The complexes fac-[ReOCl3(dppm-P,P′)] (1a), mer-[ReOCl3(dppm-P,P′)] (1b), mer-[ReCl3(dppm-P,P′)(dppom-P)] (2), [ReCl4(dppom-P,O)] (3) and mer-[ReCl3(dppm-P,P′)PPh3] (4) (dppmPh2PCH2PPh2, dppomPh2PCH2P(O)Ph2) were obtained by reaction of [ReOCl3(PPh3)2] or [AsPh4][ReOCl4] and dppm under different experimental conditions. Complex 1b is probably obtained via the intermediate formation of complexes 2 or 4. The complexes fac-[Re(NCH3)Cl3(dppm-P,P′] (5), trans-[ReNCl2(dppm-P)PPh3] (6) and [ReNCl(dppm-P,P′)2]Cl (7) were also obtained starting from [Re(NCH3)Cl3(PPh3)2] and [ReNCl2(PPh3)2], respectively. The structures of 1a and 3 were determined by X-ray crystallography. Compound 1a is monoclinic, space group P21/c, with a=11.156(4), b=17.264(5), c=14.467(5) Å and β=110.96(3)°. The molecular complex is distorted octahedral. Selected bond distances (Å) are: ReO(oxide) 1.671(6), ReCl(trans to O) 2.452(3), ReCl(trans to P) 2.365(4) and 2.373(3), ReP 2.439(3) and 2.449(2). The PReP chelation angle is 69.2(1)°. Compound 3 is orthorhombic, space group Pccn, with a=34.843(5), b=8.242(2) and c=19.342(4) Å. The molecular complex is roughly octahedral with the oxidized dppm ligand chelated through the P atom and the O atom of the PO group. Selected bond distances (Å) are: ReCl(trans one other) 2.355 (mean), ReCl(trans to P) 2.353(3), ReCl(trans to O) 2.215(5), ReO 2.087(7). The PReO chelation angle is 80.7(2)°. © 1993.
Reactivity of rhenium(V) complexes containing different cores such as [ReO]3+, [ReNR]3+ and [ReN]2+ toward bis(diphenylphosphino)methane: synthesis and crystal structures
ROSSI, Roberto;MARCHI, Andrea;MARVELLI, Lorenza;MAGON, Luciano;
1993
Abstract
The complexes fac-[ReOCl3(dppm-P,P′)] (1a), mer-[ReOCl3(dppm-P,P′)] (1b), mer-[ReCl3(dppm-P,P′)(dppom-P)] (2), [ReCl4(dppom-P,O)] (3) and mer-[ReCl3(dppm-P,P′)PPh3] (4) (dppmPh2PCH2PPh2, dppomPh2PCH2P(O)Ph2) were obtained by reaction of [ReOCl3(PPh3)2] or [AsPh4][ReOCl4] and dppm under different experimental conditions. Complex 1b is probably obtained via the intermediate formation of complexes 2 or 4. The complexes fac-[Re(NCH3)Cl3(dppm-P,P′] (5), trans-[ReNCl2(dppm-P)PPh3] (6) and [ReNCl(dppm-P,P′)2]Cl (7) were also obtained starting from [Re(NCH3)Cl3(PPh3)2] and [ReNCl2(PPh3)2], respectively. The structures of 1a and 3 were determined by X-ray crystallography. Compound 1a is monoclinic, space group P21/c, with a=11.156(4), b=17.264(5), c=14.467(5) Å and β=110.96(3)°. The molecular complex is distorted octahedral. Selected bond distances (Å) are: ReO(oxide) 1.671(6), ReCl(trans to O) 2.452(3), ReCl(trans to P) 2.365(4) and 2.373(3), ReP 2.439(3) and 2.449(2). The PReP chelation angle is 69.2(1)°. Compound 3 is orthorhombic, space group Pccn, with a=34.843(5), b=8.242(2) and c=19.342(4) Å. The molecular complex is roughly octahedral with the oxidized dppm ligand chelated through the P atom and the O atom of the PO group. Selected bond distances (Å) are: ReCl(trans one other) 2.355 (mean), ReCl(trans to P) 2.353(3), ReCl(trans to O) 2.215(5), ReO 2.087(7). The PReO chelation angle is 80.7(2)°. © 1993.I documenti in SFERA sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
