Acta Crystallographica Section E: Structure Reports Online

Acta Crystallogr Sect E Struct Rep Online. 64(Pt 3): m496-m496

μ-Hydroxido-bis[(2,2′-bipyridine)tricarbonylrhenium(I)] perrhenate

Kai Rutha, Thorsten Morawitza, Hans-Wolfram Lernera, Michael Boltea*

a. Institut 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

© Ruth et al. 2008

DOI: 10.1107/S160053680800490X

Published online: 27 February 2008

Abstract

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)°.

Related literature

For related literature, see: Gibson et al. (2003 ▶).

Experimental

Crystal data

[Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄]

M r = 1120.04

Triclinic,

a = 9.0304 (7) Å

b = 11.0506 (9) Å

c = 15.5152 (13) Å

α = 96.488 (7)°

β = 94.768 (7)°

γ = 104.038 (6)°

V = 1482.6 (2) Å³

Z = 2

Mo Kα radiation

μ = 12.28 mm⁻¹

T = 173 (2) K

0.16 × 0.15 × 0.14 mm

Data collection

Stoe IPDSII two-circle diffractometer

Absorption correction: multi-scan (MULABS; Spek, 2003 ▶; Blessing, 1995 ▶) T min = 0.142, T max = 0.188

21159 measured reflections

5550 independent reflections

4782 reflections with I > 2σ(I)

R int = 0.090

Refinement

R[F ² > 2σ(F ²)] = 0.092

wR(F ²) = 0.262

S = 1.05

5550 reflections

398 parameters

H-atom parameters constrained

Δρmax = 4.57 e Å⁻³

Δρmin = −5.65 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2001 ▶); cell refinement: 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.

Supplementary Material

Open In Web Browser

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: AT2546).

supplementary crystallographic information

Comment

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).

Experimental

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.

Refinement

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 electron density map is at 0.60Å from Re1 and the deepest hole (-5.66 e.Å⁻³) is at 0.33Å from Re3.

Figures

Fig. 1.View larger versionFig. 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.

Crystal data

See full table

Data collection

See full table

Refinement

See full table

Special details

See full table

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

See full table

Atomic displacement parameters (Å²)

See full table

Geometric parameters (Å, °)

See full table

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography

PMC Copyright Notice

The articles available from the PMC site are protected by copyright, even though access is free. Copyright is held by the respective authors or publishers who provide these articles to PMC. Users of PMC are responsible for complying with the terms and conditions defined by the copyright holder.

Users should assume that standard copyright protection applies to articles in PMC, unless an article contains an explicit license statement that gives a user additional reuse or redistribution rights. PMC does not allow automated/bulk downloading of articles that have standard copyright protection.

See the copyright notice on the PMC site, http://www.ncbi.nlm.nih.gov/pmc/about/copyright/, for further details and specific exceptions.

References

Blessing, R. H. (1995). Acta Cryst. A51, 33–38.

Gibson, D. H., Mashuta, M. S. & Yin, X. (2003). Acta Cryst. E59, m911–m913.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Spek, A. L. (2003). J. Appl. Cryst.36, 7–13.

Stoe & Cie (2001). X-AREA Stoe & Cie, Darmstadt, Germany.

[Back]

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.

[Back]

[Back]

[Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄] | Z = 2
Mr = 1120.04 | F₀₀₀ = 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 = 3.8–25.6º
c = 15.5152 (13) Å | µ = 12.28 mm⁻¹
α = 96.488 (7)º | T = 173 (2) K
β = 94.768 (7)º | Block, orange
γ = 104.038 (6)º | 0.16 × 0.15 × 0.14 mm
V = 1482.6 (2) Å³ |

[Back]

[Back]

Stoe IPDSII two-circle diffractometer | 5550 independent reflections
Radiation source: fine-focus sealed tube | 4782 reflections with I > 2σ(I)
Monochromator: graphite | Rint = 0.090
T = 173(2) K | θmax = 25.7º
ω scans | θmin = 3.7º
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

[Back]

[Back]

Refinement on F² | Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full | H-atom parameters constrained
R[F² > 2σ(F²)] = 0.092 |   w = 1/[σ²(Fo²) + (0.1565P)² + 50.8834P] where P = (Fo² + 2Fc²)/3
wR(F²) = 0.262 | (Δ/σ)max < 0.001
S = 1.05 | Δρmax = 4.57 e Å⁻³
5550 reflections | Δρmin = −5.65 e Å⁻³
398 parameters | 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)
Secondary atom site location: difference Fourier map |

[Back]

[Back]

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.

[Back]

[Back]

| 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) |

[Back]

[Back]

| U ¹¹ | U ²² | U ³³ | U ¹² | U ¹³ | U ²³
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)

[Back]

[Back]

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)

[Back]