1.1 equiv of ligand; S/C = 500; solvent MeOH (10 mL); additive HCl(aq) (240 L, 1 N); p(H2) 80 bar; 80 ; reaction time 17 h. Analysis data for ACA: GC, column PERMABOND-L-Chirasil-Val (25 m); 88 isothermal; ACA 2.0 min, R 8.3 min, S 9.1 min. EOP: EOP (144.2 mg, 1 mmol); [RuI2(p-cymene)]2 + 1.1 equiv of ligand; S/C = one hundred; solvent EtOH (10 mL); additive HCl(aq) (47.four L, 1 N); p(H2) 80 bar; 80 ; reaction time 16 h. Formation of trifluoroacetate derivative: immediately after removing the solvent and drying under decreased stress, for the remaining residue was added trifluoroacetic anhydride (two mL). Immediately after stirring for 20 min, the excess trifluoroacetic anhydride was removed by blowing argon more than the resolution as well as the residue was filtered through a quick plug of silica, which had been wetted with MeOH. Analysis information for EOP: GC, column LIPODEX-E (50 m); 80 isothermal; substrate 15.six min; R 26.6 min; S 29.7 min. X-ray Crystallography. Single crystal X-ray diffraction data for (R,Sp,Sp)-2?BH3, (R,Sp,Sp)-6, and (R,Sp,Sp)-7 were collected on a Bruker Kappa APEX-2 CCD diffractometer at T = one hundred K utilizing graphite-monochromated Mo K radiation ( = 0.71073 ? and – and -scan fine-sliced frames covering comprehensive Ewald spheres with max = 30? The information were integrated together with the program SAINT,Articleand corrections for absorption and /2 effects were applied using the program SADABS.10a The structures had been solved by direct solutions using the plan SHELXS97, and refinement on F2 was carried out with the program SHELXL97.10b Non-hydrogen atoms had been refined anisotropically. All H atoms had been placed in calculated positions and thereafter refined as riding. The absolute structures of all compounds could be unambiguously determined by anomalous dispersion effects and the Flack absolute structure parameter. Important crystallographic information are supplied under. (R,Sp,Sp)-2?BH3: compound crystallized as a solvate with a mixture of disordered CH2Cl2 and ethyl acetate in an estimated 60/40 ratio.1190319-51-7 web The chemical formula was idealized to (R,Sp,Sp)-2?BH3 H2Cl2, C47H48B2Cl2Fe2P2, Mr = 879.Buy148256-82-0 01, orange prism, 0.60 ?0.07 ?0.05 mm, monoclinic, space group P21 (No. 4), a = 11.3173(3) ? b = 9.5521(3) ? c = 20.2125(five) ? = 93.674(2)? V = 2180.56(10) ?, Z = two, = 0.893 mm-1, calcd = 1.339 g cm-3, 55105 reflections collected and merged to 12614 independent data (Rint = 0.039); just after squeezing the disordered solvent with program PLATON10c final R indices (all data) have been R1 = 0.0342, wR2 = 0.0679, 472 parameters, Flack absolute structure parameter -0.020(6), excursions in distinction Fourier map amongst -0.23 and 0.43 e ?3. (R,Sp,Sp)-6: C36H36Fe2NP, Mr = 625.33, orange block from ethyl acetate, 0.28 ?0.16 ?0.ten mm, monoclinic, space group P21 (No. four), a = 7.PMID:23376608 3616(three) ? b = 18.1714(7) ? c = 22.4087(9) ? = 99.319(2)? V = 2958.1(2) ?, Z = 4 (Z = two), = 1.061 mm-1, calcd = 1.404 g cm-3, 70046 reflections collected and merged to 17172 independent information (Rint = 0.090); final R indices (all data) have been R1 = 0.0472, wR2 = 0.0847, 727 parameters, Flack absolute structure parameter 0.017(eight), excursions in difference Fourier map amongst -0.52 and 0.73 e ?3. (R,Sp,Sp)-7: C36H36Fe2NOP, Mr = 641.33, orange block from ethyl acetate, 0.45 ?0.42 ?0.32 mm, monoclinic, space group P21 (No. four), a = 10.4728(4) ? b = eight.1019(three) ? c = 17.7567(six) ? = one hundred.508(2)? V = 1481.38(9) ?, Z = 2, = 1.064 mm-1, calcd = 1.438 g cm-3, 32255 reflections collected and merged to 8638 independent information (Rint = 0.028); final R indices (all information) w.
