(Ammine)(carbonyl)[hydridotris(pyrazol-1-yl-κN 2)borato](triphenylphosphine-κP)ruthenium(II) chloride dichloromethane disolvate

In the title compound, [Ru(CO)(NH3)(C9H10BN6)(C18H15P)]Cl·2CH2Cl2, the coordination environment around the RuII atom is distorted octahedral. One of the Ru—N(Tp) [Tp = hydridotris(pyrazol-1-yl)borate] bond lengths is slightly longer than the other two as a result of the influence of the trans CO ligand. In the crystal, N—H⋯Cl hydrogen bonds link the complex cations and Cl− anions. π–π interactions between the pyrazole rings [centroid–centroid distance = 3.764 (3) Å] are also present.


Related literature
Hydrogen-bond geometry (Å , ).  et al., 1992;Lin et al., 2008) has been used as a starting material for the synthesis of several complexes because of its substitutionally labile chloride and phosphines (Burrows, 2001). The development of Tp chemistry within group VIII has picked up the pace since then (Chen et al., 2010;Lo et al., 2010;Tong et al., 2008).
The title compound was obtained from the reaction of [Ru(Tp)(PPh 3 )(NH 3 )Cl] with CO ( Fig. 1). The ν(B-H) vibration of the title complex is found at 2481 cm -1 , which is characteristic of Tp bound to a metal center in a terdentate (N,N,N) manner. Yellow crystals were obtained by slow diffusion of hexane into a CH 2 Cl 2 solution at room temperature. The coordination geometry is approximately octahedral. One of the Ru-N(Tp) bond lengths [2.136 (3) Å] is slightly longer than the other two due to the influence of trans CO ligand (Table 1) (Gemel et al., 1996;Slugovc et al., 1998). In the crystal, N-H···Cl hydrogen bonds link the complex cations and Clanions (Table 2). π-π interactions between the pyrazole rings [centroid-centroid distance = 3.764 (3) Å] are present.

Experimental
The synthesis of the title compound was carried out as follows. To a solution of [(Tp)(PPh 3 )(NH 3 )RuCl] (0.39 g, 0.45 mmol) in methanol (20 ml), an excess of CO was added. The mixture was heated using a warm water bath for 30 min. A deep yellow color was developed during this time. The reaction mixture was stirred for a further 6 h at room temperature (298 K). Then it was concentrated to approximately half of the volume and cooled to 273 K. The yellow precipitate was filtered off, washed with ethanol and ether and dried under vacuum to give the title compound.

Refinement
H atoms were placed in idealized positions and constrained to ride on their parent atoms, with C-H = 0.95 (aromatic) and 0.99 (CH 2 ), N-H = 0.91 and B-H = 1.00 Å and with U iso (H) = 1.2(1.5 for ammine)U eq (C, B, N). The highest residual electron density was found 1.11 Å from Cl4 the deepest hole 0.78 Å from Cl3.  Molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity.

Crystal data
[Ru(CO)(NH 3 )(C 9 H 10 BN 6 )(C 18 H 15 P)]Cl·2CH 2 Cl 2 M r = 826.73 Triclinic, P1 Hall symbol: -P 1 a = 12.4813 (4) Å b = 12.5337 (4) Å c = 14.5389 (5) Å α = 83.520 (1) where P = (F o 2 + 2F c 2 )/3 (Δ/σ) max = 0.002 Δρ max = 1.38 e Å −3 Δρ min = −1.29 e Å −3 Special details Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.