Synthesis, characterization and crystal structure of fac-[Re(H2O)(CO)3{Ph2PO(CH2)3OPPh2}]BArF

Abram, 2004, vol. V M. Nicolini, U. Mazzi (Eds.), Technetium and Rhenium in Chemistry and Nuclear Medicine, n° 5, Servizi Grafici Editoriali, Padova, 1999. Abram, 2006, J. Braz. Chem. Soc., 17, 1486, 10.1590/S0103-50532006000800004 Top, 2004, ChemBioChem, 5, 1104, 10.1002/cbic.200400067 Schibli, 2002, Eur. J. Nucl. Med., 29, 1529, 10.1007/s00259-002-0900-8 Winter, 1989, vol. 1 Albertin, 2006, Eur. J. Inorg. Chem., 3451, 10.1002/ejic.200600251 Bolaño, 2005, J. Organometal. Chem., 690, 4945, 10.1016/j.jorganchem.2005.08.014 Rodríguez, 2004, Polyhedron, 23, 1045, 10.1016/j.poly.2004.01.003 Fernández-García, 2001, Polyhedron, 20, 2675, 10.1016/S0277-5387(01)00884-1 Bolaño, 1999, Polyhedron, 18, 1431, 10.1016/S0277-5387(99)00002-9 Perrin, 1988 Brookhart, 1992, Organometallics, 11, 3920, 10.1021/om00059a071 Huhmann-Vincent, 1998, J. Am. Chem. Soc., 120, 6808, 10.1021/ja980212k Yield 0.29g, 92%. Anal. calcd. for C62H40BF24O6P2Re: C, 46.66; H, 2.53%. Found: C, 46.55; H, 2.68%. MS (m/z, referred to the most abundant isotopes): 714, [M–H2O]; 684, [M–H2O–CO]. IR (KBr): ν (CO) 2052, 1978 and 1931(s) cm−1; ν(OH) 3475 (br, m) cm−1. 1H NMR (400MHz, CDCl3): δ 1.66 (m, 1H, CH2), 2.37 (m, 1H, CH2), 3.72 (m, 4H, OCH2), 7.35 (m, 8H, Ph from L), 7.43 (s, 4H, Ph from BArF), 7.50–7.70 (m, 12H, Ph from L+8H, Ph from BArF). 13C{1H} NMR (100MHz, CDCl3): δ 191.8 (t, 2JC,P=7Hz, CO trans to OH2), 189.8 (m, 2CO cis to OH2), 161.7 (q, 2JC,F=50Hz, CF3), 68.1 (s, OCH2), 30.7 (s, CH2). 31P{1H} NMR (161MHz, CDCl3): δ 122.1 (s). 19F{1H} NMR (376MHz, CDCl3): δ –62.5 (s). Huhmann-Vincent, 1999, J. Am. Chem. Soc., 38, 115 Reimann, 1973, J. Organometal. Chem., 59, 309, 10.1016/S0022-328X(00)95048-4 Carballo, 2001, Polyhedron, 20, 2371, 10.1016/S0277-5387(01)00820-8 Crystal and structure refinement data for fac-[Re(H2O)(CO)3L]BArF: Empirical formula, C62H40BF24O6P2Re; Formula weight, 1595.89; Temperature (K), 293(2) ; Wavelength (Å), 0.71073 ; Crystal system, Triclinic; Space group, P–1 ; a (Å), 14.232(1); b (Å), 14.429(2) ; c (Å), 18.680(2); α (°), 100.558(1); β (°), 103.440(1); γ (°), 107.336(1); Volume (Å3), 3427.5(4); Z, 2; Dcalc (Mg/m3), 1.546; Absorption coefficient (mm−1), 1.931; F(000), 1572; Crystal size (mm), 0.54×0.25×0.22; θ Range for data collection (°), 1.54–28.04; Index ranges, –18⩽h⩽18, –18⩽k⩽17, –24⩽l⩽17; Reflections collected, 20425; Independent reflections (Rint), 14,204 (0.0327); Reflections observed [I>2σ(I)], 7846; Data Completeness, 0.855; Absorption correction, Semiempirical from equivalents; Max. and min. transmission, 1.000 and 0.697; Refinement method, Full-matrix least-squares on F2; Data/restraints/parameters, 14,204/0/865; Goodness-of-fit on F2, 0.978; Final R indices [I>2σ(I)], R1=0.0662, wR2=0.1834; R indices (all data), R1=0.1082, wR2=0.1975; Largest diff. peak and hole (e·Å−3), 1.617 and –1.253. Sheldrick, 1996 McArdle, 1995, J. Appl. Cryst., 28, 65, 10.1107/S0021889894010642 Sheldrick, 1997 1992, Vol. C Bravo, 2005, J. Organometal. Chem., 690, 4899, 10.1016/j.jorganchem.2005.07.103 Liu, 2004, Organometallics, 23, 3153, 10.1021/om034196y Fang, 2000, Organometallics, 19, 4141, 10.1021/om0004693 Horn, 1984, Aust. J. Chem., 37, 1375, 10.1071/CH9841375