scholarly journals Synthesis, Crystal Structure and Computational Studies of 1-Phenylpiperazin-1,4-Diium Nitrate Monohydrate

2012 ◽  
Vol 9 (2) ◽  
pp. 772-779 ◽  
Author(s):  
H. Marouani ◽  
N. Raouafi ◽  
S. Toumi Akriche ◽  
S. S. Al-Deyab ◽  
M. Rzaigui
Keyword(s):  
Crystal Structure ◽  
Ground State ◽  
Ground State Structure ◽  
Computational Studies ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Moller Plesset ◽  
Homo Lumo

Reaction of phenylpiperazine and nitric acid yields the new organicinorganic hybrid material of phenylpiperazinium (C10H16N2)(NO3)2.H2O, (I). To understand the interaction between components of this salt, single crystal structure and computational studies are performed and reported. X-ray diffraction analysis was employed for the structural characterization. Computational methods were exploited for ground state structure determination and HOMO-LUMO calculations were determined. Detailed studies on ground state structure determinations as well as Electrostatic Potential Surface maps have been estimated by applying second-order Møller- Plesset (MP2) perturbation theory.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Structure, Stereochemistry and Novel 'Hydrogen Bonding' in Two Bipyridinium Salts of the B10H102- Anion

1987 ◽  
Vol 40 (12) ◽  
pp. 2097 ◽  
Author(s):  
DJ Fuller ◽  
DL Kepert ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Charge Transfer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Structure Determinations ◽  
Positively Charged

Crystal structure determinations of (LH)2(B10H10), (1), and (LH2)(B10H10), (2), L = 2,2'- bipyridine , have been carried out by single-crystal X-ray diffraction methods at 295 K, being refined by full-matrix least squares to residuals of 0.041, 0.047 for 1758, 1771 'observed' independent reflections respectively. Crystals of (1) are monoclinic, P21/n, a 12.040(7), b 17.71(1), c 11.142(4) �, β 101.78(4)�, Z 4. Crystals of (2) are monoclinic, P21/c, a 9.937(4), b 10.837(3), c 14.856(5) �, β 109 2l(3)�, Z 4. The colour of the compounds is accounted for by charge-transfer interactions of a novel type, namely between the positively charged cationic acid hydrogen atoms and the negatively charged non-apical hydrogen atoms of the anion. In yellow (1), these distances are 2.26(5) �, while in red (2), they are much shorter, being 1.89(4), 1.97(3) �.

Synthesis of Triferrocenylbenzenes by Tantalum(V)-Catalyzed Cyclotrimerization of Ethynylferrocene. The Crystal Structure of 1,3,5-Triferrocenylbenzene

1997 ◽  
Vol 62 (10) ◽  
pp. 1577-1584 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová ◽  
Jan Sedláček ◽  
Jiří Vohlídal ◽  
Miroslav Polášek
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
High Yield ◽  
Isomer Mixture ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Yield Formation

Exclusive, high-yield formation of the cyclotrimers of ethynylferrocene (1) was observed when TaCl5 in benzene was employed as catalyst. Analysis of the resulting isomer mixture by means of HPLC and 1H NMR revealed the presence of 1,3,5-triferrocenylbenzene (sym-2) and 1,2,4-triferrocenylbenzene (asym-2) in the ratio of 4 : 6. A small amount of pure sym-2 isomer was isolated, and its solid-state structure was established by single-crystal X-ray diffraction. The molecules of sym-2 possess a distorted up-up-down arrangement of the ferrocenyl groups attached to the benzene ring.

scholarly journals Crystal structures of cristobalite-type and coesite-type PON redetermined on the basis of single-crystal X-ray diffraction data

2015 ◽  
Vol 71 (11) ◽  
pp. 1325-1327 ◽  
Author(s):  
Maxim Bykov ◽  
Elena Bykova ◽  
Vadim Dyadkin ◽  
Dominik Baumann ◽  
Wolfgang Schnick ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Rotation Axis ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Anisotropic Displacement Parameters

Hitherto, phosphorus oxonitride (PON) could not be obtained in the form of single crystals and only powder diffraction experiments were feasible for structure studies. In the present work we have synthesized two polymorphs of phosphorus oxonitride, cristobalite-type (cri-PON) and coesite-type (coe-PON), in the form of single crystals and reinvestigated their crystal structures by means of in house and synchrotron single-crystal X-ray diffraction. The crystal structures ofcri-PON andcoe-PON are built from PO2N2tetrahedral units, each with a statistical distribution of oxygen and nitrogen atoms. The crystal structure of thecoe-PON phase has the space groupC2/cwith seven atomic sites in the asymmetric unit [two P and three (N,O) sites on general positions, one (N,O) site on an inversion centre and one (N,O) site on a twofold rotation axis], while thecri-PON phase possesses tetragonalI-42dsymmetry with two independent atoms in the asymmetric unit [the P atom on a fourfold inversion axis and the (N,O) site on a twofold rotation axis]. In comparison with previous structure determinations from powder data, all atoms were refined with anisotropic displacement parameters, leading to higher precision in terms of bond lengths and angles.

scholarly journals Some reflections on symmetry: pitfalls of automation and some illustrative examples

2019 ◽  
Vol 75 (12) ◽  
pp. 1812-1819 ◽  
Author(s):  
William Clegg
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Structure Validation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Basic Concepts ◽  
Software Automation

In the context of increasing hardware and software automation in the process of crystal structure determination by X-ray diffraction, and based on conference sessions presenting some of the experience of senior crystallographers for the benefit of younger colleagues, an outline is given here of some basic concepts and applications of symmetry in crystallography. Three specific examples of structure determinations are discussed, for which an understanding of these aspects of symmetry avoids mistakes that can readily be made by reliance on automatic procedures. Topics addressed include pseudo-symmetry, twinning, real and apparent disorder, chirality, and structure validation.

Crystallographic and computational studies of a new organoarsenate compound: o-anisidinium dihydroarsenate

2019 ◽  
Vol 75 (2) ◽  
pp. 128-134
Author(s):  
Ali Harchani ◽  
Damian Trzybiński ◽  
Sylwia Pawlędzio ◽  
Krzysztof Woźniak ◽  
Amor Haddad
Keyword(s):  
Crystal Structure ◽  
Solution Method ◽  
Theoretical Calculations ◽  
Hirshfeld Surface ◽  
Computational Studies ◽  
Supramolecular Architecture ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Electrophilic Reactivity

The crystal structure and the results of theoretical calculations for the new organoarsenate salt o-anisidinium dihydroarsenate (systematic name: 2-methoxyanilinium dihydrogen arsenate), C7H10NO+·H2AsO4 −, are reported. The salt, crystallizing in the triclinic space group P\overline{1}, was synthesized using a solution method and was characterized by single-crystal X-ray diffraction analysis. It possesses a layered supramolecular architecture in the crystal. The intermolecular interactions were studied using Hirshfeld surface analysis which confirmed that hydrogen bonds and H...H contacts play dominant roles in the crystal structure of the investigated system. An analysis of the electronic structure and molecular modelling using charge distribution confirms the good electrophilic reactivity of the title compound.

A diethylhydroxylaminate based mixed lithium/beryllium aggregate

2015 ◽  
Vol 70 (4) ◽  
pp. 279-282 ◽  
Author(s):  
Raphael J.F. Berger ◽  
Surajit Jana ◽  
Roland Fröhlich ◽  
Norbert W. Mitzel
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
State Structure ◽  
Distorted Tetrahedron ◽  
X Ray Diffraction ◽  
Butyl Lithium ◽  
X Ray ◽  
Weak Intermolecular Interactions ◽  
Nitrogen Donor ◽  
Structural Details

AbstractA mixed lithium/beryllium diethylhydroxylaminate compound containing nbutyl beryllium units of total molecular composition nBe(ONEt2)2 [(LiONEt2)2nBuBeONEt2]2 (1) was isolated from a reaction mixture of nbutyl lithium, N,N-diethylhydroxylamine and BeCl2 in diethylether/thf. The crystal structure of 1 has been determined by X-ray diffraction. The aggregate is composed of two ladder-type subunits connected in a beryllium-centered distorted tetrahedron of four oxygen atoms. Only the lithium atoms are engaged in coordination with the nitrogen donor atoms. The DFT calculations support the positional occupation determined for Li and Be in the crystal structure. The DFT and the solid-state structure are in excellent agreement, indicating only weak intermolecular interactions in the solid state. Structural details of metal atom coordination are discussed.

Crystal structure of Bis(2,2':6',2''-terpyridyl)cobalt(II) iodide dihydrate at 295 K and at 120 K

1983 ◽  
Vol 36 (8) ◽  
pp. 1527 ◽  
Author(s):  
BN Figgis ◽  
ES Kucharski ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ground State ◽  
Title Compound ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
A Site ◽  
Tetragonal Cell ◽  
Spin Ground State

The crystal structure of the title compound, [CO(C15H11N3)2] 12.2H2O, has been determined by single crystal X-ray diffraction methods at 295 K and at 120 K, being refined by least squares to residuals of 0.051 and 0.035 respectively for 982 and 1024 'observed' reflections at these temperatures. Both structures are based on a P42/n tetragonal cell, a c. 8.9, c c. 19.4 �, Z 2, in which only a quarter of the cation is independent, being located about a site of 4 symmetry. At room temperature (μoff c. 3.2 BM) Co-N (central, distal) are 1.942(7), 2.104(5) � diminishing to 1.912(5), 2.083(4) � at 120 K, with μoff c. 2.2 BM, corresponding to a fully populated low-spin ground state.

scholarly journals Synthesis, Crystal Structure and DFT Studies of 4-(2-(4,5-Dimethyl-2-(3,4,5-trimethoxyphenyl)-1H-imidazol-1-yl)ethyl)morpholine

2021 ◽  
Vol 33 (3) ◽  
pp. 611-616
Author(s):  
A. Prabhakaran ◽  
M. Arockia Doss ◽  
E. Dhineshkumar ◽  
R. Rajkumar
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ground State ◽  
Molecular Electrostatic Potential ◽  
Molecular Geometry ◽  
Dft Studies ◽  
X Ray Diffraction ◽  
Frontier Orbitals ◽  
One Pot ◽  
X Ray

The title compound 4-(2-(4,5-dimethyl-2-(3,4,5-trimethoxyphenyl)-1H-imidazol-1-yl)morpholine (DMTPM) was synthesized using a one-pot multicomponent approach. The molecular structure of the compound was charcterized with 1H & 13C NMR, HR-MS and single-crystal X-ray diffraction. In the ground-state, DMTPM molecular geometry was determined using the DFT based on B3LYP/6-31G(d,p) and compared to the experimental results. In addition, molecular electrostatic potential (MEP) map and molecular frontier orbitals (MFO) were performed and the results obtained were compatible with the electronic properties.

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