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CAPÍTULO 3: LA INTERACCIÓN ENTRE LOS MECANISMOS DE GOBIERNO

3.4 ENDOGENEIDAD ENTRE LOS MECANISMOS DE GOBIERNO CORPORATIVO Y EL

All reflection intensities were measured at 110(2) K using a KM4/Xcalibur (detector: Sapphire3) with enhance graphite-monochromated Mo Kα radiation (λ = 0.71073 Å) for 3 or a SuperNova diffractometer (equipped with Atlas detector) with Mo Kα radiation (λ = 0.71073 Å) for 4 under the program CrysAlisPro (Versions 1.171.36.24 or 1.171.36.32 Agilent Technologies, 2012-2013). The same program was used to refine the cell dimensions and for data reduction. The structure was solved with the program SHELXS-2013 or SHELXS-2014/7 and was refined on F2 with SHELXL-2013 or SHELXL-2014/7.30 Analytical (3) or numerical

(4) absorption corrections based on a multifaceted crystal model were applied using CrysAlisPro. The temperature of the data collection was controlled using the system Cryojet (manufactured by Oxford Instruments). The H atoms were placed at calculated positions (unless otherwise specified) using the instructions AFIX 23, AFIX 43, AFIX 137 or AFIX 147 (only for 3) with isotropic displacement parameters having values 1.2 or 1.5 times Ueq of the attached C or O atoms. For 3, the H atoms attached to the major component of the disordered lattice water molecule (i.e., O1W) were found from difference Fourier maps. Their coordinates were refined freely but the O−H bond lengths and the H…H distance were restrained to be 0.84(3) and 1.33(3) Å using the DFIX instructions, respectively. The H atoms attached to the minor component (O1’) of the disordered lattice water molecule could not be retrieved.

3, Fw = 2365.03, elongated red plate, 0.40 × 0.24 × 0.05 mm3, triclinic, P-1 (no. 2), a = 11.4357(2), b = 15.3159(3), c = 17.6072(3) Å, α = 110.3534(19), β = 92.4345(17), γ = 102.7437(19)°, V = 2796.04(10) Å3 , Z = 1, Dx = 1.405 g cm−3 , µ = 0.444 mm−1, abs. corr. range: 0.873−0.979. 34323 Reflections were measured up to a resolution of (sin θ/λ)max = 0.62 Å−1. 11276 Reflections were unique (Rint = 0.0750), of which 9507 were observed [I > 2σ(I)]. 803 Parameters were refined using 275 restraints. R1/wR2 [I > 2σ(I)]: 0.0436/0.1111. R1/wR2 [all refl.]: 0.0546/0.1172. S = 1.041. Residual electron density found between −0.67 and 0.97 e Å−3. The asymmetric unit contains one Ru complex, two ClO4- counterions, as well as some lattice solvent molecules (hexane, water and acetonitrile). The structure is mostly ordered. The two perchlorate counterions are both disordered over two orientations, and the occupancy factors of the major components refine to 0.587(17) and 0.581(5). The hexane solvent molecule is found at sites of inversion symmetry (and therefore, only half of the molecule is crystallographically independent). The water molecule is found to be disordered over two

positions. The occupancy factor of the major component refines to 0.704(6). The checkCIF report generates 3 Alert level B that are concerned with the minor component of the disordered lattice water molecule. Because its occupancy factor is too low, the H atoms cannot be retrieved experimentally.

4, Fw = 1096.94, dark thick red lath, 0.31 × 0.15 × 0.08 mm3, triclinic, P-1 (no. 2), a = 13.6824(3), b = 13.6984(3), c = 14.2579(3) Å, α = 98.249(2), β = 101.025(2), γ = 115.285(2)°, V = 2294.10(9) Å3 , Z = 2, Dx = 1.588 g cm−3 , µ = 0.510 mm−1, abs. corr. range: 0.786−1.000. 35221 Reflections were measured up to a resolution of (sinθ/λ)max = 0.65 Å−1. 10524 Reflections were unique (Rint = 0.0299), of which 9340 were observed [I > 2σ(I)]. 743 Parameters were refined using 498 restraints. R1/wR2 [I > 2σ(I)]: 0.0369/0.0900. R1/wR2 [all refl.]: 0.0432/0.0945. S = 1.059. Residual electron density found between −0.64 and 0.90 e Å−3. The two PF6- counterions are found to be disordered over two orientations. The occupancy factors of the major components of the disorder refine to 0.917(3) and 0.821(8). The occupancy factor of the lattice solvent CH3CN molecule was refined freely, and its occupancy factor refines to 0.907(7).

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