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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\overline 1 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100011033/qd0023sup1.cif
Contains datablocks II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100011033/qd0023IIsup2.hkl
Contains datablock II

CCDC reference: 150727

Computing details top

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 top
Crystal data top
[CoFe2Se2(C5H5)(CO)6]F(000) = 2128
Mr = 561.70Dx = 2.365 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
a = 34.992 (4) ÅCell parameters from 24 reflections
b = 6.6249 (6) Åθ = 9–14°
c = 14.651 (2) ŵ = 7.49 mm1
β = 111.751 (9)°T = 293 K
V = 3154.6 (6) Å3Plate, black
Z = 80.28 × 0.24 × 0.10 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1297 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.054
Graphite monochromatorθmax = 25.0°, θmin = 1.3°
ω scansh = 041
Absorption correction: ψ scan
(modified CADDAT; unpublished)
k = 07
Tmin = 0.141, Tmax = 0.473l = 1716
2811 measured reflections3 standard reflections every 60 min
2765 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.062 w = 1/[σ2(Fo2) + (0.0086P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.69(Δ/σ)max = 0.001
2765 reflectionsΔρmax = 0.45 e Å3
200 parametersΔρmin = 0.39 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00086 (2)
Special details top

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 (Å2) top
xyzUiso*/Ueq
Se10.36522 (2)0.46957 (13)0.26378 (7)0.0571 (3)
Se20.38477 (2)0.03782 (13)0.21130 (6)0.0536 (3)
Fe10.42834 (3)0.31257 (19)0.28455 (9)0.0547 (4)
Fe20.32176 (3)0.21218 (18)0.16993 (9)0.0535 (4)
Co10.37387 (3)0.16751 (16)0.34428 (8)0.0497 (3)
C1CP0.3942 (3)0.0546 (16)0.4470 (6)0.080 (3)
H1CP0.41110.16150.44500.080*
C2CP0.4074 (3)0.1320 (17)0.4925 (6)0.074 (3)
H2CP0.43450.17150.52610.074*
C3CP0.3720 (3)0.2488 (15)0.4781 (6)0.071 (3)
H3CP0.37140.38050.49950.071*
C4CP0.3383 (3)0.1309 (17)0.4259 (6)0.075 (3)
H4CP0.31100.17000.40780.075*
C5CP0.3514 (4)0.0521 (15)0.4053 (7)0.079 (3)
H5CP0.33460.15620.36970.079*
C110.4543 (3)0.5102 (14)0.3704 (7)0.066 (3)
O110.4704 (2)0.6341 (10)0.4234 (5)0.099 (3)
C120.4702 (3)0.1396 (13)0.3360 (7)0.065 (3)
O120.49759 (18)0.0334 (10)0.3689 (6)0.114 (3)
C130.4397 (3)0.3972 (14)0.1843 (8)0.072 (3)
O130.4477 (2)0.4501 (12)0.1198 (5)0.105 (3)
C210.2961 (3)0.0267 (15)0.1335 (7)0.068 (3)
O210.2804 (2)0.1784 (10)0.1096 (5)0.095 (2)
C220.3106 (3)0.3185 (14)0.0535 (6)0.063 (3)
O220.30208 (19)0.3936 (10)0.0225 (5)0.087 (2)
C230.2808 (3)0.3230 (14)0.1959 (6)0.069 (3)
O230.25415 (19)0.3949 (10)0.2146 (5)0.098 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Se10.0448 (6)0.0457 (6)0.0756 (6)0.0039 (5)0.0164 (5)0.0018 (5)
Se20.0463 (5)0.0540 (6)0.0605 (6)0.0049 (5)0.0197 (5)0.0054 (5)
Fe10.0399 (7)0.0547 (9)0.0666 (9)0.0028 (7)0.0165 (6)0.0060 (7)
Fe20.0403 (7)0.0562 (9)0.0591 (8)0.0017 (7)0.0129 (6)0.0025 (7)
Co10.0455 (7)0.0493 (7)0.0536 (7)0.0006 (6)0.0175 (6)0.0033 (6)
C1CP0.097 (9)0.070 (8)0.069 (7)0.027 (7)0.025 (7)0.008 (6)
C2CP0.061 (7)0.103 (9)0.049 (6)0.008 (7)0.010 (5)0.008 (6)
C3CP0.071 (7)0.081 (7)0.058 (6)0.006 (7)0.019 (6)0.014 (6)
C4CP0.063 (7)0.101 (9)0.065 (7)0.006 (7)0.029 (6)0.008 (7)
C5CP0.106 (10)0.057 (7)0.088 (8)0.014 (7)0.053 (8)0.004 (6)
C110.045 (6)0.068 (8)0.076 (7)0.012 (6)0.014 (5)0.013 (6)
O110.078 (5)0.091 (6)0.110 (6)0.016 (4)0.011 (5)0.034 (5)
C120.055 (6)0.055 (6)0.088 (7)0.014 (5)0.028 (6)0.001 (6)
O120.052 (4)0.087 (6)0.183 (8)0.024 (4)0.020 (5)0.046 (5)
C130.049 (6)0.070 (7)0.105 (9)0.012 (5)0.036 (6)0.019 (6)
O130.093 (5)0.126 (7)0.112 (6)0.024 (5)0.057 (5)0.034 (5)
C210.036 (5)0.079 (8)0.077 (7)0.015 (6)0.006 (5)0.007 (7)
O210.077 (5)0.075 (5)0.116 (6)0.024 (4)0.015 (4)0.008 (5)
C220.051 (6)0.075 (7)0.061 (6)0.007 (5)0.020 (5)0.002 (6)
O220.077 (5)0.091 (5)0.083 (5)0.006 (4)0.017 (4)0.005 (4)
C230.056 (6)0.057 (6)0.076 (7)0.007 (6)0.004 (5)0.009 (5)
O230.064 (5)0.108 (6)0.129 (6)0.020 (4)0.045 (5)0.001 (5)
Geometric parameters (Å, º) top
Se1—Fe12.3569 (14)Co1—C2CP2.064 (8)
Se1—Fe22.3583 (15)Co1—C3CP2.057 (8)
Se1—Co12.2853 (14)Co1—C4CP2.035 (8)
Se2—Fe12.3615 (15)Co1—C5CP2.014 (9)
Se2—Fe22.3605 (14)C1CP—C2CP1.399 (11)
Se2—Co12.2870 (13)C1CP—C5CP1.395 (11)
Fe1—Co12.5610 (16)C2CP—C3CP1.409 (11)
Fe1—C111.810 (10)C3CP—C4CP1.384 (11)
Fe1—C121.792 (9)C4CP—C5CP1.368 (11)
Fe1—C131.750 (10)C11—O111.127 (9)
Fe2—Co12.5467 (16)C12—O121.140 (9)
Fe2—C211.800 (10)C13—O131.135 (9)
Fe2—C221.751 (9)C21—O211.138 (10)
Fe2—C231.773 (9)C22—O221.153 (8)
Co1—C1CP2.035 (9)C23—O231.166 (9)
Fe1—Se1—Fe297.30 (5)C1CP—Co1—C3CP67.1 (4)
Co1—Se1—Fe166.94 (5)C1CP—Co1—C4CP66.5 (4)
Co1—Se1—Fe266.50 (5)C2CP—Co1—Se1123.9 (3)
Fe2—Se2—Fe197.11 (5)C2CP—Co1—Se2130.1 (3)
Co1—Se2—Fe166.84 (5)C2CP—Co1—Fe1101.4 (3)
Co1—Se2—Fe266.43 (5)C2CP—Co1—Fe2170.1 (3)
Se1—Fe1—Se282.25 (5)C3CP—Co1—Se1102.6 (3)
Se1—Fe1—Co155.19 (4)C3CP—Co1—Se2169.9 (3)
Se2—Fe1—Co155.19 (4)C3CP—Co1—Fe1121.2 (3)
C11—Fe1—Se188.6 (3)C3CP—Co1—Fe2131.4 (3)
C11—Fe1—Se2161.2 (3)C3CP—Co1—C2CP40.0 (3)
C11—Fe1—Co1106.2 (3)C4CP—Co1—Se1114.5 (3)
C12—Fe1—Se1156.6 (3)C4CP—Co1—Se2141.9 (3)
C12—Fe1—Se289.3 (3)C4CP—Co1—Fe1160.1 (3)
C12—Fe1—Co1102.3 (3)C4CP—Co1—Fe2103.7 (3)
C12—Fe1—C1192.8 (4)C4CP—Co1—C2CP66.5 (3)
C13—Fe1—Se1104.1 (3)C4CP—Co1—C3CP39.5 (3)
C13—Fe1—Se2100.1 (3)C5CP—Co1—Se1149.6 (3)
C13—Fe1—Co1146.8 (3)C5CP—Co1—Se2108.8 (3)
C13—Fe1—C1198.0 (4)C5CP—Co1—Fe1152.3 (3)
C13—Fe1—C1298.8 (4)C5CP—Co1—Fe2106.1 (3)
Se1—Fe2—Se282.24 (5)C5CP—Co1—C1CP40.3 (3)
Se1—Fe2—Co155.38 (4)C5CP—Co1—C2CP67.3 (4)
Se2—Fe2—Co155.40 (4)C5CP—Co1—C3CP67.1 (4)
C21—Fe2—Se1162.1 (3)C5CP—Co1—C4CP39.5 (3)
C21—Fe2—Se287.8 (3)C2CP—C1CP—Co171.2 (5)
C21—Fe2—Co1106.8 (3)C5CP—C1CP—Co169.0 (5)
C22—Fe2—Se198.1 (3)C5CP—C1CP—C2CP108.0 (9)
C22—Fe2—Se2107.2 (3)C1CP—C2CP—Co168.9 (5)
C22—Fe2—Co1147.4 (3)C1CP—C2CP—C3CP107.3 (9)
C22—Fe2—C2199.1 (4)C3CP—C2CP—Co169.7 (5)
C22—Fe2—C2397.9 (4)C2CP—C3CP—Co170.3 (5)
C23—Fe2—Se188.5 (3)C4CP—C3CP—Co169.4 (5)
C23—Fe2—Se2154.2 (3)C4CP—C3CP—C2CP107.1 (9)
C23—Fe2—Co199.7 (3)C3CP—C4CP—Co171.1 (5)
C23—Fe2—C2194.2 (4)C5CP—C4CP—Co169.4 (5)
Se1—Co1—Se285.49 (5)C5CP—C4CP—C3CP109.7 (9)
Se1—Co1—Fe157.86 (4)C1CP—C5CP—Co170.7 (6)
Se1—Co1—Fe258.12 (4)C4CP—C5CP—Co171.1 (5)
Se2—Co1—Fe157.97 (4)C4CP—C5CP—C1CP107.8 (10)
Se2—Co1—Fe258.17 (4)O11—C11—Fe1179.5 (10)
Fe2—Co1—Fe187.74 (5)O12—C12—Fe1178.3 (8)
C1CP—Co1—Se1163.3 (3)O13—C13—Fe1178.8 (9)
C1CP—Co1—Se2103.6 (3)O21—C21—Fe2178.8 (10)
C1CP—Co1—Fe1115.0 (3)O22—C22—Fe2177.1 (9)
C1CP—Co1—Fe2138.6 (3)O23—C23—Fe2178.9 (9)
C1CP—Co1—C2CP39.9 (3)
 

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