Bis[tris(3,5-dimethyl-1H-pyrazol-1-yl-κN2)methyl]sodium trifluoromethanesulfonate (original) (raw)
2012, Acta Crystallographica Section E-structure Reports Online
In the title salt, [Na(C 16 H 22 N 6) 2 ]CF 3 SO 3 , the Na + cation is coordinated by six N atoms from two tridentate tris(3,5dimethylpyrazol-1-yl)methane ligands in a distorted octahedral geometry. The Na-N distances range from 2.427 (3) to 2.507 (3) Å , intra-ligand N-Na-N angles range from 74.71 (8) to 79.31 (9) , and adjacent inter-ligand N-Na-N angles range between 100.42 (9) and 104.97 (9). The structure is twinned by inversion [occupancy factors = 0.50 (9)] and the trifluoromethanesulfonate anion is disordered, with two endover-end orientations of unequal occupancy [0.781 (3) and 0.219 (3)]. Related literature For ligand synthesis details, see: Reger et al. (2000). For structural, spectroscopic and angular overlap studies of tris-(pyrazol-1-yl)methane complexes, see: Astley et al. (1993). For details of the refinement strategy for twinned and disordered structures, see: Parkin (2000); Spek (2009). Experimental Crystal data [Na(C 16 H 22 N 6) 2 ]CF 3 O 3 S M r = 768.85 Monoclinic, Pc a = 9.0579 (1) Å b = 12.5733 (1) Å c = 16.4386 (2) Å = 90.5917 (4) V = 1872.05 (3) Å 3 Z = 2 Mo K radiation = 0.17 mm À1 T = 90 K 0.22 Â 0.18 Â 0.12 mm Data collection Nonius KappaCCD diffractometer Absorption correction: multi-scan [SCALEPACK (Otwinowski & Minor, 1997) and XABS2 (Parkin et al. 1995)] T min = 0.965, T max = 0.981 47745 measured reflections 8385 independent reflections 7036 reflections with I > 2(I) R int = 0.043 Refinement R[F 2 > 2(F 2)] = 0.041 wR(F 2) = 0.112 S = 1.09 8385 reflections 516 parameters 59 restraints H-atom parameters constrained Á max = 0.26 e Å À3 Á min = À0.27 e Å À3
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Bis[tris(3,5-dimethyl-1H-pyrazol-1-yl-κN2)methyl]sodium trifluoromethanesulfonate
Acta Crystallographica Section E Structure Reports Online, 2012
In the title salt, [Na(C 16 H 22 N 6) 2 ]CF 3 SO 3 , the Na + cation is coordinated by six N atoms from two tridentate tris(3,5dimethylpyrazol-1-yl)methane ligands in a distorted octahedral geometry. The Na-N distances range from 2.427 (3) to 2.507 (3) Å , intra-ligand N-Na-N angles range from 74.71 (8) to 79.31 (9) , and adjacent inter-ligand N-Na-N angles range between 100.42 (9) and 104.97 (9). The structure is twinned by inversion [occupancy factors = 0.50 (9)] and the trifluoromethanesulfonate anion is disordered, with two endover-end orientations of unequal occupancy [0.781 (3) and 0.219 (3)]. Related literature For ligand synthesis details, see: Reger et al. (2000). For structural, spectroscopic and angular overlap studies of tris-(pyrazol-1-yl)methane complexes, see: Astley et al. (1993). For details of the refinement strategy for twinned and disordered structures, see: Parkin (2000); Spek (2009). Experimental Crystal data [Na(C 16 H 22 N 6) 2 ]CF 3 O 3 S M r = 768.85 Monoclinic, Pc a = 9.0579 (1) Å b = 12.5733 (1) Å c = 16.4386 (2) Å = 90.5917 (4) V = 1872.05 (3) Å 3 Z = 2 Mo K radiation = 0.17 mm À1 T = 90 K 0.22 Â 0.18 Â 0.12 mm Data collection Nonius KappaCCD diffractometer Absorption correction: multi-scan [SCALEPACK (Otwinowski & Minor, 1997) and XABS2 (Parkin et al. 1995)] T min = 0.965, T max = 0.981 47745 measured reflections 8385 independent reflections 7036 reflections with I > 2(I) R int = 0.043 Refinement R[F 2 > 2(F 2)] = 0.041 wR(F 2) = 0.112 S = 1.09 8385 reflections 516 parameters 59 restraints H-atom parameters constrained Á max = 0.26 e Å À3 Á min = À0.27 e Å À3
Inorganic Chemistry, 1984
The compound NazRu(CN),N0.2H20 has been synthesized from ruthenium trichloride and sodium cyanide by oxidation with nitric acid. The orange prismatic crystals belong to the orthorhombic space group Pnmm with a = 6.303 (2) A, b = 12.084 (4) A, c = 15.833 ( 5 ) A, and Z = 4. The structure was refined with use of the initial atomic coordinates from the isostructural sodium nitroprusside, NazFe(CN)SNO-2Hz0, to R = 0.030, R , = 0.028, for 1588 independent reflections; hydrogen atoms were then located in a difference Fourier synthesis and refined with use of constraints in bond lengths R = 0.024, R , = 0.023). Important bond lengths and angles are as follows:
Structure of trisodium hexafluoromanganate(III)
Acta Crystallographica Section C Crystal Structure Communications
= 0.0144 for 550 unique reflections [Fo > 30.(Fo)]. The structure is isostructural with that of the cryolite Na3A1F6 and shows the weakest static Jahn-Teller distortion known to date for [MnF6] 3-octahedra [d(Mn-F) axial 2.0176 (8), mean equatorial 1.880 (1) A]. The ordering of the elongated octahedra is ferrodistortive. Of the Na ions, one third have octahedral and the remainder have bicapped trigonal prismatic eight coordination.
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