Bis(3,5-dimethyl-1H-pyrazole-κN 2)silver(I) hexafluoridoantimonate

The title compound, [Ag(C5H8N2)2]SbF6, contains an Ag+ cation almost linearly bonded to two N atoms of dimethylpyrazole ligands [N—Ag—N = 176.54 (18)°]. The structure exhibits hydrogen bonding between the two dimethylpyrazole H atoms and two F atoms of one hexafluoridoantimonate anion. Three relatively short Ag⋯F contacts [2.869 (6), 2.920 (7), and 3.094 (7) Å] exist between the cation and three different SbF6 − anions. The crystal used for data collection was found to be twinned by non-merohedry, with the two components being related by a 180° rotation around the real or reciprocal a axis. Integration resulted in 11.2% of the total peaks being assigned to component 1, 11.2% to component 2, and 77.6% to both components.

The title compound, [Ag(C 5 H 8 N 2 ) 2 ]SbF 6 , contains an Ag + cation almost linearly bonded to two N atoms of dimethylpyrazole ligands  ]. The structure exhibits hydrogen bonding between the two dimethylpyrazole H atoms and two F atoms of one hexafluoridoantimonate anion. Three relatively short AgÁ Á ÁF contacts [2.869 (6), 2.920 (7), and 3.094 (7) Å ] exist between the cation and three different SbF 6 À anions. The crystal used for data collection was found to be twinned by non-merohedry, with the two components being related by a 180 rotation around the real or reciprocal a axis. Integration resulted in 11.2% of the total peaks being assigned to component 1, 11.2% to component 2, and 77.6% to both components.
In the title compound (shown in Figure 1), both hydrogen atoms on the two dimethylpyrazole ligands are H-bonded to one hexafluoridoantimonate anion (distances of 2.158 (4)Å and 2.306 (4) Å). These two fluorine atoms of the anion are displaced slightly toward the hydrogen atoms resulting in a 176.5 (2)° F-Sb-F bond angle. Similar length H-bonds are seen in other dimethylpyrazolesilver(I) and pyrazolesilver(I) complexes. In a similar structure published by Gallego et al. (2004), the 3,5-dimethylpyrazole contains an additional nitro group at the pyrazole 4-position. The anion in this structure is CF 3 SO 3 -1 . In this structure, the anion H-bonds to both pyrazole ligands, however, in this case, it is the silver cation that is structurally strained into an angle of 163.7°. Structures published by Mohamed & Fackler (2002) and Gallego et al. (2005) contained pyrazole ligands that did not have the H-atom in a syn planar position; however, in these structures each H-atom bonded to a different anion.
A Mogul geometry check (Bruno et al., 2004)  The silver cation is covalently coordinated to two pyrazole ligands. One antimonate anion H-bonds to both of these pyrazole ligands. This antimonate ion together with two additional antimonate ions form three relatively short Ag···F contacts. There is a 2.869 (6) Å separation between Ag1 and F21 of the anion at -x,-y,-z. There is a 2.920 (7) Å separation between Ag1 and F19 of the anion at 1 -x,-y,-z, and there is a 3.094 (7) Å separation between Ag1 and F21 of the anion at x,y,z. A long 3.219 (7) Å A g1···F19 separation effectively places the silver ion in an octahedral coordination environment.
The view containing these contacts is shown in the enhanced Jmol figure, Figure 2. Conversely, one antimonate anion is surrounded by three silver cations with which it makes close contacts, shown in Figure 3.

Experimental
All experimental procedures were conducted in an inert atmosphere. The title compound was prepared by dissolving 0.101 g (0.293 mmol) AgSbF 6 in 10 ml anhydrous THF. A second solution was prepared separately by dissolving 0.109 g (1.14 mmol) HPz Me2 in 50 ml anhydrous THF. The two solutions were combined in a round bottom flask, capped, covered with supplementary materials sup-2 foil, and stirred for 24 h. Crystals were obtained by decanting the solution into an Erlenmeyer flask and allowing the crystals to form out of the THF solvent via slow evaporation.

Refinement
The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell Now (Bruker, 2005), with the two components being related by a 180 degree rotation around the real or reciprocal axis a. The two components were integrated using SAINT, resulting in a total of 18534 reflections. 2075 reflections (1041 unique The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones), resulting in a BASF value of 0.45154.
The R int value given is for all reflections and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS; Bruker, 2008).
All non-H atoms were refined anisotropically. All H atoms were initially identified through difference Fourier syntheses then removed and included in the refinement in the riding-model approximation (C-H = 0.93 and 0.96Å for Ar-H and CH 3 ; N-H = 0.86 Å; U iso (H) = 1.2Ueq(C) except for methyl groups, where U iso (H) = 1.5Ueq(C)). Fig. 1. The molecular structure of the title compound with the atomic numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H-atoms are shown as spheres of arbitrary size. sup-3 Fig. 3. One antimonate anion viewed with all of the silver cations within less than van der Waals' radii.