Syntheses of complexes containing the novel 1,2,3-azadiphosphole and 1,2,5-azadiphosphole ring systems: crystal and molecular structure of [Ir(η5-C5Me5)(η4-(ButCPNButPCBut)]

2000 ◽  
pp. 1659-1660 ◽  
Author(s):  
F. Geoffrey N. Cloke ◽  
Peter B. Hitchcock ◽  
John F. Nixon ◽  
D. James Wilson ◽  
Udo Schiemann ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
The Novel ◽  
Ring Systems

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

The Meisenheimer Rearrangement in Heterocyclic Synthesis. IV. Derivatives of the 2H,6H-1,5,4-Benzodioxazocine and 7H-1,6,5-Benzodioxazonine Ring Systems: X-Ray Crystal Structure of 10-Methoxy-5-methyl-7-phenyl-2,3,4,5-tetrahydro-7H-1,6,5-benzodioxazonine

1988 ◽  
Vol 41 (3) ◽  
pp. 293 ◽  
Author(s):  
JB Bremner ◽  
EJ Browne ◽  
LM Engelhardt ◽  
IWK Gunawardana ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Ring System ◽  
Heterocyclic Synthesis ◽  
Rearrangement Product ◽  
Ring Systems ◽  
X Ray ◽  
Derivatives Of ◽  
Moderate Yield

Meisenheimer rearrangement of the N-oxides (4) derived from a series of 5-aryl-4-methyl-2,3,4,5-tetrahydro-1,4-benzoxazepines (3) gave rise to eight derivatives (5) of the new 2H,6H-1,5,4-benzodioxazocine ring system. Reaction of 9-methoxy-5-methyl-6-phenyl-3,4,5,6- tetrahydro-2H-1,5-benzoxazocine (6) with 3-chloroperoxybenzoic acid gave an unstable N-oxide (7). A Meisenheimer rearrangement product from (7), 10-methoxy-5-methyl-7-phenyl-2,3,4,5-tetrahydro-7 H-1,6,5- benzodioxazonine (8), the first example of this ring system, was isolated directly in moderate yield on oxidation of (6) with cooling. The crystal and molecular structure of (8) has been determined by X-ray crystallographic methods.

Crystal and Molecular Structure of 7-Diethylamino-[1′,3′,3′-trimethyl-4-((1,3,3-trimethyl-1,3-dihydro-2H-indole-2-ylidene)methyl)-1′,3,3′,4-tetrahydrospiro[chromene-2,2′-indole]]: A Dicondensation Product From the Reaction of 4-Diethylaminosalicylaldehyde with Fischer's Base

2012 ◽  
Vol 65 (7) ◽  
pp. 779 ◽  
Author(s):  
Mohamed Ashraf ◽  
Graeme J. Gainsford ◽  
Andrew J. Kay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Atomic Resolution ◽  
Related Structure ◽  
The Novel ◽  
Data Comparison ◽  
Molecular Features

The novel molecule, 7-diethylamino-[1′,3′,3′-trimethyl-4-((1,3,3-trimethyl-1,3-dihydro-2H-indole-2-ylidene)methyl)-1′,3,3′,4-tetrahydrospiro[chromene-2,2′-indole]], was isolated as the product from the condensation of diethylaminosalicylaldehyde with two equivalents of Fischer’s base and its crystal structure determined, initially using MoKα radiation. The diffraction data at higher theta angles (d < 0.9 Å) was notably weak so a further dataset was collected using CuKα to determine the cause. Although a different crystal batch and larger crystal was used and a better dataset obtained (with significantly improved atomic resolution) the comparison shows that the essential molecular features and weak intermolecular binding are duplicated in the refinement with the latter data. Comparison is made with a closely related structure. Consistent with observations for this related structure it is proposed that the product is formed through the interception of an intermediate carbinol by Fischer’s base.

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