Synthesis and crystal structure of an M
                  4
                  L
                  6 tetrahedral cage with outward-facing pockets from a substituted pyrazolyl–pyridine ligand

The self-assembly of metal–polydentate ligands to give supramolecular tetrahedral complexes is of considerable current interest. A new ligand, 4-benzyl-2-[1-(2-{[3-(4-benzylpyridin-2-yl)-1H-pyrazol-1-yl]methyl}benzyl)-1H-pyrazol-3-yl]pyridine (L), with chelating pyrazolyl–pyridine units substituted on the 4-position of the pyridyl ring with benzyl units, has been synthesized and fully characterized. The self-assembly of L with cobalt(II) gave rise to a tetrahedral cage (hexakis{μ-4-benzyl-2-[1-(2-{[3-(4-benzylpyridin-2-yl)-1H-pyrazol-1-yl]methyl}benzyl)-1H-pyrazol-3-yl]pyridine}perchloratotetracobalt(II) octakis(perchlorate) acetonitrile undecasolvate, [Co4(ClO4)(C38H32N6)6](ClO4)7·11CH3CN) with approximate T symmetry. The X-ray crystal structure of the cage, i.e. [Co4 L 6\subsetClO4](ClO4)7, shows that the substituted benzyl groups are oriented away from the centres of their respective ligands towards the CoII vertices, making small outward-facing pockets from three benzyl rings at the corners of the tetrahedron.

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DIRECT SYNTHESIS AND CRYSTAL STRUCTURE OF BIS(BROMIDO-BIS(1,10 PHENANTHROLINE)-COPPER(II)) NITROPRUSSIDE DIMETHYLFORMAMIDE SOLVATE

Bulletin of Taras Shevchenko National University of Kyiv Chemistry ◽

10.17721/1728-2209.2018.1(55).3 ◽

2018 ◽

pp. 15-18

Author(s):

O. Vassilyeva ◽

E. Buvaylo ◽

B. Skelton

Keyword(s):

Crystal Structure ◽

Self Assembly ◽

Direct Synthesis ◽

Solvent Molecule ◽

The Self ◽

Coordination Geometry ◽

Synthesis And Crystal Structure ◽

Copper Coordination ◽

Bromide Ion ◽

Nitroprusside Anion

The title compound, [Cu(C12H8N2)2Br]2[Fe(CN)5(NO)]·C3H7NO, was prepared by the self-assembly of nitroprusside anion and Cu cation containing a bidentate amine in the reaction of copper powder and sodium nitroprusside with NH4Br and 1,10-phenanthroline (phen) in dimethylformamide (DMF). The complex is formed of discrete [Cu(phen)2Br]+ cations, nitroprusside [Fe(CN)5(NO)]2– anions and DMF molecules of crystallization. The cation has no crystallographically imposed symmetry; the metal atom coordinates two nitrogen atoms of two phen molecules and bromide ion. The copper coordination geometry is intermediate between a square pyramid and a trigonal bipyramid. The [Fe(CN)5(NO)]2– anion is located on an inversion centre with the nitrosyl group modelled as disordered with one of the CN groups. The DMF solvent molecule was found to be disordered about the crystallographic inversion centre; geometries were restrained to ideal values. In the solid state, alternating layers of cations and of anions plus DMF molecules are stacked along the b axis.

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Functionalized 1,1-Ethene Dithiolates as Ligands, V [1]. Synthesis and Crystal Structure of Palladium(II) and Platinum(II) Complexes with Dithioylidene Barbituric Acid Ligands. Molecular Structure of a 2,6-Diaminopyridine-Platinum(II) Barbiturate Complex

Zeitschrift für Naturforschung B ◽

10.1515/znb-1998-1009 ◽

1998 ◽

Vol 53 (10) ◽

pp. 1135-1143 ◽

Cited By ~ 6

Author(s):

Wolfgang Weigand ◽

Veronika Plener ◽

Heinrich Nöth ◽

Ingo Krossing ◽

Jörg Knizek ◽

...

Keyword(s):

Molecular Structure ◽

Crystal Structure ◽

Hydrogen Bonding ◽

Structural Analysis ◽

Self Assembly ◽

Barbituric Acid ◽

Supramolecular Complex ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Multiple Hydrogen Bonding

AbstractThe 1,1-ethene dithiolato ligands (dithioylidene barbituric acids) 2a-f react with palladium(II) and platinum(II) compounds L2MCI2 [M = Pd, Pt; L = PEt3, PBu3, PPh3, 1/2 dppe, 1/2 (-)-DIOP, 1/2 2,9-dimethyl phenanthroline] to give the 1,1-ethene dithiolato metal complexes . Compound 4a forms a 1:1 adduct (8) with 2,6-diaminopyridine. The compounds were characterised on the basis of their IR and NMR (1H, 13C, 31P) spectra. Complexes 4a, 4c, and 5a were further studied by X-ray structural analysis. The barbituric unit in 4a undergoes self-assembly through multiple hydrogen-bonding with complementary 2 ,6-diaminopyridine yielding the supramolecular complex 8

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3,3′-{(1E,2E)-Hydrazine-1,2-diylidenedi[(E)methylylidene]}dibenzene-1,2-diol (BCAz-H4): an easy to prepare but very useful building block for the self-assembly of triple-stranded helicates; the X-ray crystal structure of Na4[(BCAz)3Ti2]·7 dmf·H2O

Polyhedron ◽

10.1016/s0277-5387(02)01395-5 ◽

2003 ◽

Vol 22 (5) ◽

pp. 643-647 ◽

Cited By ~ 22

Author(s):

Markus Albrecht ◽

Susanne Kamptmann ◽

Roland Fröhlich

Keyword(s):

Crystal Structure ◽

Self Assembly ◽

Building Block ◽

The Self ◽

X Ray

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Synthese und Kristallstruktur von [WCl3(N 3S2)(Pyridin)] / Synthesis and Crystal Structure of [WCl3(N3S2)(Pyridine)]

Zeitschrift für Naturforschung B ◽

10.1515/znb-1986-0624 ◽

1986 ◽

Vol 41 (6) ◽

pp. 796 ◽

Cited By ~ 4

Author(s):

Heribert Wadle ◽

Elke Conradi ◽

Ulrich Müller ◽

Kurt Dehnicke

Keyword(s):

Crystal Structure ◽

Crystal Data ◽

Pyridine Ligand ◽

Tungsten Atom ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Distorted Octahedral Coordination ◽

Distorted Octahedral ◽

In Trans ◽

Moisture Sensitive

[WCl3(N3S2)(pyridine)] was obtained by the reaction of a mixture of S5N5[WCl4(N3S2)] and S4N3[WCl4(N3S2)] with pyridine in dichloromethane. It forms brown, moisture-sensitive crystal plates and was characterized by its IR spectrum and an X-ray crystal structure determination (1404 observed reflexions. R = 0.052). Crystal data: orthorhombic, space group Pbca. Z = 8, a = 708.3, b = 1275.4, c = 2628.6 pm. The tungsten atom has a distorted octahedral coordination and is part of a planar WN3S2 ring with WN bond lengths of 176 and 186 pm. The pyridine ligand (W−N 232 pm) is in trans position to the shorter WN bond.

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Organic NLO material with H-bonded 1D helical self-assembly: synthesis, X-ray crystal structure, DFT calculations, SHG measurements and thermal studies of (5Z,6E)-1,10-phenanthroline-5,6-dione dioxime

CrystEngComm ◽

10.1039/c7ce00743d ◽

2017 ◽

Vol 19 (35) ◽

pp. 5251-5258 ◽

Cited By ~ 8

Author(s):

A. Irudaya Jothi ◽

V. Alexander

Keyword(s):

Crystal Structure ◽

Dft Calculations ◽

Self Assembly ◽

Thermal Studies ◽

The Self ◽

X Ray ◽

Shg Efficiency

The role of H-bonding in the self-assembly of (5Z,6E)-1,10-phenanthroline-5,6-dione dioxime into a 1D helix and its SHG efficiency are reported.

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High-pressure synthesis and crystal structure of the mixed-cation borate Ga4In4B15O33(OH)3

Zeitschrift für Naturforschung B ◽

10.1515/znb-2019-0014 ◽

2019 ◽

Vol 74 (4) ◽

pp. 357-363

Author(s):

Daniela Vitzthum ◽

Hubert Huppertz

Keyword(s):

Crystal Structure ◽

High Pressure ◽

High Temperature ◽

Diffraction Data ◽

X Ray Diffraction ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Mixed Cation ◽

High Pressure High Temperature ◽

Pressure Synthesis

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.

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The Evaluation of TiTe2 as a Diffusion Barrier in the Formation of Low Thermal Conductivity Nanolaminates with Bi2Te3 and Sb2Te3

Advances in Science and Technology ◽

10.4028/www.scientific.net/ast.74.38 ◽

2010 ◽

Vol 74 ◽

pp. 38-47

Author(s):

Clay Mortensen ◽

Paul Zschack ◽

David C. Johnson

Keyword(s):

Thermal Conductivity ◽

Diffusion Barrier ◽

Self Assembly ◽

Low Temperatures ◽

Annealing Temperature ◽

The Self ◽

High Angle ◽

X Ray Diffraction ◽

Amorphous Precursor ◽

X Ray

The evolution of designed [(Ti-Te)]x[(Sb-Te)]y, [(Bi-Te)]x[(Sb-Te)]y, [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]y and [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors were followed as a function of annealing temperature and time using both low and high angle x-ray diffraction techniques to probe the self assembly into nanolaminate materials. The [(Bi-Te)]x[(Sb-Te)]y precursors were found to interdiffuse at low temperatures to form a (BixSb1-x)2Te3 alloy. The [(Ti-Te)]x[(Bi-Te)]y and [(Ti-Te)]x[(Sb-Te)]y precursors formed ordered nanolaminates [{(TiTe2)}1.35]x[Bi2Te3]y and [{(TiTe2)}1.35]x[Sb2Te3]y respectively. The [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]x precursors formed [{(TiTe2)}1.35]w[(Bi0.5Sb0.5)2Te3]2x nanolaminates on annealing, as the bismuth and antimony layers interdiffused. Over the range of TiTe2 thicknesses used in [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors, Bi and Sb were found to interdiffuse through the 2-4 nm thick Ti-Te layers, resulting in the formation of (BixSb1-x)2Te3 alloy layers as part of the final nanolaminated products. When the Bi-Te and Sb-Te thicknesses were equal in the amorphous precursors, symmetric [{(TiTe2)}1.35]m[(Bi0.5Sb0.5)2Te3]n nanolamiantes were formed. When the thicknesses of Bi-Te and Sb-Te layers were not equal in the amorphous precursor, asymmetric [(TiTe2)1.35]m[(BixSb1-x)2Te3]n[(TiTe2)1.35]m[(BixSb1-x)2Te3]p nanolaminates were formed. These results imply that to form (A)w(B)x(C)y nanolaminates using designed layered precursors all three components must be immiscible. To form (A)x(B)y(A)x(C)z nanolaminates, the components must be immiscible or the precursor to the A component and the A component itself must be an effective interdiffusion barrier preventing B and C from mixing.

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Synthesis and Crystal Structure of the Flexible Ligand Coordination Polymer [Co3(bpd)5.5(NCS)6(NH3)]n⋅2H2O(bpd= 1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene)

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.803.80 ◽

2013 ◽

Vol 803 ◽

pp. 80-84

Author(s):

Yu Qi Liu ◽

Yong Yang ◽

Rui Yang ◽

Xiao Jun Xu

Keyword(s):

Crystal Structure ◽

Infrared Spectroscopy ◽

Coordination Polymer ◽

Single Crystal ◽

X Ray Diffraction ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Elemental Analyses ◽

Ligand Coordination ◽

Point Symbol

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).

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Synthesis and crystal structure of (Ag,Pd)22Se6

Powder Diffraction ◽

10.1017/s0885715612000929 ◽

2013 ◽

Vol 28 (1) ◽

pp. 13-17 ◽

Cited By ~ 1

Author(s):

F. Laufek ◽

A. Vymazalová ◽

D.A. Chareev ◽

A.V. Kristavchuk ◽

J. Drahokoupil ◽

...

Keyword(s):

Crystal Structure ◽

Diffraction Data ◽

Glass Tube ◽

Structure Type ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Cell Parameters ◽

Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

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