Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801003658/ci6007sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801003658/ci6007Isup2.hkl |
CCDC reference: 159838
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.016 Å
- R factor = 0.034
- wR factor = 0.094
- Data-to-parameter ratio = 14.7
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_420 Alert C D-H Without Acceptor N(1) - H(1) ?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Me3NO (46 mg, 0.767 mmol) was added to a solution of [Re2(CO)10] (200 mg, 0.307 mmol) and benzophenone imine (103 µl, 0.614 mmol) in 1,2-dichloroethane (20 ml). The color changed immediately to dark orange. The mixture was heated at reflux temperature for 1 h. The solution was concentrated under reduced pressure to ca 3 ml and the residue set on the top of a column of neutral alumina (2 × 10 cm, activity I). Elution with hexanes afforded a small amount of unreacted [Re2(CO)10]. Subsequent elution with hexanes/dichloromethane (3:1) afforded an orange band which contained 110 mg (44%) of the title compound, which was crystallized from Et2O/hexanes at 253 K.
H atoms were placed in geometrically idealized positions employing appropriate riding models with isotropic displacement parameters constrained to 1.2 times the Ueq of their carrier atoms.
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CRYSDA (Beurskens et al., 1992); data reduction: REFLEX (Garcia-Granda et al., 1999); program(s) used to solve structure: DIRDIF (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: EUCLID (Spek, 1982); software used to prepare material for publication: SHELXL97.
Fig. 1. The structure of the title complex showing 50% probability displacement ellipsoids and the atom-numbering scheme. |
[Re2(C13H11N)(CO)9] | F(000) = 1488 |
Mr = 805.72 | Dx = 2.275 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.8071 (6) Å | Cell parameters from 2241 reflections |
b = 13.6951 (8) Å | θ = 1–25° |
c = 16.4285 (11) Å | µ = 10.25 mm−1 |
β = 102.780 (4)° | T = 293 K |
V = 2371.3 (2) Å3 | Prismatic, yellow |
Z = 4 | 0.26 × 0.10 × 0.07 mm |
Nonius CAD-4 diffractometer | 2349 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.054 |
Graphite monochromator | θmax = 26.0°, θmin = 1.9° |
ω–2θ scans | h = −13→12 |
Absorption correction: empirical (using intensity measurements) (XABS2; Parkin et al., 1995) | k = 0→16 |
Tmin = 0.113, Tmax = 0.485 | l = 0→20 |
7361 measured reflections | 3 standard reflections every 200 reflections |
4499 independent reflections | intensity decay: 2.4% |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0426P)2] where P = (Fo2 + 2Fc2)/3 |
4499 reflections | (Δ/σ)max < 0.001 |
307 parameters | Δρmax = 0.94 e Å−3 |
0 restraints | Δρmin = −1.28 e Å−3 |
[Re2(C13H11N)(CO)9] | V = 2371.3 (2) Å3 |
Mr = 805.72 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.8071 (6) Å | µ = 10.25 mm−1 |
b = 13.6951 (8) Å | T = 293 K |
c = 16.4285 (11) Å | 0.26 × 0.10 × 0.07 mm |
β = 102.780 (4)° |
Nonius CAD-4 diffractometer | 2349 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) (XABS2; Parkin et al., 1995) | Rint = 0.054 |
Tmin = 0.113, Tmax = 0.485 | 3 standard reflections every 200 reflections |
7361 measured reflections | intensity decay: 2.4% |
4499 independent reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.94 e Å−3 |
4499 reflections | Δρmin = −1.28 e Å−3 |
307 parameters |
Experimental. Anal. and spectroscopic data: Calcd for C22H11NO9Re2 (805.72): C, 32.79; H, 1.37; N, 1.74. Found: C, 33.13; H, 1.49; N, 1.83. IR (hexanes): ν(CO) 2098 (vw), 2043 (w), 2012 (w), 1987 (versus), 1980 (s), 1973 (w), 1962 (w), 1929 (w) cm-1. 1H NMR (CD2Cl2): δ 9.88 (s, 1 H, NH), 7.64–7.25 (m, 10 H, Ph2) p.p.m.. |
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 | 0.25591 (4) | 0.23125 (4) | 0.33923 (2) | 0.03652 (13) | |
Re2 | 0.48456 (4) | 0.26694 (4) | 0.48277 (3) | 0.04584 (15) | |
N1 | 0.1550 (7) | 0.1688 (6) | 0.4302 (4) | 0.0341 (19) | |
H1 | 0.1893 | 0.1150 | 0.4508 | 0.041* | |
O14 | 0.1700 (8) | 0.4435 (7) | 0.3689 (5) | 0.068 (3) | |
O15 | 0.0416 (8) | 0.1908 (7) | 0.1867 (4) | 0.068 (2) | |
O16 | 0.3742 (8) | 0.0282 (7) | 0.3178 (5) | 0.066 (2) | |
O17 | 0.4138 (9) | 0.3160 (7) | 0.2217 (5) | 0.085 (3) | |
O18 | 0.7111 (10) | 0.3128 (9) | 0.6285 (6) | 0.105 (4) | |
O19 | 0.4194 (9) | 0.0615 (7) | 0.5402 (5) | 0.072 (3) | |
O20 | 0.2814 (8) | 0.3488 (6) | 0.5735 (5) | 0.074 (3) | |
O21 | 0.4950 (9) | 0.4674 (8) | 0.3963 (6) | 0.085 (3) | |
O22 | 0.6364 (8) | 0.1639 (7) | 0.3649 (5) | 0.078 (3) | |
C1 | 0.0589 (9) | 0.1908 (8) | 0.4608 (5) | 0.035 (2) | |
C2 | 0.0347 (10) | 0.1340 (7) | 0.5339 (5) | 0.037 (2) | |
C3 | −0.0879 (11) | 0.1317 (8) | 0.5449 (6) | 0.049 (3) | |
H3 | −0.1516 | 0.1641 | 0.5074 | 0.059* | |
C4 | −0.1176 (13) | 0.0811 (8) | 0.6120 (7) | 0.056 (3) | |
H4 | −0.2002 | 0.0799 | 0.6199 | 0.067* | |
C5 | −0.0220 (14) | 0.0334 (9) | 0.6658 (8) | 0.063 (4) | |
H5 | −0.0409 | −0.0012 | 0.7102 | 0.076* | |
C6 | 0.0991 (12) | 0.0349 (8) | 0.6563 (6) | 0.052 (3) | |
H6 | 0.1625 | 0.0022 | 0.6939 | 0.063* | |
C7 | 0.1276 (11) | 0.0857 (8) | 0.5899 (5) | 0.049 (3) | |
H7 | 0.2108 | 0.0871 | 0.5832 | 0.059* | |
C8 | −0.0300 (9) | 0.2707 (8) | 0.4255 (6) | 0.039 (2) | |
C9 | −0.0470 (11) | 0.3485 (8) | 0.4760 (6) | 0.049 (3) | |
H9 | −0.0013 | 0.3517 | 0.5310 | 0.059* | |
C10 | −0.1319 (12) | 0.4206 (9) | 0.4439 (7) | 0.060 (3) | |
H10 | −0.1450 | 0.4723 | 0.4777 | 0.072* | |
C11 | −0.1963 (12) | 0.4175 (10) | 0.3640 (7) | 0.064 (4) | |
H11 | −0.2506 | 0.4683 | 0.3420 | 0.076* | |
C12 | −0.1820 (11) | 0.3400 (10) | 0.3152 (6) | 0.055 (3) | |
H12 | −0.2299 | 0.3363 | 0.2607 | 0.066* | |
C13 | −0.0980 (9) | 0.2675 (9) | 0.3455 (6) | 0.045 (3) | |
H13 | −0.0871 | 0.2157 | 0.3112 | 0.054* | |
C14 | 0.1985 (11) | 0.3651 (9) | 0.3593 (6) | 0.044 (3) | |
C15 | 0.1190 (11) | 0.2073 (8) | 0.2463 (6) | 0.044 (3) | |
C16 | 0.3304 (11) | 0.1019 (8) | 0.3264 (6) | 0.045 (3) | |
C17 | 0.3547 (11) | 0.2867 (9) | 0.2662 (6) | 0.054 (3) | |
C18 | 0.6254 (13) | 0.2947 (11) | 0.5735 (8) | 0.071 (4) | |
C19 | 0.4484 (11) | 0.1363 (11) | 0.5217 (7) | 0.053 (3) | |
C20 | 0.3577 (12) | 0.3186 (9) | 0.5398 (6) | 0.054 (3) | |
C21 | 0.4927 (11) | 0.3932 (10) | 0.4280 (7) | 0.058 (3) | |
C22 | 0.5853 (11) | 0.2033 (9) | 0.4093 (7) | 0.056 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0405 (2) | 0.0380 (3) | 0.0323 (2) | −0.0003 (2) | 0.01060 (17) | 0.00094 (19) |
Re2 | 0.0400 (3) | 0.0459 (3) | 0.0493 (3) | 0.0020 (2) | 0.0048 (2) | −0.0043 (2) |
N1 | 0.042 (5) | 0.020 (5) | 0.039 (4) | −0.001 (4) | 0.005 (4) | 0.003 (4) |
O14 | 0.089 (7) | 0.047 (6) | 0.075 (6) | 0.002 (5) | 0.033 (5) | 0.002 (5) |
O15 | 0.063 (6) | 0.088 (7) | 0.042 (4) | 0.007 (5) | −0.007 (4) | 0.001 (4) |
O16 | 0.065 (6) | 0.054 (6) | 0.079 (6) | 0.011 (5) | 0.015 (5) | −0.017 (5) |
O17 | 0.098 (7) | 0.099 (8) | 0.077 (6) | −0.025 (6) | 0.061 (6) | 0.002 (5) |
O18 | 0.070 (7) | 0.126 (11) | 0.100 (8) | −0.003 (7) | −0.019 (6) | −0.020 (7) |
O19 | 0.076 (7) | 0.061 (7) | 0.088 (6) | 0.017 (6) | 0.036 (5) | 0.006 (5) |
O20 | 0.084 (7) | 0.058 (6) | 0.088 (6) | 0.018 (5) | 0.035 (6) | −0.004 (5) |
O21 | 0.096 (8) | 0.063 (7) | 0.096 (7) | −0.018 (6) | 0.023 (6) | −0.003 (6) |
O22 | 0.065 (6) | 0.089 (8) | 0.093 (7) | 0.000 (5) | 0.042 (6) | −0.019 (5) |
C1 | 0.047 (6) | 0.032 (6) | 0.029 (5) | −0.013 (5) | 0.014 (5) | −0.005 (4) |
C2 | 0.046 (6) | 0.032 (7) | 0.034 (5) | −0.011 (5) | 0.012 (5) | −0.006 (4) |
C3 | 0.059 (8) | 0.042 (8) | 0.047 (6) | −0.008 (6) | 0.015 (6) | −0.006 (5) |
C4 | 0.079 (10) | 0.037 (8) | 0.059 (7) | −0.013 (7) | 0.031 (7) | −0.004 (6) |
C5 | 0.097 (12) | 0.034 (8) | 0.067 (8) | −0.016 (8) | 0.039 (8) | −0.007 (6) |
C6 | 0.077 (9) | 0.040 (8) | 0.033 (5) | 0.005 (7) | 0.000 (6) | 0.009 (5) |
C7 | 0.057 (8) | 0.055 (9) | 0.034 (6) | −0.001 (6) | 0.006 (5) | 0.000 (5) |
C8 | 0.030 (5) | 0.039 (7) | 0.048 (6) | 0.006 (5) | 0.007 (4) | 0.006 (5) |
C9 | 0.076 (9) | 0.039 (8) | 0.035 (6) | 0.003 (6) | 0.017 (6) | −0.003 (5) |
C10 | 0.077 (9) | 0.049 (9) | 0.060 (7) | 0.021 (7) | 0.025 (7) | 0.010 (6) |
C11 | 0.075 (9) | 0.059 (10) | 0.056 (7) | 0.029 (7) | 0.012 (7) | 0.021 (6) |
C12 | 0.049 (7) | 0.072 (10) | 0.040 (6) | 0.008 (7) | 0.001 (5) | 0.014 (6) |
C13 | 0.040 (6) | 0.053 (7) | 0.045 (5) | 0.005 (6) | 0.015 (5) | −0.002 (5) |
C14 | 0.062 (8) | 0.034 (8) | 0.039 (6) | −0.011 (6) | 0.016 (5) | −0.008 (5) |
C15 | 0.060 (8) | 0.040 (8) | 0.035 (6) | −0.002 (6) | 0.016 (6) | 0.001 (5) |
C16 | 0.052 (7) | 0.033 (8) | 0.047 (6) | −0.007 (6) | 0.007 (5) | −0.008 (5) |
C17 | 0.058 (8) | 0.063 (10) | 0.039 (6) | −0.017 (6) | 0.003 (5) | −0.010 (5) |
C18 | 0.064 (9) | 0.079 (12) | 0.069 (9) | 0.018 (8) | 0.010 (7) | 0.003 (7) |
C19 | 0.034 (6) | 0.067 (10) | 0.059 (7) | 0.002 (6) | 0.014 (5) | −0.002 (7) |
C20 | 0.072 (9) | 0.043 (8) | 0.043 (6) | −0.003 (7) | −0.001 (6) | −0.009 (5) |
C21 | 0.044 (7) | 0.055 (10) | 0.073 (8) | −0.009 (7) | 0.006 (6) | 0.008 (7) |
C22 | 0.048 (7) | 0.050 (9) | 0.063 (7) | 0.002 (6) | 0.002 (6) | 0.007 (6) |
Re1—C15 | 1.904 (11) | C1—C2 | 1.501 (12) |
Re1—C17 | 1.929 (11) | C2—C7 | 1.373 (14) |
Re1—C16 | 1.976 (12) | C2—C3 | 1.377 (13) |
Re1—C14 | 1.986 (12) | C3—C4 | 1.398 (13) |
Re1—N1 | 2.209 (7) | C3—H3 | 0.9300 |
Re1—Re2 | 3.0542 (6) | C4—C5 | 1.367 (16) |
Re2—C18 | 1.918 (14) | C4—H4 | 0.9300 |
Re2—C20 | 1.956 (12) | C5—C6 | 1.352 (16) |
Re2—C21 | 1.960 (13) | C5—H5 | 0.9300 |
Re2—C19 | 1.968 (14) | C6—C7 | 1.385 (12) |
Re2—C22 | 1.995 (12) | C6—H6 | 0.9300 |
N1—C1 | 1.285 (11) | C7—H7 | 0.9300 |
N1—H1 | 0.8600 | C8—C13 | 1.357 (13) |
O14—C14 | 1.137 (13) | C8—C9 | 1.387 (14) |
O15—C15 | 1.160 (12) | C9—C10 | 1.372 (15) |
O16—C16 | 1.136 (12) | C9—H9 | 0.9300 |
O17—C17 | 1.146 (11) | C10—C11 | 1.344 (15) |
O18—C18 | 1.169 (15) | C10—H10 | 0.9300 |
O19—C19 | 1.133 (13) | C11—C12 | 1.359 (15) |
O20—C20 | 1.166 (12) | C11—H11 | 0.9300 |
O21—C21 | 1.145 (13) | C12—C13 | 1.363 (14) |
O22—C22 | 1.143 (12) | C12—H12 | 0.9300 |
C1—C8 | 1.486 (14) | C13—H13 | 0.9300 |
C15—Re1—C17 | 90.5 (4) | C4—C3—H3 | 119.6 |
C15—Re1—C16 | 91.3 (4) | C5—C4—C3 | 118.3 (12) |
C17—Re1—C16 | 89.6 (5) | C5—C4—H4 | 120.9 |
C15—Re1—C14 | 94.4 (5) | C3—C4—H4 | 120.9 |
C17—Re1—C14 | 88.6 (4) | C6—C5—C4 | 122.0 (11) |
C16—Re1—C14 | 174.0 (5) | C6—C5—H5 | 119.0 |
C15—Re1—N1 | 93.6 (3) | C4—C5—H5 | 119.0 |
C17—Re1—N1 | 175.9 (4) | C5—C6—C7 | 119.2 (11) |
C16—Re1—N1 | 89.9 (4) | C5—C6—H6 | 120.4 |
C14—Re1—N1 | 91.5 (4) | C7—C6—H6 | 120.4 |
C15—Re1—Re2 | 177.1 (3) | C2—C7—C6 | 120.9 (10) |
C17—Re1—Re2 | 87.3 (3) | C2—C7—H7 | 119.6 |
C16—Re1—Re2 | 86.9 (3) | C6—C7—H7 | 119.6 |
C14—Re1—Re2 | 87.3 (3) | C13—C8—C9 | 119.2 (10) |
N1—Re1—Re2 | 88.6 (2) | C13—C8—C1 | 121.2 (10) |
C18—Re2—C20 | 94.3 (5) | C9—C8—C1 | 119.5 (9) |
C18—Re2—C21 | 94.2 (6) | C10—C9—C8 | 119.3 (10) |
C20—Re2—C21 | 90.5 (5) | C10—C9—H9 | 120.4 |
C18—Re2—C19 | 96.2 (6) | C8—C9—H9 | 120.4 |
C20—Re2—C19 | 87.9 (5) | C11—C10—C9 | 120.7 (11) |
C21—Re2—C19 | 169.5 (5) | C11—C10—H10 | 119.6 |
C18—Re2—C22 | 96.4 (5) | C9—C10—H10 | 119.6 |
C20—Re2—C22 | 169.0 (5) | C10—C11—C12 | 119.9 (12) |
C21—Re2—C22 | 91.2 (5) | C10—C11—H11 | 120.0 |
C19—Re2—C22 | 88.5 (5) | C12—C11—H11 | 120.0 |
C18—Re2—Re1 | 177.6 (4) | C11—C12—C13 | 120.4 (11) |
C20—Re2—Re1 | 83.9 (3) | C11—C12—H12 | 119.8 |
C21—Re2—Re1 | 84.1 (4) | C13—C12—H12 | 119.8 |
C19—Re2—Re1 | 85.4 (3) | C8—C13—C12 | 120.3 (11) |
C22—Re2—Re1 | 85.4 (3) | C8—C13—H13 | 119.8 |
C1—N1—Re1 | 137.4 (7) | C12—C13—H13 | 119.8 |
C1—N1—H1 | 111.3 | O14—C14—Re1 | 176.7 (10) |
Re1—N1—H1 | 111.3 | O15—C15—Re1 | 175.4 (9) |
N1—C1—C8 | 122.0 (8) | O16—C16—Re1 | 178.6 (10) |
N1—C1—C2 | 119.3 (10) | O17—C17—Re1 | 177.3 (11) |
C8—C1—C2 | 118.7 (8) | O18—C18—Re2 | 179.2 (14) |
C7—C2—C3 | 118.8 (9) | O19—C19—Re2 | 175.0 (11) |
C7—C2—C1 | 123.7 (9) | O20—C20—Re2 | 179.4 (11) |
C3—C2—C1 | 117.4 (10) | O21—C21—Re2 | 178.5 (12) |
C2—C3—C4 | 120.8 (11) | O22—C22—Re2 | 175.8 (11) |
C2—C3—H3 | 119.6 | ||
C17—Re1—Re2—C20 | 134.3 (5) | C8—C1—C2—C7 | −155.4 (10) |
C16—Re1—Re2—C20 | −136.0 (5) | N1—C1—C2—C3 | −155.6 (9) |
C14—Re1—Re2—C20 | 45.5 (5) | C8—C1—C2—C3 | 24.0 (14) |
N1—Re1—Re2—C20 | −46.0 (4) | C7—C2—C3—C4 | 0.0 (16) |
C17—Re1—Re2—C21 | 43.1 (5) | C1—C2—C3—C4 | −179.4 (9) |
C16—Re1—Re2—C21 | 132.9 (5) | C2—C3—C4—C5 | −0.6 (16) |
C14—Re1—Re2—C21 | −45.6 (5) | C3—C4—C5—C6 | 0.8 (18) |
N1—Re1—Re2—C21 | −137.2 (4) | C4—C5—C6—C7 | −0.4 (18) |
C17—Re1—Re2—C19 | −137.4 (5) | C3—C2—C7—C6 | 0.4 (16) |
C16—Re1—Re2—C19 | −47.7 (4) | C1—C2—C7—C6 | 179.8 (10) |
C14—Re1—Re2—C19 | 133.9 (4) | C5—C6—C7—C2 | −0.2 (17) |
N1—Re1—Re2—C19 | 42.3 (4) | N1—C1—C8—C13 | 61.2 (14) |
C17—Re1—Re2—C22 | −48.6 (5) | C2—C1—C8—C13 | −118.4 (10) |
C16—Re1—Re2—C22 | 41.1 (4) | N1—C1—C8—C9 | −120.8 (11) |
C14—Re1—Re2—C22 | −137.3 (4) | C2—C1—C8—C9 | 59.6 (13) |
N1—Re1—Re2—C22 | 131.1 (4) | C13—C8—C9—C10 | −0.1 (16) |
C15—Re1—N1—C1 | −68.8 (10) | C1—C8—C9—C10 | −178.1 (10) |
C16—Re1—N1—C1 | −160.1 (10) | C8—C9—C10—C11 | −1.4 (18) |
C14—Re1—N1—C1 | 25.7 (10) | C9—C10—C11—C12 | 3 (2) |
Re2—Re1—N1—C1 | 113.0 (10) | C10—C11—C12—C13 | −3.3 (19) |
Re1—N1—C1—C8 | 10.5 (16) | C9—C8—C13—C12 | −0.1 (16) |
Re1—N1—C1—C2 | −169.9 (7) | C1—C8—C13—C12 | 177.9 (9) |
N1—C1—C2—C7 | 25.0 (15) | C11—C12—C13—C8 | 1.8 (17) |
Experimental details
Crystal data | |
Chemical formula | [Re2(C13H11N)(CO)9] |
Mr | 805.72 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 10.8071 (6), 13.6951 (8), 16.4285 (11) |
β (°) | 102.780 (4) |
V (Å3) | 2371.3 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 10.25 |
Crystal size (mm) | 0.26 × 0.10 × 0.07 |
Data collection | |
Diffractometer | Nonius CAD-4 diffractometer |
Absorption correction | Empirical (using intensity measurements) (XABS2; Parkin et al., 1995) |
Tmin, Tmax | 0.113, 0.485 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7361, 4499, 2349 |
Rint | 0.054 |
(sin θ/λ)max (Å−1) | 0.616 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.094, 1.00 |
No. of reflections | 4499 |
No. of parameters | 307 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.94, −1.28 |
Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1994), CRYSDA (Beurskens et al., 1992), REFLEX (Garcia-Granda et al., 1999), DIRDIF (Beurskens et al., 1992), SHELXL97 (Sheldrick, 1997), EUCLID (Spek, 1982), SHELXL97.
Re1—C15 | 1.904 (11) | N1—C1 | 1.285 (11) |
Re1—C17 | 1.929 (11) | O14—C14 | 1.137 (13) |
Re1—C16 | 1.976 (12) | O15—C15 | 1.160 (12) |
Re1—C14 | 1.986 (12) | O16—C16 | 1.136 (12) |
Re1—N1 | 2.209 (7) | O17—C17 | 1.146 (11) |
Re1—Re2 | 3.0542 (6) | O18—C18 | 1.169 (15) |
Re2—C18 | 1.918 (14) | O19—C19 | 1.133 (13) |
Re2—C20 | 1.956 (12) | O20—C20 | 1.166 (12) |
Re2—C21 | 1.960 (13) | O21—C21 | 1.145 (13) |
Re2—C19 | 1.968 (14) | O22—C22 | 1.143 (12) |
Re2—C22 | 1.995 (12) | ||
C15—Re1—C17 | 90.5 (4) | C18—Re2—C21 | 94.2 (6) |
C15—Re1—C16 | 91.3 (4) | C20—Re2—C21 | 90.5 (5) |
C17—Re1—C16 | 89.6 (5) | C18—Re2—C19 | 96.2 (6) |
C15—Re1—C14 | 94.4 (5) | C20—Re2—C19 | 87.9 (5) |
C17—Re1—C14 | 88.6 (4) | C21—Re2—C19 | 169.5 (5) |
C16—Re1—C14 | 174.0 (5) | C18—Re2—C22 | 96.4 (5) |
C15—Re1—N1 | 93.6 (3) | C20—Re2—C22 | 169.0 (5) |
C17—Re1—N1 | 175.9 (4) | C21—Re2—C22 | 91.2 (5) |
C16—Re1—N1 | 89.9 (4) | C19—Re2—C22 | 88.5 (5) |
C14—Re1—N1 | 91.5 (4) | C18—Re2—Re1 | 177.6 (4) |
C15—Re1—Re2 | 177.1 (3) | C20—Re2—Re1 | 83.9 (3) |
C17—Re1—Re2 | 87.3 (3) | C21—Re2—Re1 | 84.1 (4) |
C16—Re1—Re2 | 86.9 (3) | C19—Re2—Re1 | 85.4 (3) |
C14—Re1—Re2 | 87.3 (3) | C22—Re2—Re1 | 85.4 (3) |
N1—Re1—Re2 | 88.6 (2) | C1—N1—Re1 | 137.4 (7) |
C18—Re2—C20 | 94.3 (5) |
Interest in the synthesis and reactivity of late-transition-metal amido complexes has grown considerably in recent years as a consequence of the relative scarcity of such compounds and of their potential use in carbon–nitrogen bond-forming reactions (Cabeza et al. 1998). In this field, we have recently communicated the first insertion of a non-activated alkyne into a metal–nitrogen bond, achieved onto a triruthenium cluster derived from benzophenone imine (Cabeza et al., 1997). In an extension of the interesting reactivity observed for these ruthenium complexes to other transition metals, we studied the reactivity of benzophenone imine with osmium (Cabeza et al., 2000) and rhenium carbonyl derivatives. The crystal structure reported herein of (benzophenone imine-N)nonacarbonyldirhenium(0)(Re—Re), (I), is part of this latter study.