Quantitative ortho-cycloboronation of P-phenyl groups in metallaborane chemistry and the crystal and molecular structure of the novel iso-closo-ten-vertex metallaborane [1,1,1-H(PPh3)(Ph2P-ortho-C6H4)-iso-closo-(1-IrB9H8-2-)]

Author(s):  
Jonathan Bould ◽  
Norman N. Greenwood ◽  
John D. Kennedy ◽  
Walter S. McDonald
1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  

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)).


2012 ◽  
Vol 65 (7) ◽  
pp. 779 ◽  
Author(s):  
Mohamed Ashraf ◽  
Graeme J. Gainsford ◽  
Andrew J. Kay

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.


1989 ◽  
Vol 42 (7) ◽  
pp. 1057 ◽  
Author(s):  
BF Hoskins ◽  
IAS Mcdonald

The crystal and molecular structure of the trinuclear complex L2Pd3 has been determined by single-crystal X-ray diffraction techniques at room temperatures, 20°C. The quinquedentate binucleating ligand, L3-, is formally the trianion α,α′-[(2-mercapto-5-methylbenzene-1,3-diyl )di(methylidyne)di(azino)]bis(cyclohexaemethano)ato(3-). Crystals of L2Pd3 are triclinic, PI, with a 11.896(1), b 13.4103(7), c 17.451(3) � , α 75.66(1), β 79.93(1) and γ88.99(1)�, Z 2. The structure was solved by the normal Fourier methods and refined by a least-squares procedure which gave final R and R, values of 0.046 and 0.049 respectively for the 7769 statistically significant reflections. The approximately square-planar coordination environments of the palladium centres give rise to a boat-shaped arrangement in which an approximate, non-crystallographic, twofold axis normal to the plane of the central metal is evident. The notable feature of the structure lies in the novel coordination mode adopted by the binucleating ligand. With respect to the binuclear complexes of this ligand, an electronic reorganization has occurred in one of the sidearms of both ligands which enables the formation of the pair of hydrazine bridges and also causes two of the terminal oxygen groups to become non-coordinating.


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