metal-organic compounds
μ-Hydroxido-bis[(2,2′-bipyridine)tricarbonylrhenium(I)] perrhenate
aInstitut für Anorganische Chemie, J. W. Goethe-Universität Frankfurt, Max-von-Laue-Strasse 7, 60438 Frankfurt/Main, Germany
*Correspondence e-mail: bolte@chemie.uni-frankfurt.de
The title compound, [Re2(OH)(C10H8N2)2(CO)6][ReO4], is a mixed-valence rhenium compound containing discrete anions and cations. The ReI atoms are in a slightly distorted octahedral environment, whereas the ReVII atoms show the typical tetrahedral coordination mode. The dihedral angle between the two bipyridine groups is 34.3 (7)°.
Experimental
Crystal data
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Data collection: X-AREA (Stoe & Cie, 2001); cell X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S160053680800490X/at2546sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S160053680800490X/at2546Isup2.hkl
The title compound was obtained as an oxidation and hydrolysis product of [Re(CO)3(bipy)O3SCF3] from a mixture of [Re(CO)3(bipy)O3SCF3] (54 mg, 0.09 mmol) and 17.5 ml tetrahydrofuran. X-ray quality crystals of the title compound were grown by diffusion of hexane into a solution of the mixed-valence rhenium compound [(Re(CO)3bipy)2OH]+[ReO4]- in tetrahydrofuran at ambient temperature.
H atoms were geometrically positioned and refined using a riding model with fixed individual displacement parameters [U(H) = 1.2 Ueq(C,O)] and with O—H = 0.82Å and C—H = 0.95 Å. The highest peak (4.59 e.Å-3) in the final difference
is at 0.60Å from Re1 and the deepest hole (-5.66 e.Å-3) is at 0.33Å from Re3.Data collection: X-AREA (Stoe & Cie, 2001); cell
X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. Perspective view of the title compound with the atom numbering scheme; displacement ellipsoids are at the 30% probability level. H atoms are drawn as small spheres of arbitrary radii. |
[Re2(OH)(C10H8N2)2(CO)6][ReO4] | Z = 2 |
Mr = 1120.04 | F(000) = 1028 |
Triclinic, P1 | Dx = 2.509 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.0304 (7) Å | Cell parameters from 19460 reflections |
b = 11.0506 (9) Å | θ = 3.8–25.6° |
c = 15.5152 (13) Å | µ = 12.28 mm−1 |
α = 96.488 (7)° | T = 173 K |
β = 94.768 (7)° | Block, orange |
γ = 104.038 (6)° | 0.16 × 0.15 × 0.14 mm |
V = 1482.6 (2) Å3 |
Stoe IPDSII two-circle diffractometer | 5550 independent reflections |
Radiation source: fine-focus sealed tube | 4782 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.090 |
ω scans | θmax = 25.7°, θmin = 3.7° |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | h = −10→10 |
Tmin = 0.143, Tmax = 0.188 | k = −13→13 |
21159 measured reflections | l = −18→18 |
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)] = 0.092 | H-atom parameters constrained |
wR(F2) = 0.262 | w = 1/[σ2(Fo2) + (0.1565P)2 + 50.8834P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
5550 reflections | Δρmax = 4.57 e Å−3 |
398 parameters | Δρmin = −5.65 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0058 (8) |
[Re2(OH)(C10H8N2)2(CO)6][ReO4] | γ = 104.038 (6)° |
Mr = 1120.04 | V = 1482.6 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.0304 (7) Å | Mo Kα radiation |
b = 11.0506 (9) Å | µ = 12.28 mm−1 |
c = 15.5152 (13) Å | T = 173 K |
α = 96.488 (7)° | 0.16 × 0.15 × 0.14 mm |
β = 94.768 (7)° |
Stoe IPDSII two-circle diffractometer | 5550 independent reflections |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | 4782 reflections with I > 2σ(I) |
Tmin = 0.143, Tmax = 0.188 | Rint = 0.090 |
21159 measured reflections |
R[F2 > 2σ(F2)] = 0.092 | 0 restraints |
wR(F2) = 0.262 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.1565P)2 + 50.8834P] where P = (Fo2 + 2Fc2)/3 |
5550 reflections | Δρmax = 4.57 e Å−3 |
398 parameters | Δρmin = −5.65 e Å−3 |
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 | ||
Re1 | 0.76687 (9) | 0.89450 (8) | 0.70601 (5) | 0.0392 (3) | |
C1 | 0.770 (3) | 1.024 (3) | 0.806 (2) | 0.057 (7) | |
O1 | 0.771 (3) | 1.0983 (16) | 0.8628 (12) | 0.069 (5) | |
C2 | 0.910 (3) | 1.022 (3) | 0.657 (2) | 0.062 (7) | |
O2 | 1.004 (2) | 1.0976 (19) | 0.6342 (15) | 0.073 (6) | |
C3 | 0.933 (3) | 0.858 (2) | 0.7703 (14) | 0.052 (6) | |
O3 | 1.037 (2) | 0.839 (2) | 0.8152 (13) | 0.071 (5) | |
Re2 | 0.42562 (9) | 0.72867 (7) | 0.83203 (5) | 0.0352 (3) | |
C4 | 0.419 (3) | 0.901 (2) | 0.8481 (17) | 0.052 (6) | |
O4 | 0.413 (3) | 1.0039 (17) | 0.8637 (16) | 0.077 (6) | |
C5 | 0.270 (3) | 0.706 (2) | 0.7326 (16) | 0.052 (6) | |
O5 | 0.181 (2) | 0.689 (3) | 0.6702 (13) | 0.081 (7) | |
C6 | 0.266 (3) | 0.705 (2) | 0.9084 (13) | 0.044 (5) | |
O6 | 0.175 (2) | 0.6920 (19) | 0.9559 (11) | 0.061 (5) | |
O7 | 0.6037 (16) | 0.7393 (13) | 0.7439 (9) | 0.038 (3) | |
H7 | 0.6092 | 0.6704 | 0.7208 | 0.046* | |
N11 | 0.441 (2) | 0.5359 (17) | 0.8331 (12) | 0.044 (4) | |
C11 | 0.664 (3) | 0.626 (2) | 0.9353 (15) | 0.046 (5) | |
C12 | 0.554 (4) | 0.515 (2) | 0.8855 (18) | 0.062 (8) | |
C13 | 0.574 (5) | 0.394 (3) | 0.891 (2) | 0.093 (14) | |
H13 | 0.6594 | 0.3841 | 0.9270 | 0.111* | |
C14 | 0.475 (3) | 0.290 (3) | 0.845 (2) | 0.093 (6) | |
H14 | 0.4887 | 0.2082 | 0.8462 | 0.112* | |
C15 | 0.349 (4) | 0.313 (2) | 0.796 (2) | 0.093 (6) | |
H15 | 0.2705 | 0.2424 | 0.7682 | 0.112* | |
C16 | 0.333 (5) | 0.4335 (19) | 0.786 (2) | 0.093 (6) | |
H16 | 0.2511 | 0.4449 | 0.7476 | 0.111* | |
N21 | 0.620 (2) | 0.7420 (17) | 0.9301 (11) | 0.040 (4) | |
C23 | 0.801 (4) | 0.630 (4) | 0.9854 (18) | 0.083 (11) | |
H23 | 0.8352 | 0.5555 | 0.9873 | 0.100* | |
C24 | 0.883 (4) | 0.739 (4) | 1.031 (2) | 0.079 (10) | |
H24 | 0.9750 | 0.7386 | 1.0654 | 0.095* | |
C25 | 0.846 (3) | 0.850 (5) | 1.0319 (17) | 0.094 (14) | |
H25 | 0.9072 | 0.9244 | 1.0663 | 0.113* | |
C26 | 0.701 (3) | 0.849 (2) | 0.9750 (16) | 0.053 (6) | |
H26 | 0.6697 | 0.9247 | 0.9717 | 0.063* | |
N31 | 0.728 (2) | 0.755 (2) | 0.5863 (14) | 0.051 (5) | |
C32 | 0.602 (3) | 0.747 (2) | 0.5346 (13) | 0.050 (6) | |
C33 | 0.560 (4) | 0.651 (3) | 0.4601 (17) | 0.064 (7) | |
H33 | 0.4649 | 0.6393 | 0.4249 | 0.077* | |
C34 | 0.656 (4) | 0.577 (4) | 0.4399 (18) | 0.087 (12) | |
H34 | 0.6272 | 0.5122 | 0.3915 | 0.104* | |
C35 | 0.795 (5) | 0.597 (3) | 0.490 (2) | 0.083 (9) | |
H35 | 0.8670 | 0.5513 | 0.4741 | 0.100* | |
C36 | 0.828 (4) | 0.687 (3) | 0.5675 (17) | 0.059 (7) | |
H36 | 0.9202 | 0.6991 | 0.6050 | 0.071* | |
N41 | 0.565 (2) | 0.9191 (17) | 0.6320 (11) | 0.040 (4) | |
C42 | 0.501 (2) | 0.826 (2) | 0.5597 (13) | 0.043 (5) | |
C43 | 0.365 (4) | 0.827 (3) | 0.513 (2) | 0.071 (8) | |
H43 | 0.3297 | 0.7712 | 0.4605 | 0.085* | |
C44 | 0.277 (3) | 0.911 (3) | 0.5419 (16) | 0.057 (6) | |
H44 | 0.1766 | 0.9049 | 0.5152 | 0.068* | |
C45 | 0.349 (3) | 1.003 (3) | 0.6129 (17) | 0.056 (6) | |
H45 | 0.2990 | 1.0663 | 0.6312 | 0.067* | |
C46 | 0.484 (3) | 1.005 (2) | 0.6555 (16) | 0.047 (5) | |
H46 | 0.5257 | 1.0682 | 0.7039 | 0.056* | |
Re3 | 0.84808 (14) | 0.42214 (11) | 0.72586 (9) | 0.0663 (4) | |
O31 | 0.757 (3) | 0.5413 (19) | 0.7321 (13) | 0.070 (5) | |
O32 | 0.705 (3) | 0.286 (2) | 0.7035 (13) | 0.092 (8) | |
O33 | 0.930 (4) | 0.422 (3) | 0.831 (2) | 0.126 (12) | |
O34 | 0.922 (6) | 0.429 (3) | 0.639 (2) | 0.157 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0339 (5) | 0.0455 (5) | 0.0412 (5) | 0.0145 (3) | 0.0033 (3) | 0.0087 (3) |
C1 | 0.042 (12) | 0.061 (15) | 0.080 (19) | 0.022 (11) | 0.010 (11) | 0.038 (14) |
O1 | 0.117 (17) | 0.035 (8) | 0.046 (10) | 0.010 (9) | 0.009 (10) | −0.014 (7) |
C2 | 0.037 (12) | 0.060 (15) | 0.09 (2) | 0.005 (11) | 0.005 (12) | 0.017 (14) |
O2 | 0.063 (12) | 0.063 (11) | 0.087 (14) | −0.007 (9) | 0.009 (10) | 0.035 (10) |
C3 | 0.062 (14) | 0.065 (15) | 0.029 (10) | 0.026 (12) | 0.012 (10) | −0.014 (10) |
O3 | 0.057 (11) | 0.098 (15) | 0.066 (12) | 0.047 (11) | −0.013 (9) | 0.005 (10) |
Re2 | 0.0400 (5) | 0.0361 (5) | 0.0358 (5) | 0.0188 (3) | 0.0109 (3) | 0.0060 (3) |
C4 | 0.057 (14) | 0.055 (14) | 0.057 (14) | 0.031 (11) | 0.027 (11) | 0.012 (11) |
O4 | 0.091 (14) | 0.045 (10) | 0.116 (18) | 0.041 (10) | 0.056 (13) | 0.023 (10) |
C5 | 0.061 (14) | 0.055 (13) | 0.050 (13) | 0.018 (11) | 0.031 (12) | 0.025 (11) |
O5 | 0.052 (10) | 0.14 (2) | 0.051 (11) | 0.011 (11) | −0.008 (9) | 0.047 (12) |
C6 | 0.059 (13) | 0.054 (12) | 0.034 (10) | 0.039 (11) | 0.007 (9) | 0.017 (9) |
O6 | 0.069 (11) | 0.080 (12) | 0.048 (10) | 0.027 (9) | 0.032 (9) | 0.025 (9) |
O7 | 0.042 (7) | 0.032 (7) | 0.044 (8) | 0.014 (6) | 0.012 (6) | 0.005 (6) |
N11 | 0.047 (10) | 0.041 (9) | 0.047 (10) | 0.008 (8) | 0.016 (8) | 0.012 (8) |
C11 | 0.043 (11) | 0.061 (13) | 0.045 (12) | 0.027 (10) | 0.009 (9) | 0.015 (10) |
C12 | 0.10 (2) | 0.050 (13) | 0.058 (15) | 0.045 (14) | 0.051 (15) | 0.025 (12) |
C13 | 0.18 (4) | 0.09 (2) | 0.066 (18) | 0.10 (3) | 0.08 (2) | 0.053 (17) |
C14 | 0.144 (16) | 0.030 (7) | 0.103 (14) | 0.003 (9) | 0.071 (12) | −0.001 (8) |
C15 | 0.144 (16) | 0.030 (7) | 0.103 (14) | 0.003 (9) | 0.071 (12) | −0.001 (8) |
C16 | 0.144 (16) | 0.030 (7) | 0.103 (14) | 0.003 (9) | 0.071 (12) | −0.001 (8) |
N21 | 0.041 (9) | 0.045 (9) | 0.031 (8) | 0.008 (7) | 0.013 (7) | 0.003 (7) |
C23 | 0.08 (2) | 0.15 (3) | 0.041 (14) | 0.07 (2) | 0.011 (14) | 0.004 (18) |
C24 | 0.059 (17) | 0.13 (3) | 0.065 (19) | 0.05 (2) | 0.036 (15) | 0.01 (2) |
C25 | 0.041 (14) | 0.18 (4) | 0.034 (13) | −0.006 (19) | −0.008 (11) | −0.025 (18) |
C26 | 0.051 (13) | 0.045 (12) | 0.052 (13) | −0.002 (10) | 0.006 (10) | −0.008 (10) |
N31 | 0.042 (10) | 0.058 (12) | 0.058 (12) | 0.016 (9) | 0.011 (9) | 0.018 (9) |
C32 | 0.060 (14) | 0.062 (14) | 0.019 (9) | 0.000 (11) | 0.000 (9) | 0.007 (9) |
C33 | 0.081 (18) | 0.067 (16) | 0.046 (14) | 0.032 (14) | 0.013 (12) | −0.017 (12) |
C34 | 0.12 (3) | 0.12 (3) | 0.037 (14) | 0.08 (3) | 0.024 (17) | −0.007 (16) |
C35 | 0.10 (3) | 0.08 (2) | 0.08 (2) | 0.035 (19) | 0.04 (2) | 0.016 (17) |
C36 | 0.086 (18) | 0.062 (15) | 0.051 (14) | 0.051 (14) | 0.025 (13) | 0.014 (11) |
N41 | 0.046 (9) | 0.049 (10) | 0.036 (9) | 0.029 (8) | 0.015 (7) | 0.010 (7) |
C42 | 0.042 (11) | 0.054 (12) | 0.026 (9) | 0.000 (9) | 0.001 (8) | 0.002 (9) |
C43 | 0.064 (17) | 0.08 (2) | 0.067 (18) | 0.011 (15) | 0.010 (14) | 0.017 (15) |
C44 | 0.033 (11) | 0.10 (2) | 0.043 (12) | 0.029 (12) | 0.005 (9) | 0.012 (13) |
C45 | 0.064 (15) | 0.069 (16) | 0.052 (14) | 0.036 (13) | 0.014 (11) | 0.030 (12) |
C46 | 0.048 (12) | 0.050 (12) | 0.049 (13) | 0.022 (10) | 0.014 (10) | 0.008 (10) |
Re3 | 0.0648 (7) | 0.0588 (7) | 0.0775 (9) | 0.0190 (5) | 0.0181 (6) | 0.0039 (6) |
O31 | 0.095 (14) | 0.065 (11) | 0.068 (12) | 0.045 (11) | 0.037 (11) | 0.016 (9) |
O32 | 0.109 (18) | 0.091 (16) | 0.048 (11) | −0.020 (13) | 0.006 (11) | −0.008 (10) |
O33 | 0.17 (3) | 0.11 (2) | 0.11 (2) | 0.08 (2) | −0.03 (2) | −0.008 (17) |
O34 | 0.27 (5) | 0.087 (19) | 0.15 (3) | 0.06 (2) | 0.13 (3) | 0.027 (19) |
Re1—C3 | 1.88 (3) | C23—C24 | 1.34 (5) |
Re1—C2 | 1.93 (3) | C23—H23 | 0.9500 |
Re1—C1 | 1.98 (3) | C24—C25 | 1.34 (6) |
Re1—O7 | 2.146 (14) | C24—H24 | 0.9500 |
Re1—N41 | 2.165 (17) | C25—C26 | 1.51 (4) |
Re1—N31 | 2.22 (2) | C25—H25 | 0.9500 |
C1—O1 | 1.13 (3) | C26—H26 | 0.9500 |
C2—O2 | 1.15 (3) | N31—C32 | 1.32 (3) |
C3—O3 | 1.20 (3) | N31—C36 | 1.33 (3) |
Re2—C4 | 1.91 (2) | C32—C33 | 1.43 (3) |
Re2—C6 | 1.93 (2) | C32—C42 | 1.46 (4) |
Re2—C5 | 1.95 (3) | C33—C34 | 1.36 (4) |
Re2—N11 | 2.171 (18) | C33—H33 | 0.9500 |
Re2—O7 | 2.185 (14) | C34—C35 | 1.38 (5) |
Re2—N21 | 2.190 (18) | C34—H34 | 0.9500 |
C4—O4 | 1.15 (3) | C35—C36 | 1.43 (4) |
C5—O5 | 1.17 (3) | C35—H35 | 0.9500 |
C6—O6 | 1.15 (3) | C36—H36 | 0.9500 |
O7—H7 | 0.8199 | N41—C46 | 1.37 (3) |
N11—C12 | 1.33 (4) | N41—C42 | 1.41 (3) |
N11—C16 | 1.39 (4) | C42—C43 | 1.37 (4) |
C11—C23 | 1.39 (4) | C43—C44 | 1.41 (4) |
C11—N21 | 1.44 (3) | C43—H43 | 0.9500 |
C11—C12 | 1.47 (4) | C44—C45 | 1.41 (4) |
C12—C13 | 1.40 (3) | C44—H44 | 0.9500 |
C13—C14 | 1.35 (5) | C45—C46 | 1.33 (4) |
C13—H13 | 0.9500 | C45—H45 | 0.9500 |
C14—C15 | 1.41 (4) | C46—H46 | 0.9500 |
C14—H14 | 0.9500 | Re3—O34 | 1.56 (3) |
C15—C16 | 1.40 (3) | Re3—O32 | 1.71 (2) |
C15—H15 | 0.9500 | Re3—O31 | 1.710 (18) |
C16—H16 | 0.9500 | Re3—O33 | 1.73 (3) |
N21—C26 | 1.32 (3) | ||
C3—Re1—C2 | 89.7 (12) | C15—C16—H16 | 121.2 |
C3—Re1—C1 | 86.7 (9) | C26—N21—C11 | 122 (2) |
C2—Re1—C1 | 88.0 (12) | C26—N21—Re2 | 123.2 (17) |
C3—Re1—O7 | 92.6 (9) | C11—N21—Re2 | 114.8 (14) |
C2—Re1—O7 | 172.7 (10) | C24—C23—C11 | 120 (3) |
C1—Re1—O7 | 99.1 (8) | C24—C23—H23 | 120.2 |
C3—Re1—N41 | 174.9 (10) | C11—C23—H23 | 120.2 |
C2—Re1—N41 | 94.8 (9) | C23—C24—C25 | 125 (3) |
C1—Re1—N41 | 95.9 (8) | C23—C24—H24 | 117.5 |
O7—Re1—N41 | 82.7 (6) | C25—C24—H24 | 117.5 |
C3—Re1—N31 | 102.1 (8) | C24—C25—C26 | 117 (3) |
C2—Re1—N31 | 93.7 (11) | C24—C25—H25 | 121.7 |
C1—Re1—N31 | 171.1 (8) | C26—C25—H25 | 121.7 |
O7—Re1—N31 | 79.1 (6) | N21—C26—C25 | 119 (3) |
N41—Re1—N31 | 75.2 (7) | N21—C26—H26 | 120.7 |
O1—C1—Re1 | 179 (2) | C25—C26—H26 | 120.7 |
O2—C2—Re1 | 174 (3) | C32—N31—C36 | 123 (2) |
O3—C3—Re1 | 176.5 (18) | C32—N31—Re1 | 114.8 (17) |
C4—Re2—C6 | 84.8 (9) | C36—N31—Re1 | 122.3 (18) |
C4—Re2—C5 | 86.5 (11) | N31—C32—C33 | 119 (3) |
C6—Re2—C5 | 89.6 (9) | N31—C32—C42 | 119 (2) |
C4—Re2—N11 | 172.1 (9) | C33—C32—C42 | 122 (2) |
C6—Re2—N11 | 91.2 (8) | C34—C33—C32 | 120 (3) |
C5—Re2—N11 | 100.3 (9) | C34—C33—H33 | 120.0 |
C4—Re2—O7 | 99.7 (8) | C32—C33—H33 | 120.0 |
C6—Re2—O7 | 175.5 (7) | C33—C34—C35 | 120 (3) |
C5—Re2—O7 | 90.3 (7) | C33—C34—H34 | 120.2 |
N11—Re2—O7 | 84.4 (6) | C35—C34—H34 | 120.2 |
C4—Re2—N21 | 98.5 (9) | C34—C35—C36 | 119 (3) |
C6—Re2—N21 | 97.7 (7) | C34—C35—H35 | 120.6 |
C5—Re2—N21 | 171.5 (8) | C36—C35—H35 | 120.6 |
N11—Re2—N21 | 75.3 (7) | N31—C36—C35 | 120 (3) |
O7—Re2—N21 | 82.2 (6) | N31—C36—H36 | 120.2 |
O4—C4—Re2 | 175 (2) | C35—C36—H36 | 120.2 |
O5—C5—Re2 | 176 (2) | C46—N41—C42 | 117.9 (19) |
O6—C6—Re2 | 178 (2) | C46—N41—Re1 | 125.9 (15) |
Re1—O7—Re2 | 132.8 (6) | C42—N41—Re1 | 115.6 (14) |
Re1—O7—H7 | 113.6 | C43—C42—N41 | 120 (2) |
Re2—O7—H7 | 113.6 | C43—C42—C32 | 126 (2) |
C12—N11—C16 | 119 (2) | N41—C42—C32 | 113.5 (18) |
C12—N11—Re2 | 118.4 (16) | C42—C43—C44 | 122 (3) |
C16—N11—Re2 | 122.6 (18) | C42—C43—H43 | 119.2 |
C23—C11—N21 | 119 (3) | C44—C43—H43 | 119.2 |
C23—C11—C12 | 128 (3) | C45—C44—C43 | 115 (2) |
N21—C11—C12 | 113.7 (19) | C45—C44—H44 | 122.4 |
N11—C12—C13 | 123 (3) | C43—C44—H44 | 122.4 |
N11—C12—C11 | 117 (2) | C46—C45—C44 | 123 (2) |
C13—C12—C11 | 120 (3) | C46—C45—H45 | 118.7 |
C14—C13—C12 | 121 (4) | C44—C45—H45 | 118.7 |
C14—C13—H13 | 119.4 | C45—C46—N41 | 122 (2) |
C12—C13—H13 | 119.4 | C45—C46—H46 | 118.8 |
C13—C14—C15 | 115 (3) | N41—C46—H46 | 118.8 |
C13—C14—H14 | 122.3 | O34—Re3—O32 | 102.9 (18) |
C15—C14—H14 | 122.3 | O34—Re3—O31 | 104.5 (15) |
C14—C15—C16 | 124 (3) | O32—Re3—O31 | 105.8 (13) |
C14—C15—H15 | 118.1 | O34—Re3—O33 | 130 (2) |
C16—C15—H15 | 118.1 | O32—Re3—O33 | 105.1 (15) |
N11—C16—C15 | 118 (3) | O31—Re3—O33 | 106.2 (12) |
N11—C16—H16 | 121.2 | ||
C3—Re1—C1—O1 | −168 (100) | C12—C11—N21—C26 | 176 (2) |
C2—Re1—C1—O1 | 102 (100) | C23—C11—N21—Re2 | 169.9 (19) |
O7—Re1—C1—O1 | −76 (100) | C12—C11—N21—Re2 | −11 (2) |
N41—Re1—C1—O1 | 7 (100) | C4—Re2—N21—C26 | −4.7 (19) |
N31—Re1—C1—O1 | 1 (100) | C6—Re2—N21—C26 | −90.6 (18) |
C3—Re1—C2—O2 | −19 (27) | C5—Re2—N21—C26 | 121 (5) |
C1—Re1—C2—O2 | 68 (27) | N11—Re2—N21—C26 | −179.8 (18) |
O7—Re1—C2—O2 | −127 (25) | O7—Re2—N21—C26 | 94.0 (18) |
N41—Re1—C2—O2 | 164 (27) | C4—Re2—N21—C11 | −178.0 (15) |
N31—Re1—C2—O2 | −121 (27) | C6—Re2—N21—C11 | 96.1 (15) |
C2—Re1—C3—O3 | 102 (42) | C5—Re2—N21—C11 | −53 (6) |
C1—Re1—C3—O3 | 14 (42) | N11—Re2—N21—C11 | 6.9 (13) |
O7—Re1—C3—O3 | −85 (42) | O7—Re2—N21—C11 | −79.3 (14) |
N41—Re1—C3—O3 | −106 (40) | N21—C11—C23—C24 | 3 (4) |
N31—Re1—C3—O3 | −164 (41) | C12—C11—C23—C24 | −176 (3) |
C6—Re2—C4—O4 | 35 (28) | C11—C23—C24—C25 | −1 (5) |
C5—Re2—C4—O4 | 125 (29) | C23—C24—C25—C26 | −1 (5) |
N11—Re2—C4—O4 | −25 (33) | C11—N21—C26—C25 | 1 (3) |
O7—Re2—C4—O4 | −145 (28) | Re2—N21—C26—C25 | −171.7 (18) |
N21—Re2—C4—O4 | −62 (29) | C24—C25—C26—N21 | 1 (4) |
C4—Re2—C5—O5 | 131 (33) | C3—Re1—N31—C32 | 170.4 (17) |
C6—Re2—C5—O5 | −144 (33) | C2—Re1—N31—C32 | −99.1 (18) |
N11—Re2—C5—O5 | −53 (33) | C1—Re1—N31—C32 | 1 (6) |
O7—Re2—C5—O5 | 32 (33) | O7—Re1—N31—C32 | 80.1 (16) |
N21—Re2—C5—O5 | 5 (37) | N41—Re1—N31—C32 | −5.1 (16) |
C4—Re2—C6—O6 | −85 (55) | C3—Re1—N31—C36 | −11 (2) |
C5—Re2—C6—O6 | −171 (55) | C2—Re1—N31—C36 | 79 (2) |
N11—Re2—C6—O6 | 88 (55) | C1—Re1—N31—C36 | 179 (5) |
O7—Re2—C6—O6 | 101 (57) | O7—Re1—N31—C36 | −102 (2) |
N21—Re2—C6—O6 | 13 (56) | N41—Re1—N31—C36 | 173 (2) |
C3—Re1—O7—Re2 | 108.3 (10) | C36—N31—C32—C33 | 8 (4) |
C2—Re1—O7—Re2 | −143 (7) | Re1—N31—C32—C33 | −174.1 (19) |
C1—Re1—O7—Re2 | 21.2 (12) | C36—N31—C32—C42 | −179 (2) |
N41—Re1—O7—Re2 | −73.6 (10) | Re1—N31—C32—C42 | −1 (3) |
N31—Re1—O7—Re2 | −149.9 (11) | N31—C32—C33—C34 | −5 (4) |
C4—Re2—O7—Re1 | 13.1 (12) | C42—C32—C33—C34 | −178 (3) |
C6—Re2—O7—Re1 | −173 (9) | C32—C33—C34—C35 | −1 (5) |
C5—Re2—O7—Re1 | 99.5 (11) | C33—C34—C35—C36 | 6 (5) |
N11—Re2—O7—Re1 | −160.1 (10) | C32—N31—C36—C35 | −3 (4) |
N21—Re2—O7—Re1 | −84.3 (10) | Re1—N31—C36—C35 | 179 (2) |
C4—Re2—N11—C12 | −40 (7) | C34—C35—C36—N31 | −4 (5) |
C6—Re2—N11—C12 | −99.6 (17) | C3—Re1—N41—C46 | 123 (8) |
C5—Re2—N11—C12 | 170.6 (17) | C2—Re1—N41—C46 | −86 (2) |
O7—Re2—N11—C12 | 81.4 (16) | C1—Re1—N41—C46 | 2.2 (19) |
N21—Re2—N11—C12 | −2.0 (16) | O7—Re1—N41—C46 | 100.6 (18) |
C4—Re2—N11—C16 | 136 (6) | N31—Re1—N41—C46 | −178.8 (19) |
C6—Re2—N11—C16 | 76 (2) | C3—Re1—N41—C42 | −48 (9) |
C5—Re2—N11—C16 | −14 (2) | C2—Re1—N41—C42 | 103.1 (17) |
O7—Re2—N11—C16 | −102.9 (19) | C1—Re1—N41—C42 | −168.5 (15) |
N21—Re2—N11—C16 | 174 (2) | O7—Re1—N41—C42 | −70.1 (14) |
C16—N11—C12—C13 | 4 (3) | N31—Re1—N41—C42 | 10.6 (14) |
Re2—N11—C12—C13 | −179.8 (18) | C46—N41—C42—C43 | 3 (3) |
C16—N11—C12—C11 | −179 (2) | Re1—N41—C42—C43 | 174.5 (19) |
Re2—N11—C12—C11 | −3 (3) | C46—N41—C42—C32 | 174.2 (19) |
C23—C11—C12—N11 | −171 (3) | Re1—N41—C42—C32 | −14 (2) |
N21—C11—C12—N11 | 9 (3) | N31—C32—C42—C43 | −179 (2) |
C23—C11—C12—C13 | 5 (4) | C33—C32—C42—C43 | −7 (4) |
N21—C11—C12—C13 | −174 (2) | N31—C32—C42—N41 | 10 (3) |
N11—C12—C13—C14 | −3 (4) | C33—C32—C42—N41 | −177 (2) |
C11—C12—C13—C14 | −180 (2) | N41—C42—C43—C44 | −8 (4) |
C12—C13—C14—C15 | −2 (4) | C32—C42—C43—C44 | −178 (2) |
C13—C14—C15—C16 | 7 (5) | C42—C43—C44—C45 | 9 (4) |
C12—N11—C16—C15 | 0 (4) | C43—C44—C45—C46 | −6 (4) |
Re2—N11—C16—C15 | −176 (2) | C44—C45—C46—N41 | 2 (4) |
C14—C15—C16—N11 | −6 (5) | C42—N41—C46—C45 | 0 (3) |
C23—C11—N21—C26 | −4 (3) | Re1—N41—C46—C45 | −170.4 (18) |
Experimental details
Crystal data | |
Chemical formula | [Re2(OH)(C10H8N2)2(CO)6][ReO4] |
Mr | 1120.04 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 9.0304 (7), 11.0506 (9), 15.5152 (13) |
α, β, γ (°) | 96.488 (7), 94.768 (7), 104.038 (6) |
V (Å3) | 1482.6 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 12.28 |
Crystal size (mm) | 0.16 × 0.15 × 0.14 |
Data collection | |
Diffractometer | Stoe IPDSII two-circle diffractometer |
Absorption correction | Multi-scan (MULABS; Spek, 2003; Blessing, 1995) |
Tmin, Tmax | 0.143, 0.188 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21159, 5550, 4782 |
Rint | 0.090 |
(sin θ/λ)max (Å−1) | 0.609 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.092, 0.262, 1.05 |
No. of reflections | 5550 |
No. of parameters | 398 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.1565P)2 + 50.8834P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 4.57, −5.65 |
Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL-Plus (Sheldrick, 2008).
References
Blessing, R. H. (1995). Acta Cryst. A51, 33–38. CrossRef CAS Web of Science IUCr Journals Google Scholar
Gibson, D. H., Mashuta, M. S. & Yin, X. (2003). Acta Cryst. E59, m911–m913. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany. Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
We report here the X-ray crystal structure analysis of the mixed-valence rhenium compound [(Re(CO)3bipy)2OH]+[ReO4]- (bipy = C10H6N2). Thereby Re features in the cation an oxidation state +1 whereas in the perrhenate anion the Re center possesses the oxidation number +7. Surprisingly we have obtained the title compound as an oxidation and hydrolysis product of [Re(CO)3(bipy)O3SCF3]. X-ray quality crystals of the title compound were grown by diffusion of hexane into a tetrahydrofuran solution of the mixed-valence rhenium compound [(Re(CO)3bipy)2OH]+[ReO4]- at ambient temperature.
The title compound, [C26H17N4O7Re2]+[ReO4]-, is a mixed-valence rhenium compound containing discrete anions and cations. The ReI atoms are in a slightly distorted octahedral environment, whereas the ReVII atoms show the typical tetrahedral coordination mode. The dihedral angle between the two bipyridine moieties is 34.3 (7)°. A comparable compound with the bipyridine residues substituted by methyl groups in the para-position to the N atoms was determined by Gibson et al. (2003).