On the (non-)existence of Tutton salts with formula types [M(H2O)6](ClO4)2(H2O)2and Na2M(SO4)2(H2O)6(Mis a first-row transition metal)

2013 ◽  
Vol 69 (9) ◽  
pp. 990-994 ◽  
Author(s):  
Matthias Weil
Keyword(s):  
Transition Metal ◽  
Water Molecule ◽  
Ammonium Cation ◽  
Crystal Chemical ◽  
Intensity Data ◽  
Sulfate Anion ◽  
Tutton Salts ◽  
Structure Factors

Two structures of the Tutton salt family, originally reported with composition [Cu(H2O)6](ClO4)2(H2O)2and Na2Cu(SO4)2(H2O)6, have been redetermined based on the original intensity data. With respect to the original [Cu(H2O)6](ClO4)2(H2O)2model, the perchlorate anion and the noncoordinating water molecule are replaced by a sulfate anion and an ammonium cation. With respect to the original Na2Cu(SO4)2(H2O)6model, the sodium site is replaced by a mixed-occupancy potassium/ammonium site. The resulting revised formulae are (NH4)2Cu(SO4)2(H2O)6[diammonium hexaaquacopper(II) disulfate] and [(NH4)1.176K0.824]Cu(SO4)2(H2O)6, respectively. In both cases, the redetermination led to chemically more sensible structure models, accompanied by lower reliability factors. Three other reported structures with formula types [M(H2O)6](ClO4)2(H2O)2or Na2M(SO4)2(H2O)6(Mis a first row transition metal) have also been re-examined. From crystal–chemical considerations, their existence is likewise questioned. It is shown that the deposition of structure factors is beneficial for detailed re-examinations of problematic structure models.

scholarly journals Cyclooctanaminium hydrogen succinate monohydrate

2012 ◽  
Vol 68 (4) ◽  
pp. o1204-o1204 ◽  
Author(s):  
Sanaz Khorasani ◽  
Manuel A. Fernandes
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Ammonium Cation ◽  
Water Molecules ◽  
Hydrated Salt ◽  
A Chain ◽  
Hydrogen Bonded

In the title hydrated salt, C8H18N+·C4H5O4−·H2O, the cyclooctyl ring of the cation is disordered over two positions in a 0.833 (3):0.167 (3) ratio. The structure contains various O—H.·O and N—H...O interactions, forming a hydrogen-bonded layer of molecules perpendicular to thecaxis. In each layer, the ammonium cation hydrogen bonds to two hydrogen succinate anions and one water molecule. Each hydrogen succinate anion hydrogen bonds to neighbouring anions, forming a chain of molecules along thebaxis. In addition, each hydrogen succinate anion hydrogen bonds to two water molecules and the ammonium cation.

Crystal structure of atropine sulfate monohydrate, (C17H24NO3)2(SO4)·(H2O)

2019 ◽  
Vol 34 (4) ◽  
pp. 389-395 ◽  
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Water Molecule ◽  
Powder Diffraction ◽  
Density Functional ◽  
Atropine Sulfate ◽  
Strong Hydrogen Bond ◽  
Hydroxyl Groups ◽  
Hydrogen Atoms ◽  
Sulfate Anion

The crystal structure of atropine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atropine sulfate monohydrate crystallizes in space group P21/n (#14) with a = 19.2948(5), b = 6.9749(2), c = 26.9036(5) Å, β = 94.215(2)°, V = 3610.86(9) Å3, and Z = 4. Each of the two independent protonated nitrogen atoms participates in a strong hydrogen bond to the sulfate anion. Each of the two independent hydroxyl groups acts as a donor in a hydrogen bond to the sulfate anion, but only one of the water molecule hydrogen atoms acts as a hydrogen bond donor to the sulfate anion. The hydrogen bonds are all discrete but link the cations, anion, and water molecule along [101]. Although atropine and hyoscyamine (atropine is racemic hyoscyamine) crystal structures share some features, such as hydrogen bonding and phenyl–phenyl packing, the powder patterns show that the structures are very different. The powder pattern for atropine sulfate monohydrate has been submitted to ICDD for inclusion in the Powder Diffraction File™.

scholarly journals A new one-dimensional NiIIcoordination polymer with a two-dimensional supramolecular architecture

2017 ◽  
Vol 73 (2) ◽  
pp. 192-195
Author(s):  
Kai-Long Zhong
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Sulfate Ions ◽  
Sulfate Anion ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral ◽  
Metal Organic

A new one-dimensional NiIIcoordination polymer of 1,3,5-tris(imidazol-1-ylmethyl)benzene, namelycatena-poly[[aqua(sulfato-κO)hemi(μ-ethane-1,2-diol-κ2O:O′)[μ3-1,3,5-tris(1H-imidazol-1-ylmethyl)benzene-κ3N3,N3′,N3′′]nickel(II)] ethane-1,2-diol monosolvate monohydrate], {[Ni(SO4)(C18H18N6)(C2H6O2)0.5(H2O)]·C2H6O2·H2O}n, was synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The NiIIcation is coordinated by three N atoms of three different 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands, one O atom of an ethane-1,2-diol molecule, by a sulfate anion and a water molecule, forming a distorted octahedral NiN3O3coordination geometry. The tripodal 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands link the NiIIcations, generating metal–organic chains running along the [100] direction. Adjacent chains are further connected by O—H...O hydrogen bonds, resulting in a two-dimensional supermolecular architecture running parallel to the (001) plane. Another water molecule and a second ethane-1,2-diol molecule are non-coordinating and are linked to the coordinating sulfate ionsviaO—H...O hydrogen bonds.

Transition Metal-centered Trigonal Prisms as BuildingUnits in RE14T3In3 (RE = Y, Ho, Er, Tm, Lu; T = Pd, Ir, Pt) and Y4IrIn

2007 ◽  
Vol 62 (12) ◽  
pp. 1574-1580 ◽  
Author(s):  
Roman Zaremba ◽  
Ute Ch. Rodewald ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Transition Metal ◽  
Three Dimensional ◽  
Crystal Chemical ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Type Space ◽  
Arc Melting ◽  
Trigonal Prisms

The indides RE14T3In3 (RE = Y, Ho, Er, Tm, Lu; T = Pd, Ir, Pt) and Y4IrIn were synthesized from the elements by arc-melting and subsequent annealing for crystal growth. Their structures were characterized on the basis of X-ray powder and single crystal data: Lu14Co3In3-type, space group P42/nmc, a = 970.2(1), c = 2340.7(5) pm for Y13.95Pd3In3.05, a = 959.7(1), c = 2309.0(5) pm for Ho14Pd2.95In3, a = 955.5(1), c = 2305.1(5) pm for Er14Pd3In3, a = 950.9(1), c = 2291.6(5) pm for Tm13.90Pd3In3.10, a = 944.4(1), c = 2275.5(5) pm for Lu13.93Pd3In3.07, a = 962.9(1), c = 2343.0(5) pm for Y13.86Ir2.97In3.02, a = 967.6(1), c = 2347.8(5) pm for Y13.92Pt3.05In2.91, and Gd4RhIn-type, space group F 4̅3m, a = 1368.6(2) pm for Y4IrIn. The main structural motifs are transition metal-centered trigonal prisms of the rare earth elements which are condensed to twodimensional networks in the RE14T3In3 indides and to a three-dimensional one in Y4IrIn. The indium atoms in both structure types show segregation in the metal-rich matrix, i. e. In2 dumbbells in the RE14T3In3 indides (309 pm In2-In2 in Y13.86Ir2.97In3.02) and In4 tetrahedra (322 pm In-In) in Y4IrIn. The crystal chemical peculiarities of both structure types are discussed.

scholarly journals Crystal structure of NH4[La(SO4)2(H2O)]

2015 ◽  
Vol 71 (6) ◽  
pp. 663-666 ◽  
Author(s):  
Meriem Benslimane ◽  
Yasmine Kheira Redjel ◽  
Hocine Merazig ◽  
Jean-Claude Daran
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Water Molecule ◽  
Three Dimensional ◽  
Sulfate Anion ◽  
Hydrogen Bonding Interactions ◽  
Trigonal Prisms ◽  
Hydrogen Bonded

The principal building units in the crystal structure of ammonium aquabis(sulfato)lanthanate(III) are slightly distorted SO4tetrahedra, LaO9polyhedra in the form of distorted tricapped trigonal prisms, and NH4+ions. The La3+cation is coordinated by eight O atoms from six different sulfate tetrahedra, two of which are bidentate coordinating and four monodentate, as well as one O atom from a water molecule; each sulfate anion bridges three La3+cations. These bridging modes result in the formation of a three-dimensional anionic [La(SO4)2(H2O)]−framework that is stabilized by O—H...O hydrogen-bonding interactions. The disordered ammonium cations are situated in the cavities of this framework and are hydrogen-bonded to six surrounding O atoms.

Ternary Intermetallic Compounds LnMn2Al10 (Ln = Y, La-Nd, Sm, Gd-Dy) and LnRe2Al10 (Ln = Ce, Pr, Sm) with CaCr2Al10-Type Structure

1998 ◽  
Vol 53 (7) ◽  
pp. 673-678 ◽  
Author(s):  
Verena M.T. Thiede ◽  
Wolfgang Jeitschko
Keyword(s):  
Transition Metal ◽  
Type Structure ◽  
Variable Parameters ◽  
X Ray ◽  
Metal Atoms ◽  
Transition Metal Atoms ◽  
Structural Relationships ◽  
Structure Factors ◽  
Ternary Intermetallic Compounds ◽  
First Time

Abstract The twelve title compounds have been prepared for the first time. Their CaCr2Al10-type structure (P4/nmm, Z = 4) was refined from single-crystal X-ray data for the three representatives TbMnAl10 (a = 1274.3(2) pm, c = 511.4(2) pm, R = 0.025 for 680 structure factors F and 43 variable parameters V), CeRe2Al10 (a = 1295.5(5) pm, c = 517.2(4) pm, R = 0.054 for 810 F and 46 V), and SmRe2Al10 (a = 1291.5(2) pm, c = 516.5(1) pm, R = 0.021 for 622 F and 46 V). The atomic positions of the lanthanoid and transition metal atoms are fully occupied. Significant deviations from the full occupancies were observed for two aluminum sites in TbMn2Al10 and for all five aluminum sites of the two rhenium-containing compounds, resulting in the compositions TbMn2Al9.63(2), CeRe2Al9.52(8), and SmRe2Al9.16(9). The cell volume of CeRe2Al10 and to a smaller extent also that of CeMn2Al10 indicate mixed or intermediate +III/+IV valencies of the cerium atoms in these compounds. The structural relationships between the three closely related body-centered tetragonal structures of ThMn12, CeMniAl8, DyFe6Al6 and the primitive tetragonal structure of CaCr2Al10 are briefly discussed.

Ternary Antimonides LnTSb3 with Ln = La-Nd, Sm and T = V, Cr

1995 ◽  
Vol 50 (6) ◽  
pp. 899-904 ◽  
Author(s):  
Markus Brylak ◽  
Wolfgang Jeitschko
Keyword(s):  
Transition Metal ◽  
Single Crystal ◽  
Structure Type ◽  
Variable Parameters ◽  
X Ray ◽  
Metal Site ◽  
Metal Atoms ◽  
Transition Metal Atoms ◽  
Structure Factors ◽  
Infinite Strings

The title compounds were prepared by reaction of the elemental components. They crystallize in a new structure type, which was determined from single-crystal X -ray data of CeCrSb3: Pbcm, a = 1310.8(3), b = 618.4(1), c = 607.9(1) pm, Z = 4, R = 0.029 for 648 structure factors and 32 variable parameters. The structure of the antimonide CeVSb3 is isotypic: a = 1319.0(2), b = 623.92(8), c = 603.03(8) pm , R = 0.041 for 477 structure factors and 32 variables. The transition metal site and one of the three antimony sites were found to have partial occupancies resulting in the exact compositions CeV0,91(1)Sb2,916(4) and CeCr0,901(9)Sb2,909(4). The structures contain fractional Sb -Sb bonds with distances varying between 301,5 and 316.4 pm. The transition metal atoms have octahedral antimony coordination. These TSb6 octahedra share faces resulting in linear infinite strings with V - V and Cr - Cr bond distances of 301.5 and 304.0 pm, respectively. The structure of these com pounds contains building elements, which are also found in antimonides with ThCr2Si2, CaBe2Ge2, and HfCuSi2 type structures.

New symmetry and structure for spinel

1983 ◽  
Vol 386 (1791) ◽  
pp. 333-345 ◽  
Keyword(s):  
Crystal Structure ◽  
Experimental Data ◽  
Physical Properties ◽  
Magnesium Aluminate ◽  
Intensity Data ◽  
Structure Parameter ◽  
X Ray Diffraction ◽  
Diffraction Intensity ◽  
X Ray ◽  
Structure Factors

The crystal structure of magnesium aluminate is conventionally described within a symmetry corresponding to the centrosymmetrical space group Fd3m but this has created difficulties for the interpretation of many of its physical properties. Therefore, extensive X-ray diffraction intensity data have been collected from a small spherical synthetic single crystal and used for a structure parameter refinement assuming F4̅3m symmetry as proposed by Grimes ( Phil. Mag . 26, 1217‒1226 (1972)), and also for refinement according to conventional symmetry. The F4̅3m assumption yields the first direct measurement of the suspected deviations from the centrosymmetrical structure, and is found to provide a significantly superior fit to the experimental data, especially at high angles and with reflexions having structure factors less than 10.0. The weak reflexions include nine that are forbidden under Fd3m symmetry and it is shown that there is satisfactory agreement between observed and calculated structure factors in these cases.

Crystal structure of hyoscyamine sulfate monohydrate, (C17H24NO3)2(SO4)(H2O)

2020 ◽  
Vol 35 (4) ◽  
pp. 286-292
Author(s):  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Powder Diffraction ◽  
Density Functional ◽  
Minimum Energy ◽  
Hydroxyl Group ◽  
Powder Diffraction Data ◽  
Powder Diffraction File ◽  
Sulfate Anion ◽  
X Ray

The crystal structure of hyoscyamine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Hyoscyamine sulfate monohydrate crystallizes in space group P21 (#4) with a = 6.60196(2), b = 12.95496(3), c = 20.93090(8) Å, β = 94.8839(2)°, V = 1783.680(5) Å3, and Z = 2. Despite the traditional description as a dihydrate, hyoscyamine sulfate crystallizes as a monohydrate. The two independent hyoscyamine cations have different conformations, which have similar energies. One of the cations is close to the minimum-energy conformation. Each of the protonated nitrogen atoms in the cations acts as a donor to the sulfate anion. The hydroxyl group of one cation acts as a donor to the sulfate anion, while the hydroxyl group of the other cation acts as a donor to the water molecule. The water molecule acts as a donor to two different sulfate anions. The cations and anions are linked by complex chains of hydrogen bonds along the a-axis. The powder pattern has been submitted for inclusion in the Powder Diffraction File™ (PDF®).

U3TiSb5, U3VSb5, U3CrSb5, and U3MnSb5 with "Anti"-Hf5Sn3Cu Type Structure

1994 ◽  
Vol 49 (6) ◽  
pp. 747-752 ◽  
Author(s):  
Markus Brylak ◽  
Wolfgang Jeitschko
Keyword(s):  
Transition Metal ◽  
Single Crystals ◽  
Type Structure ◽  
Interatomic Distances ◽  
X Ray ◽  
Lattice Constants ◽  
Arc Melting ◽  
Metal Atoms ◽  
Transition Metal Atoms ◽  
Structure Factors

The title compounds have been prepared from the elemental components by arc-melting and subsequent annealing. Single crystals of U3TiSb5 and U3MnSb5 were obtained from a tin flux and their structures were determined from single-crystal X-ray data: P63/mcm, Z = 2; a = 913.9(2), c = 611.2(1) pm, R = 0.011 (233 structure factors, 14 variables) for U3TiSb5 and a = 916.8(2), c = 613.2(1) pm, R = 0.015 (427 structure factors, 14 variables) for U3MnSb5. The lattice constants of the isotypic compounds are: a = 908.2(2), c = 608.3(2) pm for U3VSb5 and a = 911.0(1), c = 611.5(1) pm for U3CrSb5. The structure of these antimonides may be regarded as an “anti”-type structure of Hf5Sn3Cu with the antimony atoms on the hafnium sites, while the positions of the uranium and transition metal atoms correspond to the positions of the tin and copper atoms. A comparison of the interatomic distances of U3TiSb5 with those of U3Sb4, USb2, and a-antimony suggests oxidation numbers according to (U+III)3Ti+IV(Sb1-III)3(Sb2-II)2, where the Sb2 atoms form weakly bonded chains

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