Solution-mediated and single-crystal to single-crystal transformations of cucurbit[6]uril host–guest complexes with dopamine

CrystEngComm ◽  
2020 ◽  
Vol 22 (4) ◽  
pp. 634-638 ◽  
Author(s):  
Oksana Danylyuk ◽  
Marta Worzakowska ◽  
Joanna Osypiuk-Tomasik ◽  
Volodymyr Sashuk ◽  
Karolina Kedra-Krolik
Keyword(s):  
Single Crystal ◽  
Crystal Lattice ◽  
Structural Transformations ◽  
Water Molecules ◽  
Macrocyclic Cavity

The structural transformations of cucurbit[6]uril–dopamine complexes are associated with loss of water molecules either from the macrocyclic cavity or from the crystal lattice.

scholarly journals Phase transformations in cucurbituril host-guest complexes

2014 ◽  
Vol 70 (a1) ◽  
pp. C646-C646
Author(s):  
Oksana Danylyuk ◽  
Karolina Kedra-Krolik ◽  
Marta Worzakowska ◽  
Joanna Osypiuk-Tomasik ◽  
Vladimir Fedin
Keyword(s):  
Single Crystal ◽  
Crystal Lattice ◽  
Supramolecular Assembly ◽  
Water Molecules ◽  
Guest Molecules ◽  
X Ray ◽  
Host Guest Complex ◽  
Crystallographic Study ◽  
Partial Dehydration ◽  
Structure Changes

The retention of crystallinity upon desolvation of molecular crystals is not common, as the molecules are rigidly and densely packed in the crystals and the original framework usually collapses once solvent is removed from the structure. However, in rare cases the host framework remains substantially unaffected by solvent (guest) removal yielding structure with open channels or discrete lattice voids that can show permanent porosity. [1] Furthermore, sometimes happens, the desolvation process proceeds as single-crystal to single-crystal transformation resulting in distortion and sliding of the structure, changes in conformation, coordination modes and/or space group. Here we would like to present crystallographic study and thermal analysis on the dehydration process of the crystalline supramolecular complex between macrocyclic host cucurbit[6]uril and dopamine. In the solid state the 1:1 host-guest complex assembles into hexameric tubes with water-filled interior channels. Another set of water channels is created between three neighboring tubes in the crystal lattice. The crystals of such supramolecular assembly are not stable when out from mother solution and immediately start to loose water upon exposure to air. However, despite severe cracking the crystals dried in air maintained their integrity and still gave satisfactory diffraction pattern. The X-ray analysis showed significant decrease in the unit cell volume of the partially dehydrated crystals that corresponds to the liberation of some of the water molecules from the channels. Moreover, the reorganization of dopamine guest molecules has occurred in the crystal lattice as a response to the escape of water molecules from the structure. The partial dehydration and reorganization of the supramolecular framework proceeds via a single-crystal to single-crystal mechanism.

Laser Raman polarization spectra of natural zeolite-natrolite

1981 ◽  
Vol 46 (12) ◽  
pp. 3043-3048 ◽  
Author(s):  
František Pechar ◽  
Ivan Gregora ◽  
Drahoš Rykl
Keyword(s):  
Single Crystal ◽  
Crystal Lattice ◽  
Natural Zeolite ◽  
Room Temperature ◽  
Water Molecules ◽  
Laser Raman ◽  
Polarization Spectra ◽  
Internal Vibrations

Raman polarization spectra of single crystal of natrolite Na2Al2Si3O10.2 H2O have been measured in the region 4 000 to 50 cm-1 at room temperature. The spectra have been measured in the conventional rectangular geometry. The found maxima of the polarization spectra of single crystal of the mineral investigated can be divided into four groups according to pertinence to individual vibrations: (i) translation and rotation vibrations of water molecules in interaction with the crystal lattice, (ii) internal vibrations of the bonds Al-O, Si-O inside the tetrahedrons, (iii) internal vibrations of bonds of the water molecules, (iv) external vibrations between the (Al,Si)O4 tetrahedrons.

Konkurrierende Liganden: Theophyllin als nicht- und stark koordinierender Ligand in Quecksilber(II)-Komplexen / Competing Ligands: Theophylline as Non- and Strongly Coordinating Ligand in Mercury(II) Complexes

2006 ◽  
Vol 61 (6) ◽  
pp. 758-765 ◽  
Author(s):  
Matthias Nolte ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Oxygen Atom ◽  
Water Molecule ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Water Molecules ◽  
Slow Evaporation ◽  
Monoclinic Symmetry ◽  
X Ray ◽  
Chloride Ligand

[{Hg(CF3)2}(ThpH)(H2O)](H2O) (1), [{Hg4(Thp)4}(ClO4)4(H2O)8](H2O)4 (2), [{Hg(ThpH)2} (NO3)](NO3) (3) and {Hg(Thp)Cl}(H2O) (4) (ThpH = theophylline, C7H8N4O2) have been synthesized by slow evaporation of aqueous solutions of the mercuric salts Hg(CF3)2, Hg(ClO4)2, Hg(NO3)2, or HgCl2 and theophylline. Their crystal structures were determined on the basis of single crystal X-ray data. The coordination polymers 1 and 2 crystallize with triclinic symmetry, P1̅ (no. 2), with a = 468.8(2), b = 1256.4(5), c = 1445.5(6) pm, α = 67.15(3), β = 89.21(3), γ = 89.40(3)° and a = 833.6(1), b = 1862.7(2), c = 2182.9(2) pm, α = 111.61(1), β = 90.98(1), γ = 95.51(1)°, respectively. 3 and 4 crystallize with monoclinic symmetry, Pc (no. 7), a =1194.1(1), b=1258.8(2), c=735.5(2) pm, β =96.96(2)° and P21/n (no. 14), a=1069.0(2), b =911.6(1), c=1089.9(2) pm and β = 96.87(2)°. In 1 the theophylline molecules are non-coordinating to mercury and leave the Hg(CF3)2 molecule unchanged. Only weak electrostatic attractions to one keto-oxygen atom of theophylline and one water molecule hold this co-crystallisate together. In 2, the theophyllinate anion, Thp−, strongly coordinates with both N(7) and N(9) to HgII forming a large ring with eight Hg atoms that incorporates the water molecules. One sort of nitrate ions in 3 is weakly attached to HgII with the theophylline molecules still bound strongly through N(9). The chloride ligand and the theophyllinate ion seem to have the same strengths as ligands in 4 as they are both attached to HgII with the shortest distances possible

Solid-state dynamics and single-crystal to single-crystal structural transformations in octakis(3-chloropropyl)octasilsesquioxane and octavinyloctasilsesquioxane

2017 ◽  
Vol 19 (40) ◽  
pp. 27516-27529 ◽  
Author(s):  
A. Kowalewska ◽  
M. Nowacka ◽  
M. Włodarska ◽  
B. Zgardzińska ◽  
R. Zaleski ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Transformations ◽  
Crystal Lattices ◽  
Thermally Induced ◽  
Crystal Structural

Thermally induced formation of symmetric crystal lattices in functional POSS proceeds via different mechanisms and results in unique reversible phenomena.

Magnetic field induced local structural transformations in the optically excited states 5F2 and 5F3 of HoFe3(BO3)4 single crystal

2019 ◽  
Vol 476 ◽  
pp. 177-182 ◽  
Author(s):  
A.V. Malakhovskii ◽  
S.L. Gnatchenko ◽  
I.S. Kachur ◽  
V.G. Piryatinskaya ◽  
I.A. Gudim
Keyword(s):  
Magnetic Field ◽  
Single Crystal ◽  
Excited States ◽  
Structural Transformations

scholarly journals Synthesis, Single Crystal Structural Investigation, Hirshfeld Surface Analysis, Thermoanalysis and Spectroscopic Study of Two New Cu(II) and Co(II) Transition-Metal Complexes

Crystals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 986
Author(s):  
Rim Boubakri ◽  
Mirosław Szybowicz ◽  
Mariola Sadej ◽  
Sarra Soudani ◽  
Frédéric Lefebvre ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Organic Ligand ◽  
Free Water ◽  
Pyrimidine Ring ◽  
Water Molecules ◽  
Absorption Bands ◽  
Infrared And Raman Spectroscopy ◽  
Homo And Lumo ◽  
Coordinated Water

Two new complexes, [Cu(dimpyr)2(H2O)2](NO3)2.2H2O (1) and (Hamdimpy)2[CoCl4].H2O (2), with the monodentate ligand 2-amino-6-methylpyrimidin-4-(1H)-one (dimpyr) and the countercation 4-amino-2,6-dimetylpyrimidium (Hamdimpy), respectively, were prepared and characterized by single crystal X-ray diffraction, elemental analysis and IR spectroscopy. In (1), the Cu(II) cation is tetracoordinated, in a square plan fashion, by two nitrogen atoms from the pyrimidine ring of the organic ligand and two oxygen atoms of two coordinated water molecules. In the atomic arrangement, the CuO2N2 square planes are interconnected via the formation of O-H…O hydrogen bonds involving both coordinated and free water molecules and NO3− nitrate anions to form inorganic layers parallel to the (a, b) plane at z = (2n + 1)/4. In (2), the central atom Co(II) is four-coordinated in a distorted tetrahedral fashion by four Cl− ions. The [CoCl4]2− tetrahedra are arranged parallel to the plane (110) at x = (2n + 1)/2 and the organic cations are grafted between them by establishing with them hydrogen bonds of CH…Cl and NH…Cl types. The vibrational absorption bands were identified by infrared and Raman spectroscopy. Intermolecular interactions were investigated via Hirshfeld surfaces and electronic properties such as HOMO and LUMO energies were derived. The two compounds were characterized by thermal analysis to determine their thermal behavior with respect to temperature.

scholarly journals Magnetically Oriented Powder Crystal to Indexing and Structure Determination

2014 ◽  
Vol 70 (a1) ◽  
pp. C1560-C1560
Author(s):  
Fumiko Kimura ◽  
Wataru Oshima ◽  
Hiroko Matsumoto ◽  
Hidehiro Uekusa ◽  
Kazuaki Aburaya ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Powder Diffraction ◽  
Diffraction Method ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Lattice Parameters

In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.

Crystal Structure of Calcium Picrate Pentahydrate: A New Eight-Coordinate Stereochemistry for [M(bidentate)2(unidentate)4]

1979 ◽  
Vol 32 (2) ◽  
pp. 301 ◽  
Author(s):  
V Diakiw ◽  
TW Hambley ◽  
DL Kepert ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Title Compound ◽  
Lattice Site ◽  
The Other ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triangular Face ◽  
X Ray

The crystal structure of the title compound, Ca(C6H2N307)2,5H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.049 for 1513 'observed' reflections. Crystals are orthorhombic, Pmab, a 24.169(6), b l0.292(7), c 8.554(2) �, Z 4. The stereochemistry about the calcium has not been observed previously for the system [M(bidentate)2- (unidentate)4]; in the present structure, the calcium is coordinated by a pair of bidentate picrate ligands and the four water molecules in an array in which three of the water molecules occupy a triangular face of a square antiprism, the overall array having m symmetry. The remaining water molecule occupies a lattice site with no close interaction with the other species.

Crystal structure of coalingite

1971 ◽  
Vol 38 (295) ◽  
pp. 286-294 ◽  
Author(s):  
J. Pastor-Rodriguez ◽  
H. F. W. Taylor
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Water Molecules ◽  
Structural Elements ◽  
Structural Element ◽  
X Ray ◽  
Octahedral Sites ◽  
Carbonate Ions ◽  
Disordered Layer ◽  
Ray Methods

SummaryThe crystal structure of coalingite (Mg10Fe2(OH)24(CO3)·2H2O) has been determined using single-crystal X-ray methods. The mineral is trigonal, with space group Rm, aH = 3·12, cH = 37·4 Å, Z = ½, and (0001) cleavage. The structure is of a layer type, and is based on a structural element about 12·5 Å thick in the c-direction and consisting of two brucite-like layers and one disordered layer containing carbonate ions and water molecules and resembling those in sjögrenite and pyroaurite. The unit cell comprises three of these structural elements stacked together in the c-direction. The Mg2+ and Fe3+ ions are randomly distributed among all the octahedral sites of the brucite-like layers. The structure closely resembles those of sjögrenite and pyroaurite, but has two brucite-like layers between each CO32−−H2O layer where these have one. There is a tendency to random interstratification, and the crystals appear to contain intergrown regions of brucite and of sjögrenite or pyroaurite. Coalingite-K probably has a similar structure, but with three brucite-like layers between each -H2O layer; its idealized formula is probably Mg16Fe2(OH)36(CO3).2H2O.

scholarly journals Spectral, Thermal, Crystal Structure, Hirshfeld Surface Analyses and Biological Activities of New Hydrazinium Dipicolinato Copper(II) Tetrahydrate

2019 ◽  
Vol 31 (8) ◽  
pp. 1755-1761
Author(s):  
K. Naresh ◽  
B.N. Sivasankar
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Water Clusters ◽  
Hirshfeld Surface ◽  
Water Molecules ◽  
X Ray ◽  
Biological Studies ◽  
Calf Thymus ◽  
Hydrazinium Cation

A new copper complex of pyridine-2,6-dicarboxylate containing hydrazinium cation, formulated as (N2H5)2[Cu(PDC)2]·4H2O (PDC = pyridine-2,6-dicarboxylate) has been synthesized from copper(II) nitrate, hydrazine hydrate and pyridine-2,6-dicarboxylic acid as a single crystal and characterized by elemental analysis and spectroscopic (IR and UV-visible), thermal (TG/DTG), single crystal X-ray diffraction and biological studies. A six-coordinate complex with a distorted octahedral geometry around Cu(II) ion is proposed and confirmed by X-ray single crystal method. The structure reveals that two pyridine-2,6-dicarboxylate species acting as tridentate ligands and hydrazinium cation present as a counter ion along with non-coordinated four water molecules. The structural units of copper(II) is mutually held by the hydrogen bonds and π···π and C–O···π interactions. The copper(II) complex is connected to one another via O–H···O hydrogen bonds, forming water clusters, which plays an important role in the stabilization of the crystal structure. In the water clusters, the water molecules are trapped by the cooperative association of coordination interactions as well as hydrogen bonds. Both cation and anion interactions and crystal from various types of intermolecular contacts and their importance were explored using Hirshfeld surface analysis. This indicates that O···H/H···O interactions are the superior interactions conforming excessive H-bond in the molecular structure. The interaction of copper(II) complex with calf thymus DNA (CT-DNA) was investigated by electronic absorption spectroscopic technique. The electronic evidence strongly shows that the compound interacts with calf thymus through intercalation with a binding constant of Kb = 5.7 × 104 M–1.

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