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In the structure of the title compound, [Ir2Cl3H2(C36H28P2)2]BF4·2CH2Cl2, the bimetallic cation features a confacial bi­octa­hedral structure that is held together by three bridging chloride ions and is very close to C2 symmetric. The hydrides are in a syn orientation (trans to the same halide bridge), and the chelating bis­(phosphine) atropisomers display a racemic (R,R)/(S,S) configuration. Because of the high trans-bond-weakening influence of the hydride ligands, the Ir—Cl bonds trans to Ir—H [2.5262 (7) and 2.5365 (7) Å] are significantly longer than those opposite the Ir—P linkages [2.4287 (7)–2.4672 (8) Å]. The Ir—P distances vary between 2.2464 (9) and 2.2565 (8) Å. This study illustrates the usefulness of steri­cally demanding biaryl-based P2 ligands in the synthesis of halide-bridged Ir2 complexes, which are valuable precursors of versatile catalysts for homogeneous C=O hydrogenation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108004198/jz3123sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108004198/jz3123Isup2.hkl
Contains datablock I

CCDC reference: 682803

Comment top

Recently, we reported on the oxidative addition of HCl to several bis(phosphine)-coordinated (cyclooctadiene)iridium(I) complexes, namely [Ir(η4-1,5-C8H12)L2]BF4 with L2 = (R)-2,2'-bis(diphenylphosphino)-1,1'-binaphthyl [(R)-binap)], (2S,4S)-2,4-bis(diphenylphosphino)pentane [(S,S)-bdpp], and (1S,2S)-bis(diphenylphosphino)cyclopentane [(S,S)-bdpcp]. Whereas reactions between hydrogen chloride and [Ir(η4-1,5-C8H12){(S,S)-bdpp}]BF4 or [Ir(η4-1,5-C8H12){(S,S)-bdpcp}]BF4 yielded the usual mononuclear adducts, similar treatment of [Ir(η4-1,5-C8H12){(R)-binap}]BF4 furnished the triply chlorido-bridged diiridium complex [Ir2(H)2{(R)-binap}2(µ-Cl)3]BF4. We proposed that the action of HCl on the (R)-binap-containing precursor also produces a mononuclear iridium(III) complex as a first intermediate, where the greater bulkiness of the two `Ph2Pnaphthyl' building blocks of the binap ligand compared with that of the two `Ph2Palkyl' halves of the bdpp and bdpcp chelate phosphines facilitates the decoordination of the diene ligand through steric pressure. Bridge-closing combination of the remaining [Ir(H)(Cl){(R)-binap}]+ fragments would then lead to [Ir2(H)2{(R)-binap}2(µ-Cl)2]2+, which stabilizes to [Ir2(H)2{(R)-binap}2(µ-Cl)3]+ by the addition of an extra chloride ion provided by the excess of HCl (Dahlenburg et al., 2007). We expected that the formation of triply halido-bridged diiridium complexes [Ir2(H)2(L2)(µ-X)3]+ from hydrogen halides HX and iridium(I) cations [Ir(η4-1,5-C8H12)L2]+ bearing sterically congested bis(phosphines) similar to, or different from, the binap ligand could be a general reaction. Hence, we set out to prepare additional members of this family of compounds because previous work had shown that opening of the µ-Cl bridges of [Ir2(H)2{(R)-binap}2(µ-Cl)3]BF4 by various N,N nucleophiles presents a useful method of synthesis for the otherwise involved mixed-ligand bis(chelates) [Ir(H)(Cl){(R)-binap}(1,2-diamine)]BF4, which are of interest as (pre)catalysts for the enantioselective hydrogenation of ketones (Dahlenburg et al., 2007).

In this context, we came across the reaction between hydrogen chloride and [Ir(η4-1,5-C8H12)(rac-biphep)]BF4, where rac-biphep is racemic 2,2'-bis(diphenylphosphino)-1,1'-biphenyl as an examplary binap-like chelate ligand which, because of its chiral flexibility, cannot be obtained as resolved enantiomers but can adopt stereochemically robust atropisomeric conformations in metal complexes bearing enantiopure coligands (Becker et al., 2001; Korenaga et al., 2001; Mikami et al., 2001, 2002, 2004, 2005a,b). As anticipated, bimetallic [Ir2(H)2(biphep)2(µ-Cl)3]BF4 was isolated from the reaction solution. 1H and 31P{1H} NMR spectroscopy proved the presence, in a 1:1 molar ratio, of two diastereomers, (I) and (II), differing only in the relative disposition of the hydride ligands and the pairwise configuration of the axially chiral bis(phosphine) chelates, which is syn or anti (trans to the same or to two different bridging chlorides) with regard to the orientation of the two Ir—H bonds, and (R,R)/(S,S) or (R,S) with regard to the chirality of the pair of possible biphep atropisomers. The racemic syn form, (I), with the two biphep ligands in an (R,R) or (S,S) configuration, could be separated as the title addition compound (I)·2CH2Cl2 by crystallizing the isomeric mixture from CH2Cl2–diethyl ether, and this structure is presented here.

The molecular structure of the title (S,S) enantiomeric complex salt, including the CH2Cl2 solvent molecules, is shown in Fig. 1. While a few structural studies on biphep complexes of Ru, Rh, Pd and Pt have been reported in recent years (Becker et al., 2001; Doherty et al., 2005; Korenaga et al., 2001; Mikami et al., 2001, 2002, 2004, 2005a,b; Osawara et al., 2000), the title compound appears to be the first crystallographically characterized example with iridium as the central metal (Cambridge Structural Database, Version 5.28; Allen, 2002).

The geometry of the bimetallic cation can be described as triply chlorido-bridged confacial bioctahedral, with two syn-aligned Ir—H bonds trans to the same halide bridge. The overall structure of the cationic component is virtually C2 symmetric, with the twofold rotation axis passing through the midpoints of the Ir···Ir vector and the chloride ligand Cl1 trans to both hydrides.

The pairwise shared coordination planes spanned by one metal centre and two bridging chloride ligands are inclined to each other at angles between 120.81 (5) and 127.01 (5)°, with the interplanar angles of the three Ir(µ-Cl)Ir bridges varying from 118.20 (2) to 121.61 (2)°. All of these parameters compare favourably with those determined previously for the related binap complex [Ir2(H)2{(R)-binap}2(µ-Cl)3]BF4 (Dahlenburg et al., 2007). The greater chiral flexibility of the biphep system than that of the binap ligand is mirrored by the angles between the normals to the two pairs of phenyl planes in the biphenyl units, which amount to 61.0 (1) and 65.7 (1)° and thus clearly fall below the range of 68–81° spanned by the corresponding dihedral angles between the naphthyl planes in [Ir2(H)2{(R)-binap}2(µ-Cl)3]BF4 (Dahlenburg et al., 2007) and [Ir2(H)2{(R)-binap}2(µ-Cl)(µ-OCH3)2]Cl (Tani et al., 1998a,b).

As a result of the high trans-bond-weakening influence of the hydride ligands, the Ir—Cl bonds trans to Ir—H are much longer than those opposite Ir—P (Table 1) and are amongst the longest IrIII—µ-Cl distances reported to date (Dahlenburg et al., 2007). The Ir—P bond lengths and the obtuse P—Ir—P angles agree well with the corresponding distances and valence angles of structurally characterized iridium complexes of the binap ligand (Dahlenburg et al., 2007; Dorta et al., 1997; Tani et al.,1998a,b; Yamagata et al., 1997, 2006).

Related literature top

For related literature, see: Allen (2002); Becker et al. (2001); Dahlenburg et al. (2007); Doherty et al. (2005); Dorta et al. (1997); Korenaga et al. (2001); Mikami et al. (2001, 2002, 2004, 2005a, 2005b); Osawara et al. (2000); Tani et al. (1998a, 1998b); Yamagata et al. (1997, 2006).

Experimental top

A solution of dry hydrogen chloride in diethyl ether was added dropwise to a THF solution (30 ml) of [Ir(η4-1,5-C8H12)(rac-biphep)]BF4 (142 mg, 0.16 mmol), which was obtained from [Ir2(η4-1,5-C8H12)2(µ-Cl)2] and the phosphine in the presence of AgBF4, similar to the procedure previously described for the preparation of [Ir(η4-1,5-C8H12){(R)-binap}]BF4 and related complex salts (Dahlenburg et al., 2007). The dark-red mixture gradually became pale yellow and the addition of HCl was stopped when no further alteration of the colour was discernible. After stirring for an additional 30 min and concentration of the solution to ~1 ml, the product was precipitated by adding diethyl ether (50 ml), washed with 3 × 2 ml of the same solvent and dried under vacuum. Yield: 120 mg (95%) of colourless [Ir2(H)2(biphep)2(µ-Cl)3]BF4 as a 1:1 molar mixture of the syn-(R,R)/(S,S) diastereomer, (I), and the anti-(R,S) form, (II). Elemental analysis, found: C 53.74, H 3.85%; calculated for C72H58BCl3F4Ir2P4 (1624.75): C 53.23, H 3.60%. Spectroscopic analysis for (I): 1H NMR (CDCl3, δ, p.p.m.): -23.04 (dd, 2JP,H = 15.61, 2JP',H = 21.67 Hz, 2 IrH); 31P{1H} NMR (CDCl3, δ, p.p.m.): -1.67, -7.52 (both d, 2JP,P' = 20.0 Hz, 1 P each). Spectroscopic analysis for (II): 1H NMR (CDCl3, δ, p.p.m.): -22.47 (dd, 2JP,H = 16.07, 2JP',H = 22.01 Hz, 1 IrH), -22.73 (dd, 2JP,H = 16.66, 2JP',H = 21.43 Hz, 1 IrH); 31P{1H} NMR (CDCl3, δ, p.p.m.): 0.00, -1.96, -4.14, -7.43 (all d, 2JP,P' = 18.0 Hz each, all 1 P).

Slow diffusion of diethyl ether into a saturated solution of the isomeric mixture in CH2Cl2 resulted in the deposition of single crystals of the title addition compound (I)·2CH2Cl2.

Refinement top

Carbon-bonded H atoms were positioned geometrically, with C—H = 0.95–0.99 Å, and refined using appropriate riding models, with Uiso(H) = 1.2Ueq(C). The positions of the two hydride ligands were derived from a final ΔF map; during refinement, their Uiso values were fixed at 1.5Ueq(Ir).

Computing details top

Data collection: COLLECT (Bruker, 2002); cell refinement: EVALCCD (Duisenberg et al., 2003); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL (Bruker, 2002); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: publCIF (Version 1.9.2; Westrip, 2008).

Figures top
[Figure 1] Fig. 1. The structure of (I)·2CH2Cl2, including the two CH2Cl2 solvent molecules, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 40% probability level. Carbon-bonded H atoms of the complex cation have been omitted for clarity.
syn-Tri-µ-chlorido-bis{[(R,R)/(S,S)-2,2'-bis(diphenylphosphino)-1,1'- biphenyl]hydridoiridium(III)} tetrafluoridoborate dichloromethane disolvate top
Crystal data top
[Ir2Cl3H2(C36H28P2)2]BF4·2CH2Cl2Z = 2
Mr = 1794.48F(000) = 1760
Triclinic, P1Dx = 1.717 Mg m3
Hall symbol: -P1Mo Kα radiation, λ = 0.71073 Å
a = 13.6578 (14) ÅCell parameters from 339 reflections
b = 14.7640 (6) Åθ = 6.0–20.0°
c = 18.5300 (11) ŵ = 4.25 mm1
α = 68.701 (3)°T = 150 K
β = 86.357 (6)°Irregular, colourless
γ = 86.228 (5)°0.17 × 0.14 × 0.14 mm
V = 3470.5 (4) Å3
Data collection top
Bruker Nonius KappaCCD
diffractometer
16517 independent reflections
Radiation source: fine-focus sealed tube13333 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
Detector resolution: 9 pixels mm-1θmax = 27.9°, θmin = 3.3°
ω–rotations with 1.90 ° and 123 sec per frame scansh = 1717
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
k = 1919
Tmin = 0.463, Tmax = 0.550l = 2424
85276 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)] = 0.026Hydrogen site location: geom except Ir bound hydrogens difmap
wR(F2) = 0.052H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.014P)2 + 7.4384P]
where P = (Fo2 + 2Fc2)/3
16517 reflections(Δ/σ)max = 0.002
835 parametersΔρmax = 2.05 e Å3
0 restraintsΔρmin = 1.07 e Å3
Crystal data top
[Ir2Cl3H2(C36H28P2)2]BF4·2CH2Cl2γ = 86.228 (5)°
Mr = 1794.48V = 3470.5 (4) Å3
Triclinic, P1Z = 2
a = 13.6578 (14) ÅMo Kα radiation
b = 14.7640 (6) ŵ = 4.25 mm1
c = 18.5300 (11) ÅT = 150 K
α = 68.701 (3)°0.17 × 0.14 × 0.14 mm
β = 86.357 (6)°
Data collection top
Bruker Nonius KappaCCD
diffractometer
16517 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
13333 reflections with I > 2σ(I)
Tmin = 0.463, Tmax = 0.550Rint = 0.041
85276 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.052H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 2.05 e Å3
16517 reflectionsΔρmin = 1.07 e Å3
835 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ir10.863382 (9)0.661588 (8)0.684299 (7)0.01511 (3)
H10.906 (2)0.657 (2)0.6124 (19)0.023*
Ir20.739005 (9)0.861637 (8)0.689832 (6)0.01460 (3)
H20.721 (2)0.943 (2)0.6196 (19)0.022*
Cl10.78098 (6)0.70047 (5)0.79624 (4)0.01786 (15)
Cl20.71081 (6)0.74837 (5)0.62574 (4)0.02013 (15)
Cl30.90771 (6)0.82950 (5)0.64792 (4)0.01879 (15)
P11.00653 (6)0.59680 (5)0.73916 (4)0.01594 (16)
P20.81485 (6)0.51544 (6)0.69107 (5)0.01937 (17)
P30.58106 (6)0.87799 (6)0.72688 (4)0.01616 (16)
P40.78729 (6)0.98078 (5)0.72661 (4)0.01591 (16)
C10.9909 (2)0.4781 (2)0.81594 (17)0.0176 (6)
C20.9808 (3)0.4755 (2)0.89223 (19)0.0243 (7)
H2A0.98780.53320.90250.029*
C30.9608 (3)0.3897 (3)0.95296 (19)0.0290 (8)
H3A0.95220.38931.00440.035*
C40.9534 (3)0.3051 (2)0.9391 (2)0.0276 (8)
H4A0.94080.24610.98100.033*
C50.9644 (3)0.3061 (2)0.8645 (2)0.0249 (7)
H5A0.96140.24680.85570.030*
C60.9797 (2)0.3923 (2)0.80133 (18)0.0197 (7)
C70.9820 (2)0.3865 (2)0.72275 (18)0.0203 (7)
C81.0518 (3)0.3232 (2)0.7059 (2)0.0260 (7)
H8A1.09740.28730.74370.031*
C91.0559 (3)0.3116 (3)0.6351 (2)0.0348 (9)
H9A1.10440.26850.62430.042*
C100.9895 (3)0.3629 (3)0.5800 (2)0.0373 (9)
H10A0.99270.35570.53100.045*
C110.9180 (3)0.4247 (3)0.5961 (2)0.0312 (8)
H11A0.87170.45860.55820.037*
C120.9128 (2)0.4381 (2)0.66702 (19)0.0205 (7)
C131.0693 (2)0.6649 (2)0.78717 (17)0.0195 (6)
C141.0231 (3)0.7354 (2)0.81171 (18)0.0235 (7)
H14A0.95500.75080.80410.028*
C151.0754 (3)0.7840 (3)0.8475 (2)0.0277 (8)
H15A1.04270.83300.86320.033*
C161.1730 (3)0.7621 (3)0.8601 (2)0.0326 (9)
H16A1.20840.79600.88410.039*
C171.2199 (3)0.6901 (3)0.8377 (3)0.0461 (11)
H17A1.28750.67350.84720.055*
C181.1684 (3)0.6420 (3)0.8013 (2)0.0363 (9)
H18A1.20130.59280.78580.044*
C191.1034 (2)0.5841 (2)0.67083 (17)0.0182 (6)
C201.1126 (3)0.6600 (2)0.59978 (19)0.0251 (7)
H20A1.06570.71330.58680.030*
C211.1895 (3)0.6586 (3)0.54787 (19)0.0301 (8)
H21A1.19580.71120.49970.036*
C221.2575 (3)0.5803 (3)0.5663 (2)0.0287 (8)
H22A1.30960.57860.53030.034*
C231.2496 (3)0.5049 (2)0.63685 (19)0.0238 (7)
H23A1.29630.45150.64950.029*
C241.1734 (2)0.5071 (2)0.68928 (18)0.0197 (7)
H24A1.16880.45570.73830.024*
C250.7598 (2)0.4300 (2)0.7795 (2)0.0225 (7)
C260.7349 (3)0.4547 (2)0.8439 (2)0.0283 (8)
H26A0.74550.51820.84260.034*
C270.6943 (3)0.3858 (3)0.9107 (2)0.0393 (10)
H27A0.67750.40250.95500.047*
C280.6785 (3)0.2934 (3)0.9127 (3)0.0441 (11)
H28A0.65060.24690.95820.053*
C290.7032 (3)0.2686 (3)0.8488 (3)0.0413 (10)
H29A0.69230.20500.85050.050*
C300.7436 (3)0.3357 (3)0.7826 (2)0.0323 (8)
H30A0.76060.31800.73880.039*
C310.7215 (3)0.5375 (2)0.6190 (2)0.0268 (8)
C320.6267 (3)0.5074 (3)0.6415 (2)0.0331 (9)
H32A0.61110.46830.69390.040*
C330.5543 (3)0.5350 (3)0.5870 (3)0.0462 (11)
H33A0.48920.51460.60240.055*
C340.5759 (3)0.5910 (3)0.5116 (3)0.0490 (13)
H34A0.52560.61000.47520.059*
C350.6704 (4)0.6201 (3)0.4879 (2)0.0411 (11)
H35A0.68550.65730.43500.049*
C360.7432 (3)0.5946 (2)0.5418 (2)0.0315 (9)
H36A0.80780.61620.52610.038*
C370.5708 (2)0.8909 (2)0.82169 (17)0.0168 (6)
C380.5480 (2)0.8120 (2)0.88836 (19)0.0231 (7)
H38A0.53130.75260.88430.028*
C390.5494 (2)0.8194 (2)0.96044 (18)0.0216 (7)
H39A0.53630.76421.00560.026*
C400.5696 (2)0.9061 (2)0.96781 (19)0.0238 (7)
H40A0.56950.91091.01750.029*
C410.5898 (2)0.9853 (2)0.90182 (19)0.0217 (7)
H41A0.60251.04530.90660.026*
C420.5920 (2)0.9798 (2)0.82814 (17)0.0175 (6)
C430.6133 (2)1.0712 (2)0.76059 (17)0.0172 (6)
C440.5465 (2)1.1504 (2)0.74946 (19)0.0231 (7)
H44A0.48921.14310.78250.028*
C450.5623 (3)1.2395 (2)0.6911 (2)0.0288 (8)
H45A0.51521.29210.68340.035*
C460.6466 (3)1.2511 (2)0.6444 (2)0.0302 (8)
H46A0.65821.31230.60470.036*
C470.7143 (3)1.1741 (2)0.65520 (19)0.0264 (8)
H47A0.77281.18320.62330.032*
C480.6982 (2)1.0831 (2)0.71230 (17)0.0183 (6)
C490.5116 (2)0.7734 (2)0.73181 (19)0.0204 (7)
C500.5394 (3)0.6791 (2)0.7797 (2)0.0256 (7)
H50A0.59170.66910.81360.031*
C510.4915 (3)0.5997 (3)0.7784 (2)0.0317 (8)
H51A0.51000.53600.81220.038*
C520.4169 (3)0.6132 (3)0.7281 (2)0.0364 (9)
H52A0.38440.55880.72680.044*
C530.3898 (3)0.7061 (3)0.6795 (2)0.0389 (9)
H53A0.33900.71540.64450.047*
C540.4360 (3)0.7860 (3)0.6815 (2)0.0300 (8)
H54A0.41610.84970.64840.036*
C550.5052 (2)0.9803 (2)0.66626 (18)0.0204 (7)
C560.4162 (3)1.0031 (3)0.6984 (2)0.0274 (8)
H56A0.39930.96890.75160.033*
C570.3524 (3)1.0750 (3)0.6534 (2)0.0335 (9)
H57A0.29221.09050.67590.040*
C580.3756 (3)1.1243 (3)0.5761 (2)0.0378 (10)
H58A0.33091.17270.54510.045*
C590.4635 (3)1.1032 (3)0.5440 (2)0.0401 (10)
H59A0.48021.13810.49090.048*
C600.5283 (3)1.0307 (3)0.5888 (2)0.0298 (8)
H60A0.58861.01590.56610.036*
C610.8238 (2)0.9573 (2)0.82518 (18)0.0190 (6)
C620.8528 (3)1.0351 (3)0.8435 (2)0.0283 (8)
H62A0.85281.09870.80520.034*
C630.8815 (3)1.0195 (3)0.9174 (2)0.0348 (9)
H63A0.90141.07240.92980.042*
C640.8814 (3)0.9271 (3)0.9734 (2)0.0317 (8)
H64A0.90310.91641.02360.038*
C650.8500 (3)0.8501 (3)0.95661 (19)0.0275 (8)
H65A0.84800.78710.99570.033*
C660.8213 (2)0.8654 (2)0.88226 (18)0.0215 (7)
H66A0.79980.81260.87050.026*
C670.8949 (2)1.0313 (2)0.66480 (19)0.0213 (7)
C680.8876 (3)1.0664 (2)0.58386 (19)0.0264 (8)
H68A0.82541.07100.56230.032*
C690.9698 (3)1.0942 (2)0.5353 (2)0.0319 (9)
H69A0.96401.11860.48070.038*
C701.0597 (3)1.0867 (3)0.5660 (3)0.0466 (11)
H70A1.11621.10600.53240.056*
C711.0693 (3)1.0516 (4)0.6448 (3)0.0488 (12)
H71A1.13221.04600.66560.059*
C720.9862 (3)1.0239 (3)0.6945 (2)0.0332 (9)
H72A0.99280.99990.74910.040*
B10.6658 (4)0.7034 (3)0.1944 (2)0.0326 (10)
F110.60863 (17)0.77401 (15)0.14101 (12)0.0376 (5)
F120.67463 (19)0.72846 (17)0.25906 (13)0.0453 (6)
F130.75870 (19)0.6974 (2)0.16131 (15)0.0573 (7)
F140.6224 (2)0.61524 (18)0.21617 (17)0.0687 (9)
C1000.7413 (3)0.9350 (3)0.1381 (2)0.0366 (9)
H10B0.74930.89360.10610.044*
H10C0.69960.90090.18450.044*
Cl110.85706 (9)0.95000 (10)0.16734 (8)0.0577 (3)
Cl120.68270 (9)1.04513 (9)0.08503 (8)0.0564 (3)
C2000.3078 (4)0.4082 (5)0.9488 (4)0.0719 (16)
H20B0.30310.44490.89250.086*
H20C0.31440.33800.95700.086*
Cl210.41236 (10)0.44210 (9)0.98166 (8)0.0609 (3)
Cl220.20185 (11)0.43078 (12)0.99651 (9)0.0786 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.01962 (7)0.01236 (6)0.01465 (6)0.00167 (5)0.00436 (5)0.00625 (5)
Ir20.01946 (7)0.01146 (6)0.01296 (6)0.00000 (5)0.00029 (5)0.00469 (5)
Cl10.0236 (4)0.0148 (3)0.0150 (3)0.0018 (3)0.0013 (3)0.0049 (3)
Cl20.0255 (4)0.0181 (3)0.0201 (4)0.0052 (3)0.0090 (3)0.0105 (3)
Cl30.0227 (4)0.0138 (3)0.0191 (4)0.0007 (3)0.0041 (3)0.0058 (3)
P10.0197 (4)0.0132 (4)0.0161 (4)0.0004 (3)0.0034 (3)0.0063 (3)
P20.0231 (4)0.0150 (4)0.0231 (4)0.0023 (3)0.0101 (3)0.0096 (3)
P30.0193 (4)0.0136 (4)0.0161 (4)0.0018 (3)0.0020 (3)0.0056 (3)
P40.0201 (4)0.0130 (4)0.0151 (4)0.0028 (3)0.0036 (3)0.0060 (3)
C10.0163 (15)0.0162 (14)0.0181 (15)0.0023 (12)0.0049 (12)0.0028 (12)
C20.0288 (19)0.0228 (16)0.0214 (16)0.0070 (14)0.0041 (14)0.0067 (14)
C30.036 (2)0.0323 (19)0.0165 (16)0.0077 (16)0.0037 (14)0.0049 (14)
C40.0287 (19)0.0204 (16)0.0245 (17)0.0053 (14)0.0053 (14)0.0040 (14)
C50.0252 (18)0.0170 (15)0.0310 (18)0.0016 (14)0.0063 (14)0.0059 (14)
C60.0176 (16)0.0171 (15)0.0235 (16)0.0015 (12)0.0085 (13)0.0054 (13)
C70.0263 (18)0.0125 (14)0.0229 (16)0.0007 (13)0.0057 (13)0.0067 (13)
C80.0284 (19)0.0182 (16)0.0317 (19)0.0041 (14)0.0093 (15)0.0090 (14)
C90.037 (2)0.032 (2)0.043 (2)0.0129 (17)0.0091 (18)0.0241 (18)
C100.049 (3)0.037 (2)0.037 (2)0.0134 (19)0.0122 (18)0.0265 (18)
C110.043 (2)0.0265 (18)0.0302 (19)0.0115 (16)0.0186 (17)0.0172 (16)
C120.0241 (17)0.0149 (15)0.0263 (17)0.0016 (13)0.0075 (14)0.0113 (13)
C130.0231 (17)0.0195 (15)0.0166 (15)0.0053 (13)0.0016 (13)0.0065 (13)
C140.0251 (18)0.0257 (17)0.0225 (16)0.0016 (14)0.0024 (14)0.0118 (14)
C150.036 (2)0.0255 (17)0.0276 (18)0.0050 (16)0.0005 (15)0.0160 (15)
C160.033 (2)0.041 (2)0.035 (2)0.0145 (17)0.0006 (16)0.0252 (18)
C170.024 (2)0.070 (3)0.067 (3)0.000 (2)0.0119 (19)0.049 (3)
C180.027 (2)0.044 (2)0.051 (2)0.0039 (17)0.0095 (18)0.034 (2)
C190.0200 (16)0.0188 (15)0.0181 (15)0.0002 (13)0.0039 (12)0.0089 (13)
C200.0297 (19)0.0200 (16)0.0217 (16)0.0049 (14)0.0032 (14)0.0036 (13)
C210.037 (2)0.0288 (18)0.0174 (16)0.0035 (16)0.0030 (15)0.0007 (14)
C220.0291 (19)0.035 (2)0.0229 (17)0.0023 (16)0.0013 (14)0.0130 (15)
C230.0240 (18)0.0228 (16)0.0264 (17)0.0038 (14)0.0059 (14)0.0109 (14)
C240.0210 (17)0.0193 (15)0.0194 (15)0.0008 (13)0.0069 (13)0.0068 (13)
C250.0184 (16)0.0160 (15)0.0327 (18)0.0025 (13)0.0071 (14)0.0069 (14)
C260.0268 (19)0.0199 (16)0.037 (2)0.0031 (14)0.0004 (15)0.0085 (15)
C270.040 (2)0.034 (2)0.039 (2)0.0062 (18)0.0103 (18)0.0090 (18)
C280.033 (2)0.026 (2)0.061 (3)0.0117 (17)0.011 (2)0.0014 (19)
C290.034 (2)0.0232 (19)0.066 (3)0.0126 (17)0.002 (2)0.013 (2)
C300.0257 (19)0.0252 (18)0.052 (2)0.0045 (15)0.0092 (17)0.0196 (17)
C310.034 (2)0.0187 (16)0.0346 (19)0.0097 (15)0.0185 (16)0.0175 (15)
C320.031 (2)0.0289 (19)0.050 (2)0.0094 (16)0.0197 (18)0.0257 (18)
C330.034 (2)0.050 (3)0.071 (3)0.016 (2)0.029 (2)0.039 (2)
C340.051 (3)0.047 (3)0.066 (3)0.028 (2)0.044 (2)0.039 (2)
C350.065 (3)0.030 (2)0.038 (2)0.021 (2)0.032 (2)0.0230 (18)
C360.042 (2)0.0248 (18)0.036 (2)0.0116 (16)0.0201 (17)0.0202 (16)
C370.0157 (15)0.0182 (15)0.0166 (15)0.0013 (12)0.0011 (12)0.0063 (12)
C380.0244 (18)0.0212 (16)0.0230 (17)0.0036 (14)0.0004 (14)0.0069 (14)
C390.0154 (16)0.0208 (16)0.0196 (16)0.0034 (13)0.0038 (12)0.0031 (13)
C400.0225 (17)0.0335 (19)0.0166 (15)0.0024 (15)0.0012 (13)0.0107 (14)
C410.0198 (17)0.0243 (16)0.0258 (17)0.0012 (13)0.0000 (13)0.0148 (14)
C420.0165 (15)0.0180 (15)0.0172 (15)0.0007 (12)0.0017 (12)0.0058 (12)
C430.0212 (16)0.0164 (14)0.0174 (15)0.0035 (13)0.0007 (12)0.0097 (12)
C440.0228 (17)0.0205 (16)0.0282 (17)0.0009 (13)0.0019 (14)0.0120 (14)
C450.034 (2)0.0201 (17)0.0326 (19)0.0057 (15)0.0019 (16)0.0116 (15)
C460.043 (2)0.0138 (15)0.0286 (18)0.0010 (15)0.0062 (16)0.0024 (14)
C470.036 (2)0.0168 (16)0.0238 (17)0.0014 (14)0.0100 (15)0.0060 (14)
C480.0259 (18)0.0123 (14)0.0175 (15)0.0012 (13)0.0013 (13)0.0069 (12)
C490.0216 (17)0.0174 (15)0.0250 (17)0.0050 (13)0.0013 (13)0.0108 (13)
C500.0240 (18)0.0234 (17)0.0322 (19)0.0052 (14)0.0007 (15)0.0127 (15)
C510.028 (2)0.0204 (17)0.046 (2)0.0061 (15)0.0070 (17)0.0121 (16)
C520.035 (2)0.0275 (19)0.054 (3)0.0137 (17)0.0046 (19)0.0222 (18)
C530.037 (2)0.041 (2)0.048 (2)0.0083 (19)0.0097 (19)0.024 (2)
C540.031 (2)0.0278 (18)0.035 (2)0.0039 (16)0.0058 (16)0.0147 (16)
C550.0235 (17)0.0171 (15)0.0221 (16)0.0005 (13)0.0064 (13)0.0083 (13)
C560.0258 (19)0.0302 (19)0.0282 (18)0.0033 (15)0.0048 (15)0.0130 (15)
C570.029 (2)0.038 (2)0.039 (2)0.0089 (17)0.0105 (17)0.0215 (18)
C580.043 (2)0.0282 (19)0.044 (2)0.0161 (18)0.0236 (19)0.0150 (18)
C590.053 (3)0.035 (2)0.0235 (19)0.0079 (19)0.0120 (18)0.0002 (16)
C600.033 (2)0.0277 (18)0.0251 (18)0.0028 (16)0.0031 (15)0.0058 (15)
C610.0173 (16)0.0224 (16)0.0199 (15)0.0014 (13)0.0010 (12)0.0109 (13)
C620.036 (2)0.0260 (18)0.0262 (18)0.0088 (16)0.0031 (15)0.0123 (15)
C630.040 (2)0.041 (2)0.035 (2)0.0130 (18)0.0011 (17)0.0261 (18)
C640.031 (2)0.049 (2)0.0219 (17)0.0056 (17)0.0019 (15)0.0199 (17)
C650.0304 (19)0.0321 (19)0.0193 (16)0.0010 (16)0.0016 (14)0.0089 (15)
C660.0230 (17)0.0219 (16)0.0220 (16)0.0005 (13)0.0002 (13)0.0113 (14)
C670.0275 (18)0.0128 (14)0.0255 (17)0.0071 (13)0.0094 (14)0.0100 (13)
C680.033 (2)0.0172 (16)0.0262 (18)0.0011 (14)0.0086 (15)0.0059 (14)
C690.040 (2)0.0211 (17)0.0317 (19)0.0044 (16)0.0178 (17)0.0082 (15)
C700.044 (3)0.051 (3)0.049 (3)0.028 (2)0.028 (2)0.024 (2)
C710.030 (2)0.073 (3)0.055 (3)0.025 (2)0.014 (2)0.036 (3)
C720.030 (2)0.043 (2)0.034 (2)0.0159 (17)0.0089 (16)0.0208 (18)
B10.043 (3)0.023 (2)0.030 (2)0.0067 (19)0.0082 (19)0.0076 (17)
F110.0452 (14)0.0332 (12)0.0292 (11)0.0089 (10)0.0106 (10)0.0053 (9)
F120.0616 (17)0.0434 (13)0.0302 (12)0.0071 (12)0.0106 (11)0.0126 (11)
F130.0485 (16)0.0715 (18)0.0565 (16)0.0227 (14)0.0083 (13)0.0319 (15)
F140.102 (2)0.0303 (13)0.0666 (18)0.0134 (15)0.0338 (17)0.0016 (13)
C1000.033 (2)0.039 (2)0.044 (2)0.0077 (18)0.0019 (18)0.0217 (19)
Cl110.0445 (7)0.0784 (8)0.0685 (8)0.0069 (6)0.0221 (6)0.0465 (7)
Cl120.0570 (7)0.0489 (6)0.0690 (8)0.0105 (6)0.0258 (6)0.0264 (6)
C2000.054 (3)0.095 (4)0.090 (4)0.006 (3)0.023 (3)0.059 (4)
Cl210.0541 (7)0.0497 (7)0.0836 (9)0.0070 (6)0.0114 (7)0.0276 (7)
Cl220.0504 (8)0.0973 (11)0.0725 (9)0.0026 (8)0.0027 (7)0.0130 (8)
Geometric parameters (Å, º) top
Ir1—P12.2518 (8)C33—H33A0.9500
Ir1—P22.2565 (8)C34—C351.381 (7)
Ir1—Cl32.4287 (7)C34—H34A0.9500
Ir1—Cl22.4672 (8)C35—C361.391 (5)
Ir1—Cl12.5262 (7)C35—H35A0.9500
Ir1—H11.44 (3)C36—H36A0.9500
Ir2—P32.2464 (9)C37—C381.391 (4)
Ir2—P42.2526 (8)C37—C421.411 (4)
Ir2—Cl22.4374 (7)C38—C391.381 (5)
Ir2—Cl32.4563 (8)C38—H38A0.9500
Ir2—Cl12.5365 (7)C39—C401.382 (5)
Ir2—H21.44 (3)C39—H39A0.9500
P1—C191.821 (3)C40—C411.379 (5)
P1—C11.828 (3)C40—H40A0.9500
P1—C131.843 (3)C41—C421.395 (4)
P2—C251.819 (3)C41—H41A0.9500
P2—C311.833 (3)C42—C431.500 (4)
P2—C121.840 (3)C43—C441.397 (4)
P3—C551.824 (3)C43—C481.398 (4)
P3—C371.830 (3)C44—C451.385 (5)
P3—C491.836 (3)C44—H44A0.9500
P4—C611.827 (3)C45—C461.377 (5)
P4—C671.827 (3)C45—H45A0.9500
P4—C481.828 (3)C46—C471.382 (5)
C1—C21.398 (4)C46—H46A0.9500
C1—C61.407 (4)C47—C481.396 (4)
C2—C31.384 (5)C47—H47A0.9500
C2—H2A0.9500C49—C541.392 (5)
C3—C41.373 (5)C49—C501.395 (5)
C3—H3A0.9500C50—C511.388 (5)
C4—C51.377 (5)C50—H50A0.9500
C4—H4A0.9500C51—C521.380 (6)
C5—C61.399 (4)C51—H51A0.9500
C5—H5A0.9500C52—C531.381 (6)
C6—C71.488 (4)C52—H52A0.9500
C7—C81.392 (5)C53—C541.387 (5)
C7—C121.413 (4)C53—H53A0.9500
C8—C91.380 (5)C54—H54A0.9500
C8—H8A0.9500C55—C601.382 (5)
C9—C101.380 (5)C55—C561.395 (5)
C9—H9A0.9500C56—C571.382 (5)
C10—C111.386 (5)C56—H56A0.9500
C10—H10A0.9500C57—C581.377 (6)
C11—C121.395 (5)C57—H57A0.9500
C11—H11A0.9500C58—C591.374 (6)
C13—C141.382 (4)C58—H58A0.9500
C13—C181.391 (5)C59—C601.393 (5)
C14—C151.391 (5)C59—H59A0.9500
C14—H14A0.9500C60—H60A0.9500
C15—C161.367 (5)C61—C661.385 (4)
C15—H15A0.9500C61—C621.398 (4)
C16—C171.381 (5)C62—C631.381 (5)
C16—H16A0.9500C62—H62A0.9500
C17—C181.389 (5)C63—C641.381 (5)
C17—H17A0.9500C63—H63A0.9500
C18—H18A0.9500C64—C651.382 (5)
C19—C201.390 (4)C64—H64A0.9500
C19—C241.392 (4)C65—C661.390 (4)
C20—C211.383 (5)C65—H65A0.9500
C20—H20A0.9500C66—H66A0.9500
C21—C221.389 (5)C67—C721.377 (5)
C21—H21A0.9500C67—C681.406 (5)
C22—C231.378 (5)C68—C691.379 (5)
C22—H22A0.9500C68—H68A0.9500
C23—C241.385 (5)C69—C701.366 (6)
C23—H23A0.9500C69—H69A0.9500
C24—H24A0.9500C70—C711.374 (6)
C25—C261.386 (5)C70—H70A0.9500
C25—C301.405 (4)C71—C721.399 (5)
C26—C271.395 (5)C71—H71A0.9500
C26—H26A0.9500C72—H72A0.9500
C27—C281.383 (6)B1—F141.378 (5)
C27—H27A0.9500B1—F111.384 (5)
C28—C291.376 (6)B1—F131.385 (5)
C28—H28A0.9500B1—F121.391 (5)
C29—C301.376 (6)C100—Cl121.738 (4)
C29—H29A0.9500C100—Cl111.756 (4)
C30—H30A0.9500C100—H10B0.9900
C31—C321.386 (5)C100—H10C0.9900
C31—C361.394 (5)C200—Cl221.725 (6)
C32—C331.393 (5)C200—Cl211.757 (5)
C32—H32A0.9500C200—H20B0.9900
C33—C341.365 (7)C200—H20C0.9900
P1—Ir1—P292.35 (3)C25—C30—H30A119.9
P1—Ir1—Cl395.11 (3)C32—C31—C36119.5 (3)
P2—Ir1—Cl3167.70 (3)C32—C31—P2120.7 (3)
P1—Ir1—Cl2174.05 (3)C36—C31—P2119.4 (3)
P2—Ir1—Cl293.52 (3)C31—C32—C33119.6 (4)
Cl3—Ir1—Cl279.29 (3)C31—C32—H32A120.2
P1—Ir1—Cl198.28 (3)C33—C32—H32A120.2
P2—Ir1—Cl1108.34 (3)C34—C33—C32120.7 (4)
Cl3—Ir1—Cl180.26 (2)C34—C33—H33A119.7
Cl2—Ir1—Cl178.91 (2)C32—C33—H33A119.7
P1—Ir1—H188.2 (14)C33—C34—C35120.5 (4)
P2—Ir1—H179.3 (13)C33—C34—H34A119.8
Cl3—Ir1—H191.2 (13)C35—C34—H34A119.8
Cl2—Ir1—H193.8 (13)C34—C35—C36119.6 (4)
Cl1—Ir1—H1169.6 (13)C34—C35—H35A120.2
P3—Ir2—P493.80 (3)C36—C35—H35A120.2
P3—Ir2—Cl295.58 (3)C35—C36—C31120.2 (4)
P4—Ir2—Cl2167.55 (3)C35—C36—H36A119.9
P3—Ir2—Cl3174.60 (3)C31—C36—H36A119.9
P4—Ir2—Cl391.50 (3)C38—C37—C42119.4 (3)
Cl2—Ir2—Cl379.33 (3)C38—C37—P3120.6 (2)
P3—Ir2—Cl197.83 (3)C42—C37—P3119.9 (2)
P4—Ir2—Cl1107.55 (3)C39—C38—C37120.4 (3)
Cl2—Ir2—Cl179.27 (2)C39—C38—H38A119.8
Cl3—Ir2—Cl179.53 (3)C37—C38—H38A119.8
P3—Ir2—H288.1 (13)C38—C39—C40121.0 (3)
P4—Ir2—H281.1 (13)C38—C39—H39A119.5
Cl2—Ir2—H291.1 (13)C40—C39—H39A119.5
Cl3—Ir2—H293.7 (13)C41—C40—C39118.9 (3)
Cl1—Ir2—H2169.1 (13)C41—C40—H40A120.5
Ir1—Cl1—Ir282.56 (2)C39—C40—H40A120.5
Ir2—Cl2—Ir185.85 (2)C40—C41—C42121.8 (3)
Ir1—Cl3—Ir286.28 (2)C40—C41—H41A119.1
C19—P1—C1108.54 (14)C42—C41—H41A119.1
C19—P1—C13100.68 (14)C41—C42—C37118.5 (3)
C1—P1—C13103.28 (14)C41—C42—C43117.0 (3)
C19—P1—Ir1114.03 (10)C37—C42—C43124.5 (3)
C1—P1—Ir1111.59 (10)C44—C43—C48118.9 (3)
C13—P1—Ir1117.60 (11)C44—C43—C42116.9 (3)
C25—P2—C31104.13 (16)C48—C43—C42124.0 (3)
C25—P2—C12101.49 (15)C45—C44—C43121.3 (3)
C31—P2—C12106.06 (15)C45—C44—H44A119.4
C25—P2—Ir1121.92 (11)C43—C44—H44A119.4
C31—P2—Ir1107.60 (11)C46—C45—C44119.5 (3)
C12—P2—Ir1114.27 (11)C46—C45—H45A120.2
C55—P3—C37103.64 (14)C44—C45—H45A120.2
C55—P3—C49102.05 (15)C45—C46—C47120.1 (3)
C37—P3—C49108.81 (14)C45—C46—H46A119.9
C55—P3—Ir2118.97 (11)C47—C46—H46A119.9
C37—P3—Ir2111.08 (10)C46—C47—C48121.0 (3)
C49—P3—Ir2111.48 (11)C46—C47—H47A119.5
C61—P4—C67104.80 (15)C48—C47—H47A119.5
C61—P4—C48101.26 (14)C47—C48—C43119.1 (3)
C67—P4—C48105.77 (14)C47—C48—P4121.2 (2)
C61—P4—Ir2122.08 (11)C43—C48—P4119.7 (2)
C67—P4—Ir2106.56 (10)C54—C49—C50118.5 (3)
C48—P4—Ir2114.99 (11)C54—C49—P3120.0 (3)
C2—C1—C6119.2 (3)C50—C49—P3121.1 (3)
C2—C1—P1117.3 (2)C51—C50—C49120.7 (3)
C6—C1—P1123.3 (2)C51—C50—H50A119.6
C3—C2—C1120.7 (3)C49—C50—H50A119.6
C3—C2—H2A119.6C52—C51—C50120.1 (3)
C1—C2—H2A119.6C52—C51—H51A119.9
C4—C3—C2120.2 (3)C50—C51—H51A119.9
C4—C3—H3A119.9C53—C52—C51119.6 (3)
C2—C3—H3A119.9C53—C52—H52A120.2
C3—C4—C5119.8 (3)C51—C52—H52A120.2
C3—C4—H4A120.1C52—C53—C54120.6 (4)
C5—C4—H4A120.1C52—C53—H53A119.7
C4—C5—C6121.5 (3)C54—C53—H53A119.7
C4—C5—H5A119.2C53—C54—C49120.3 (3)
C6—C5—H5A119.2C53—C54—H54A119.8
C5—C6—C1118.4 (3)C49—C54—H54A119.8
C5—C6—C7117.0 (3)C60—C55—C56119.0 (3)
C1—C6—C7124.6 (3)C60—C55—P3122.9 (3)
C8—C7—C12119.3 (3)C56—C55—P3117.9 (2)
C8—C7—C6118.1 (3)C57—C56—C55120.3 (3)
C12—C7—C6122.5 (3)C57—C56—H56A119.8
C9—C8—C7121.1 (3)C55—C56—H56A119.8
C9—C8—H8A119.4C58—C57—C56120.4 (4)
C7—C8—H8A119.4C58—C57—H57A119.8
C8—C9—C10119.8 (3)C56—C57—H57A119.8
C8—C9—H9A120.1C59—C58—C57119.8 (3)
C10—C9—H9A120.1C59—C58—H58A120.1
C9—C10—C11120.1 (3)C57—C58—H58A120.1
C9—C10—H10A119.9C58—C59—C60120.3 (4)
C11—C10—H10A119.9C58—C59—H59A119.8
C10—C11—C12121.1 (3)C60—C59—H59A119.8
C10—C11—H11A119.4C55—C60—C59120.2 (4)
C12—C11—H11A119.4C55—C60—H60A119.9
C11—C12—C7118.5 (3)C59—C60—H60A119.9
C11—C12—P2121.6 (3)C66—C61—C62119.4 (3)
C7—C12—P2119.8 (2)C66—C61—P4121.9 (2)
C14—C13—C18118.2 (3)C62—C61—P4118.7 (2)
C14—C13—P1123.9 (3)C63—C62—C61120.0 (3)
C18—C13—P1117.9 (3)C63—C62—H62A120.0
C13—C14—C15120.7 (3)C61—C62—H62A120.0
C13—C14—H14A119.7C64—C63—C62120.2 (3)
C15—C14—H14A119.7C64—C63—H63A119.9
C16—C15—C14120.8 (3)C62—C63—H63A119.9
C16—C15—H15A119.6C63—C64—C65120.4 (3)
C14—C15—H15A119.6C63—C64—H64A119.8
C15—C16—C17119.3 (3)C65—C64—H64A119.8
C15—C16—H16A120.3C64—C65—C66119.6 (3)
C17—C16—H16A120.3C64—C65—H65A120.2
C16—C17—C18120.2 (4)C66—C65—H65A120.2
C16—C17—H17A119.9C61—C66—C65120.4 (3)
C18—C17—H17A119.9C61—C66—H66A119.8
C17—C18—C13120.8 (4)C65—C66—H66A119.8
C17—C18—H18A119.6C72—C67—C68118.5 (3)
C13—C18—H18A119.6C72—C67—P4121.8 (3)
C20—C19—C24119.0 (3)C68—C67—P4119.1 (3)
C20—C19—P1117.6 (2)C69—C68—C67120.7 (4)
C24—C19—P1123.1 (2)C69—C68—H68A119.6
C21—C20—C19120.5 (3)C67—C68—H68A119.6
C21—C20—H20A119.8C70—C69—C68119.9 (4)
C19—C20—H20A119.8C70—C69—H69A120.0
C20—C21—C22119.9 (3)C68—C69—H69A120.0
C20—C21—H21A120.1C69—C70—C71120.7 (4)
C22—C21—H21A120.1C69—C70—H70A119.7
C23—C22—C21120.1 (3)C71—C70—H70A119.7
C23—C22—H22A119.9C70—C71—C72119.8 (4)
C21—C22—H22A119.9C70—C71—H71A120.1
C22—C23—C24119.9 (3)C72—C71—H71A120.1
C22—C23—H23A120.0C67—C72—C71120.3 (4)
C24—C23—H23A120.0C67—C72—H72A119.8
C23—C24—C19120.6 (3)C71—C72—H72A119.8
C23—C24—H24A119.7F14—B1—F11109.3 (4)
C19—C24—H24A119.7F14—B1—F13110.2 (3)
C26—C25—C30119.3 (3)F11—B1—F13109.3 (3)
C26—C25—P2122.1 (2)F14—B1—F12109.8 (3)
C30—C25—P2118.6 (3)F11—B1—F12109.7 (3)
C25—C26—C27119.8 (3)F13—B1—F12108.5 (4)
C25—C26—H26A120.1Cl12—C100—Cl11112.5 (2)
C27—C26—H26A120.1Cl12—C100—H10B109.1
C28—C27—C26120.2 (4)Cl11—C100—H10B109.1
C28—C27—H27A119.9Cl12—C100—H10C109.1
C26—C27—H27A119.9Cl11—C100—H10C109.1
C29—C28—C27120.2 (4)H10B—C100—H10C107.8
C29—C28—H28A119.9Cl22—C200—Cl21111.7 (3)
C27—C28—H28A119.9Cl22—C200—H20B109.3
C30—C29—C28120.3 (4)Cl21—C200—H20B109.3
C30—C29—H29A119.9Cl22—C200—H20C109.3
C28—C29—H29A119.9Cl21—C200—H20C109.3
C29—C30—C25120.3 (4)H20B—C200—H20C107.9
C29—C30—H30A119.9

Experimental details

Crystal data
Chemical formula[Ir2Cl3H2(C36H28P2)2]BF4·2CH2Cl2
Mr1794.48
Crystal system, space groupTriclinic, P1
Temperature (K)150
a, b, c (Å)13.6578 (14), 14.7640 (6), 18.5300 (11)
α, β, γ (°)68.701 (3), 86.357 (6), 86.228 (5)
V3)3470.5 (4)
Z2
Radiation typeMo Kα
µ (mm1)4.25
Crystal size (mm)0.17 × 0.14 × 0.14
Data collection
DiffractometerBruker Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.463, 0.550
No. of measured, independent and
observed [I > 2σ(I)] reflections
85276, 16517, 13333
Rint0.041
(sin θ/λ)max1)0.658
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.052, 1.03
No. of reflections16517
No. of parameters835
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)2.05, 1.07

Computer programs: COLLECT (Bruker, 2002), EVALCCD (Duisenberg et al., 2003), SHELXTL (Bruker, 2002), ORTEP-3 for Windows (Farrugia, 1997), publCIF (Version 1.9.2; Westrip, 2008).

Selected geometric parameters (Å, º) top
Ir1—P12.2518 (8)Ir2—P32.2464 (9)
Ir1—P22.2565 (8)Ir2—P42.2526 (8)
Ir1—Cl32.4287 (7)Ir2—Cl22.4374 (7)
Ir1—Cl22.4672 (8)Ir2—Cl32.4563 (8)
Ir1—Cl12.5262 (7)Ir2—Cl12.5365 (7)
Ir1—H11.44 (3)Ir2—H21.44 (3)
P1—Ir1—P292.35 (3)P4—Ir2—Cl2167.55 (3)
P1—Ir1—Cl395.11 (3)P3—Ir2—Cl3174.60 (3)
P2—Ir1—Cl3167.70 (3)P4—Ir2—Cl391.50 (3)
P1—Ir1—Cl2174.05 (3)Cl2—Ir2—Cl379.33 (3)
P2—Ir1—Cl293.52 (3)P3—Ir2—Cl197.83 (3)
Cl3—Ir1—Cl279.29 (3)P4—Ir2—Cl1107.55 (3)
P1—Ir1—Cl198.28 (3)Cl2—Ir2—Cl179.27 (2)
P2—Ir1—Cl1108.34 (3)Cl3—Ir2—Cl179.53 (3)
Cl3—Ir1—Cl180.26 (2)P3—Ir2—H288.1 (13)
Cl2—Ir1—Cl178.91 (2)P4—Ir2—H281.1 (13)
P1—Ir1—H188.2 (14)Cl2—Ir2—H291.1 (13)
P2—Ir1—H179.3 (13)Cl3—Ir2—H293.7 (13)
Cl3—Ir1—H191.2 (13)Cl1—Ir2—H2169.1 (13)
Cl2—Ir1—H193.8 (13)Ir1—Cl1—Ir282.56 (2)
Cl1—Ir1—H1169.6 (13)Ir2—Cl2—Ir185.85 (2)
P3—Ir2—P493.80 (3)Ir1—Cl3—Ir286.28 (2)
P3—Ir2—Cl295.58 (3)
 

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