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Acta Cryst. (2013). E69, m547    [ doi:10.1107/S1600536813025300 ]

Bis([eta]2-ethylene)([eta]5-indenyl)iridium(I)

J. S. Merola

Abstract top

The asymmetric unit of the title compound, [Ir(C9H7)(C2H4)2], consists of two independent molecules. The bonding between iridium and the five-membered ring of the indenyl ligand shows the usual asymmetry associated with the typical ring slippage responsible for the enhanced activity of indenyl metal compounds when compared with the analogous cyclopentadienyl metal compound. There are three short Ir-C bonds of 2.210 (3), 2.190 (4) and 2.220 (3) Å and two long Ir-C bonds to the C atoms that are part of the fused six-membered ring of 2.349 (4) and 2.366 (3) Å for one of the independent molecules [2.208 (4), 2.222 (3), 2.197 (4) Å for the short distances and 2.371 (3) and 2.358 (3) Å for the long distances in the second molecule]. This results in both indenyl ligands being slightly kinked, with dihedral angles of 6.8 (4)° and 6.5 (4)°.

Comment top

The indenyl ligand has been shown to be very flexible in terms of its coordination to metals. An increased reactivity that is displayed by indenyl metal complexes compared with cyclopentadienyl complexes has been dubbed the "indenyl effect". The effect was first described by Mawby's group (Hart-Davis et al., 1970) and was further quantified by Basolo's group (Rerek et al., 1983) We have previously reported on the synthesis and structure of η3-indenyliridium complexes formed by reaction of an η5-indenyliridiumbis(olefin) complex and small phosphine ligands such as PMe3 or PhPMe2 (Merola et al., 1986). The smallest olefin complex of indenyl iridium, (η5-Indenyl)bis(η2-ethylene)iridium(I), 1, is the subject of this report. The thermal ellipsoid plot for both independent molecules of 1 is shown in figure 1. The most interesting aspects of the bonding are highlighted in table 1 showing the three short and two long bond distances of the "slipped" indenyl rings.

Figure 2 shows the "fold" of the indenyl ligand which imparts non-planarity of the 6-membered ring from the 5-membered ring. The angle between the planes defined by C1, C2 and C9 and that defined by C3, C8, C7, C4, C5 and C6 is 6.5 (4)° and 6.8 (4)° for the "A" and "B" molecules.

Related literature top

For X-ray crystal structures of the analogous rhodium complex, see: CCDC:576585 (Marder et al., 1987); CCDC:567925 (Mlekuz et al., 1986). For a variable temperature NMR study of the title compound, see: Szajek et al. (1991). The structure of an η3-indenyliridium complex can be found in CCDC:563532 (Merola et al., 1986). For seminal discussions on the "indenyl effect" see: Hart-Davis et al. (1970); Rerek et al. (1983). The synthesis of [Ir(C2H2)2Cl]2 can be found in Herde et al. (1974).

Experimental top

[Ir(C2H2)2Cl]2 was synthesized by the reaction between [Ir(C8H14)2IrCl]2 and ethylene (Herde et al., 1974). The title compound was prepared by the reaction between lithium indenide and [Ir(C2H2)2Cl]2 in anhydrous THF. Crystals of the title compound were grown by the slow evaporation of a pentane solution. The title compound has also been reported previously prepared by this same method (Szajek et al., 1991).

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. Hydrogen atoms were found in difference maps and refined using a riding model with C-H distances of 0.93 Å (Cindenyl) and 0.97 Å (Cethylene). Uiso(H) values were set to 1.2Ueq of the attached carbon atom.

Computing details top

Data collection: CrysAlis PRO (Agilent, 2013); cell refinement: CrysAlis PRO (Agilent, 2013); data reduction: CrysAlis PRO (Agilent, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot of the two indepenent molecules of the title compound. Ellipsoids are shown at 50% probability.
[Figure 2] Fig. 2. Ball and stick drawing of title compound showing the fold angle of the indenyl rings for both independent molecules. Ethylene ligands and hydrogen atoms omitted for clarity.
Bis(η2-ethylene)(η5-indenyl)iridium(I) top
Crystal data top
[Ir(C9H7)(C2H4)2]F(000) = 1360
Mr = 363.45Dx = 2.286 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
a = 7.73182 (11) ÅCell parameters from 34473 reflections
b = 10.77708 (13) Åθ = 3.1–32.0°
c = 25.6818 (5) ŵ = 12.57 mm1
β = 98.4034 (15)°T = 100 K
V = 2117.00 (5) Å3Prism, clear orange
Z = 80.45 × 0.33 × 0.22 mm
Data collection top
Agilent Xcalibur, Sapphire2
diffractometer
6917 independent reflections
Radiation source: Enhance (Mo) X-ray Source6733 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 8.3438 pixels mm-1θmax = 32.0°, θmin = 2.9°
ω and π scansh = 1111
Absorption correction: gaussian
(CrysAlis PRO; Agilent, 2013)
k = 1515
Tmin = 0.020, Tmax = 0.142l = 3837
55683 measured reflections
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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.055H-atom parameters constrained
S = 1.46 w = 1/[σ2(Fo2) + (0.P)2 + 12.8207P]
where P = (Fo2 + 2Fc2)/3
6917 reflections(Δ/σ)max = 0.001
253 parametersΔρmax = 1.69 e Å3
0 restraintsΔρmin = 2.04 e Å3
Crystal data top
[Ir(C9H7)(C2H4)2]V = 2117.00 (5) Å3
Mr = 363.45Z = 8
Monoclinic, P21/cMo Kα radiation
a = 7.73182 (11) ŵ = 12.57 mm1
b = 10.77708 (13) ÅT = 100 K
c = 25.6818 (5) Å0.45 × 0.33 × 0.22 mm
β = 98.4034 (15)°
Data collection top
Agilent Xcalibur, Sapphire2
diffractometer
6917 independent reflections
Absorption correction: gaussian
(CrysAlis PRO; Agilent, 2013)
6733 reflections with I > 2σ(I)
Tmin = 0.020, Tmax = 0.142Rint = 0.027
55683 measured reflectionsθmax = 32.0°
Refinement top
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.P)2 + 12.8207P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055Δρmax = 1.69 e Å3
S = 1.46Δρmin = 2.04 e Å3
6917 reflectionsAbsolute structure: ?
253 parametersAbsolute structure parameter: ?
0 restraintsRogers parameter: ?
H-atom parameters constrained
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
Ir1A0.306000 (16)0.166573 (12)0.397616 (5)0.00973 (3)
Ir1B0.187010 (16)0.186101 (12)0.088370 (5)0.01014 (3)
C1A0.1325 (5)0.2945 (3)0.43319 (14)0.0147 (6)
H1A0.13860.30690.46930.018*
C1B0.3647 (5)0.0581 (4)0.05469 (15)0.0177 (7)
H1B0.36000.04430.01870.021*
C2A0.2281 (5)0.3620 (3)0.39842 (15)0.0155 (7)
H2A0.31610.41970.40850.019*
C2B0.4684 (5)0.1505 (4)0.08498 (15)0.0165 (7)
H2B0.53270.21280.07160.020*
C3A0.1632 (5)0.3244 (3)0.34461 (15)0.0146 (6)
C3B0.4555 (4)0.1297 (3)0.13992 (14)0.0142 (6)
C4A0.2031 (5)0.3653 (4)0.29522 (16)0.0204 (7)
H4A0.28460.42800.29310.024*
C4B0.5348 (5)0.1890 (4)0.18694 (16)0.0183 (7)
H4B0.61350.25390.18560.022*
C5A0.1184 (5)0.3100 (4)0.25073 (17)0.0247 (9)
H5A0.14170.33680.21800.030*
C5B0.4929 (5)0.1488 (4)0.23413 (16)0.0215 (8)
H5B0.54500.18660.26510.026*
C6A0.0051 (6)0.2120 (4)0.25316 (17)0.0241 (8)
H6A0.06050.17670.22210.029*
C6B0.3727 (6)0.0515 (4)0.23698 (16)0.0235 (8)
H6B0.34900.02600.26980.028*
C7A0.0433 (5)0.1694 (4)0.30037 (16)0.0191 (7)
H7A0.12090.10380.30170.023*
C7B0.2895 (5)0.0069 (4)0.19267 (17)0.0200 (7)
H7B0.20780.06930.19520.024*
C8A0.0379 (4)0.2272 (3)0.34746 (14)0.0134 (6)
C8B0.3318 (4)0.0306 (3)0.14296 (14)0.0136 (6)
C9A0.0265 (4)0.2051 (3)0.40240 (14)0.0138 (6)
H9A0.03890.14300.41550.017*
C9B0.2694 (5)0.0093 (3)0.08948 (15)0.0157 (7)
H9B0.18280.06810.07950.019*
C10A0.5669 (5)0.1874 (4)0.43434 (16)0.0179 (7)
H10A0.59610.26530.45250.022*
H10B0.62030.11560.45310.022*
C10B0.0726 (5)0.1574 (4)0.05168 (16)0.0180 (7)
H10C0.12700.22520.03040.022*
H10D0.09940.07620.03620.022*
C11A0.5626 (4)0.1880 (3)0.37850 (15)0.0158 (7)
H11A0.61290.11650.36320.019*
H11B0.58860.26630.36270.019*
C11B0.0704 (4)0.1672 (3)0.10706 (15)0.0156 (6)
H11C0.09530.09200.12540.019*
H11D0.12300.24110.11960.019*
C12A0.3065 (5)0.0121 (3)0.43176 (15)0.0164 (7)
H12A0.40910.03430.45650.020*
H12B0.19750.03980.44240.020*
C12B0.1810 (5)0.3641 (4)0.05277 (16)0.0187 (7)
H12C0.28850.39200.04110.022*
H12D0.07670.38460.02850.022*
C13A0.3210 (5)0.0231 (3)0.37742 (16)0.0163 (7)
H13A0.22080.05750.35490.020*
H13B0.43240.05200.36890.020*
C13B0.1702 (5)0.3777 (3)0.10754 (15)0.0155 (6)
H13C0.05920.40620.11660.019*
H13D0.27100.41360.12920.019*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir1A0.00901 (5)0.00969 (5)0.01044 (6)0.00009 (4)0.00123 (4)0.00033 (4)
Ir1B0.00871 (5)0.01052 (5)0.01127 (6)0.00065 (4)0.00171 (4)0.00062 (4)
C1A0.0151 (15)0.0157 (15)0.0135 (16)0.0026 (12)0.0025 (12)0.0021 (12)
C1B0.0170 (16)0.0220 (18)0.0145 (17)0.0068 (13)0.0036 (13)0.0016 (14)
C2A0.0129 (15)0.0108 (14)0.0222 (18)0.0001 (12)0.0009 (13)0.0015 (13)
C2B0.0113 (14)0.0216 (17)0.0174 (17)0.0029 (12)0.0044 (12)0.0029 (14)
C3A0.0132 (14)0.0140 (15)0.0166 (17)0.0050 (12)0.0016 (12)0.0007 (13)
C3B0.0120 (14)0.0156 (15)0.0146 (16)0.0030 (12)0.0010 (12)0.0016 (12)
C4A0.0213 (18)0.0215 (18)0.0190 (18)0.0057 (14)0.0051 (14)0.0069 (14)
C4B0.0142 (15)0.0195 (17)0.0197 (18)0.0022 (13)0.0028 (13)0.0002 (14)
C5A0.0223 (19)0.036 (2)0.0161 (18)0.0099 (17)0.0053 (15)0.0069 (16)
C5B0.0211 (18)0.027 (2)0.0148 (17)0.0056 (15)0.0036 (14)0.0030 (15)
C6A0.0212 (18)0.036 (2)0.0138 (17)0.0082 (16)0.0027 (14)0.0037 (16)
C6B0.026 (2)0.031 (2)0.0134 (17)0.0086 (16)0.0046 (15)0.0065 (15)
C7A0.0136 (15)0.0221 (18)0.0201 (18)0.0024 (13)0.0029 (13)0.0050 (14)
C7B0.0170 (16)0.0198 (17)0.024 (2)0.0021 (13)0.0065 (14)0.0078 (15)
C8A0.0106 (14)0.0145 (15)0.0146 (16)0.0018 (11)0.0008 (12)0.0007 (12)
C8B0.0119 (14)0.0137 (15)0.0149 (16)0.0020 (12)0.0005 (12)0.0015 (12)
C9A0.0115 (14)0.0157 (15)0.0146 (16)0.0010 (12)0.0029 (12)0.0002 (12)
C9B0.0153 (15)0.0127 (15)0.0183 (17)0.0030 (12)0.0006 (13)0.0013 (13)
C10A0.0117 (15)0.0206 (17)0.0203 (18)0.0031 (13)0.0017 (13)0.0045 (14)
C10B0.0107 (15)0.0224 (18)0.0200 (18)0.0005 (13)0.0004 (13)0.0029 (14)
C11A0.0115 (14)0.0154 (15)0.0211 (18)0.0005 (12)0.0044 (12)0.0015 (13)
C11B0.0103 (14)0.0158 (15)0.0211 (18)0.0017 (12)0.0043 (12)0.0011 (13)
C12A0.0181 (16)0.0116 (15)0.0190 (18)0.0007 (12)0.0012 (13)0.0052 (13)
C12B0.0197 (17)0.0157 (16)0.0220 (19)0.0025 (13)0.0070 (14)0.0059 (14)
C13A0.0167 (16)0.0107 (14)0.0220 (19)0.0010 (12)0.0051 (13)0.0000 (13)
C13B0.0173 (16)0.0132 (15)0.0156 (17)0.0004 (12)0.0014 (13)0.0002 (12)
Geometric parameters (Å, º) top
Ir1A—C1A2.210 (3)C5A—H5A0.9300
Ir1A—C2A2.190 (4)C5A—C6A1.430 (7)
Ir1A—C3A2.349 (4)C5B—H5B0.9300
Ir1A—C8A2.366 (3)C5B—C6B1.409 (6)
Ir1A—C9A2.220 (3)C6A—H6A0.9300
Ir1A—C10A2.109 (4)C6A—C7A1.367 (6)
Ir1A—C11A2.123 (3)C6B—H6B0.9300
Ir1A—C12A2.114 (3)C6B—C7B1.374 (6)
Ir1A—C13A2.115 (4)C7A—H7A0.9300
Ir1B—C1B2.208 (4)C7A—C8A1.421 (5)
Ir1B—C2B2.222 (3)C7B—H7B0.9300
Ir1B—C3B2.371 (3)C7B—C8B1.421 (5)
Ir1B—C8B2.358 (3)C8A—C9A1.445 (5)
Ir1B—C9B2.197 (4)C8B—C9B1.451 (5)
Ir1B—C10B2.111 (4)C9A—H9A0.9300
Ir1B—C11B2.123 (3)C9B—H9B0.9300
Ir1B—C12B2.121 (4)C10A—H10A0.9700
Ir1B—C13B2.129 (4)C10A—H10B0.9700
C1A—H1A0.9300C10A—C11A1.428 (5)
C1A—C2A1.435 (5)C10B—H10C0.9700
C1A—C9A1.426 (5)C10B—H10D0.9700
C1B—H1B0.9300C10B—C11B1.422 (5)
C1B—C2B1.433 (5)C11A—H11A0.9700
C1B—C9B1.434 (5)C11A—H11B0.9700
C2A—H2A0.9300C11B—H11C0.9700
C2A—C3A1.456 (5)C11B—H11D0.9700
C2B—H2B0.9300C12A—H12A0.9700
C2B—C3B1.445 (5)C12A—H12B0.9700
C3A—C4A1.417 (5)C12A—C13A1.419 (5)
C3A—C8A1.435 (5)C12B—H12C0.9700
C3B—C4B1.422 (5)C12B—H12D0.9700
C3B—C8B1.442 (5)C12B—C13B1.427 (5)
C4A—H4A0.9300C13A—H13A0.9700
C4A—C5A1.367 (6)C13A—H13B0.9700
C4B—H4B0.9300C13B—H13C0.9700
C4B—C5B1.368 (6)C13B—H13D0.9700
C1A—Ir1A—C3A61.69 (13)C2B—C3B—Ir1B66.12 (19)
C1A—Ir1A—C8A61.10 (13)C4B—C3B—Ir1B126.3 (3)
C1A—Ir1A—C9A37.56 (13)C4B—C3B—C2B132.5 (4)
C2A—Ir1A—C1A38.07 (14)C4B—C3B—C8B119.6 (3)
C2A—Ir1A—C3A37.20 (13)C8B—C3B—Ir1B71.75 (19)
C2A—Ir1A—C8A61.29 (13)C8B—C3B—C2B107.9 (3)
C2A—Ir1A—C9A63.17 (13)C3A—C4A—H4A120.9
C3A—Ir1A—C8A35.43 (12)C5A—C4A—C3A118.1 (4)
C9A—Ir1A—C3A61.18 (13)C5A—C4A—H4A120.9
C9A—Ir1A—C8A36.55 (13)C3B—C4B—H4B120.7
C10A—Ir1A—C1A110.30 (15)C5B—C4B—C3B118.7 (4)
C10A—Ir1A—C2A98.05 (15)C5B—C4B—H4B120.7
C10A—Ir1A—C3A121.30 (14)C4A—C5A—H5A119.1
C10A—Ir1A—C8A156.62 (14)C4A—C5A—C6A121.8 (4)
C10A—Ir1A—C9A146.06 (15)C6A—C5A—H5A119.1
C10A—Ir1A—C11A39.44 (15)C4B—C5B—H5B119.2
C10A—Ir1A—C12A88.13 (15)C4B—C5B—C6B121.6 (4)
C10A—Ir1A—C13A97.41 (15)C6B—C5B—H5B119.2
C11A—Ir1A—C1A132.10 (14)C5A—C6A—H6A119.4
C11A—Ir1A—C2A99.50 (14)C7A—C6A—C5A121.2 (4)
C11A—Ir1A—C3A99.40 (13)C7A—C6A—H6A119.4
C11A—Ir1A—C8A128.14 (14)C5B—C6B—H6B119.0
C11A—Ir1A—C9A160.23 (14)C7B—C6B—C5B122.0 (4)
C12A—Ir1A—C1A111.18 (14)C7B—C6B—H6B119.0
C12A—Ir1A—C2A148.74 (15)C6A—C7A—H7A120.6
C12A—Ir1A—C3A150.56 (14)C6A—C7A—C8A118.7 (4)
C12A—Ir1A—C8A115.17 (14)C8A—C7A—H7A120.6
C12A—Ir1A—C9A95.20 (14)C6B—C7B—H7B120.9
C12A—Ir1A—C11A104.42 (14)C6B—C7B—C8B118.1 (4)
C12A—Ir1A—C13A39.23 (15)C8B—C7B—H7B120.9
C13A—Ir1A—C1A139.61 (14)C3A—C8A—Ir1A71.65 (19)
C13A—Ir1A—C2A162.85 (14)C3A—C8A—C9A107.9 (3)
C13A—Ir1A—C3A126.52 (14)C7A—C8A—Ir1A125.8 (3)
C13A—Ir1A—C8A102.03 (14)C7A—C8A—C3A119.6 (3)
C13A—Ir1A—C9A106.42 (14)C7A—C8A—C9A132.5 (3)
C13A—Ir1A—C11A87.83 (14)C9A—C8A—Ir1A66.22 (19)
C1B—Ir1B—C2B37.74 (14)C3B—C8B—Ir1B72.7 (2)
C1B—Ir1B—C3B61.00 (13)C3B—C8B—C9B107.4 (3)
C1B—Ir1B—C8B61.37 (13)C7B—C8B—Ir1B125.7 (3)
C2B—Ir1B—C3B36.48 (13)C7B—C8B—C3B120.0 (3)
C2B—Ir1B—C8B61.19 (13)C7B—C8B—C9B132.5 (3)
C8B—Ir1B—C3B35.51 (12)C9B—C8B—Ir1B65.48 (19)
C9B—Ir1B—C1B38.00 (14)Ir1A—C9A—H9A118.0
C9B—Ir1B—C2B63.37 (14)C1A—C9A—Ir1A70.85 (19)
C9B—Ir1B—C3B61.27 (13)C1A—C9A—C8A108.5 (3)
C9B—Ir1B—C8B36.94 (13)C1A—C9A—H9A125.7
C10B—Ir1B—C1B109.80 (15)C8A—C9A—Ir1A77.2 (2)
C10B—Ir1B—C2B146.00 (15)C8A—C9A—H9A125.7
C10B—Ir1B—C3B155.32 (14)Ir1B—C9B—H9B117.0
C10B—Ir1B—C8B119.92 (14)C1B—C9B—Ir1B71.4 (2)
C10B—Ir1B—C9B96.90 (15)C1B—C9B—C8B108.0 (3)
C10B—Ir1B—C11B39.26 (15)C1B—C9B—H9B126.0
C10B—Ir1B—C12B88.89 (15)C8B—C9B—Ir1B77.6 (2)
C10B—Ir1B—C13B99.14 (15)C8B—C9B—H9B126.0
C11B—Ir1B—C1B133.24 (15)Ir1A—C10A—H10A116.5
C11B—Ir1B—C2B161.22 (14)Ir1A—C10A—H10B116.5
C11B—Ir1B—C3B128.47 (14)H10A—C10A—H10B113.5
C11B—Ir1B—C8B100.21 (13)C11A—C10A—Ir1A70.8 (2)
C11B—Ir1B—C9B100.64 (14)C11A—C10A—H10A116.5
C11B—Ir1B—C13B87.13 (14)C11A—C10A—H10B116.5
C12B—Ir1B—C1B111.80 (15)Ir1B—C10B—H10C116.5
C12B—Ir1B—C2B95.70 (14)Ir1B—C10B—H10D116.5
C12B—Ir1B—C3B115.72 (14)H10C—C10B—H10D113.5
C12B—Ir1B—C8B151.18 (14)C11B—C10B—Ir1B70.8 (2)
C12B—Ir1B—C9B149.22 (15)C11B—C10B—H10C116.5
C12B—Ir1B—C11B102.79 (15)C11B—C10B—H10D116.5
C12B—Ir1B—C13B39.24 (15)Ir1A—C11A—H11A116.7
C13B—Ir1B—C1B139.24 (15)Ir1A—C11A—H11B116.7
C13B—Ir1B—C2B105.64 (14)C10A—C11A—Ir1A69.7 (2)
C13B—Ir1B—C3B101.37 (13)C10A—C11A—H11A116.7
C13B—Ir1B—C8B126.20 (13)C10A—C11A—H11B116.7
C13B—Ir1B—C9B162.21 (14)H11A—C11A—H11B113.7
Ir1A—C1A—H1A123.7Ir1B—C11B—H11C116.6
C2A—C1A—Ir1A70.2 (2)Ir1B—C11B—H11D116.6
C2A—C1A—H1A126.2C10B—C11B—Ir1B69.9 (2)
C9A—C1A—Ir1A71.6 (2)C10B—C11B—H11C116.6
C9A—C1A—H1A126.2C10B—C11B—H11D116.6
C9A—C1A—C2A107.7 (3)H11C—C11B—H11D113.6
Ir1B—C1B—H1B123.5Ir1A—C12A—H12A116.6
C2B—C1B—Ir1B71.6 (2)Ir1A—C12A—H12B116.6
C2B—C1B—H1B125.9H12A—C12A—H12B113.6
C2B—C1B—C9B108.1 (3)C13A—C12A—Ir1A70.4 (2)
C9B—C1B—Ir1B70.6 (2)C13A—C12A—H12A116.6
C9B—C1B—H1B125.9C13A—C12A—H12B116.6
Ir1A—C2A—H2A117.0Ir1B—C12B—H12C116.5
C1A—C2A—Ir1A71.7 (2)Ir1B—C12B—H12D116.5
C1A—C2A—H2A125.9H12C—C12B—H12D113.5
C1A—C2A—C3A108.1 (3)C13B—C12B—Ir1B70.7 (2)
C3A—C2A—Ir1A77.4 (2)C13B—C12B—H12C116.5
C3A—C2A—H2A125.9C13B—C12B—H12D116.5
Ir1B—C2B—H2B117.9Ir1A—C13A—H13A116.6
C1B—C2B—Ir1B70.6 (2)Ir1A—C13A—H13B116.6
C1B—C2B—H2B126.0C12A—C13A—Ir1A70.4 (2)
C1B—C2B—C3B108.0 (3)C12A—C13A—H13A116.6
C3B—C2B—Ir1B77.4 (2)C12A—C13A—H13B116.6
C3B—C2B—H2B126.0H13A—C13A—H13B113.6
C2A—C3A—Ir1A65.45 (19)Ir1B—C13B—H13C116.6
C4A—C3A—Ir1A126.7 (3)Ir1B—C13B—H13D116.6
C4A—C3A—C2A132.2 (4)C12B—C13B—Ir1B70.1 (2)
C4A—C3A—C8A120.5 (3)C12B—C13B—H13C116.6
C8A—C3A—Ir1A72.9 (2)C12B—C13B—H13D116.6
C8A—C3A—C2A107.2 (3)H13C—C13B—H13D113.6

Experimental details

Crystal data
Chemical formula[Ir(C9H7)(C2H4)2]
Mr363.45
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)7.73182 (11), 10.77708 (13), 25.6818 (5)
β (°) 98.4034 (15)
V3)2117.00 (5)
Z8
Radiation typeMo Kα
µ (mm1)12.57
Crystal size (mm)0.45 × 0.33 × 0.22
Data collection
DiffractometerAgilent Xcalibur, Sapphire2
diffractometer
Absorption correctionGaussian
(CrysAlis PRO; Agilent, 2013)
Tmin, Tmax0.020, 0.142
No. of measured, independent and
observed [I > 2σ(I)] reflections
55683, 6917, 6733
Rint0.027
(sin θ/λ)max1)0.745
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.055, 1.46
No. of reflections6917
No. of parameters253
No. of restraints0
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.P)2 + 12.8207P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.69, 2.04

Computer programs: CrysAlis PRO (Agilent, 2013), SHELXS97 (Sheldrick, 2008), SHELXL2013 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009).

Selected Ir to indenyl bond distances Å. top
Ir1A—C1A2.210 (3)Ir1B—C1B2.208 (4)
Ir1A—C2A2.190 (4)Ir1B—C2B2.222 (3)
Ir1A—C3A2.349 (4)Ir1B—C3B2.371 (3)
Ir1A—C8A2.366 (3)Ir1B—C8B2.358 (3)
Ir1A—C9A2.220 (3)Ir1B—C9B2.197 (4)
Selected Ir to indenyl bond distances Å. top
Ir1A—C1A2.210 (3)Ir1B—C1B2.208 (4)
Ir1A—C2A2.190 (4)Ir1B—C2B2.222 (3)
Ir1A—C3A2.349 (4)Ir1B—C3B2.371 (3)
Ir1A—C8A2.366 (3)Ir1B—C8B2.358 (3)
Ir1A—C9A2.220 (3)Ir1B—C9B2.197 (4)
Acknowledgements top

The author thanks the National Science Foundation for funds (CHE-01311288) for the purchase of the diffractometer. The author recognizes the payment of the open access fee by Virginia Tech University Libraries.

references
References top

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