Redetermination of hexa­carbonyl­([eta]⁵-cyclo­penta­dienyl)­bis([mu]₃-selenido)­diiron(II)­cobalt(II)

The structure of the title compound, hexa­carbonyl-1[kappa]³C,2[kappa]³C-[3([eta]⁵)-cyclo­penta­dienyl]­bis([mu]₃-selenido)­diiron(II)­cobalt(II),[CoFe₂([mu]₃-Se)₂(C₅H₅)(CO)₆], was redetermined at room temperature and the correct C2/c space group was assumed instead of the previously reported P space group [Mathur et al. (1995). Organometallics, 14, 2115-2118]. Analysis of the literature data showed that the previously reported triclinic parameters correspond to a primitive subcell of the actual monoclinic C-centred cell with cell dimensions close to those found by us. The title compound appeared to be isostructural with the sulfur-selenium analogue.

Computing details

Data collection: CD4CA0 in CAD-4 User's Manual (Enraf-Nonius, 1985); cell refinement: CD4CA0; data reduction: XCAD (local program); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Bis(µ3-seleno)(η⁵-cyclopentadienyl)hexacarbonyldiironcobalt

Crystal data

[CoFe2Se2(C5H5)(CO)6]	F(000) = 2128
Mr = 561.70	Dx = 2.365 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
a = 34.992 (4) Å	Cell parameters from 24 reflections
b = 6.6249 (6) Å	θ = 9–14°
c = 14.651 (2) Å	µ = 7.49 mm^−1
β = 111.751 (9)°	T = 293 K
V = 3154.6 (6) Å^3	Plate, black
Z = 8	0.28 × 0.24 × 0.10 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	1297 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.054
Graphite monochromator	θmax = 25.0°, θmin = 1.3°
ω scans	h = 0→41
Absorption correction: ψ scan (modified CADDAT; unpublished)	k = 0→7
Tmin = 0.141, Tmax = 0.473	l = −17→16
2811 measured reflections	3 standard reflections every 60 min
2765 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.028	H-atom parameters constrained
wR(F^2) = 0.062	w = 1/[σ^2(Fo^2) + (0.0086P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.69	(Δ/σ)max = 0.001
2765 reflections	Δρmax = 0.45 e Å^−3
200 parameters	Δρmin = −0.39 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00086 (2)

Special details

Experimental. none

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R- factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Se1	0.36522 (2)	0.46957 (13)	0.26378 (7)	0.0571 (3)
Se2	0.38477 (2)	0.03782 (13)	0.21130 (6)	0.0536 (3)
Fe1	0.42834 (3)	0.31257 (19)	0.28455 (9)	0.0547 (4)
Fe2	0.32176 (3)	0.21218 (18)	0.16993 (9)	0.0535 (4)
Co1	0.37387 (3)	0.16751 (16)	0.34428 (8)	0.0497 (3)
C1CP	0.3942 (3)	−0.0546 (16)	0.4470 (6)	0.080 (3)
H1CP	0.4111	−0.1615	0.4450	0.080*
C2CP	0.4074 (3)	0.1320 (17)	0.4925 (6)	0.074 (3)
H2CP	0.4345	0.1715	0.5261	0.074*
C3CP	0.3720 (3)	0.2488 (15)	0.4781 (6)	0.071 (3)
H3CP	0.3714	0.3805	0.4995	0.071*
C4CP	0.3383 (3)	0.1309 (17)	0.4259 (6)	0.075 (3)
H4CP	0.3110	0.1700	0.4078	0.075*
C5CP	0.3514 (4)	−0.0521 (15)	0.4053 (7)	0.079 (3)
H5CP	0.3346	−0.1562	0.3697	0.079*
C11	0.4543 (3)	0.5102 (14)	0.3704 (7)	0.066 (3)
O11	0.4704 (2)	0.6341 (10)	0.4234 (5)	0.099 (3)
C12	0.4702 (3)	0.1396 (13)	0.3360 (7)	0.065 (3)
O12	0.49759 (18)	0.0334 (10)	0.3689 (6)	0.114 (3)
C13	0.4397 (3)	0.3972 (14)	0.1843 (8)	0.072 (3)
O13	0.4477 (2)	0.4501 (12)	0.1198 (5)	0.105 (3)
C21	0.2961 (3)	−0.0267 (15)	0.1335 (7)	0.068 (3)
O21	0.2804 (2)	−0.1784 (10)	0.1096 (5)	0.095 (2)
C22	0.3106 (3)	0.3185 (14)	0.0535 (6)	0.063 (3)
O22	0.30208 (19)	0.3936 (10)	−0.0225 (5)	0.087 (2)
C23	0.2808 (3)	0.3230 (14)	0.1959 (6)	0.069 (3)
O23	0.25415 (19)	0.3949 (10)	0.2146 (5)	0.098 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.0448 (6)	0.0457 (6)	0.0756 (6)	0.0039 (5)	0.0164 (5)	−0.0018 (5)
Se2	0.0463 (5)	0.0540 (6)	0.0605 (6)	0.0049 (5)	0.0197 (5)	−0.0054 (5)
Fe1	0.0399 (7)	0.0547 (9)	0.0666 (9)	0.0028 (7)	0.0165 (6)	0.0060 (7)
Fe2	0.0403 (7)	0.0562 (9)	0.0591 (8)	0.0017 (7)	0.0129 (6)	−0.0025 (7)
Co1	0.0455 (7)	0.0493 (7)	0.0536 (7)	0.0006 (6)	0.0175 (6)	−0.0033 (6)
C1CP	0.097 (9)	0.070 (8)	0.069 (7)	0.027 (7)	0.025 (7)	0.008 (6)
C2CP	0.061 (7)	0.103 (9)	0.049 (6)	0.008 (7)	0.010 (5)	0.008 (6)
C3CP	0.071 (7)	0.081 (7)	0.058 (6)	0.006 (7)	0.019 (6)	−0.014 (6)
C4CP	0.063 (7)	0.101 (9)	0.065 (7)	0.006 (7)	0.029 (6)	0.008 (7)
C5CP	0.106 (10)	0.057 (7)	0.088 (8)	−0.014 (7)	0.053 (8)	−0.004 (6)
C11	0.045 (6)	0.068 (8)	0.076 (7)	0.012 (6)	0.014 (5)	0.013 (6)
O11	0.078 (5)	0.091 (6)	0.110 (6)	−0.016 (4)	0.011 (5)	−0.034 (5)
C12	0.055 (6)	0.055 (6)	0.088 (7)	−0.014 (5)	0.028 (6)	0.001 (6)
O12	0.052 (4)	0.087 (6)	0.183 (8)	0.024 (4)	0.020 (5)	0.046 (5)
C13	0.049 (6)	0.070 (7)	0.105 (9)	0.012 (5)	0.036 (6)	0.019 (6)
O13	0.093 (5)	0.126 (7)	0.112 (6)	0.024 (5)	0.057 (5)	0.034 (5)
C21	0.036 (5)	0.079 (8)	0.077 (7)	0.015 (6)	0.006 (5)	0.007 (7)
O21	0.077 (5)	0.075 (5)	0.116 (6)	−0.024 (4)	0.015 (4)	−0.008 (5)
C22	0.051 (6)	0.075 (7)	0.061 (6)	0.007 (5)	0.020 (5)	0.002 (6)
O22	0.077 (5)	0.091 (5)	0.083 (5)	0.006 (4)	0.017 (4)	0.005 (4)
C23	0.056 (6)	0.057 (6)	0.076 (7)	−0.007 (6)	0.004 (5)	−0.009 (5)
O23	0.064 (5)	0.108 (6)	0.129 (6)	0.020 (4)	0.045 (5)	−0.001 (5)

Geometric parameters (Å, º)

Se1—Fe1	2.3569 (14)	Co1—C2CP	2.064 (8)
Se1—Fe2	2.3583 (15)	Co1—C3CP	2.057 (8)
Se1—Co1	2.2853 (14)	Co1—C4CP	2.035 (8)
Se2—Fe1	2.3615 (15)	Co1—C5CP	2.014 (9)
Se2—Fe2	2.3605 (14)	C1CP—C2CP	1.399 (11)
Se2—Co1	2.2870 (13)	C1CP—C5CP	1.395 (11)
Fe1—Co1	2.5610 (16)	C2CP—C3CP	1.409 (11)
Fe1—C11	1.810 (10)	C3CP—C4CP	1.384 (11)
Fe1—C12	1.792 (9)	C4CP—C5CP	1.368 (11)
Fe1—C13	1.750 (10)	C11—O11	1.127 (9)
Fe2—Co1	2.5467 (16)	C12—O12	1.140 (9)
Fe2—C21	1.800 (10)	C13—O13	1.135 (9)
Fe2—C22	1.751 (9)	C21—O21	1.138 (10)
Fe2—C23	1.773 (9)	C22—O22	1.153 (8)
Co1—C1CP	2.035 (9)	C23—O23	1.166 (9)
Fe1—Se1—Fe2	97.30 (5)	C1CP—Co1—C3CP	67.1 (4)
Co1—Se1—Fe1	66.94 (5)	C1CP—Co1—C4CP	66.5 (4)
Co1—Se1—Fe2	66.50 (5)	C2CP—Co1—Se1	123.9 (3)
Fe2—Se2—Fe1	97.11 (5)	C2CP—Co1—Se2	130.1 (3)
Co1—Se2—Fe1	66.84 (5)	C2CP—Co1—Fe1	101.4 (3)
Co1—Se2—Fe2	66.43 (5)	C2CP—Co1—Fe2	170.1 (3)
Se1—Fe1—Se2	82.25 (5)	C3CP—Co1—Se1	102.6 (3)
Se1—Fe1—Co1	55.19 (4)	C3CP—Co1—Se2	169.9 (3)
Se2—Fe1—Co1	55.19 (4)	C3CP—Co1—Fe1	121.2 (3)
C11—Fe1—Se1	88.6 (3)	C3CP—Co1—Fe2	131.4 (3)
C11—Fe1—Se2	161.2 (3)	C3CP—Co1—C2CP	40.0 (3)
C11—Fe1—Co1	106.2 (3)	C4CP—Co1—Se1	114.5 (3)
C12—Fe1—Se1	156.6 (3)	C4CP—Co1—Se2	141.9 (3)
C12—Fe1—Se2	89.3 (3)	C4CP—Co1—Fe1	160.1 (3)
C12—Fe1—Co1	102.3 (3)	C4CP—Co1—Fe2	103.7 (3)
C12—Fe1—C11	92.8 (4)	C4CP—Co1—C2CP	66.5 (3)
C13—Fe1—Se1	104.1 (3)	C4CP—Co1—C3CP	39.5 (3)
C13—Fe1—Se2	100.1 (3)	C5CP—Co1—Se1	149.6 (3)
C13—Fe1—Co1	146.8 (3)	C5CP—Co1—Se2	108.8 (3)
C13—Fe1—C11	98.0 (4)	C5CP—Co1—Fe1	152.3 (3)
C13—Fe1—C12	98.8 (4)	C5CP—Co1—Fe2	106.1 (3)
Se1—Fe2—Se2	82.24 (5)	C5CP—Co1—C1CP	40.3 (3)
Se1—Fe2—Co1	55.38 (4)	C5CP—Co1—C2CP	67.3 (4)
Se2—Fe2—Co1	55.40 (4)	C5CP—Co1—C3CP	67.1 (4)
C21—Fe2—Se1	162.1 (3)	C5CP—Co1—C4CP	39.5 (3)
C21—Fe2—Se2	87.8 (3)	C2CP—C1CP—Co1	71.2 (5)
C21—Fe2—Co1	106.8 (3)	C5CP—C1CP—Co1	69.0 (5)
C22—Fe2—Se1	98.1 (3)	C5CP—C1CP—C2CP	108.0 (9)
C22—Fe2—Se2	107.2 (3)	C1CP—C2CP—Co1	68.9 (5)
C22—Fe2—Co1	147.4 (3)	C1CP—C2CP—C3CP	107.3 (9)
C22—Fe2—C21	99.1 (4)	C3CP—C2CP—Co1	69.7 (5)
C22—Fe2—C23	97.9 (4)	C2CP—C3CP—Co1	70.3 (5)
C23—Fe2—Se1	88.5 (3)	C4CP—C3CP—Co1	69.4 (5)
C23—Fe2—Se2	154.2 (3)	C4CP—C3CP—C2CP	107.1 (9)
C23—Fe2—Co1	99.7 (3)	C3CP—C4CP—Co1	71.1 (5)
C23—Fe2—C21	94.2 (4)	C5CP—C4CP—Co1	69.4 (5)
Se1—Co1—Se2	85.49 (5)	C5CP—C4CP—C3CP	109.7 (9)
Se1—Co1—Fe1	57.86 (4)	C1CP—C5CP—Co1	70.7 (6)
Se1—Co1—Fe2	58.12 (4)	C4CP—C5CP—Co1	71.1 (5)
Se2—Co1—Fe1	57.97 (4)	C4CP—C5CP—C1CP	107.8 (10)
Se2—Co1—Fe2	58.17 (4)	O11—C11—Fe1	179.5 (10)
Fe2—Co1—Fe1	87.74 (5)	O12—C12—Fe1	178.3 (8)
C1CP—Co1—Se1	163.3 (3)	O13—C13—Fe1	178.8 (9)
C1CP—Co1—Se2	103.6 (3)	O21—C21—Fe2	178.8 (10)
C1CP—Co1—Fe1	115.0 (3)	O22—C22—Fe2	177.1 (9)
C1CP—Co1—Fe2	138.6 (3)	O23—C23—Fe2	178.9 (9)
C1CP—Co1—C2CP	39.9 (3)