Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801011278/cf6096sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801011278/cf6096Isup2.hkl |
CCDC reference: 170879
Key indicators
- Single-crystal X-ray study
- T = 220 K
- Mean (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
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
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.
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).
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.
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. |
C18H8N2O8Re2 | Z = 4 |
Mr = 752.66 | F(000) = 1376 |
Triclinic, P1 | Dx = 2.566 Mg m−3 |
a = 10.155 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.586 (5) Å | Cell parameters from 43 reflections |
c = 14.972 (8) Å | θ = 12.5–14.5° |
α = 80.55 (5)° | µ = 12.47 mm−1 |
β = 73.07 (4)° | T = 220 K |
γ = 85.40 (5)° | Plate, red |
V = 1948.1 (16) Å3 | 0.65 × 0.24 × 0.09 mm |
Stoe Stadi-4 four-circle diffractometer | 5903 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.0 |
Graphite monochromator | θmax = 25.0°, θmin = 2.6° |
ω/θ scans | h = −11→12 |
Absorption correction: part of the refinement model (ΔF) (DIFABS; Walker & Stuart, 1983) | k = −15→16 |
Tmin = 0.049, Tmax = 0.310 | l = 0→17 |
6852 measured reflections | 3 standard reflections every 60 min |
6852 independent reflections | intensity decay: random variation +−3.2% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H-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 parameters | Δρmax = 2.74 e Å−3 |
0 restraints | Δρmin = −2.72 e Å−3 |
C18H8N2O8Re2 | γ = 85.40 (5)° |
Mr = 752.66 | V = 1948.1 (16) Å3 |
Triclinic, P1 | Z = 4 |
a = 10.155 (5) Å | Mo Kα radiation |
b = 13.586 (5) Å | µ = 12.47 mm−1 |
c = 14.972 (8) Å | T = 220 K |
α = 80.55 (5)° | 0.65 × 0.24 × 0.09 mm |
β = 73.07 (4)° |
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 = 0.310 | 3 standard reflections every 60 min |
6852 measured reflections | intensity decay: random variation +−3.2% |
6852 independent reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.082P)2 + 20.6P] where P = (Fo2 + 2Fc2)/3 |
6852 reflections | Δρmax = 2.74 e Å−3 |
542 parameters | Δρmin = −2.72 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | 0.84644 (5) | 0.72901 (4) | 0.96382 (3) | 0.02809 (16) | |
Re2 | 0.53124 (5) | 0.71670 (4) | 1.04708 (3) | 0.02721 (16) | |
N1 | 0.8327 (9) | 0.8829 (8) | 0.9839 (7) | 0.027 (2) | |
C2 | 0.8416 (11) | 0.9037 (9) | 1.0678 (9) | 0.025 (2) | |
C3 | 0.8340 (13) | 1.0011 (10) | 1.0871 (10) | 0.033 (3) | |
H3 | 0.8412 | 1.0137 | 1.1460 | 0.040* | |
C4 | 0.8156 (13) | 1.0803 (10) | 1.0184 (10) | 0.037 (3) | |
H4 | 0.8086 | 1.1473 | 1.0304 | 0.044* | |
C5 | 0.8080 (14) | 1.0593 (11) | 0.9340 (11) | 0.039 (3) | |
H5 | 0.7960 | 1.1118 | 0.8863 | 0.047* | |
C6 | 0.8178 (13) | 0.9611 (10) | 0.9184 (10) | 0.036 (3) | |
H6 | 0.8138 | 0.9478 | 0.8589 | 0.043* | |
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' | 0.8784 | 0.8852 | 1.2420 | 0.043* | |
C4' | 0.8979 (13) | 0.7357 (11) | 1.2818 (10) | 0.039 (3) | |
H4' | 0.9027 | 0.7382 | 1.3438 | 0.047* | |
C5' | 0.9084 (13) | 0.6463 (11) | 1.2482 (10) | 0.040 (3) | |
H5' | 0.9254 | 0.5860 | 1.2859 | 0.048* | |
C6' | 0.8942 (12) | 0.6444 (11) | 1.1599 (9) | 0.032 (3) | |
H6' | 0.9010 | 0.5819 | 1.1379 | 0.039* | |
C11 | 0.8510 (14) | 0.5874 (11) | 0.9642 (11) | 0.040 (3) | |
O11 | 0.8537 (12) | 0.5035 (8) | 0.9648 (10) | 0.062 (3) | |
C12 | 1.0396 (14) | 0.7294 (11) | 0.9022 (11) | 0.040 (3) | |
O12 | 1.1545 (10) | 0.7256 (10) | 0.8604 (8) | 0.058 (3) | |
C13 | 0.8117 (13) | 0.7510 (10) | 0.8432 (8) | 0.034 (3) | |
O13 | 0.7885 (11) | 0.7705 (10) | 0.7713 (8) | 0.057 (3) | |
C21 | 0.5504 (16) | 0.6269 (13) | 0.9519 (11) | 0.046 (4) | |
O21 | 0.5626 (13) | 0.5751 (9) | 0.8970 (8) | 0.059 (3) | |
C22 | 0.5279 (14) | 0.8338 (12) | 0.9513 (11) | 0.041 (3) | |
O22 | 0.5298 (11) | 0.9025 (10) | 0.8966 (8) | 0.057 (3) | |
C23 | 0.5370 (13) | 0.8117 (11) | 1.1342 (10) | 0.036 (3) | |
O23 | 0.5442 (11) | 0.8660 (8) | 1.1815 (8) | 0.050 (3) | |
C24 | 0.3340 (14) | 0.6995 (11) | 1.0942 (10) | 0.035 (3) | |
O24 | 0.2186 (10) | 0.6913 (9) | 1.1181 (8) | 0.051 (3) | |
C25 | 0.5882 (14) | 0.6058 (10) | 1.1340 (9) | 0.034 (3) | |
O25 | 0.6218 (11) | 0.5440 (8) | 1.1841 (8) | 0.049 (3) | |
Re3 | 0.24594 (5) | 0.65085 (4) | 0.41160 (3) | 0.02698 (16) | |
Re4 | 0.19284 (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* | 0.6719 | 0.9298 | 0.3953 | 0.046* | |
C4* | 0.5425 (15) | 1.0203 (11) | 0.3307 (10) | 0.042 (3) | |
H4* | 0.6108 | 1.0623 | 0.2878 | 0.050* | |
C5* | 0.4070 (17) | 1.0352 (11) | 0.3314 (10) | 0.045 (4) | |
H5* | 0.3809 | 1.0875 | 0.2887 | 0.054* | |
C6* | 0.3084 (14) | 0.9737 (10) | 0.3944 (9) | 0.035 (3) | |
H6* | 0.2146 | 0.9857 | 0.3951 | 0.042* | |
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*B | 0.7096 | 0.8118 | 0.4996 | 0.051* | |
C4*' | 0.6417 (14) | 0.7090 (11) | 0.6143 (10) | 0.039 (3) | |
H4*B | 0.7291 | 0.6933 | 0.6252 | 0.046* | |
C5*' | 0.5284 (15) | 0.6611 (14) | 0.6722 (11) | 0.053 (4) | |
H5*B | 0.5356 | 0.6121 | 0.7238 | 0.064* | |
C6*' | 0.4051 (14) | 0.6847 (12) | 0.6547 (10) | 0.041 (3) | |
H6*B | 0.3263 | 0.6514 | 0.6956 | 0.049* | |
C31 | 0.2893 (14) | 0.5514 (11) | 0.5137 (10) | 0.038 (3) | |
O31 | 0.3186 (13) | 0.4977 (10) | 0.5707 (10) | 0.069 (4) | |
C32 | 0.0478 (13) | 0.6280 (10) | 0.4698 (10) | 0.034 (3) | |
O32 | −0.0672 (10) | 0.6144 (8) | 0.5018 (8) | 0.048 (3) | |
C33 | 0.4430 (13) | 0.6847 (9) | 0.3690 (10) | 0.031 (3) | |
O33 | 0.5563 (10) | 0.7035 (8) | 0.3468 (7) | 0.042 (2) | |
C34 | 0.2555 (14) | 0.5606 (11) | 0.3224 (10) | 0.039 (3) | |
O34 | 0.2543 (12) | 0.5077 (8) | 0.2698 (7) | 0.049 (3) | |
C35 | 0.2082 (13) | 0.7750 (10) | 0.3314 (9) | 0.034 (3) | |
O35 | 0.1877 (11) | 0.8473 (8) | 0.2866 (8) | 0.047 (2) | |
C41 | 0.0901 (13) | 0.6923 (11) | 0.6436 (9) | 0.034 (3) | |
O41 | 0.0339 (11) | 0.6278 (9) | 0.6957 (8) | 0.053 (3) | |
C42 | 0.1400 (13) | 0.8848 (11) | 0.6500 (10) | 0.036 (3) | |
O42 | 0.1009 (12) | 0.9358 (10) | 0.7055 (8) | 0.058 (3) | |
C43 | 0.0336 (14) | 0.8477 (10) | 0.5133 (10) | 0.035 (3) | |
O43 | −0.0613 (10) | 0.8751 (9) | 0.4896 (9) | 0.054 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0261 (3) | 0.0283 (3) | 0.0312 (3) | 0.00319 (19) | −0.0084 (2) | −0.0095 (2) |
Re2 | 0.0265 (3) | 0.0255 (3) | 0.0299 (3) | −0.00139 (19) | −0.0077 (2) | −0.0049 (2) |
N1 | 0.019 (5) | 0.026 (6) | 0.029 (5) | −0.001 (4) | 0.000 (4) | 0.000 (4) |
C2 | 0.019 (5) | 0.021 (6) | 0.036 (7) | 0.002 (4) | −0.010 (5) | −0.004 (5) |
C3 | 0.034 (7) | 0.029 (7) | 0.039 (7) | 0.003 (5) | −0.012 (6) | −0.007 (6) |
C4 | 0.033 (7) | 0.027 (7) | 0.049 (8) | 0.010 (5) | −0.008 (6) | −0.013 (6) |
C5 | 0.034 (7) | 0.036 (8) | 0.047 (8) | −0.002 (6) | −0.014 (6) | −0.002 (6) |
C6 | 0.034 (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) |
C11 | 0.041 (7) | 0.032 (8) | 0.051 (9) | 0.011 (6) | −0.016 (6) | −0.014 (7) |
O11 | 0.067 (7) | 0.032 (7) | 0.095 (10) | 0.014 (5) | −0.029 (7) | −0.025 (6) |
C12 | 0.035 (7) | 0.039 (8) | 0.051 (8) | 0.011 (6) | −0.013 (6) | −0.027 (7) |
O12 | 0.026 (5) | 0.085 (9) | 0.061 (7) | 0.003 (5) | −0.001 (5) | −0.025 (7) |
C13 | 0.040 (7) | 0.037 (8) | 0.016 (6) | 0.005 (6) | 0.001 (5) | −0.001 (5) |
O13 | 0.054 (6) | 0.082 (9) | 0.037 (6) | 0.021 (6) | −0.021 (5) | −0.017 (6) |
C21 | 0.050 (8) | 0.052 (10) | 0.042 (8) | −0.015 (7) | −0.024 (7) | 0.007 (7) |
O21 | 0.081 (8) | 0.051 (7) | 0.051 (7) | −0.006 (6) | −0.016 (6) | −0.031 (6) |
C22 | 0.032 (7) | 0.040 (9) | 0.043 (8) | −0.004 (6) | −0.005 (6) | 0.003 (7) |
O22 | 0.051 (6) | 0.065 (8) | 0.044 (6) | 0.006 (6) | −0.003 (5) | 0.002 (6) |
C23 | 0.029 (6) | 0.040 (8) | 0.036 (7) | −0.008 (6) | −0.008 (5) | 0.002 (6) |
O23 | 0.064 (7) | 0.044 (6) | 0.051 (6) | −0.008 (5) | −0.020 (5) | −0.022 (5) |
C24 | 0.034 (7) | 0.036 (8) | 0.037 (7) | −0.001 (6) | −0.015 (6) | 0.000 (6) |
O24 | 0.033 (6) | 0.054 (7) | 0.062 (7) | 0.000 (5) | −0.010 (5) | −0.008 (6) |
C25 | 0.040 (7) | 0.030 (7) | 0.032 (7) | −0.015 (6) | −0.006 (6) | −0.005 (6) |
O25 | 0.052 (6) | 0.040 (6) | 0.059 (7) | −0.011 (5) | −0.030 (5) | 0.014 (5) |
Re3 | 0.0268 (3) | 0.0234 (3) | 0.0300 (3) | 0.00046 (19) | −0.0071 (2) | −0.0041 (2) |
Re4 | 0.0212 (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) |
C31 | 0.038 (7) | 0.029 (7) | 0.041 (8) | −0.001 (6) | −0.010 (6) | 0.011 (6) |
O31 | 0.071 (8) | 0.061 (8) | 0.071 (8) | 0.005 (6) | −0.031 (7) | 0.019 (7) |
C32 | 0.032 (7) | 0.027 (7) | 0.046 (8) | 0.009 (5) | −0.016 (6) | −0.009 (6) |
O32 | 0.039 (6) | 0.038 (6) | 0.066 (7) | −0.006 (4) | −0.009 (5) | −0.008 (5) |
C33 | 0.040 (8) | 0.010 (6) | 0.045 (8) | 0.008 (5) | −0.017 (6) | −0.007 (5) |
O33 | 0.031 (5) | 0.040 (6) | 0.055 (6) | −0.003 (4) | −0.010 (4) | −0.003 (5) |
C34 | 0.032 (7) | 0.042 (9) | 0.040 (8) | 0.001 (6) | −0.008 (6) | 0.001 (7) |
O34 | 0.062 (7) | 0.047 (7) | 0.040 (6) | −0.002 (5) | −0.013 (5) | −0.012 (5) |
C35 | 0.038 (7) | 0.031 (8) | 0.033 (7) | −0.017 (6) | −0.010 (6) | −0.001 (6) |
O35 | 0.062 (7) | 0.032 (6) | 0.051 (6) | −0.001 (5) | −0.025 (5) | −0.001 (5) |
C41 | 0.029 (6) | 0.039 (8) | 0.031 (7) | −0.007 (6) | −0.003 (5) | −0.006 (6) |
O41 | 0.049 (6) | 0.051 (7) | 0.044 (6) | −0.016 (5) | 0.009 (5) | 0.003 (5) |
C42 | 0.030 (6) | 0.034 (8) | 0.045 (8) | −0.008 (6) | −0.011 (6) | −0.006 (6) |
O42 | 0.059 (7) | 0.068 (8) | 0.050 (7) | 0.000 (6) | −0.007 (5) | −0.038 (6) |
C43 | 0.035 (7) | 0.024 (7) | 0.047 (8) | −0.002 (5) | −0.012 (6) | −0.003 (6) |
O43 | 0.034 (5) | 0.052 (7) | 0.082 (8) | 0.009 (5) | −0.027 (6) | −0.012 (6) |
Re1—Re2 | 3.0856 (18) | Re4—C41 | 1.927 (14) |
Re1—N1 | 2.149 (10) | Re4—C42 | 1.918 (14) |
Re1—N1' | 2.184 (11) | Re4—C43 | 1.935 (14) |
Re1—C11 | 1.920 (15) | N1*—C2* | 1.336 (15) |
Re1—C12 | 1.909 (14) | N1*—C6* | 1.351 (17) |
Re1—C13 | 1.910 (13) | C2*—C3* | 1.387 (18) |
Re2—C21 | 1.982 (17) | C2*—C2*' | 1.470 (19) |
Re2—C22 | 1.964 (16) | C3*—C4* | 1.40 (2) |
Re2—C23 | 1.995 (14) | C4*—C5* | 1.37 (2) |
Re2—C24 | 1.940 (13) | C5*—C6* | 1.38 (2) |
Re2—C25 | 1.988 (15) | N1*'—C2*' | 1.378 (16) |
N1—C2 | 1.360 (16) | N1*'—C6*' | 1.330 (19) |
N1—C6 | 1.353 (17) | C2*'—C3*' | 1.398 (17) |
C2—C3 | 1.391 (17) | C3*'—C4*' | 1.36 (2) |
C2—C2' | 1.486 (17) | C4*'—C5*' | 1.36 (2) |
C3—C4 | 1.40 (2) | C5*'—C6*' | 1.36 (2) |
C4—C5 | 1.37 (2) | C31—O31 | 1.121 (17) |
C5—C6 | 1.38 (2) | C32—O32 | 1.144 (16) |
N1'—C2' | 1.371 (16) | C33—O33 | 1.139 (16) |
N1'—C6' | 1.326 (17) | C34—O34 | 1.153 (18) |
C2'—C3' | 1.363 (17) | C35—O35 | 1.136 (17) |
C3'—C4' | 1.38 (2) | C41—O41 | 1.140 (17) |
C4'—C5' | 1.37 (2) | C42—O42 | 1.133 (17) |
C5'—C6' | 1.377 (19) | C43—O43 | 1.136 (16) |
C11—O11 | 1.136 (17) | C3—H3 | 0.95 |
C12—O12 | 1.154 (17) | C4—H4 | 0.95 |
C13—O13 | 1.154 (16) | C5—H5 | 0.95 |
C21—O21 | 1.142 (19) | C6—H6 | 0.95 |
C22—O22 | 1.134 (18) | C3'—H3' | 0.95 |
C23—O23 | 1.123 (17) | C4'—H4' | 0.95 |
C24—O24 | 1.130 (16) | C5'—H5' | 0.95 |
C25—O25 | 1.131 (17) | C6'—H6' | 0.95 |
Re3—Re4 | 3.0816 (18) | C3*—H3* | 0.95 |
Re3—C31 | 1.994 (14) | C4*—H4* | 0.95 |
Re3—C32 | 1.973 (14) | C5*—H5* | 0.95 |
Re3—C33 | 1.982 (13) | C6*—H6* | 0.95 |
Re3—C34 | 1.934 (16) | C3*'—H3*B | 0.95 |
Re3—C35 | 1.984 (15) | C4*'—H4*B | 0.95 |
Re4—N1* | 2.166 (11) | C5*'—H5*B | 0.95 |
Re4—N1*' | 2.170 (10) | C6*'—H6*B | 0.95 |
C13—Re1—C12 | 89.4 (6) | C42—Re4—C43 | 89.2 (6) |
C13—Re1—C11 | 90.0 (6) | C41—Re4—C43 | 91.8 (6) |
C12—Re1—C11 | 89.1 (6) | C42—Re4—N1*' | 94.3 (5) |
C13—Re1—N1 | 96.9 (5) | C41—Re4—N1*' | 95.4 (5) |
C12—Re1—N1 | 94.5 (5) | C43—Re4—N1*' | 172.0 (5) |
C11—Re1—N1 | 172.2 (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—Re3 | 173.8 (4) |
C13—Re1—Re2 | 85.9 (4) | C41—Re4—Re3 | 85.1 (4) |
C12—Re1—Re2 | 174.0 (4) | C43—Re4—Re3 | 87.0 (4) |
C11—Re1—Re2 | 87.2 (4) | N1*'—Re4—Re3 | 90.1 (3) |
N1—Re1—Re2 | 89.8 (2) | N1*—Re4—Re3 | 89.9 (3) |
N1'—Re1—Re2 | 90.9 (3) | C2*—N1*—C6* | 117.6 (11) |
C24—Re2—C22 | 97.6 (6) | C2*—N1*—Re4 | 118.4 (8) |
C24—Re2—C21 | 92.0 (6) | C6*—N1*—Re4 | 124.0 (8) |
C22—Re2—C21 | 90.4 (6) | N1*—C2*—C3* | 124.4 (13) |
C24—Re2—C25 | 97.8 (6) | N1*—C2*—C2*' | 114.8 (10) |
C22—Re2—C25 | 164.5 (5) | C3*—C2*—C2*' | 120.8 (12) |
C21—Re2—C25 | 90.9 (6) | C2*—C3*—C4* | 116.9 (13) |
C24—Re2—C23 | 95.3 (5) | C5*—C4*—C3* | 119.3 (13) |
C22—Re2—C23 | 87.3 (6) | C4*—C5*—C6* | 119.8 (15) |
C21—Re2—C23 | 172.6 (6) | N1*—C6*—C5* | 121.9 (13) |
C25—Re2—C23 | 89.5 (5) | C6*'—N1*'—C2*' | 118.6 (11) |
C24—Re2—Re1 | 175.3 (4) | C6*'—N1*'—Re4 | 125.3 (9) |
C22—Re2—Re1 | 83.7 (4) | C2*'—N1*'—Re4 | 115.9 (8) |
C21—Re2—Re1 | 83.5 (4) | N1*'—C2*'—C3*' | 119.0 (13) |
C25—Re2—Re1 | 81.1 (4) | N1*'—C2*'—C2* | 116.1 (10) |
C23—Re2—Re1 | 89.3 (4) | C3*'—C2*'—C2* | 124.9 (12) |
C6—N1—C2 | 117.5 (11) | C4*'—C3*'—C2*' | 119.8 (14) |
C6—N1—Re1 | 124.6 (9) | C3*'—C4*'—C5*' | 120.1 (13) |
C2—N1—Re1 | 117.9 (8) | C6*'—C5*'—C4*' | 118.7 (15) |
N1—C2—C3 | 122.0 (12) | N1*'—C6*'—C5*' | 123.6 (14) |
N1—C2—C2' | 115.8 (10) | O31—C31—Re3 | 177.0 (13) |
C3—C2—C2' | 122.1 (11) | O32—C32—Re3 | 178.6 (12) |
C2—C3—C4 | 119.1 (12) | O33—C33—Re3 | 178.3 (12) |
C5—C4—C3 | 118.8 (13) | O34—C34—Re3 | 176.6 (12) |
C4—C5—C6 | 119.5 (14) | O35—C35—Re3 | 178.5 (11) |
N1—C6—C5 | 123.1 (13) | O41—C41—Re4 | 177.4 (13) |
C6'—N1'—C2' | 118.1 (11) | O42—C42—Re4 | 175.9 (12) |
C6'—N1'—Re1 | 124.5 (9) | O43—C43—Re4 | 178.6 (13) |
C2'—N1'—Re1 | 117.4 (8) | C2—C3—H3 | 120.4 |
N1'—C2'—C3' | 121.5 (12) | C4—C3—H3 | 120.5 |
N1'—C2'—C2 | 113.9 (10) | C5—C4—H4 | 120.6 |
C3'—C2'—C2 | 124.7 (12) | C3—C4—H4 | 120.6 |
C2'—C3'—C4' | 120.2 (13) | C4—C5—H5 | 120.3 |
C5'—C4'—C3' | 117.8 (13) | C6—C5—H5 | 120.3 |
C4'—C5'—C6' | 119.9 (13) | N1—C6—H6 | 118.4 |
N1'—C6'—C5' | 122.4 (13) | C5—C6—H6 | 118.4 |
O11—C11—Re1 | 179.7 (14) | C2'—C3'—H3' | 119.9 |
O12—C12—Re1 | 175.1 (12) | C4'—C3'—H3' | 119.9 |
O13—C13—Re1 | 175.6 (13) | C5'—C4'—H4' | 121.1 |
O21—C21—Re2 | 179.5 (14) | C3'—C4'—H4' | 121.1 |
O22—C22—Re2 | 177.7 (13) | C4'—C5'—H5' | 120.1 |
O23—C23—Re2 | 177.9 (12) | C6'—C5'—H5' | 120.1 |
O24—C24—Re2 | 177.2 (13) | N1'—C6'—H6' | 118.8 |
O25—C25—Re2 | 178.7 (11) | C5'—C6'—H6' | 118.8 |
C34—Re3—C32 | 91.2 (6) | C2*—C3*—H3* | 121.5 |
C34—Re3—C33 | 97.2 (5) | C4*—C3*—H3* | 121.5 |
C32—Re3—C33 | 171.5 (5) | C5*—C4*—H4* | 120.4 |
C34—Re3—C31 | 97.9 (6) | C3*—C4*—H4* | 120.4 |
C32—Re3—C31 | 89.8 (6) | C4*—C5*—H5* | 120.1 |
C33—Re3—C31 | 87.8 (5) | C6*—C5*—H5* | 120.1 |
C34—Re3—C35 | 97.0 (6) | N1*—C6*—H6* | 119.0 |
C32—Re3—C35 | 92.2 (5) | C5*—C6*—H6* | 119.0 |
C33—Re3—C35 | 88.0 (5) | C4*'—C3*'—H3*B | 120.1 |
C31—Re3—C35 | 164.9 (6) | C2*'—C3*'—H3*B | 120.1 |
C34—Re3—Re4 | 173.0 (4) | C3*'—C4*'—H4*B | 119.9 |
C32—Re3—Re4 | 82.4 (4) | C5*'—C4*'—H4*B | 119.9 |
C33—Re3—Re4 | 89.3 (3) | C6*'—C5*'—H5*B | 120.7 |
C31—Re3—Re4 | 85.0 (4) | C4*'—C5*'—H5*B | 120.7 |
C35—Re3—Re4 | 80.5 (4) | N1*'—C6*'—H6*B | 118.2 |
C42—Re4—C41 | 90.2 (6) | C5*'—C6*'—H6*B | 118.2 |
Experimental details
Crystal data | |
Chemical formula | C18H8N2O8Re2 |
Mr | 752.66 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 1948.1 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 12.47 |
Crystal size (mm) | 0.65 × 0.24 × 0.09 |
Data collection | |
Diffractometer | Stoe Stadi-4 four-circle diffractometer |
Absorption correction | Part of the refinement model (ΔF) (DIFABS; Walker & Stuart, 1983) |
Tmin, Tmax | 0.049, 0.310 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6852, 6852, 5903 |
Rint | 0.0 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.136, 1.11 |
No. of reflections | 6852 |
No. of parameters | 542 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.082P)2 + 20.6P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 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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