Bis{[(η5)-cyclopentadienyl]tris(diethyl phosphito-κ3P,P′,P′′)cobaltate(III)-κ3O,O′,O′′]oxovanadium(IV)}-μ-oxalate

McLauchlan, C.C.; Anderson, A.E.

doi:10.1107/S1600536808024458

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 9| September 2008| Pages m1129-m1130

doi:10.1107/S1600536808024458

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Bis{[(η⁵)-cyclopentadienyl]tris(diethyl phosphito-κ³P,P′,P′′)cobaltate(III)-κ³O,O′,O′′]oxovanadium(IV)}-μ-oxalate

Craig C. McLauchlan ^a ^* and Alexander E. Anderson ^a

^aDepartment of Chemistry, Illinois State University, Campus Box 4160, Normal, IL 61790-4160, USA
^*Correspondence e-mail: mclauchlan@ilstu.edu

(Received 9 July 2008; accepted 31 July 2008; online 6 August 2008)

The title compound {systematic name: bis[1,4(η⁵)-cyclopentadienyl]hexakis(μ-diethyl phosphito)-1:2κ⁶P:O;3:4κ⁶O:P-μ-oxalato-2:3κ⁴O¹,O²:O^1′,O^2′-dioxido-2κO,3κO-1,4-dicobalt(III)-2,3-divanadium(IV)}, [Co₂V₂(C₅H₅)₂(C₂O₄)(C₄H₁₀O₃P)₆O₂], is an oxalate-bridged dinuclear complex of oxovanadium(IV). The geometric center of the dimer lies on an inversion center. The unique Co atom is bonded to three P atoms and a cyclopentadienyl ring. The unique V atom has six O atom neighbors in an approximately octahedral arrangement; the V—O bond trans to the V=O bond is significantly lengthened.

Related literature

The title compound was synthesized by oxidation of the known {[Cp(P^OEt)₃Co]VCl}₂(μ-C₂O₄) dimer (Weberski & McLauchlan, 2007a ). For related literature on vanadium-oxalate species, see: Salta et al. (1996 ); Triki et al. (2000 ); Li et al. (2003 ); Min et al. (2005 ); Tatiersky et al. (2005 ); Yang et al. (2006 ); Costisor et al. (2001 ). For related literature on the ligand, see: Kläui (1979 ); Kläui et al. (1987 ); Kamenar et al. (1988 ); Ward et al. (1998 ); Kölle & Englert (2002 ); Weberski & McLauchlan (2007b ).

Experimental

Crystal data

[Co₂V₂(C₅H₅)₂(C₂O₄)(C₄H₁₀O₃P)₆O₂]
M_r = 1292.48
Monoclinic, C 2/c
a = 28.364 (5) Å
b = 10.9825 (18) Å
c = 19.976 (3) Å
β = 117.412 (2)°
V = 5524.0 (16) Å³
Z = 4
Mo Kα radiation
μ = 1.17 mm⁻¹
T = 180 (2) K
0.63 × 0.33 × 0.06 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (APEX2; Bruker, 2008 ) T_min = 0.682, T_max = 0.932
26145 measured reflections
6845 independent reflections
5617 reflections with I > 2σ(I)
R_int = 0.036

Refinement

R[F² > 2σ(F²)] = 0.040
wR(F²) = 0.109
S = 1.00
6845 reflections
323 parameters
H-atom parameters constrained
Δρ_max = 0.70 e Å⁻³
Δρ_min = −0.45 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

V1—O3	1.594 (2)
V1—O1P	1.9932 (18)
V1—O3P	2.0145 (18)
V1—O1	2.0490 (18)
V1—O2	2.0727 (17)
V1—O2P	2.2077 (18)

O3—V1—O1P	97.46 (9)
O3—V1—O3P	99.73 (9)
O1P—V1—O3P	91.75 (7)
O3—V1—O1	99.26 (9)
O1P—V1—O1	89.59 (7)
O3P—V1—O1	160.61 (8)
O3—V1—O2	96.64 (9)
O1P—V1—O2	164.10 (8)
O3P—V1—O2	93.07 (7)
O1—V1—O2	80.91 (7)
O3—V1—O2P	177.13 (9)
O1P—V1—O2P	84.59 (7)
O3P—V1—O2P	82.17 (7)
O1—V1—O2P	78.71 (7)
O2—V1—O2P	81.07 (7)
C1—O1—V1	112.73 (16)
C2—O2—V1	112.22 (17)
Symmetry code: (i) $[-x, y, -z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2008); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808024458/ww2126sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808024458/ww2126Isup2.hkl

checkCIF report

Comment top

The title compound, {[Cp(P^OEt)₃Co]VO}₂(µ-C₂O₄), (I), (Cp = cyclopentadienyl anion, C₅H₅^-, P^OEt = diethylphosphite anion, C₄H₁₀O₃P^-) was synthesized by oxidation of the known {[Cp(P^OEt)₃Co]VCl}₂(µ-C₂O₄) dimer (Weberski & McLauchlan, 2007a).

Dozens of both terminal (e.g., Tatiersky et al., 2005; Costisor et al., 2006) and bridging (e.g., Salta et al., 1996; Triki et al., 2000; Li et al., 2003; Min et al., 2005; Yang et al., 2006) oxalato complexes have been reported for vanadium. The distances and angles in (I) (Table 1) are comparable to those in these known reported structures for oxalate bridging complexes. Similarly, the distances and angles in (I) are comparable to the previously reported structures involving the ligand (Kläui, 1979; Kläui et al., 1987; Kamenar et al., 1988; Ward et al., 1998; Kölle & Englert, 2002; Weberski & McLauchlan, 2007b)

The geometric center of the dimer lies on the inversion center (Fig. 1).

Some minor disorder, as may be expected, is present in the ethyl groups and the Cp ring, which results in some slightly elongated ellipsoids, but the disorder was not modeled.

Related literature top

The title compound was synthesized by oxidation of the known {[Cp(P^OEt)₃Co]VCl}₂(µ-C₂O₄) dimer (Weberski & McLauchlan, 2007a). For related literature on vanadium-oxalate species, see: Salta et al. (1996); Triki et al. (2000); Li et al. (2003); Min et al. (2005); Tatiersky et al. (2005); Yang et al. (2006); Costisor et al. (2001). For related literature on the ligand, see: Kläui (1979); Kläui et al. (1987); Kamenar et al. (1988); Ward et al. (1998); Kölle & Englert (2002); Weberski & McLauchlan (2007b).

Experimental top

Compound (I) was synthesized by serendipitous air oxidation of the known {[Cp(P^OEt)₃Co]VCl}₂(µ-C₂O₄) dimer (Weberski & McLauchlan, 2007a) in diethyl ether (Cp = cyclopentadienyl anion, C₅H₅^-, P^OEt = diethylphosphite anion, C₄H₁₀O₃P^-). An amount of 44 mg of green, X-ray diffraction quality crystals of (I) were grown from the unoptimized slow evaporation of an ether solution at ca 300 K. The crystals shatter at 100 K. Anal. Calcd. for C₃₆H₇₀Co₂O₂₄P₆V₂: C, 33.45; H, 5.46. Found: C, 33.85; H, 5.65. The compound decomposes above 473 K. Infrared (cm^-1): 441, 478, 590, 728, 771, 835, 930, 977, 1031, 1129, 1262, 1353, 1388, 1426, 1444, 1477, 1625, 2345, 2367, 2930, 2979, 3423. Magnetic susceptibility (Evans method, uncorrected), χ_m (χ_mT) 1.65 x 10^-3 erg*G^-2mol^-1 (0.492). Electronic absorbance (UV/vis, CH₃CN, λ, nm(ε, M^-1 cm^-1)): 242 (42000), 333 (5700), 485 (124), 656 (116).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: APEX2 (Bruker, 2008); data reduction: APEX2 (Bruker, 2008); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. View of the molecular structure of (I) showing 50% displacement ellipsoids (arbitrary spheres for the H atoms). Symmetry code: (i) -x, y, -z + 1/2.

Bis[1,4(η⁵)-cyclopentadienyl]hexakis(µ-diethyl phosphito)-1:2κ⁶P:O;3:4κ⁶O:P-µ-oxalato-2:3κ⁴O¹,O²:O^1',O^2'- dioxido-2κO,3κO-1,4-dicobalt(III)-2,3-divanadium(IV) top

Crystal data top

[Co₂V₂(C₅H₅)₂(C₂O₄)(C₄H₁₀O₃P)₆O₂]	F(000) = 2672
M_r = 1292.48	D_x = 1.554 Mg m⁻³
Monoclinic, C2/c	Melting point: dec. 473(1) K
Hall symbol: -C 2yc	Mo Kα radiation, λ = 0.71073 Å
a = 28.364 (5) Å	Cell parameters from 9976 reflections
b = 10.9825 (18) Å	θ = 5.0–63.5°
c = 19.976 (3) Å	µ = 1.17 mm⁻¹
β = 117.412 (2)°	T = 180 K
V = 5524.0 (16) Å³	Plate, green
Z = 4	0.63 × 0.33 × 0.06 mm

Data collection top

Bruker SMART APEX CCD diffractometer	6845 independent reflections
Radiation source: fine-focus sealed tube	5617 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
ω scans	θ_max = 28.3°, θ_min = 2.0°
Absorption correction: multi-scan (APEX2; Bruker, 2008)	h = −37→37
T_min = 0.682, T_max = 0.932	k = −14→14
26145 measured reflections	l = −26→26

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.109	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.0479P)² + 16.0571P] where P = (F_o² + 2F_c²)/3
6845 reflections	(Δ/σ)_max = 0.001
323 parameters	Δρ_max = 0.70 e Å⁻³
0 restraints	Δρ_min = −0.45 e Å⁻³

Crystal data top

[Co₂V₂(C₅H₅)₂(C₂O₄)(C₄H₁₀O₃P)₆O₂]	V = 5524.0 (16) Å³
M_r = 1292.48	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 28.364 (5) Å	µ = 1.17 mm⁻¹
b = 10.9825 (18) Å	T = 180 K
c = 19.976 (3) Å	0.63 × 0.33 × 0.06 mm
β = 117.412 (2)°

Data collection top

Bruker SMART APEX CCD diffractometer	6845 independent reflections
Absorption correction: multi-scan (APEX2; Bruker, 2008)	5617 reflections with I > 2σ(I)
T_min = 0.682, T_max = 0.932	R_int = 0.037
26145 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	0 restraints
wR(F²) = 0.109	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.0479P)² + 16.0571P] where P = (F_o² + 2F_c²)/3
6845 reflections	Δρ_max = 0.70 e Å⁻³
323 parameters	Δρ_min = −0.45 e Å⁻³

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
V1	0.028671 (16)	0.78146 (4)	0.13941 (2)	0.02455 (10)
Co1	0.176050 (13)	0.74072 (3)	0.16646 (2)	0.02774 (10)
P1	0.11499 (3)	0.60266 (6)	0.12884 (4)	0.02764 (14)
P2	0.15939 (3)	0.78092 (6)	0.26021 (4)	0.02754 (14)
P3	0.11777 (3)	0.87517 (6)	0.09797 (4)	0.02816 (15)
O1	0.00650 (7)	0.66231 (15)	0.19874 (10)	0.0286 (4)
O2	0.01090 (7)	0.90562 (15)	0.20266 (10)	0.0275 (4)
C1	0.0000	0.7134 (3)	0.2500	0.0245 (7)
C2	0.0000	0.8544 (3)	0.2500	0.0248 (7)
O3	−0.02642 (8)	0.79215 (18)	0.06448 (11)	0.0379 (4)
O1P	0.05862 (7)	0.64296 (16)	0.10672 (11)	0.0309 (4)
O1A	0.13253 (8)	0.50150 (17)	0.19333 (11)	0.0375 (4)
O2A	0.11265 (8)	0.5267 (2)	0.05926 (12)	0.0428 (5)
C1A	0.09433 (16)	0.4095 (3)	0.1891 (2)	0.0563 (9)
H1AA	0.0580	0.4430	0.1613	0.068*
H1AB	0.0970	0.3382	0.1606	0.068*
C2A	0.1032 (2)	0.3716 (6)	0.2616 (3)	0.105 (2)
H2AA	0.0772	0.3089	0.2567	0.157*
H2AB	0.0994	0.4415	0.2893	0.157*
H2AC	0.1392	0.3383	0.2892	0.157*
C3A	0.06647 (12)	0.5172 (3)	−0.01328 (17)	0.0377 (6)
H3AA	0.0420	0.5859	−0.0204	0.045*
H3AB	0.0474	0.4402	−0.0163	0.045*
C4A	0.08407 (16)	0.5198 (4)	−0.0731 (2)	0.0567 (9)
H4AA	0.0530	0.5145	−0.1228	0.085*
H4AB	0.1077	0.4506	−0.0663	0.085*
H4AC	0.1031	0.5960	−0.0695	0.085*
O2P	0.10274 (7)	0.76760 (15)	0.24648 (10)	0.0273 (4)
O1B	0.18059 (8)	0.91352 (19)	0.29463 (14)	0.0444 (5)
O2B	0.19748 (8)	0.6950 (2)	0.32940 (11)	0.0397 (5)
C1B	0.14588 (12)	1.0097 (3)	0.29536 (18)	0.0403 (6)
H1BA	0.1091	0.9928	0.2566	0.048*
H1BB	0.1570	1.0881	0.2826	0.048*
C2B	0.1473 (2)	1.0196 (5)	0.3698 (3)	0.0848 (15)
H2BA	0.1262	1.0900	0.3702	0.127*
H2BB	0.1841	1.0301	0.4087	0.127*
H2BC	0.1325	0.9454	0.3800	0.127*
C3B	0.18998 (16)	0.6875 (4)	0.3955 (2)	0.0542 (9)
H3BA	0.1516	0.6810	0.3806	0.065*
H3BB	0.2038	0.7621	0.4261	0.065*
C4B	0.21855 (14)	0.5785 (3)	0.4410 (2)	0.0535 (8)
H4BA	0.2162	0.5779	0.4884	0.080*
H4BB	0.2559	0.5818	0.4519	0.080*
H4BC	0.2022	0.5043	0.4124	0.080*
O3P	0.07192 (7)	0.90314 (15)	0.11549 (10)	0.0287 (4)
O1C	0.09368 (8)	0.83591 (19)	0.01116 (11)	0.0396 (5)
O2C	0.14763 (8)	1.00128 (18)	0.10399 (14)	0.0469 (6)
C1C	0.04967 (13)	0.9052 (3)	−0.04630 (17)	0.0448 (7)
H1CA	0.0637	0.9746	−0.0633	0.054*
H1CB	0.0270	0.9378	−0.0248	0.054*
C2C	0.01791 (18)	0.8257 (3)	−0.1108 (2)	0.0791 (15)
H2CA	−0.0109	0.8730	−0.1500	0.119*
H2CB	0.0028	0.7590	−0.0942	0.119*
H2CC	0.0406	0.7921	−0.1312	0.119*
C3C	0.12391 (11)	1.1198 (2)	0.09617 (17)	0.0337 (6)
H3CA	0.1295	1.1500	0.1460	0.040*
H3CB	0.0852	1.1152	0.0624	0.040*
C4C	0.14959 (12)	1.2044 (3)	0.0636 (2)	0.0435 (7)
H4CA	0.1356	1.2869	0.0607	0.065*
H4CB	0.1419	1.1767	0.0129	0.065*
H4CC	0.1881	1.2048	0.0959	0.065*
C32	0.24880 (11)	0.6532 (3)	0.22456 (19)	0.0429 (7)
H32	0.2576	0.5990	0.2656	0.051*
C33	0.25670 (12)	0.7796 (3)	0.2303 (2)	0.0523 (9)
H33	0.2718	0.8255	0.2757	0.063*
C34	0.23856 (15)	0.8257 (4)	0.1582 (3)	0.0677 (13)
H34	0.2394	0.9088	0.1455	0.081*
C35	0.21853 (15)	0.7274 (5)	0.1062 (2)	0.0696 (13)
H35	0.2030	0.7329	0.0529	0.084*
C36	0.22599 (12)	0.6204 (3)	0.1488 (2)	0.0512 (8)
H36	0.2170	0.5401	0.1293	0.061*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.0245 (2)	0.02041 (19)	0.0309 (2)	0.00117 (15)	0.01458 (17)	−0.00023 (15)
Co1	0.02674 (18)	0.02207 (16)	0.0390 (2)	0.00463 (12)	0.01910 (15)	0.00510 (13)
P1	0.0314 (3)	0.0205 (3)	0.0336 (3)	0.0033 (2)	0.0171 (3)	−0.0002 (2)
P2	0.0246 (3)	0.0253 (3)	0.0329 (3)	−0.0018 (2)	0.0135 (3)	−0.0004 (2)
P3	0.0298 (3)	0.0221 (3)	0.0388 (4)	0.0052 (2)	0.0212 (3)	0.0071 (3)
O1	0.0325 (9)	0.0175 (8)	0.0429 (10)	−0.0020 (6)	0.0236 (8)	−0.0026 (7)
O2	0.0315 (9)	0.0180 (7)	0.0401 (10)	0.0001 (6)	0.0225 (8)	0.0006 (7)
C1	0.0187 (14)	0.0185 (14)	0.0369 (18)	0.000	0.0133 (13)	0.000
C2	0.0228 (15)	0.0172 (14)	0.0347 (18)	0.000	0.0135 (14)	0.000
O3	0.0314 (10)	0.0348 (10)	0.0419 (11)	0.0034 (8)	0.0120 (9)	0.0001 (8)
O1P	0.0326 (9)	0.0253 (8)	0.0389 (10)	−0.0003 (7)	0.0198 (8)	−0.0065 (7)
O1A	0.0433 (11)	0.0241 (9)	0.0435 (11)	−0.0020 (8)	0.0185 (9)	0.0064 (8)
O2A	0.0421 (11)	0.0443 (12)	0.0396 (11)	0.0125 (9)	0.0168 (9)	−0.0094 (9)
C1A	0.072 (2)	0.0375 (17)	0.058 (2)	−0.0188 (16)	0.0285 (19)	0.0034 (15)
C2A	0.118 (4)	0.133 (5)	0.067 (3)	−0.067 (4)	0.046 (3)	0.004 (3)
C3A	0.0390 (15)	0.0340 (14)	0.0414 (15)	−0.0036 (11)	0.0196 (12)	−0.0083 (12)
C4A	0.063 (2)	0.068 (2)	0.0461 (19)	−0.0039 (18)	0.0307 (17)	−0.0128 (17)
O2P	0.0272 (9)	0.0254 (8)	0.0306 (9)	−0.0009 (7)	0.0144 (7)	0.0002 (7)
O1B	0.0359 (11)	0.0347 (10)	0.0677 (14)	−0.0093 (8)	0.0282 (10)	−0.0180 (10)
O2B	0.0324 (10)	0.0495 (12)	0.0351 (10)	0.0043 (9)	0.0138 (8)	0.0074 (9)
C1B	0.0377 (15)	0.0304 (13)	0.0549 (18)	−0.0032 (11)	0.0232 (14)	−0.0044 (12)
C2B	0.113 (4)	0.084 (3)	0.079 (3)	0.037 (3)	0.063 (3)	0.007 (3)
C3B	0.066 (2)	0.054 (2)	0.0445 (18)	0.0085 (17)	0.0268 (17)	0.0085 (16)
C4B	0.0481 (19)	0.061 (2)	0.0481 (19)	0.0047 (16)	0.0192 (15)	0.0151 (16)
O3P	0.0307 (9)	0.0229 (8)	0.0380 (10)	0.0055 (7)	0.0205 (8)	0.0054 (7)
O1C	0.0442 (11)	0.0435 (11)	0.0368 (11)	0.0169 (9)	0.0234 (9)	0.0103 (9)
O2C	0.0412 (11)	0.0224 (9)	0.0897 (18)	0.0063 (8)	0.0407 (12)	0.0144 (10)
C1C	0.0518 (18)	0.0427 (16)	0.0379 (16)	0.0138 (14)	0.0190 (14)	0.0120 (13)
C2C	0.076 (3)	0.0360 (18)	0.077 (3)	−0.0013 (18)	−0.006 (2)	0.0073 (18)
C3C	0.0346 (13)	0.0231 (12)	0.0444 (15)	0.0049 (10)	0.0191 (12)	0.0044 (11)
C4C	0.0403 (16)	0.0289 (13)	0.0593 (19)	0.0005 (12)	0.0212 (14)	0.0141 (13)
C32	0.0280 (13)	0.0427 (16)	0.0587 (19)	0.0143 (12)	0.0206 (13)	0.0114 (14)
C33	0.0287 (14)	0.0448 (17)	0.085 (3)	−0.0015 (13)	0.0273 (16)	−0.0089 (17)
C34	0.047 (2)	0.050 (2)	0.132 (4)	0.0157 (16)	0.063 (2)	0.034 (2)
C35	0.046 (2)	0.122 (4)	0.057 (2)	0.035 (2)	0.0371 (18)	0.028 (2)
C36	0.0349 (16)	0.0471 (18)	0.076 (2)	0.0107 (13)	0.0294 (16)	−0.0104 (17)

Geometric parameters (Å, º) top

V1—O3	1.594 (2)	C4A—H4AB	0.9800
V1—O1P	1.9932 (18)	C4A—H4AC	0.9800
V1—O3P	2.0145 (18)	O1B—C1B	1.449 (3)
V1—O1	2.0490 (18)	O2B—C3B	1.433 (4)
V1—O2	2.0727 (17)	C1B—C2B	1.473 (5)
V1—O2P	2.2077 (18)	C1B—H1BA	0.9900
Co1—C35	2.063 (3)	C1B—H1BB	0.9900
Co1—C34	2.077 (3)	C2B—H2BA	0.9800
Co1—C32	2.079 (3)	C2B—H2BB	0.9800
Co1—C36	2.082 (3)	C2B—H2BC	0.9800
Co1—C33	2.087 (3)	C3B—C4B	1.496 (5)
Co1—P1	2.1597 (8)	C3B—H3BA	0.9900
Co1—P3	2.1684 (7)	C3B—H3BB	0.9900
Co1—P2	2.1774 (8)	C4B—H4BA	0.9800
P1—O1P	1.5156 (19)	C4B—H4BB	0.9800
P1—O2A	1.596 (2)	C4B—H4BC	0.9800
P1—O1A	1.597 (2)	O1C—C1C	1.461 (3)
P2—O2P	1.5075 (18)	O2C—C3C	1.441 (3)
P2—O1B	1.604 (2)	C1C—C2C	1.471 (5)
P2—O2B	1.610 (2)	C1C—H1CA	0.9900
P3—O3P	1.5257 (18)	C1C—H1CB	0.9900
P3—O2C	1.599 (2)	C2C—H2CA	0.9800
P3—O1C	1.603 (2)	C2C—H2CB	0.9800
O1—C1	1.253 (2)	C2C—H2CC	0.9800
O2—C2	1.255 (2)	C3C—C4C	1.501 (4)
C1—O1ⁱ	1.254 (2)	C3C—H3CA	0.9900
C1—C2	1.549 (4)	C3C—H3CB	0.9900
C2—O2ⁱ	1.255 (2)	C4C—H4CA	0.9800
O1A—C1A	1.455 (4)	C4C—H4CB	0.9800
O2A—C3A	1.442 (3)	C4C—H4CC	0.9800
C1A—C2A	1.415 (5)	C32—C36	1.391 (5)
C1A—H1AA	0.9900	C32—C33	1.402 (5)
C1A—H1AB	0.9900	C32—H32	0.9500
C2A—H2AA	0.9800	C33—C34	1.383 (6)
C2A—H2AB	0.9800	C33—H33	0.9500
C2A—H2AC	0.9800	C34—C35	1.422 (7)
C3A—C4A	1.492 (4)	C34—H34	0.9500
C3A—H3AA	0.9900	C35—C36	1.409 (6)
C3A—H3AB	0.9900	C35—H35	0.9500
C4A—H4AA	0.9800	C36—H36	0.9500

O3—V1—O1P	97.46 (9)	C3A—C4A—H4AA	109.5
O3—V1—O3P	99.73 (9)	C3A—C4A—H4AB	109.5
O1P—V1—O3P	91.75 (7)	H4AA—C4A—H4AB	109.5
O3—V1—O1	99.26 (9)	C3A—C4A—H4AC	109.5
O1P—V1—O1	89.59 (7)	H4AA—C4A—H4AC	109.5
O3P—V1—O1	160.61 (8)	H4AB—C4A—H4AC	109.5
O3—V1—O2	96.64 (9)	P2—O2P—V1	128.96 (11)
O1P—V1—O2	164.10 (8)	C1B—O1B—P2	122.94 (18)
O3P—V1—O2	93.07 (7)	C3B—O2B—P2	119.9 (2)
O1—V1—O2	80.91 (7)	O1B—C1B—C2B	111.2 (3)
O3—V1—O2P	177.13 (9)	O1B—C1B—H1BA	109.4
O1P—V1—O2P	84.59 (7)	C2B—C1B—H1BA	109.4
O3P—V1—O2P	82.17 (7)	O1B—C1B—H1BB	109.4
O1—V1—O2P	78.71 (7)	C2B—C1B—H1BB	109.4
O2—V1—O2P	81.07 (7)	H1BA—C1B—H1BB	108.0
C35—Co1—C34	40.17 (18)	C1B—C2B—H2BA	109.5
C35—Co1—C32	66.22 (14)	C1B—C2B—H2BB	109.5
C34—Co1—C32	65.66 (14)	H2BA—C2B—H2BB	109.5
C35—Co1—C36	39.74 (16)	C1B—C2B—H2BC	109.5
C34—Co1—C36	66.39 (15)	H2BA—C2B—H2BC	109.5
C32—Co1—C36	39.06 (14)	H2BB—C2B—H2BC	109.5
C35—Co1—C33	66.45 (17)	O2B—C3B—C4B	109.7 (3)
C34—Co1—C33	38.81 (17)	O2B—C3B—H3BA	109.7
C32—Co1—C33	39.33 (13)	C4B—C3B—H3BA	109.7
C36—Co1—C33	66.01 (14)	O2B—C3B—H3BB	109.7
C35—Co1—P1	109.73 (16)	C4B—C3B—H3BB	109.7
C34—Co1—P1	149.89 (15)	H3BA—C3B—H3BB	108.2
C32—Co1—P1	107.49 (9)	C3B—C4B—H4BA	109.5
C36—Co1—P1	89.69 (10)	C3B—C4B—H4BB	109.5
C33—Co1—P1	146.52 (10)	H4BA—C4B—H4BB	109.5
C35—Co1—P3	99.24 (11)	C3B—C4B—H4BC	109.5
C34—Co1—P3	94.27 (10)	H4BA—C4B—H4BC	109.5
C32—Co1—P3	159.92 (9)	H4BB—C4B—H4BC	109.5
C36—Co1—P3	134.90 (11)	P3—O3P—V1	126.68 (10)
C33—Co1—P3	123.29 (10)	C1C—O1C—P3	119.63 (19)
P1—Co1—P3	90.13 (3)	C3C—O2C—P3	124.74 (17)
C35—Co1—P2	158.80 (14)	O1C—C1C—C2C	109.7 (3)
C34—Co1—P2	120.59 (15)	O1C—C1C—H1CA	109.7
C32—Co1—P2	99.57 (10)	C2C—C1C—H1CA	109.7
C36—Co1—P2	135.08 (11)	O1C—C1C—H1CB	109.7
C33—Co1—P2	92.52 (11)	C2C—C1C—H1CB	109.7
P1—Co1—P2	89.13 (3)	H1CA—C1C—H1CB	108.2
P3—Co1—P2	90.02 (3)	C1C—C2C—H2CA	109.5
O1P—P1—O2A	106.46 (11)	C1C—C2C—H2CB	109.5
O1P—P1—O1A	109.47 (11)	H2CA—C2C—H2CB	109.5
O2A—P1—O1A	102.22 (12)	C1C—C2C—H2CC	109.5
O1P—P1—Co1	117.76 (8)	H2CA—C2C—H2CC	109.5
O2A—P1—Co1	112.03 (9)	H2CB—C2C—H2CC	109.5
O1A—P1—Co1	107.79 (8)	O2C—C3C—C4C	108.1 (2)
O2P—P2—O1B	108.90 (10)	O2C—C3C—H3CA	110.1
O2P—P2—O2B	109.71 (11)	C4C—C3C—H3CA	110.1
O1B—P2—O2B	101.13 (12)	O2C—C3C—H3CB	110.1
O2P—P2—Co1	117.32 (8)	C4C—C3C—H3CB	110.1
O1B—P2—Co1	111.45 (9)	H3CA—C3C—H3CB	108.4
O2B—P2—Co1	107.08 (8)	C3C—C4C—H4CA	109.5
O3P—P3—O2C	106.64 (10)	C3C—C4C—H4CB	109.5
O3P—P3—O1C	108.57 (11)	H4CA—C4C—H4CB	109.5
O2C—P3—O1C	105.17 (13)	C3C—C4C—H4CC	109.5
O3P—P3—Co1	118.37 (7)	H4CA—C4C—H4CC	109.5
O2C—P3—Co1	108.60 (8)	H4CB—C4C—H4CC	109.5
O1C—P3—Co1	108.72 (8)	C36—C32—C33	108.8 (3)
C1—O1—V1	112.73 (16)	C36—C32—Co1	70.59 (17)
C2—O2—V1	112.22 (17)	C33—C32—Co1	70.64 (17)
O1—C1—O1ⁱ	126.8 (3)	C36—C32—H32	125.6
O1—C1—C2	116.59 (15)	C33—C32—H32	125.6
O1ⁱ—C1—C2	116.59 (15)	Co1—C32—H32	124.8
O2—C2—O2ⁱ	126.8 (3)	C34—C33—C32	108.0 (4)
O2—C2—C1	116.60 (15)	C34—C33—Co1	70.2 (2)
O2ⁱ—C2—C1	116.60 (15)	C32—C33—Co1	70.03 (17)
P1—O1P—V1	132.76 (11)	C34—C33—H33	126.0
C1A—O1A—P1	119.3 (2)	C32—C33—H33	126.0
C3A—O2A—P1	124.59 (18)	Co1—C33—H33	125.3
C2A—C1A—O1A	111.6 (3)	C33—C34—C35	108.3 (3)
C2A—C1A—H1AA	109.3	C33—C34—Co1	70.99 (19)
O1A—C1A—H1AA	109.3	C35—C34—Co1	69.4 (2)
C2A—C1A—H1AB	109.3	C33—C34—H34	125.8
O1A—C1A—H1AB	109.3	C35—C34—H34	125.8
H1AA—C1A—H1AB	108.0	Co1—C34—H34	125.4
C1A—C2A—H2AA	109.5	C36—C35—C34	107.1 (3)
C1A—C2A—H2AB	109.5	C36—C35—Co1	70.88 (19)
H2AA—C2A—H2AB	109.5	C34—C35—Co1	70.5 (2)
C1A—C2A—H2AC	109.5	C36—C35—H35	126.4
H2AA—C2A—H2AC	109.5	C34—C35—H35	126.4
H2AB—C2A—H2AC	109.5	Co1—C35—H35	123.9
O2A—C3A—C4A	108.6 (3)	C32—C36—C35	107.8 (3)
O2A—C3A—H3AA	110.0	C32—C36—Co1	70.35 (17)
C4A—C3A—H3AA	110.0	C35—C36—Co1	69.38 (19)
O2A—C3A—H3AB	110.0	C32—C36—H36	126.1
C4A—C3A—H3AB	110.0	C35—C36—H36	126.1
H3AA—C3A—H3AB	108.3	Co1—C36—H36	125.7

C35—Co1—P1—O1P	−128.14 (15)	O3P—V1—O2P—P2	−32.47 (13)
C34—Co1—P1—O1P	−127.0 (2)	O1—V1—O2P—P2	150.71 (14)
C32—Co1—P1—O1P	161.50 (13)	O2—V1—O2P—P2	−126.85 (14)
C36—Co1—P1—O1P	−163.17 (14)	O2P—P2—O1B—C1B	−12.3 (3)
C33—Co1—P1—O1P	155.0 (2)	O2B—P2—O1B—C1B	−127.8 (2)
P3—Co1—P1—O1P	−28.28 (9)	Co1—P2—O1B—C1B	118.7 (2)
P2—Co1—P1—O1P	61.74 (9)	O2P—P2—O2B—C3B	−42.2 (3)
C35—Co1—P1—O2A	−4.20 (15)	O1B—P2—O2B—C3B	72.7 (3)
C34—Co1—P1—O2A	−3.1 (2)	Co1—P2—O2B—C3B	−170.6 (2)
C32—Co1—P1—O2A	−74.56 (13)	P2—O1B—C1B—C2B	99.8 (4)
C36—Co1—P1—O2A	−39.23 (14)	P2—O2B—C3B—C4B	163.9 (2)
C33—Co1—P1—O2A	−81.1 (2)	O2C—P3—O3P—V1	−165.84 (14)
P3—Co1—P1—O2A	95.66 (9)	O1C—P3—O3P—V1	81.30 (15)
P2—Co1—P1—O2A	−174.32 (9)	Co1—P3—O3P—V1	−43.18 (16)
C35—Co1—P1—O1A	107.49 (14)	O3—V1—O3P—P3	−109.89 (15)
C34—Co1—P1—O1A	108.6 (2)	O1P—V1—O3P—P3	−12.01 (14)
C32—Co1—P1—O1A	37.13 (13)	O1—V1—O3P—P3	81.7 (3)
C36—Co1—P1—O1A	72.46 (14)	O2—V1—O3P—P3	152.83 (14)
C33—Co1—P1—O1A	30.6 (2)	O2P—V1—O3P—P3	72.28 (14)
P3—Co1—P1—O1A	−152.64 (9)	O3P—P3—O1C—C1C	44.0 (2)
P2—Co1—P1—O1A	−62.63 (9)	O2C—P3—O1C—C1C	−69.8 (2)
C35—Co1—P2—O2P	173.1 (4)	Co1—P3—O1C—C1C	174.1 (2)
C34—Co1—P2—O2P	151.66 (14)	O3P—P3—O2C—C3C	−22.9 (3)
C32—Co1—P2—O2P	−141.04 (12)	O1C—P3—O2C—C3C	92.3 (3)
C36—Co1—P2—O2P	−122.13 (16)	Co1—P3—O2C—C3C	−151.5 (2)
C33—Co1—P2—O2P	−179.98 (13)	P3—O1C—C1C—C2C	−152.3 (3)
P1—Co1—P2—O2P	−33.44 (8)	P3—O2C—C3C—C4C	−149.4 (2)
P3—Co1—P2—O2P	56.69 (8)	C35—Co1—C32—C36	−37.8 (2)
C35—Co1—P2—O1B	46.6 (4)	C34—Co1—C32—C36	−81.9 (3)
C34—Co1—P2—O1B	25.17 (15)	C33—Co1—C32—C36	−119.1 (3)
C32—Co1—P2—O1B	92.47 (13)	P1—Co1—C32—C36	66.6 (2)
C36—Co1—P2—O1B	111.37 (17)	P3—Co1—C32—C36	−83.8 (3)
C33—Co1—P2—O1B	53.52 (14)	P2—Co1—C32—C36	158.71 (19)
P1—Co1—P2—O1B	−159.94 (9)	C35—Co1—C32—C33	81.3 (3)
P3—Co1—P2—O1B	−69.81 (9)	C34—Co1—C32—C33	37.1 (2)
C35—Co1—P2—O2B	−63.1 (4)	C36—Co1—C32—C33	119.1 (3)
C34—Co1—P2—O2B	−84.57 (15)	P1—Co1—C32—C33	−174.3 (2)
C32—Co1—P2—O2B	−17.27 (13)	P3—Co1—C32—C33	35.3 (4)
C36—Co1—P2—O2B	1.64 (17)	P2—Co1—C32—C33	−82.2 (2)
C33—Co1—P2—O2B	−56.21 (13)	C36—C32—C33—C34	0.3 (3)
P1—Co1—P2—O2B	90.33 (9)	Co1—C32—C33—C34	−60.2 (2)
P3—Co1—P2—O2B	−179.54 (9)	C36—C32—C33—Co1	60.5 (2)
C35—Co1—P3—O3P	172.13 (18)	C35—Co1—C33—C34	38.0 (2)
C34—Co1—P3—O3P	−147.70 (17)	C32—Co1—C33—C34	118.7 (3)
C32—Co1—P3—O3P	−146.0 (3)	C36—Co1—C33—C34	81.6 (3)
C36—Co1—P3—O3P	151.80 (16)	P1—Co1—C33—C34	128.5 (2)
C33—Co1—P3—O3P	−120.05 (16)	P3—Co1—C33—C34	−47.6 (3)
P1—Co1—P3—O3P	62.11 (9)	P2—Co1—C33—C34	−139.3 (2)
P2—Co1—P3—O3P	−27.02 (9)	C35—Co1—C33—C32	−80.7 (2)
C35—Co1—P3—O2C	−66.20 (18)	C34—Co1—C33—C32	−118.7 (3)
C34—Co1—P3—O2C	−26.03 (18)	C36—Co1—C33—C32	−37.1 (2)
C32—Co1—P3—O2C	−24.4 (3)	P1—Co1—C33—C32	9.8 (3)
C36—Co1—P3—O2C	−86.53 (17)	P3—Co1—C33—C32	−166.27 (17)
C33—Co1—P3—O2C	1.62 (17)	P2—Co1—C33—C32	102.1 (2)
P1—Co1—P3—O2C	−176.22 (10)	C32—C33—C34—C35	0.5 (4)
P2—Co1—P3—O2C	94.65 (10)	Co1—C33—C34—C35	−59.6 (2)
C35—Co1—P3—O1C	47.72 (18)	C32—C33—C34—Co1	60.1 (2)
C34—Co1—P3—O1C	87.88 (17)	C35—Co1—C34—C33	−119.0 (3)
C32—Co1—P3—O1C	89.6 (3)	C32—Co1—C34—C33	−37.6 (2)
C36—Co1—P3—O1C	27.39 (17)	C36—Co1—C34—C33	−80.5 (2)
C33—Co1—P3—O1C	115.54 (16)	P1—Co1—C34—C33	−120.6 (3)
P1—Co1—P3—O1C	−62.30 (9)	P3—Co1—C34—C33	141.8 (2)
P2—Co1—P3—O1C	−151.43 (9)	P2—Co1—C34—C33	49.2 (2)
O3—V1—O1—C1	−104.15 (14)	C32—Co1—C34—C35	81.4 (2)
O1P—V1—O1—C1	158.36 (13)	C36—Co1—C34—C35	38.4 (2)
O3P—V1—O1—C1	64.2 (3)	C33—Co1—C34—C35	119.0 (3)
O2—V1—O1—C1	−8.84 (12)	P1—Co1—C34—C35	−1.6 (4)
O2P—V1—O1—C1	73.79 (12)	P3—Co1—C34—C35	−99.3 (2)
O3—V1—O2—C2	103.96 (13)	P2—Co1—C34—C35	168.18 (19)
O1P—V1—O2—C2	−48.4 (3)	C33—C34—C35—C36	−1.2 (4)
O3P—V1—O2—C2	−155.87 (12)	Co1—C34—C35—C36	−61.8 (2)
O1—V1—O2—C2	5.59 (11)	C33—C34—C35—Co1	60.6 (2)
O2P—V1—O2—C2	−74.30 (12)	C34—Co1—C35—C36	117.0 (3)
V1—O1—C1—O1ⁱ	−169.74 (13)	C32—Co1—C35—C36	37.1 (2)
V1—O1—C1—C2	10.26 (13)	C33—Co1—C35—C36	80.2 (2)
V1—O2—C2—O2ⁱ	177.97 (13)	P1—Co1—C35—C36	−63.9 (2)
V1—O2—C2—C1	−2.03 (13)	P3—Co1—C35—C36	−157.4 (2)
O1—C1—C2—O2	−5.76 (13)	P2—Co1—C35—C36	87.8 (5)
O1ⁱ—C1—C2—O2	174.24 (13)	C32—Co1—C35—C34	−79.8 (2)
O1—C1—C2—O2ⁱ	174.24 (13)	C36—Co1—C35—C34	−117.0 (3)
O1ⁱ—C1—C2—O2ⁱ	−5.76 (13)	C33—Co1—C35—C34	−36.7 (2)
O2A—P1—O1P—V1	−155.10 (15)	P1—Co1—C35—C34	179.1 (2)
O1A—P1—O1P—V1	95.11 (16)	P3—Co1—C35—C34	85.7 (2)
Co1—P1—O1P—V1	−28.41 (18)	P2—Co1—C35—C34	−29.2 (5)
O3—V1—O1P—P1	153.83 (16)	C33—C32—C36—C35	−1.1 (3)
O3P—V1—O1P—P1	53.77 (16)	Co1—C32—C36—C35	59.5 (2)
O1—V1—O1P—P1	−106.88 (16)	C33—C32—C36—Co1	−60.6 (2)
O2—V1—O1P—P1	−53.9 (4)	C34—C35—C36—C32	1.4 (4)
O2P—V1—O1P—P1	−28.19 (16)	Co1—C35—C36—C32	−60.1 (2)
O1P—P1—O1A—C1A	39.5 (3)	C34—C35—C36—Co1	61.5 (2)
O2A—P1—O1A—C1A	−73.0 (3)	C35—Co1—C36—C32	118.8 (3)
Co1—P1—O1A—C1A	168.8 (2)	C34—Co1—C36—C32	79.9 (2)
O1P—P1—O2A—C3A	8.5 (3)	C33—Co1—C36—C32	37.3 (2)
O1A—P1—O2A—C3A	123.3 (2)	P1—Co1—C36—C32	−118.93 (19)
Co1—P1—O2A—C3A	−121.6 (2)	P3—Co1—C36—C32	151.20 (16)
P1—O1A—C1A—C2A	−148.7 (4)	P2—Co1—C36—C32	−30.5 (3)
P1—O2A—C3A—C4A	141.6 (3)	C34—Co1—C36—C35	−38.9 (3)
O1B—P2—O2P—V1	101.82 (15)	C32—Co1—C36—C35	−118.8 (3)
O2B—P2—O2P—V1	−148.35 (13)	C33—Co1—C36—C35	−81.4 (3)
Co1—P2—O2P—V1	−25.91 (15)	P1—Co1—C36—C35	122.3 (2)
O3—V1—O2P—P2	−164.0 (17)	P3—Co1—C36—C35	32.4 (3)
O1P—V1—O2P—P2	60.05 (13)	P2—Co1—C36—C35	−149.2 (2)

Symmetry code: (i) −x, y, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Co₂V₂(C₅H₅)₂(C₂O₄)(C₄H₁₀O₃P)₆O₂]
M_r	1292.48
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	180
a, b, c (Å)	28.364 (5), 10.9825 (18), 19.976 (3)
β (°)	117.412 (2)
V (Å³)	5524.0 (16)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.17
Crystal size (mm)	0.63 × 0.33 × 0.06

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (APEX2; Bruker, 2008)
T_min, T_max	0.682, 0.932
No. of measured, independent and observed [I > 2σ(I)] reflections	26145, 6845, 5617
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.109, 1.00
No. of reflections	6845
No. of parameters	323
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0479P)² + 16.0571P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.70, −0.45

Computer programs: APEX2 (Bruker, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

V1—O3	1.594 (2)	V1—O2P	2.2077 (18)
V1—O1P	1.9932 (18)	O1—C1	1.253 (2)
V1—O3P	2.0145 (18)	O2—C2	1.255 (2)
V1—O1	2.0490 (18)	C1—C2	1.549 (4)
V1—O2	2.0727 (17)

O3—V1—O1P	97.46 (9)	O3—V1—O2P	177.13 (9)
O3—V1—O3P	99.73 (9)	O1P—V1—O2P	84.59 (7)
O1P—V1—O3P	91.75 (7)	O3P—V1—O2P	82.17 (7)
O3—V1—O1	99.26 (9)	O1—V1—O2P	78.71 (7)
O1P—V1—O1	89.59 (7)	O2—V1—O2P	81.07 (7)
O3P—V1—O1	160.61 (8)	C1—O1—V1	112.73 (16)
O3—V1—O2	96.64 (9)	C2—O2—V1	112.22 (17)
O1P—V1—O2	164.10 (8)	O1—C1—C2	116.59 (15)
O3P—V1—O2	93.07 (7)	O2—C2—C1	116.60 (15)
O1—V1—O2	80.91 (7)

V1—O1—C1—C2	10.26 (13)	V1—O2—C2—C1	−2.03 (13)
V1—O2—C2—O2ⁱ	177.97 (13)	O1—C1—C2—O2	−5.76 (13)

Symmetry code: (i) −x, y, −z+1/2.

Acknowledgements

This work was supported by Illinois State University, the American Chemical Society Petroleum Research Fund (46064-B3) and the National Science Foundation (US, CHE-0645081). The authors also thank the STaRBURSTT Cyberdiffraction Consortium and Dr M. Zeller (Youngstown State University) for the collection of the X-ray intensity data.

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