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In the title compound, [Re2(C10H8N2)(CO)8], both Re atoms have distorted octahedral coordination geometry. The carbonyls of the Re(CO)5 moiety are fully staggered relative to those of the Re(CO)3 unit. We are currently interested in the application of Re-di­imine complexes as catalysts for the photo- and electro-chemical reduction of CO2. The (2,2'-bi­pyridine)Re(CO)3. radical, a key intermediate in the [Cl(2,2'-bi­pyridine)Re(CO)3] catalytic CO2 reduction cycle, is formed by Cl- loss from [Cl(2,2'-bi­pyridine)Re(CO)3]-.. We synthesized the title compound as a precursor to the (2,2'-bi­pyridine)Re(CO)3. radical and so that we can ex­amine the structural features of the (2,2'-bi­pyridine)Re(CO)3 moiety following irradiation of the title compound.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801011278/cf6096sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801011278/cf6096Isup2.hkl
Contains datablock I

CCDC reference: 170879

Key indicators

  • Single-crystal X-ray study
  • T = 220 K
  • Mean [sigma](C-C) = 0.019 Å
  • R factor = 0.046
  • wR factor = 0.136
  • Data-to-parameter ratio = 12.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.049 0.310 Tmin and Tmax expected: 0.039 0.310 RR = 1.270 Please check that your absorption correction is appropriate.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

no comment

Experimental top

The title compound was prepared by refluxing [Re2(CO)10] with excess bipyridyl in xylene for 3 days. The xylene was removed and the residual starting material extracted by dissolution in diethyl ether and precipitating the product with pentane. Crystals were obtained by slow concentration of an acetone solution in the dark.

Refinement top

The crystal was transferred into the nitrogen stream of an Oxford Cryosystems open-flow cryostat (Cosier & Glazer, 1986) operating at 150 (2) K. The crystal used was unsuitable for absorption correction using ψ scans (µ × tmid 3.0) and it was not possible to index and measure crystal faces with sufficient accuracy for a numerical correction. Furthermore, because of the low symmetry we could not employ HABITUS (Herrendorf, 1995) to optimize the crystal shape and dimensions. We reluctantly, therefore, had to use DIFABS (Walker & Stuart, 1983) to apply empirical corrections. The final residual electron density extrema lie near Re2. H atoms were placed geometrically and refined riding at a distance of 0.95 Å from their parent C atoms with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: STADI4 (Stoe & Cie, 1997); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2001); software used to prepare material for publication: SHELXL97 and PLATON.

Figures top
[Figure 1] Fig. 1. A general view of one of the two independent molecules of the title compound showing the atom numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.
(I) top
Crystal data top
C18H8N2O8Re2Z = 4
Mr = 752.66F(000) = 1376
Triclinic, P1Dx = 2.566 Mg m3
a = 10.155 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.586 (5) ÅCell parameters from 43 reflections
c = 14.972 (8) Åθ = 12.5–14.5°
α = 80.55 (5)°µ = 12.47 mm1
β = 73.07 (4)°T = 220 K
γ = 85.40 (5)°Plate, red
V = 1948.1 (16) Å30.65 × 0.24 × 0.09 mm
Data collection top
Stoe Stadi-4 four-circle
diffractometer
5903 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.0
Graphite monochromatorθmax = 25.0°, θmin = 2.6°
ω/θ scansh = 1112
Absorption correction: part of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
k = 1516
Tmin = 0.049, Tmax = 0.310l = 017
6852 measured reflections3 standard reflections every 60 min
6852 independent reflections intensity decay: random variation +3.2%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.082P)2 + 20.6P]
where P = (Fo2 + 2Fc2)/3
6852 reflections(Δ/σ)max = 0.03
542 parametersΔρmax = 2.74 e Å3
0 restraintsΔρmin = 2.72 e Å3
Crystal data top
C18H8N2O8Re2γ = 85.40 (5)°
Mr = 752.66V = 1948.1 (16) Å3
Triclinic, P1Z = 4
a = 10.155 (5) ÅMo Kα radiation
b = 13.586 (5) ŵ = 12.47 mm1
c = 14.972 (8) ÅT = 220 K
α = 80.55 (5)°0.65 × 0.24 × 0.09 mm
β = 73.07 (4)°
Data collection top
Stoe Stadi-4 four-circle
diffractometer
5903 reflections with I > 2σ(I)
Absorption correction: part of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
Rint = 0.0
Tmin = 0.049, Tmax = 0.3103 standard reflections every 60 min
6852 measured reflections intensity decay: random variation +3.2%
6852 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.136H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.082P)2 + 20.6P]
where P = (Fo2 + 2Fc2)/3
6852 reflectionsΔρmax = 2.74 e Å3
542 parametersΔρmin = 2.72 e Å3
Special details top

Experimental. The crystal used for data collection was unsuitable for absorption correction using ψ scans (µ*tmid 3.0) and it was not possible to index and measure crystal faces with sufficient accuracy for a numerical correction. Furthermore, the low crystal symmetry meant that it was not possible to optimize the crystal dimensions and shape using HABITUS. Relectantly therefore we resorted to the use of DIFABS to apply empirical corrections. The final residual electron density extrema lie near the Re atoms.

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) top
xyzUiso*/Ueq
Re10.84644 (5)0.72901 (4)0.96382 (3)0.02809 (16)
Re20.53124 (5)0.71670 (4)1.04708 (3)0.02721 (16)
N10.8327 (9)0.8829 (8)0.9839 (7)0.027 (2)
C20.8416 (11)0.9037 (9)1.0678 (9)0.025 (2)
C30.8340 (13)1.0011 (10)1.0871 (10)0.033 (3)
H30.84121.01371.14600.040*
C40.8156 (13)1.0803 (10)1.0184 (10)0.037 (3)
H40.80861.14731.03040.044*
C50.8080 (14)1.0593 (11)0.9340 (11)0.039 (3)
H50.79601.11180.88630.047*
C60.8178 (13)0.9611 (10)0.9184 (10)0.036 (3)
H60.81380.94780.85890.043*
N1'0.8713 (10)0.7265 (8)1.1042 (8)0.031 (2)
C2'0.8656 (11)0.8163 (10)1.1358 (9)0.026 (3)
C3'0.8803 (13)0.8219 (11)1.2224 (10)0.036 (3)
H3'0.87840.88521.24200.043*
C4'0.8979 (13)0.7357 (11)1.2818 (10)0.039 (3)
H4'0.90270.73821.34380.047*
C5'0.9084 (13)0.6463 (11)1.2482 (10)0.040 (3)
H5'0.92540.58601.28590.048*
C6'0.8942 (12)0.6444 (11)1.1599 (9)0.032 (3)
H6'0.90100.58191.13790.039*
C110.8510 (14)0.5874 (11)0.9642 (11)0.040 (3)
O110.8537 (12)0.5035 (8)0.9648 (10)0.062 (3)
C121.0396 (14)0.7294 (11)0.9022 (11)0.040 (3)
O121.1545 (10)0.7256 (10)0.8604 (8)0.058 (3)
C130.8117 (13)0.7510 (10)0.8432 (8)0.034 (3)
O130.7885 (11)0.7705 (10)0.7713 (8)0.057 (3)
C210.5504 (16)0.6269 (13)0.9519 (11)0.046 (4)
O210.5626 (13)0.5751 (9)0.8970 (8)0.059 (3)
C220.5279 (14)0.8338 (12)0.9513 (11)0.041 (3)
O220.5298 (11)0.9025 (10)0.8966 (8)0.057 (3)
C230.5370 (13)0.8117 (11)1.1342 (10)0.036 (3)
O230.5442 (11)0.8660 (8)1.1815 (8)0.050 (3)
C240.3340 (14)0.6995 (11)1.0942 (10)0.035 (3)
O240.2186 (10)0.6913 (9)1.1181 (8)0.051 (3)
C250.5882 (14)0.6058 (10)1.1340 (9)0.034 (3)
O250.6218 (11)0.5440 (8)1.1841 (8)0.049 (3)
Re30.24594 (5)0.65085 (4)0.41160 (3)0.02698 (16)
Re40.19284 (5)0.79814 (4)0.55540 (3)0.02662 (16)
N1*0.3415 (10)0.8972 (8)0.4548 (7)0.027 (2)
C2*0.4734 (12)0.8846 (9)0.4545 (8)0.026 (3)
C3*0.5790 (14)0.9424 (10)0.3939 (10)0.038 (3)
H3*0.67190.92980.39530.046*
C4*0.5425 (15)1.0203 (11)0.3307 (10)0.042 (3)
H4*0.61081.06230.28780.050*
C5*0.4070 (17)1.0352 (11)0.3314 (10)0.045 (4)
H5*0.38091.08750.28870.054*
C6*0.3084 (14)0.9737 (10)0.3944 (9)0.035 (3)
H6*0.21460.98570.39510.042*
N1*'0.3884 (10)0.7521 (8)0.5832 (8)0.031 (2)
C2*'0.5009 (12)0.8041 (10)0.5261 (9)0.029 (3)
C3*'0.6301 (13)0.7795 (13)0.5408 (10)0.042 (4)
H3*B0.70960.81180.49960.051*
C4*'0.6417 (14)0.7090 (11)0.6143 (10)0.039 (3)
H4*B0.72910.69330.62520.046*
C5*'0.5284 (15)0.6611 (14)0.6722 (11)0.053 (4)
H5*B0.53560.61210.72380.064*
C6*'0.4051 (14)0.6847 (12)0.6547 (10)0.041 (3)
H6*B0.32630.65140.69560.049*
C310.2893 (14)0.5514 (11)0.5137 (10)0.038 (3)
O310.3186 (13)0.4977 (10)0.5707 (10)0.069 (4)
C320.0478 (13)0.6280 (10)0.4698 (10)0.034 (3)
O320.0672 (10)0.6144 (8)0.5018 (8)0.048 (3)
C330.4430 (13)0.6847 (9)0.3690 (10)0.031 (3)
O330.5563 (10)0.7035 (8)0.3468 (7)0.042 (2)
C340.2555 (14)0.5606 (11)0.3224 (10)0.039 (3)
O340.2543 (12)0.5077 (8)0.2698 (7)0.049 (3)
C350.2082 (13)0.7750 (10)0.3314 (9)0.034 (3)
O350.1877 (11)0.8473 (8)0.2866 (8)0.047 (2)
C410.0901 (13)0.6923 (11)0.6436 (9)0.034 (3)
O410.0339 (11)0.6278 (9)0.6957 (8)0.053 (3)
C420.1400 (13)0.8848 (11)0.6500 (10)0.036 (3)
O420.1009 (12)0.9358 (10)0.7055 (8)0.058 (3)
C430.0336 (14)0.8477 (10)0.5133 (10)0.035 (3)
O430.0613 (10)0.8751 (9)0.4896 (9)0.054 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.0261 (3)0.0283 (3)0.0312 (3)0.00319 (19)0.0084 (2)0.0095 (2)
Re20.0265 (3)0.0255 (3)0.0299 (3)0.00139 (19)0.0077 (2)0.0049 (2)
N10.019 (5)0.026 (6)0.029 (5)0.001 (4)0.000 (4)0.000 (4)
C20.019 (5)0.021 (6)0.036 (7)0.002 (4)0.010 (5)0.004 (5)
C30.034 (7)0.029 (7)0.039 (7)0.003 (5)0.012 (6)0.007 (6)
C40.033 (7)0.027 (7)0.049 (8)0.010 (5)0.008 (6)0.013 (6)
C50.034 (7)0.036 (8)0.047 (8)0.002 (6)0.014 (6)0.002 (6)
C60.034 (7)0.036 (8)0.033 (7)0.005 (6)0.005 (5)0.002 (6)
N1'0.025 (5)0.026 (6)0.046 (6)0.001 (4)0.017 (5)0.005 (5)
C2'0.013 (5)0.033 (7)0.034 (7)0.000 (5)0.007 (5)0.007 (5)
C3'0.035 (7)0.043 (8)0.038 (7)0.003 (6)0.019 (6)0.016 (6)
C4'0.031 (7)0.048 (9)0.041 (8)0.004 (6)0.018 (6)0.001 (7)
C5'0.028 (6)0.042 (8)0.045 (8)0.000 (6)0.015 (6)0.010 (6)
C6'0.023 (6)0.040 (8)0.034 (7)0.003 (5)0.006 (5)0.008 (6)
C110.041 (7)0.032 (8)0.051 (9)0.011 (6)0.016 (6)0.014 (7)
O110.067 (7)0.032 (7)0.095 (10)0.014 (5)0.029 (7)0.025 (6)
C120.035 (7)0.039 (8)0.051 (8)0.011 (6)0.013 (6)0.027 (7)
O120.026 (5)0.085 (9)0.061 (7)0.003 (5)0.001 (5)0.025 (7)
C130.040 (7)0.037 (8)0.016 (6)0.005 (6)0.001 (5)0.001 (5)
O130.054 (6)0.082 (9)0.037 (6)0.021 (6)0.021 (5)0.017 (6)
C210.050 (8)0.052 (10)0.042 (8)0.015 (7)0.024 (7)0.007 (7)
O210.081 (8)0.051 (7)0.051 (7)0.006 (6)0.016 (6)0.031 (6)
C220.032 (7)0.040 (9)0.043 (8)0.004 (6)0.005 (6)0.003 (7)
O220.051 (6)0.065 (8)0.044 (6)0.006 (6)0.003 (5)0.002 (6)
C230.029 (6)0.040 (8)0.036 (7)0.008 (6)0.008 (5)0.002 (6)
O230.064 (7)0.044 (6)0.051 (6)0.008 (5)0.020 (5)0.022 (5)
C240.034 (7)0.036 (8)0.037 (7)0.001 (6)0.015 (6)0.000 (6)
O240.033 (6)0.054 (7)0.062 (7)0.000 (5)0.010 (5)0.008 (6)
C250.040 (7)0.030 (7)0.032 (7)0.015 (6)0.006 (6)0.005 (6)
O250.052 (6)0.040 (6)0.059 (7)0.011 (5)0.030 (5)0.014 (5)
Re30.0268 (3)0.0234 (3)0.0300 (3)0.00046 (19)0.0071 (2)0.0041 (2)
Re40.0212 (2)0.0273 (3)0.0311 (3)0.00023 (19)0.00580 (19)0.0071 (2)
N1*0.026 (5)0.031 (6)0.027 (5)0.000 (4)0.011 (4)0.009 (4)
C2*0.027 (6)0.020 (6)0.029 (6)0.005 (5)0.001 (5)0.006 (5)
C3*0.038 (7)0.030 (7)0.046 (8)0.006 (6)0.004 (6)0.015 (6)
C4*0.049 (8)0.035 (8)0.036 (8)0.015 (6)0.000 (6)0.008 (6)
C5*0.063 (10)0.034 (8)0.036 (8)0.009 (7)0.010 (7)0.002 (6)
C6*0.044 (7)0.030 (7)0.034 (7)0.006 (6)0.011 (6)0.014 (6)
N1*'0.029 (5)0.032 (6)0.035 (6)0.003 (4)0.012 (4)0.006 (5)
C2*'0.020 (5)0.037 (7)0.031 (6)0.002 (5)0.006 (5)0.015 (6)
C3*'0.024 (6)0.067 (11)0.044 (8)0.002 (6)0.014 (6)0.025 (8)
C4*'0.037 (7)0.046 (9)0.037 (7)0.016 (6)0.017 (6)0.016 (7)
C5*'0.041 (8)0.076 (12)0.040 (8)0.014 (8)0.013 (7)0.004 (8)
C6*'0.030 (7)0.059 (10)0.034 (7)0.002 (6)0.009 (6)0.012 (7)
C310.038 (7)0.029 (7)0.041 (8)0.001 (6)0.010 (6)0.011 (6)
O310.071 (8)0.061 (8)0.071 (8)0.005 (6)0.031 (7)0.019 (7)
C320.032 (7)0.027 (7)0.046 (8)0.009 (5)0.016 (6)0.009 (6)
O320.039 (6)0.038 (6)0.066 (7)0.006 (4)0.009 (5)0.008 (5)
C330.040 (8)0.010 (6)0.045 (8)0.008 (5)0.017 (6)0.007 (5)
O330.031 (5)0.040 (6)0.055 (6)0.003 (4)0.010 (4)0.003 (5)
C340.032 (7)0.042 (9)0.040 (8)0.001 (6)0.008 (6)0.001 (7)
O340.062 (7)0.047 (7)0.040 (6)0.002 (5)0.013 (5)0.012 (5)
C350.038 (7)0.031 (8)0.033 (7)0.017 (6)0.010 (6)0.001 (6)
O350.062 (7)0.032 (6)0.051 (6)0.001 (5)0.025 (5)0.001 (5)
C410.029 (6)0.039 (8)0.031 (7)0.007 (6)0.003 (5)0.006 (6)
O410.049 (6)0.051 (7)0.044 (6)0.016 (5)0.009 (5)0.003 (5)
C420.030 (6)0.034 (8)0.045 (8)0.008 (6)0.011 (6)0.006 (6)
O420.059 (7)0.068 (8)0.050 (7)0.000 (6)0.007 (5)0.038 (6)
C430.035 (7)0.024 (7)0.047 (8)0.002 (5)0.012 (6)0.003 (6)
O430.034 (5)0.052 (7)0.082 (8)0.009 (5)0.027 (6)0.012 (6)
Geometric parameters (Å, º) top
Re1—Re23.0856 (18)Re4—C411.927 (14)
Re1—N12.149 (10)Re4—C421.918 (14)
Re1—N1'2.184 (11)Re4—C431.935 (14)
Re1—C111.920 (15)N1*—C2*1.336 (15)
Re1—C121.909 (14)N1*—C6*1.351 (17)
Re1—C131.910 (13)C2*—C3*1.387 (18)
Re2—C211.982 (17)C2*—C2*'1.470 (19)
Re2—C221.964 (16)C3*—C4*1.40 (2)
Re2—C231.995 (14)C4*—C5*1.37 (2)
Re2—C241.940 (13)C5*—C6*1.38 (2)
Re2—C251.988 (15)N1*'—C2*'1.378 (16)
N1—C21.360 (16)N1*'—C6*'1.330 (19)
N1—C61.353 (17)C2*'—C3*'1.398 (17)
C2—C31.391 (17)C3*'—C4*'1.36 (2)
C2—C2'1.486 (17)C4*'—C5*'1.36 (2)
C3—C41.40 (2)C5*'—C6*'1.36 (2)
C4—C51.37 (2)C31—O311.121 (17)
C5—C61.38 (2)C32—O321.144 (16)
N1'—C2'1.371 (16)C33—O331.139 (16)
N1'—C6'1.326 (17)C34—O341.153 (18)
C2'—C3'1.363 (17)C35—O351.136 (17)
C3'—C4'1.38 (2)C41—O411.140 (17)
C4'—C5'1.37 (2)C42—O421.133 (17)
C5'—C6'1.377 (19)C43—O431.136 (16)
C11—O111.136 (17)C3—H30.95
C12—O121.154 (17)C4—H40.95
C13—O131.154 (16)C5—H50.95
C21—O211.142 (19)C6—H60.95
C22—O221.134 (18)C3'—H3'0.95
C23—O231.123 (17)C4'—H4'0.95
C24—O241.130 (16)C5'—H5'0.95
C25—O251.131 (17)C6'—H6'0.95
Re3—Re43.0816 (18)C3*—H3*0.95
Re3—C311.994 (14)C4*—H4*0.95
Re3—C321.973 (14)C5*—H5*0.95
Re3—C331.982 (13)C6*—H6*0.95
Re3—C341.934 (16)C3*'—H3*B0.95
Re3—C351.984 (15)C4*'—H4*B0.95
Re4—N1*2.166 (11)C5*'—H5*B0.95
Re4—N1*'2.170 (10)C6*'—H6*B0.95
C13—Re1—C1289.4 (6)C42—Re4—C4389.2 (6)
C13—Re1—C1190.0 (6)C41—Re4—C4391.8 (6)
C12—Re1—C1189.1 (6)C42—Re4—N1*'94.3 (5)
C13—Re1—N196.9 (5)C41—Re4—N1*'95.4 (5)
C12—Re1—N194.5 (5)C43—Re4—N1*'172.0 (5)
C11—Re1—N1172.2 (5)C42—Re4—N1*95.4 (5)
C13—Re1—N1'171.3 (5)C41—Re4—N1*169.1 (5)
C12—Re1—N1'94.3 (5)C43—Re4—N1*97.6 (5)
C11—Re1—N1'98.0 (5)N1*'—Re4—N1*74.9 (4)
N1—Re1—N1'74.9 (4)C42—Re4—Re3173.8 (4)
C13—Re1—Re285.9 (4)C41—Re4—Re385.1 (4)
C12—Re1—Re2174.0 (4)C43—Re4—Re387.0 (4)
C11—Re1—Re287.2 (4)N1*'—Re4—Re390.1 (3)
N1—Re1—Re289.8 (2)N1*—Re4—Re389.9 (3)
N1'—Re1—Re290.9 (3)C2*—N1*—C6*117.6 (11)
C24—Re2—C2297.6 (6)C2*—N1*—Re4118.4 (8)
C24—Re2—C2192.0 (6)C6*—N1*—Re4124.0 (8)
C22—Re2—C2190.4 (6)N1*—C2*—C3*124.4 (13)
C24—Re2—C2597.8 (6)N1*—C2*—C2*'114.8 (10)
C22—Re2—C25164.5 (5)C3*—C2*—C2*'120.8 (12)
C21—Re2—C2590.9 (6)C2*—C3*—C4*116.9 (13)
C24—Re2—C2395.3 (5)C5*—C4*—C3*119.3 (13)
C22—Re2—C2387.3 (6)C4*—C5*—C6*119.8 (15)
C21—Re2—C23172.6 (6)N1*—C6*—C5*121.9 (13)
C25—Re2—C2389.5 (5)C6*'—N1*'—C2*'118.6 (11)
C24—Re2—Re1175.3 (4)C6*'—N1*'—Re4125.3 (9)
C22—Re2—Re183.7 (4)C2*'—N1*'—Re4115.9 (8)
C21—Re2—Re183.5 (4)N1*'—C2*'—C3*'119.0 (13)
C25—Re2—Re181.1 (4)N1*'—C2*'—C2*116.1 (10)
C23—Re2—Re189.3 (4)C3*'—C2*'—C2*124.9 (12)
C6—N1—C2117.5 (11)C4*'—C3*'—C2*'119.8 (14)
C6—N1—Re1124.6 (9)C3*'—C4*'—C5*'120.1 (13)
C2—N1—Re1117.9 (8)C6*'—C5*'—C4*'118.7 (15)
N1—C2—C3122.0 (12)N1*'—C6*'—C5*'123.6 (14)
N1—C2—C2'115.8 (10)O31—C31—Re3177.0 (13)
C3—C2—C2'122.1 (11)O32—C32—Re3178.6 (12)
C2—C3—C4119.1 (12)O33—C33—Re3178.3 (12)
C5—C4—C3118.8 (13)O34—C34—Re3176.6 (12)
C4—C5—C6119.5 (14)O35—C35—Re3178.5 (11)
N1—C6—C5123.1 (13)O41—C41—Re4177.4 (13)
C6'—N1'—C2'118.1 (11)O42—C42—Re4175.9 (12)
C6'—N1'—Re1124.5 (9)O43—C43—Re4178.6 (13)
C2'—N1'—Re1117.4 (8)C2—C3—H3120.4
N1'—C2'—C3'121.5 (12)C4—C3—H3120.5
N1'—C2'—C2113.9 (10)C5—C4—H4120.6
C3'—C2'—C2124.7 (12)C3—C4—H4120.6
C2'—C3'—C4'120.2 (13)C4—C5—H5120.3
C5'—C4'—C3'117.8 (13)C6—C5—H5120.3
C4'—C5'—C6'119.9 (13)N1—C6—H6118.4
N1'—C6'—C5'122.4 (13)C5—C6—H6118.4
O11—C11—Re1179.7 (14)C2'—C3'—H3'119.9
O12—C12—Re1175.1 (12)C4'—C3'—H3'119.9
O13—C13—Re1175.6 (13)C5'—C4'—H4'121.1
O21—C21—Re2179.5 (14)C3'—C4'—H4'121.1
O22—C22—Re2177.7 (13)C4'—C5'—H5'120.1
O23—C23—Re2177.9 (12)C6'—C5'—H5'120.1
O24—C24—Re2177.2 (13)N1'—C6'—H6'118.8
O25—C25—Re2178.7 (11)C5'—C6'—H6'118.8
C34—Re3—C3291.2 (6)C2*—C3*—H3*121.5
C34—Re3—C3397.2 (5)C4*—C3*—H3*121.5
C32—Re3—C33171.5 (5)C5*—C4*—H4*120.4
C34—Re3—C3197.9 (6)C3*—C4*—H4*120.4
C32—Re3—C3189.8 (6)C4*—C5*—H5*120.1
C33—Re3—C3187.8 (5)C6*—C5*—H5*120.1
C34—Re3—C3597.0 (6)N1*—C6*—H6*119.0
C32—Re3—C3592.2 (5)C5*—C6*—H6*119.0
C33—Re3—C3588.0 (5)C4*'—C3*'—H3*B120.1
C31—Re3—C35164.9 (6)C2*'—C3*'—H3*B120.1
C34—Re3—Re4173.0 (4)C3*'—C4*'—H4*B119.9
C32—Re3—Re482.4 (4)C5*'—C4*'—H4*B119.9
C33—Re3—Re489.3 (3)C6*'—C5*'—H5*B120.7
C31—Re3—Re485.0 (4)C4*'—C5*'—H5*B120.7
C35—Re3—Re480.5 (4)N1*'—C6*'—H6*B118.2
C42—Re4—C4190.2 (6)C5*'—C6*'—H6*B118.2

Experimental details

Crystal data
Chemical formulaC18H8N2O8Re2
Mr752.66
Crystal system, space groupTriclinic, P1
Temperature (K)220
a, b, c (Å)10.155 (5), 13.586 (5), 14.972 (8)
α, β, γ (°)80.55 (5), 73.07 (4), 85.40 (5)
V3)1948.1 (16)
Z4
Radiation typeMo Kα
µ (mm1)12.47
Crystal size (mm)0.65 × 0.24 × 0.09
Data collection
DiffractometerStoe Stadi-4 four-circle
diffractometer
Absorption correctionPart of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
Tmin, Tmax0.049, 0.310
No. of measured, independent and
observed [I > 2σ(I)] reflections
6852, 6852, 5903
Rint0.0
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.136, 1.11
No. of reflections6852
No. of parameters542
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.082P)2 + 20.6P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.74, 2.72

Computer programs: STADI4 (Stoe & Cie, 1997), STADI4, X-RED (Stoe & Cie, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2001), SHELXL97 and PLATON.

 

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