metal-organic compounds
Tris(2,2′-bipyridine-κ2N,N′)cobalt(II) bis(hexafluoridophosphate)
aAksaray University, Faculty of Arts and Sciences, Department of Chemistry, 68100 Aksaray, Turkey, and bDepartment of Chemistry, Leicester University, Leicester LE1 7RH, England
*Correspondence e-mail: amentes@aksaray.edu.tr
In the title compound, [Co(C10H8N2)3](PF6)2, the CoII atom is coordinated by the six N atoms of three 2,2′-bipyridyl ligands and adopts a highly distorted octahedral geometry. The crystal used was a twin, the refined ratio of twin components being 0.820 (1):0.180 (1). The features weak C—H⋯F interactions, forming a three-dimensional network.
Experimental
Crystal data
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Data collection: APEX2 (Bruker, 2005); cell SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536812050234/lr2090sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812050234/lr2090Isup2.hkl
Tris(bipyridine)cobalt(II) hexafluorophosphate was prepared by stirring a mixture of a solution containing Co(O2CC2F5)2 (0.100 g, 0.25 mmol) and bipyridine (0.120 g, 0.77 mmol) in ethanol (10 ml). The reaction mixture was stirred for 2 h. After this time NaPF6 (0.100 g, 0.59 mmol) was added and stirred for 1 h. Solid of title compound was obtained by slow evaporation of an ethanol solution in refrigerator (Yield 0.150 g, 79%; m.p. 594 K). Yellow block crystals were obtained in acetonitrile/ethanol (1:1) solution after few days. ATR-IR: 1603 ν(C=N), 1566 ν(C=C) cm-1.
Hydrogen atoms were included in calculated positions (C—H = 0.95 Å) riding on the bonded atom with isotropic displacement parameters set to 1.2Ueq(C) for all hydrogen atoms. All non-H atoms were refined with anisotropic displacement ellipsoids.
is indicated and applying the twin instruction [TWIN 0 1 0, 1 0 0, 0 0 - 1] with a BASF parameter in SHELXTL (Sheldrick, 2008), the R1 value drops to 0.049 (0.0886 without TWIN Instruction) and wR2 value drops to 0.0883 (0.2284 without TWIN instruction).The reaction of Cobalt(II) pentafluoropropionate with NaPF6 in the presence of 2,2'-bipyridine yields the coordination compound tris(bipyridine)cobalt(II) hexafluorophosphate (1), [Co(bipy)3][PF6]2. Crystals were grown by allowing slow evaporation of the complex in ethanol. The title complex crystallizes in the
P3(2) in contrast to the related compound [Co(bipy)3][Mo6O19]2 which crystallizes in P21/n (Liu et al., 2010). The structure of (1) is shown in Fig. 1. Within the divalent complex cations, the cobalt atoms are each surrounded by six N atoms of three chelating bipy ligands to complete a distorted octahedral coordination with d(Co—N) = 2.098 (7) – 2.149 (8) Å, the cis and trans N—Co—N bond angles in the range 76.6 (3) – 96.9 (3) and 167.6 (3) – 170.5 (3)°, respectively. Such distances are similar to those found in other related structures (Liu et al., 2008, Chygorin et al. 2012). There has been great interest in homoleptic imine complexes, because of great potential applications in many fields such as, catalysis, material science and medicine. The crystal packing of the title compound is presented in Fig. 2. The is stabilized by weak intermolecular C—H···F bonds.For related structures, see: Chygorin et al. (2012); Liu et al. (2008, 2010).
Data collection: APEX2 (Bruker, 2005); cell
SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. The molecular structure of (1). Displacement ellipsoids are drawn at the 30% probability level. | |
Fig. 2. A view of the crystal packing of the title compound. |
[Co(C10H8N2)3](PF6)2 | Dx = 1.678 Mg m−3 |
Mr = 817.42 | Melting point: 594 K |
Trigonal, P32 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 32 | Cell parameters from 812 reflections |
a = 10.3524 (18) Å | θ = 2.3–28.2° |
c = 26.140 (6) Å | µ = 0.73 mm−1 |
V = 2426.2 (8) Å3 | T = 150 K |
Z = 3 | Needle, yellow |
F(000) = 1233 | 0.35 × 0.16 × 0.13 mm |
Bruker APEX 2000 CCD area-detector diffractometer | 6285 independent reflections |
Radiation source: fine-focus sealed tube | 5344 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.087 |
phi and ω scans | θmax = 26.0°, θmin = 0.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | h = −12→12 |
Tmin = 0.581, Tmax = 0.862 | k = −12→12 |
19252 measured reflections | l = −32→32 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.088 | w = 1/[σ2(Fo2) + (0.0279P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.94 | (Δ/σ)max = 0.002 |
6285 reflections | Δρmax = 0.30 e Å−3 |
461 parameters | Δρmin = −0.31 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 3114 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.010 (18) |
[Co(C10H8N2)3](PF6)2 | Z = 3 |
Mr = 817.42 | Mo Kα radiation |
Trigonal, P32 | µ = 0.73 mm−1 |
a = 10.3524 (18) Å | T = 150 K |
c = 26.140 (6) Å | 0.35 × 0.16 × 0.13 mm |
V = 2426.2 (8) Å3 |
Bruker APEX 2000 CCD area-detector diffractometer | 6285 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | 5344 reflections with I > 2σ(I) |
Tmin = 0.581, Tmax = 0.862 | Rint = 0.087 |
19252 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | H-atom parameters constrained |
wR(F2) = 0.088 | Δρmax = 0.30 e Å−3 |
S = 0.94 | Δρmin = −0.31 e Å−3 |
6285 reflections | Absolute structure: Flack (1983), 3114 Friedel pairs |
461 parameters | Absolute structure parameter: 0.010 (18) |
1 restraint |
Experimental. SADABS (Bruker, 2005). Absorption correction based on 7715 reflections;Rint 0.1489 before correction and 0.0570 after. |
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 F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.31501 (7) | 0.63587 (6) | 0.16543 (3) | 0.02682 (14) | |
N1 | 0.5410 (4) | 0.7831 (4) | 0.18887 (15) | 0.0288 (9) | |
N2 | 0.4286 (4) | 0.5271 (4) | 0.13828 (15) | 0.0286 (9) | |
N3 | 0.2500 (4) | 0.5252 (4) | 0.23714 (14) | 0.0278 (9) | |
N4 | 0.2286 (4) | 0.7570 (4) | 0.20398 (14) | 0.0270 (9) | |
N5 | 0.1048 (4) | 0.4858 (4) | 0.13110 (14) | 0.0285 (9) | |
N6 | 0.3326 (4) | 0.7329 (4) | 0.09234 (14) | 0.0321 (9) | |
C1 | 0.5893 (5) | 0.9086 (5) | 0.21651 (19) | 0.0322 (11) | |
H1 | 0.5220 | 0.9440 | 0.2229 | 0.039* | |
C2 | 0.7309 (5) | 0.9875 (6) | 0.23577 (18) | 0.0339 (12) | |
H2 | 0.7617 | 1.0756 | 0.2552 | 0.041* | |
C3 | 0.8278 (6) | 0.9347 (6) | 0.22598 (19) | 0.0426 (13) | |
H3 | 0.9265 | 0.9853 | 0.2392 | 0.051* | |
C4 | 0.7788 (6) | 0.8074 (6) | 0.19675 (19) | 0.0394 (13) | |
H4 | 0.8443 | 0.7703 | 0.1895 | 0.047* | |
C5 | 0.6371 (5) | 0.7354 (5) | 0.17835 (17) | 0.0270 (10) | |
C6 | 0.5765 (5) | 0.5992 (5) | 0.14565 (17) | 0.0271 (10) | |
C7 | 0.6663 (6) | 0.5535 (6) | 0.12261 (19) | 0.0353 (11) | |
H7 | 0.7711 | 0.6079 | 0.1279 | 0.042* | |
C8 | 0.6041 (6) | 0.4286 (6) | 0.0919 (2) | 0.0411 (13) | |
H8 | 0.6653 | 0.3981 | 0.0747 | 0.049* | |
C9 | 0.4511 (6) | 0.3490 (6) | 0.0865 (2) | 0.0374 (13) | |
H9 | 0.4042 | 0.2593 | 0.0671 | 0.045* | |
C10 | 0.3682 (5) | 0.4021 (5) | 0.10954 (18) | 0.0348 (12) | |
H10 | 0.2630 | 0.3483 | 0.1051 | 0.042* | |
C11 | 0.2541 (6) | 0.4024 (5) | 0.24997 (19) | 0.0365 (13) | |
H11 | 0.3111 | 0.3731 | 0.2296 | 0.044* | |
C12 | 0.1780 (6) | 0.3163 (5) | 0.2920 (2) | 0.0383 (13) | |
H12 | 0.1845 | 0.2307 | 0.3007 | 0.046* | |
C13 | 0.0928 (6) | 0.3568 (6) | 0.3209 (2) | 0.0452 (14) | |
H13 | 0.0366 | 0.2974 | 0.3491 | 0.054* | |
C14 | 0.0903 (6) | 0.4854 (6) | 0.3082 (2) | 0.0425 (13) | |
H14 | 0.0332 | 0.5162 | 0.3278 | 0.051* | |
C15 | 0.1714 (5) | 0.5678 (5) | 0.26678 (17) | 0.0282 (10) | |
C16 | 0.1795 (5) | 0.7093 (5) | 0.25162 (18) | 0.0286 (11) | |
C17 | 0.1413 (6) | 0.7889 (6) | 0.2842 (2) | 0.0392 (13) | |
H17 | 0.1033 | 0.7519 | 0.3174 | 0.047* | |
C18 | 0.1594 (7) | 0.9260 (6) | 0.2675 (2) | 0.0486 (15) | |
H18 | 0.1396 | 0.9862 | 0.2900 | 0.058* | |
C19 | 0.2056 (6) | 0.9712 (6) | 0.2188 (2) | 0.0395 (13) | |
H19 | 0.2144 | 1.0613 | 0.2062 | 0.047* | |
C20 | 0.2391 (5) | 0.8847 (5) | 0.18840 (19) | 0.0312 (11) | |
H20 | 0.2716 | 0.9171 | 0.1544 | 0.037* | |
C21 | −0.0026 (5) | 0.3604 (6) | 0.1512 (2) | 0.0385 (12) | |
H21 | 0.0053 | 0.3407 | 0.1862 | 0.046* | |
C22 | −0.1253 (6) | 0.2570 (6) | 0.1241 (2) | 0.0435 (14) | |
H22 | −0.1999 | 0.1683 | 0.1400 | 0.052* | |
C23 | −0.1365 (6) | 0.2856 (6) | 0.0737 (2) | 0.0456 (14) | |
H23 | −0.2178 | 0.2151 | 0.0536 | 0.055* | |
C24 | −0.0301 (6) | 0.4160 (6) | 0.0526 (2) | 0.0405 (13) | |
H24 | −0.0391 | 0.4384 | 0.0180 | 0.049* | |
C25 | 0.0928 (5) | 0.5172 (6) | 0.08174 (19) | 0.0302 (11) | |
C26 | 0.2129 (5) | 0.6598 (5) | 0.06185 (18) | 0.0305 (11) | |
C27 | 0.2036 (6) | 0.7188 (6) | 0.01585 (19) | 0.0425 (14) | |
H27 | 0.1168 | 0.6670 | −0.0047 | 0.051* | |
C28 | 0.3202 (7) | 0.8532 (6) | −0.0003 (2) | 0.0453 (14) | |
H28 | 0.3144 | 0.8953 | −0.0320 | 0.054* | |
C29 | 0.4451 (6) | 0.9257 (6) | 0.0299 (2) | 0.0438 (14) | |
H29 | 0.5286 | 1.0173 | 0.0193 | 0.053* | |
C30 | 0.4453 (6) | 0.8611 (6) | 0.07615 (19) | 0.0391 (13) | |
H30 | 0.5307 | 0.9113 | 0.0974 | 0.047* | |
P1 | 0.6353 (2) | 0.34156 (18) | 0.26409 (5) | 0.0455 (4) | |
F1 | 0.7904 (4) | 0.4131 (6) | 0.23794 (18) | 0.1132 (18) | |
F2 | 0.6499 (10) | 0.2092 (8) | 0.2842 (2) | 0.210 (4) | |
F3 | 0.7010 (5) | 0.4240 (6) | 0.31495 (16) | 0.1132 (18) | |
F4 | 0.4748 (5) | 0.2696 (4) | 0.29142 (15) | 0.0856 (13) | |
F5 | 0.6100 (5) | 0.4687 (5) | 0.24542 (17) | 0.0983 (15) | |
F6 | 0.5659 (6) | 0.2568 (6) | 0.21402 (18) | 0.147 (2) | |
P2 | 0.03045 (17) | 0.98203 (18) | 0.07188 (5) | 0.0404 (4) | |
F7 | 0.1988 (3) | 1.0180 (4) | 0.06828 (15) | 0.0606 (10) | |
F8 | −0.0149 (4) | 0.8242 (4) | 0.09591 (15) | 0.0720 (12) | |
F9 | 0.0629 (4) | 1.0539 (3) | 0.12771 (11) | 0.0566 (9) | |
F10 | −0.1379 (3) | 0.9457 (4) | 0.07615 (14) | 0.0608 (10) | |
F11 | 0.0790 (4) | 1.1424 (3) | 0.04879 (12) | 0.0582 (9) | |
F12 | −0.0020 (4) | 0.9120 (4) | 0.01613 (13) | 0.0643 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0283 (4) | 0.0289 (3) | 0.0231 (3) | 0.0142 (3) | −0.0001 (3) | 0.0007 (3) |
N1 | 0.030 (2) | 0.028 (2) | 0.026 (2) | 0.0130 (19) | −0.0016 (17) | 0.0015 (17) |
N2 | 0.031 (2) | 0.029 (2) | 0.026 (2) | 0.0143 (19) | 0.0033 (18) | 0.0013 (18) |
N3 | 0.032 (2) | 0.029 (2) | 0.024 (2) | 0.0158 (19) | −0.0067 (18) | −0.0026 (17) |
N4 | 0.027 (2) | 0.029 (2) | 0.027 (2) | 0.0162 (18) | 0.0002 (17) | 0.0004 (18) |
N5 | 0.027 (2) | 0.033 (2) | 0.026 (2) | 0.0156 (19) | −0.0062 (17) | −0.0019 (18) |
N6 | 0.033 (2) | 0.034 (2) | 0.029 (2) | 0.017 (2) | −0.0004 (18) | 0.0030 (18) |
C1 | 0.037 (3) | 0.033 (3) | 0.031 (3) | 0.020 (2) | 0.003 (2) | 0.002 (2) |
C2 | 0.036 (3) | 0.031 (3) | 0.027 (3) | 0.010 (2) | 0.003 (2) | −0.003 (2) |
C3 | 0.032 (3) | 0.054 (4) | 0.036 (3) | 0.017 (3) | −0.004 (2) | −0.008 (3) |
C4 | 0.032 (3) | 0.049 (3) | 0.040 (3) | 0.023 (3) | 0.003 (2) | −0.007 (3) |
C5 | 0.035 (3) | 0.026 (2) | 0.021 (2) | 0.016 (2) | −0.001 (2) | 0.001 (2) |
C6 | 0.031 (3) | 0.026 (3) | 0.022 (3) | 0.012 (2) | 0.000 (2) | 0.001 (2) |
C7 | 0.036 (3) | 0.035 (3) | 0.037 (3) | 0.020 (3) | 0.000 (2) | −0.003 (2) |
C8 | 0.039 (3) | 0.041 (3) | 0.047 (3) | 0.023 (3) | 0.010 (3) | −0.003 (3) |
C9 | 0.043 (3) | 0.031 (3) | 0.038 (3) | 0.018 (3) | 0.001 (2) | −0.005 (2) |
C10 | 0.027 (3) | 0.030 (3) | 0.040 (3) | 0.008 (2) | −0.002 (2) | −0.003 (2) |
C11 | 0.041 (3) | 0.031 (3) | 0.040 (3) | 0.020 (2) | 0.000 (2) | −0.003 (2) |
C12 | 0.047 (3) | 0.026 (3) | 0.041 (3) | 0.018 (3) | −0.002 (3) | 0.006 (2) |
C13 | 0.061 (4) | 0.042 (3) | 0.032 (3) | 0.026 (3) | 0.007 (3) | 0.010 (3) |
C14 | 0.054 (3) | 0.050 (3) | 0.032 (3) | 0.032 (3) | 0.012 (3) | 0.008 (3) |
C15 | 0.032 (2) | 0.031 (3) | 0.022 (2) | 0.016 (2) | −0.003 (2) | −0.001 (2) |
C16 | 0.022 (2) | 0.030 (3) | 0.030 (3) | 0.010 (2) | 0.002 (2) | 0.003 (2) |
C17 | 0.059 (4) | 0.046 (3) | 0.025 (3) | 0.036 (3) | 0.007 (3) | 0.010 (3) |
C18 | 0.072 (4) | 0.053 (4) | 0.044 (4) | 0.049 (3) | −0.001 (3) | −0.004 (3) |
C19 | 0.052 (3) | 0.037 (3) | 0.040 (3) | 0.030 (3) | −0.005 (3) | −0.001 (3) |
C20 | 0.030 (3) | 0.032 (3) | 0.030 (3) | 0.014 (2) | 0.001 (2) | 0.006 (2) |
C21 | 0.028 (3) | 0.044 (3) | 0.037 (3) | 0.014 (3) | 0.002 (2) | 0.002 (2) |
C22 | 0.034 (3) | 0.041 (3) | 0.044 (3) | 0.009 (3) | −0.004 (2) | 0.004 (3) |
C23 | 0.030 (3) | 0.050 (4) | 0.045 (4) | 0.011 (3) | −0.008 (3) | −0.004 (3) |
C24 | 0.044 (3) | 0.052 (4) | 0.028 (3) | 0.026 (3) | −0.009 (2) | −0.003 (3) |
C25 | 0.027 (3) | 0.036 (3) | 0.030 (3) | 0.018 (2) | 0.002 (2) | 0.003 (2) |
C26 | 0.033 (3) | 0.038 (3) | 0.028 (3) | 0.023 (2) | 0.000 (2) | −0.004 (2) |
C27 | 0.052 (4) | 0.053 (4) | 0.025 (3) | 0.028 (3) | −0.001 (3) | 0.005 (3) |
C28 | 0.056 (4) | 0.055 (4) | 0.028 (3) | 0.030 (3) | 0.006 (3) | 0.010 (3) |
C29 | 0.054 (4) | 0.045 (3) | 0.032 (3) | 0.025 (3) | 0.012 (3) | 0.008 (2) |
C30 | 0.045 (3) | 0.042 (3) | 0.024 (3) | 0.017 (3) | 0.002 (2) | 0.002 (2) |
P1 | 0.0655 (11) | 0.0525 (10) | 0.0310 (9) | 0.0388 (9) | 0.0047 (7) | 0.0015 (7) |
F1 | 0.064 (3) | 0.187 (5) | 0.088 (3) | 0.062 (3) | 0.025 (2) | −0.003 (3) |
F2 | 0.424 (12) | 0.227 (7) | 0.152 (5) | 0.293 (9) | 0.170 (7) | 0.125 (5) |
F3 | 0.094 (3) | 0.200 (5) | 0.047 (2) | 0.075 (4) | −0.028 (2) | −0.044 (3) |
F4 | 0.089 (3) | 0.077 (3) | 0.074 (3) | 0.029 (2) | 0.034 (2) | 0.009 (2) |
F5 | 0.126 (4) | 0.107 (4) | 0.101 (3) | 0.087 (3) | 0.032 (3) | 0.055 (3) |
F6 | 0.148 (5) | 0.124 (4) | 0.074 (3) | −0.004 (4) | 0.016 (3) | −0.057 (3) |
P2 | 0.0351 (8) | 0.0404 (8) | 0.0340 (8) | 0.0101 (6) | −0.0021 (6) | −0.0015 (7) |
F7 | 0.0390 (19) | 0.050 (2) | 0.081 (3) | 0.0129 (16) | −0.0036 (18) | −0.0054 (18) |
F8 | 0.073 (3) | 0.0357 (19) | 0.087 (3) | 0.0123 (18) | 0.017 (2) | 0.0097 (18) |
F9 | 0.067 (2) | 0.056 (2) | 0.0326 (17) | 0.0197 (18) | −0.0080 (15) | −0.0012 (14) |
F10 | 0.0332 (17) | 0.068 (2) | 0.066 (2) | 0.0142 (17) | −0.0034 (16) | −0.0194 (19) |
F11 | 0.072 (2) | 0.0511 (19) | 0.0422 (19) | 0.0244 (19) | −0.0013 (18) | 0.0096 (16) |
F12 | 0.060 (2) | 0.072 (2) | 0.048 (2) | 0.0230 (19) | −0.0049 (17) | −0.0207 (19) |
Co1—N2 | 2.117 (4) | C14—C15 | 1.374 (7) |
Co1—N3 | 2.123 (4) | C14—H14 | 0.9500 |
Co1—N6 | 2.124 (4) | C15—C16 | 1.479 (6) |
Co1—N4 | 2.124 (4) | C16—C17 | 1.374 (7) |
Co1—N5 | 2.139 (4) | C17—C18 | 1.405 (7) |
Co1—N1 | 2.146 (4) | C17—H17 | 0.9500 |
N1—C5 | 1.342 (6) | C18—C19 | 1.357 (7) |
N1—C1 | 1.345 (6) | C18—H18 | 0.9500 |
N2—C6 | 1.340 (6) | C19—C20 | 1.366 (7) |
N2—C10 | 1.349 (6) | C19—H19 | 0.9500 |
N3—C11 | 1.336 (6) | C20—H20 | 0.9500 |
N3—C15 | 1.347 (6) | C21—C22 | 1.379 (7) |
N4—C20 | 1.335 (6) | C21—H21 | 0.9500 |
N4—C16 | 1.342 (6) | C22—C23 | 1.367 (7) |
N5—C21 | 1.324 (6) | C22—H22 | 0.9500 |
N5—C25 | 1.352 (6) | C23—C24 | 1.362 (7) |
N6—C30 | 1.324 (6) | C23—H23 | 0.9500 |
N6—C26 | 1.344 (6) | C24—C25 | 1.402 (7) |
C1—C2 | 1.368 (6) | C24—H24 | 0.9500 |
C1—H1 | 0.9500 | C25—C26 | 1.469 (7) |
C2—C3 | 1.385 (7) | C26—C27 | 1.374 (6) |
C2—H2 | 0.9500 | C27—C28 | 1.375 (7) |
C3—C4 | 1.382 (7) | C27—H27 | 0.9500 |
C3—H3 | 0.9500 | C28—C29 | 1.374 (8) |
C4—C5 | 1.359 (6) | C28—H28 | 0.9500 |
C4—H4 | 0.9500 | C29—C30 | 1.383 (7) |
C5—C6 | 1.493 (6) | C29—H29 | 0.9500 |
C6—C7 | 1.374 (6) | C30—H30 | 0.9500 |
C7—C8 | 1.378 (7) | P1—F6 | 1.539 (5) |
C7—H7 | 0.9500 | P1—F3 | 1.542 (4) |
C8—C9 | 1.380 (7) | P1—F2 | 1.544 (5) |
C8—H8 | 0.9500 | P1—F5 | 1.545 (4) |
C9—C10 | 1.368 (7) | P1—F1 | 1.551 (4) |
C9—H9 | 0.9500 | P1—F4 | 1.609 (4) |
C10—H10 | 0.9500 | P2—F12 | 1.587 (4) |
C11—C12 | 1.386 (7) | P2—F8 | 1.587 (4) |
C11—H11 | 0.9500 | P2—F10 | 1.592 (3) |
C12—C13 | 1.376 (7) | P2—F7 | 1.592 (4) |
C12—H12 | 0.9500 | P2—F11 | 1.594 (4) |
C13—C14 | 1.385 (7) | P2—F9 | 1.596 (3) |
C13—H13 | 0.9500 | ||
N2—Co1—N3 | 96.86 (15) | C14—C15—C16 | 122.7 (4) |
N2—Co1—N6 | 90.63 (15) | N4—C16—C17 | 121.6 (4) |
N3—Co1—N6 | 168.13 (15) | N4—C16—C15 | 115.9 (4) |
N2—Co1—N4 | 169.58 (15) | C17—C16—C15 | 122.5 (4) |
N3—Co1—N4 | 77.66 (14) | C16—C17—C18 | 118.7 (5) |
N6—Co1—N4 | 96.28 (15) | C16—C17—H17 | 120.6 |
N2—Co1—N5 | 96.15 (15) | C18—C17—H17 | 120.6 |
N3—Co1—N5 | 92.62 (14) | C19—C18—C17 | 119.0 (5) |
N6—Co1—N5 | 77.38 (15) | C19—C18—H18 | 120.5 |
N4—Co1—N5 | 92.97 (14) | C17—C18—H18 | 120.5 |
N2—Co1—N1 | 77.02 (15) | C18—C19—C20 | 118.8 (5) |
N3—Co1—N1 | 94.01 (14) | C18—C19—H19 | 120.6 |
N6—Co1—N1 | 96.65 (15) | C20—C19—H19 | 120.6 |
N4—Co1—N1 | 94.39 (15) | N4—C20—C19 | 123.3 (5) |
N5—Co1—N1 | 171.00 (15) | N4—C20—H20 | 118.3 |
C5—N1—C1 | 118.6 (4) | C19—C20—H20 | 118.3 |
C5—N1—Co1 | 115.2 (3) | N5—C21—C22 | 123.6 (5) |
C1—N1—Co1 | 125.9 (3) | N5—C21—H21 | 118.2 |
C6—N2—C10 | 117.8 (4) | C22—C21—H21 | 118.2 |
C6—N2—Co1 | 116.1 (3) | C23—C22—C21 | 118.1 (5) |
C10—N2—Co1 | 125.6 (3) | C23—C22—H22 | 120.9 |
C11—N3—C15 | 118.6 (4) | C21—C22—H22 | 120.9 |
C11—N3—Co1 | 125.6 (3) | C24—C23—C22 | 119.5 (5) |
C15—N3—Co1 | 114.3 (3) | C24—C23—H23 | 120.3 |
C20—N4—C16 | 118.4 (4) | C22—C23—H23 | 120.3 |
C20—N4—Co1 | 126.2 (3) | C23—C24—C25 | 120.1 (5) |
C16—N4—Co1 | 114.6 (3) | C23—C24—H24 | 119.9 |
C21—N5—C25 | 118.8 (4) | C25—C24—H24 | 119.9 |
C21—N5—Co1 | 126.6 (3) | N5—C25—C24 | 119.8 (4) |
C25—N5—Co1 | 114.1 (3) | N5—C25—C26 | 116.5 (4) |
C30—N6—C26 | 118.5 (4) | C24—C25—C26 | 123.7 (5) |
C30—N6—Co1 | 125.9 (3) | N6—C26—C27 | 121.2 (5) |
C26—N6—Co1 | 115.5 (3) | N6—C26—C25 | 115.8 (4) |
N1—C1—C2 | 123.0 (5) | C27—C26—C25 | 123.0 (5) |
N1—C1—H1 | 118.5 | C26—C27—C28 | 119.9 (5) |
C2—C1—H1 | 118.5 | C26—C27—H27 | 120.1 |
C1—C2—C3 | 117.9 (5) | C28—C27—H27 | 120.1 |
C1—C2—H2 | 121.1 | C29—C28—C27 | 119.1 (5) |
C3—C2—H2 | 121.1 | C29—C28—H28 | 120.5 |
C4—C3—C2 | 119.1 (5) | C27—C28—H28 | 120.5 |
C4—C3—H3 | 120.5 | C28—C29—C30 | 117.8 (5) |
C2—C3—H3 | 120.5 | C28—C29—H29 | 121.1 |
C5—C4—C3 | 120.0 (5) | C30—C29—H29 | 121.1 |
C5—C4—H4 | 120.0 | N6—C30—C29 | 123.4 (5) |
C3—C4—H4 | 120.0 | N6—C30—H30 | 118.3 |
N1—C5—C4 | 121.4 (4) | C29—C30—H30 | 118.3 |
N1—C5—C6 | 115.3 (4) | F6—P1—F3 | 178.5 (3) |
C4—C5—C6 | 123.3 (4) | F6—P1—F2 | 90.5 (4) |
N2—C6—C7 | 121.7 (4) | F3—P1—F2 | 89.2 (4) |
N2—C6—C5 | 115.6 (4) | F6—P1—F5 | 89.3 (3) |
C7—C6—C5 | 122.6 (4) | F3—P1—F5 | 90.9 (3) |
C6—C7—C8 | 119.9 (5) | F2—P1—F5 | 176.2 (4) |
C6—C7—H7 | 120.0 | F6—P1—F1 | 88.5 (3) |
C8—C7—H7 | 120.0 | F3—P1—F1 | 92.9 (3) |
C7—C8—C9 | 118.6 (5) | F2—P1—F1 | 92.1 (4) |
C7—C8—H8 | 120.7 | F5—P1—F1 | 91.7 (3) |
C9—C8—H8 | 120.7 | F6—P1—F4 | 91.9 (3) |
C10—C9—C8 | 118.6 (5) | F3—P1—F4 | 86.6 (2) |
C10—C9—H9 | 120.7 | F2—P1—F4 | 88.6 (3) |
C8—C9—H9 | 120.7 | F5—P1—F4 | 87.6 (2) |
N2—C10—C9 | 123.2 (5) | F1—P1—F4 | 179.2 (3) |
N2—C10—H10 | 118.4 | F12—P2—F8 | 90.4 (2) |
C9—C10—H10 | 118.4 | F12—P2—F10 | 90.0 (2) |
N3—C11—C12 | 122.2 (5) | F8—P2—F10 | 90.2 (2) |
N3—C11—H11 | 118.9 | F12—P2—F7 | 90.5 (2) |
C12—C11—H11 | 118.9 | F8—P2—F7 | 89.4 (2) |
C13—C12—C11 | 119.0 (5) | F10—P2—F7 | 179.4 (2) |
C13—C12—H12 | 120.5 | F12—P2—F11 | 90.7 (2) |
C11—C12—H12 | 120.5 | F8—P2—F11 | 178.6 (2) |
C12—C13—C14 | 118.9 (5) | F10—P2—F11 | 90.6 (2) |
C12—C13—H13 | 120.5 | F7—P2—F11 | 89.8 (2) |
C14—C13—H13 | 120.5 | F12—P2—F9 | 179.4 (2) |
C15—C14—C13 | 119.1 (5) | F8—P2—F9 | 90.2 (2) |
C15—C14—H14 | 120.5 | F10—P2—F9 | 89.79 (19) |
C13—C14—H14 | 120.5 | F7—P2—F9 | 89.68 (19) |
N3—C15—C14 | 122.1 (4) | F11—P2—F9 | 88.70 (19) |
N3—C15—C16 | 115.2 (4) | ||
N2—Co1—N1—C5 | −3.2 (3) | C10—N2—C6—C7 | 3.6 (7) |
N3—Co1—N1—C5 | 92.9 (3) | Co1—N2—C6—C7 | −169.0 (4) |
N6—Co1—N1—C5 | −92.3 (3) | C10—N2—C6—C5 | −179.1 (4) |
N4—Co1—N1—C5 | 170.8 (3) | Co1—N2—C6—C5 | 8.2 (5) |
N2—Co1—N1—C1 | −176.9 (4) | N1—C5—C6—N2 | −11.1 (6) |
N3—Co1—N1—C1 | −80.8 (4) | C4—C5—C6—N2 | 168.7 (5) |
N6—Co1—N1—C1 | 94.0 (4) | N1—C5—C6—C7 | 166.1 (4) |
N4—Co1—N1—C1 | −2.9 (4) | C4—C5—C6—C7 | −14.1 (7) |
N3—Co1—N2—C6 | −95.6 (3) | N2—C6—C7—C8 | −1.4 (7) |
N6—Co1—N2—C6 | 93.7 (3) | C5—C6—C7—C8 | −178.4 (4) |
N4—Co1—N2—C6 | −38.0 (10) | C6—C7—C8—C9 | −2.3 (7) |
N5—Co1—N2—C6 | 171.0 (3) | C7—C8—C9—C10 | 3.6 (8) |
N1—Co1—N2—C6 | −3.0 (3) | C6—N2—C10—C9 | −2.2 (7) |
N3—Co1—N2—C10 | 92.5 (4) | Co1—N2—C10—C9 | 169.6 (4) |
N6—Co1—N2—C10 | −78.3 (4) | C8—C9—C10—N2 | −1.4 (8) |
N4—Co1—N2—C10 | 150.0 (7) | C15—N3—C11—C12 | 1.3 (7) |
N5—Co1—N2—C10 | −0.9 (4) | Co1—N3—C11—C12 | −164.1 (4) |
N1—Co1—N2—C10 | −175.0 (4) | N3—C11—C12—C13 | 1.4 (8) |
N2—Co1—N3—C11 | −14.2 (4) | C11—C12—C13—C14 | −2.4 (8) |
N6—Co1—N3—C11 | 114.6 (8) | C12—C13—C14—C15 | 0.8 (8) |
N4—Co1—N3—C11 | 174.8 (4) | C11—N3—C15—C14 | −3.0 (7) |
N5—Co1—N3—C11 | 82.4 (4) | Co1—N3—C15—C14 | 164.0 (4) |
N1—Co1—N3—C11 | −91.5 (4) | C11—N3—C15—C16 | 176.7 (4) |
N2—Co1—N3—C15 | 179.9 (3) | Co1—N3—C15—C16 | −16.3 (5) |
N6—Co1—N3—C15 | −51.3 (9) | C13—C14—C15—N3 | 2.0 (8) |
N4—Co1—N3—C15 | 8.9 (3) | C13—C14—C15—C16 | −177.7 (5) |
N5—Co1—N3—C15 | −83.6 (3) | C20—N4—C16—C17 | −0.3 (7) |
N1—Co1—N3—C15 | 102.5 (3) | Co1—N4—C16—C17 | 170.2 (4) |
N2—Co1—N4—C20 | 111.0 (8) | C20—N4—C16—C15 | −179.5 (4) |
N3—Co1—N4—C20 | 170.1 (4) | Co1—N4—C16—C15 | −9.1 (5) |
N6—Co1—N4—C20 | −20.3 (4) | N3—C15—C16—N4 | 17.1 (6) |
N5—Co1—N4—C20 | −97.9 (4) | C14—C15—C16—N4 | −163.2 (5) |
N1—Co1—N4—C20 | 76.9 (4) | N3—C15—C16—C17 | −162.1 (4) |
N2—Co1—N4—C16 | −58.6 (9) | C14—C15—C16—C17 | 17.6 (7) |
N3—Co1—N4—C16 | 0.5 (3) | N4—C16—C17—C18 | −2.3 (8) |
N6—Co1—N4—C16 | 170.2 (3) | C15—C16—C17—C18 | 176.9 (5) |
N5—Co1—N4—C16 | 92.5 (3) | C16—C17—C18—C19 | 3.9 (9) |
N1—Co1—N4—C16 | −92.7 (3) | C17—C18—C19—C20 | −2.8 (9) |
N2—Co1—N5—C21 | 87.5 (4) | C16—N4—C20—C19 | 1.4 (7) |
N3—Co1—N5—C21 | −9.7 (4) | Co1—N4—C20—C19 | −167.8 (4) |
N6—Co1—N5—C21 | 176.8 (4) | C18—C19—C20—N4 | 0.2 (8) |
N4—Co1—N5—C21 | −87.5 (4) | C25—N5—C21—C22 | 1.9 (7) |
N2—Co1—N5—C25 | −84.1 (3) | Co1—N5—C21—C22 | −169.4 (4) |
N3—Co1—N5—C25 | 178.7 (3) | N5—C21—C22—C23 | 0.0 (8) |
N6—Co1—N5—C25 | 5.2 (3) | C21—C22—C23—C24 | −2.1 (8) |
N4—Co1—N5—C25 | 100.9 (3) | C22—C23—C24—C25 | 2.4 (8) |
N2—Co1—N6—C30 | −88.2 (4) | C21—N5—C25—C24 | −1.5 (7) |
N3—Co1—N6—C30 | 142.5 (7) | Co1—N5—C25—C24 | 170.8 (4) |
N4—Co1—N6—C30 | 84.0 (4) | C21—N5—C25—C26 | 178.3 (4) |
N5—Co1—N6—C30 | 175.7 (4) | Co1—N5—C25—C26 | −9.4 (5) |
N1—Co1—N6—C30 | −11.1 (4) | C23—C24—C25—N5 | −0.6 (7) |
N2—Co1—N6—C26 | 96.2 (3) | C23—C24—C25—C26 | 179.6 (5) |
N3—Co1—N6—C26 | −33.1 (9) | C30—N6—C26—C27 | −2.9 (7) |
N4—Co1—N6—C26 | −91.6 (3) | Co1—N6—C26—C27 | 173.1 (4) |
N5—Co1—N6—C26 | 0.1 (3) | C30—N6—C26—C25 | 179.1 (4) |
N1—Co1—N6—C26 | 173.2 (3) | Co1—N6—C26—C25 | −4.9 (5) |
C5—N1—C1—C2 | −2.1 (7) | N5—C25—C26—N6 | 9.7 (6) |
Co1—N1—C1—C2 | 171.4 (4) | C24—C25—C26—N6 | −170.5 (5) |
N1—C1—C2—C3 | 0.2 (7) | N5—C25—C26—C27 | −168.3 (5) |
C1—C2—C3—C4 | 1.1 (8) | C24—C25—C26—C27 | 11.5 (7) |
C2—C3—C4—C5 | −0.4 (8) | N6—C26—C27—C28 | 1.9 (8) |
C1—N1—C5—C4 | 2.8 (7) | C25—C26—C27—C28 | 179.8 (5) |
Co1—N1—C5—C4 | −171.4 (4) | C26—C27—C28—C29 | 0.5 (8) |
C1—N1—C5—C6 | −177.5 (4) | C27—C28—C29—C30 | −1.8 (8) |
Co1—N1—C5—C6 | 8.3 (5) | C26—N6—C30—C29 | 1.5 (7) |
C3—C4—C5—N1 | −1.5 (8) | Co1—N6—C30—C29 | −174.0 (4) |
C3—C4—C5—C6 | 178.7 (4) | C28—C29—C30—N6 | 0.8 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
C24—H24···F2i | 0.95 | 2.49 | 3.324 (7) | 146 |
C23—H23···F4i | 0.95 | 2.55 | 3.253 (7) | 131 |
C18—H18···F11ii | 0.95 | 2.52 | 3.149 (6) | 124 |
C13—H13···F10iii | 0.95 | 2.50 | 3.208 (6) | 131 |
C10—H10···F11iv | 0.95 | 2.51 | 3.265 (6) | 137 |
C9—H9···F7iv | 0.95 | 2.33 | 3.136 (6) | 142 |
C7—H7···F8v | 0.95 | 2.38 | 3.160 (7) | 139 |
C2—H2···F2vi | 0.95 | 2.33 | 3.081 (7) | 136 |
Symmetry codes: (i) −y, x−y, z−1/3; (ii) −x+y−1, −x+1, z+1/3; (iii) −x+y−1, −x, z+1/3; (iv) x, y−1, z; (v) x+1, y, z; (vi) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Co(C10H8N2)3](PF6)2 |
Mr | 817.42 |
Crystal system, space group | Trigonal, P32 |
Temperature (K) | 150 |
a, c (Å) | 10.3524 (18), 26.140 (6) |
V (Å3) | 2426.2 (8) |
Z | 3 |
Radiation type | Mo Kα |
µ (mm−1) | 0.73 |
Crystal size (mm) | 0.35 × 0.16 × 0.13 |
Data collection | |
Diffractometer | Bruker APEX 2000 CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2005) |
Tmin, Tmax | 0.581, 0.862 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 19252, 6285, 5344 |
Rint | 0.087 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.088, 0.94 |
No. of reflections | 6285 |
No. of parameters | 461 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.30, −0.31 |
Absolute structure | Flack (1983), 3114 Friedel pairs |
Absolute structure parameter | 0.010 (18) |
Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
C24—H24···F2i | 0.95 | 2.49 | 3.324 (7) | 145.9 |
C23—H23···F4i | 0.95 | 2.55 | 3.253 (7) | 131.4 |
C18—H18···F11ii | 0.95 | 2.52 | 3.149 (6) | 123.8 |
C13—H13···F10iii | 0.95 | 2.50 | 3.208 (6) | 131.2 |
C10—H10···F11iv | 0.95 | 2.51 | 3.265 (6) | 137.0 |
C9—H9···F7iv | 0.95 | 2.33 | 3.136 (6) | 141.8 |
C7—H7···F8v | 0.95 | 2.38 | 3.160 (7) | 139.2 |
C2—H2···F2vi | 0.95 | 2.33 | 3.081 (7) | 135.7 |
Symmetry codes: (i) −y, x−y, z−1/3; (ii) −x+y−1, −x+1, z+1/3; (iii) −x+y−1, −x, z+1/3; (iv) x, y−1, z; (v) x+1, y, z; (vi) x, y+1, z. |
Acknowledgements
The authors are grateful to Leicester University for the use of the X-ray diffractometer.
References
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chygorin, E. N., Petrusenko, S. R., Kokozay, V. N., Omelchenko, I. V. & Shishkin, O. V. (2012). Acta Cryst. E68, m233–m234. CSD CrossRef IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Liu, W., Xu, W., Lin, J.-L. & Xie, H.-Z. (2008). Acta Cryst. E64, m1586. Web of Science CSD CrossRef IUCr Journals Google Scholar
Liu, Y., Zhang, X., Xue, Z. & Sheng, J. (2010). Acta Cryst. E66, m756–m757. Web of Science CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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The reaction of Cobalt(II) pentafluoropropionate with NaPF6 in the presence of 2,2'-bipyridine yields the coordination compound tris(bipyridine)cobalt(II) hexafluorophosphate (1), [Co(bipy)3][PF6]2. Crystals were grown by allowing slow evaporation of the complex in ethanol. The title complex crystallizes in the space group P3(2) in contrast to the related compound [Co(bipy)3][Mo6O19]2 which crystallizes in P21/n (Liu et al., 2010). The structure of (1) is shown in Fig. 1. Within the divalent complex cations, the cobalt atoms are each surrounded by six N atoms of three chelating bipy ligands to complete a distorted octahedral coordination with d(Co—N) = 2.098 (7) – 2.149 (8) Å, the cis and trans N—Co—N bond angles in the range 76.6 (3) – 96.9 (3) and 167.6 (3) – 170.5 (3)°, respectively. Such distances are similar to those found in other related structures (Liu et al., 2008, Chygorin et al. 2012). There has been great interest in homoleptic imine complexes, because of great potential applications in many fields such as, catalysis, material science and medicine. The crystal packing of the title compound is presented in Fig. 2. The crystal structure is stabilized by weak intermolecular C—H···F bonds.