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The crystal structure model of decafluorocyclohex-1-ene at 4.2 K derived from simulated powder diffraction data and solid-state energy minimization [Smrcok et al. (2013). Acta Cryst. B69, 395-404] is found to be incomplete. In this study it is completed by an additional alternative molecular orientation revealed from the difference density analysis and direct space search. The structure is refined by the derivative difference method in the rigid-body approximation leading to perfect agreement between observed and calculated neutron powder patterns.
Supporting information
CCDC reference: 971462
Crystal data, data collection and structure refinement details are summarized in Table 1.
S2. Results and discussion
top
Program(s) used to refine structure: Powder diffraction, Derivative Difference Method (DDM)
L.A. Solovyov, J. Appl. Cryst. 37 (2004) 743.
Crystal data top
C6F10 | V = 765.2 (2) Å3 |
Mr = 262.06 | Z = 4 |
Monoclinic, P21/n | Dx = 2.276 Mg m−3 |
Hall symbol: -P 2yn | Neutron radiation, λ = 1.9090 Å |
a = 11.9302 (18) Å | T = 4 K |
b = 7.2371 (11) Å | white |
c = 9.6574 (14) Å | ?, ? × ? × ? mm |
β = 113.408 (3)° | |
Data collection top
D1A diffractometer | 2θmin = 10.000°, 2θmax = 53.950°, 2θstep = 0.050° |
Refinement top
Least-squares matrix: full | χ2 = 1.189 |
Rp = 0.023 | 880 data points |
Rwp = 0.026 | 15 parameters |
Rexp = 0.024 | 0 restraints |
RBragg = 0.016 | (Δ/σ)max = 0.004 |
R(F) = 0.013 | |
Crystal data top
C6F10 | β = 113.408 (3)° |
Mr = 262.06 | V = 765.2 (2) Å3 |
Monoclinic, P21/n | Z = 4 |
a = 11.9302 (18) Å | Neutron radiation, λ = 1.9090 Å |
b = 7.2371 (11) Å | T = 4 K |
c = 9.6574 (14) Å | ?, ? × ? × ? mm |
Data collection top
D1A diffractometer | 2θmin = 10.000°, 2θmax = 53.950°, 2θstep = 0.050° |
Refinement top
Rp = 0.023 | χ2 = 1.189 |
Rwp = 0.026 | 880 data points |
Rexp = 0.024 | 15 parameters |
RBragg = 0.016 | 0 restraints |
R(F) = 0.013 | |
Special details top
Refinement. Two independent C6F10 molecules were refined as rigid-bodies The molecular conformations were derived from DFT energy minimization |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.28017 | 0.31597 | 0.03928 | 0.012 (2)* | 0.5613 (36) |
C2 | 0.21245 | 0.48241 | −0.05893 | 0.012 (2)* | 0.5613 (36) |
C3 | 0.30225 | 0.64368 | −0.04860 | 0.012 (2)* | 0.5613 (36) |
C4 | 0.39367 | 0.67412 | 0.10920 | 0.012 (2)* | 0.5613 (36) |
C5 | 0.35140 | 0.37295 | 0.20749 | 0.012 (2)* | 0.5613 (36) |
C6 | 0.41518 | 0.55498 | 0.22272 | 0.012 (2)* | 0.5613 (36) |
F1 | 0.45731 | 0.83080 | 0.12841 | 0.0235 (15)* | 0.5613 (36) |
F2 | 0.36231 | 0.60485 | −0.14047 | 0.0235 (15)* | 0.5613 (36) |
F3 | 0.23645 | 0.80149 | −0.10200 | 0.0235 (15)* | 0.5613 (36) |
F4 | 0.15444 | 0.42784 | −0.20460 | 0.0235 (15)* | 0.5613 (36) |
F5 | 0.12714 | 0.54334 | −0.00821 | 0.0235 (15)* | 0.5613 (36) |
F6 | 0.49917 | 0.59075 | 0.36072 | 0.0235 (15)* | 0.5613 (36) |
F7 | 0.27043 | 0.38048 | 0.27693 | 0.0235 (15)* | 0.5613 (36) |
F8 | 0.43454 | 0.23834 | 0.27830 | 0.0235 (15)* | 0.5613 (36) |
F9 | 0.36179 | 0.25022 | −0.01606 | 0.0235 (15)* | 0.5613 (36) |
F10 | 0.19961 | 0.17950 | 0.02990 | 0.0235 (15)* | 0.5613 (36) |
C11 | 0.85045 | 0.15282 | 0.68327 | 0.012 (2)* | 0.4387 (36) |
C12 | 0.77404 | 0.18367 | 0.51310 | 0.012 (2)* | 0.4387 (36) |
C13 | 0.70225 | 0.00616 | 0.43667 | 0.012 (2)* | 0.4387 (36) |
C14 | 0.77945 | −0.16442 | 0.48557 | 0.012 (2)* | 0.4387 (36) |
C15 | 0.94052 | −0.01268 | 0.71026 | 0.012 (2)* | 0.4387 (36) |
C16 | 0.88399 | −0.17348 | 0.60838 | 0.012 (2)* | 0.4387 (36) |
F11 | 0.73521 | −0.31193 | 0.39749 | 0.0235 (15)* | 0.4387 (36) |
F12 | 0.60120 | −0.00999 | 0.47156 | 0.0235 (15)* | 0.4387 (36) |
F13 | 0.66080 | 0.02618 | 0.28409 | 0.0235 (15)* | 0.4387 (36) |
F14 | 0.85208 | 0.22791 | 0.44611 | 0.0235 (15)* | 0.4387 (36) |
F15 | 0.69531 | 0.32562 | 0.49376 | 0.0235 (15)* | 0.4387 (36) |
F16 | 0.94857 | −0.32991 | 0.64663 | 0.0235 (15)* | 0.4387 (36) |
F17 | 1.04159 | 0.04708 | 0.68716 | 0.0235 (15)* | 0.4387 (36) |
F18 | 0.98065 | −0.06532 | 0.85764 | 0.0235 (15)* | 0.4387 (36) |
F19 | 0.77290 | 0.11453 | 0.75235 | 0.0235 (15)* | 0.4387 (36) |
F110 | 0.91347 | 0.30880 | 0.74460 | 0.0235 (15)* | 0.4387 (36) |
Geometric parameters (Å, º) top
C1—C2 | 1.549 | C11—C12 | 1.550 |
C1—C5 | 1.562 | C11—C15 | 1.562 |
C1—F9 | 1.369 | C11—F19 | 1.371 |
C1—F10 | 1.357 | C11—F110 | 1.358 |
C2—C1 | 1.549 | C12—C11 | 1.550 |
C2—C3 | 1.560 | C12—C13 | 1.563 |
C2—F4 | 1.356 | C12—F14 | 1.368 |
C2—F5 | 1.368 | C12—F15 | 1.359 |
C3—C2 | 1.560 | C13—C12 | 1.563 |
C3—C4 | 1.502 | C13—C14 | 1.499 |
C3—F2 | 1.381 | C13—F12 | 1.375 |
C3—F3 | 1.365 | C13—F13 | 1.367 |
C4—C3 | 1.502 | C14—C13 | 1.499 |
C4—C6 | 1.341 | C14—C16 | 1.339 |
C4—F1 | 1.338 | C14—F11 | 1.338 |
C5—C1 | 1.562 | C15—C11 | 1.562 |
C5—C6 | 1.502 | C15—C16 | 1.501 |
C5—F7 | 1.382 | C15—F17 | 1.380 |
C5—F8 | 1.365 | C15—F18 | 1.366 |
C6—C4 | 1.341 | C16—C14 | 1.339 |
C6—C5 | 1.502 | C16—C15 | 1.501 |
C6—F6 | 1.338 | C16—F16 | 1.339 |
| | | |
C2—C1—C5 | 111.38 | C12—C11—C15 | 111.62 |
C2—C1—F9 | 108.67 | C12—C11—F19 | 108.08 |
C2—C1—F10 | 109.56 | C12—C11—F110 | 110.01 |
C5—C1—F9 | 108.52 | C15—C11—F19 | 108.70 |
C5—C1—F10 | 109.91 | C15—C11—F110 | 109.92 |
F9—C1—F10 | 108.74 | F19—C11—F110 | 108.43 |
C1—C2—C3 | 111.45 | C11—C12—C13 | 111.40 |
C1—C2—F4 | 109.88 | C11—C12—F14 | 108.26 |
C1—C2—F5 | 108.18 | C11—C12—F15 | 109.65 |
C3—C2—F4 | 109.84 | C13—C12—F14 | 109.03 |
C3—C2—F5 | 108.60 | C13—C12—F15 | 109.79 |
F4—C2—F5 | 108.83 | F14—C12—F15 | 108.65 |
C2—C3—C4 | 112.09 | C12—C13—C14 | 112.29 |
C2—C3—F2 | 108.89 | C12—C13—F12 | 109.09 |
C2—C3—F3 | 108.64 | C12—C13—F13 | 108.91 |
C4—C3—F2 | 109.90 | C14—C13—F12 | 109.38 |
C4—C3—F3 | 109.98 | C14—C13—F13 | 109.79 |
F2—C3—F3 | 107.21 | F12—C13—F13 | 107.26 |
C3—C4—C6 | 123.98 | C13—C14—C16 | 124.40 |
C3—C4—F1 | 114.78 | C13—C14—F11 | 114.23 |
C6—C4—F1 | 121.23 | C16—C14—F11 | 121.33 |
C1—C5—C6 | 112.67 | C11—C15—C16 | 112.32 |
C1—C5—F7 | 108.69 | C11—C15—F17 | 108.65 |
C1—C5—F8 | 108.78 | C11—C15—F18 | 108.67 |
C6—C5—F7 | 109.35 | C16—C15—F17 | 110.12 |
C6—C5—F8 | 110.36 | C16—C15—F18 | 109.78 |
F7—C5—F8 | 106.81 | F17—C15—F18 | 107.15 |
C4—C6—C5 | 124.14 | C14—C16—C15 | 124.16 |
C4—C6—F6 | 121.24 | C14—C16—F16 | 121.10 |
C5—C6—F6 | 114.59 | C15—C16—F16 | 114.73 |
Experimental details
Crystal data |
Chemical formula | C6F10 |
Mr | 262.06 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 4 |
a, b, c (Å) | 11.9302 (18), 7.2371 (11), 9.6574 (14) |
β (°) | 113.408 (3) |
V (Å3) | 765.2 (2) |
Z | 4 |
Radiation type | Neutron, λ = 1.9090 Å |
Specimen shape, size (mm) | ?, ? × ? × ? |
|
Data collection |
Diffractometer | D1A diffractometer |
Specimen mounting | ? |
Data collection mode | ? |
Scan method | ? |
2θ values (°) | 2θmin = 10.000 2θmax = 53.950 2θstep = 0.050 |
|
Refinement |
R factors and goodness of fit | Rp = 0.023, Rwp = 0.026, Rexp = 0.024, RBragg = 0.016, R(F) = 0.013, χ2 = 1.189 |
No. of data points | 880 |
No. of parameters | 15 |
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