Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301095X/om6143sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680301095X/om6143Isup2.hkl |
CCDC reference: 217361
An equimolar mixture of [Re(bpy)(CO)3Cl] and AgSbF6 in acetonitrile was refluxed under anaerobic condition for 16 h, after which the resulting solution was filtered to give a yellow solution. The filtrate was evaporated under vacuum to afford a yellow–orange solid which was redissolved in dichloromethane and layered with diethyl ether to form well shaped yellow crystals suitable for X-ray diffraction analysis.
The H-atom positions were generated geometrically (C—H distance fixed at 0.96 or 0.93 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms before the final cycle of least-squares refinement.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. A view of the complex cation of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2 | Z = 4 |
Mr = 745.68 | F(000) = 1388 |
Triclinic, P1 | Dx = 2.214 Mg m−3 |
a = 8.4548 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.4176 (5) Å | Cell parameters from 6027 reflections |
c = 22.6477 (9) Å | θ = 0.9–25.1° |
α = 86.510 (1)° | µ = 6.81 mm−1 |
β = 79.359 (1)° | T = 293 K |
γ = 73.167 (1)° | Prism, orange |
V = 2236.66 (16) Å3 | 0.62 × 0.38 × 0.28 mm |
Siemens SMART CCD diffractometer | 7840 independent reflections |
Radiation source: fine-focus sealed tube | 6151 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ω scans | θmax = 25.1°, θmin = 0.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→9 |
Tmin = 0.057, Tmax = 0.149 | k = −14→14 |
11706 measured reflections | l = −26→26 |
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)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0667P)2 + 20.7333P] where P = (Fo2 + 2Fc2)/3 |
7840 reflections | (Δ/σ)max = 0.001 |
550 parameters | Δρmax = 1.26 e Å−3 |
0 restraints | Δρmin = −2.02 e Å−3 |
[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2 | γ = 73.167 (1)° |
Mr = 745.68 | V = 2236.66 (16) Å3 |
Triclinic, P1 | Z = 4 |
a = 8.4548 (4) Å | Mo Kα radiation |
b = 12.4176 (5) Å | µ = 6.81 mm−1 |
c = 22.6477 (9) Å | T = 293 K |
α = 86.510 (1)° | 0.62 × 0.38 × 0.28 mm |
β = 79.359 (1)° |
Siemens SMART CCD diffractometer | 7840 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 6151 reflections with I > 2σ(I) |
Tmin = 0.057, Tmax = 0.149 | Rint = 0.032 |
11706 measured reflections |
R[F2 > 2σ(F2)] = 0.061 | 0 restraints |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0667P)2 + 20.7333P] where P = (Fo2 + 2Fc2)/3 |
7840 reflections | Δρmax = 1.26 e Å−3 |
550 parameters | Δρmin = −2.02 e Å−3 |
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 | 0.66333 (6) | 0.14111 (4) | 0.13980 (2) | 0.04834 (16) | |
Re2 | −0.26131 (6) | 0.14160 (4) | 0.70347 (2) | 0.05098 (17) | |
Sb1 | 0.13813 (13) | −0.36601 (11) | 0.08256 (6) | 0.0794 (3) | |
Sb2 | 0.21981 (15) | 0.21487 (12) | 0.45634 (6) | 0.0893 (4) | |
Cl1 | −0.5291 (13) | 0.5431 (8) | 0.7271 (4) | 0.179 (3) | |
Cl2 | −0.7327 (12) | 0.6185 (7) | 0.6361 (3) | 0.158 (3) | |
F11 | 0.3322 (18) | −0.3558 (15) | 0.0320 (7) | 0.162 (6) | |
F12 | 0.086 (5) | −0.225 (2) | 0.1029 (16) | 0.38 (2) | |
F13 | 0.210 (5) | −0.5101 (16) | 0.0675 (12) | 0.34 (2) | |
F14 | −0.058 (2) | −0.372 (2) | 0.1294 (9) | 0.260 (13) | |
F15 | 0.055 (2) | −0.347 (3) | 0.0167 (9) | 0.35 (2) | |
F16 | 0.230 (2) | −0.395 (3) | 0.1472 (8) | 0.32 (2) | |
F21 | 0.156 (6) | 0.231 (3) | 0.3924 (16) | 0.44 (3) | |
F22 | 0.405 (3) | 0.247 (2) | 0.4233 (18) | 0.36 (2) | |
F23 | 0.047 (3) | 0.1832 (15) | 0.5027 (14) | 0.289 (17) | |
F24 | 0.320 (8) | 0.170 (3) | 0.5167 (18) | 0.47 (4) | |
F25 | 0.155 (4) | 0.3547 (14) | 0.4765 (16) | 0.38 (2) | |
F26 | 0.296 (3) | 0.0587 (17) | 0.4411 (9) | 0.227 (10) | |
O22 | 0.6503 (16) | −0.1004 (9) | 0.1685 (5) | 0.083 (3) | |
O41 | 0.7876 (15) | 0.1375 (12) | 0.2589 (5) | 0.096 (4) | |
O42 | 1.0275 (12) | 0.0525 (11) | 0.0737 (5) | 0.085 (3) | |
O101 | −0.5184 (16) | 0.0187 (12) | 0.6891 (6) | 0.103 (4) | |
O102 | −0.5296 (13) | 0.3033 (10) | 0.7919 (5) | 0.082 (3) | |
O104 | −0.1884 (16) | −0.0092 (11) | 0.8130 (6) | 0.096 (4) | |
N1 | 0.5493 (12) | 0.1540 (9) | 0.0607 (5) | 0.050 (2) | |
N2 | 0.3971 (12) | 0.2124 (8) | 0.1721 (5) | 0.052 (2) | |
N11 | 0.6605 (13) | 0.3132 (10) | 0.1183 (5) | 0.055 (3) | |
N12 | −0.0560 (15) | 0.0373 (10) | 0.6431 (5) | 0.060 (3) | |
N101 | −0.0861 (13) | 0.2394 (9) | 0.7032 (4) | 0.054 (3) | |
N102 | −0.2890 (13) | 0.2535 (9) | 0.6260 (4) | 0.052 (2) | |
C1 | 0.6597 (17) | 0.4034 (13) | 0.1056 (6) | 0.059 (3) | |
C2 | 0.665 (2) | 0.5166 (12) | 0.0893 (8) | 0.077 (4) | |
H2A | 0.7662 | 0.5143 | 0.0615 | 0.115* | |
H2B | 0.6618 | 0.5566 | 0.1247 | 0.115* | |
H2C | 0.5696 | 0.5543 | 0.0709 | 0.115* | |
C3 | 0.059 (2) | −0.0109 (12) | 0.6136 (7) | 0.065 (4) | |
C4 | 0.214 (2) | −0.0767 (16) | 0.5765 (9) | 0.109 (7) | |
H3A | 0.2035 | −0.0675 | 0.5349 | 0.164* | |
H3B | 0.2348 | −0.1548 | 0.5876 | 0.164* | |
H3C | 0.3067 | −0.0509 | 0.5827 | 0.164* | |
C5 | −0.561 (4) | 0.614 (3) | 0.6639 (11) | 0.156 (11) | |
H5A | −0.4642 | 0.5829 | 0.6332 | 0.188* | |
H5B | −0.5628 | 0.6911 | 0.6702 | 0.188* | |
C11 | 0.6571 (16) | −0.0105 (13) | 0.1584 (6) | 0.058 (3) | |
C21 | 0.3811 (15) | 0.2083 (10) | 0.0681 (5) | 0.049 (3) | |
C22 | 0.2981 (19) | 0.2262 (12) | 0.0206 (7) | 0.068 (4) | |
H22A | 0.1845 | 0.2649 | 0.0261 | 0.082* | |
C23 | 0.382 (2) | 0.1872 (15) | −0.0350 (8) | 0.084 (5) | |
H23A | 0.3253 | 0.1979 | −0.0673 | 0.100* | |
C24 | 0.553 (2) | 0.1316 (13) | −0.0431 (6) | 0.067 (4) | |
H24A | 0.6127 | 0.1043 | −0.0804 | 0.081* | |
C25 | 0.6279 (17) | 0.1188 (12) | 0.0065 (6) | 0.059 (3) | |
H25A | 0.7424 | 0.0828 | 0.0015 | 0.071* | |
C31 | 0.2981 (14) | 0.2407 (11) | 0.1297 (6) | 0.054 (3) | |
C32 | 0.1254 (18) | 0.2923 (13) | 0.1460 (8) | 0.074 (4) | |
H32A | 0.0577 | 0.3123 | 0.1168 | 0.088* | |
C33 | 0.058 (2) | 0.3131 (16) | 0.2052 (9) | 0.093 (6) | |
H33A | −0.0574 | 0.3451 | 0.2164 | 0.111* | |
C34 | 0.157 (2) | 0.2872 (18) | 0.2475 (8) | 0.096 (6) | |
H34A | 0.1119 | 0.3038 | 0.2876 | 0.115* | |
C35 | 0.3281 (17) | 0.2353 (14) | 0.2299 (6) | 0.069 (4) | |
H35A | 0.3963 | 0.2160 | 0.2590 | 0.083* | |
C41 | 0.8922 (18) | 0.0873 (12) | 0.0989 (6) | 0.061 (3) | |
C42 | 0.7439 (17) | 0.1365 (13) | 0.2142 (7) | 0.065 (4) | |
C101 | −0.422 (2) | 0.0632 (15) | 0.6936 (6) | 0.074 (4) | |
C102 | −0.4298 (17) | 0.2423 (13) | 0.7583 (6) | 0.060 (3) | |
C104 | −0.2125 (19) | 0.0471 (14) | 0.7713 (7) | 0.069 (4) | |
C152 | 0.0148 (18) | 0.2259 (13) | 0.7440 (6) | 0.067 (4) | |
H15A | 0.0086 | 0.1728 | 0.7745 | 0.080* | |
C153 | 0.127 (2) | 0.2875 (16) | 0.7425 (8) | 0.087 (5) | |
H15B | 0.1961 | 0.2768 | 0.7713 | 0.104* | |
C154 | 0.135 (2) | 0.3644 (19) | 0.6974 (10) | 0.106 (7) | |
H15C | 0.2108 | 0.4065 | 0.6947 | 0.127* | |
C155 | 0.030 (2) | 0.3805 (14) | 0.6553 (8) | 0.083 (5) | |
H15D | 0.0326 | 0.4342 | 0.6250 | 0.099* | |
C156 | −0.0793 (17) | 0.3156 (11) | 0.6593 (6) | 0.058 (3) | |
C157 | −0.1941 (15) | 0.3255 (11) | 0.6167 (6) | 0.053 (3) | |
C158 | −0.2050 (19) | 0.4009 (14) | 0.5698 (7) | 0.074 (4) | |
H15E | −0.1395 | 0.4506 | 0.5643 | 0.089* | |
C159 | −0.311 (2) | 0.4029 (17) | 0.5316 (8) | 0.090 (5) | |
H15F | −0.3180 | 0.4543 | 0.4999 | 0.108* | |
C160 | −0.408 (2) | 0.3298 (17) | 0.5389 (8) | 0.090 (5) | |
H16A | −0.4797 | 0.3287 | 0.5124 | 0.108* | |
C161 | −0.394 (2) | 0.2599 (15) | 0.5869 (8) | 0.080 (4) | |
H16B | −0.4622 | 0.2121 | 0.5936 | 0.096* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0403 (3) | 0.0546 (3) | 0.0482 (3) | −0.0104 (2) | −0.0082 (2) | 0.0009 (2) |
Re2 | 0.0452 (3) | 0.0570 (3) | 0.0512 (3) | −0.0165 (2) | −0.0065 (2) | −0.0001 (2) |
Sb1 | 0.0547 (6) | 0.0911 (8) | 0.0952 (8) | −0.0215 (5) | −0.0144 (5) | −0.0137 (6) |
Sb2 | 0.0676 (7) | 0.1099 (10) | 0.0914 (8) | −0.0360 (7) | 0.0014 (6) | −0.0018 (7) |
Cl1 | 0.218 (9) | 0.170 (7) | 0.136 (6) | −0.040 (6) | −0.035 (6) | 0.037 (5) |
Cl2 | 0.191 (8) | 0.165 (7) | 0.126 (5) | −0.073 (6) | −0.025 (5) | 0.024 (5) |
F11 | 0.125 (11) | 0.225 (17) | 0.153 (13) | −0.091 (12) | 0.006 (9) | −0.016 (11) |
F12 | 0.51 (5) | 0.16 (2) | 0.40 (4) | −0.13 (3) | 0.21 (4) | −0.12 (2) |
F13 | 0.55 (5) | 0.104 (14) | 0.29 (3) | −0.10 (2) | 0.17 (3) | −0.010 (15) |
F14 | 0.122 (12) | 0.48 (4) | 0.210 (18) | −0.171 (19) | 0.075 (12) | −0.14 (2) |
F15 | 0.080 (10) | 0.75 (6) | 0.159 (16) | 0.03 (2) | −0.047 (10) | −0.06 (3) |
F16 | 0.134 (15) | 0.67 (6) | 0.122 (14) | −0.04 (2) | −0.050 (11) | −0.02 (2) |
F21 | 0.65 (7) | 0.45 (5) | 0.34 (4) | −0.18 (5) | −0.38 (5) | 0.15 (4) |
F22 | 0.144 (17) | 0.31 (3) | 0.56 (5) | −0.086 (19) | 0.15 (3) | 0.03 (3) |
F23 | 0.171 (17) | 0.131 (14) | 0.47 (4) | −0.037 (12) | 0.17 (2) | −0.007 (19) |
F24 | 0.89 (10) | 0.35 (4) | 0.39 (5) | −0.33 (6) | −0.44 (6) | 0.17 (4) |
F25 | 0.38 (4) | 0.070 (10) | 0.57 (5) | −0.072 (15) | 0.27 (4) | −0.040 (18) |
F26 | 0.25 (2) | 0.177 (17) | 0.21 (2) | −0.047 (16) | 0.069 (17) | −0.053 (15) |
O22 | 0.121 (10) | 0.056 (7) | 0.069 (7) | −0.027 (6) | −0.010 (6) | 0.008 (5) |
O41 | 0.088 (8) | 0.141 (11) | 0.069 (7) | −0.033 (8) | −0.031 (6) | −0.012 (7) |
O42 | 0.045 (6) | 0.116 (9) | 0.077 (7) | −0.004 (6) | 0.001 (5) | 0.005 (6) |
O101 | 0.095 (9) | 0.124 (11) | 0.113 (10) | −0.073 (9) | 0.003 (7) | −0.028 (8) |
O102 | 0.066 (6) | 0.094 (8) | 0.083 (7) | −0.028 (6) | 0.016 (6) | −0.031 (6) |
O104 | 0.105 (9) | 0.099 (9) | 0.089 (8) | −0.033 (7) | −0.033 (7) | 0.030 (7) |
N1 | 0.039 (5) | 0.055 (6) | 0.056 (6) | −0.011 (5) | −0.010 (4) | −0.004 (5) |
N2 | 0.042 (5) | 0.044 (6) | 0.067 (7) | −0.010 (4) | −0.003 (5) | 0.001 (5) |
N11 | 0.048 (6) | 0.067 (8) | 0.053 (6) | −0.019 (5) | −0.014 (5) | 0.003 (5) |
N12 | 0.061 (7) | 0.064 (7) | 0.054 (7) | −0.019 (6) | −0.008 (6) | 0.007 (6) |
N101 | 0.050 (6) | 0.069 (7) | 0.050 (6) | −0.030 (5) | −0.010 (5) | 0.011 (5) |
N102 | 0.051 (6) | 0.060 (7) | 0.047 (6) | −0.014 (5) | −0.018 (5) | 0.000 (5) |
C1 | 0.052 (8) | 0.065 (10) | 0.057 (8) | −0.016 (7) | −0.006 (6) | −0.005 (7) |
C2 | 0.077 (10) | 0.056 (9) | 0.097 (12) | −0.023 (8) | −0.012 (9) | 0.001 (8) |
C3 | 0.068 (9) | 0.050 (8) | 0.074 (9) | −0.019 (7) | 0.002 (8) | −0.010 (7) |
C4 | 0.094 (13) | 0.079 (13) | 0.113 (15) | 0.007 (10) | 0.034 (11) | −0.005 (11) |
C5 | 0.15 (2) | 0.17 (3) | 0.109 (19) | 0.00 (2) | 0.015 (17) | 0.011 (17) |
C11 | 0.047 (7) | 0.073 (10) | 0.053 (7) | −0.015 (7) | −0.012 (6) | 0.005 (7) |
C21 | 0.047 (7) | 0.053 (7) | 0.051 (7) | −0.017 (6) | −0.016 (5) | 0.005 (6) |
C22 | 0.067 (9) | 0.060 (9) | 0.078 (10) | −0.012 (7) | −0.023 (8) | −0.004 (7) |
C23 | 0.092 (12) | 0.097 (13) | 0.079 (11) | −0.040 (10) | −0.045 (10) | 0.019 (9) |
C24 | 0.087 (11) | 0.074 (10) | 0.049 (8) | −0.034 (8) | −0.014 (7) | −0.005 (7) |
C25 | 0.056 (8) | 0.066 (9) | 0.048 (7) | −0.010 (6) | 0.002 (6) | −0.013 (6) |
C31 | 0.035 (6) | 0.050 (7) | 0.068 (8) | 0.000 (5) | −0.006 (6) | −0.002 (6) |
C32 | 0.048 (8) | 0.074 (10) | 0.091 (11) | −0.006 (7) | −0.015 (8) | 0.006 (8) |
C33 | 0.047 (9) | 0.100 (14) | 0.112 (15) | −0.003 (9) | 0.010 (9) | −0.012 (11) |
C34 | 0.075 (12) | 0.125 (16) | 0.072 (11) | −0.020 (11) | 0.011 (9) | −0.011 (10) |
C35 | 0.050 (8) | 0.095 (11) | 0.056 (8) | −0.014 (7) | 0.004 (6) | −0.019 (8) |
C41 | 0.056 (8) | 0.071 (9) | 0.058 (8) | −0.017 (7) | −0.013 (7) | 0.003 (7) |
C42 | 0.052 (8) | 0.070 (9) | 0.075 (10) | −0.015 (7) | −0.022 (7) | −0.006 (7) |
C101 | 0.065 (9) | 0.097 (12) | 0.057 (9) | −0.031 (9) | 0.012 (7) | −0.019 (8) |
C102 | 0.055 (8) | 0.073 (9) | 0.062 (8) | −0.036 (7) | −0.009 (7) | 0.002 (7) |
C104 | 0.062 (9) | 0.085 (11) | 0.056 (8) | −0.015 (8) | −0.008 (7) | 0.004 (8) |
C152 | 0.067 (9) | 0.086 (10) | 0.060 (8) | −0.030 (8) | −0.033 (7) | 0.010 (7) |
C153 | 0.090 (12) | 0.113 (14) | 0.080 (11) | −0.054 (11) | −0.038 (9) | 0.012 (10) |
C154 | 0.074 (11) | 0.136 (18) | 0.131 (17) | −0.063 (12) | −0.029 (11) | 0.008 (14) |
C155 | 0.093 (12) | 0.081 (11) | 0.088 (11) | −0.045 (10) | −0.029 (10) | 0.028 (9) |
C156 | 0.055 (8) | 0.059 (8) | 0.065 (8) | −0.028 (6) | −0.002 (6) | −0.001 (7) |
C157 | 0.047 (7) | 0.060 (8) | 0.050 (7) | −0.007 (6) | −0.011 (5) | 0.001 (6) |
C158 | 0.063 (9) | 0.074 (10) | 0.074 (10) | −0.006 (8) | −0.008 (8) | 0.008 (8) |
C159 | 0.087 (12) | 0.098 (14) | 0.080 (11) | −0.011 (11) | −0.034 (10) | 0.019 (10) |
C160 | 0.084 (12) | 0.112 (15) | 0.072 (11) | −0.005 (11) | −0.048 (9) | 0.011 (10) |
C161 | 0.071 (10) | 0.087 (12) | 0.090 (12) | −0.027 (9) | −0.030 (9) | 0.007 (9) |
Re1—C11 | 1.917 (16) | C2—H2A | 0.9600 |
Re1—C42 | 1.922 (15) | C2—H2B | 0.9600 |
Re1—C41 | 1.927 (14) | C2—H2C | 0.9600 |
Re1—N11 | 2.157 (12) | C3—C4 | 1.47 (2) |
Re1—N1 | 2.163 (10) | C4—H3A | 0.9600 |
Re1—N2 | 2.169 (10) | C4—H3B | 0.9600 |
Re2—C102 | 1.907 (16) | C4—H3C | 0.9600 |
Re2—C104 | 1.908 (16) | C5—H5A | 0.9700 |
Re2—C101 | 1.939 (17) | C5—H5B | 0.9700 |
Re2—N12 | 2.145 (12) | C21—C22 | 1.362 (18) |
Re2—N101 | 2.169 (10) | C21—C31 | 1.465 (18) |
Re2—N102 | 2.175 (10) | C22—C23 | 1.37 (2) |
Sb1—F15 | 1.740 (18) | C22—H22A | 0.9300 |
Sb1—F13 | 1.748 (19) | C23—C24 | 1.39 (2) |
Sb1—F12 | 1.75 (2) | C23—H23A | 0.9300 |
Sb1—F16 | 1.753 (18) | C24—C25 | 1.369 (19) |
Sb1—F14 | 1.815 (13) | C24—H24A | 0.9300 |
Sb1—F11 | 1.852 (13) | C25—H25A | 0.9300 |
Sb2—F21 | 1.62 (2) | C31—C32 | 1.402 (18) |
Sb2—F24 | 1.72 (3) | C32—C33 | 1.37 (2) |
Sb2—F25 | 1.726 (18) | C32—H32A | 0.9300 |
Sb2—F22 | 1.754 (18) | C33—C34 | 1.35 (2) |
Sb2—F23 | 1.764 (16) | C33—H33A | 0.9300 |
Sb2—F26 | 1.89 (2) | C34—C35 | 1.40 (2) |
Cl1—C5 | 1.66 (3) | C34—H34A | 0.9300 |
Cl2—C5 | 1.67 (3) | C35—H35A | 0.9300 |
O22—C11 | 1.142 (16) | C152—C153 | 1.38 (2) |
O41—C42 | 1.142 (16) | C152—H15A | 0.9300 |
O42—C41 | 1.150 (16) | C153—C154 | 1.36 (3) |
O101—C101 | 1.128 (18) | C153—H15B | 0.9300 |
O102—C102 | 1.152 (16) | C154—C155 | 1.39 (2) |
O104—C104 | 1.154 (17) | C154—H15C | 0.9300 |
N1—C25 | 1.318 (15) | C155—C156 | 1.38 (2) |
N1—C21 | 1.370 (15) | C155—H15D | 0.9300 |
N2—C35 | 1.341 (16) | C156—C157 | 1.465 (18) |
N2—C31 | 1.354 (16) | C157—C158 | 1.37 (2) |
N11—C1 | 1.138 (17) | C158—C159 | 1.35 (2) |
N12—C3 | 1.107 (17) | C158—H15E | 0.9300 |
N101—C156 | 1.335 (16) | C159—C160 | 1.38 (3) |
N101—C152 | 1.342 (16) | C159—H15F | 0.9300 |
N102—C161 | 1.348 (18) | C160—C161 | 1.35 (2) |
N102—C157 | 1.348 (16) | C160—H16A | 0.9300 |
C1—C2 | 1.44 (2) | C161—H16B | 0.9300 |
C11—Re1—C42 | 86.1 (6) | H2B—C2—H2C | 109.5 |
C11—Re1—C41 | 90.5 (6) | N12—C3—C4 | 178.0 (19) |
C42—Re1—C41 | 89.2 (6) | C3—C4—H3A | 109.5 |
C11—Re1—N11 | 177.8 (5) | C3—C4—H3B | 109.5 |
C42—Re1—N11 | 95.3 (5) | H3A—C4—H3B | 109.5 |
C41—Re1—N11 | 91.3 (5) | C3—C4—H3C | 109.5 |
C11—Re1—N1 | 94.5 (5) | H3A—C4—H3C | 109.5 |
C42—Re1—N1 | 174.6 (5) | H3B—C4—H3C | 109.5 |
C41—Re1—N1 | 96.2 (5) | Cl1—C5—Cl2 | 118.9 (19) |
N11—Re1—N1 | 83.9 (4) | Cl1—C5—H5A | 107.6 |
C11—Re1—N2 | 93.7 (5) | Cl2—C5—H5A | 107.6 |
C42—Re1—N2 | 99.1 (5) | Cl1—C5—H5B | 107.6 |
C41—Re1—N2 | 170.9 (5) | Cl2—C5—H5B | 107.6 |
N11—Re1—N2 | 84.4 (4) | H5A—C5—H5B | 107.0 |
N1—Re1—N2 | 75.5 (4) | O22—C11—Re1 | 178.2 (12) |
C102—Re2—C104 | 86.8 (6) | C22—C21—N1 | 121.0 (12) |
C102—Re2—C101 | 89.9 (6) | C22—C21—C31 | 123.2 (12) |
C104—Re2—C101 | 88.4 (7) | N1—C21—C31 | 115.8 (10) |
C102—Re2—N12 | 174.6 (5) | C21—C22—C23 | 119.9 (14) |
C104—Re2—N12 | 93.4 (5) | C21—C22—H22A | 120.1 |
C101—Re2—N12 | 95.6 (5) | C23—C22—H22A | 120.1 |
C102—Re2—N101 | 91.8 (5) | C22—C23—C24 | 119.8 (14) |
C104—Re2—N101 | 99.0 (6) | C22—C23—H23A | 120.1 |
C101—Re2—N101 | 172.5 (5) | C24—C23—H23A | 120.1 |
N12—Re2—N101 | 82.8 (4) | C25—C24—C23 | 116.9 (14) |
C102—Re2—N102 | 95.3 (5) | C25—C24—H24A | 121.6 |
C104—Re2—N102 | 173.3 (5) | C23—C24—H24A | 121.6 |
C101—Re2—N102 | 98.0 (6) | N1—C25—C24 | 124.5 (13) |
N12—Re2—N102 | 83.9 (4) | N1—C25—H25A | 117.8 |
N101—Re2—N102 | 74.6 (4) | C24—C25—H25A | 117.8 |
F15—Sb1—F13 | 88.0 (17) | N2—C31—C32 | 120.4 (13) |
F15—Sb1—F12 | 99 (2) | N2—C31—C21 | 115.9 (10) |
F13—Sb1—F12 | 173 (2) | C32—C31—C21 | 123.6 (13) |
F15—Sb1—F16 | 175.8 (17) | C33—C32—C31 | 119.4 (15) |
F13—Sb1—F16 | 87.9 (18) | C33—C32—H32A | 120.3 |
F12—Sb1—F16 | 85.5 (18) | C31—C32—H32A | 120.3 |
F15—Sb1—F14 | 93.4 (10) | C34—C33—C32 | 120.3 (15) |
F13—Sb1—F14 | 94.9 (13) | C34—C33—H33A | 119.9 |
F12—Sb1—F14 | 87.7 (13) | C32—C33—H33A | 119.9 |
F16—Sb1—F14 | 87.8 (10) | C33—C34—C35 | 119.0 (16) |
F15—Sb1—F11 | 84.0 (9) | C33—C34—H34A | 120.5 |
F13—Sb1—F11 | 86.1 (10) | C35—C34—H34A | 120.5 |
F12—Sb1—F11 | 91.7 (11) | N2—C35—C34 | 121.8 (15) |
F16—Sb1—F11 | 94.8 (9) | N2—C35—H35A | 119.1 |
F14—Sb1—F11 | 177.2 (10) | C34—C35—H35A | 119.1 |
F21—Sb2—F24 | 167 (2) | O42—C41—Re1 | 177.8 (14) |
F21—Sb2—F25 | 97 (2) | O41—C42—Re1 | 177.5 (14) |
F24—Sb2—F25 | 95 (2) | O101—C101—Re2 | 178.3 (13) |
F21—Sb2—F22 | 91 (2) | O102—C102—Re2 | 178.9 (12) |
F24—Sb2—F22 | 85 (2) | O104—C104—Re2 | 177.8 (14) |
F25—Sb2—F22 | 83.1 (13) | N101—C152—C153 | 122.6 (14) |
F21—Sb2—F23 | 100 (2) | N101—C152—H15A | 118.7 |
F24—Sb2—F23 | 85 (2) | C153—C152—H15A | 118.7 |
F25—Sb2—F23 | 93.8 (9) | C154—C153—C152 | 117.7 (15) |
F22—Sb2—F23 | 168.9 (18) | C154—C153—H15B | 121.1 |
F21—Sb2—F26 | 87.6 (17) | C152—C153—H15B | 121.1 |
F24—Sb2—F26 | 80.4 (16) | C153—C154—C155 | 120.3 (16) |
F25—Sb2—F26 | 175.0 (16) | C153—C154—H15C | 119.8 |
F22—Sb2—F26 | 97.5 (12) | C155—C154—H15C | 119.8 |
F23—Sb2—F26 | 84.7 (9) | C156—C155—C154 | 118.9 (15) |
C25—N1—C21 | 118.0 (11) | C156—C155—H15D | 120.6 |
C25—N1—Re1 | 126.0 (9) | C154—C155—H15D | 120.6 |
C21—N1—Re1 | 115.9 (8) | N101—C156—C155 | 121.0 (13) |
C35—N2—C31 | 119.2 (11) | N101—C156—C157 | 116.1 (11) |
C35—N2—Re1 | 124.5 (9) | C155—C156—C157 | 123.0 (13) |
C31—N2—Re1 | 116.2 (8) | N102—C157—C158 | 121.2 (13) |
C1—N11—Re1 | 178.5 (11) | N102—C157—C156 | 115.4 (11) |
C3—N12—Re2 | 173.2 (12) | C158—C157—C156 | 123.4 (13) |
C156—N101—C152 | 119.4 (11) | C159—C158—C157 | 119.8 (17) |
C156—N101—Re2 | 117.2 (8) | C159—C158—H15E | 120.1 |
C152—N101—Re2 | 123.4 (9) | C157—C158—H15E | 120.1 |
C161—N102—C157 | 116.5 (12) | C158—C159—C160 | 120.9 (17) |
C161—N102—Re2 | 126.7 (10) | C158—C159—H15F | 119.5 |
C157—N102—Re2 | 116.8 (8) | C160—C159—H15F | 119.5 |
N11—C1—C2 | 178.1 (15) | C161—C160—C159 | 115.9 (15) |
C1—C2—H2A | 109.5 | C161—C160—H16A | 122.1 |
C1—C2—H2B | 109.5 | C159—C160—H16A | 122.1 |
H2A—C2—H2B | 109.5 | N102—C161—C160 | 125.6 (16) |
C1—C2—H2C | 109.5 | N102—C161—H16B | 117.2 |
H2A—C2—H2C | 109.5 | C160—C161—H16B | 117.2 |
Experimental details
Crystal data | |
Chemical formula | [Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2 |
Mr | 745.68 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.4548 (4), 12.4176 (5), 22.6477 (9) |
α, β, γ (°) | 86.510 (1), 79.359 (1), 73.167 (1) |
V (Å3) | 2236.66 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.81 |
Crystal size (mm) | 0.62 × 0.38 × 0.28 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.057, 0.149 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11706, 7840, 6151 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.061, 0.161, 1.13 |
No. of reflections | 7840 |
No. of parameters | 550 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0667P)2 + 20.7333P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.26, −2.02 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), XPREP (Siemens, 1994), SHELXTL (Siemens, 1994), SHELXTL.
Re1—C11 | 1.917 (16) | Re2—C102 | 1.907 (16) |
Re1—C42 | 1.922 (15) | Re2—C104 | 1.908 (16) |
Re1—C41 | 1.927 (14) | Re2—C101 | 1.939 (17) |
Re1—N11 | 2.157 (12) | Re2—N12 | 2.145 (12) |
Re1—N1 | 2.163 (10) | Re2—N101 | 2.169 (10) |
Re1—N2 | 2.169 (10) | Re2—N102 | 2.175 (10) |
Rhenium(I)–tricarbonyl–diimine systems are of increasing interest because of their rich photoluminescent properties and the possible effect in electrochemically promoted reductions of carbon dioxide (Yam et al., 1997; Gibson et al., 1998). Herein is described a crystal structure of a rhenium(I) complex, [Re(CO)3(C10H8N2)2(CH3CN)]SbF6·0.5CH2Cl2, (I), which was prepared according to literature methods (Fredericks et al., 1979) except for using AgSbF6 to remove the chlorine ligand.
The asymmetric unit of (I) contains two similar units. A perspective drawing of the complex cation of (I) with the atomic numbering scheme is depicted in Fig. 1 and selected bonding parameters are presented in Table 1.
Three carbonyl ligands at each Re atom are arranged in a facial configuration. Each Re atom adopts a slightly distorted octahedral geormetry with the C11—Re1—N11 and C101—Re2—N101 bond angles being 177.8 (5) and 172.5 (5)°, respectively. The N1—Re1—N2 [75.5 (4)°] and N101—Re2—N102 [74.6 (4)°] bond angles are far from 90° due to the bite angle of the chelating bipyridyl (byp) ligand (Yam et al., 1995, 1996). The average bond distances of Re—N [2.163 (11) Å] and Re—C [1.920 (16) Å] are found to be comparable to previously determined rhenium(I)–tricarbonyl–diimine structures (Chen et al., 1989; Yam et al., 1997; Hevia et al., 2002).