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Crystals of Hg[Fe(CO)2(η5–C5H5)]2 contain discrete molecules with crystallographically imposed twofold symmetry, Hg—Fe 2.5546 (10) Å and an Fe—Hg—Fe angle of 156.34 (6)°, the most acute yet found for a simple Hg[MLn]2 species.
Supporting information
CCDC reference: 180759
Key indicators
- Single-crystal X-ray study
- T = 203 K
- Mean (C-C) = 0.014 Å
- R factor = 0.037
- wR factor = 0.100
- Data-to-parameter ratio = 17.8
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level A:
ABSTM_02 Alert A Crystal and compound unsuitable for non-numerical
corrections. Product of mu and tmid > 3.0
Value of mu given = 12.705 tmid = 0.480
| Author response: Absorption correction with SADABS appeared to give a satisfactory
correction.
|
General Notes
REFLT_03
From the CIF: _diffrn_reflns_theta_max 28.30
From the CIF: _reflns_number_total 1726
Count of symmetry unique reflns 1070
Completeness (_total/calc) 161.31%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 656
Fraction of Friedel pairs measured 0.613
Are heavy atom types Z>Si present yes
Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check
Data collection: SMART (Siemens, 1994); cell refinement: SAINT (Siemens, 1994); data reduction: SADABS (Blessing, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Bis[cyclopentadienyl(dicarbonyl)iron]mercury(II)
top
Crystal data top
[HgFe2(C5H5)2(CO)4] | Dx = 2.572 Mg m−3 |
Mr = 554.51 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P43212 | Cell parameters from 1726 reflections |
a = 11.6756 (1) Å | θ = 2–28° |
c = 10.5030 (1) Å | µ = 12.71 mm−1 |
V = 1431.77 (2) Å3 | T = 203 K |
Z = 4 | Prism, brown |
F(000) = 1032 | 0.58 × 0.48 × 0.36 mm |
Data collection top
Siemens SMART CCD diffractometer | 1726 independent reflections |
Radiation source: fine-focus sealed tube | 1687 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
multi–scan | θmax = 28.3°, θmin = 2.5° |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995) | h = −15→15 |
Tmin = 0.003, Tmax = 0.011 | k = 0→15 |
3323 measured reflections | l = 0→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.100 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.034P)2 + 16.5365P] where P = (Fo2 + 2Fc2)/3 |
1726 reflections | (Δ/σ)max < 0.001 |
97 parameters | Δρmax = 1.72 e Å−3 |
0 restraints | Δρmin = −2.49 e Å−3 |
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 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 | |
Hg1 | 0.24290 (2) | 0.24290 (2) | 0.0000 | 0.02149 (14) | |
Fe1 | 0.28631 (9) | 0.26284 (8) | 0.23736 (10) | 0.0163 (2) | |
O1 | 0.0939 (6) | 0.1212 (7) | 0.3137 (7) | 0.0350 (18) | |
O2 | 0.1532 (7) | 0.4720 (6) | 0.2192 (8) | 0.0394 (18) | |
C1 | 0.1683 (7) | 0.1758 (8) | 0.2800 (7) | 0.0224 (16) | |
C2 | 0.2057 (8) | 0.3893 (7) | 0.2223 (8) | 0.0227 (17) | |
C11 | 0.4212 (8) | 0.3354 (8) | 0.3394 (9) | 0.0252 (19) | |
H11 | 0.4171 | 0.4043 | 0.3855 | 0.030* | |
C12 | 0.4516 (9) | 0.3252 (9) | 0.2082 (9) | 0.028 (2) | |
H12 | 0.4692 | 0.3858 | 0.1526 | 0.033* | |
C13 | 0.4505 (8) | 0.2069 (10) | 0.1772 (10) | 0.029 (2) | |
H13 | 0.4691 | 0.1743 | 0.0981 | 0.035* | |
C14 | 0.4158 (8) | 0.1469 (9) | 0.2888 (8) | 0.026 (2) | |
H14 | 0.4061 | 0.0672 | 0.2954 | 0.031* | |
C15 | 0.3984 (8) | 0.2269 (9) | 0.3880 (8) | 0.0263 (19) | |
H15 | 0.3756 | 0.2098 | 0.4717 | 0.032* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hg1 | 0.02664 (17) | 0.02664 (17) | 0.0112 (2) | 0.00052 (16) | −0.00007 (10) | 0.00007 (10) |
Fe1 | 0.0168 (5) | 0.0190 (5) | 0.0132 (5) | −0.0003 (4) | −0.0001 (4) | −0.0013 (4) |
O1 | 0.033 (4) | 0.041 (5) | 0.031 (4) | −0.010 (3) | 0.008 (3) | 0.005 (3) |
O2 | 0.041 (4) | 0.032 (4) | 0.045 (5) | 0.012 (3) | −0.001 (3) | −0.003 (3) |
C1 | 0.023 (4) | 0.028 (4) | 0.016 (4) | 0.000 (3) | −0.002 (3) | 0.005 (3) |
C2 | 0.028 (4) | 0.021 (4) | 0.019 (4) | −0.001 (3) | −0.002 (3) | −0.004 (3) |
C11 | 0.025 (5) | 0.029 (5) | 0.022 (4) | −0.001 (4) | −0.006 (4) | −0.007 (4) |
C12 | 0.023 (4) | 0.034 (5) | 0.027 (5) | −0.006 (4) | 0.001 (4) | 0.000 (4) |
C13 | 0.015 (4) | 0.042 (6) | 0.030 (5) | 0.005 (4) | 0.006 (3) | 0.002 (4) |
C14 | 0.026 (4) | 0.031 (5) | 0.021 (4) | 0.007 (4) | −0.007 (3) | 0.000 (3) |
C15 | 0.027 (4) | 0.037 (5) | 0.015 (4) | 0.004 (4) | −0.008 (3) | 0.000 (4) |
Geometric parameters (Å, º) top
Hg1—Fe1 | 2.5546 (10) | Fe1—C13 | 2.121 (9) |
Hg1—Fe1i | 2.5546 (10) | O1—C1 | 1.135 (10) |
Fe1—C2 | 1.758 (9) | O2—C2 | 1.144 (11) |
Fe1—C1 | 1.769 (8) | C11—C15 | 1.391 (14) |
Fe1—C12 | 2.085 (10) | C11—C12 | 1.428 (13) |
Fe1—C11 | 2.085 (9) | C12—C13 | 1.419 (15) |
Fe1—C15 | 2.096 (8) | C13—C14 | 1.424 (14) |
Fe1—C14 | 2.100 (9) | C14—C15 | 1.413 (13) |
| | | |
Fe1—Hg1—Fe1i | 156.37 (5) | C1—Fe1—Hg1 | 92.3 (3) |
C2—Fe1—C1 | 95.0 (4) | C12—Fe1—Hg1 | 94.1 (3) |
C2—Fe1—C12 | 100.9 (4) | C11—Fe1—Hg1 | 133.5 (3) |
C1—Fe1—C12 | 163.4 (4) | C15—Fe1—Hg1 | 147.4 (3) |
C2—Fe1—C11 | 96.3 (4) | C14—Fe1—Hg1 | 109.6 (3) |
C1—Fe1—C11 | 133.7 (4) | C13—Fe1—Hg1 | 82.0 (3) |
C12—Fe1—C11 | 40.0 (4) | O1—C1—Fe1 | 176.5 (8) |
C2—Fe1—C15 | 124.8 (4) | O2—C2—Fe1 | 176.5 (8) |
C1—Fe1—C15 | 100.4 (4) | C15—C11—C12 | 109.0 (9) |
C12—Fe1—C15 | 66.6 (4) | C15—C11—Fe1 | 71.0 (5) |
C11—Fe1—C15 | 38.9 (4) | C12—C11—Fe1 | 70.0 (6) |
C2—Fe1—C14 | 161.8 (4) | C13—C12—C11 | 107.5 (9) |
C1—Fe1—C14 | 97.2 (4) | C13—C12—Fe1 | 71.7 (6) |
C12—Fe1—C14 | 66.2 (4) | C11—C12—Fe1 | 69.9 (6) |
C11—Fe1—C14 | 65.5 (4) | C12—C13—C14 | 107.0 (9) |
C15—Fe1—C14 | 39.4 (4) | C12—C13—Fe1 | 68.9 (6) |
C2—Fe1—C13 | 135.7 (4) | C14—C13—Fe1 | 69.5 (5) |
C1—Fe1—C13 | 127.0 (4) | C15—C14—C13 | 108.8 (9) |
C12—Fe1—C13 | 39.4 (4) | C15—C14—Fe1 | 70.2 (5) |
C11—Fe1—C13 | 66.1 (4) | C13—C14—Fe1 | 71.1 (6) |
C15—Fe1—C13 | 66.3 (4) | C11—C15—C14 | 107.7 (8) |
C14—Fe1—C13 | 39.4 (4) | C11—C15—Fe1 | 70.1 (5) |
C2—Fe1—Hg1 | 83.3 (3) | C14—C15—Fe1 | 70.5 (5) |
Symmetry code: (i) y, x, −z. |
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