Synthesis, crystal structure and selected properties of K2[Ni(dien)2]{[Ni(dien)]2Ta6O19}·11 H2O

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Dana-Céline Krause ◽  
Sebastian Mangelsen ◽  
Christian Näther ◽  
Wolfgang Bensch
Keyword(s):  
Crystal Structure ◽  
Water Sorption ◽  
Room Temperature ◽  
Water Molecules ◽  
Compound K ◽  
Common Edge ◽  
Crystal Water ◽  
3D Network ◽  
Sample Water ◽  
Partial Water

Abstract The new compound K2[Ni(dien)2]{[Ni(dien)]2Ta6O19}·11 H2O crystallized at room temperature applying a diffusion based reaction in a H2O/DMSO mixture using K8{Ta6O19}·16 H2O, Ni(NO3)2·6H2O and dien (diethylenetriamine). In the crystal structure, the Lindqvist-type anion [Ta6O19]8– is structurally expanded by two octahedrally Ni2+-centered complexes via three Ni–µ 2-O–Ta bonds thus generating the new {[Ni(dien)]2Ta6O19}4– anion. Two KO8 polyhedra share a common edge to form a K2O14 moiety, which connects the {[Ni(dien)]2Ta6O19}4– cluster shells into chains. The isolated [Ni(dien)2]2+ complexes are located in voids generated by the structural arrangement of the chains. An extended hydrogen bonding network between the different constituents generates a 3D network. The crystal water molecules can be thermally removed to form a highly crystalline dehydrated compound. Partial water uptake leads to the formation of a crystalline intermediate with a reduced unit cell volume compared to the fully hydrated sample. Water sorption experiments demonstrate that the fully dehydrated sample can be fully reconverted to the hydrated compound. The crystal field splitting parameters for the octahedrally coordinated Ni2+-centered complexes have been evaluated from an UV/Vis spectrum yielding D q = 1056 cm−1 and B = 887 cm−1.

scholarly journals Synthesis and crystal structure of bis[μ-N,N-bis(2-aminoethyl)ethane-1,2-diamine]bis[N,N-bis(2-aminoethyl)ethane-1,2-diamine]-μ4-oxido-hexa-μ3-oxido-octa-μ2-oxido-tetraoxidotetranickel(II)hexatantalum(V) nonadecahydrate

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Dana-Céline Krause ◽  
Christian Näther ◽  
Wolfgang Bensch
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Point Group ◽  
Organic Ligand ◽  
Group Symmetry ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Crystal Water ◽  
Synthesis And Crystal Structure ◽  
X Ray

Reaction of K8{Ta6O19}·16H2O with [Ni(tren)(H2O)Cl]Cl·H2O in different solvents led to the formation of single crystals of the title compound, [Ni4Ta6O19(C6H18N4)4]·19H2O or {[Ni2(κ4-tren)(μ-κ3-tren)]2Ta6O19}·19H2O (tren is N,N-bis(2-aminoethyl)-1,2-ethanediamine, C6H18N4). In its crystal structure, one Lindqvist-type anion {Ta6O19}8– (point group symmetry \overline{1}) is connected to two NiII cations, with both of them coordinated by one tren ligand into discrete units. Both NiII cations are sixfold coordinated by O atoms of the anion and N atoms of the organic ligand, resulting in slightly distorted [NiON5] octahedra for one and [NiO3N3] octahedra for the other cation. These clusters are linked by intermolecular O—H...O and N—H...O hydrogen bonding involving water molecules into layers parallel to the bc plane. Some of these water molecules are positionally disordered and were refined using a split model. Powder X-ray diffraction revealed that a pure crystalline phase was obtained but that on storage at room-temperature this compound decomposed because of the loss of crystal water molecules.

scholarly journals Crystal structure of the new hybrid material bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate

2015 ◽  
Vol 71 (11) ◽  
pp. 1384-1387
Author(s):  
Marwen Chouri ◽  
Habib Boughzala
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Molar Ratio ◽  
Water Molecules ◽  
Site Symmetry ◽  
Two Dimensional ◽  
Slow Evaporation ◽  
Solution Ph

The title compound bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate, (C6H14N2)2[Bi2Cl10]·2H2O, was obtained by slow evaporation at room temperature of a hydrochloric aqueous solution (pH = 1) containing bismuth(III) nitrate and 1,4-diazabicyclo[2.2.2]octane (DABCO) in a 1:2 molar ratio. The structure displays a two-dimensional arrangement parallel to (100) of isolated [Bi2Cl10]4−bioctahedra (site symmetry -1) separated by layers of organic 1,4-diazoniabicyclo[2.2.2]octane dications [(DABCOH2)2+] and water molecules. O—H...Cl, N—H...O and N—H...Cl hydrogen bonds lead to additional cohesion of the structure.

scholarly journals Substitutions of Zr4+/V5+ for Y3+/Mo6+ in Y2Mo3O12 for Less Hygroscopicity and Low Thermal Expansion Properties

Materials ◽  
2019 ◽  
Vol 12 (23) ◽  
pp. 3945 ◽  
Author(s):  
Qiang Ma ◽  
Lulu Chen ◽  
Heng Qi ◽  
Qi Xu ◽  
Baohe Yuan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Expansion ◽  
Crystal Structures ◽  
Room Temperature ◽  
Crystal Water ◽  
Thermal Expansion Property ◽  
Expansion Property ◽  
Low Thermal Expansion ◽  
Substitution Content ◽  
Structure And Microstructure

In this investigation, ZrxY2−xVxMo3−xO12 (0 ≤ x ≤ 1.4) is developed and the effects of the substitutions of Zr4+/V5+ for Y3+/Mo6+ in Y2Mo3O12 on the hygroscopicity and thermal expansion property are investigated. For the smaller substitution content (x ≤ 0.5), their crystal structures remain orthorhombic, while there is crystal water still in the lattice. The linear coefficients of thermal expansions (CTEs), for x = 0.1, 0.3, 0.5, and 0.7, are about −4.30 × 10−6, −0.97 × 10−6, 0.85 × 10−6, and 0.77 × 10−6 K−1, respectively, from 476 to 773 K, which means that the linear CTE could be changed linearly with the substitution content of Zr4+/V5+ for Y3+/Mo6+ in Y2Mo3O12. As long as the substitution content reaches x = 1.3/1.4, almost no hygroscopicity and low thermal expansion from room temperature are obtained and are discussed in relation to the crystal structure and microstructure.

Crystal Structures of Piperazinium Tetrabromocadmate(II)-Monohydrate [C4H12N2]CdBr4 · H2O, PiperaziniumTetraiodocadmate(II) [C4H12N2]CdI4, and Bis(trimethylsulphonium) Tetrabromocadmate(II) [(CH3)3S]2CdBr4

2002 ◽  
Vol 57 (5) ◽  
pp. 503-508 ◽  
Author(s):  
Hideta Ishihara ◽  
Keizo Horiuchi ◽  
Thorsten M. Gesing ◽  
Shi-qi Dou ◽  
J.-Christian Buhl ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Room Temperature ◽  
Water Molecules ◽  
Temperature Phase

Piperazinium tetrabromocadmate(II)-monohydrate, [C4H12N2]CdBr4 · H2O (1) crystallizes with isolated [CdBr4]2- anions, piperazinium cations, and water molecules (monoclinic, P21/c, Z = 4, a = 698.7(1), b = 1348.6(3), and c = 1432.4(3) pm, β = 92.97(3)˚ at 293 K). The crystal structure of 1 is almost the same as that reported in Inorg. Chim. Acta 187, 141 (1991). The crystal of piperazinium tetraiodocadmate(II), [C4H14N2]CdI4 (2) consists of isolated [CdI4]2- anions and piperazinium cations (orthorhombic,P212121, Z=4, a = 903.2(5), b = 1226.3(6), and c = 1307.9(7) pm at 293 K). The room temperature phase of bis(trimethylsulphonium) tetrabromocadmate( II), [(CH3)3S]2CdBr4 (3) has isolated [CdBr4]2- anions and trimethylsulphonium cations (orthorhombic, P212121, Z = 4, a = 911.3(1), b = 1329.2(2), and c = 1454.7(2) pm at 293 K).

scholarly journals Hydrogen Bond Studies. 125. A Deuteron Magnetic Resonance Study of Strontium Formate Dihydrate, Sr(HCOO)2 · 2D2O

1977 ◽  
Vol 32 (9) ◽  
pp. 1025-1029 ◽  
Author(s):  
Bo Berglund ◽  
Jörgen Tegenfeldt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Magnetic Resonance ◽  
Electric Field Gradient ◽  
Room Temperature ◽  
Coupling Constants ◽  
Water Molecules ◽  
Magnetic Resonance Study ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

AbstractA room temperature (25 °C) deuteron magnetic resonance (DMR) study of a single crystal of Sr (HCOO)2 · 2 D2O is reported. Signals from all water molecules in the unit cell have been detected, and all four independent electric field gradient (EFG) tensors at the water deuterons have been determined from 409 quadrupole splittings. All spectra were recorded by rotating the crystal about one arbitrarily selected axis. The following quadrupole coupling constants and asymmetry parameters for the deuterons were obtained: 213.5(4), 189.3(4), 195.7(4) and 200.7(5) kHz and 0.117(3), 0.110(4), 0.116(4) and 0.098(3). The directions of the eigenvalues are qualitatively consistent with the crystal structure refined by Galigné 1; the result is in disagreement, however, with the earlier DMR study of Sr (DCOO)2 · 2 D2O (Reference 2).

A hexaniobate expanded by six [Hg(cyclam)]2+ complexes via Hg–O bonds yields a positively charged polyoxoniobate cluster

2020 ◽  
Vol 75 (1-2) ◽  
pp. 233-237 ◽  
Author(s):  
Philipp Müscher-Polzin ◽  
Christian Näther ◽  
Wolfgang Bensch
Keyword(s):  
Hydrogen Bonding ◽  
Title Compound ◽  
Room Temperature ◽  
Bond Formation ◽  
Water Molecules ◽  
The Novel ◽  
Temperature Reaction ◽  
Crystal Water ◽  
Nitrate Anions ◽  
Positively Charged

AbstractThe room temperature reaction of Hg(NO3)2 · H2O, cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane) and K8{Nb6O19} · 16 H2O in a mixture of H2O and DMSO led to crystallization of the novel compound {[Hg(cyclam)]6Nb6O19}(NO3)4 · 14 H2O, which is the first mercury containing polyoxoniobate. The structure consists of a {Nb6O19}8− cluster core which is expanded by six [Hg(cyclam)]2+ complexes via Hg–μ2-O–Nb bond formation. The title compound contains a positively charged polyoxoniobate cluster. The crystal water molecules form small aggregates by O–H · · · O hydrogen bonding which are joined into larger aggregates by N–O · · · H–O hydrogen bonding integrating the nitrate anions.

scholarly journals Redetermination of the crystal structure of 3,5-dimethylpyrazolium β-octamolybdate tetrahydrate

2015 ◽  
Vol 71 (12) ◽  
pp. m244-m245 ◽  
Author(s):  
Tatiana R. Amarante ◽  
Isabel S. Gonçalves ◽  
Filipe A. Almeida Paz
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Three Dimensional ◽  
Site Occupancy ◽  
Temperature Data ◽  
Water Molecules ◽  
Compound C ◽  
Metal Atoms ◽  
Anisotropic Displacement Parameters ◽  
Difference Fourier

The title compound, (C5H9N2)4[Mo8O26]·4H2O, was reported previously from a room-temperature data collection from which only the metal atoms could be refined anisotropically [FitzRoyet al.(1989).Inorg. Chim. Acta,157, 187–194]. The current redetermination at 180 (2) K models all the non-H atoms with anisotropic displacement parameters and fully describes the supramolecular N—H...O and O—H...O hydrogen-bonded network connecting the 3,5-dimethylpyrazolium cations, the water molecules of crystallization and the β-octamolybdate anion. All H atoms involved in the three-dimensional hydrogen-bonding network could be located from difference Fourier maps, with the exception of those of one disordered water molecule, firstly seen in this structural report [refined over two distinct locations with site-occupancy factors of 0.65 (2) and 0.35 (2)]. The complete β-octamolybdate anion is generated by a crystallographic inversion centre.

scholarly journals Crystal water as the molecular glue for obtaining different co-crystal ratios: the case of gallic acid tris-caffeine hexahydrate

2018 ◽  
Vol 74 (4) ◽  
pp. 559-562
Author(s):  
L. Vella-Zarb ◽  
U. Baisch
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Gallic Acid ◽  
Carbonyl Oxygen ◽  
Crystalline Solid ◽  
Water Molecules ◽  
Crystal Water ◽  
Classical Hydrogen Bond ◽  
Additional Hydrogen

The crystal structure of the hexahydrate co-crystal of gallic acid and caffeine, C7H6O5·3C8H10N4O2·6H2O or GAL3CAF·6H2O, is a remarkable example of the importance of hydrate water acting as structural glue to facilitate the crystallization of two components of different stoichiometries and thus to compensate an imbalance of hydrogen-bond donors and acceptors. The water molecules provide the additional hydrogen bonds required to form a crystalline solid. Whereas the majority of hydrogen bonds forming the intermolecular network between gallic acid and caffeine are formed by crystal water, only one direct classical hydrogen bond between two molecules is formed between the carboxylic oxygen of gallic acid and the carbonyl oxygen of caffeine with d(D...A) = 2.672 (2) Å. All other hydrogen bonds either involve crystal water or utilize protonated carbon atoms as donors.

scholarly journals (NH4)Mg(HSO4)(SO4)(H2O)2 and NaSc(CrO4)2(H2O)2, two crystal structures comprising kröhnkite-type chains, and the temperature-induced phase transition (NH4)Mg(HSO4)(SO4)(H2O)2\rightleftharpoons (NH4)MgH(SO4)2(H2O)2

2021 ◽  
Vol 77 (3) ◽  
pp. 144-151
Author(s):  
Matthias Weil ◽  
Uwe Kolitsch
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Classification Scheme ◽  
Three Dimensional ◽  
Structure Type ◽  
Group Symmetry ◽  
Water Molecules

The crystal structure of the mineral kröhnkite, Na2Cu(SO4)2(H2O)2, contains infinite chains composed of [CuO4(OH2)2] octahedra corner-linked with SO4 tetrahedra. Such or similar tetrahedral–octahedral `kröhnkite-type' chains are present in the crystal structures of numerous compounds with the composition AnM(XO4)2(H2O)2. The title compounds, (NH4)Mg(HSO4)(SO4)(H2O)2, ammonium magnesium hydrogen sulfate sulfate dihydrate, and NaSc(CrO4)2(H2O)2, sodium scandium bis(chromate) dihydrate, are members of the large family with such kröhnkite-type chains. At 100 K, (NH4)Mg(HSO4)(SO4)(H2O)2 has an unprecedented triclinic crystal structure and contains [MgO4(OH2)2] octahedra linked by SO3(OH) and SO4 tetrahedra into chains extending parallel to [\overline{1}10]. Adjacent chains are linked by very strong hydrogen bonds between SO3(OH) and SO4 tetrahedra into layers parallel to (111). Ammonium cations and water molecules connect adjacent layers through hydrogen-bonding interactions of medium-to-weak strength into a three-dimensional network. (NH4)Mg(HSO4)(SO4)(H2O)2 shows a reversible phase transition and crystallizes at room temperature in structure type E in the classification scheme for structures with kröhnkite-type chains, with half of the unit-cell volume for the resulting triclinic cell, and with disordered H atoms of the ammonium tetrahedron and the H atom between two symmetry-related sulfate groups. IR spectroscopic room-temperature data for the latter phase are provided. Monoclinic NaSc(CrO4)2(H2O)2 adopts structure type F1 in the classification scheme for structures with kröhnkite-type chains. Here, [ScO4(OH2)2] octahedra (point group symmetry \overline{1}) are linked by CrO4 tetrahedra into chains parallel to [010]. The Na+ cations (site symmetry 2) have a [6 + 2] coordination and connect adjacent chains into a three-dimensional framework that is consolidated by medium–strong hydrogen bonds involving the water molecules. Quantitative structural comparisons are made between NaSc(CrO4)2(H2O)2 and its isotypic NaM(CrO4)2(H2O)2 (M = Al and Fe) analogues.

scholarly journals Synthesis and crystal structure of catena-poly[[hexaaqua{μ3-2-[bis(carboxylatomethyl)amino]terephthalato}dicobalt(II)] pentahydrate] containing water tapes and pentamers

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Jie Ma ◽  
Wen-Zhi Zhang ◽  
Jie Xiong ◽  
Chun-Yan Yan
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Three Dimensional ◽  
Free Water ◽  
Water Molecules ◽  
Synthesis And Crystal Structure ◽  
One Dimensional ◽  
Uncoordinated Water Molecule ◽  
Distorted Octahedral ◽  
Water Ligands

The title coordination polymer, {[Co2(C12H7NO8)(H2O)6]·5H2O} n , was crystallized at room temperature from an aqueous solution of 2-aminodiacetic terephthalic acid (H4adtp) and cobalt(II) nitrate. The asymmetric unit consists of one adtp4− ligand, one and two half CoII ions, six water ligands coordinated to CoII ions and five uncoordinated water molecules. Two of the cobalt cations lie on centres of inversion and are coordinated in octahedral O2(OH2)4 environments, whereas the other adopts a slightly distorted octahedral NO3(OH2)2 environment. The crystal structure contains parallel stacked, one-dimensional zigzag chains, {[Co2(C12H7NO8)(H2O)6]} n , which assemble into a three-dimensional supramolecular architecture via networks of hydrogen bonds involving the coordinated and free water molecules. One-dimensional `water tapes' are formed, containing alternating six-membered and twelve-membered rings of water molecules, together with water pentamers, in which a central uncoordinated water molecule is hydrogen bonded to two coordinated and two free water molecules in a tetrahedral arrangement.

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