The First Heterodinuclear Complexes with Bis(cyclopentadienyl)methane Bridges
Tóm tắt
Từ khóa
Tài liệu tham khảo
Nesmeyanov A. N., 1977, Izv. Akad. Nauk SSSR Ser. Khim., 10, 2352
(a)R. E.Schmidt M.Birkhahn W.Massa P.Kiprof E.Herdtweck STRUX‐II program for analyzing X‐ray data Universität Marburg (1980) and Technische Universität München (1985/87).3acrystallizes as orangered prisms from hexane. The observed extinctions (0kl:k= 2 n + 1 h0l:l= 2 n + 1 0kl:l= 2 n + 1) are consistent with the orthorhombic space groupPbca(Nr. 61);a= 1465.0(1) b= 1604.1(1) c= 1036.7(1) pm;V= 2436 × 106pm3; C14H9MnO3;Z= 8; ϱcaled= 1.528 g cm−3; Syntex P21 MoKαradiation (λ = 71.073 pm) graphite monochromator;T= −50 ± 1°C 1.0° ≤ θ ≤ 26.0° ; ω scan; variable scan width and measuring timetmax= 70 s. 2983 measured reflections 2039 (NO) unique reflections withI> 1.0 σ(I) and 192 (NV) parameters full‐matrix least‐squares refinement.R= Σ([F0]−[Fc])/ΣF0= 0.037;Rw= [Σw(|F0|−|Fc|)2/ΣwF]1/2= 0.033; GOF = [Σw(|F0|−|Fc|)2/(NO−NV)]1/2= 2.047 withw= 1/σ2(F0). The structure was solved by Patterson methods and the difference Fourier technique; empirical absorption correction μ = 10.4 cm−1. The positions of the hydrogen atoms were obtained from difference Fourier syntheses and refined with a collective isotropic temperature factor. Anomalous dispersion was taken into consideration. After the final cycle of refinement the residual electron density was + 0.32 e/Å3and −0.38 e/Å3for shift/err < 0.00.