Each IrIII ion in the title compound, [Ir(C10H15)Cl2(H2O)], is six-coordinated by two chloride ions, one water molecule and a pentamethylcyclopentadienyl (Cp*) ligand in a three-legged piano-stool geometry, assuming that the Cp* ligand functions as a tridentate ligand. There is hydrogen bonding between the water H atoms and the Cl atoms of adjacent molecules.
Supporting information
CCDC reference: 624012
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.015 Å
- R factor = 0.037
- wR factor = 0.083
- Data-to-parameter ratio = 17.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT416_ALERT_2_B Short Intra D-H..H-D H1A .. H1B .. 1.70 Ang.
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.83
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.833
Tmax scaled 0.349 Tmin scaled 0.304
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
Aquadichloro(
η5-pentamethylcyclopentadienyl)iridium(III)
top
Crystal data top
[Ir(C10H15)Cl2(H2O)] | F(000) = 784 |
Mr = 416.34 | Dx = 2.104 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.723 (5) Å | Cell parameters from 924 reflections |
b = 7.853 (5) Å | θ = 2.8–27.1° |
c = 19.591 (12) Å | µ = 10.53 mm−1 |
β = 101.662 (8)° | T = 293 K |
V = 1314.3 (14) Å3 | Block, red |
Z = 4 | 0.12 × 0.11 × 0.10 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2303 independent reflections |
Radiation source: fine-focus sealed tube | 2095 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 25.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −10→6 |
Tmin = 0.365, Tmax = 0.419 | k = −8→9 |
5235 measured reflections | l = −22→23 |
Refinement top
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.083 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (13.7468P)2 + 14.5636P] where P = (Fo2 + 2Fc2)/3 |
2303 reflections | (Δ/σ)max < 0.001 |
132 parameters | Δρmax = 1.37 e Å−3 |
0 restraints | Δρmin = −1.42 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ir1 | 0.20461 (4) | 0.05916 (4) | 0.399382 (18) | 0.03113 (13) | |
Cl4 | 0.3950 (3) | −0.1625 (3) | 0.39442 (15) | 0.0517 (7) | |
Cl5 | 0.0117 (3) | −0.1604 (3) | 0.40498 (14) | 0.0474 (6) | |
O1 | 0.2651 (10) | 0.0112 (11) | 0.5099 (4) | 0.068 (2) | |
H1A | 0.1935 | −0.0375 | 0.4805 | 0.081* | |
H1B | 0.3391 | 0.0666 | 0.5352 | 0.081* | |
C3 | 0.2144 (12) | 0.3282 (11) | 0.4063 (5) | 0.035 (2) | |
C4 | 0.2611 (16) | 0.4270 (15) | 0.4729 (6) | 0.060 (3) | |
H4A | 0.2688 | 0.5457 | 0.4624 | 0.090* | |
H4B | 0.3606 | 0.3869 | 0.4980 | 0.090* | |
H4C | 0.1837 | 0.4117 | 0.5010 | 0.090* | |
C5 | 0.0648 (12) | 0.1908 (12) | 0.3109 (4) | 0.037 (2) | |
C6 | 0.0592 (12) | 0.2786 (11) | 0.3769 (5) | 0.036 (2) | |
C7 | 0.3158 (12) | 0.2720 (13) | 0.3636 (5) | 0.040 (2) | |
C8 | 0.2224 (13) | 0.1879 (13) | 0.3039 (5) | 0.040 (2) | |
C9 | −0.0730 (15) | 0.1203 (15) | 0.2619 (6) | 0.062 (3) | |
H9A | −0.1244 | 0.2099 | 0.2326 | 0.093* | |
H9B | −0.1446 | 0.0718 | 0.2879 | 0.093* | |
H9C | −0.0392 | 0.0338 | 0.2337 | 0.093* | |
C10 | 0.4871 (14) | 0.312 (2) | 0.3723 (7) | 0.075 (4) | |
H10A | 0.4996 | 0.4174 | 0.3489 | 0.113* | |
H10B | 0.5385 | 0.2223 | 0.3526 | 0.113* | |
H10C | 0.5325 | 0.3233 | 0.4210 | 0.113* | |
C11 | 0.2847 (17) | 0.1157 (18) | 0.2445 (6) | 0.069 (4) | |
H11A | 0.2037 | 0.0523 | 0.2147 | 0.103* | |
H11B | 0.3711 | 0.0415 | 0.2622 | 0.103* | |
H11C | 0.3193 | 0.2066 | 0.2186 | 0.103* | |
C12 | −0.0845 (15) | 0.3186 (17) | 0.4029 (6) | 0.062 (3) | |
H12A | −0.0647 | 0.3044 | 0.4526 | 0.093* | |
H12B | −0.1670 | 0.2431 | 0.3817 | 0.093* | |
H12C | −0.1150 | 0.4341 | 0.3913 | 0.093* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ir1 | 0.0359 (2) | 0.02371 (19) | 0.0320 (2) | 0.00030 (18) | 0.00266 (14) | 0.00026 (17) |
Cl4 | 0.0477 (15) | 0.0376 (15) | 0.0672 (18) | 0.0110 (12) | 0.0054 (13) | −0.0030 (13) |
Cl5 | 0.0493 (15) | 0.0388 (15) | 0.0536 (15) | −0.0092 (12) | 0.0088 (12) | 0.0012 (12) |
O1 | 0.078 (6) | 0.065 (6) | 0.051 (5) | −0.012 (5) | −0.009 (4) | 0.009 (4) |
C3 | 0.046 (6) | 0.022 (4) | 0.034 (5) | 0.002 (4) | 0.003 (4) | 0.010 (4) |
C4 | 0.086 (9) | 0.034 (6) | 0.056 (7) | 0.007 (6) | 0.004 (6) | −0.012 (6) |
C5 | 0.053 (6) | 0.026 (5) | 0.027 (4) | 0.001 (4) | −0.003 (4) | 0.010 (4) |
C6 | 0.043 (6) | 0.019 (5) | 0.044 (5) | 0.005 (4) | 0.006 (4) | 0.011 (4) |
C7 | 0.046 (6) | 0.034 (6) | 0.040 (5) | −0.003 (5) | 0.007 (5) | 0.009 (5) |
C8 | 0.058 (7) | 0.034 (5) | 0.033 (5) | 0.009 (5) | 0.015 (5) | 0.008 (4) |
C9 | 0.069 (8) | 0.048 (7) | 0.056 (7) | −0.007 (6) | −0.018 (6) | 0.003 (6) |
C10 | 0.049 (7) | 0.097 (11) | 0.077 (9) | −0.007 (8) | 0.006 (7) | 0.036 (9) |
C11 | 0.096 (10) | 0.069 (9) | 0.047 (7) | 0.018 (8) | 0.028 (7) | 0.004 (6) |
C12 | 0.075 (9) | 0.055 (8) | 0.060 (7) | 0.028 (7) | 0.021 (6) | 0.024 (6) |
Geometric parameters (Å, º) top
Ir1—C3 | 2.118 (9) | C5—C6 | 1.474 (13) |
Ir1—C7 | 2.122 (10) | C5—C9 | 1.486 (14) |
Ir1—C6 | 2.132 (9) | C6—C12 | 1.479 (15) |
Ir1—O1 | 2.156 (8) | C7—C8 | 1.442 (14) |
Ir1—C8 | 2.159 (9) | C7—C10 | 1.503 (15) |
Ir1—C5 | 2.169 (9) | C8—C11 | 1.492 (14) |
Ir1—Cl4 | 2.421 (3) | C9—H9A | 0.9600 |
Ir1—Cl5 | 2.428 (3) | C9—H9B | 0.9600 |
Ir1—H1A | 1.7822 | C9—H9C | 0.9600 |
O1—H1A | 0.8501 | C10—H10A | 0.9600 |
O1—H1B | 0.8500 | C10—H10B | 0.9600 |
C3—C7 | 1.407 (14) | C10—H10C | 0.9600 |
C3—C6 | 1.414 (14) | C11—H11A | 0.9600 |
C3—C4 | 1.502 (14) | C11—H11B | 0.9600 |
C4—H4A | 0.9600 | C11—H11C | 0.9600 |
C4—H4B | 0.9600 | C12—H12A | 0.9600 |
C4—H4C | 0.9600 | C12—H12B | 0.9600 |
C5—C8 | 1.409 (14) | C12—H12C | 0.9600 |
| | | |
C3—Ir1—C7 | 38.8 (4) | H4B—C4—H4C | 109.5 |
C3—Ir1—C6 | 38.9 (4) | C8—C5—C6 | 107.4 (8) |
C7—Ir1—C6 | 65.6 (4) | C8—C5—C9 | 127.5 (10) |
C3—Ir1—O1 | 96.4 (3) | C6—C5—C9 | 125.1 (10) |
C7—Ir1—O1 | 115.7 (4) | C8—C5—Ir1 | 70.6 (5) |
C6—Ir1—O1 | 111.3 (4) | C6—C5—Ir1 | 68.6 (5) |
C3—Ir1—C8 | 65.1 (4) | C9—C5—Ir1 | 126.1 (7) |
C7—Ir1—C8 | 39.4 (4) | C3—C6—C5 | 106.7 (9) |
C6—Ir1—C8 | 65.6 (4) | C3—C6—C12 | 127.5 (10) |
O1—Ir1—C8 | 155.0 (4) | C5—C6—C12 | 125.6 (10) |
C3—Ir1—C5 | 65.5 (4) | C3—C6—Ir1 | 70.0 (5) |
C7—Ir1—C5 | 65.2 (4) | C5—C6—Ir1 | 71.3 (5) |
C6—Ir1—C5 | 40.1 (4) | C12—C6—Ir1 | 127.6 (7) |
O1—Ir1—C5 | 150.4 (4) | C3—C7—C8 | 107.8 (9) |
C8—Ir1—C5 | 38.0 (4) | C3—C7—C10 | 126.6 (10) |
C3—Ir1—Cl4 | 134.5 (3) | C8—C7—C10 | 125.1 (10) |
C7—Ir1—Cl4 | 100.9 (3) | C3—C7—Ir1 | 70.5 (5) |
C6—Ir1—Cl4 | 163.1 (3) | C8—C7—Ir1 | 71.7 (6) |
O1—Ir1—Cl4 | 83.3 (3) | C10—C7—Ir1 | 129.7 (8) |
C8—Ir1—Cl4 | 97.6 (3) | C5—C8—C7 | 108.4 (8) |
C5—Ir1—Cl4 | 126.2 (3) | C5—C8—C11 | 126.8 (10) |
C3—Ir1—Cl5 | 136.5 (3) | C7—C8—C11 | 124.8 (11) |
C7—Ir1—Cl5 | 160.4 (3) | C5—C8—Ir1 | 71.4 (5) |
C6—Ir1—Cl5 | 101.2 (3) | C7—C8—Ir1 | 68.9 (5) |
O1—Ir1—Cl5 | 82.0 (2) | C11—C8—Ir1 | 126.8 (8) |
C8—Ir1—Cl5 | 122.9 (3) | C5—C9—H9A | 109.5 |
C5—Ir1—Cl5 | 95.3 (3) | C5—C9—H9B | 109.5 |
Cl4—Ir1—Cl5 | 88.76 (10) | H9A—C9—H9B | 109.5 |
C3—Ir1—H1A | 112.1 | C5—C9—H9C | 109.5 |
C7—Ir1—H1A | 137.9 | H9A—C9—H9C | 109.5 |
C6—Ir1—H1A | 113.0 | H9B—C9—H9C | 109.5 |
O1—Ir1—H1A | 22.5 | C7—C10—H10A | 109.5 |
C8—Ir1—H1A | 177.1 | C7—C10—H10B | 109.5 |
C5—Ir1—H1A | 142.4 | H10A—C10—H10B | 109.5 |
Cl4—Ir1—H1A | 83.8 | C7—C10—H10C | 109.5 |
Cl5—Ir1—H1A | 59.6 | H10A—C10—H10C | 109.5 |
Ir1—O1—H1A | 53.2 | H10B—C10—H10C | 109.5 |
Ir1—O1—H1B | 120.0 | C8—C11—H11A | 109.5 |
H1A—O1—H1B | 173.2 | C8—C11—H11B | 109.5 |
C7—C3—C6 | 109.6 (9) | H11A—C11—H11B | 109.5 |
C7—C3—C4 | 125.9 (10) | C8—C11—H11C | 109.5 |
C6—C3—C4 | 124.5 (10) | H11A—C11—H11C | 109.5 |
C7—C3—Ir1 | 70.8 (6) | H11B—C11—H11C | 109.5 |
C6—C3—Ir1 | 71.1 (5) | C6—C12—H12A | 109.5 |
C4—C3—Ir1 | 124.9 (7) | C6—C12—H12B | 109.5 |
C3—C4—H4A | 109.5 | H12A—C12—H12B | 109.5 |
C3—C4—H4B | 109.5 | C6—C12—H12C | 109.5 |
H4A—C4—H4B | 109.5 | H12A—C12—H12C | 109.5 |
C3—C4—H4C | 109.5 | H12B—C12—H12C | 109.5 |
H4A—C4—H4C | 109.5 | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···Cl5 | 0.85 | 2.17 | 3.015 (9) | 180 |
O1—H1B···Cl4i | 0.85 | 2.56 | 3.387 (9) | 164 |
Symmetry code: (i) −x+1, −y, −z+1. |