Bis[bis­(penta­methyl­cyclo­penta­dien­yl)cobalt(III)] tetra­chlorido­cobaltate(II) di­chloro­methane disolvate

Merola, J.S.; Ngo, M.; Karpin, G.W.

doi:10.1107/S160053681302254X

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 9| September 2013| Page m504

doi:10.1107/S160053681302254X

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Bis[bis(pentamethylcyclopentadienyl)cobalt(III)] tetrachloridocobaltate(II) dichloromethane disolvate

Joseph S. Merola,^a ^* Mai Ngo ^a and George W. Karpin ^a

^aDepartment of Chemistry, Virginia Tech, Blacksburg, VA 24061, USA
^*Correspondence e-mail: jmerola@vt.edu

(Received 9 August 2013; accepted 10 August 2013; online 17 August 2013)

The title compound, [Co(C₁₀H₁₅)₂]₂[CoCl₄]·2CH₂Cl₂, was isolated as a dichloromethane solvate and was formed in the reaction between lithium pentamethylcyclopentadienide and anyhydrous cobalt(II) chloride in tetrahydrofuran. There are two decamethylcobaltocenium cations, one tetrachloridocobaltate(II) anion and two dichloromethane solvent molecules in the formula unit. There is a slight disorder of the dichloromethane solvent which was treated with a two-site model [occupancy rates = 0.765 (4) and 0.235 (4)]. The dichloromethane molecules display significant C—H⋯Cl interactions with the tetrachloridocobaltate(II) dianion. The cobalt atom of the decamethylcobaltocenium cation sits on a twofold rotation axis, with only one pentamethylcyclopentadiene ligand being unique and the second generated by symmetry. The cobalt atom of the [CoCl₄]⁻² ion sits on a special site with -4 symmetry, with one unique chloride ligand and the others generated by the fourfold inversion axis.

Related literature

For a related structure with a (THF)₂LiCl₂CoCl₂ monoanion and the decamethylcobaltocenium cation, see: Dehnen & Zimmermann (2000 ) (CCDC 135478). The structure of a related dimer synthesized by Koelle et al. (1986 ) was determined by Olson & Dahl (1986 ) (CCDC 566220). For a discussion of the role of chloroform and dichloromethane solvent molecules in crystal packing, see: Allen et al. (2013 ).

Experimental

Crystal data

[Co(C₁₀H₁₅)₂]₂[CoCl₄]·2CH₂Cl₂
M_r = 1033.35
Tetragonal, P 4₂ /n
a = 12.20980 (12) Å
c = 16.2811 (3) Å
V = 2427.17 (7) Å³
Z = 2
Mo Kα radiation
μ = 1.48 mm⁻¹
T = 101 K
0.27 × 0.24 × 0.18 mm

Data collection

Agilent Xcalibur Gemini Ultra diffractometer with Eos detector
Absorption correction: gaussian (CrysAlis PRO; Agilent, 2013 ) T_min = 0.755, T_max = 0.821
26858 measured reflections
4161 independent reflections
3394 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.091
S = 1.04
4161 reflections
130 parameters
H-atom parameters constrained
Δρ_max = 1.21 e Å⁻³
Δρ_min = −1.07 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C11—H⋯Cl1ⁱ	0.97	2.71	3.548 (3)	145
C11—HA⋯Cl1ⁱⁱ	0.97	2.71	3.548 (3)	145
Symmetry codes: (i) $[-y+{\script{3\over 2}}, x-1, -z+{\script{1\over 2}}]$ ; (ii) $[y+1, -x+{\script{3\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis PRO (Agilent, 2013); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009 ); software used to prepare material for publication: OLEX2.

Supporting information

Crystal structure: contains datablock I. DOI: 10.1107/S160053681302254X/zl2564sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681302254X/zl2564Isup2.hkl

checkCIF report

Comment top

Koelle et al. (1986) reported on the preparation of a pentamethylcyclopentadienylcobalt chloro-bridged dimeric compound that represents an excellent precursor to other mononuclear complexes via bridge-splitting reactions. There is no doubt that Koelle et al. made the described bridged complex since Olson & Dahl (1986) published a crystal structure of the dimer. However, in our laboratories, regardless of the stoichiometry used in attempts to make the chloro bridged dimer described by Koelle et al. (1986), the title compound was the only material isolated. The composition of the title compound consists of two decamethylcobaltocenium cations, one tetrachlorocobalt(II) dianion, and two molecules of dichloromethane. The dichloromethane molecules were slightly disordered and the disorder was treated successfully by a two site model with occupancies of 76.5 (4) and 23.5 (4)%. Dehnen & Zimmerman (2000) noted a similar product in attempts to make selenium-bridged compounds and noted the decamethylcoblatocenium ion was formed depending on the temperature of the reaction. In their case, the CoCl₄^-2 ion was linked via chloride bridges to a bis-THF Li⁺ cation.

In the structure reported here, the CoCl₄^-2 ion shows significant interaction with the dichloromethane of solvation. Recently, Allen et al. (2013) examined the Cambridge Crystallographic Data Base and analyzed crystallographic evidence of C—H···Cl hydrogen bonding for both CH₂Cl₂ and CHCl₃. In that paper, for the specific case of CH₂Cl₂ interacting with Cl-, they note C—H···Cl interactions with H···Cl distances ranging from 2.33 to 2.95 Å and C—H···Cl angles ranging from 120° to 170° for a set of 63 structures. In the title structure, the H···Cl distance is 2.72 Å with a C—H···Cl angle of 145.0°. These parameters would place the C—H···Cl interaction for the title structure very nearly at the median of the structures analyzed by Allen et al. (2013).

In the structure reported here, the CoCl₄^2- ion is also distorted from perfect tetrahedral geometry with the Cl—Co—Cl angles involved in the hydrogen bonding compressed to 100.04 (2)° and the remaining Cl—Co—Cl angles are 114.385 (12)°. While it is important not to make too much of a qualitative observation, the strength of the C—H···Cl interaction may also be responsible for the relative stability of these crystals in open air. Our experience is that, in the abence of a significant attractive interaction, dichlromethane molecules quite easily evaporate from crystals with loss of crystallinity at room temperature.

Related literature top

For a related structure with a (THF)₂LiCl₂CoCl₂ mono anion and the decamethylcobaltocenium ion, see Dehnen & Zimmermann (2000) (CCDC 135478)·The structure of a related dimer synthesized by Koelle et al. (1986) was determined by Olson & Dahl (1986) (CCDC 566220). Allen et al. (2013) discuss the role of chloroform and dichloromethane solvent molecules in crystal packing.

Experimental top

The procedure described by Koelle et al.(1986) was followed using lithium pentamethylcyclopentadienide (LiCp*) and anhydrous cobalt(II) chloride in tetrahydrofuran. Instead of obtaining the hexane soluble brown dimer as described, the reaction produced a green solid. Dissolution of the solid in dichloromethane followed by slow diffusion of diethyl ether produced well formed green prisms of the title compound that are very air stable and retain the dichloromethane of solvation even after several weeks exposure to the open atmosphere at room temperature.

Computing details top

Data collection: CrysAlis PRO (Agilent, 2013); cell refinement: CrysAlis PRO (Agilent, 2013); data reduction: CrysAlis PRO (Agilent, 2013); program(s) used to solve structure: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Figures top

	Fig. 1. Plot of the title compound displaying the complete molecular fragments with thermal ellipsoids shown at 50% probability level. Only the major component (76.3 (4)%) of the disordered dichloromethane solvate is shown. Symmetry codes: (1) 3/2 - x, 1/2 - y, z; (2) 3/2 - x, 3/2 - y, z; (3) y, 3/2 - x, 3/2 - z; (4) 3/2 - y, x, 3/2 - z
	Fig. 2. Thermal ellipsoid plot of the CoCl₄^-2 ion showing C—H···Cl interactions with the dichloromethane solvate. Atoms are named with the symmetry operation that generated them. Only the major component (76.3 (4)%) of the disordered dichloromethane solvate is shown.

Bis[bis(pentamethylcyclopentadienyl)cobalt(III)] tetrachloridocobaltate(II) dichloromethane disolvate top

Crystal data top

[Co(C₁₀H₁₅)₂]₂[CoCl₄]·2CH₂Cl₂	D_x = 1.408 Mg m⁻³
M_r = 1029.32	Mo Kα radiation, λ = 0.7107 Å
Tetragonal, P4₂/n	Cell parameters from 8251 reflections
a = 12.20980 (12) Å	θ = 4.2–32.2°
c = 16.2811 (3) Å	µ = 1.48 mm⁻¹
V = 2427.17 (7) Å³	T = 101 K
Z = 2	Prism, clear green
F(000) = 1066	0.27 × 0.24 × 0.18 mm

Data collection top

Agilent Xcalibur (Eos, Gemini ultra) diffractometer	4161 independent reflections
Radiation source: Enhance (Mo) X-ray Source	3394 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
Detector resolution: 16.0122 pixels mm^-1	θ_max = 32.5°, θ_min = 3.4°
ω scans	h = −18→17
Absorption correction: gaussian (CrysAlis PRO; Agilent, 2013)	k = −18→12
T_min = 0.755, T_max = 0.821	l = −24→21
26858 measured reflections

Refinement top

Refinement on F²	Primary atom site location: heavy-atom method
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.037	Hydrogen site location: constr
wR(F²) = 0.091	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0319P)² + 2.9104P] where P = (F_o² + 2F_c²)/3
4161 reflections	(Δ/σ)_max = 0.001
130 parameters	Δρ_max = 1.21 e Å⁻³
0 restraints	Δρ_min = −1.07 e Å⁻³

Crystal data top

[Co(C₁₀H₁₅)₂]₂[CoCl₄]·2CH₂Cl₂	Z = 2
M_r = 1029.32	Mo Kα radiation
Tetragonal, P4₂/n	µ = 1.48 mm⁻¹
a = 12.20980 (12) Å	T = 101 K
c = 16.2811 (3) Å	0.27 × 0.24 × 0.18 mm
V = 2427.17 (7) Å³

Data collection top

Agilent Xcalibur (Eos, Gemini ultra) diffractometer	4161 independent reflections
Absorption correction: gaussian (CrysAlis PRO; Agilent, 2013)	3394 reflections with I > 2σ(I)
T_min = 0.755, T_max = 0.821	R_int = 0.037
26858 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.091	H-atom parameters constrained
S = 1.04	Δρ_max = 1.21 e Å⁻³
4161 reflections	Δρ_min = −1.07 e Å⁻³
130 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	Occ. (<1)
Co1	0.7500	0.2500	0.361342 (19)	0.01381 (8)
C1	0.86792 (13)	0.37038 (14)	0.36190 (10)	0.0171 (3)
C2	0.79973 (13)	0.38033 (14)	0.29066 (10)	0.0169 (3)
C3	0.68885 (14)	0.39523 (14)	0.31700 (11)	0.0193 (3)
C4	0.68838 (14)	0.39480 (15)	0.40471 (11)	0.0206 (3)
C5	0.79870 (14)	0.37984 (14)	0.43257 (10)	0.0188 (3)
C6	0.98932 (14)	0.35672 (16)	0.36341 (11)	0.0221 (3)
H6A	1.0095	0.3102	0.4085	0.033*
H6B	1.0235	0.4270	0.3699	0.033*
H6C	1.0131	0.3242	0.3128	0.033*
C7	0.83672 (15)	0.38171 (16)	0.20305 (11)	0.0231 (4)
H7A	0.9052	0.3436	0.1984	0.035*
H7B	0.8459	0.4561	0.1853	0.035*
H7C	0.7828	0.3464	0.1693	0.035*
C8	0.59249 (15)	0.41374 (17)	0.26198 (13)	0.0268 (4)
H8A	0.5987	0.3678	0.2144	0.040*
H8B	0.5906	0.4891	0.2452	0.040*
H8C	0.5263	0.3962	0.2910	0.040*
C9	0.59133 (16)	0.41372 (19)	0.45881 (14)	0.0318 (4)
H9A	0.5256	0.3966	0.4292	0.048*
H9B	0.5896	0.4891	0.4756	0.048*
H9C	0.5965	0.3676	0.5064	0.048*
C10	0.83534 (17)	0.38163 (18)	0.52022 (12)	0.0281 (4)
H10A	0.7814	0.3462	0.5539	0.042*
H10B	0.8443	0.4561	0.5379	0.042*
H10C	0.9039	0.3437	0.5251	0.042*
Co2	1.2500	0.2500	0.2500	0.01550 (10)
Cl1	1.11315 (3)	0.29420 (4)	0.15956 (3)	0.02050 (9)
C11	1.2500	0.2500	0.5298 (2)	0.0505 (9)
H	1.2150	0.1964	0.4946	0.061*	0.3825 (19)
HA	1.2850	0.3036	0.4946	0.061*	0.3825 (19)
HB	1.2469	0.1859	0.4946	0.061*	0.1175 (19)
HC	1.2531	0.3141	0.4946	0.061*	0.1175 (19)
Cl2	1.35262 (12)	0.1830 (2)	0.58797 (8)	0.0726 (5)	0.765 (4)
Cl2A	1.3635 (4)	0.2446 (6)	0.5851 (3)	0.0726 (5)	0.235 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.01106 (14)	0.01787 (15)	0.01251 (14)	0.00152 (11)	0.000	0.000
C1	0.0155 (7)	0.0193 (7)	0.0167 (7)	−0.0010 (6)	−0.0006 (6)	−0.0008 (6)
C2	0.0162 (7)	0.0183 (7)	0.0163 (7)	0.0004 (6)	−0.0001 (6)	0.0012 (6)
C3	0.0172 (7)	0.0186 (7)	0.0221 (8)	0.0032 (6)	−0.0017 (6)	−0.0003 (6)
C4	0.0186 (8)	0.0208 (8)	0.0224 (8)	0.0032 (6)	0.0015 (6)	−0.0042 (6)
C5	0.0177 (7)	0.0217 (8)	0.0171 (7)	−0.0002 (6)	0.0007 (6)	−0.0042 (6)
C6	0.0151 (7)	0.0317 (9)	0.0195 (8)	−0.0029 (7)	−0.0005 (6)	0.0007 (7)
C7	0.0219 (8)	0.0304 (9)	0.0169 (8)	−0.0021 (7)	0.0005 (6)	0.0031 (7)
C8	0.0191 (8)	0.0298 (9)	0.0316 (10)	0.0068 (7)	−0.0050 (7)	0.0037 (8)
C9	0.0223 (9)	0.0390 (11)	0.0342 (11)	0.0054 (8)	0.0083 (8)	−0.0124 (9)
C10	0.0272 (9)	0.0399 (11)	0.0171 (8)	−0.0027 (8)	−0.0007 (7)	−0.0060 (8)
Co2	0.01459 (13)	0.01459 (13)	0.0173 (2)	0.000	0.000	0.000
Cl1	0.01695 (18)	0.0238 (2)	0.02071 (18)	0.00320 (14)	−0.00162 (14)	−0.00033 (15)
C11	0.056 (2)	0.069 (3)	0.0266 (16)	0.000 (2)	0.000	0.000
Cl2	0.0681 (7)	0.0970 (14)	0.0527 (5)	0.0388 (9)	−0.0021 (5)	0.0055 (8)
Cl2A	0.0681 (7)	0.0970 (14)	0.0527 (5)	0.0388 (9)	−0.0021 (5)	0.0055 (8)

Geometric parameters (Å, º) top

Co1—C1ⁱ	2.0576 (17)	C7—H7B	0.9600
Co1—C1	2.0576 (17)	C7—H7C	0.9600
Co1—C2ⁱ	2.0556 (17)	C8—H8A	0.9600
Co1—C2	2.0556 (17)	C8—H8B	0.9600
Co1—C3	2.0550 (17)	C8—H8C	0.9600
Co1—C3ⁱ	2.0550 (17)	C9—H9A	0.9600
Co1—C4ⁱ	2.0470 (17)	C9—H9B	0.9600
Co1—C4	2.0470 (17)	C9—H9C	0.9600
Co1—C5ⁱ	2.0521 (17)	C10—H10A	0.9600
Co1—C5	2.0522 (17)	C10—H10B	0.9600
C1—C2	1.433 (2)	C10—H10C	0.9600
C1—C5	1.432 (2)	Co2—Cl1ⁱⁱ	2.2915 (4)
C1—C6	1.492 (2)	Co2—Cl1ⁱⁱⁱ	2.2915 (4)
C2—C3	1.432 (2)	Co2—Cl1	2.2915 (4)
C2—C7	1.496 (2)	Co2—Cl1^iv	2.2915 (4)
C3—C4	1.428 (3)	C11—H	0.9700
C3—C8	1.496 (2)	C11—HA	0.9700
C4—C5	1.433 (2)	C11—HB	0.9700
C4—C9	1.494 (3)	C11—HC	0.9700
C5—C10	1.496 (3)	C11—Cl2ⁱⁱⁱ	1.771 (2)
C6—H6A	0.9600	C11—Cl2	1.771 (2)
C6—H6B	0.9600	C11—Cl2Aⁱⁱⁱ	1.654 (5)
C6—H6C	0.9600	C11—Cl2A	1.654 (5)
C7—H7A	0.9600

C1—Co1—C1ⁱ	179.49 (9)	C9—C4—Co1	128.93 (14)
C2—Co1—C1ⁱ	139.66 (7)	C1—C5—Co1	69.81 (9)
C2ⁱ—Co1—C1ⁱ	40.78 (6)	C1—C5—C4	108.10 (15)
C2—Co1—C1	40.78 (6)	C1—C5—C10	126.23 (16)
C2ⁱ—Co1—C1	139.66 (7)	C4—C5—Co1	69.34 (10)
C2—Co1—C2ⁱ	111.91 (9)	C4—C5—C10	125.54 (16)
C3—Co1—C1ⁱ	111.33 (7)	C10—C5—Co1	129.57 (14)
C3ⁱ—Co1—C1ⁱ	68.86 (7)	C1—C6—H6A	109.5
C3ⁱ—Co1—C1	111.33 (7)	C1—C6—H6B	109.5
C3—Co1—C1	68.86 (7)	C1—C6—H6C	109.5
C3ⁱ—Co1—C2	111.35 (7)	H6A—C6—H6B	109.5
C3—Co1—C2	40.77 (7)	H6A—C6—H6C	109.5
C3—Co1—C2ⁱ	111.35 (7)	H6B—C6—H6C	109.5
C3ⁱ—Co1—C2ⁱ	40.77 (7)	C2—C7—H7A	109.5
C3—Co1—C3ⁱ	138.87 (10)	C2—C7—H7B	109.5
C4ⁱ—Co1—C1	110.99 (7)	C2—C7—H7C	109.5
C4—Co1—C1	68.82 (7)	H7A—C7—H7B	109.5
C4—Co1—C1ⁱ	110.99 (7)	H7A—C7—H7C	109.5
C4ⁱ—Co1—C1ⁱ	68.82 (7)	H7B—C7—H7C	109.5
C4ⁱ—Co1—C2ⁱ	68.47 (7)	C3—C8—H8A	109.5
C4ⁱ—Co1—C2	138.86 (7)	C3—C8—H8B	109.5
C4—Co1—C2	68.47 (7)	C3—C8—H8C	109.5
C4—Co1—C2ⁱ	138.86 (7)	H8A—C8—H8B	109.5
C4ⁱ—Co1—C3	179.56 (8)	H8A—C8—H8C	109.5
C4—Co1—C3	40.75 (7)	H8B—C8—H8C	109.5
C4ⁱ—Co1—C3ⁱ	40.74 (7)	C4—C9—H9A	109.5
C4—Co1—C3ⁱ	179.56 (8)	C4—C9—H9B	109.5
C4ⁱ—Co1—C4	139.65 (11)	C4—C9—H9C	109.5
C4ⁱ—Co1—C5ⁱ	40.92 (7)	H9A—C9—H9B	109.5
C4ⁱ—Co1—C5	111.46 (7)	H9A—C9—H9C	109.5
C4—Co1—C5ⁱ	111.46 (7)	H9B—C9—H9C	109.5
C4—Co1—C5	40.92 (7)	C5—C10—H10A	109.5
C5—Co1—C1	40.79 (7)	C5—C10—H10B	109.5
C5ⁱ—Co1—C1	138.77 (7)	C5—C10—H10C	109.5
C5ⁱ—Co1—C1ⁱ	40.79 (7)	H10A—C10—H10B	109.5
C5—Co1—C1ⁱ	138.77 (7)	H10A—C10—H10C	109.5
C5—Co1—C2ⁱ	179.55 (7)	H10B—C10—H10C	109.5
C5ⁱ—Co1—C2ⁱ	68.45 (7)	Cl1ⁱⁱⁱ—Co2—Cl1ⁱⁱ	114.385 (12)
C5ⁱ—Co1—C2	179.55 (7)	Cl1ⁱⁱⁱ—Co2—Cl1	100.04 (2)
C5—Co1—C2	68.45 (7)	Cl1ⁱⁱ—Co2—Cl1	114.385 (11)
C5ⁱ—Co1—C3	139.45 (7)	Cl1ⁱⁱⁱ—Co2—Cl1^iv	114.386 (11)
C5—Co1—C3	68.73 (7)	Cl1ⁱⁱ—Co2—Cl1^iv	100.04 (2)
C5—Co1—C3ⁱ	139.45 (7)	Cl1—Co2—Cl1^iv	114.385 (11)
C5ⁱ—Co1—C3ⁱ	68.72 (7)	H—C11—HA	107.5
C5ⁱ—Co1—C5	111.19 (10)	H—C11—HC	102.2
C2—C1—Co1	69.54 (9)	HA—C11—HB	102.2
C2—C1—C6	126.87 (15)	HB—C11—HC	107.6
C5—C1—Co1	69.40 (10)	Cl2ⁱⁱⁱ—C11—H	108.4
C5—C1—C2	107.49 (14)	Cl2—C11—H	108.4
C5—C1—C6	125.60 (15)	Cl2ⁱⁱⁱ—C11—HA	108.4
C6—C1—Co1	127.98 (13)	Cl2—C11—HA	108.4
C1—C2—Co1	69.69 (9)	Cl2ⁱⁱⁱ—C11—HB	131.4
C1—C2—C7	126.67 (15)	Cl2—C11—HB	88.3
C3—C2—Co1	69.59 (10)	Cl2ⁱⁱⁱ—C11—HC	88.3
C3—C2—C1	108.52 (14)	Cl2—C11—HC	131.4
C3—C2—C7	124.72 (15)	Cl2—C11—Cl2ⁱⁱⁱ	115.3 (2)
C7—C2—Co1	129.17 (13)	Cl2Aⁱⁱⁱ—C11—H	88.8
C2—C3—Co1	69.64 (9)	Cl2A—C11—H	131.6
C2—C3—C8	125.70 (16)	Cl2Aⁱⁱⁱ—C11—HA	131.6
C4—C3—Co1	69.33 (10)	Cl2A—C11—HA	88.8
C4—C3—C2	107.63 (15)	Cl2A—C11—HB	108.7
C4—C3—C8	126.60 (16)	Cl2Aⁱⁱⁱ—C11—HB	108.7
C8—C3—Co1	128.79 (13)	Cl2A—C11—HC	108.7
C3—C4—Co1	69.93 (10)	Cl2Aⁱⁱⁱ—C11—HC	108.7
C3—C4—C5	108.25 (15)	Cl2A—C11—Cl2ⁱⁱⁱ	108.7 (2)
C3—C4—C9	126.30 (17)	Cl2Aⁱⁱⁱ—C11—Cl2	108.7 (2)
C5—C4—Co1	69.73 (10)	Cl2A—C11—Cl2Aⁱⁱⁱ	114.1 (4)
C5—C4—C9	125.35 (17)

Symmetry codes: (i) −x+3/2, −y+1/2, z; (ii) y+1, −x+3/2, −z+1/2; (iii) −x+5/2, −y+1/2, z; (iv) −y+3/2, x−1, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C11—H···Cl1^iv	0.97	2.71	3.548 (3)	145
C11—HA···Cl1ⁱⁱ	0.97	2.71	3.548 (3)	145

Symmetry codes: (ii) y+1, −x+3/2, −z+1/2; (iv) −y+3/2, x−1, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C11—H···Cl1ⁱ	0.97	2.71	3.548 (3)	145.0
C11—HA···Cl1ⁱⁱ	0.97	2.71	3.548 (3)	145.0

Symmetry codes: (i) −y+3/2, x−1, −z+1/2; (ii) y+1, −x+3/2, −z+1/2.

Acknowledgements

The authors thank the US National Science Foundation for funding (grant No. CHE-01311288) for the purchase of the Oxford Diffraction Xcalibur2 single-crystal diffractometer.

References

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Bis[bis­­(penta­methyl­cyclo­penta­dien­yl)cobalt(III)] tetra­chlorido­cobaltate(II) di­chloro­methane disolvate

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metal-organic compounds

Bis[bis(pentamethylcyclopentadienyl)cobalt(III)] tetrachloridocobaltate(II) dichloromethane disolvate