Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804028910/nc6008sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804028910/nc6008Isup2.hkl |
CCDC reference: 258665
Data collection: P3 Software (Siemens, 1993); cell refinement: P3 Software; data reduction: XDISK in SHELXTL/PC (Sheldrick, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL/PC; software used to prepare material for publication: PLATON (Spek, 2003).
[WFe(C6H8P)2(CO)5] | F(000) = 1152 |
Mr = 601.93 | Dx = 2.009 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 48 reflections |
a = 13.279 (13) Å | θ = 3.6–14.0° |
b = 10.857 (9) Å | µ = 6.69 mm−1 |
c = 14.061 (12) Å | T = 293 K |
β = 101.02 (7)° | Prism, red |
V = 1990 (3) Å3 | 0.46 × 0.13 × 0.11 mm |
Z = 4 |
Siemens P3 diffractometer | 3802 reflections with I > 2σ(I) |
Radiation source: X-ray tube, FK60-10 Siemens Mo tube | Rint = 0.018 |
Graphite monochromator | θmax = 27.5°, θmin = 2.4° |
ω–2θ scans | h = −17→16 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→14 |
Tmin = 0.236, Tmax = 0.480 | l = 0→18 |
4752 measured reflections | 3 standard reflections every 100 reflections |
4567 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | H-atom parameters constrained |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + (0.0306P)2 + 1.1109P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
4567 reflections | Δρmax = 0.71 e Å−3 |
240 parameters | Δρmin = −0.67 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: 0.00038 (9) |
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 on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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. |
x | y | z | Uiso*/Ueq | ||
W | 0.344268 (12) | 0.337052 (14) | 0.272226 (11) | 0.03728 (6) | |
Fe | 0.19263 (4) | 0.64207 (4) | 0.08580 (3) | 0.02999 (11) | |
P1 | 0.25445 (7) | 0.53049 (9) | 0.21759 (7) | 0.0347 (2) | |
P11 | 0.15788 (11) | 0.49949 (12) | −0.03491 (8) | 0.0568 (3) | |
O1 | 0.4571 (3) | 0.0935 (3) | 0.3518 (3) | 0.0757 (11) | |
O2 | 0.2470 (4) | 0.3415 (4) | 0.4615 (3) | 0.0851 (13) | |
O3 | 0.1516 (3) | 0.1931 (4) | 0.1559 (3) | 0.0778 (11) | |
O4 | 0.4447 (4) | 0.3263 (4) | 0.0843 (3) | 0.0878 (13) | |
O5 | 0.5224 (3) | 0.5134 (3) | 0.3760 (3) | 0.0761 (11) | |
C2 | 0.1264 (3) | 0.5803 (4) | 0.1994 (3) | 0.0369 (8) | |
H2 | 0.0705 | 0.5277 | 0.1949 | 0.044* | |
C3 | 0.1185 (3) | 0.7101 (4) | 0.1922 (3) | 0.0394 (8) | |
C4 | 0.2157 (3) | 0.7684 (3) | 0.2008 (3) | 0.0384 (8) | |
C5 | 0.2964 (3) | 0.6824 (3) | 0.2131 (3) | 0.0365 (8) | |
H5 | 0.3650 | 0.7042 | 0.2182 | 0.044* | |
C6 | 0.0173 (4) | 0.7787 (5) | 0.1809 (4) | 0.0621 (13) | |
H61 | 0.0089 | 0.8100 | 0.2427 | 0.093* | |
H62 | −0.0381 | 0.7235 | 0.1563 | 0.093* | |
H63 | 0.0171 | 0.8458 | 0.1365 | 0.093* | |
C7 | 0.2320 (4) | 0.9059 (4) | 0.2021 (3) | 0.0597 (12) | |
H71 | 0.2365 | 0.9362 | 0.2670 | 0.090* | |
H72 | 0.1755 | 0.9447 | 0.1601 | 0.090* | |
H73 | 0.2945 | 0.9243 | 0.1802 | 0.090* | |
C12 | 0.0855 (3) | 0.6368 (4) | −0.0428 (3) | 0.0467 (10) | |
H12 | 0.0146 | 0.6375 | −0.0483 | 0.056* | |
C13 | 0.1444 (3) | 0.7451 (4) | −0.0400 (2) | 0.0412 (9) | |
C14 | 0.2510 (3) | 0.7186 (4) | −0.0280 (3) | 0.0395 (8) | |
C15 | 0.2695 (3) | 0.5910 (4) | −0.0228 (3) | 0.0487 (10) | |
H15 | 0.3351 | 0.5576 | −0.0138 | 0.058* | |
C16 | 0.0987 (4) | 0.8724 (4) | −0.0503 (3) | 0.0567 (12) | |
H161 | 0.0945 | 0.9006 | −0.1157 | 0.085* | |
H162 | 0.1412 | 0.9275 | −0.0066 | 0.085* | |
H163 | 0.0312 | 0.8703 | −0.0353 | 0.085* | |
C17 | 0.3340 (4) | 0.8132 (5) | −0.0216 (3) | 0.0580 (12) | |
H171 | 0.3431 | 0.8347 | −0.0857 | 0.087* | |
H172 | 0.3969 | 0.7804 | 0.0145 | 0.087* | |
H173 | 0.3151 | 0.8853 | 0.0104 | 0.087* | |
C21 | 0.4163 (3) | 0.1814 (4) | 0.3223 (3) | 0.0481 (10) | |
C22 | 0.2801 (4) | 0.3407 (4) | 0.3929 (4) | 0.0524 (11) | |
C23 | 0.2215 (4) | 0.2429 (4) | 0.1989 (4) | 0.0514 (10) | |
C24 | 0.4093 (3) | 0.3307 (4) | 0.1514 (4) | 0.0529 (11) | |
C25 | 0.4615 (3) | 0.4480 (4) | 0.3393 (3) | 0.0508 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
W | 0.04242 (9) | 0.03226 (9) | 0.03754 (9) | 0.00719 (7) | 0.00858 (6) | 0.00337 (7) |
Fe | 0.0355 (2) | 0.0312 (3) | 0.0241 (2) | −0.00114 (19) | 0.00751 (19) | 0.00059 (19) |
P1 | 0.0404 (5) | 0.0327 (5) | 0.0310 (5) | 0.0035 (4) | 0.0064 (4) | 0.0028 (4) |
P11 | 0.0859 (9) | 0.0447 (6) | 0.0403 (6) | −0.0149 (6) | 0.0137 (6) | −0.0108 (5) |
O1 | 0.085 (3) | 0.049 (2) | 0.092 (3) | 0.0261 (19) | 0.014 (2) | 0.011 (2) |
O2 | 0.117 (3) | 0.085 (3) | 0.068 (2) | 0.009 (2) | 0.054 (3) | 0.010 (2) |
O3 | 0.059 (2) | 0.069 (2) | 0.100 (3) | −0.0047 (18) | 0.002 (2) | −0.016 (2) |
O4 | 0.111 (3) | 0.087 (3) | 0.081 (3) | −0.003 (2) | 0.059 (3) | −0.010 (2) |
O5 | 0.061 (2) | 0.062 (2) | 0.095 (3) | −0.0034 (18) | −0.010 (2) | −0.005 (2) |
C2 | 0.0431 (19) | 0.041 (2) | 0.0294 (18) | −0.0001 (16) | 0.0128 (15) | 0.0053 (16) |
C3 | 0.047 (2) | 0.044 (2) | 0.0300 (18) | 0.0110 (17) | 0.0134 (16) | 0.0035 (17) |
C4 | 0.058 (2) | 0.0314 (19) | 0.0267 (18) | 0.0000 (16) | 0.0093 (16) | −0.0022 (15) |
C5 | 0.0389 (18) | 0.041 (2) | 0.0298 (17) | −0.0047 (15) | 0.0062 (14) | −0.0010 (16) |
C6 | 0.064 (3) | 0.067 (3) | 0.059 (3) | 0.030 (2) | 0.020 (2) | 0.003 (3) |
C7 | 0.100 (4) | 0.033 (2) | 0.048 (3) | −0.006 (2) | 0.019 (3) | −0.006 (2) |
C12 | 0.046 (2) | 0.058 (3) | 0.033 (2) | −0.0105 (19) | 0.0000 (16) | 0.0012 (18) |
C13 | 0.047 (2) | 0.052 (2) | 0.0225 (18) | −0.0026 (18) | 0.0017 (15) | 0.0058 (17) |
C14 | 0.044 (2) | 0.051 (2) | 0.0243 (17) | −0.0072 (17) | 0.0095 (15) | 0.0023 (16) |
C15 | 0.056 (2) | 0.059 (3) | 0.034 (2) | 0.008 (2) | 0.0191 (18) | −0.0039 (19) |
C16 | 0.069 (3) | 0.056 (3) | 0.043 (2) | 0.007 (2) | 0.006 (2) | 0.012 (2) |
C17 | 0.057 (3) | 0.073 (3) | 0.046 (2) | −0.018 (2) | 0.015 (2) | 0.005 (2) |
C21 | 0.052 (2) | 0.038 (2) | 0.054 (2) | 0.0073 (18) | 0.0092 (19) | 0.0001 (19) |
C22 | 0.060 (3) | 0.046 (2) | 0.053 (3) | 0.014 (2) | 0.016 (2) | 0.010 (2) |
C23 | 0.051 (2) | 0.043 (2) | 0.061 (3) | 0.006 (2) | 0.012 (2) | 0.000 (2) |
C24 | 0.052 (2) | 0.048 (3) | 0.062 (3) | 0.006 (2) | 0.019 (2) | −0.003 (2) |
C25 | 0.045 (2) | 0.048 (3) | 0.057 (3) | 0.012 (2) | 0.003 (2) | 0.008 (2) |
W—P1 | 2.464 (2) | C13—C14 | 1.422 (6) |
W—C21 | 2.002 (5) | C13—C16 | 1.506 (6) |
W—C22 | 2.040 (5) | C14—C15 | 1.406 (6) |
W—C23 | 2.031 (5) | C14—C17 | 1.496 (6) |
W—C24 | 2.048 (5) | C2—H2 | 0.93 |
W—C25 | 2.050 (5) | C5—H5 | 0.93 |
P1—C2 | 1.755 (4) | C6—H61 | 0.96 |
P1—C5 | 1.746 (4) | C6—H62 | 0.96 |
P11—C12 | 1.765 (5) | C6—H63 | 0.96 |
P11—C15 | 1.766 (5) | C7—H71 | 0.96 |
O1—C21 | 1.137 (5) | C7—H72 | 0.96 |
O2—C22 | 1.134 (6) | C7—H73 | 0.96 |
O3—C23 | 1.142 (6) | C12—H12 | 0.93 |
O4—C24 | 1.134 (6) | C15—H15 | 0.93 |
O5—C25 | 1.125 (5) | C16—H161 | 0.96 |
C2—C3 | 1.415 (6) | C16—H162 | 0.96 |
C3—C4 | 1.422 (6) | C16—H163 | 0.96 |
C3—C6 | 1.518 (6) | C17—H171 | 0.96 |
C4—C5 | 1.408 (5) | C17—H172 | 0.96 |
C4—C7 | 1.508 (6) | C17—H173 | 0.96 |
C12—C13 | 1.409 (5) | ||
P1···P11 | 3.553 (4) | ||
P1—W—C21 | 177.58 (13) | W—C22—O2 | 178.1 (5) |
P1—W—C22 | 89.34 (13) | W—C23—O3 | 177.9 (4) |
P1—W—C23 | 88.68 (14) | W—C24—O4 | 179.4 (5) |
P1—W—C24 | 91.48 (13) | W—C25—O5 | 176.6 (4) |
P1—W—C25 | 85.55 (14) | P1—C2—H2 | 124.0 |
C21—W—C22 | 88.36 (18) | C3—C2—H2 | 124.0 |
C21—W—C23 | 92.10 (19) | P1—C5—H5 | 123.5 |
C21—W—C24 | 90.82 (19) | C4—C5—H5 | 123.5 |
C21—W—C25 | 93.72 (18) | C3—C6—H61 | 109.5 |
C22—W—C23 | 90.6 (2) | C3—C6—H62 | 109.5 |
C22—W—C24 | 179.15 (17) | C3—C6—H63 | 109.5 |
C22—W—C25 | 90.4 (2) | H61—C6—H62 | 109.5 |
C23—W—C24 | 89.2 (2) | H61—C6—H63 | 110.5 |
C23—W—C25 | 174.12 (17) | H62—C6—H63 | 109.5 |
C24—W—C25 | 89.9 (2) | C4—C7—H71 | 109.5 |
W—P1—C2 | 134.87 (14) | C4—C7—H72 | 109.5 |
W—P1—C5 | 132.65 (14) | C4—C7—H73 | 109.5 |
C2—P1—C5 | 90.61 (19) | H71—C7—H72 | 109.5 |
C12—P11—C15 | 88.2 (2) | H71—C7—H73 | 109.5 |
P1—C2—C3 | 112.0 (3) | H72—C7—H73 | 109.5 |
C2—C3—C4 | 112.5 (3) | P11—C12—H12 | 122.9 |
C2—C3—C6 | 123.3 (3) | C13—C12—H12 | 122.9 |
C4—C3—C6 | 124.1 (4) | P11—C15—H15 | 122.8 |
C3—C4—C5 | 111.9 (3) | C14—C15—H15 | 122.8 |
C3—C4—C7 | 124.6 (4) | C13—C16—H161 | 109.5 |
C5—C4—C7 | 123.4 (4) | C13—C16—H162 | 109.5 |
P1—C5—C4 | 113.0 (3) | C13—C16—H163 | 109.5 |
P11—C12—C13 | 114.2 (3) | H161—C16—H162 | 109.5 |
C12—C13—C14 | 111.7 (4) | H161—C16—H163 | 109.5 |
C12—C13—C16 | 123.5 (4) | H162—C16—H163 | 109.5 |
C14—C13—C16 | 124.8 (4) | C14—C17—H171 | 109.5 |
C13—C14—C15 | 111.4 (4) | C14—C17—H172 | 109.5 |
C13—C14—C17 | 124.9 (4) | C14—C17—H173 | 109.5 |
C15—C14—C17 | 123.6 (4) | H171—C17—H172 | 109.5 |
P11—C15—C14 | 114.5 (3) | H171—C17—H173 | 109.5 |
W—C21—O1 | 179.2 (4) | H172—C17—H173 | 109.5 |