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).

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.

Kristallstruktur von [Mo(Co)3(Ncme)(Srbu)]2 / Crystal Structure of [Mo(CO)3(NCMe)(S'Bu)]2

1998 ◽  
Vol 53 (3) ◽  
pp. 378-380
Author(s):  
Mike R. Kopp ◽  
Bernhard Neumüller
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Structure Determination ◽  
Space Group ◽  
X Ray

Abstract Single crystals of [Mo(CO)3(NCMe)(S′Bu)]2 (1) and [{Mo(CO)3}2{Mo(CO)2}{S′Bu}4] (2) were obtained by the reaction of [Mo(CO)3(NCMe)3] with [(PhCH2)2GaS′Bu]2 in 1,4-dio-xane. The X-ray structure determination of 1 showed the presence of a Mo2S2 four-membe-red ring with a Mo-Mo bond length of 296,7(1) pm. Space group Pbca, Z = 4, lattice dimen­sions at -80°C: a = 1588,2(3), b = 905,8(1), c = 1676,0(1) pm, R1 = 0,0555.

Darstellung und Kristallstrukturanalyse von K3BiO3 und Rb3BiO3 / Synthesis and Crystal Structure Determination of K3BiO3 and Rb3BiO3

1997 ◽  
Vol 52 (9) ◽  
pp. 1031-1036 ◽  
Author(s):  
Nicola Zoche ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Structure Determination ◽  
Solid State Reactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Binary Compounds ◽  
First Time

K3BiO3 and Rb3BiO3 have been synthesized for the first time by solid state reactions of the respective binary compounds. K3BiO3 was obtained from Bi2O3 and K2O at 550 °C, Rb3BiO3 from Bi2O3 and Rb2O at 650 °C. The compounds were structurally examined by single-crystal X -ray investigations (K3BiO3: I 4̅ 3 m, a = 1070.15(2) pm, Z = 8; Rb3BiO3: P 21 3, a = 875.48(2) pm, Z = 4). The structures reveal “isolated” BiO33- groups. While K3BiO3 is isostructural to Na3BiO3, Rb3BiO3 has the same crystal structure as Cs3BiO3.

The Structure of 1,1'-Oxalylbisisatin, a Reactive α-Oxo Imide

1987 ◽  
Vol 40 (10) ◽  
pp. 1755
Author(s):  
DS Black ◽  
N Chaichit ◽  
BM Gatehouse ◽  
GI Moss
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Bond Angle ◽  
Crystal Structure Determination ◽  
Cyclic Imide ◽  
X Ray

The X-ray crystal structure determination of the reactive α-oxo imide 1,1'-oxalylbisisatin (1) is described. Bond length and bond angle details are compared with those of seven similar cyclic imide structures (2)-(8).

scholarly journals Synthesis of N-Silylated Diaminosulfanes from Functionally Substituted Sulfur Diimides and Hexachlorodisilane and Octachlorotrisilane-Multinuclear Magnetic Resonance Studies and X-Ray Structure Determination of a Non-Cyclic Diaminosulfane

1993 ◽  
Vol 48 (3) ◽  
pp. 249-257 ◽  
Author(s):  
Max Herberhold ◽  
Silke Gerstmann ◽  
Wolfgang Milius ◽  
Bernd Wrackmeyer
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Magnetic Resonance ◽  
Functional Groups ◽  
Structure Determination ◽  
Quantitative Yield ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Cp Mas Nmr

Sulfur diimides R1(NSN)R2 (1) with different substituents R1 and/or R2 or with functional groups react with hexachlorodisilane (2) or octachlorotrisilane (3) to give the corresponding diaminosulfanes (4, 5) in quantitative yield. The formation of cyclic intermediates prior to the redox process is discussed. The products have been characterized by 1H, 13C, 15N and 29Si NMR in solution as well as by 15N and 29Si CP/MAS NMR in the solid state (4a, 4f). The crystal structure of ClMe2Si(Cl3Si)NSN(SiCl3)SiMe2Cl (4f) has been determined: space group PĪ (no. 2) with a = 864.2(2), b = 1096.8(2), c = 1232.7(2) pm and Z = 2.

Über bicyclische Diacyloxy-pentafluoro-μ3-oxotriborane 2.2.6.10.10-Pentafluoro-4.8-dialkyl-1.3.5.7.9-pentaoxa-2.6.10-triborabicyclo(4.4.0)decadiene: Darstellung, Molekül- und Kristallstruktur

1985 ◽  
Vol 40 (7) ◽  
pp. 934-941 ◽  
Author(s):  
Herbert Binder ◽  
Walter Matheis ◽  
Gernot Heckmann ◽  
Hans-Jörg Deiseroth ◽  
Han Fu-Son
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Insertion Reaction ◽  
X Ray

Abstract Bicyclic acyloxyfluoroboranes 3 react with BF3 by an insertion reaction to form bicyclic diacyloxy- pentafluoro-μ3-oxotriboranes of the 2.2.6.10.10-pentafluoro-4.8-dialkyl-1.3.5.7.9-pentaoxa- 2.6.10-tribora-bicyclo(4.4.0)decadiene type 4. A X-ray crystal structure determination of 4b is reported. NM R data of 4b in the solid state and in solution are discussed.

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