Bis(μ-di­phenyl­phosphan­yl)bis­[(tri­methyl­phosphane)cobalt(I)](Co—Co)

Beck, R.; Klein, H.-F.

doi:10.1107/S1600536813027384

metal-organic compounds

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Volume 69| Part 11| November 2013| Page m604

doi:10.1107/S1600536813027384

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Bis(μ-diphenylphosphanyl)bis[(trimethylphosphane)cobalt(I)](Co—Co)

Robert Beck ^a ^* and Hans-Friedrich Klein ^a

^aEduard-Zintl-Institut, Darmstadt University of Technology, 64287 Darmstadt, Germany
^*Correspondence e-mail: metallacycle@gmail.com

(Received 30 July 2013; accepted 5 October 2013; online 16 October 2013)

The title compound, [Co₂{P(C₆H₅)₂}₂(C₃H₉P)₄], was obtained by the addition of diphenylphosphane to a solution of Co(CH₃)(C₃H₉P)₄. The dinuclear complex molecule exhibits inversion symmetry with the inversion centre located between the two Co^I atoms. The short Co—Co distance of 2.3670 (8) Å lies within the range of metal–metal double bonds. As a result of inversion symmetry, the four-membered Co₂P₂ core is rigorously planar, and the two bridging P(C₆H₅)₂-ligands and the terminal C₃H₉P ligands are arranged in a pseudo-tetrahedral fashion about the Co^I atom.

CCDC reference: 965035

Related literature

For related homobimetallic cobalt complexes, see: Harley et al. (1983 ); Jones et al. (1983 ); Winterhalter et al. (2001 ): For related salt metathesis reactions, see: Klein et al. (1988 , 2003 ); Klein & Karsch (1975 ).

Experimental

Crystal data

[Co₂(C₁₂H₁₀P)₂(C₃H₉P)₄]
M_r = 792.49
Monoclinic, P 2₁ /c
a = 10.318 (2) Å
b = 19.262 (4) Å
c = 10.721 (2) Å
β = 113.32 (3)°
V = 1956.8 (7) Å³
Z = 2
Mo Kα radiation
μ = 1.12 mm⁻¹
T = 173 K
0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.912, T_max = 0.940
37952 measured reflections
5413 independent reflections
3251 reflections with I > 2σ(I)
R_int = 0.062

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.083
S = 0.81
5413 reflections
205 parameters
H-atom parameters constrained
Δρ_max = 0.45 e Å⁻³
Δρ_min = −0.86 e Å⁻³

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC reference: 965035

Crystal structure: contains datablock I. DOI: 10.1107/S1600536813027384/wm2765sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813027384/wm2765Isup2.hkl

checkCIF report

Comment top

The synthesis of bimetallic complexes with bridging anionic PR₂ ligands (R = aryl or alkyl) are long time established (Harley et al., 1983), and numerous variants of synthetic approaches were developed (Jones et al., 1983). During the course of our investigations into the chemistry of cyclometallation of triphenylphosphane derivatives (Winterhalter et al., 2001), we isolated, structurally and spectroscopically characterized a series of ortho-metallated cobalt complexes (Klein et al., 2003). Using previous method allowed to synthesize a related bimetallic cobalt complex via salt metathesis of CoCl(PMe₃)₃ with LiPPMe₂ in high yield (Klein et al., 1988).

The molecular structure of the bimetallic title complex, (I), [Co(C₃H₉P)₂(µ₂-P(C₆H₅)₂)]₂, is shown in Fig. 1. The complex exhibits a crystallographically imposed inversion centre in the middle of the molecule. Each Co^I atom has a distorted tetrahedral coordination geometry with a short Co—Co distance of 2.3670 (8) Å, slightly longer than found for other Co═Co distances of homobimetallic cobalt complexes. Each set of terminal ligands is trans with respect to the Co═Co bond. Both bridging µ₂-PPh₂ and PMe₃-ligands are bent away from the central Co₂P₂ core with the distortion from idealized tetrahedral geometry being greater for the larger PPh₂ group with 115.13 (3)°.

The crystal packing of compound (I) can be described as being composed of rods of single molecules stacked along [100] and [001], with the Co₂P₂ cores arranged in alternating directions (Fig. 2).

Related literature top

For related homobimetallic cobalt complexes, see: Harley et al. (1983); Jones et al. (1983); Winterhalter et al. (2001): For related salt metathesis reactions, see: Klein et al. (1988, 2003); Klein & Karsch (1975).

Experimental top

Standard vacuum techniques were used in manipulations of volatile and air sensitive material. Literature methods were applied for the preparation of Co(CH₃)(PMe₃)₄ (Klein & Karsch, 1975). Other chemicals were used as purchased. The title compound bis(µ₂-diphenylphosphino)tetrakis(trimethylphosphane) dicobalt(I) was synthesized by combining stoichiometric amounts of diphenylphosphane (118 mg, 0.63 mmol) in 20 ml of n-pentane at 203 K with a sample of Co(CH₃)(PMe₃)₄ (240 mg, 0.63 mmol) in 20 ml of n-pentane, effecting a change of color from red to dark brown. After warm-up, the mixture was kept stirring at 293 K for 16 h, and then the volatiles were removed in vacuo to give a dark brown, waxy solid. This was dissolved in a mixture of 10 ml of n-pentane / diethyl ether (3:1) and crystallized at 253 K to give brown rhombic crystals, which were suitable for X-ray diffraction. Isolated yield 145 mg (58%); m. p. 391–393 K (dec.). ¹H NMR (300 MHz, THF-d₈, 293 K, p.p.m.): δ = 0.88 (s(br), 36H, PCH₃); 7.03 - 7.11 (m, 12H, Ar—H); 7.51 – 7.56 (m, 8H, Ar—H); - ³¹P{¹H} NMR (121 MHz, THF-d₈, 297 K, p.p.m.): δ = 4.66 (s(br), 4P, PCH₃), 12.3 (s(br), 2P, PPh₂). Anal. Calcd. for C₃₆H₅₆Co₂P₆ (792.5): C, 54.56; H, 7.12; P, 23.45: Found: C, 54.88; H, 6.72; P 23.98%.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Figures top

	Fig. 1. The molecular structure of compound (I), with atom labels and thermal displacement parameters of the atoms drawn at the 50% probability level for non-H atoms; H atoms were omitted for clarity. Symmetry code (i) -x, 1 - y, -z indicates symmetry-related atoms generated by a crystallographic inversion centre.
	Fig. 2. Crystal packing of compound (I) viewed along [001].

Bis(µ-diphenylphosphanyl)bis[(trimethylphosphane)cobalt(I)](Co—Co) top

Crystal data top

[Co₂(C₁₂H₁₀P)₂(C₃H₉P)₄]	F(000) = 832
M_r = 792.49	D_x = 1.345 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.318 (2) Å	Cell parameters from 864 reflections
b = 19.262 (4) Å	θ = 3.0–26.0°
c = 10.721 (2) Å	µ = 1.12 mm⁻¹
β = 113.32 (3)°	T = 173 K
V = 1956.8 (7) Å³	Block, brown
Z = 2	0.12 × 0.10 × 0.08 mm

Data collection top

Bruker APEX CCD diffractometer	5413 independent reflections
Radiation source: fine-focus sealed tube	3251 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
phi and ω scans	θ_max = 29.5°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −14→14
T_min = 0.912, T_max = 0.940	k = −26→26
37952 measured reflections	l = −14→12

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 = 0.81	w = 1/[σ²(F_o²) + (0.0484P)²] where P = (F_o² + 2F_c²)/3
5413 reflections	(Δ/σ)_max = 0.001
205 parameters	Δρ_max = 0.45 e Å⁻³
0 restraints	Δρ_min = −0.86 e Å⁻³

Crystal data top

[Co₂(C₁₂H₁₀P)₂(C₃H₉P)₄]	V = 1956.8 (7) Å³
M_r = 792.49	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.318 (2) Å	µ = 1.12 mm⁻¹
b = 19.262 (4) Å	T = 173 K
c = 10.721 (2) Å	0.12 × 0.10 × 0.08 mm
β = 113.32 (3)°

Data collection top

Bruker APEX CCD diffractometer	5413 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	3251 reflections with I > 2σ(I)
T_min = 0.912, T_max = 0.940	R_int = 0.062
37952 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.083	H-atom parameters constrained
S = 0.81	Δρ_max = 0.45 e Å⁻³
5413 reflections	Δρ_min = −0.86 e Å⁻³
205 parameters

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	U_iso*/U_eq
Co1	0.05854 (3)	0.453786 (15)	0.07344 (3)	0.02705 (8)
P1	0.01598 (6)	0.55315 (3)	0.14726 (6)	0.02866 (12)
P2	0.00076 (7)	0.36275 (3)	0.15980 (6)	0.03557 (15)
P3	0.28562 (6)	0.43802 (3)	0.16358 (6)	0.03235 (14)
C1	0.1571 (2)	0.61095 (11)	0.2607 (2)	0.0314 (5)
C2	0.2519 (2)	0.64148 (12)	0.2142 (3)	0.0379 (5)
H2	0.2402	0.6342	0.1227	0.045*
C3	0.3630 (3)	0.68225 (13)	0.2982 (3)	0.0461 (6)
H3	0.4249	0.7034	0.2634	0.055*
C4	0.3839 (3)	0.69221 (14)	0.4325 (3)	0.0479 (7)
H4	0.4611	0.7193	0.4909	0.057*
C5	0.2914 (3)	0.66245 (14)	0.4807 (3)	0.0448 (6)
H5	0.3049	0.6692	0.5728	0.054*
C6	0.1783 (3)	0.62262 (12)	0.3958 (2)	0.0360 (5)
H6	0.1146	0.6031	0.4303	0.043*
C7	−0.1106 (2)	0.56800 (12)	0.2273 (2)	0.0304 (5)
C8	−0.1900 (2)	0.62912 (12)	0.1978 (2)	0.0347 (5)
H8	−0.1728	0.6637	0.1430	0.042*
C9	−0.2939 (3)	0.64003 (13)	0.2478 (3)	0.0385 (5)
H9	−0.3478	0.6816	0.2259	0.046*
C10	−0.3189 (3)	0.59079 (13)	0.3289 (3)	0.0397 (6)
H10	−0.3916	0.5977	0.3609	0.048*
C11	−0.2371 (3)	0.53124 (14)	0.3632 (3)	0.0412 (6)
H11	−0.2517	0.4977	0.4213	0.049*
C12	−0.1339 (3)	0.52056 (13)	0.3129 (2)	0.0356 (5)
H12	−0.0779	0.4797	0.3378	0.043*
C13	−0.1791 (3)	0.35558 (15)	0.1568 (3)	0.0485 (7)
H13A	−0.1993	0.3965	0.2005	0.073*
H13B	−0.1856	0.3137	0.2059	0.073*
H13C	−0.2478	0.3528	0.0625	0.073*
C14	0.0125 (3)	0.27953 (13)	0.0821 (3)	0.0465 (6)
H14A	−0.0508	0.2801	−0.0143	0.070*
H14B	−0.0151	0.2419	0.1280	0.070*
H14C	0.1097	0.2721	0.0909	0.070*
C15	0.1016 (3)	0.34134 (16)	0.3393 (3)	0.0525 (7)
H15A	0.2003	0.3327	0.3546	0.079*
H15B	0.0617	0.2997	0.3629	0.079*
H15C	0.0965	0.3802	0.3962	0.079*
C16	0.3665 (3)	0.35193 (14)	0.1710 (3)	0.0450 (6)
H16A	0.3405	0.3213	0.2304	0.068*
H16B	0.4694	0.3567	0.2071	0.068*
H16C	0.3327	0.3320	0.0796	0.068*
C17	0.3846 (3)	0.48700 (14)	0.0843 (3)	0.0419 (6)
H17A	0.3540	0.4730	−0.0110	0.063*
H17B	0.4857	0.4775	0.1323	0.063*
H17C	0.3673	0.5368	0.0890	0.063*
C18	0.3801 (3)	0.46387 (13)	0.3413 (2)	0.0401 (6)
H18A	0.3655	0.5135	0.3509	0.060*
H18B	0.4811	0.4547	0.3693	0.060*
H18C	0.3442	0.4373	0.3988	0.060*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.02893 (15)	0.02544 (14)	0.02803 (15)	−0.00128 (12)	0.01259 (11)	−0.00020 (12)
P1	0.0307 (3)	0.0278 (3)	0.0289 (3)	−0.0012 (2)	0.0132 (2)	−0.0022 (2)
P2	0.0428 (4)	0.0298 (3)	0.0350 (3)	−0.0054 (2)	0.0164 (3)	0.0019 (2)
P3	0.0299 (3)	0.0338 (3)	0.0320 (3)	0.0013 (2)	0.0108 (2)	−0.0002 (2)
C1	0.0301 (11)	0.0251 (10)	0.0356 (12)	0.0023 (8)	0.0095 (10)	−0.0021 (9)
C2	0.0325 (12)	0.0364 (12)	0.0439 (14)	−0.0014 (9)	0.0142 (11)	−0.0024 (11)
C3	0.0336 (13)	0.0367 (13)	0.0651 (18)	−0.0008 (10)	0.0162 (13)	0.0016 (12)
C4	0.0344 (13)	0.0395 (14)	0.0557 (17)	0.0006 (11)	0.0028 (12)	−0.0098 (12)
C5	0.0376 (13)	0.0461 (14)	0.0396 (14)	0.0038 (11)	0.0035 (11)	−0.0097 (11)
C6	0.0323 (12)	0.0355 (12)	0.0353 (12)	0.0018 (9)	0.0083 (10)	−0.0030 (10)
C7	0.0317 (11)	0.0327 (11)	0.0259 (11)	−0.0023 (9)	0.0105 (9)	−0.0054 (9)
C8	0.0382 (13)	0.0321 (11)	0.0350 (12)	−0.0017 (9)	0.0156 (10)	−0.0035 (9)
C9	0.0362 (13)	0.0383 (13)	0.0404 (13)	0.0039 (10)	0.0145 (11)	−0.0044 (10)
C10	0.0339 (12)	0.0505 (15)	0.0374 (13)	−0.0002 (11)	0.0171 (11)	−0.0045 (11)
C11	0.0439 (14)	0.0472 (15)	0.0380 (13)	0.0008 (11)	0.0220 (11)	0.0054 (11)
C12	0.0361 (12)	0.0365 (12)	0.0358 (12)	0.0020 (10)	0.0159 (10)	0.0018 (10)
C13	0.0543 (17)	0.0484 (15)	0.0512 (16)	−0.0161 (12)	0.0297 (14)	−0.0055 (12)
C14	0.0529 (16)	0.0309 (12)	0.0516 (16)	−0.0010 (11)	0.0164 (13)	0.0017 (11)
C15	0.0659 (18)	0.0481 (16)	0.0425 (15)	−0.0118 (14)	0.0204 (14)	0.0074 (12)
C16	0.0410 (14)	0.0445 (14)	0.0438 (15)	0.0086 (11)	0.0106 (12)	−0.0019 (11)
C17	0.0334 (13)	0.0527 (15)	0.0395 (13)	−0.0042 (11)	0.0144 (11)	−0.0033 (12)
C18	0.0363 (12)	0.0437 (14)	0.0374 (13)	0.0023 (11)	0.0115 (10)	−0.0009 (11)

Geometric parameters (Å, º) top

Co1—Co1ⁱ	2.3670 (8)	C8—H8	0.9500
Co1—P1ⁱ	2.1835 (9)	C8—C9	1.391 (3)
Co1—P1	2.1812 (7)	C9—H9	0.9500
Co1—P2	2.1735 (7)	C9—C10	1.378 (4)
Co1—P3	2.1734 (9)	C10—H10	0.9500
P1—Co1ⁱ	2.1835 (9)	C10—C11	1.385 (4)
P1—C1	1.854 (2)	C11—H11	0.9500
P1—C7	1.847 (2)	C11—C12	1.387 (3)
P2—C13	1.849 (3)	C12—H12	0.9500
P2—C14	1.833 (3)	C13—H13A	0.9800
P2—C15	1.836 (3)	C13—H13B	0.9800
P3—C16	1.844 (3)	C13—H13C	0.9800
P3—C17	1.829 (3)	C14—H14A	0.9800
P3—C18	1.833 (3)	C14—H14B	0.9800
C1—C2	1.392 (3)	C14—H14C	0.9800
C1—C6	1.394 (3)	C15—H15A	0.9800
C2—H2	0.9500	C15—H15B	0.9800
C2—C3	1.388 (3)	C15—H15C	0.9800
C3—H3	0.9500	C16—H16A	0.9800
C3—C4	1.383 (4)	C16—H16B	0.9800
C4—H4	0.9500	C16—H16C	0.9800
C4—C5	1.377 (4)	C17—H17A	0.9800
C5—H5	0.9500	C17—H17B	0.9800
C5—C6	1.392 (3)	C17—H17C	0.9800
C6—H6	0.9500	C18—H18A	0.9800
C7—C8	1.397 (3)	C18—H18B	0.9800
C7—C12	1.382 (3)	C18—H18C	0.9800

P1—Co1—Co1ⁱ	57.21 (2)	C9—C8—C7	120.8 (2)
P1ⁱ—Co1—Co1ⁱ	57.11 (2)	C9—C8—H8	119.6
P1—Co1—P1ⁱ	114.32 (2)	C8—C9—H9	119.9
P2—Co1—Co1ⁱ	137.42 (3)	C10—C9—C8	120.3 (2)
P2—Co1—P1ⁱ	111.96 (3)	C10—C9—H9	119.9
P2—Co1—P1	115.13 (3)	C9—C10—H10	120.3
P3—Co1—Co1ⁱ	125.27 (3)	C9—C10—C11	119.4 (2)
P3—Co1—P1ⁱ	109.18 (4)	C11—C10—H10	120.3
P3—Co1—P1	107.32 (3)	C10—C11—H11	120.0
P3—Co1—P2	97.30 (3)	C10—C11—C12	120.0 (2)
Co1—P1—Co1ⁱ	65.68 (2)	C12—C11—H11	120.0
C1—P1—Co1	123.13 (7)	C7—C12—C11	121.5 (2)
C1—P1—Co1ⁱ	126.59 (8)	C7—C12—H12	119.2
C7—P1—Co1ⁱ	120.15 (7)	C11—C12—H12	119.2
C7—P1—Co1	125.83 (7)	P2—C13—H13A	109.5
C7—P1—C1	96.80 (10)	P2—C13—H13B	109.5
C13—P2—Co1	119.71 (10)	P2—C13—H13C	109.5
C14—P2—Co1	115.68 (10)	H13A—C13—H13B	109.5
C14—P2—C13	99.98 (13)	H13A—C13—H13C	109.5
C14—P2—C15	99.68 (14)	H13B—C13—H13C	109.5
C15—P2—Co1	119.38 (10)	P2—C14—H14A	109.5
C15—P2—C13	98.61 (14)	P2—C14—H14B	109.5
C16—P3—Co1	122.34 (9)	P2—C14—H14C	109.5
C17—P3—Co1	115.06 (9)	H14A—C14—H14B	109.5
C17—P3—C16	99.05 (13)	H14A—C14—H14C	109.5
C17—P3—C18	100.24 (12)	H14B—C14—H14C	109.5
C18—P3—Co1	117.43 (9)	P2—C15—H15A	109.5
C18—P3—C16	98.85 (12)	P2—C15—H15B	109.5
C2—C1—P1	119.95 (18)	P2—C15—H15C	109.5
C2—C1—C6	117.4 (2)	H15A—C15—H15B	109.5
C6—C1—P1	122.54 (19)	H15A—C15—H15C	109.5
C1—C2—H2	119.2	H15B—C15—H15C	109.5
C3—C2—C1	121.6 (3)	P3—C16—H16A	109.5
C3—C2—H2	119.2	P3—C16—H16B	109.5
C2—C3—H3	119.9	P3—C16—H16C	109.5
C4—C3—C2	120.2 (3)	H16A—C16—H16B	109.5
C4—C3—H3	119.9	H16A—C16—H16C	109.5
C3—C4—H4	120.4	H16B—C16—H16C	109.5
C5—C4—C3	119.2 (2)	P3—C17—H17A	109.5
C5—C4—H4	120.4	P3—C17—H17B	109.5
C4—C5—H5	119.7	P3—C17—H17C	109.5
C4—C5—C6	120.7 (3)	H17A—C17—H17B	109.5
C6—C5—H5	119.7	H17A—C17—H17C	109.5
C1—C6—H6	119.5	H17B—C17—H17C	109.5
C5—C6—C1	120.9 (2)	P3—C18—H18A	109.5
C5—C6—H6	119.5	P3—C18—H18B	109.5
C8—C7—P1	119.00 (18)	P3—C18—H18C	109.5
C12—C7—P1	123.14 (18)	H18A—C18—H18B	109.5
C12—C7—C8	117.8 (2)	H18A—C18—H18C	109.5
C7—C8—H8	119.6	H18B—C18—H18C	109.5

Symmetry code: (i) −x, −y+1, −z.

Experimental details

Crystal data
Chemical formula	[Co₂(C₁₂H₁₀P)₂(C₃H₉P)₄]
M_r	792.49
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	10.318 (2), 19.262 (4), 10.721 (2)
β (°)	113.32 (3)
V (Å³)	1956.8 (7)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.12
Crystal size (mm)	0.12 × 0.10 × 0.08

Data collection
Diffractometer	Bruker APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2003)
T_min, T_max	0.912, 0.940
No. of measured, independent and observed [I > 2σ(I)] reflections	37952, 5413, 3251
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.692

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.083, 0.81
No. of reflections	5413
No. of parameters	205
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.45, −0.86

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 2012), OLEX2 (Dolomanov et al., 2009).

Acknowledgements

Financial support of this work by the Fonds der Chemischen Industrie is gratefully acknowledged.

References

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