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Acta Crystallogr Sect E Struct Rep Online. 2008 March 1; 64(Pt 3): m496.
Published online 2008 February 27. doi:  10.1107/S160053680800490X
PMCID: PMC2960830

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

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 [triangle]).

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Object name is e-64-0m496-scheme1.jpg

Experimental

Crystal data

  • [Re2(OH)(C10H8N2)2(CO)6][ReO4]
  • M r = 1120.04
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m496-efi1.jpg
  • 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 [triangle]; Blessing, 1995 [triangle]) 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 [triangle]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680800490X/at2546sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680800490X/at2546Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

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.
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

[Re2(OH)(C10H8N2)2(CO)6][ReO4]Z = 2
Mr = 1120.04F000 = 1028
Triclinic, P1Dx = 2.509 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 9.0304 (7) ÅCell parameters from 19460 reflections
b = 11.0506 (9) Åθ = 3.8–25.6º
c = 15.5152 (13) ŵ = 12.28 mm1
α = 96.488 (7)ºT = 173 (2) K
β = 94.768 (7)ºBlock, orange
γ = 104.038 (6)º0.16 × 0.15 × 0.14 mm
V = 1482.6 (2) Å3

Data collection

Stoe IPDSII two-circle diffractometer5550 independent reflections
Radiation source: fine-focus sealed tube4782 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.090
T = 173(2) Kθmax = 25.7º
ω scansθmin = 3.7º
Absorption correction: multi-scan(MULABS; Spek, 2003; Blessing, 1995)h = −10→10
Tmin = 0.143, Tmax = 0.188k = −13→13
21159 measured reflectionsl = −18→18

Refinement

Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-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 = 1.05Δρmax = 4.57 e Å3
5550 reflectionsΔρmin = −5.65 e Å3
398 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0058 (8)
Secondary atom site location: difference Fourier map

Special details

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.

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

xyzUiso*/Ueq
Re10.76687 (9)0.89450 (8)0.70601 (5)0.0392 (3)
C10.770 (3)1.024 (3)0.806 (2)0.057 (7)
O10.771 (3)1.0983 (16)0.8628 (12)0.069 (5)
C20.910 (3)1.022 (3)0.657 (2)0.062 (7)
O21.004 (2)1.0976 (19)0.6342 (15)0.073 (6)
C30.933 (3)0.858 (2)0.7703 (14)0.052 (6)
O31.037 (2)0.839 (2)0.8152 (13)0.071 (5)
Re20.42562 (9)0.72867 (7)0.83203 (5)0.0352 (3)
C40.419 (3)0.901 (2)0.8481 (17)0.052 (6)
O40.413 (3)1.0039 (17)0.8637 (16)0.077 (6)
C50.270 (3)0.706 (2)0.7326 (16)0.052 (6)
O50.181 (2)0.689 (3)0.6702 (13)0.081 (7)
C60.266 (3)0.705 (2)0.9084 (13)0.044 (5)
O60.175 (2)0.6920 (19)0.9559 (11)0.061 (5)
O70.6037 (16)0.7393 (13)0.7439 (9)0.038 (3)
H70.60920.67040.72080.046*
N110.441 (2)0.5359 (17)0.8331 (12)0.044 (4)
C110.664 (3)0.626 (2)0.9353 (15)0.046 (5)
C120.554 (4)0.515 (2)0.8855 (18)0.062 (8)
C130.574 (5)0.394 (3)0.891 (2)0.093 (14)
H130.65940.38410.92700.111*
C140.475 (3)0.290 (3)0.845 (2)0.093 (6)
H140.48870.20820.84620.112*
C150.349 (4)0.313 (2)0.796 (2)0.093 (6)
H150.27050.24240.76820.112*
C160.333 (5)0.4335 (19)0.786 (2)0.093 (6)
H160.25110.44490.74760.111*
N210.620 (2)0.7420 (17)0.9301 (11)0.040 (4)
C230.801 (4)0.630 (4)0.9854 (18)0.083 (11)
H230.83520.55550.98730.100*
C240.883 (4)0.739 (4)1.031 (2)0.079 (10)
H240.97500.73861.06540.095*
C250.846 (3)0.850 (5)1.0319 (17)0.094 (14)
H250.90720.92441.06630.113*
C260.701 (3)0.849 (2)0.9750 (16)0.053 (6)
H260.66970.92470.97170.063*
N310.728 (2)0.755 (2)0.5863 (14)0.051 (5)
C320.602 (3)0.747 (2)0.5346 (13)0.050 (6)
C330.560 (4)0.651 (3)0.4601 (17)0.064 (7)
H330.46490.63930.42490.077*
C340.656 (4)0.577 (4)0.4399 (18)0.087 (12)
H340.62720.51220.39150.104*
C350.795 (5)0.597 (3)0.490 (2)0.083 (9)
H350.86700.55130.47410.100*
C360.828 (4)0.687 (3)0.5675 (17)0.059 (7)
H360.92020.69910.60500.071*
N410.565 (2)0.9191 (17)0.6320 (11)0.040 (4)
C420.501 (2)0.826 (2)0.5597 (13)0.043 (5)
C430.365 (4)0.827 (3)0.513 (2)0.071 (8)
H430.32970.77120.46050.085*
C440.277 (3)0.911 (3)0.5419 (16)0.057 (6)
H440.17660.90490.51520.068*
C450.349 (3)1.003 (3)0.6129 (17)0.056 (6)
H450.29901.06630.63120.067*
C460.484 (3)1.005 (2)0.6555 (16)0.047 (5)
H460.52571.06820.70390.056*
Re30.84808 (14)0.42214 (11)0.72586 (9)0.0663 (4)
O310.757 (3)0.5413 (19)0.7321 (13)0.070 (5)
O320.705 (3)0.286 (2)0.7035 (13)0.092 (8)
O330.930 (4)0.422 (3)0.831 (2)0.126 (12)
O340.922 (6)0.429 (3)0.639 (2)0.157 (17)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Re10.0339 (5)0.0455 (5)0.0412 (5)0.0145 (3)0.0033 (3)0.0087 (3)
C10.042 (12)0.061 (15)0.080 (19)0.022 (11)0.010 (11)0.038 (14)
O10.117 (17)0.035 (8)0.046 (10)0.010 (9)0.009 (10)−0.014 (7)
C20.037 (12)0.060 (15)0.09 (2)0.005 (11)0.005 (12)0.017 (14)
O20.063 (12)0.063 (11)0.087 (14)−0.007 (9)0.009 (10)0.035 (10)
C30.062 (14)0.065 (15)0.029 (10)0.026 (12)0.012 (10)−0.014 (10)
O30.057 (11)0.098 (15)0.066 (12)0.047 (11)−0.013 (9)0.005 (10)
Re20.0400 (5)0.0361 (5)0.0358 (5)0.0188 (3)0.0109 (3)0.0060 (3)
C40.057 (14)0.055 (14)0.057 (14)0.031 (11)0.027 (11)0.012 (11)
O40.091 (14)0.045 (10)0.116 (18)0.041 (10)0.056 (13)0.023 (10)
C50.061 (14)0.055 (13)0.050 (13)0.018 (11)0.031 (12)0.025 (11)
O50.052 (10)0.14 (2)0.051 (11)0.011 (11)−0.008 (9)0.047 (12)
C60.059 (13)0.054 (12)0.034 (10)0.039 (11)0.007 (9)0.017 (9)
O60.069 (11)0.080 (12)0.048 (10)0.027 (9)0.032 (9)0.025 (9)
O70.042 (7)0.032 (7)0.044 (8)0.014 (6)0.012 (6)0.005 (6)
N110.047 (10)0.041 (9)0.047 (10)0.008 (8)0.016 (8)0.012 (8)
C110.043 (11)0.061 (13)0.045 (12)0.027 (10)0.009 (9)0.015 (10)
C120.10 (2)0.050 (13)0.058 (15)0.045 (14)0.051 (15)0.025 (12)
C130.18 (4)0.09 (2)0.066 (18)0.10 (3)0.08 (2)0.053 (17)
C140.144 (16)0.030 (7)0.103 (14)0.003 (9)0.071 (12)−0.001 (8)
C150.144 (16)0.030 (7)0.103 (14)0.003 (9)0.071 (12)−0.001 (8)
C160.144 (16)0.030 (7)0.103 (14)0.003 (9)0.071 (12)−0.001 (8)
N210.041 (9)0.045 (9)0.031 (8)0.008 (7)0.013 (7)0.003 (7)
C230.08 (2)0.15 (3)0.041 (14)0.07 (2)0.011 (14)0.004 (18)
C240.059 (17)0.13 (3)0.065 (19)0.05 (2)0.036 (15)0.01 (2)
C250.041 (14)0.18 (4)0.034 (13)−0.006 (19)−0.008 (11)−0.025 (18)
C260.051 (13)0.045 (12)0.052 (13)−0.002 (10)0.006 (10)−0.008 (10)
N310.042 (10)0.058 (12)0.058 (12)0.016 (9)0.011 (9)0.018 (9)
C320.060 (14)0.062 (14)0.019 (9)0.000 (11)0.000 (9)0.007 (9)
C330.081 (18)0.067 (16)0.046 (14)0.032 (14)0.013 (12)−0.017 (12)
C340.12 (3)0.12 (3)0.037 (14)0.08 (3)0.024 (17)−0.007 (16)
C350.10 (3)0.08 (2)0.08 (2)0.035 (19)0.04 (2)0.016 (17)
C360.086 (18)0.062 (15)0.051 (14)0.051 (14)0.025 (13)0.014 (11)
N410.046 (9)0.049 (10)0.036 (9)0.029 (8)0.015 (7)0.010 (7)
C420.042 (11)0.054 (12)0.026 (9)0.000 (9)0.001 (8)0.002 (9)
C430.064 (17)0.08 (2)0.067 (18)0.011 (15)0.010 (14)0.017 (15)
C440.033 (11)0.10 (2)0.043 (12)0.029 (12)0.005 (9)0.012 (13)
C450.064 (15)0.069 (16)0.052 (14)0.036 (13)0.014 (11)0.030 (12)
C460.048 (12)0.050 (12)0.049 (13)0.022 (10)0.014 (10)0.008 (10)
Re30.0648 (7)0.0588 (7)0.0775 (9)0.0190 (5)0.0181 (6)0.0039 (6)
O310.095 (14)0.065 (11)0.068 (12)0.045 (11)0.037 (11)0.016 (9)
O320.109 (18)0.091 (16)0.048 (11)−0.020 (13)0.006 (11)−0.008 (10)
O330.17 (3)0.11 (2)0.11 (2)0.08 (2)−0.03 (2)−0.008 (17)
O340.27 (5)0.087 (19)0.15 (3)0.06 (2)0.13 (3)0.027 (19)

Geometric parameters (Å, °)

Re1—C31.88 (3)C23—C241.34 (5)
Re1—C21.93 (3)C23—H230.9500
Re1—C11.98 (3)C24—C251.34 (6)
Re1—O72.146 (14)C24—H240.9500
Re1—N412.165 (17)C25—C261.51 (4)
Re1—N312.22 (2)C25—H250.9500
C1—O11.13 (3)C26—H260.9500
C2—O21.15 (3)N31—C321.32 (3)
C3—O31.20 (3)N31—C361.33 (3)
Re2—C41.91 (2)C32—C331.43 (3)
Re2—C61.93 (2)C32—C421.46 (4)
Re2—C51.95 (3)C33—C341.36 (4)
Re2—N112.171 (18)C33—H330.9500
Re2—O72.185 (14)C34—C351.38 (5)
Re2—N212.190 (18)C34—H340.9500
C4—O41.15 (3)C35—C361.43 (4)
C5—O51.17 (3)C35—H350.9500
C6—O61.15 (3)C36—H360.9500
O7—H70.8199N41—C461.37 (3)
N11—C121.33 (4)N41—C421.41 (3)
N11—C161.39 (4)C42—C431.37 (4)
C11—C231.39 (4)C43—C441.41 (4)
C11—N211.44 (3)C43—H430.9500
C11—C121.47 (4)C44—C451.41 (4)
C12—C131.40 (3)C44—H440.9500
C13—C141.35 (5)C45—C461.33 (4)
C13—H130.9500C45—H450.9500
C14—C151.41 (4)C46—H460.9500
C14—H140.9500Re3—O341.56 (3)
C15—C161.40 (3)Re3—O321.71 (2)
C15—H150.9500Re3—O311.710 (18)
C16—H160.9500Re3—O331.73 (3)
N21—C261.32 (3)
C3—Re1—C289.7 (12)C15—C16—H16121.2
C3—Re1—C186.7 (9)C26—N21—C11122 (2)
C2—Re1—C188.0 (12)C26—N21—Re2123.2 (17)
C3—Re1—O792.6 (9)C11—N21—Re2114.8 (14)
C2—Re1—O7172.7 (10)C24—C23—C11120 (3)
C1—Re1—O799.1 (8)C24—C23—H23120.2
C3—Re1—N41174.9 (10)C11—C23—H23120.2
C2—Re1—N4194.8 (9)C23—C24—C25125 (3)
C1—Re1—N4195.9 (8)C23—C24—H24117.5
O7—Re1—N4182.7 (6)C25—C24—H24117.5
C3—Re1—N31102.1 (8)C24—C25—C26117 (3)
C2—Re1—N3193.7 (11)C24—C25—H25121.7
C1—Re1—N31171.1 (8)C26—C25—H25121.7
O7—Re1—N3179.1 (6)N21—C26—C25119 (3)
N41—Re1—N3175.2 (7)N21—C26—H26120.7
O1—C1—Re1179 (2)C25—C26—H26120.7
O2—C2—Re1174 (3)C32—N31—C36123 (2)
O3—C3—Re1176.5 (18)C32—N31—Re1114.8 (17)
C4—Re2—C684.8 (9)C36—N31—Re1122.3 (18)
C4—Re2—C586.5 (11)N31—C32—C33119 (3)
C6—Re2—C589.6 (9)N31—C32—C42119 (2)
C4—Re2—N11172.1 (9)C33—C32—C42122 (2)
C6—Re2—N1191.2 (8)C34—C33—C32120 (3)
C5—Re2—N11100.3 (9)C34—C33—H33120.0
C4—Re2—O799.7 (8)C32—C33—H33120.0
C6—Re2—O7175.5 (7)C33—C34—C35120 (3)
C5—Re2—O790.3 (7)C33—C34—H34120.2
N11—Re2—O784.4 (6)C35—C34—H34120.2
C4—Re2—N2198.5 (9)C34—C35—C36119 (3)
C6—Re2—N2197.7 (7)C34—C35—H35120.6
C5—Re2—N21171.5 (8)C36—C35—H35120.6
N11—Re2—N2175.3 (7)N31—C36—C35120 (3)
O7—Re2—N2182.2 (6)N31—C36—H36120.2
O4—C4—Re2175 (2)C35—C36—H36120.2
O5—C5—Re2176 (2)C46—N41—C42117.9 (19)
O6—C6—Re2178 (2)C46—N41—Re1125.9 (15)
Re1—O7—Re2132.8 (6)C42—N41—Re1115.6 (14)
Re1—O7—H7113.6C43—C42—N41120 (2)
Re2—O7—H7113.6C43—C42—C32126 (2)
C12—N11—C16119 (2)N41—C42—C32113.5 (18)
C12—N11—Re2118.4 (16)C42—C43—C44122 (3)
C16—N11—Re2122.6 (18)C42—C43—H43119.2
C23—C11—N21119 (3)C44—C43—H43119.2
C23—C11—C12128 (3)C45—C44—C43115 (2)
N21—C11—C12113.7 (19)C45—C44—H44122.4
N11—C12—C13123 (3)C43—C44—H44122.4
N11—C12—C11117 (2)C46—C45—C44123 (2)
C13—C12—C11120 (3)C46—C45—H45118.7
C14—C13—C12121 (4)C44—C45—H45118.7
C14—C13—H13119.4C45—C46—N41122 (2)
C12—C13—H13119.4C45—C46—H46118.8
C13—C14—C15115 (3)N41—C46—H46118.8
C13—C14—H14122.3O34—Re3—O32102.9 (18)
C15—C14—H14122.3O34—Re3—O31104.5 (15)
C14—C15—C16124 (3)O32—Re3—O31105.8 (13)
C14—C15—H15118.1O34—Re3—O33130 (2)
C16—C15—H15118.1O32—Re3—O33105.1 (15)
N11—C16—C15118 (3)O31—Re3—O33106.2 (12)
N11—C16—H16121.2
C3—Re1—C1—O1−168 (100)C12—C11—N21—C26176 (2)
C2—Re1—C1—O1102 (100)C23—C11—N21—Re2169.9 (19)
O7—Re1—C1—O1−76 (100)C12—C11—N21—Re2−11 (2)
N41—Re1—C1—O17(100)C4—Re2—N21—C26−4.7 (19)
N31—Re1—C1—O11(100)C6—Re2—N21—C26−90.6 (18)
C3—Re1—C2—O2−19 (27)C5—Re2—N21—C26121 (5)
C1—Re1—C2—O268 (27)N11—Re2—N21—C26−179.8 (18)
O7—Re1—C2—O2−127 (25)O7—Re2—N21—C2694.0 (18)
N41—Re1—C2—O2164 (27)C4—Re2—N21—C11−178.0 (15)
N31—Re1—C2—O2−121 (27)C6—Re2—N21—C1196.1 (15)
C2—Re1—C3—O3102 (42)C5—Re2—N21—C11−53 (6)
C1—Re1—C3—O314 (42)N11—Re2—N21—C116.9 (13)
O7—Re1—C3—O3−85 (42)O7—Re2—N21—C11−79.3 (14)
N41—Re1—C3—O3−106 (40)N21—C11—C23—C243(4)
N31—Re1—C3—O3−164 (41)C12—C11—C23—C24−176 (3)
C6—Re2—C4—O435 (28)C11—C23—C24—C25−1(5)
C5—Re2—C4—O4125 (29)C23—C24—C25—C26−1(5)
N11—Re2—C4—O4−25 (33)C11—N21—C26—C251(3)
O7—Re2—C4—O4−145 (28)Re2—N21—C26—C25−171.7 (18)
N21—Re2—C4—O4−62 (29)C24—C25—C26—N211(4)
C4—Re2—C5—O5131 (33)C3—Re1—N31—C32170.4 (17)
C6—Re2—C5—O5−144 (33)C2—Re1—N31—C32−99.1 (18)
N11—Re2—C5—O5−53 (33)C1—Re1—N31—C321(6)
O7—Re2—C5—O532 (33)O7—Re1—N31—C3280.1 (16)
N21—Re2—C5—O55(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—C3679 (2)
N11—Re2—C6—O688 (55)C1—Re1—N31—C36179 (5)
O7—Re2—C6—O6101 (57)O7—Re1—N31—C36−102 (2)
N21—Re2—C6—O613 (56)N41—Re1—N31—C36173 (2)
C3—Re1—O7—Re2108.3 (10)C36—N31—C32—C338(4)
C2—Re1—O7—Re2−143 (7)Re1—N31—C32—C33−174.1 (19)
C1—Re1—O7—Re221.2 (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—Re113.1 (12)C42—C32—C33—C34−178 (3)
C6—Re2—O7—Re1−173 (9)C32—C33—C34—C35−1(5)
C5—Re2—O7—Re199.5 (11)C33—C34—C35—C366(5)
N11—Re2—O7—Re1−160.1 (10)C32—N31—C36—C35−3(4)
N21—Re2—O7—Re1−84.3 (10)Re1—N31—C36—C35179 (2)
C4—Re2—N11—C12−40 (7)C34—C35—C36—N31−4(5)
C6—Re2—N11—C12−99.6 (17)C3—Re1—N41—C46123 (8)
C5—Re2—N11—C12170.6 (17)C2—Re1—N41—C46−86 (2)
O7—Re2—N11—C1281.4 (16)C1—Re1—N41—C462.2 (19)
N21—Re2—N11—C12−2.0 (16)O7—Re1—N41—C46100.6 (18)
C4—Re2—N11—C16136 (6)N31—Re1—N41—C46−178.8 (19)
C6—Re2—N11—C1676 (2)C3—Re1—N41—C42−48 (9)
C5—Re2—N11—C16−14 (2)C2—Re1—N41—C42103.1 (17)
O7—Re2—N11—C16−102.9 (19)C1—Re1—N41—C42−168.5 (15)
N21—Re2—N11—C16174 (2)O7—Re1—N41—C42−70.1 (14)
C16—N11—C12—C134(3)N31—Re1—N41—C4210.6 (14)
Re2—N11—C12—C13−179.8 (18)C46—N41—C42—C433(3)
C16—N11—C12—C11−179 (2)Re1—N41—C42—C43174.5 (19)
Re2—N11—C12—C11−3(3)C46—N41—C42—C32174.2 (19)
C23—C11—C12—N11−171 (3)Re1—N41—C42—C32−14 (2)
N21—C11—C12—N119(3)N31—C32—C42—C43−179 (2)
C23—C11—C12—C135(4)C33—C32—C42—C43−7(4)
N21—C11—C12—C13−174 (2)N31—C32—C42—N4110 (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—C167(5)C42—C43—C44—C459(4)
C12—N11—C16—C150(4)C43—C44—C45—C46−6(4)
Re2—N11—C16—C15−176 (2)C44—C45—C46—N412(4)
C14—C15—C16—N11−6(5)C42—N41—C46—C450(3)
C23—C11—N21—C26−4(3)Re1—N41—C46—C45−170.4 (18)

Footnotes

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

References

  • Blessing, R. H. (1995). Acta Cryst. A51, 33–38. [PubMed]
  • Gibson, D. H., Mashuta, M. S. & Yin, X. (2003). Acta Cryst. E59, m911–m913.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2003). J. Appl. Cryst.36, 7–13.
  • Stoe & Cie (2001). X-AREA Stoe & Cie, Darmstadt, Germany.

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