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The structure of the title compound, hexacarbonyl-1
3C,2
3C-[3(
5)-cyclopentadienyl]bis(
3-selenido)diiron(II)cobalt(II),[CoFe
2(
3-Se)
2(C
5H
5)(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.
Supporting information
CCDC reference: 150727
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 = 561.70 | 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) Å3 | Plate, black |
Z = 8 | 0.28 × 0.24 × 0.10 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1297 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed 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Absorption correction: ψ scan (modified CADDAT; unpublished) | k = 0→7 |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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.028 | H-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 reflections | Δρmax = 0.45 e Å−3 |
200 parameters | Δρmin = −0.39 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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) | | |
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