related to 41 topological types. The structural correlations were revealed between rosenbuschite, lavenite, hiortdahlite, woehlerite, siedozerite and the minerals of the eudialyte family.


2012 ◽  
Vol 210 (4) ◽  
pp. 649-657 ◽  
Author(s):  
Simon Perraud ◽  
Etienne Quesnel ◽  
Stéphanie Parola ◽  
Jérémy Barbé ◽  
Viviane Muffato ◽  
...  

Author(s):  
K. J. Morrissey ◽  
M. A. Subramanian ◽  
C. C. Torardi ◽  
E. M. McCarron ◽  
J. C. Calabrese ◽  
...  

It is important to combine characterization techniques such as electron microscopy with novel materials synthesis in the study of high Tc superconducting phases. Results from electron microscopy studies have been correlated with structure determinations made using x-ray and neutron diffraction (1.2,3.4). Superconducting phases studied to date include YBa2Cu3O7-x, La1.25Ba1.75Cu3O7, Bi2Sr2CuO6, Bi2Sr2CaCu2O8, Tl2Ba2CuO6 Tl2Ba2CaCu2O8, and Tl2Ba2Ca2Cu3O8. A comparison between structures and defect populations suggests that structural defects, which modify the Cu-O arrangement (sheets or chains) intergrowths and grain boundaries, will affect superconductivity. Techniques used in this investigation include HREM, CBED, AEM, SAD and conventional imaging techniques.Samples characterized in this study were prepared in our laboratory, using both conventional and novel synthesis routes. Powder samples in the Tl-Ba-Cu-O system were prepared by heating mixtures of high purity BaO2, Tl2O2 and CuO to 850-900°C in sealed gold tubes for 1-6 hours (3,4). Similar procedures were followed in the Bi2Sr2CaCu2O8 system using Bi2O3, CaCO3, SrO2/Sr(NO3)2 and CuO. heating the mixtures in air at 700-900°C for 12-36 hours (2.4).


2013 ◽  
Vol 68 (5-6) ◽  
pp. 616-624 ◽  
Author(s):  
Tanja Schustereit ◽  
Harald Henning ◽  
Thomas Schleid ◽  
Ingo Hartenbach

The lanthanoid(III) bromide ortho-oxomolybdates(VI) LnBr[MoO4] (Ln = Pr, Nd, Sm, Gd - Lu) crystallize triclinically in the space group P1 (a=686 - 689, b=713 - 741, c=1066 - 1121 pm, a =103 - 106, b =107 - 108, g = 92 - 95°) with Z =4. The crystal structure contains two crystallographically distinguishable Ln3+ cations, each one with a coordination number of seven plus one. (Ln1)3+ is surrounded by three bromide and four plus one oxide anions, while for (Ln2)3+ just one bromide and six plus one oxide anions belong to the coordination sphere. Considering the smallest lanthanoids, however, the distances to the farthest anions increase so much that their contribution to the coordination spheres becomes negligible in both cases. The polyhedra around (Ln1)3+ are connected to each other via common edges, which consist of two crystallographically identical Br- anions (Br1). Furthermore, the common structure of the LnBr[MoO4] series contains two crystallographically different, discrete [MoO4]2- ortho-oxomolybdate(VI) tetrahedra. Two plus one oxygen atoms of each [(Mo1)O4]2- unit are used to interconnect the polyhedra around (Ln1)3+ and (Ln2)3+ together with one Br- anion (Br2). The connection between two polyhedra around (Ln2)3+ is generated exclusively by two plus one oxygen atoms of two [(Mo2)O4]2- anions. The complete structural arrangement can be considered as a bundle of primitively packed 1¥{LnBr[MoO4]} chains with two alternating motifs of linkage, which are running parallel along [012].


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