Syntheses and crystal structures of solvate complexes of alkaline earth and lanthanoid metal iodides with N,N-dimethylformamide

2020 ◽  
Vol 235 (8-9) ◽  
pp. 401-411
Author(s):  
Constantin Hoch
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
Sphere Packing ◽  
Complex Salt ◽  
Monodentate Ligand ◽  
Metal Iodide ◽  
Metal Iodides

AbstractThe solvate complexes that can be obtained by either dissolving metal iodides in N,N-dimethylformamide (DMF) or by synthesising them in DMF have the general composition [M(DMF)x]Iy. DMF shows to behave as simple monodentate ligand with low sterical impact, so that x in the composition follows the radius of My+. We present here the crystal structures of the alkaline earth and lanthanoid metal iodide complexes [Mg(DMF)6]I2, [Ca(DMF)6]I2, [Sr(DMF)7]I2, [Ba(DMF)8]I2, [La(DMF)9]I3, [Ln(DMF)8]I3 (isotypic series for Ln = Nd, Sm, Eu, Dy, Gd, Er, Yb and Lu) and for the tris-triiodide complex salt [Sc(DMF)6](I3)3. Their different crystal structure types can be compared on the basis of the packing topologies of the nearly spherical cationic entities which show simple sphere packing motifs.

Crystal Structures and Thermal Behavior of Alkaline Earth Tricyanomethanides

2008 ◽  
Vol 63 (3) ◽  
pp. 285-288 ◽  
Author(s):  
Karl E. Bessler ◽  
Claudia C. Gatto ◽  
Lincoln L. Romualdo ◽  
Javier A. Ellena ◽  
Maria J. de A. Sales
Keyword(s):  
Crystal Structure ◽  
Coordination Polymer ◽  
Thermal Behavior ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
Three Dimensional ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Interpenetrating Networks ◽  
X Ray

The alkaline earth tricyanomethanides Mg(tcm)2 · 2H2O, Ca(tcm)2, Sr(tcm)2 ・H2O and Ba(tcm)2 · 2H2O were prepared from aqueous solutions of the respective chlorides and silver tricyanomethanide. Their IR spectra and thermal behavior are described. The crystal structures of Ca(tcm)2 and Ba(tcm)2 · 2H2O were determined by single crystal X-ray diffraction. The structure of Ca(tcm)2 is of the type found for several transition metal tricyanomethanides [1], containing two independent interpenetrating networks. Ba(tcm)2 · 2H2O has a unique crystal structure corresponding to a three-dimensional coordination polymer with nine fold coordinated Ba atoms connected by water molecules and tricyanomethanide anions.

Crystal structures and thermal decomposition of permanganates AE[MnO4]2·n H2O with the heavy alkaline earth elements (AE=Ca, Sr and Ba)

2017 ◽  
Vol 72 (8) ◽  
pp. 555-562 ◽  
Author(s):  
Harald Henning ◽  
Jörg M. Bauchert ◽  
Maurice Conrad ◽  
Thomas Schleid
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Orthorhombic Space Group ◽  
Crystal Water ◽  
Space Group ◽  
The Third ◽  
Cation Exchange Column

AbstractReexamination of the syntheses and crystal structures as well as studies of the thermal decomposition of the heavy alkaline earth metal permanganates Ca[MnO4]2·4 H2O, Sr[MnO4]2·3 H2O and Ba[MnO4]2 are the focus of this work. As an alternative to the very inelegant Muthmann method, established for the synthesis of Ba[MnO4]2 a long time ago, we employed a cation-exchange column loaded with Ba2+ cations and passed through an aqueous potassium-permanganate solution. We later used this alternative also with strontium- and calcium-loaded columns and all the compounds synthesized this way were indistinguishable from the products of the established methods. Ca[MnO4]2·4 H2O exhibiting [CaO8] polyhedra crystallizes in the orthorhombic space group Pccn with the lattice parameters a=1397.15(9), b=554.06(4) and c=1338.97(9) pm with Z=4, whereas Sr[MnO4]2·3 H2O with [SrO10] polyhedra adopts the cubic space group P213 with a=964.19(7) pm and Z=4. So the harder the AE2+ cation, the higher its demand for hydration in aqueous solution. Consequently, the crystal structure of Ba[MnO4]2 in the orthorhombic space group Fddd with a=742.36(5), b=1191.23(7) and c=1477.14(9) pm with Z=8 lacks any crystal water, but contains [BaO12] polyhedra. During the thermal decomposition of Ca[MnO4]2·4 H2O, the compound expels up to two water molecules of hydration, before the crystal structure collapses after the loss of the third H2O molecule at 157°C. The crystal structure of Sr[MnO4]2·3 H2O breaks down after the expulsion of the third water molecule as well, but this already occurs at 148°C. For both the calcium and the strontium permanganate samples, orthobixbyite-type α-Mn2O3 and the oxomanganates(III,IV) AEMn3O6 (AE=Ca and Sr) remain as final decomposition products at 800°C next to amorphous phases. On the other hand, the already anhydrous Ba[MnO4]2 thermally decomposes to hollandite-type BaMn8O16 and BaMnO3 at 800°C.

Crystal structures and reference X-ray powder diffraction patterns of Sr4−xCaxPb2O8 (x=1,2,3)

1998 ◽  
Vol 13 (4) ◽  
pp. 232-240 ◽  
Author(s):  
W. Wong-Ng ◽  
J. A. Kaduk ◽  
W. Greenwood
Keyword(s):  
Crystal Structure ◽  
Solid Solution ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Alkaline Earth ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
X Ray ◽  
Diffraction Patterns

The crystal structure of the solid solution alkaline earth plumbate phase Sr4−xCaxPb2O8 was investigated using the X-ray Rietveld technique for x=1, 2, and 3. The lattice parameters a, b, c, and V were found to decrease linearly as the Sr at site 4h was replaced by Ca. The structure features chains of edge-sharing PbO6 octahedra, linked by seven-coordinated (Ca/Sr)–O monocapped trigonal prisms. The structure is similar to that of Pb3O4, which can be reformulated as Pb2IIPbIVO4. X-ray diffraction patterns for the solid solution members SrCa3Pb2O8, Sr2Ca2Pb2O8, and Sr3CaPb2O8 were prepared for inclusion in the Powder Diffraction File.

Neue Erdalkalimetall-reiche binäre Indide: Ca2In, Sr28In11 und Sr5In3 / New Alkaline Earth Rich Binary Indides: Ca2In, Sr28In11 und Sr5In3

2004 ◽  
Vol 59 (6) ◽  
pp. 619-628 ◽  
Author(s):  
Marco Wendorff ◽  
Caroline Röhr
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Electronic Structures ◽  
Alkaline Earth ◽  
Structure Type ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Binary Alkaline

The new binary alkaline earth rich indides Ca2In (orthorhombic, space group Pnma, a =727.5(2), b = 537.1(2), c = 999.0(3) pm, Z = 4, R1 = 0.0252, Co2Si structure type) and Sr28In11 (orthorhombic, space group Imm2, a=582.6(3), b=6687.8(9), c=823.5(6) pm, Z =2, R1=0.0571, Ca28Ga11 structure type) have been synthesized from stoichiometric melts of the elements. Both crystal structures exhibit isolated In atoms coordinated by seven to ten alkaline earth atoms. In the crystal structure of Sr5In3 (tetragonal, space group I4/mcm, a = 874.4(3), c = 1642.9(8) pm, Z = 4, R1 = 0.0347, Cr5B3 structure type) isolated In atoms coexist with In2 dumbbells exhibiting short In-In contacts (284.4 pm). The electronic structures of the less elaborate compounds Ca2In and Sr5In3 are discussed in comparison with those of the closely related, nominally electron precise Zintl compounds Ca2Sn and Sr5Sn3.

Die Kristallstrukturell von CaHg(SCN)4 · nH2O (n = 2,3). Verwandtschaftsbeziehungen zwischen den Verbindungsklassen der Tetrathiocyanatomercurate(II) von Erdalkaliionen und 3d-Metallionen / The Crystal Structures of CaHg(SCN)4 · nH2O (n = 2, 3). Relations between Tetrathiocyanatomercurates(II) of the Alkaline-Earth-Ions and Ions of the 3d-Type

1983 ◽  
Vol 38 (8) ◽  
pp. 911-916 ◽  
Author(s):  
Klaus Brodersen ◽  
Hans-U. Hummel
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
The Other ◽  
Monoclinic Space Group ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
Metal Atoms ◽  
Nearest Neighbours

CaHg(SCN)4 · nH2O (n = 2(1), n = 3(2)) were isolated from an aqueous solution of Ca(NCS)2 · 4H2O and Hg(SCN)2· 1 is compared with the analogous MgHg(SCN)4 · 2H2O by means of powder patterns. The crystal structure of 2 has been determined. 2 is monoclinic, space group P21/c with a =9.469(4), b = 22.781(5), c = 6.587(4) Å, β = 93.6(3)°, Z = 4, dc = 2.46 g · cm-3.The structure was refined to R = 7.42 and Rw = 4.96% for 1224 independent reflec­tions.The species MHg(SCN)4 · 2H2O (M = Mg, Ca, Ni) contain nearly tetrahedral Hg(SCN)4 and octahedral M(OH2)2(NCS)4 groups which are joined by Hg-SCN-M bridges.In contrast the structures of the other compounds MHg(SCN)4 · nH2O (M = Co, n = 0; M = Ca, Sr, n = 3) are based on the diamond net. There is tetrahedral coordination of all the metal atoms, M having 4 N and Hg 4 S nearest neighbours. In the hydrates the H2O molecules are situated additionally at the Ca and Sr atoms [*].

Effect of solution acidity on the crystallization of polychromates in uranyl-bearing systems: synthesis and crystal structures of Rb2[(UO2)(Cr2O7)(NO3)2] and two new polymorphs of Rb2Cr3O10

2021 ◽  
Vol 236 (1-2) ◽  
pp. 11-21
Author(s):  
Evgeny V. Nazarchuk ◽  
Oleg I. Siidra ◽  
Dmitry O. Charkin ◽  
Stepan N. Kalmykov ◽  
Elena L. Kotova
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Crystal Structures ◽  
Hydrothermal Treatment ◽  
Ambient Conditions ◽  
Screw Axis ◽  
3D Framework ◽  
Solution Acidity

Abstract Three new rubidium polychromates, Rb2[(UO2)(Cr2O7)(NO3)2] (1), γ-Rb2Cr3O10 (2) and δ-Rb2Cr3O10 (3) were prepared by combination of hydrothermal treatment at 220 °C and evaporation of aqueous solutions under ambient conditions. Compound 1 is monoclinic, P 2 1 / c $P{2}_{1}/c$ , a = 13.6542(19), b = 19.698(3), c = 11.6984(17) Å, β = 114.326(2)°, V = 2867.0(7) Å3, R 1 = 0.040; 2 is hexagonal, P 6 3 / m $P{6}_{3}/m$ , a = 11.991(2), c = 12.828(3) Å, γ = 120°, V = 1597.3(5) Å3, R 1 = 0.031; 3 is monoclinic, P 2 1 / n $P{2}_{1}/n$ , a = 7.446(3), b = 18.194(6), c = 7.848(3) Å, β = 99.953(9)°, V = 1047.3(7) Å3, R 1 = 0.037. In the crystal structure of 1, UO8 bipyramids and NO3 groups share edges to form [(UO2)(NO3)2] species which share common corners with dichromate Cr2O7 groups producing novel type of uranyl dichromate chains [(UO2)(Cr2O7)(NO3)2]2−. In the structures of new Rb2Cr3O10 polymorphs, CrO4 tetrahedra share vertices to form Cr3O10 2− species. The trichromate groups are aligned along the 63 screw axis forming channels running in the ab plane in the structure of 2. The Rb cations reside between the channels and in their centers completing the structure. The trichromate anions are linked by the Rb+ cations into a 3D framework in the structure of 3. Effect of solution acidity on the crystallization of polychromates in uranyl-bearing systems is discussed.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

Sign in / Sign up

Export Citation Format

Share Document