research papers
The crystal structure of pentamethylcyclopentadienylsodium, [NaC10H15] (NaCp*), has been determined from high-resolution X-ray powder diffraction. The compound crystallizes in space group Cmcm with lattice parameters a = 4.61030 (3), b = 16.4621 (3), c = 14.6751 (2) Å, V = 1113.77 (4) Å3 (Z = 4). NaCp* forms polymeric multidecker chains along the a axis. The Rietveld refinement (Rp = 0.050 and RF = 0.163) shows that the Cp* moieties occupy, with disorder, two different orientations rotated away from the eclipsed conformation by ±13.8°.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810101237X/na0125sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S010876810101237X/na0125Isup2.rtv |
CCDC reference: 174973
pentamethylcyclopentadienylsodium top
Crystal data top
NaC10H15 | Z = 4 |
Mr = 158.22 | ? radiation, λ = 0.491213(2) Å |
Orthorhombic, Cmcm | T = 298 K |
a = 4.61030 (3) Å | white |
b = 16.4621 (3) Å | cylinder, ? × ? × ? mm |
c = 14.6751 (2) Å | Specimen preparation: Prepared at 298 K K and ambient kPa |
V = 1113.77 (4) Å3 |
Data collection top
Beamline BM16 at the European Synchrotron Radiation Facility, Grenoble,
France diffractometer | Data collection mode: transmission |
Radiation source: synchrotron, ESRF beamlime BM16 | Scan method: continuous |
Si 111 monochromator | 2θmin = 2.003°, 2θmax = 25.994°, 2θstep = 0.003° |
Specimen mounting: 0.7 mm quartz capillary |
Refinement top
Least-squares matrix: full | ? data points |
Rp = 0.050 | Profile function: Pseudo-voigt function (Thompson, Cox & Hastings, 1987) with an additional symmetry correction according to Finger, Cox & Jephcoat (1994). Anisotropic strain-broadening effects were modeled following the method by Stephens (1999). |
Rwp = 0.066 | 9 parameters |
Rexp = ? | |
R(F2) = 0.136 | Background function: visually estimated fixed background |
χ2 = 0.168 |
Crystal data top
NaC10H15 | V = 1113.77 (4) Å3 |
Mr = 158.22 | Z = 4 |
Orthorhombic, Cmcm | ? radiation, λ = 0.491213(2) Å |
a = 4.61030 (3) Å | T = 298 K |
b = 16.4621 (3) Å | cylinder, ? × ? × ? mm |
c = 14.6751 (2) Å |
Data collection top
Beamline BM16 at the European Synchrotron Radiation Facility, Grenoble,
France diffractometer | Scan method: continuous |
Specimen mounting: 0.7 mm quartz capillary | 2θmin = 2.003°, 2θmax = 25.994°, 2θstep = 0.003° |
Data collection mode: transmission |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
NA1 | 0.5 | 0.1422 (2) | 0.25 | 0.10021 | |
C1 | 0.0 | 0.07422 (10) | 0.23026 (12) | 0.0428 (12)* | .5 |
C2 | 0.0 | 0.10664 (14) | 0.31979 (7) | 0.0428 (12)* | .5 |
C3 | 0.0 | 0.19256 (14) | 0.31287 (8) | 0.0428 (12)* | .5 |
C4 | 0.0 | 0.21325 (11) | 0.21907 (12) | 0.0428 (12)* | .5 |
C5 | 0.0 | 0.14011 (15) | 0.168011 (9) | 0.0428 (12)* | .5 |
C6 | 0.0 | −0.01446 (12) | 0.2057 (3) | 0.1775 (16)* | .75 |
C7 | 0.0 | 0.0584 (2) | 0.40680 (15) | 0.1775 (16)* | .75 |
C8 | 0.0 | 0.2514 (2) | 0.39126 (18) | 0.1775 (16)* | .75 |
C9 | 0.0 | 0.29789 (14) | 0.1805 (3) | 0.1775 (16)* | .75 |
C10 | 0.0 | 0.1336 (3) | 0.065787 (20 | 0.1775 (16)* | .75 |
Experimental details
Crystal data | |
Chemical formula | NaC10H15 |
Mr | 158.22 |
Crystal system, space group | Orthorhombic, Cmcm |
Temperature (K) | 298 |
a, b, c (Å) | 4.61030 (3), 16.4621 (3), 14.6751 (2) |
V (Å3) | 1113.77 (4) |
Z | 4 |
Radiation type | ?, λ = 0.491213(2) Å |
µ (mm−1) | ? |
Specimen shape, size (mm) | Cylinder, ? × ? × ? |
Data collection | |
Data collection method | Beamline BM16 at the European Synchrotron Radiation Facility, Grenoble, France |
Specimen mounting | 0.7 mm quartz capillary |
Data collection mode | Transmission |
Scan method | Continuous |
2θ values (°) | 2θmin = 2.003 2θmax = 25.994 2θstep = 0.003 |
Refinement | |
R factors and goodness of fit | Rp = 0.050, Rwp = 0.066, Rexp = ?, R(F2) = 0.136, χ2 = 0.168 |
No. of data points | ? |
No. of parameters | 9 |
No. of restraints | ? |
Computer programs: GSAS.