Carbonyl­di­chloro­hydridobis­(tri­methyl­phosphine)­iridium(III)

The crystal structure of the title compound, [IrCl₂H(C₃H₉P)₂(CO)] or [IrCl₂(H)(CO)(PMe₃)₂], has been determined. The compound is an octahedral iridium(III) complex with trans tri­methyl­phosphine and cis chloride ligands.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](O-C) = 0.011 Å
• R factor = 0.042
• wR factor = 0.100
• Data-to-parameter ratio = 24.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         P2

Alert level C
PLAT128_ALERT_4_C Non-standard setting of Space group Pc      ....    Pn
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.31 Ratio
PLAT731_ALERT_1_C Bond    Calc     1.60(7), Rep     1.60(2) ......       3.50 su-Rat
              IR1  -H1      1.555   1.555

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.57
           From the CIF: _reflns_number_total               3176
           Count of symmetry unique reflns         1694
           Completeness (_total/calc)            187.49%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1482
           Fraction of Friedel pairs measured     0.875
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1996); cell refinement: SAINT (Bruker, 1996); data reduction: SHELXTL (Bruker, 2001) and SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(1)

Crystal data

[IrCl2H(C3H9P)2(CO)]	F(000) = 420
Mr = 444.26	Dx = 2.031 Mg m^−3
Monoclinic, Pn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P -2yac	Cell parameters from 5819 reflections
a = 6.472 (2) Å	θ = 2–40°
b = 13.156 (4) Å	µ = 9.75 mm^−1
c = 8.598 (3) Å	T = 173 K
β = 97.157 (5)°	Block, orange
V = 726.4 (4) Å^3	0.20 × 0.10 × 0.05 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	3176 independent reflections
Radiation source: fine-focus sealed tube	2964 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.075
Detector resolution: 8.192 pixels mm^-1	θmax = 27.6°, θmin = 1.6°
frames, each covering 0.3° in ω scans	h = −8→8
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	k = −16→17
Tmin = 0.310, Tmax = 0.613	l = −11→11
7494 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.042	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.100	w = 1/[σ^2(Fo^2) + (0.0144P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max < 0.001
3176 reflections	Δρmax = 2.70 e Å^−3
128 parameters	Δρmin = −3.57 e Å^−3
3 restraints	Absolute structure: Flack (1983), 1482 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.149 (13)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	1.0420 (13)	0.3113 (7)	0.7435 (10)	0.0320 (17)
C2	1.1657 (18)	0.4692 (7)	1.0321 (11)	0.049 (2)
H2A	1.2090	0.5129	1.1227	0.073*
H2B	1.0541	0.5027	0.9632	0.073*
H2C	1.2847	0.4570	0.9744	0.073*
C3	1.2949 (16)	0.2941 (8)	1.2214 (12)	0.046 (2)
H3A	1.4056	0.2788	1.1569	0.070*
H3B	1.2511	0.2313	1.2690	0.070*
H3C	1.3471	0.3423	1.3040	0.070*
C4	0.8931 (15)	0.3871 (7)	1.2353 (12)	0.041 (2)
H4A	0.9711	0.4178	1.3286	0.062*
H4B	0.8185	0.3269	1.2659	0.062*
H4C	0.7929	0.4365	1.1850	0.062*
C5	0.786 (3)	0.1484 (13)	0.5178 (13)	0.106 (7)
H5A	0.9322	0.1379	0.5025	0.159*
H5B	0.7452	0.2183	0.4891	0.159*
H5C	0.6980	0.1008	0.4515	0.159*
C6	0.831 (3)	−0.0049 (9)	0.7503 (18)	0.085 (4)
H6A	0.7468	−0.0486	0.6748	0.127*
H6B	0.8083	−0.0240	0.8570	0.127*
H6C	0.9787	−0.0132	0.7381	0.127*
C7	0.4731 (17)	0.1223 (10)	0.7128 (17)	0.074 (4)
H7A	0.4100	0.1827	0.6597	0.112*
H7B	0.4393	0.1204	0.8208	0.112*
H7C	0.4184	0.0612	0.6570	0.112*
Cl1	0.6100 (4)	0.35400 (16)	0.8662 (3)	0.0414 (5)
Cl2	0.7829 (4)	0.14469 (16)	1.0945 (3)	0.0403 (5)
Ir1	0.92263 (18)	0.242795 (17)	0.89647 (15)	0.02626 (11)
O1	1.1115 (11)	0.3544 (6)	0.6500 (8)	0.0538 (18)
P1	1.0728 (3)	0.35008 (16)	1.0984 (3)	0.0307 (4)
P2	0.7558 (4)	0.12727 (18)	0.7147 (3)	0.0365 (5)
H1	1.135 (10)	0.179 (7)	0.917 (11)	0.055*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.030 (4)	0.035 (5)	0.032 (4)	0.003 (3)	0.007 (3)	0.000 (3)
C2	0.068 (6)	0.020 (4)	0.064 (6)	−0.009 (4)	0.030 (5)	−0.005 (4)
C3	0.042 (5)	0.044 (6)	0.051 (5)	0.000 (4)	−0.001 (4)	−0.005 (5)
C4	0.043 (5)	0.028 (4)	0.058 (5)	−0.002 (4)	0.023 (4)	−0.011 (4)
C5	0.159 (17)	0.104 (13)	0.049 (8)	−0.069 (12)	−0.009 (9)	0.001 (7)
C6	0.102 (10)	0.037 (6)	0.105 (10)	0.028 (7)	−0.026 (8)	−0.032 (7)
C7	0.046 (6)	0.058 (8)	0.116 (11)	−0.010 (5)	0.000 (7)	−0.040 (7)
Cl1	0.0392 (11)	0.0245 (10)	0.0613 (13)	0.0097 (8)	0.0102 (10)	0.0045 (9)
Cl2	0.0568 (13)	0.0218 (10)	0.0443 (11)	−0.0015 (9)	0.0147 (10)	0.0042 (8)
Ir1	0.02997 (17)	0.01981 (15)	0.03020 (16)	0.0048 (2)	0.00845 (12)	0.0010 (3)
O1	0.053 (4)	0.054 (5)	0.055 (4)	−0.003 (3)	0.009 (3)	0.015 (3)
P1	0.0358 (11)	0.0192 (10)	0.0389 (11)	−0.0025 (8)	0.0119 (9)	−0.0018 (8)
P2	0.0427 (12)	0.0279 (12)	0.0385 (11)	0.0043 (9)	0.0035 (10)	−0.0019 (9)

Geometric parameters (Å, º)

C1—O1	1.123 (11)	C5—H5B	0.9800
C1—Ir1	1.842 (9)	C5—H5C	0.9800
C2—P1	1.797 (9)	C6—P2	1.821 (12)
C2—H2A	0.9800	C6—H6A	0.9800
C2—H2B	0.9800	C6—H6B	0.9800
C2—H2C	0.9800	C6—H6C	0.9800
C3—P1	1.830 (10)	C7—P2	1.829 (12)
C3—H3A	0.9800	C7—H7A	0.9800
C3—H3B	0.9800	C7—H7B	0.9800
C3—H3C	0.9800	C7—H7C	0.9800
C4—P1	1.821 (9)	Cl1—Ir1	2.484 (2)
C4—H4A	0.9800	Cl2—Ir1	2.401 (3)
C4—H4B	0.9800	Ir1—P2	2.345 (3)
C4—H4C	0.9800	Ir1—P1	2.352 (3)
C5—P2	1.751 (12)	Ir1—H1	1.60 (2)
C5—H5A	0.9800
O1—C1—Ir1	178.6 (8)	P2—C7—H7B	109.5
P1—C2—H2A	109.5	H7A—C7—H7B	109.5
P1—C2—H2B	109.5	P2—C7—H7C	109.5
H2A—C2—H2B	109.5	H7A—C7—H7C	109.5
P1—C2—H2C	109.5	H7B—C7—H7C	109.5
H2A—C2—H2C	109.5	C1—Ir1—P2	92.3 (3)
H2B—C2—H2C	109.5	C1—Ir1—P1	93.6 (3)
P1—C3—H3A	109.5	P2—Ir1—P1	174.11 (12)
P1—C3—H3B	109.5	C1—Ir1—Cl2	176.3 (3)
H3A—C3—H3B	109.5	P2—Ir1—Cl2	86.63 (9)
P1—C3—H3C	109.5	P1—Ir1—Cl2	87.51 (10)
H3A—C3—H3C	109.5	C1—Ir1—Cl1	92.6 (3)
H3B—C3—H3C	109.5	P2—Ir1—Cl1	90.60 (10)
P1—C4—H4A	109.5	P1—Ir1—Cl1	88.86 (9)
P1—C4—H4B	109.5	Cl2—Ir1—Cl1	90.98 (10)
H4A—C4—H4B	109.5	C1—Ir1—H1	84 (4)
P1—C4—H4C	109.5	P2—Ir1—H1	93 (4)
H4A—C4—H4C	109.5	P1—Ir1—H1	88 (4)
H4B—C4—H4C	109.5	Cl2—Ir1—H1	92 (4)
P2—C5—H5A	109.5	Cl1—Ir1—H1	176 (4)
P2—C5—H5B	109.5	C2—P1—C4	103.7 (4)
H5A—C5—H5B	109.5	C2—P1—C3	105.3 (5)
P2—C5—H5C	109.5	C4—P1—C3	104.7 (5)
H5A—C5—H5C	109.5	C2—P1—Ir1	114.4 (3)
H5B—C5—H5C	109.5	C4—P1—Ir1	113.5 (3)
P2—C6—H6A	109.5	C3—P1—Ir1	114.1 (3)
P2—C6—H6B	109.5	C5—P2—C6	104.7 (9)
H6A—C6—H6B	109.5	C5—P2—C7	103.3 (8)
P2—C6—H6C	109.5	C6—P2—C7	102.4 (7)
H6A—C6—H6C	109.5	C5—P2—Ir1	116.3 (5)
H6B—C6—H6C	109.5	C6—P2—Ir1	114.6 (4)
P2—C7—H7A	109.5	C7—P2—Ir1	114.0 (4)
C1—Ir1—P1—C2	17.7 (5)	C1—Ir1—P2—C5	−3.4 (8)
Cl2—Ir1—P1—C2	−165.9 (4)	Cl2—Ir1—P2—C5	−179.8 (8)
Cl1—Ir1—P1—C2	−74.8 (4)	Cl1—Ir1—P2—C5	89.3 (8)
C1—Ir1—P1—C4	136.5 (5)	C1—Ir1—P2—C6	119.2 (7)
Cl2—Ir1—P1—C4	−47.0 (4)	Cl2—Ir1—P2—C6	−57.3 (7)
Cl1—Ir1—P1—C4	44.0 (4)	Cl1—Ir1—P2—C6	−148.2 (7)
C1—Ir1—P1—C3	−103.6 (5)	C1—Ir1—P2—C7	−123.4 (6)
Cl2—Ir1—P1—C3	72.8 (4)	Cl2—Ir1—P2—C7	60.2 (6)
Cl1—Ir1—P1—C3	163.8 (4)	Cl1—Ir1—P2—C7	−30.8 (6)