Syntheses and Spectroscopic Studies of Some New Diazaphospholes and Diazaphosphorinanes. Crystal Structure of 4

2005 ◽  
Vol 60 (10) ◽  
pp. 1021-1026 ◽  
Author(s):  
Khodayar Gholivand ◽  
Zahra Shariatinia ◽  
Mehrdad Pourayoubi ◽  
Sedigheh Farshadian
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Spectroscopic Studies ◽  
Coupling Constants ◽  
Crystalline Lattice ◽  
Polymeric Chain ◽  
Ring Strain ◽  
One Dimensional ◽  
X Ray ◽  
X Ray Crystallography

New diazaphospholes and diazaphosphorinanes with formula were synthesized and characterized by 1H, 13C, 31P NMR and IR spectroscopy and elemental analysis. The structure of compound 1 has been determined by X-ray crystallography. A one-dimensional polymeric chain was observed in the crystalline lattice produced by intermolecular -P=O. . .H-N- and -C=O. . .H-N-hydrogen bonds. Compounds 1 and 2 contain five-membered rings and show high values for 2J(PNH) and 2J(P,C) coupling constants due to the ring strain. These constants are reduced seriously in compounds with six-membered rings. In compound 6 with CCl3C(O)NH moiety, all phosphorus-hydrogen couplings are zero.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

A Zinc(II)-Silver(I) Bimetallic Coordination Polymer Assembled Through Argentophilic and π-π Interactions, f[Zn(phen)2(H2O) {Ag(CN)2g][Ag(CN)2]·MeOH}n (phen=1,10-Phenanthroline)

2013 ◽  
Vol 68 (2) ◽  
pp. 161-167 ◽  
Author(s):  
Muhammad Monim-ul-Mehbooba ◽  
Muhammad Ramzan ◽  
Tobias Rüffe ◽  
Heinrich Lang ◽  
Shafqat Naddem ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Hydrogen Bonds ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography ◽  
3D Network ◽  
Argentophilic Interactions

A cyanido-bridged Zn(II)-Ag(I) bimetallic coordination polymer, {[Zn(phen)2(H2O){Ag(CN)2}] [Ag(CN)2]·MeOH}n (1), was prepared using ZnCl2, 1,10-phenanthroline (phen) and K[Ag(CN)2] and characterized by IR spectroscopy, thermal analysis and X-ray crystallography. The crystal structure of 1 consists of dinuclear [Zn(phen)2(H2O){Ag(CN)2}]+ cations, [Ag(CN)2]- anions and a methanol molecule. The non-coordinated [Ag(CN)2]- anions are linked to the [Zn(phen)2(H2O){Ag(CN)2}]+ complex cations through argentophilic interactions leading to the formation of chains. The chains are connected by hydrogen bonds and π-π interactions to give a 3D network.

scholarly journals Comparison of the Photochemical Reaction of Photoactive Yellow Protein in Crystal with Reaction in Solution1

2003 ◽  
Vol 17 (2-3) ◽  
pp. 345-353 ◽  
Author(s):  
Eriko Mano ◽  
Hironari Kamikubo ◽  
Yasushi Imamoto ◽  
Mikio Kataoka
Keyword(s):  
Photochemical Reaction ◽  
Structural Changes ◽  
Spectroscopic Studies ◽  
Crystalline Lattice ◽  
Photoactive Yellow Protein ◽  
X Ray ◽  
X Ray Crystallography ◽  
Solution Condition ◽  
Active Intermediate ◽  
Ectothiorhodospira Halophila

Photoactive yellow protein (PYP) is a photoreceptor protein for the negative phototaxis ofEctothiorhodospira halophila. The crystal structures of several photo‒intermediates have been revealed by X-ray crystallography. In the crystal structure of the active intermediate, PYPM, no significant structural changes were observed except for the vicinity of the chromophore. On the contrary, spectroscopic studies with solution condition demonstrated that global structural changes occur during the photo‒cycle. In order to reveal the origin of the discrepancies, we measured the reaction kinetics upon illumination under crystal condition and to compare them with those observed under solution condition. The reactive portion decreases with the increase of crystallinity. The rate constant of PYPMdecay also decreases with the increase of crystallinity. These results suggest two possibilities: (1) PYP in crystal does not react by the illumination; (2) the photoreaction rate is highly accelerated in crystal. Consequently, the photoreaction in crystal is considered to be highly influenced by the force constraint from crystalline lattice.

scholarly journals Crystal structure of an oxalate-bridged tetranuclear 8-hydroxyquinoline Zn(II) cluster: [Zn4Q6(Ox)]0.5n

2011 ◽  
Vol 76 (4) ◽  
pp. 529-537 ◽  
Author(s):  
Jiajun Wang ◽  
Qiang Wang ◽  
Yanjun Sun ◽  
Yuemei Wang ◽  
Guosheng Zhao ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Stacking Interactions ◽  
Monoclinic System ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polymeric Chains

The chain structure of a tetranuclear zinc(II) cluster [Zn4Q6(Ox)]0.5n ([Zn4 (C9H6NO)6(C2O4)]0.5n) (1) (Q = 8- hydroxyquinoline anion, Ox = oxalate dianion) was determined by X-ray crystallography and characterized by elemental analysis, IR spectroscopy and thermal analysis. It crystallizes in the monoclinic system, space group P21/n (No. 14), with the lattice parameters a = 13.2222(15) ?, b = 11.0566(12) ?, c = 16.2224(18) ?, ? = 92.1770(10)?, V = 2369.9(5) ?3, Z = 4, Mr = 607.23 g mol-1, Dc = 1.702 g cm-3. The tetranuclear zinc(II) clusters form 1D polymeric chains parallel to the b-axis. The ?-? stacking interactions involving aryl rings support the formation of the 1D polymeric structure. The neighboring polymeric chains are connected by C-H???? interactions.

scholarly journals Why crystal structure analysis works: a one-dimensional crystallography teaching tool

2015 ◽  
Vol 48 (3) ◽  
pp. 901-905 ◽  
Author(s):  
A. Alan Pinkerton
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Teaching Tool ◽  
One Dimensional ◽  
X Ray ◽  
X Ray Crystallography ◽  
Scientific Calculator ◽  
Hypothetical Structure

A teaching tool is proposed to help beginner students of crystallography understand how crystallographic calculations work. Examples of the most important methods taught in X-ray crystallography courses have been adapted to a one-dimensional hypothetical structure. All calculations can be carried out in class with a scientific calculator or by using a simple spreadsheet.

Crystal Structure of an Ammonium Dithiocyanatocuprate(I) Complex with 18-Crown-6, [NH4(18-Crown-6){Cu(NCS)2}] Obtained from Zero Valent Metal

1997 ◽  
Vol 52 (11) ◽  
pp. 1311-1314 ◽  
Author(s):  
Julia A. Manskaya ◽  
Volodimir N. Kokozay ◽  
Konstantin V. Domasevitch
Keyword(s):  
Crystal Structure ◽  
Direct Method ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
X Ray Crystallography ◽  
A Direct Method

The new macrocyclic dithiocyanatocuprate(I) complex [NH4(18-crown-6){Cu(NCS)2}] has been prepared using a direct method of interaction and characterized by X-ray crystallography (orthorhombic, space group Cmc21, with a = 12.453(2), b = 21.650(4), c = 8.151(2) Å, V = 2197.6(8) Å3, Z = 4 , R1 (F) = 0.054; wR2(F2) = 0.141 for 972 unique reflections with I > 2σ(I) and R1(F) = 0.082; w/?2(F2) = 0.210 for all 1098 unique reflections). The lattice comprises complex cations [NH4(18-crown-6)]+ and infinite polymeric anions [Cu(NCS)2]- of a one-dimensional zig-zag structure. The copper atoms adopt three-fold coordination [CuN2S] (Cu-N 1,89( 1), 1,90( 1) Å; Cu-S 2.278(4) Å).

Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2ClSnO2PMe2

1998 ◽  
Vol 53 (7) ◽  
pp. 699-703 ◽  
Author(s):  
Abdel-Fattah Shihada ◽  
Frank Weller
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Studies ◽  
Chain Structure ◽  
Polymeric Chain ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Axis Of Symmetry ◽  
Ir Bands ◽  
Distorted Trigonal Bipyramidal

Abstract Diethylchlorotin dimethylphosphinate has been synthesized by treating (Et2ClSn)2O with HO2PMe2 in toluene. Single crystal X-ray analysis shows that O2PMe2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The Sn-Cl bond lies on a C2 axis of symmetry in the (C2v) OCClSnCO unit. Et2ClSnO2PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, β= 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSnO2PMe2 are assigned and the mass spectrum is reported and discussed.

Hydrothermal Synthesis, Crystal Structure and Properties of a Novel 3D Metal-Organic Cd(II) Coordination Polymer Based on Helical Units

2013 ◽  
Vol 68 (2) ◽  
pp. 127-132
Author(s):  
Hai-Hua Li ◽  
Peng Zhang ◽  
Jia-Yi Pu ◽  
Yu-Ying Zhao ◽  
Chong-Zhen Mei
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Elemental Analysis ◽  
Metal Organic Framework ◽  
Structure And Properties ◽  
X Ray ◽  
X Ray Crystallography ◽  
Metal Organic

A metal-organic framework based on 4-methylphthalic acid (H2L) and 4,4’-bipyridine (bpy), namely {[Cd(L)(bpy)1:5]·2(H2O)}n (1), has been synthesized hydrothermally and characterized by IR spectroscopy, elemental analysis, thermogravimetry, and single-crystal X-ray crystallography. Complex 1 exhibits a 3D coordination network based on layers. Each layer consists of left- or right-handed {Cd-L-Cd-bpy-Cd-L-Cd-bpy}n double helices.Water molecules are also incorporated in the network. Compound 1 shows fluorescence at ca. 360 nm upon excitation at 304 nm.

The synthesis, crystal structure and magnetic properties of a one-dimensional terbium(III)–octacyanidomolybdate(V) assembly

2014 ◽  
Vol 70 (12) ◽  
pp. 1169-1173 ◽  
Author(s):  
Hong Shen
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Ir Spectroscopy ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Cyanide Ligands ◽  
Ferromagnetic Interactions

A one-dimensional cyanide-bridged coordination polymer, poly[[aquadi-μ-cyanido-κ4C:N-hexacyanido-κ6C-(dimethylformamide-κO)bis(3,4,7,8-tetramethyl-1,10-phenanthroline-κ2N,N′)terbium(III)molybdate(V)] 4.5-hydrate], [MoTb(CN)8(C16H16N2)2(C3H7NO)(H2O)]·4.5H2O}n, has been prepared and characterized through IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The compound consists of one-dimensional chains in which cationic [Tb(tmphen)2(DMF)(H2O)]3+(tmphen is 3,4,7,8-tetramethyl-1,10-phenanthroline) and anionic [MoV(CN)8]3−units are linked in an alternating fashion through bridging cyanide ligands. Neighbouring chains are connected by three types of hydrogen bonds (O—H...O, O—H...N and C—H...O) and by π–π interactions to form a three-dimensional supramolecular structure. In addition, magnetic investigations show that ferromagnetic interactions exist in the compound.

scholarly journals Crystal structure, thermal behavior and spectroscopic studies of a new organic hydrogen arsenate

2013 ◽  
Vol 9 (2) ◽  
pp. 1953-1964
Author(s):  
Sami Soukrata ◽  
Mohamed Belhouchet ◽  
Karim Adil ◽  
Tahar Mhiri
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Protonic Conduction ◽  
Structure Directing Agent ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network ◽  
The One

The present paper undertakes the study of a title organic-inorganic hybrid material 2-amino-3-benzyloxy pyridinium dihydrogenmonoarsenate, [C12H13N2O]H2AsO4, which has been synthesized by slow evaporation at room temperature using 2-amino-3-benzyloxypyridine as the structure-directing agent. The structure was determined by single-crystal X-ray diffraction at 296 K. This compound is crystallized in the noncentrosymmetric orthorhombic space group P212121 with the lattice parameters a = 4.89 (7), b = 10.41 (1), c = 26.79 (3) Å, V = 1364.3 (3) Å3, and Z = 4. The crystal structure has been determined and refined to R1 = 0.0363 and wR2 = 0.1246 using 5438 independent reflections. The atomic arrangement can be described by infinite anionic chains running parallel to the [100] direction. The organic entities are located between these chains. H-bonds connecting the different species play an important role in the one-dimensional network cohesion. This compound is also characterized by solid-state 13C MAS NMR, IR, Raman spectroscopy and TG-ATD thermal analysis. Moreover, protonic conduction of this compound determined by impedance has been studied in the temperature range 299 - 403 K.

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