Serendipitous Isolation of a Trinuclear Silver Complex Containing a Bridging Tridentate Cyanide

1997 ◽  
Vol 50 (12) ◽  
pp. 1195 ◽  
Author(s):  
Chris M. Hartshorn ◽  
Peter J. Steel
Keyword(s):  
Single Crystal ◽  
Silver Complex ◽  
Two Dimensional ◽  
Asymmetric Unit ◽  
Cyanide Ion ◽  
Maximum Dimension ◽  
X Ray ◽  
Nitrate Anions ◽  
Silver Atoms

The X-ray structure of a single crystal of a complex of formula C34H33Ag3N15O6 is described (P 21/c, Z4, a 10·943(1), b 33·873(5), c 10·416(2) Å, β 102·54(1)°, R 0·0363). The asymmetric unit of this compound contains three silver atoms, two nitrate anions, a bridging tridentate cyanide ion, and one and a half molecules of the bridging tetrapodal ligand 1,2,4,5-tetrakis(pyrazol-1-ylmethyl)benzene. By virtue of the bridging nature of the ligand, these units further assemble into large macrocyclic rings, with a maximum dimension of >24 Å. These rings then interlock to produce an intriguing two-dimensional metallopolymeric network.

Crystal Structure of Eu2PdSi3

2003 ◽  
Vol 58 (10) ◽  
pp. 971-974 ◽  
Author(s):  
U. Ch. Rodewald ◽  
R.-D. Hoffmann ◽  
R. Pöttgen ◽  
E.V. Sampathkumaran
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Two Dimensional ◽  
Silica Tube ◽  
Variable Parameters ◽  
X Ray

Single crystals of Eu2PdSi3 were obtained from an arc-melted sample that was further annealed at 1020 K for seven days in a silica tube. The structure of Eu2PdSi3 was refined from single crystal X-ray diffractometer data: P6/mmm, a = 831.88(12), c = 435.88(9) pm, wR2 = 0.1175, 265 F2 values, and 13 variable parameters. It crystallizes with the U2RuSi3 structure, a superstructure of the AlB2 type. The palladium and silicon atoms form a planar two-dimensional [PdSi3] network. The two crystallographically different europium atoms have hexagonal prismatic coordinations Eu1Si12 and Eu2Pd4Si8. The Pd-Si and Si-Si distances within the [PdSi3] network are 244 and 236 pm, respectively.

Synthesis, Structure and Properties of Two-Dimensional Coordination Polymer Based on 3,5-di(benzimidazol-1-yl)pyridine

2020 ◽  
Vol 42 (2) ◽  
pp. 249-249
Author(s):  
Guo Jun Wu Guo Jun Wu
Keyword(s):  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Photocatalytic Degradation ◽  
Elemental Analysis ◽  
Solvothermal Reaction ◽  
Two Dimensional ◽  
Structure And Properties ◽  
X Ray Diffraction ◽  
X Ray

[Cu(L)(AIP)·1.5H2O]n (1) [L= 3,5-di(benzimidazol-1-yl)pyridine, H2AIP= 5-aminoisophthalic acid] was prepared by the solvothermal reaction, which was characterized by single-crystal X–ray diffraction, infrared spectroscopy, and elemental analysis. 1 exhibits an infinite two dimensional [Cu(AIP)]n sheet parallel to (0 1 1) crystal plane. Furthermore, complex 1 displays good photocatalytic degradation of methyl blue (MB).

scholarly journals Single-crystal neutron diffraction study of β-Cs3(HSO4)2[H2−x (S x P1−x )O4] (x ≃ 0.5) at 15 K

1999 ◽  
Vol 55 (3) ◽  
pp. 285-296 ◽  
Author(s):  
S. M. Haile ◽  
W. T. Klooster
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Local Structure ◽  
Unit Cell Volume ◽  
Structural Models ◽  
Neutron Diffraction Study ◽  
Unit Cell ◽  
Asymmetric Unit ◽  
X Ray ◽  
Anisotropic Displacement Parameters

The structure of β-Cs3(HSO4)2[H2−x (S x P1−x )O4] has been examined by single-crystal neutron diffraction at 15 K. The compound crystallizes in space group C2/c and contains four formula units in the unit cell, with lattice parameters a = 19.769 (9), b = 7.685 (2), c = 8.858 (3) Å and β = 100.60 (4)°. Refinement of P, S and H site occupancies indicated that the value of x (in the stoichiometry) is 0.500 (6). This, together with the unit-cell volume of 1322.8 (14) Å3, implies a density of 3.463 Mg m−3. The structure contains zigzag rows of XO4 anions, where X = P or S, that alternate, in a checkerboard fashion, with zigzag rows of Cs cations. Moreover, there is one proton site, H(3), with an occupancy of 0.25 and one X-atom site, X(1), that is occupied by 0.5 P and 0.5 S. These features are in general agreement with a previous X-ray structure determination carried out at 298 K. In contrast to the X-ray study, however, it was found that two different structural models adequately fit the diffraction data. In the first model, the proton vacancies and the P atoms were assumed to be randomly distributed over the H(3) and X(1) sites, respectively, and to have no impact on the local structure. In the second model, several atoms were assigned split occupancies over two neighboring sites, to reflect the presence or absence of a proton vacancy, and the presence of P or S on the X(1) site. Refinement assuming the first model, in which anisotropic displacement parameters for 12 of 14 atom sites in the asymmetric unit were employed, yielded residuals w R(F 2) = 0.084 and w R(F) = 0.038. For the second model, in which anisotropic displacement parameters were utilized for only the five atoms that were not split relative to the first model, the residuals were w R(F 2) = 0.081 and w R(F) = 0.036.

scholarly journals Use of Imaging Plates in X-Ray Analysis

1997 ◽  
Vol 29 (1-2) ◽  
pp. 89-101 ◽  
Author(s):  
M. Ermrich ◽  
F. Hahn ◽  
E. R. Wölfel
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Powder Diffraction ◽  
Polycrystalline Materials ◽  
Imaging Plate ◽  
Two Dimensional ◽  
X Ray ◽  
Working Principle ◽  
Imaging Plates

Two-dimensional detectors have opened a new area for the investigation of both single crystals and polycrystalline materials. The working principle of Imaging Plates is described. Some characteristics and the advantages of an Imaging Plate are discussed using the STOE Imaging Plate Diffraction System for different kinds of X-ray analysis: (i) single crystal diffractometry, (ii) powder diffraction and (iii) stress and texture investigations.

Structure of [(tmpp)2Ag]+2[Ag5I7]2-; an Unusual Ionic Adduct of Tris(2,4,6-trimethoxyphenyl)phosphine (tmpp) With Silver(I) Iodide

1992 ◽  
Vol 45 (11) ◽  
pp. 1909 ◽  
Author(s):  
LJ Baker ◽  
GA Bowmaker ◽  
y Effend ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Asymmetric Unit ◽  
Tertiary Phosphine ◽  
Polymeric Structure ◽  
Coordination Numbers ◽  
Ladder Polymer ◽  
Silver Atoms

A single-crystal structure determination is reported for [( tmpp )2Ag]+2 [Ag5I7]2-, a product isolated from the reaction of the highly basic, sterically hindered tertiary phosphine ligand tris (2,4,6-trimethoxypheny1) phosphine ( tmpp ) with silver(I) iodide. This complex is triclinic, P1, a 22.01(2), b 19.98(1), c 16.48(1) � , α 94.49(6), β 92.46(7), γ 116.76(5)',Z 2; R was 0.11 for 3436 'observed' reflections. The asymmetric unit contains two crystallographically inequivalent [( tmpp )2Ag]+ cations in which the silver atoms are quasi-linearly coordinated to two phosphorus atoms with P-Ag-P angles of 175.9(9) and 179(1)°, and a mean Ag-P distance of 2.38 � . The anion has a novel one-dimensionally polymeric structure which is based on a double-stranded 'ladder' polymer of AgI units to which are bonded one I- and one AgI2-unit for every four AgI units. In the resulting polymer, all silver atoms are four-coordinate, while iodide coordination numbers of two, three and four are observed, with associated Ag-I distances of 2.75-2.86(1), 2.72-2.91(1) and 2.90-3-08(1) � respectively.

Structure and Stereochemistry of Adducts of Tris(dipivaloylmethanato)europium(III), Eu(dpm)3, with Some Dipolar Aprotic Unidentate O-Donors

2020 ◽  
Vol 73 (6) ◽  
pp. 455
Author(s):  
Eric J. Chan ◽  
Jack M. Harrowfield ◽  
Brian W. Skelton ◽  
Alexandre N. Sobolev ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Dimethyl Sulfoxide ◽  
The Other ◽  
Asymmetric Unit ◽  
X Ray ◽  
Metal Atoms ◽  
Oxygen Donor ◽  
Trigonal Prismatic

Single crystal X-ray structural characterisations are reported for adducts of the form [(L-O)Eu(O,O′-dpm)3] obtained by the crystallisation of tris(dipivaloylmethanato)europium(iii) (dpm=[HC(C(tBu).CO)2]−) from an array of dipolar aprotic oxygen-donor solvents L (L=N-methylpyrrolidinone (nmp), trimethylphosphate, (MeO)3PO, (tmp), hexamethylphosphoramide (hmpa), dimethylacetamide (dma), dimethyl sulfoxide (dmso), and the bidentate octamethylpyrophosphoramide (ompa). In all adducts, the resulting arrays contain seven-coordinate metal atoms, which adopt two different isomeric forms of the mono-capped trigonal prismatic stereochemistry, the L=dma and dmso adducts corresponding to one type, nmp and tmp the other. The adduct formed with ompa behaves as a pair of discrete metal environments bridged by the O-ompa-O′ ligand, thus; [(dpm-O,O′)3Eu(O-ompa-O′)Eu(O,O′-dpm)3], and is found in two forms, one in which both Eu environments is of the tmp type, the other of the dmso/dma type. In the hmpa adduct, the asymmetric unit of the structure is a disordered composite of both types. In none of the adducts is there any further solvation beyond coordination of a single L.

Preparation and Crystal Structure Er (III) Complex with 2-Formylbenzenesulfonic Sodium-3-Thiosemicarbazide

2011 ◽  
Vol 396-398 ◽  
pp. 993-996
Author(s):  
Xi Shi Tai
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Layered Structure ◽  
Ir Spectrum ◽  
Two Dimensional ◽  
Single Crystal Diffraction ◽  
Element Analysis ◽  
X Ray ◽  
Complex Forms

A novel ligand containing sulfonic has been synthesized using 2-formylbenzenesulfonic sodium and 3-thiosemicarbazide as starting materials, and a Er (III) complex was synthesized. The ligand was characterized by element analysis and IR spectrum. The crystal structure of the Er (III) complex was determined by X-ray single crystal diffraction. The results showed that the compound was triclinic, with P-1, a = 1.0596(4) nm, b = 1.3700(5) nm, c = 1.8305(7) nm, V = 2.4726(16) nm3, Z=2, M r= 1244.42, De =1.671 g/cm3, T = 273(2) K, F (000) = 1270, R = 0.0517 and wR = 0.1124. The complex forms two-dimensional layered structure through hydrogen bonds and π-π stacking.

scholarly journals Dynamics of Water in Crystal Hydrates

1967 ◽  
Vol 22 (9) ◽  
pp. 1440-1451 ◽  
Author(s):  
Ingo Berthold ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Dynamical Behaviour ◽  
Water Molecules ◽  
Intensity Data ◽  
Two Dimensional ◽  
Fourier Synthesis ◽  
Hydrogen Atoms ◽  
X Ray ◽  
H Nmr

The crystal structure of Na2S2O6·2 H2O has been refined by means of single crystal X-ray intensity data. The structure of the isotypic Li2S2O6·2 H20 was also determined by single crystal studies. Two dimensional differential FOURIER synthesis revealed the approximate positions of the hydrogen atoms. From 1H-NMR investigations, the crystal structure, and information gained by IR spectroscopy the complete atomic arrangement in these two substances was obtained. The influence of the dynamical behaviour of the water molecules is taken into account in determining the hydrogen positions.

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