Trans alkenylpyridine and alkenylamine complexes of platinum

2000 ◽  
Vol 78 (5) ◽  
pp. 568-576 ◽  
Author(s):  
Michael P Shaver ◽  
Christopher M Vogels ◽  
Andrew I Wallbank ◽  
Tracy L Hennigar ◽  
Kumar Biradha ◽  
...  

Addition of cis-cyclooctene (coe) to K2PtCl4 gives trans-[PtCl2(coe)]2 (1), which reacts with excess coe to give trans-PtCl2(coe)2 (2). Compound 2 was characterized by an X-ray diffraction study and crystals were found to be triclinic, a = 5.7838(5), b = 7.4347(6), c = 9.9972(9) Å, α = 83.924(1), β = 87.844(2), γ = 73.546(1)°, Z = 1, with space group P1-. Addition of 4-vinylpyridine (4vp) to 1 gave trans-PtCl2(4vp)2 (5) which was also characterized by an X-ray diffraction study. Crystals of 5 were monoclinic, a = 8.2255(6), b = 12.8254(10), c = 6.9624(5) Å, β = 98.8230(10)°, Z = 2, with space group P21/c. Although alkenylamines react with 1 to give a mixture of products, addition of one equivalent of apve (H2NCH2CH2CH2OCHβCH2) to 1 cleanly afforded the organometallic product trans-PtCl2(coe)(thmo) (thmo = tetrahydro-2-methyl-1,3-oxazine) arising from a metal-catalyzed intramolecular hydroamination of the starting alkenylamine. Initial investigations into the functionalization of metal complexes containing pendant alkene groups have shown that catecholborane can be added in some cases, using a rhodium catalyst, to give the corresponding organoboronate ester platinum compounds.Key words: alkenylamines, alkenylpyridines, hydroamination, hydroboration, platinum.

2000 ◽  
Vol 53 (8) ◽  
pp. 693 ◽  
Author(s):  
M. Karen J. Gagnon ◽  
Timothy R. St. Germain ◽  
Christopher M. Vogels ◽  
Robert A. McNamara ◽  
Nicholas J. Taylor ◽  
...  

We have prepared four potentially lipophilic N-substituted hydroxypyridinones containing unsaturated hydrocarbon groups. The propyl vinyl ether derivative (3) has been characterized by an X-ray diffraction study. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands, have also been prepared. The pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Initial investigations into the hydroboration of the alkene groups in the pyridinone ligands and corresponding metal complexes is presented. Crystals of (3) are monoclinic, with a 10.466(1), b 13.388(1), c 15.386(2) Å, β 102.343(8)˚, Z 8, space group P21/n.


1990 ◽  
Vol 04 (12) ◽  
pp. 791-794 ◽  
Author(s):  
YANG JI-LIAN ◽  
YE CHUN-TANG ◽  
ZHANG BAI-SHENG ◽  
LI JI-ZHOU ◽  
KANG JIAN ◽  
...  

The polycrystalline sample of (Bi–Pb)2Sr2Ca2Cu3O10 with Tc=107 K was prepared. The X-ray diffraction proved that the sample is single phase. The crystal structure study on the sample has been carried out by neutron diffraction. The result shows that its structure is tetragonal body-centre structure with space group of I4/mmm, containing a few oxygen atoms at 4e site in Bi–Pb layers.


2013 ◽  
Vol 11 (5) ◽  
pp. 811-816
Author(s):  
Patrick Ferland ◽  
Kathleen Prosser ◽  
Jeremy Bourque ◽  
Ian Edwards ◽  
Nathan Hamilton ◽  
...  

AbstractIn this study, the addition of boranes to (E)-(η5-C5H5)2Zr(CH=CHPh)Cl (3) has been examined in order to investigate the regioselectivity of these ‘hydroboration’ reactions. We have found that these additions proceed with remarkable selectivity to give exclusive formation of a saturated organic molecule where one carbon atom has both the boron and the zirconium fragments. These reactions do not proceed via a conventional hydroboration reaction, but instead go through an initial transmetalation step to generate (E)-(η5-C5H5)2Zr(H)Cl (1) and the corresponding alkenyl boron intermediate, whereupon subsequent hydrozirconation of this latter species gives the geminal products. An x-ray diffraction study has been conducted on gem-(η5-C5H5)2Zr(CH(Bpin)CH2Ph)Cl (pin = 1, 2-O2C2Me4) (2). Crystals of 2 were orthorhombic with a = 18.545(3) Å, b = 15.713(3) Å, c = 16.157(3) Å in the space group Pccn. An x-ray diffraction study has also been conducted on the trinuclear zirconium oxide species (η5-C5H5)2ZrO2[ZrCl(η5-C5H5)2]2(4). Crystals of 4 were orthorhombic with a = 13.6000(8) Å, b = 14.2252(8) Å, c = 17.6500(10) Å in the space group P2(1)2(1)2(1).


1988 ◽  
Vol 02 (08) ◽  
pp. 985-991 ◽  
Author(s):  
X. CHU ◽  
Z.H. MAI ◽  
Y.F. YAN ◽  
J.H. WANG ◽  
D.N. ZHENG ◽  
...  

X-ray precession technique1 has been utilized to study the reciprocal space of the superconducting single crystal Bi 2 Sr 2 CaCu 2 O y. An average structure with space group of Pnnn and a real structure with the superspace group of [Formula: see text] or [Formula: see text] have been found for this one dimensional modulated incommensurate material. As well, a basic structure with the space group of Fmmm is derived from the experimental data.


1985 ◽  
Vol 38 (9) ◽  
pp. 1381 ◽  
Author(s):  
CHL Kennard ◽  
EJ O'Reilly ◽  
G Smith ◽  
TCW Mak

The crystal structures of 2-formylphenoxyacetic acid ( ofpaH ), tetraaquabis (2-formylphenoxyacetato)-cobalt(II) (1) and tetraaquabis (2- formylphenoxyacetato )zinc(II) (2) have been determined by X-ray diffraction and refined to residuals R 0.039, 0.058 and 0.045 for 1197, 1178 and 1230 observed reflections respectively. 2-Formylphenoxyacetic acid crystallizes in a monoclinic cell, space group P21/n with a 8.066(2), b 7.375(1), c 14.206(2) Ǻ, β 98.12(1)° and Z 4. The planar molecules form unusual hydrogen-bonded chain polymers (O…O 2.694(3)Ǻ] linked through the carboxyl groups. The complexes (1) and (2) are isomorphous, the comparative cells being a 5.036(1), b 13.463(3), c 15.083(4) Ǻ, β 96.88(2)° for (1), and a 5.044(1), b 13.481(3), c 15.055(4) Ǻ, β 96.95(2)° for (2), with Z 2 and space group P21. The complexes have four waters and two trans-related carboxyl oxygens [mean M-O distances 2.129(5) and 2.117(3) Ǻ respectively] completing almost regular octahedral stereochemistries . The nickel(II) complex [Ni( ofpa )(H2O)4] is probably not isostructural with (1) and (2), and the copper(II) complex is also different, with formula [Cu( ofpa )2(H2O)2].


1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.


2000 ◽  
Vol 53 (8) ◽  
pp. 687 ◽  
Author(s):  
Noah A. Epstein ◽  
Jennifer L. Horton ◽  
Christopher M. Vogels ◽  
Nicholas J. Taylor ◽  
Stephen A. Westcott

We have prepared four N-substituted hydroxypyridinones containing alcohol and morpholine groups. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands have also been synthesized. The ethanolamine derivative, cis-MoO2(hep)2 (5), has been characterized by an X-ray diffraction study whereby the pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Crystals of (5) are triclinic, with a 9.1930(7), b 14.2718(8), c 14.6219(9) Å, α 106.816(5), β 95.902(5), γ 96.350(5)°, Z 4, space group P–1.


1987 ◽  
Vol 42 (9) ◽  
pp. 1107-1109 ◽  
Author(s):  
Frank Edelmann ◽  
Claudia Spang ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick ◽  
Nayla Keweloh ◽  
...  

(PhAsNSN)2 (1) reacts with M(CO)4(C7H8) (M = a Cr. b Mo) to yield (PhAsNSN)2M(CO)4 (2). 2a and 2b are dark red air stable complexes. 2b was characterized by X-ray diffraction. Crystals of 2b are monoclinic, space group C2/c, with a = 2884.7(4). b = 1166.2(2), c = 1344.1(2) pm, fβ = 104.81(2)° and Z = 8. The molecule exhibits approximate mm (C2v) symmetry with mean bond lengths: Mo-As 255.1. Mo-C 201.8. As-N 186.2 and S -N 152.8 pm.


1999 ◽  
Vol 14 (2) ◽  
pp. 145-146
Author(s):  
Liangqin Nong ◽  
Lingmin Zeng

An X-ray diffraction pattern for ErNi2Ge2 at room temperature is reported. ErNi2Ge2 is tetragonal with lattice parameters a=4.0191(2) Å, c=9.7643(2) Å, space group I4/mmm, and Z=2. The lattice parameters derived from Rietveld analysis agree well with the results of a least-squares refinement.


Sign in / Sign up

Export Citation Format

Share Document