scholarly journals Structures and properties of Saturn-like complexes composed of oligothiophene macrocycle with methano[60]fullerene and [70]fullerene

2017 ◽  
Vol 95 (3) ◽  
pp. 315-319 ◽  
Author(s):  
Masahiko Iyoda ◽  
Hideyuki Shimizu ◽  
Shinobu Aoyagi ◽  
Hiroshi Okada ◽  
Biao Zhou ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Acceptor Interaction ◽  
X Ray ◽  
Covalent Interaction ◽  
Structures And Properties ◽  
Fullerene Complexes ◽  
Donor Acceptor ◽  
Short Contacts

π-Expanded oligothienylene macrocycle with a large inner cavity incorporates fullerenes such as methano[60]fullerene (C61H2) and [70]fullerene (C70) inside to form Saturn-like complexes. Although the oligothiophene macrocycle weakly interacts with fullerenes in solution, it forms stable Saturn-like fullerene complexes in the solid state. X-ray analysis of the Saturn-like complexes exhibited short contacts between the sulfur atoms of the oligothiophene macrocycle and fullerene carbons, which hinder the rotation of fullerenes. As a result, the non-covalent interaction between the oligothiophene macrocycle and fullerenes was employed in crystal structure determination of fullerenes. UV–vis–NIR spectra of the Saturn-like complexes showed weak donor–acceptor interaction between the oligothiophene macrocycle and fullerenes.

Structural Properties of a Dimeric Phenylcyanamidocopper(I) Complex, [{Cu(PPh3)2(C6H5NCN)}2]

2000 ◽  
Vol 53 (12) ◽  
pp. 971 ◽  
Author(s):  
Eric W. Ainscough ◽  
Andrew M. Brodie ◽  
Peter C. Healy ◽  
Joyce M. Waters
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Properties ◽  
Structure Determination ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
X Ray ◽  
Angle Spinning

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

scholarly journals Metallation of Isatin (2,3-Indolinedione). X-Ray Structure and Solution Behavior of Bis(Isatinato)Mercury(II)

1995 ◽  
Vol 2 (2) ◽  
pp. 81-90 ◽  
Author(s):  
Angel Garcia-Raso ◽  
Juan J. Fiol ◽  
Elies Molins ◽  
Antonia M. Calafat ◽  
Patricia A. Marzilli ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Metal Complex ◽  
Bond Length ◽  
Spectral Data ◽  
Structure Determination ◽  
Monoclinic System ◽  
Heterocyclic Nitrogen ◽  
X Ray

The first X-ray structure of an isatin (2,3-indolinedione, isaH) metal complex, bis(isatinato)memury(II) (C16H8N2O4Hg) (1), was determined. (1) was obtained from the reaction of isaH with mercury(II) acetate in methanol. Analogously, treatment of sodium saccharinate and mercury(II) acetate in methanol yielded Hg(saccharinato)2•0.5CH3OH (3). (1) crystallizes in the monoclinic system, space group P21/a with a = 7.299(1) Å, b = 8.192(1) Å, c = 11.601(1) Å , β = 105.82(1)°, V = 667.4 Å3, Z = 2, Dcalc = 2.452 g cm−3, MoKα radiation(λ = 0.71073 Å), μ = 115.5 cm-1, F(000) = 460, 21(1) °C. The structure was refined on the basis of 2023 observed reflections to R= 0.044. The two deprotonated, non coplanar isa ligands are trans to each other in a head to tail orientation and bound to the Hg through the nitrogen in a linear N-Hg-N arrangement. The Hg atom is at the center of symmetry of the complex and displaced by 0.62 Å from the two planes of the isa ligands (τ Hg-N1-C2-O2= -16°). The Hg-N bond length is 2.015 Å. Noπ-aryl-memury(ll)-π-aryl stacking interaction was observed either in the solid state or in the solution state. The IR, electronic, and H1 and C13NMR spectral data of (1) and (3) suggest binding of the memury to the heterocyclic nitrogen, in agreement with the crystal structure determination of (1).

Synthesen und Kristallstrukturen von PPh4[RuCl4(NO)(NSCl)] und (PPh4)2[RuCl4(NS)]2·4C H2Cl2 / Syntheses and Crystal Structures of PPh4[RuCl4(NO)(NSCl)] and (PPh4)2[RuCl4(NS)]2·4C H2Cl2

1986 ◽  
Vol 41 (5) ◽  
pp. 560-566 ◽  
Author(s):  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Udo Demant ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Crystal Data ◽  
Acceptor Interaction ◽  
X Ray ◽  
Bond Lengths ◽  
Vacuum Pyrolysis ◽  
Structure Determinations ◽  
Donor Acceptor

Abstract By reaction of trithiazylchloride, (NSCl)3, with PPh4[RuCl4(NO)]2 in dichloromethane the thiazylchloridenitrosyl complex PPh4[RuCl4(NO)(NSCl)] is obtained; its vacuum pyrolysis at 200-220 °C yields the thionitrosyl com plex (PPh4)2[RuCl4(NS)]2 which crystallizes from CH2Cl2 solution with four molecules of CH2Cl2. Both com pounds were charaterized by their IR spectra and by X-ray crystal structure determinations. Crystal data: PPh4[RuCl4(NO)(NSCl)], mono­clinic, space group P 21/n, Z = 4, a = 982.6, b = 1700.0, c = 1772.3 pm , β = 104.79° (2548 observed reflexions, R = 0.046); (PPh4)2[RuCl4(NS)]2·4CH2Cl2, triclinic, P1̄ , Z = 1, a = 952.9, b = 1380.0, c = 1458.5 pm , α = 112.91, β = 106.67, γ = 92.61° (3760 observed reflexions, R = 0.053). In the [RuCl4(NO)(NSCl)]⊖ ion the nitrosyl and thiazyl chloride ligands occupy ex ­ positions; bond lengths indicate double bonds in the linear Ru=N=O group, while the NSCl molecule is attached by a donor-acceptor interaction Ru-N≡S̲-Cl , although with a rather short Ru-N bond of 198 pm (N≡S 144 pm, S-Cl 213 pm). The centrosymmetric [RuCl4(NS)]22⊖ ions have chloro bridges and NS ligands in axial positions; the nearly linear Ru=N=S group has bond lengths Ru=N 175 pm and N=S 147 pm.

Synthesis and X-ray structure determination of the Ir–Ag–Ir donor–acceptor metal–metal bonded complex [{(η5-C5Me5)(CO)2Ir}2Ag][BF4]

1989 ◽  
Vol 67 (11) ◽  
pp. 1832-1836 ◽  
Author(s):  
Frederick W. B. Einstein ◽  
Richard H. Jones ◽  
Xiaoheng Zhang ◽  
Derek Sutton
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Metal ◽  
Donor Acceptor ◽  
Silver Metal

The title complex (2) has been synthesized from the reaction of (η5-C5Me5)Ir(CO)2 (1) with AgBF4. Complex 2 crystallizes in the monoclinic space group P21/c with a = 12.355(2) Å, b = 13.713(2) Å, c = 16.672(3) Å, β = 97.70(1)°, and Z = 4. The structure was solved by using 3131 observed reflections (I ≥ 2.5σ(I)) in the range 0° < 2θ < 50° to final discrepancy indices of RF = 0.032 and RwF = 0.038. The cation may be described as consisting of two molecules of 1 bound to Ag+ by donor–acceptor Ir → Ag bonds. The Ir—Ag—Ir skeleton is nearly linear (angle 173.67(6)°). The Ag—Ir bond lengths are equal (2.659(1) Å), and the two molecules of 1 are disposed mutually trans, to give the cation approximate (noncrystallographic) C2h symmetry. Keywords: complex, iridium, silver, metal-metal bond, X-ray, crystal, structure, carbonyl, donor-acceptor, pentamethylcyclopentadienyl.

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