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In the title compound, [WFe(C6H8P)2(CO)5], the phospho­lyl rings in the diphosphaferrocene moiety are in a skew conformation. The intramolecular distance between the P atoms of 3.553 (4) Å indicates a secondary bonding interaction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804028910/nc6008sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804028910/nc6008Isup2.hkl
Contains datablock I

CCDC reference: 258665

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.026
  • wR factor = 0.059
  • Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT328_ALERT_2_B Check for Possibly Missing H on sp3? Phosphor .. P11
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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).

Pentacarbonyl(3,3',4,4'-tetramethyl-1,1'-diphosphaferrocene-κP)tungsten(0) top
Crystal data top
[WFe(C6H8P)2(CO)5]F(000) = 1152
Mr = 601.93Dx = 2.009 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 48 reflections
a = 13.279 (13) Åθ = 3.6–14.0°
b = 10.857 (9) ŵ = 6.69 mm1
c = 14.061 (12) ÅT = 293 K
β = 101.02 (7)°Prism, red
V = 1990 (3) Å30.46 × 0.13 × 0.11 mm
Z = 4
Data collection top
Siemens P3
diffractometer
3802 reflections with I > 2σ(I)
Radiation source: X-ray tube, FK60-10 Siemens Mo tubeRint = 0.018
Graphite monochromatorθmax = 27.5°, θmin = 2.4°
ω–2θ scansh = 1716
Absorption correction: ψ scan
(North et al., 1968)
k = 014
Tmin = 0.236, Tmax = 0.480l = 018
4752 measured reflections3 standard reflections every 100 reflections
4567 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: structure-invariant direct methods
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026H-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 reflectionsΔρmax = 0.71 e Å3
240 parametersΔρmin = 0.67 e Å3
0 restraintsExtinction correction: SHELXL97, FC*=KFC[1+0.001XFC2Λ3/SIN(2Θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00038 (9)
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 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
W0.344268 (12)0.337052 (14)0.272226 (11)0.03728 (6)
Fe0.19263 (4)0.64207 (4)0.08580 (3)0.02999 (11)
P10.25445 (7)0.53049 (9)0.21759 (7)0.0347 (2)
P110.15788 (11)0.49949 (12)0.03491 (8)0.0568 (3)
O10.4571 (3)0.0935 (3)0.3518 (3)0.0757 (11)
O20.2470 (4)0.3415 (4)0.4615 (3)0.0851 (13)
O30.1516 (3)0.1931 (4)0.1559 (3)0.0778 (11)
O40.4447 (4)0.3263 (4)0.0843 (3)0.0878 (13)
O50.5224 (3)0.5134 (3)0.3760 (3)0.0761 (11)
C20.1264 (3)0.5803 (4)0.1994 (3)0.0369 (8)
H20.07050.52770.19490.044*
C30.1185 (3)0.7101 (4)0.1922 (3)0.0394 (8)
C40.2157 (3)0.7684 (3)0.2008 (3)0.0384 (8)
C50.2964 (3)0.6824 (3)0.2131 (3)0.0365 (8)
H50.36500.70420.21820.044*
C60.0173 (4)0.7787 (5)0.1809 (4)0.0621 (13)
H610.00890.81000.24270.093*
H620.03810.72350.15630.093*
H630.01710.84580.13650.093*
C70.2320 (4)0.9059 (4)0.2021 (3)0.0597 (12)
H710.23650.93620.26700.090*
H720.17550.94470.16010.090*
H730.29450.92430.18020.090*
C120.0855 (3)0.6368 (4)0.0428 (3)0.0467 (10)
H120.01460.63750.04830.056*
C130.1444 (3)0.7451 (4)0.0400 (2)0.0412 (9)
C140.2510 (3)0.7186 (4)0.0280 (3)0.0395 (8)
C150.2695 (3)0.5910 (4)0.0228 (3)0.0487 (10)
H150.33510.55760.01380.058*
C160.0987 (4)0.8724 (4)0.0503 (3)0.0567 (12)
H1610.09450.90060.11570.085*
H1620.14120.92750.00660.085*
H1630.03120.87030.03530.085*
C170.3340 (4)0.8132 (5)0.0216 (3)0.0580 (12)
H1710.34310.83470.08570.087*
H1720.39690.78040.01450.087*
H1730.31510.88530.01040.087*
C210.4163 (3)0.1814 (4)0.3223 (3)0.0481 (10)
C220.2801 (4)0.3407 (4)0.3929 (4)0.0524 (11)
C230.2215 (4)0.2429 (4)0.1989 (4)0.0514 (10)
C240.4093 (3)0.3307 (4)0.1514 (4)0.0529 (11)
C250.4615 (3)0.4480 (4)0.3393 (3)0.0508 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W0.04242 (9)0.03226 (9)0.03754 (9)0.00719 (7)0.00858 (6)0.00337 (7)
Fe0.0355 (2)0.0312 (3)0.0241 (2)0.00114 (19)0.00751 (19)0.00059 (19)
P10.0404 (5)0.0327 (5)0.0310 (5)0.0035 (4)0.0064 (4)0.0028 (4)
P110.0859 (9)0.0447 (6)0.0403 (6)0.0149 (6)0.0137 (6)0.0108 (5)
O10.085 (3)0.049 (2)0.092 (3)0.0261 (19)0.014 (2)0.011 (2)
O20.117 (3)0.085 (3)0.068 (2)0.009 (2)0.054 (3)0.010 (2)
O30.059 (2)0.069 (2)0.100 (3)0.0047 (18)0.002 (2)0.016 (2)
O40.111 (3)0.087 (3)0.081 (3)0.003 (2)0.059 (3)0.010 (2)
O50.061 (2)0.062 (2)0.095 (3)0.0034 (18)0.010 (2)0.005 (2)
C20.0431 (19)0.041 (2)0.0294 (18)0.0001 (16)0.0128 (15)0.0053 (16)
C30.047 (2)0.044 (2)0.0300 (18)0.0110 (17)0.0134 (16)0.0035 (17)
C40.058 (2)0.0314 (19)0.0267 (18)0.0000 (16)0.0093 (16)0.0022 (15)
C50.0389 (18)0.041 (2)0.0298 (17)0.0047 (15)0.0062 (14)0.0010 (16)
C60.064 (3)0.067 (3)0.059 (3)0.030 (2)0.020 (2)0.003 (3)
C70.100 (4)0.033 (2)0.048 (3)0.006 (2)0.019 (3)0.006 (2)
C120.046 (2)0.058 (3)0.033 (2)0.0105 (19)0.0000 (16)0.0012 (18)
C130.047 (2)0.052 (2)0.0225 (18)0.0026 (18)0.0017 (15)0.0058 (17)
C140.044 (2)0.051 (2)0.0243 (17)0.0072 (17)0.0095 (15)0.0023 (16)
C150.056 (2)0.059 (3)0.034 (2)0.008 (2)0.0191 (18)0.0039 (19)
C160.069 (3)0.056 (3)0.043 (2)0.007 (2)0.006 (2)0.012 (2)
C170.057 (3)0.073 (3)0.046 (2)0.018 (2)0.015 (2)0.005 (2)
C210.052 (2)0.038 (2)0.054 (2)0.0073 (18)0.0092 (19)0.0001 (19)
C220.060 (3)0.046 (2)0.053 (3)0.014 (2)0.016 (2)0.010 (2)
C230.051 (2)0.043 (2)0.061 (3)0.006 (2)0.012 (2)0.000 (2)
C240.052 (2)0.048 (3)0.062 (3)0.006 (2)0.019 (2)0.003 (2)
C250.045 (2)0.048 (3)0.057 (3)0.012 (2)0.003 (2)0.008 (2)
Geometric parameters (Å, º) top
W—P12.464 (2)C13—C141.422 (6)
W—C212.002 (5)C13—C161.506 (6)
W—C222.040 (5)C14—C151.406 (6)
W—C232.031 (5)C14—C171.496 (6)
W—C242.048 (5)C2—H20.93
W—C252.050 (5)C5—H50.93
P1—C21.755 (4)C6—H610.96
P1—C51.746 (4)C6—H620.96
P11—C121.765 (5)C6—H630.96
P11—C151.766 (5)C7—H710.96
O1—C211.137 (5)C7—H720.96
O2—C221.134 (6)C7—H730.96
O3—C231.142 (6)C12—H120.93
O4—C241.134 (6)C15—H150.93
O5—C251.125 (5)C16—H1610.96
C2—C31.415 (6)C16—H1620.96
C3—C41.422 (6)C16—H1630.96
C3—C61.518 (6)C17—H1710.96
C4—C51.408 (5)C17—H1720.96
C4—C71.508 (6)C17—H1730.96
C12—C131.409 (5)
P1···P113.553 (4)
P1—W—C21177.58 (13)W—C22—O2178.1 (5)
P1—W—C2289.34 (13)W—C23—O3177.9 (4)
P1—W—C2388.68 (14)W—C24—O4179.4 (5)
P1—W—C2491.48 (13)W—C25—O5176.6 (4)
P1—W—C2585.55 (14)P1—C2—H2124.0
C21—W—C2288.36 (18)C3—C2—H2124.0
C21—W—C2392.10 (19)P1—C5—H5123.5
C21—W—C2490.82 (19)C4—C5—H5123.5
C21—W—C2593.72 (18)C3—C6—H61109.5
C22—W—C2390.6 (2)C3—C6—H62109.5
C22—W—C24179.15 (17)C3—C6—H63109.5
C22—W—C2590.4 (2)H61—C6—H62109.5
C23—W—C2489.2 (2)H61—C6—H63110.5
C23—W—C25174.12 (17)H62—C6—H63109.5
C24—W—C2589.9 (2)C4—C7—H71109.5
W—P1—C2134.87 (14)C4—C7—H72109.5
W—P1—C5132.65 (14)C4—C7—H73109.5
C2—P1—C590.61 (19)H71—C7—H72109.5
C12—P11—C1588.2 (2)H71—C7—H73109.5
P1—C2—C3112.0 (3)H72—C7—H73109.5
C2—C3—C4112.5 (3)P11—C12—H12122.9
C2—C3—C6123.3 (3)C13—C12—H12122.9
C4—C3—C6124.1 (4)P11—C15—H15122.8
C3—C4—C5111.9 (3)C14—C15—H15122.8
C3—C4—C7124.6 (4)C13—C16—H161109.5
C5—C4—C7123.4 (4)C13—C16—H162109.5
P1—C5—C4113.0 (3)C13—C16—H163109.5
P11—C12—C13114.2 (3)H161—C16—H162109.5
C12—C13—C14111.7 (4)H161—C16—H163109.5
C12—C13—C16123.5 (4)H162—C16—H163109.5
C14—C13—C16124.8 (4)C14—C17—H171109.5
C13—C14—C15111.4 (4)C14—C17—H172109.5
C13—C14—C17124.9 (4)C14—C17—H173109.5
C15—C14—C17123.6 (4)H171—C17—H172109.5
P11—C15—C14114.5 (3)H171—C17—H173109.5
W—C21—O1179.2 (4)H172—C17—H173109.5
 

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