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The crystal structure of the title compound, [IrCl2H(C18H15P)2(CO)] or [IrCl2(H)(CO)(PPh3)2], has been determined. The compound is an octahedral iridium(III) complex with trans phosphine and cis chloride ligands. The molecule sits on a crystallographic twofold axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804000479/dn6111sup1.cif
Contains datablocks global, 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804000479/dn61112sup2.hkl
Contains datablock 2

CCDC reference: 234794

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.056
  • wR factor = 0.153
  • Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.126 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.13 PLAT301_ALERT_3_C Main Residue Disorder ......................... 7.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXL97.

(2) top
Crystal data top
[IrCl2H(C18H15P)2(CO)]F(000) = 1608
Mr = 816.66Dx = 1.702 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6054 reflections
a = 23.548 (6) Åθ = 2–27°
b = 9.596 (2) ŵ = 4.49 mm1
c = 15.623 (3) ÅT = 173 K
β = 115.505 (6)°Block, orange
V = 3186.2 (12) Å30.2 × 0.2 × 0.1 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
3675 independent reflections
Radiation source: fine-focus sealed tube2347 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.126
Detector resolution: 8.192 pixels mm-1θmax = 27.6°, θmin = 1.9°
Frames, each covering 0.3° in ω scansh = 3030
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1212
Tmin = 0.440, Tmax = 0.640l = 2020
13634 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)] = 0.056Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.153H atoms treated by a mixture of independent and constrained refinement
S = 0.94 w = 1/[σ2(Fo2) + (0.0863P)2]
where P = (Fo2 + 2Fc2)/3
3675 reflections(Δ/σ)max = 0.001
204 parametersΔρmax = 1.92 e Å3
4 restraintsΔρmin = 2.47 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*/UeqOcc. (<1)
C10.0896 (3)0.7712 (9)0.1203 (5)0.0281 (17)
C20.0989 (4)0.8597 (10)0.0571 (5)0.0347 (19)
H20.10750.95570.07160.042*
C30.0953 (4)0.8063 (10)0.0270 (6)0.039 (2)
H30.10090.86670.07100.047*
C40.0838 (4)0.6682 (10)0.0483 (6)0.044 (2)
H40.08270.63310.10580.053*
C50.0736 (5)0.5788 (12)0.0134 (7)0.054 (3)
H50.06410.48340.00270.064*
C60.0776 (5)0.6302 (10)0.0995 (7)0.047 (2)
H60.07200.56950.14330.056*
C70.1197 (3)1.0103 (9)0.2476 (5)0.0289 (17)
C80.0780 (4)1.1095 (8)0.1886 (6)0.0353 (19)
H80.03901.08070.13940.042*
C90.0929 (4)1.2490 (11)0.2011 (7)0.045 (2)
H90.06321.31530.16150.054*
C100.1504 (5)1.2956 (10)0.2703 (7)0.045 (2)
H100.16081.39190.27740.054*
C110.1916 (5)1.1971 (10)0.3280 (6)0.045 (2)
H110.23071.22660.37660.054*
C120.1779 (4)1.0582 (10)0.3176 (5)0.037 (2)
H120.20790.99300.35780.044*
C130.1625 (3)0.7269 (9)0.3170 (5)0.0320 (18)
C140.2189 (4)0.7325 (12)0.3085 (6)0.046 (2)
H140.22170.78790.26000.056*
C150.2707 (4)0.6590 (11)0.3695 (6)0.049 (3)
H150.30950.66590.36470.059*
C160.2657 (4)0.5741 (10)0.4385 (6)0.041 (2)
H160.30110.52190.48030.049*
C170.2096 (4)0.5657 (10)0.4463 (5)0.038 (2)
H170.20630.50740.49310.046*
C180.1575 (4)0.6432 (9)0.3851 (6)0.0342 (18)
H180.11890.63820.39060.041*
Cl10.00000.5565 (3)0.25000.0259 (5)
Ir10.00000.81339 (5)0.25000.03115 (17)
H10.00000.980 (2)0.25000.047*
P10.09527 (8)0.8273 (2)0.23534 (12)0.0245 (4)
Cl20.0525 (2)0.8352 (7)0.0862 (4)0.0371 (14)0.50
C190.0420 (11)0.823 (4)0.1199 (10)0.039 (3)0.50
O10.0689 (5)0.8223 (17)0.0369 (9)0.039 (3)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.021 (3)0.036 (5)0.030 (4)0.002 (3)0.014 (3)0.004 (3)
C20.035 (4)0.042 (5)0.030 (4)0.002 (4)0.016 (3)0.001 (4)
C30.038 (4)0.053 (6)0.032 (4)0.008 (4)0.021 (3)0.001 (5)
C40.037 (4)0.067 (8)0.032 (4)0.011 (5)0.019 (3)0.013 (4)
C50.066 (6)0.054 (7)0.055 (6)0.014 (6)0.040 (5)0.018 (5)
C60.077 (7)0.033 (5)0.052 (5)0.010 (5)0.048 (5)0.009 (4)
C70.029 (4)0.033 (5)0.030 (4)0.006 (3)0.018 (3)0.002 (3)
C80.035 (4)0.022 (4)0.049 (5)0.007 (4)0.019 (4)0.001 (4)
C90.043 (5)0.034 (5)0.068 (6)0.007 (5)0.033 (5)0.006 (5)
C100.055 (6)0.036 (6)0.056 (5)0.010 (5)0.036 (5)0.006 (5)
C110.051 (5)0.056 (7)0.034 (4)0.018 (5)0.024 (4)0.012 (5)
C120.038 (4)0.045 (6)0.028 (4)0.013 (4)0.014 (3)0.005 (4)
C130.026 (4)0.042 (5)0.029 (4)0.004 (4)0.013 (3)0.002 (4)
C140.035 (4)0.078 (7)0.033 (4)0.013 (5)0.022 (4)0.013 (5)
C150.028 (4)0.087 (8)0.034 (4)0.020 (5)0.014 (3)0.015 (5)
C160.026 (4)0.053 (6)0.039 (4)0.014 (4)0.009 (3)0.003 (4)
C170.033 (4)0.051 (6)0.028 (4)0.002 (4)0.011 (3)0.003 (4)
C180.029 (4)0.040 (5)0.034 (4)0.005 (4)0.014 (3)0.003 (4)
Cl10.0247 (12)0.0223 (13)0.0287 (11)0.0000.0095 (10)0.000
Ir10.0265 (2)0.0375 (3)0.0340 (2)0.0000.01724 (17)0.000
P10.0188 (8)0.0322 (12)0.0236 (8)0.0018 (8)0.0102 (7)0.0006 (9)
Cl20.024 (3)0.060 (4)0.021 (2)0.000 (3)0.004 (3)0.003 (4)
C190.013 (5)0.065 (8)0.039 (7)0.011 (6)0.012 (6)0.003 (9)
O10.013 (5)0.065 (8)0.039 (7)0.011 (6)0.012 (6)0.003 (9)
Geometric parameters (Å, º) top
C1—C21.388 (11)C12—H120.9500
C1—C61.392 (12)C13—C181.378 (11)
C1—P11.825 (7)C13—C141.391 (11)
C2—C31.379 (11)C13—P11.824 (8)
C2—H20.9500C14—C151.376 (12)
C3—C41.364 (11)C14—H140.9500
C3—H30.9500C15—C161.397 (12)
C4—C51.385 (13)C15—H150.9500
C4—H40.9500C16—C171.381 (11)
C5—C61.398 (12)C16—H160.9500
C5—H50.9500C17—C181.401 (11)
C6—H60.9500C17—H170.9500
C7—C81.393 (11)C18—H180.9500
C7—C121.413 (11)Cl1—Ir12.465 (3)
C7—P11.832 (8)Ir1—C19i1.840 (14)
C8—C91.377 (13)Ir1—C191.840 (14)
C8—H80.9500Ir1—Cl2i2.323 (5)
C9—C101.394 (14)Ir1—Cl22.323 (5)
C9—H90.9500Ir1—P12.3549 (18)
C10—C111.377 (13)Ir1—P1i2.3549 (18)
C10—H100.9500Ir1—H11.60 (2)
C11—C121.364 (12)C19—O11.173 (14)
C11—H110.9500
C2—C1—C6120.5 (7)C17—C16—C15120.3 (8)
C2—C1—P1123.5 (7)C17—C16—H16119.9
C6—C1—P1116.0 (6)C15—C16—H16119.9
C3—C2—C1119.1 (8)C16—C17—C18119.9 (8)
C3—C2—H2120.5C16—C17—H17120.0
C1—C2—H2120.5C18—C17—H17120.0
C4—C3—C2121.1 (8)C13—C18—C17119.7 (8)
C4—C3—H3119.4C13—C18—H18120.1
C2—C3—H3119.4C17—C18—H18120.1
C3—C4—C5120.5 (8)C19i—Ir1—C19174 (2)
C3—C4—H4119.7C19i—Ir1—Cl2i2.2 (13)
C5—C4—H4119.7C19—Ir1—Cl2i171.8 (11)
C4—C5—C6119.3 (9)C19i—Ir1—Cl2171.8 (11)
C4—C5—H5120.3C19—Ir1—Cl22.2 (13)
C6—C5—H5120.3Cl2i—Ir1—Cl2169.7 (3)
C1—C6—C5119.4 (9)C19i—Ir1—P191.3 (8)
C1—C6—H6120.3C19—Ir1—P188.3 (8)
C5—C6—H6120.3Cl2i—Ir1—P191.43 (13)
C8—C7—C12117.5 (8)Cl2—Ir1—P187.98 (13)
C8—C7—P1119.1 (6)C19i—Ir1—P1i88.3 (8)
C12—C7—P1123.3 (6)C19—Ir1—P1i91.3 (8)
C9—C8—C7120.5 (8)Cl2i—Ir1—P1i87.98 (13)
C9—C8—H8119.8Cl2—Ir1—P1i91.43 (13)
C7—C8—H8119.8P1—Ir1—P1i173.50 (10)
C8—C9—C10121.7 (9)C19i—Ir1—Cl193.0 (12)
C8—C9—H9119.2C19—Ir1—Cl193.0 (12)
C10—C9—H9119.2Cl2i—Ir1—Cl195.17 (16)
C11—C10—C9117.6 (9)Cl2—Ir1—Cl195.17 (16)
C11—C10—H10121.2P1—Ir1—Cl193.25 (5)
C9—C10—H10121.2P1i—Ir1—Cl193.25 (5)
C12—C11—C10122.0 (8)C19i—Ir1—H187.0 (12)
C12—C11—H11119.0C19—Ir1—H187.0 (12)
C10—C11—H11119.0Cl2i—Ir1—H184.83 (16)
C11—C12—C7120.7 (8)Cl2—Ir1—H184.83 (16)
C11—C12—H12119.6P1—Ir1—H186.75 (5)
C7—C12—H12119.6P1i—Ir1—H186.75 (5)
C18—C13—C14119.9 (8)Cl1—Ir1—H1180.000 (5)
C18—C13—P1120.7 (6)C13—P1—C1101.9 (4)
C14—C13—P1119.3 (6)C13—P1—C7107.1 (4)
C15—C14—C13120.8 (8)C1—P1—C7105.8 (4)
C15—C14—H14119.6C13—P1—Ir1118.6 (3)
C13—C14—H14119.6C1—P1—Ir1114.2 (2)
C14—C15—C16119.3 (8)C7—P1—Ir1108.3 (2)
C14—C15—H15120.3O1—C19—Ir1177 (3)
C16—C15—H15120.3
C6—C1—C2—C30.7 (12)C14—C13—P1—Ir1179.2 (7)
P1—C1—C2—C3178.2 (6)C2—C1—P1—C13115.6 (7)
C1—C2—C3—C41.0 (13)C6—C1—P1—C1362.1 (7)
C2—C3—C4—C51.9 (14)C2—C1—P1—C73.7 (7)
C3—C4—C5—C62.3 (15)C6—C1—P1—C7174.0 (6)
C2—C1—C6—C51.2 (14)C2—C1—P1—Ir1115.3 (6)
P1—C1—C6—C5178.9 (8)C6—C1—P1—Ir167.1 (7)
C4—C5—C6—C12.0 (15)C8—C7—P1—C13176.2 (6)
C12—C7—C8—C92.1 (11)C12—C7—P1—C137.1 (7)
P1—C7—C8—C9174.8 (6)C8—C7—P1—C168.1 (7)
C7—C8—C9—C102.1 (13)C12—C7—P1—C1115.3 (6)
C8—C9—C10—C111.7 (13)C8—C7—P1—Ir154.8 (6)
C9—C10—C11—C121.4 (13)C12—C7—P1—Ir1121.9 (6)
C10—C11—C12—C71.5 (13)C19i—Ir1—P1—C1342.4 (12)
C8—C7—C12—C111.8 (11)C19—Ir1—P1—C13143.5 (12)
P1—C7—C12—C11175.0 (6)Cl2i—Ir1—P1—C1344.6 (4)
C18—C13—C14—C152.2 (15)Cl2—Ir1—P1—C13145.7 (4)
P1—C13—C14—C15179.5 (8)Cl1—Ir1—P1—C1350.7 (3)
C13—C14—C15—C162.2 (15)C19i—Ir1—P1—C1162.6 (12)
C14—C15—C16—C170.9 (15)C19—Ir1—P1—C123.3 (12)
C15—C16—C17—C180.4 (13)Cl2i—Ir1—P1—C1164.8 (3)
C14—C13—C18—C170.9 (13)Cl2—Ir1—P1—C125.5 (3)
P1—C13—C18—C17179.2 (6)Cl1—Ir1—P1—C169.5 (3)
C16—C17—C18—C130.4 (13)C19i—Ir1—P1—C779.8 (12)
C18—C13—P1—C1125.5 (7)C19—Ir1—P1—C794.2 (12)
C14—C13—P1—C152.8 (8)Cl2i—Ir1—P1—C777.6 (3)
C18—C13—P1—C7123.6 (7)Cl2—Ir1—P1—C792.0 (3)
C14—C13—P1—C758.1 (8)Cl1—Ir1—P1—C7172.9 (2)
C18—C13—P1—Ir10.8 (8)
Symmetry code: (i) x, y, z+1/2.
 

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