scholarly journals Neue Synthesewege zu neutralen gemischtsubstituierten Eisen-Schwefel-Clustern / Novel Synthetic Pathways to Neutral Mixed-Ligand Iron-Sulfur Clusters

1996 ◽  
Vol 51 (7) ◽  
pp. 1040-1048 ◽  
Author(s):  
M. Harmjanz ◽  
C. Junghans ◽  
U.-A. Opitz ◽  
B. Bahlmann ◽  
S. Pohl
Keyword(s):  
Elemental Sulfur ◽  
Large Excess ◽  
Iron Sulfur Clusters ◽  
Thiourea Derivatives ◽  
X Ray ◽  
X Ray Crystallography ◽  
Iron Sulfur ◽  
Neutral Ligands ◽  
High Yields ◽  
Sulfur Donor

The reaction of [Fe(NiSiMe3)2)2] with thiols RSH, elemental sulfur, and neutral ligands L (with sulfur donor atoms, e. g. thiourea derivatives) gives [Fe4S4(SR)2L2] clusters in high yields. The structure of [Fe4S4(2.4.6-(C3H7)3C6H2-S)2(dpdmi)2] (dpdmi: diisopropyldimethyl- imidazolthion) was determined by X-ray crystallography.When [Fe4S4I4]2- is reacted with a large excess of PMePh2 or PMe2Ph [F6S6I2(PMePh2)4] and [Fe6S6l2(PMe2Ph)4]. respectively, are obtained in nearly quantitative yield. Basket-like structures of the [Fe6S6]2+ cores were detected by X-ray structure analysis. While [Fe4S4(SR)4]2- clusters do not react with phosphanes at ambient temperature 2:2 functional­ized species like [Fe4S4(SR)2(tmtu)2] lead to basket-type clusters [Fe6S6(SR)2(PR3)4].

[Fe4S4l2+-Cluster mit Thioharnstoffliganden: [FeIL3][Fe4S4I3L]' (L = (Me2N)2CS) und [Fe4S4I2L'2](L' = (C4H9NH)2CS)

1991 ◽  
Vol 46 (1) ◽  
pp. 68-74 ◽  
Author(s):  
Siegfried Pohl ◽  
Ulrich Bierbach
Keyword(s):  
X Ray Diffraction ◽  
Neutral Cluster ◽  
Iron Sulfur Clusters ◽  
Triclinic Space Group ◽  
Terminal Ligand ◽  
Space Group ◽  
X Ray ◽  
Iron Sulfur ◽  
Neutral Ligands ◽  
Back Donation

(1)The mixed terminal ligand iron-sulfur clusters [F eIL 3][Fe4S4I3L] and [Fe4S4I2L '2] (2) with the neutral ligands L = (M e2N )2CS and L' = (C4H 9N H )2CS have been synthesized by the reaction o f F eI2L2 with 1.5 equivalents o f Fe(C O )5 and 2 equivalents o f sulfur and by the reaction o f F eI2L '2 with 3 equivalents o f Fe(CO)^ and 4 equivalents o f sulfur, respectively. The crystal structures o f 1 and 2 were determined from single crystal X -ray diffraction data. 1 crystallizes in the triclinic space group P 1 with a = 968.6( 1), b = 1466.2( 1), c = 1679.1(1) pm, a = 91.51(1),/?= 93.43( 1), y = 90.82( 1)°, V = 2379.2 * 106 pm 5, Z = 2, R = 0.054. 2 crystallizes in the m onoclinic space group P2 Jn with a = 930.2(1), b = 1666.1(1), c = 2335.6(1) pm, β = 97.26°, V = 3 5 90.8 x 106 pm 3, Z = 4. R = 0.055. The anion [Fe4S4I3L] o f 1 exhibits a nearly undistorted [Fe4S4]2+ core. The F e - S distance to the thiourea ligand is found at 230.6 pm. The m ost striking feature o f the neutral cluster o f 2 is the very short F e - F e distance (268.7 pm) between the iron atom s with thiourea ligation which is possibly a consequence of back-donation. The F e - S thiourea distances in 2 were found to be 230.8 and 231.5 pm , respectively.

scholarly journals Silylated gallium and indium chalcogenide ring systems as potential precursors to ME (E=O, S) materials

2013 ◽  
Vol 11 (7) ◽  
pp. 1225-1238
Author(s):  
Iliana Medina-Ramírez ◽  
Cynthia Floyd ◽  
Joel Mague ◽  
Mark Fink
Keyword(s):  
Thermal Decomposition ◽  
Room Temperature ◽  
Membered Ring ◽  
Molecular Structures ◽  
Nmr Studies ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields ◽  
Vt Nmr ◽  
State 1

AbstractThe reaction of R3M (M=Ga, In) with HESiR′3 (E=O, S; R′3=Ph3, iPr3, Et3, tBuMe2) leads to the formation of (Me2GaOSiPh3)2(1); (Me2GaOSitBuMe2)2(2); (Me2GaOSiEt3)2(3); (Me2InOSiPh3)2(4); (Me2InOSitBuMe2)2(5); (Me2InOSiEt3)2(6); (Me2GaSSiPh3)2(7); (Et2GaSSiPh3)2(8); (Me2GaSSiiPr3)2(9); (Et2GaSSiiPr3)2(10); (Me2InSSiPh3)3(11); (Me2InSSiiPr3)n(12), in high yields at room temperature. The compounds have been characterized by multinuclear NMR and in most cases by X-ray crystallography. The molecular structures of (1), (4), (7) and (8) have been determined. Compounds (3), (6) and (10) are liquids at room temperature. In the solid state, (1), (4), (7) and (9) are dimers with central core of the dimer being composed of a M2E2 four-membered ring. VT-NMR studies of (7) show facile redistribution between four- and six-membered rings in solution. The thermal decomposition of (1)–(12) was examined by TGA and range from 200 to 350°C. Bulk pyrolysis of (1) and (2) led to the formation of Ga2O3; (4) and (5) In metal; (7)–(10) GaS and (11)–(12) InS powders, respectively.

Heterometallische Cluster durch ligandunterstützte Metallfragmentkondensation / Heterometallic Clusters by Ligand Assisted Metal Fragment Condensation

1991 ◽  
Vol 46 (9) ◽  
pp. 1169-1176 ◽  
Author(s):  
Wolfgang Rohde ◽  
Gert Fendesak
Keyword(s):  
Double Bond ◽  
Chelate Complexes ◽  
Heterometallic Clusters ◽  
X Ray ◽  
X Ray Crystallography ◽  
Inert Solvent ◽  
Fragment Condensation ◽  
Olefinic Double Bond ◽  
High Yields ◽  
Iron Fragment

Dicobalt complexes of 3-vinylpropargylic alcohol derivatives react with biscyclooctenetricarbonyliron to give new chelate complexes of the iron tricarbonyl fragment with the olefinic double bond and the alcohol oxygen atom bound to the iron fragment. These compounds react upon heating in an inert solvent to give FeCo-alkynyl cluster complexes in high yields. One of these compounds has been structurally characterized by X-ray crystallography.

scholarly journals Synthesis, Characterization, and Antibacterial and Anti-Inflammatory Activities of New Pyrimidine and Thiophene Derivatives

2018 ◽  
Vol 2018 ◽  
pp. 1-11
Author(s):  
Siham Lahsasni ◽  
Dunya A. M. Al-Hemyari ◽  
Hazem A. Ghabbour ◽  
Yahia Nasser Mabkhoot ◽  
Fadilah S. Aleanizy ◽  
...  
Keyword(s):  
Nucleophilic Substitution ◽  
Phenyl Isothiocyanate ◽  
Standard Drug ◽  
Thiourea Derivatives ◽  
X Ray ◽  
X Ray Crystallography ◽  
Lead Compounds ◽  
Antimicrobial Studies ◽  
Thiophene Derivatives ◽  
Anti Inflammatory

Substituted[4,5]thieno[2,3-d]thiazolo[3,2-a]pyrimidin-5-one (3a–b) and pyrimidin-5(6H)-imine (3c–e) were synthesized via reaction of the starting compounds, ethyl 2-amino-substituted[b]thiophene-3-carboxylate (2a–c) and 2-amino-substituted [b]thiophene-3-carbonitrile (2d–f), respectively, with 2-bromothiazole. Synthesis of (bromo-substituted[b]thiophen-2-yl)alkanamide derivatives (4a–e) and thieno[2,3-d][1,3]oxazin-4-imine derivative (5) was accomplished via reaction of the starting compounds with bromoalkyl chloride through nucleophilic substitution; however, for the synthesis of compound 5, nucleophilic substitution was followed by nucleophilic addition to a nitrile group to form the oxazinimine ring. 1-(3-cyano-substituted[b]thiophen-2-yl)-3-(4-(trifluoromethyl)phenyl)thiourea derivatives (6a–c) were obtained via reaction of the starting compounds (2d–f) and 4-(trifluoromethyl phenyl)isothiocyanate. The lead compounds (2d–f) rapidly reacted with 4-(trifluoromethyl)benzaldehyde or 4-(2-pyridyl)benzaldehyde in acidic medium to yield compounds (7a–f) in large quantities. X-ray crystallography of compounds 4c and 7e confirmed their structures. Antimicrobial studies revealed that compound 6a was equally potent to ampicillin against Bacillus strains. Moreover, compounds 3e, 4d, and 6a possessed greater anti-inflammatory potency than that of the standard drug.

Activation of C–Cl Bonds: Synthesis and Structural Characterization of [Ru2(μ-Cl)(μ-PtBu2)(μ- Ph2PN(H)PPh2)(CO)4]

2013 ◽  
Vol 68 (5-6) ◽  
pp. 743-746 ◽  
Author(s):  
Tobias Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Carbon Tetrachloride ◽  
Single Crystals ◽  
Structural Characterization ◽  
Title Compound ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields

The synthesis and structural characterization of the complex [Ru2(μ-Cl)(μ-PtBu2)(μ-dppa)(CO)4] (4, dppa = Ph2PN(H)PPh2) are reported. The title compound and two other related complexes were obtained in high yields by the reaction of the coordinatively unsaturated species [Ru2(μ-H)(μ-PtBu2)(μ-PˆP)(CO)4] (PˆP = dppa, 3; PˆP =Ph2PN(Ph)PPh2, 5; PˆP =Ph2PN(CH2Ph)PPh2, 6) with carbon tetrachloride. Single crystals of 4 grown from dichloromethane-acetone have been analyzed by X-ray crystallography

Nano ZrO2: an efficient, recyclable, and inexpensive catalyst for diastereoselective three-component Mannich reactions

2014 ◽  
Vol 92 (7) ◽  
pp. 659-664 ◽  
Author(s):  
M. Saeed Abaee ◽  
Elahe Akbarzadeh ◽  
Abbas Shockravi ◽  
Mohammad M. Mojtahedi ◽  
Hamid Reza Khavasi
Keyword(s):  
Spectroscopic Data ◽  
Room Temperature ◽  
Aromatic Aldehydes ◽  
Significant Loss ◽  
Mannich Reactions ◽  
X Ray ◽  
X Ray Crystallography ◽  
Aniline Derivatives ◽  
High Yields ◽  
Acyclic Ketones

A facile procedure is developed for the three-component Mannich reactions of several heterocyclic, homocyclic, and acyclic ketones by using catalytic quantities of nano ZrO2. As a result, the starting ketones undergo rapid reactions with a variety of aromatic aldehydes and aniline derivatives at room temperature to produce stereoselectively high yields of the corresponding anti β-amino ketones. Interestingly, the catalyst could be recycled for several runs in a row without significant loss of its activity. The structure of the products was assigned based on their spectroscopic data and the anti stereoselectivity was confirmed by X-ray crystallography.

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