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[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2 was isolated from the reaction between [Re(bpy)(CO)3Cl], where bpy = 2,2'-bipyridine, and AgSbF6 in aceto­nitrile. The rhenium atom has a distorted octahedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301095X/om6143sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301095X/om6143Isup2.hkl
Contains datablock I

CCDC reference: 217361

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.023 Å
  • R factor = 0.061
  • wR factor = 0.161
  • Data-to-parameter ratio = 14.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

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).

Experimental top

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.

Refinement top

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.

Computing details top

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.

Figures top
[Figure 1] Fig. 1. A view of the complex cation of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.
(2,2'-Bipyridine-κ2N,N')tricarbonyl(acetonitrile-κN)rhenium(I) hexafluoroantimonate dichloromethane hemisolvate top
Crystal data top
[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2Z = 4
Mr = 745.68F(000) = 1388
Triclinic, P1Dx = 2.214 Mg m3
a = 8.4548 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.4176 (5) ÅCell parameters from 6027 reflections
c = 22.6477 (9) Åθ = 0.9–25.1°
α = 86.510 (1)°µ = 6.81 mm1
β = 79.359 (1)°T = 293 K
γ = 73.167 (1)°Prism, orange
V = 2236.66 (16) Å30.62 × 0.38 × 0.28 mm
Data collection top
Siemens SMART CCD
diffractometer
7840 independent reflections
Radiation source: fine-focus sealed tube6151 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scansθmax = 25.1°, θmin = 0.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 109
Tmin = 0.057, Tmax = 0.149k = 1414
11706 measured reflectionsl = 2626
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)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.161H-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 parametersΔρmax = 1.26 e Å3
0 restraintsΔρmin = 2.02 e Å3
Crystal data top
[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2γ = 73.167 (1)°
Mr = 745.68V = 2236.66 (16) Å3
Triclinic, P1Z = 4
a = 8.4548 (4) ÅMo Kα radiation
b = 12.4176 (5) ŵ = 6.81 mm1
c = 22.6477 (9) ÅT = 293 K
α = 86.510 (1)°0.62 × 0.38 × 0.28 mm
β = 79.359 (1)°
Data collection top
Siemens SMART CCD
diffractometer
7840 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
6151 reflections with I > 2σ(I)
Tmin = 0.057, Tmax = 0.149Rint = 0.032
11706 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0610 restraints
wR(F2) = 0.161H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0667P)2 + 20.7333P]
where P = (Fo2 + 2Fc2)/3
7840 reflectionsΔρmax = 1.26 e Å3
550 parametersΔρmin = 2.02 e Å3
Special details top

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
Re10.66333 (6)0.14111 (4)0.13980 (2)0.04834 (16)
Re20.26131 (6)0.14160 (4)0.70347 (2)0.05098 (17)
Sb10.13813 (13)0.36601 (11)0.08256 (6)0.0794 (3)
Sb20.21981 (15)0.21487 (12)0.45634 (6)0.0893 (4)
Cl10.5291 (13)0.5431 (8)0.7271 (4)0.179 (3)
Cl20.7327 (12)0.6185 (7)0.6361 (3)0.158 (3)
F110.3322 (18)0.3558 (15)0.0320 (7)0.162 (6)
F120.086 (5)0.225 (2)0.1029 (16)0.38 (2)
F130.210 (5)0.5101 (16)0.0675 (12)0.34 (2)
F140.058 (2)0.372 (2)0.1294 (9)0.260 (13)
F150.055 (2)0.347 (3)0.0167 (9)0.35 (2)
F160.230 (2)0.395 (3)0.1472 (8)0.32 (2)
F210.156 (6)0.231 (3)0.3924 (16)0.44 (3)
F220.405 (3)0.247 (2)0.4233 (18)0.36 (2)
F230.047 (3)0.1832 (15)0.5027 (14)0.289 (17)
F240.320 (8)0.170 (3)0.5167 (18)0.47 (4)
F250.155 (4)0.3547 (14)0.4765 (16)0.38 (2)
F260.296 (3)0.0587 (17)0.4411 (9)0.227 (10)
O220.6503 (16)0.1004 (9)0.1685 (5)0.083 (3)
O410.7876 (15)0.1375 (12)0.2589 (5)0.096 (4)
O421.0275 (12)0.0525 (11)0.0737 (5)0.085 (3)
O1010.5184 (16)0.0187 (12)0.6891 (6)0.103 (4)
O1020.5296 (13)0.3033 (10)0.7919 (5)0.082 (3)
O1040.1884 (16)0.0092 (11)0.8130 (6)0.096 (4)
N10.5493 (12)0.1540 (9)0.0607 (5)0.050 (2)
N20.3971 (12)0.2124 (8)0.1721 (5)0.052 (2)
N110.6605 (13)0.3132 (10)0.1183 (5)0.055 (3)
N120.0560 (15)0.0373 (10)0.6431 (5)0.060 (3)
N1010.0861 (13)0.2394 (9)0.7032 (4)0.054 (3)
N1020.2890 (13)0.2535 (9)0.6260 (4)0.052 (2)
C10.6597 (17)0.4034 (13)0.1056 (6)0.059 (3)
C20.665 (2)0.5166 (12)0.0893 (8)0.077 (4)
H2A0.76620.51430.06150.115*
H2B0.66180.55660.12470.115*
H2C0.56960.55430.07090.115*
C30.059 (2)0.0109 (12)0.6136 (7)0.065 (4)
C40.214 (2)0.0767 (16)0.5765 (9)0.109 (7)
H3A0.20350.06750.53490.164*
H3B0.23480.15480.58760.164*
H3C0.30670.05090.58270.164*
C50.561 (4)0.614 (3)0.6639 (11)0.156 (11)
H5A0.46420.58290.63320.188*
H5B0.56280.69110.67020.188*
C110.6571 (16)0.0105 (13)0.1584 (6)0.058 (3)
C210.3811 (15)0.2083 (10)0.0681 (5)0.049 (3)
C220.2981 (19)0.2262 (12)0.0206 (7)0.068 (4)
H22A0.18450.26490.02610.082*
C230.382 (2)0.1872 (15)0.0350 (8)0.084 (5)
H23A0.32530.19790.06730.100*
C240.553 (2)0.1316 (13)0.0431 (6)0.067 (4)
H24A0.61270.10430.08040.081*
C250.6279 (17)0.1188 (12)0.0065 (6)0.059 (3)
H25A0.74240.08280.00150.071*
C310.2981 (14)0.2407 (11)0.1297 (6)0.054 (3)
C320.1254 (18)0.2923 (13)0.1460 (8)0.074 (4)
H32A0.05770.31230.11680.088*
C330.058 (2)0.3131 (16)0.2052 (9)0.093 (6)
H33A0.05740.34510.21640.111*
C340.157 (2)0.2872 (18)0.2475 (8)0.096 (6)
H34A0.11190.30380.28760.115*
C350.3281 (17)0.2353 (14)0.2299 (6)0.069 (4)
H35A0.39630.21600.25900.083*
C410.8922 (18)0.0873 (12)0.0989 (6)0.061 (3)
C420.7439 (17)0.1365 (13)0.2142 (7)0.065 (4)
C1010.422 (2)0.0632 (15)0.6936 (6)0.074 (4)
C1020.4298 (17)0.2423 (13)0.7583 (6)0.060 (3)
C1040.2125 (19)0.0471 (14)0.7713 (7)0.069 (4)
C1520.0148 (18)0.2259 (13)0.7440 (6)0.067 (4)
H15A0.00860.17280.77450.080*
C1530.127 (2)0.2875 (16)0.7425 (8)0.087 (5)
H15B0.19610.27680.77130.104*
C1540.135 (2)0.3644 (19)0.6974 (10)0.106 (7)
H15C0.21080.40650.69470.127*
C1550.030 (2)0.3805 (14)0.6553 (8)0.083 (5)
H15D0.03260.43420.62500.099*
C1560.0793 (17)0.3156 (11)0.6593 (6)0.058 (3)
C1570.1941 (15)0.3255 (11)0.6167 (6)0.053 (3)
C1580.2050 (19)0.4009 (14)0.5698 (7)0.074 (4)
H15E0.13950.45060.56430.089*
C1590.311 (2)0.4029 (17)0.5316 (8)0.090 (5)
H15F0.31800.45430.49990.108*
C1600.408 (2)0.3298 (17)0.5389 (8)0.090 (5)
H16A0.47970.32870.51240.108*
C1610.394 (2)0.2599 (15)0.5869 (8)0.080 (4)
H16B0.46220.21210.59360.096*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.0403 (3)0.0546 (3)0.0482 (3)0.0104 (2)0.0082 (2)0.0009 (2)
Re20.0452 (3)0.0570 (3)0.0512 (3)0.0165 (2)0.0065 (2)0.0001 (2)
Sb10.0547 (6)0.0911 (8)0.0952 (8)0.0215 (5)0.0144 (5)0.0137 (6)
Sb20.0676 (7)0.1099 (10)0.0914 (8)0.0360 (7)0.0014 (6)0.0018 (7)
Cl10.218 (9)0.170 (7)0.136 (6)0.040 (6)0.035 (6)0.037 (5)
Cl20.191 (8)0.165 (7)0.126 (5)0.073 (6)0.025 (5)0.024 (5)
F110.125 (11)0.225 (17)0.153 (13)0.091 (12)0.006 (9)0.016 (11)
F120.51 (5)0.16 (2)0.40 (4)0.13 (3)0.21 (4)0.12 (2)
F130.55 (5)0.104 (14)0.29 (3)0.10 (2)0.17 (3)0.010 (15)
F140.122 (12)0.48 (4)0.210 (18)0.171 (19)0.075 (12)0.14 (2)
F150.080 (10)0.75 (6)0.159 (16)0.03 (2)0.047 (10)0.06 (3)
F160.134 (15)0.67 (6)0.122 (14)0.04 (2)0.050 (11)0.02 (2)
F210.65 (7)0.45 (5)0.34 (4)0.18 (5)0.38 (5)0.15 (4)
F220.144 (17)0.31 (3)0.56 (5)0.086 (19)0.15 (3)0.03 (3)
F230.171 (17)0.131 (14)0.47 (4)0.037 (12)0.17 (2)0.007 (19)
F240.89 (10)0.35 (4)0.39 (5)0.33 (6)0.44 (6)0.17 (4)
F250.38 (4)0.070 (10)0.57 (5)0.072 (15)0.27 (4)0.040 (18)
F260.25 (2)0.177 (17)0.21 (2)0.047 (16)0.069 (17)0.053 (15)
O220.121 (10)0.056 (7)0.069 (7)0.027 (6)0.010 (6)0.008 (5)
O410.088 (8)0.141 (11)0.069 (7)0.033 (8)0.031 (6)0.012 (7)
O420.045 (6)0.116 (9)0.077 (7)0.004 (6)0.001 (5)0.005 (6)
O1010.095 (9)0.124 (11)0.113 (10)0.073 (9)0.003 (7)0.028 (8)
O1020.066 (6)0.094 (8)0.083 (7)0.028 (6)0.016 (6)0.031 (6)
O1040.105 (9)0.099 (9)0.089 (8)0.033 (7)0.033 (7)0.030 (7)
N10.039 (5)0.055 (6)0.056 (6)0.011 (5)0.010 (4)0.004 (5)
N20.042 (5)0.044 (6)0.067 (7)0.010 (4)0.003 (5)0.001 (5)
N110.048 (6)0.067 (8)0.053 (6)0.019 (5)0.014 (5)0.003 (5)
N120.061 (7)0.064 (7)0.054 (7)0.019 (6)0.008 (6)0.007 (6)
N1010.050 (6)0.069 (7)0.050 (6)0.030 (5)0.010 (5)0.011 (5)
N1020.051 (6)0.060 (7)0.047 (6)0.014 (5)0.018 (5)0.000 (5)
C10.052 (8)0.065 (10)0.057 (8)0.016 (7)0.006 (6)0.005 (7)
C20.077 (10)0.056 (9)0.097 (12)0.023 (8)0.012 (9)0.001 (8)
C30.068 (9)0.050 (8)0.074 (9)0.019 (7)0.002 (8)0.010 (7)
C40.094 (13)0.079 (13)0.113 (15)0.007 (10)0.034 (11)0.005 (11)
C50.15 (2)0.17 (3)0.109 (19)0.00 (2)0.015 (17)0.011 (17)
C110.047 (7)0.073 (10)0.053 (7)0.015 (7)0.012 (6)0.005 (7)
C210.047 (7)0.053 (7)0.051 (7)0.017 (6)0.016 (5)0.005 (6)
C220.067 (9)0.060 (9)0.078 (10)0.012 (7)0.023 (8)0.004 (7)
C230.092 (12)0.097 (13)0.079 (11)0.040 (10)0.045 (10)0.019 (9)
C240.087 (11)0.074 (10)0.049 (8)0.034 (8)0.014 (7)0.005 (7)
C250.056 (8)0.066 (9)0.048 (7)0.010 (6)0.002 (6)0.013 (6)
C310.035 (6)0.050 (7)0.068 (8)0.000 (5)0.006 (6)0.002 (6)
C320.048 (8)0.074 (10)0.091 (11)0.006 (7)0.015 (8)0.006 (8)
C330.047 (9)0.100 (14)0.112 (15)0.003 (9)0.010 (9)0.012 (11)
C340.075 (12)0.125 (16)0.072 (11)0.020 (11)0.011 (9)0.011 (10)
C350.050 (8)0.095 (11)0.056 (8)0.014 (7)0.004 (6)0.019 (8)
C410.056 (8)0.071 (9)0.058 (8)0.017 (7)0.013 (7)0.003 (7)
C420.052 (8)0.070 (9)0.075 (10)0.015 (7)0.022 (7)0.006 (7)
C1010.065 (9)0.097 (12)0.057 (9)0.031 (9)0.012 (7)0.019 (8)
C1020.055 (8)0.073 (9)0.062 (8)0.036 (7)0.009 (7)0.002 (7)
C1040.062 (9)0.085 (11)0.056 (8)0.015 (8)0.008 (7)0.004 (8)
C1520.067 (9)0.086 (10)0.060 (8)0.030 (8)0.033 (7)0.010 (7)
C1530.090 (12)0.113 (14)0.080 (11)0.054 (11)0.038 (9)0.012 (10)
C1540.074 (11)0.136 (18)0.131 (17)0.063 (12)0.029 (11)0.008 (14)
C1550.093 (12)0.081 (11)0.088 (11)0.045 (10)0.029 (10)0.028 (9)
C1560.055 (8)0.059 (8)0.065 (8)0.028 (6)0.002 (6)0.001 (7)
C1570.047 (7)0.060 (8)0.050 (7)0.007 (6)0.011 (5)0.001 (6)
C1580.063 (9)0.074 (10)0.074 (10)0.006 (8)0.008 (8)0.008 (8)
C1590.087 (12)0.098 (14)0.080 (11)0.011 (11)0.034 (10)0.019 (10)
C1600.084 (12)0.112 (15)0.072 (11)0.005 (11)0.048 (9)0.011 (10)
C1610.071 (10)0.087 (12)0.090 (12)0.027 (9)0.030 (9)0.007 (9)
Geometric parameters (Å, º) top
Re1—C111.917 (16)C2—H2A0.9600
Re1—C421.922 (15)C2—H2B0.9600
Re1—C411.927 (14)C2—H2C0.9600
Re1—N112.157 (12)C3—C41.47 (2)
Re1—N12.163 (10)C4—H3A0.9600
Re1—N22.169 (10)C4—H3B0.9600
Re2—C1021.907 (16)C4—H3C0.9600
Re2—C1041.908 (16)C5—H5A0.9700
Re2—C1011.939 (17)C5—H5B0.9700
Re2—N122.145 (12)C21—C221.362 (18)
Re2—N1012.169 (10)C21—C311.465 (18)
Re2—N1022.175 (10)C22—C231.37 (2)
Sb1—F151.740 (18)C22—H22A0.9300
Sb1—F131.748 (19)C23—C241.39 (2)
Sb1—F121.75 (2)C23—H23A0.9300
Sb1—F161.753 (18)C24—C251.369 (19)
Sb1—F141.815 (13)C24—H24A0.9300
Sb1—F111.852 (13)C25—H25A0.9300
Sb2—F211.62 (2)C31—C321.402 (18)
Sb2—F241.72 (3)C32—C331.37 (2)
Sb2—F251.726 (18)C32—H32A0.9300
Sb2—F221.754 (18)C33—C341.35 (2)
Sb2—F231.764 (16)C33—H33A0.9300
Sb2—F261.89 (2)C34—C351.40 (2)
Cl1—C51.66 (3)C34—H34A0.9300
Cl2—C51.67 (3)C35—H35A0.9300
O22—C111.142 (16)C152—C1531.38 (2)
O41—C421.142 (16)C152—H15A0.9300
O42—C411.150 (16)C153—C1541.36 (3)
O101—C1011.128 (18)C153—H15B0.9300
O102—C1021.152 (16)C154—C1551.39 (2)
O104—C1041.154 (17)C154—H15C0.9300
N1—C251.318 (15)C155—C1561.38 (2)
N1—C211.370 (15)C155—H15D0.9300
N2—C351.341 (16)C156—C1571.465 (18)
N2—C311.354 (16)C157—C1581.37 (2)
N11—C11.138 (17)C158—C1591.35 (2)
N12—C31.107 (17)C158—H15E0.9300
N101—C1561.335 (16)C159—C1601.38 (3)
N101—C1521.342 (16)C159—H15F0.9300
N102—C1611.348 (18)C160—C1611.35 (2)
N102—C1571.348 (16)C160—H16A0.9300
C1—C21.44 (2)C161—H16B0.9300
C11—Re1—C4286.1 (6)H2B—C2—H2C109.5
C11—Re1—C4190.5 (6)N12—C3—C4178.0 (19)
C42—Re1—C4189.2 (6)C3—C4—H3A109.5
C11—Re1—N11177.8 (5)C3—C4—H3B109.5
C42—Re1—N1195.3 (5)H3A—C4—H3B109.5
C41—Re1—N1191.3 (5)C3—C4—H3C109.5
C11—Re1—N194.5 (5)H3A—C4—H3C109.5
C42—Re1—N1174.6 (5)H3B—C4—H3C109.5
C41—Re1—N196.2 (5)Cl1—C5—Cl2118.9 (19)
N11—Re1—N183.9 (4)Cl1—C5—H5A107.6
C11—Re1—N293.7 (5)Cl2—C5—H5A107.6
C42—Re1—N299.1 (5)Cl1—C5—H5B107.6
C41—Re1—N2170.9 (5)Cl2—C5—H5B107.6
N11—Re1—N284.4 (4)H5A—C5—H5B107.0
N1—Re1—N275.5 (4)O22—C11—Re1178.2 (12)
C102—Re2—C10486.8 (6)C22—C21—N1121.0 (12)
C102—Re2—C10189.9 (6)C22—C21—C31123.2 (12)
C104—Re2—C10188.4 (7)N1—C21—C31115.8 (10)
C102—Re2—N12174.6 (5)C21—C22—C23119.9 (14)
C104—Re2—N1293.4 (5)C21—C22—H22A120.1
C101—Re2—N1295.6 (5)C23—C22—H22A120.1
C102—Re2—N10191.8 (5)C22—C23—C24119.8 (14)
C104—Re2—N10199.0 (6)C22—C23—H23A120.1
C101—Re2—N101172.5 (5)C24—C23—H23A120.1
N12—Re2—N10182.8 (4)C25—C24—C23116.9 (14)
C102—Re2—N10295.3 (5)C25—C24—H24A121.6
C104—Re2—N102173.3 (5)C23—C24—H24A121.6
C101—Re2—N10298.0 (6)N1—C25—C24124.5 (13)
N12—Re2—N10283.9 (4)N1—C25—H25A117.8
N101—Re2—N10274.6 (4)C24—C25—H25A117.8
F15—Sb1—F1388.0 (17)N2—C31—C32120.4 (13)
F15—Sb1—F1299 (2)N2—C31—C21115.9 (10)
F13—Sb1—F12173 (2)C32—C31—C21123.6 (13)
F15—Sb1—F16175.8 (17)C33—C32—C31119.4 (15)
F13—Sb1—F1687.9 (18)C33—C32—H32A120.3
F12—Sb1—F1685.5 (18)C31—C32—H32A120.3
F15—Sb1—F1493.4 (10)C34—C33—C32120.3 (15)
F13—Sb1—F1494.9 (13)C34—C33—H33A119.9
F12—Sb1—F1487.7 (13)C32—C33—H33A119.9
F16—Sb1—F1487.8 (10)C33—C34—C35119.0 (16)
F15—Sb1—F1184.0 (9)C33—C34—H34A120.5
F13—Sb1—F1186.1 (10)C35—C34—H34A120.5
F12—Sb1—F1191.7 (11)N2—C35—C34121.8 (15)
F16—Sb1—F1194.8 (9)N2—C35—H35A119.1
F14—Sb1—F11177.2 (10)C34—C35—H35A119.1
F21—Sb2—F24167 (2)O42—C41—Re1177.8 (14)
F21—Sb2—F2597 (2)O41—C42—Re1177.5 (14)
F24—Sb2—F2595 (2)O101—C101—Re2178.3 (13)
F21—Sb2—F2291 (2)O102—C102—Re2178.9 (12)
F24—Sb2—F2285 (2)O104—C104—Re2177.8 (14)
F25—Sb2—F2283.1 (13)N101—C152—C153122.6 (14)
F21—Sb2—F23100 (2)N101—C152—H15A118.7
F24—Sb2—F2385 (2)C153—C152—H15A118.7
F25—Sb2—F2393.8 (9)C154—C153—C152117.7 (15)
F22—Sb2—F23168.9 (18)C154—C153—H15B121.1
F21—Sb2—F2687.6 (17)C152—C153—H15B121.1
F24—Sb2—F2680.4 (16)C153—C154—C155120.3 (16)
F25—Sb2—F26175.0 (16)C153—C154—H15C119.8
F22—Sb2—F2697.5 (12)C155—C154—H15C119.8
F23—Sb2—F2684.7 (9)C156—C155—C154118.9 (15)
C25—N1—C21118.0 (11)C156—C155—H15D120.6
C25—N1—Re1126.0 (9)C154—C155—H15D120.6
C21—N1—Re1115.9 (8)N101—C156—C155121.0 (13)
C35—N2—C31119.2 (11)N101—C156—C157116.1 (11)
C35—N2—Re1124.5 (9)C155—C156—C157123.0 (13)
C31—N2—Re1116.2 (8)N102—C157—C158121.2 (13)
C1—N11—Re1178.5 (11)N102—C157—C156115.4 (11)
C3—N12—Re2173.2 (12)C158—C157—C156123.4 (13)
C156—N101—C152119.4 (11)C159—C158—C157119.8 (17)
C156—N101—Re2117.2 (8)C159—C158—H15E120.1
C152—N101—Re2123.4 (9)C157—C158—H15E120.1
C161—N102—C157116.5 (12)C158—C159—C160120.9 (17)
C161—N102—Re2126.7 (10)C158—C159—H15F119.5
C157—N102—Re2116.8 (8)C160—C159—H15F119.5
N11—C1—C2178.1 (15)C161—C160—C159115.9 (15)
C1—C2—H2A109.5C161—C160—H16A122.1
C1—C2—H2B109.5C159—C160—H16A122.1
H2A—C2—H2B109.5N102—C161—C160125.6 (16)
C1—C2—H2C109.5N102—C161—H16B117.2
H2A—C2—H2C109.5C160—C161—H16B117.2

Experimental details

Crystal data
Chemical formula[Re(C2H3N)(C10H8N2)2(CO)3][SbF6]·0.5CH2Cl2
Mr745.68
Crystal system, space groupTriclinic, 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)
V3)2236.66 (16)
Z4
Radiation typeMo Kα
µ (mm1)6.81
Crystal size (mm)0.62 × 0.38 × 0.28
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.057, 0.149
No. of measured, independent and
observed [I > 2σ(I)] reflections
11706, 7840, 6151
Rint0.032
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.061, 0.161, 1.13
No. of reflections7840
No. of parameters550
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0667P)2 + 20.7333P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.26, 2.02

Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), XPREP (Siemens, 1994), SHELXTL (Siemens, 1994), SHELXTL.

Selected bond lengths (Å) top
Re1—C111.917 (16)Re2—C1021.907 (16)
Re1—C421.922 (15)Re2—C1041.908 (16)
Re1—C411.927 (14)Re2—C1011.939 (17)
Re1—N112.157 (12)Re2—N122.145 (12)
Re1—N12.163 (10)Re2—N1012.169 (10)
Re1—N22.169 (10)Re2—N1022.175 (10)
 

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