Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113029211/sk3514sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113029211/sk3514Isup2.hkl |
CCDC reference: 968242
The compound (Fig. 2) crystallizes in the monoclinic space group P21/c. The molecules are situated on crystallographic inversion centres, located at the mid-point of the central –N═N– bond. The OOC—Ph—N═N—Ph—COO fragment is almost planar. The N—O bond length [1.308 (5) Å] is within the range of distribution in comparison to 325 known N—O bond lengths [1.28 (4) Å] for nitroxide radicals (Allen, 2002). The molecules are arranged in thick layers parallel to (100) (i.e. in the bc plane). The –N═N– group is in the centre of this layer, whereas the piperidine N-oxide fragments are positioned at the surfaces of the layers (see Fig. 3). In the b direction, neighbouring molecules are parallel, but in the c direction, the central units of neighbouring molecules form an angle of about 58°. Each molecule is surrounded by 14 neighbouring molecules. The molecules are mainly connected by dispersive interactions supported by polarisation and weak Coulombic interactions. The intramolecular distance between the two oxygen radicals of the N-oxyl centres in each molecule is 23.658 (6) Å. The closest intermolecular O···O distance is 4.886 (6) Å, which indicates that interactions between the radicals do not play a role in the molecular packing.
The title compound was synthesised by the addition of 4-hydroxy-2,2,6,6-tetramethylpiperidineoxyl (TEMPOL) to azobenzene-4,4'-dicarbonyl dichloride. The crude product was recrystallised from ethanol as an orange powder. Elemental analysis calculated: C 66.39, H 7.31, N 9.72%; found: C 66.17, H 7.42, N 9.47%.
Differential thermal and thermogravimetrical analysis (DTA/TGA) were performed on a SETARAM (TGA 92) device. Approximately 10–15 mg of the sample was filled into corundum crucibles and measured from 293 to 773 K at a rate of 3 K min-1 under a nitrogen atmosphere.
For the crystal structure determination from laboratory X-ray powder diffraction data, the diffractogram was recorded in transmission mode on aa Stoe STADI-P diffractometer with a Ge(111) monochromator and a linear position-sensitive detector using Cu Kα1 radiation. The sample was measured for 26 h in a 0.7 mm capillary. The software WinXPOW (Stoe & Cie, 2004) was used for data acquisition.
For indexing and structure solution, the powder pattern was truncated to a real-space resolution of approximately 2.58 Å, which for Cu Kα1 radiation corresponds to the range 3.0–34.8° in 2θ. The background was subtracted with a Bayesian high-pass filter (David & Sivia, 2001). The indexing was performed with the program DICVOL91 (Boultif & Louër, 1991). For the structure solution, DASH (David et al., 2006) was used. The starting molecular geometry, including H atoms, was generated using the force field CHARMM (Brooks et al.,1983). The asymmetric unit contains only half a molecule, thus half a molecule was used for the structure solution.
The structure was refined by the Rietveld method using the program TOPAS (Coelho, 2007) and the full 2θ range. Initially a Pawley refinement was carried out, refining the background, unit-cell parameters, zero-point error, peak-width and peak-asymmetry parameters. To allow the peak profiles to be described as accurately as possible, anisotropic peak broadening was included in a second Pawley refinement step, which improved the fit noticeably. The refinement converged with Rexp = 2.198%, Rexp' = 4.870%, Rwp = 2.345%, Rwp' = 5.196 %, Rp = 1.785%, Rp' = 5.356 % and a goodness-of-fit (gof) = 1.067 (the values with a prime denote the background-subtracted values). 89 restraints were used.
In the Rietveld refinement, the profile parameters, the cell parameters, the scale parameter, the background parameters and the atomic positions were allowed to refine. The molecule is situated on a crystallographic inversion center located on the midpoint of its N═N double bond. To fix the molecule at the inversion centre, the two N atoms of the –N═N– group were both included, but with occupancies of 0.5. Suitable chemical restraints were added for bond lengths, valence angles and the planarity of the benzene rings. A common isotropic displacement parameter for C, N and O atoms was refined. The isotropic displacement parameter of the H atoms was constrained at 1.2 times the global isotropic displacement parameter. The C—H bond lengths were set at the standard value of 0.96 Å, as obtained from the Cambridge Structural Database (Allen, 2002) for single-crystal studies at room temperature. Crystal data, data collection and structure refinement details are summarized in Table 1.
The DTA/TGA shows no mass loss or gain up to about 498 K. This indicates that the crystals do not contain water or solvent molecules in the lattice. The DTA exhibits a sharp endothermic signal at 498 K (melting point), followed by a broad exothermic signal at 502 K with a large weight loss resulting from decomposition.
The powder pattern could be indexed without ambiguity, resulting in a monoclinic unit cell with corresponding figures of merit M(20) = 28.4 (de Wolff, 1968) and F(20) = 52.8 (Smith & Snyder, 1979) as indices for the quality of indexing. A comparison of the unit-cell volume (V = 1574 Å3) with Hofmann's volume increments (Hofmann, 2002) led to the estimation that Z = 2. Subsequently, a Pawley (1981) refinement was carried out to extract integrated intensities and their correlations, converging with a Pawley χ2 value of 1.916. The space group was determined as P21/c from the refinement using Bayesian statistical analysis (Markvardsen et al., 2001). The crystal structure was solved without problems from the powder pattern in direct space with simulated annealing. The number of simulated annealing runs was increased from 10 to 50 in order to obtain better statistics regarding reproducibility. The subsequently Rietveld refinement converged with an excellent fit (Rexp = 2.330%, Rexp' = 6.774%, Rwp = 3.096%, Rwp' = 8.999%, Rp = 2.352%, Rp' = 9.287% and a gof = 1.329); the difference curve is almost a straight line (Fig. 1).
The compound (Fig. 2) crystallizes in the monoclinic space group P21/c. The molecules are situated on crystallographic inversion centres, located at the mid-point of the central –N═N– bond. The OOC—Ph—N═N—Ph—COO fragment is almost planar. The N—O bond length [1.308 (5) Å] is within the range of distribution in comparison to 325 known N—O bond lengths [1.28 (4) Å] for nitroxide radicals (Allen, 2002). The molecules are arranged in thick layers parallel to (100) (i.e. in the bc plane). The –N═N– group is in the centre of this layer, whereas the piperidine N-oxide fragments are positioned at the surfaces of the layers (see Fig. 3). In the b direction, neighbouring molecules are parallel, but in the c direction, the central units of neighbouring molecules form an angle of about 58°. Each molecule is surrounded by 14 neighbouring molecules. The molecules are mainly connected by dispersive interactions supported by polarisation and weak Coulombic interactions. The intramolecular distance between the two oxygen radicals of the N-oxyl centres in each molecule is 23.658 (6) Å. The closest intermolecular O···O distance is 4.886 (6) Å, which indicates that interactions between the radicals do not play a role in the molecular packing.
Data collection: WinXPOW (Stoe & Cie, 2004); cell refinement: TOPAS Academic (Coelho, 2007); data reduction: DASH (David et al., 2006); program(s) used to solve structure: DASH (David et al., 2006); program(s) used to refine structure: TOPAS Academic (Coelho, 2007); molecular graphics: Mercury (Macrae et al., 2008).
C32H42N4O6 | F(000) = 620.0 |
Mr = 578.7 | standard setting |
Monoclinic, P21/c | Dx = 1.222 Mg m−3 |
Hall symbol: -P 2ybc | Melting point: 498.38 K |
a = 19.3355 (5) Å | Cu Kα1 radiation, λ = 1.54056 Å |
b = 5.9277 (2) Å | µ = 0.69 mm−1 |
c = 14.5264 (4) Å | T = 293 K |
β = 109.222 (1)° | Particle morphology: needles |
V = 1572.12 (8) Å3 | cylinder, 30 × 0.7 mm |
Z = 2 |
Stoe Stadi-P diffractometer | Data collection mode: transmission |
Radiation source: sealed x-ray tube | Scan method: step |
Primary focussing Ge 111 monochromator | 2θmin = 2.0°, 2θmax = 79.99°, 2θstep = 0.01° |
Specimen mounting: 0.7 mm glass capillary |
Least-squares matrix: full with fixed elements per cycle | 114 parameters |
Rp = 9.336 | 59 restraints |
Rwp = 8.997 | 67 constraints |
Rexp = 6.772 | H-atom parameters not refined |
RBragg = 0.929 | Weighting scheme based on measured s.u.'s w = 1/σ[Yõbs~]2 |
χ2 = 1.329 | (Δ/σ)max = 0.001 |
7700 data points | Background function: Chebyshev polynomials with 20 refinable coefficients |
Excluded region(s): none | Preferred orientation correction: none |
Profile function: Fundamental Parameters Line Profile Fitting Approach (Cheary et al., 2004) |
C32H42N4O6 | V = 1572.12 (8) Å3 |
Mr = 578.7 | Z = 2 |
Monoclinic, P21/c | Cu Kα1 radiation, λ = 1.54056 Å |
a = 19.3355 (5) Å | µ = 0.69 mm−1 |
b = 5.9277 (2) Å | T = 293 K |
c = 14.5264 (4) Å | cylinder, 30 × 0.7 mm |
β = 109.222 (1)° |
Stoe Stadi-P diffractometer | Scan method: step |
Specimen mounting: 0.7 mm glass capillary | 2θmin = 2.0°, 2θmax = 79.99°, 2θstep = 0.01° |
Data collection mode: transmission |
Rp = 9.336 | 7700 data points |
Rwp = 8.997 | 114 parameters |
Rexp = 6.772 | 59 restraints |
RBragg = 0.929 | H-atom parameters not refined |
χ2 = 1.329 |
x | y | z | Uiso*/Ueq | ||
N1 | 0.0050 (2) | 0.0500 (6) | −0.03407 (19) | 0.05216 | |
N2 | −0.35613 (17) | −0.7331 (7) | −0.6456 (2) | 0.05216 | |
O2 | −0.1901 (3) | −0.0374 (8) | −0.4832 (3) | 0.05216 | |
O3 | −0.2265 (2) | −0.3401 (7) | −0.4226 (3) | 0.05216 | |
O1 | −0.3938 (2) | −0.8778 (8) | −0.7109 (3) | 0.05216 | |
C1 | −0.04371 (13) | −0.0071 (5) | −0.12878 (18) | 0.05216 | |
C2 | −0.04509 (13) | 0.1392 (4) | −0.2037 (2) | 0.05216 | |
H2 | −0.01623 | 0.27453 | −0.19060 | 0.06260 | |
C3 | −0.08821 (12) | 0.0846 (4) | −0.2969 (2) | 0.05216 | |
H3 | −0.08844 | 0.18696 | −0.34826 | 0.06260 | |
C4 | −0.12977 (13) | −0.1144 (5) | −0.3158 (2) | 0.05216 | |
C5 | −0.12746 (10) | −0.2574 (5) | −0.2397 (2) | 0.05216 | |
H5 | −0.15538 | −0.39466 | −0.25133 | 0.06260 | |
C6 | −0.08454 (12) | −0.2057 (4) | −0.14597 (18) | 0.05216 | |
H6 | −0.08368 | −0.30835 | −0.09450 | 0.06260 | |
C7 | −0.1826 (3) | −0.1614 (7) | −0.4152 (3) | 0.05216 | |
C8 | −0.28021 (17) | −0.3874 (5) | −0.51578 (19) | 0.05216 | |
H8 | −0.29762 | −0.24241 | −0.54313 | 0.06260 | |
C9 | −0.24189 (17) | −0.5243 (5) | −0.5733 (2) | 0.05216 | |
H9A | −0.20477 | −0.43766 | −0.58765 | 0.06260 | |
H9B | −0.21789 | −0.64859 | −0.53296 | 0.06260 | |
C10 | −0.29508 (17) | −0.6202 (6) | −0.6673 (2) | 0.05216 | |
C13 | −0.25209 (16) | −0.7833 (5) | −0.7061 (2) | 0.05216 | |
H13A | −0.22538 | −0.88483 | −0.65532 | 0.06260 | |
H13B | −0.28686 | −0.86555 | −0.75776 | 0.06260 | |
H13C | −0.21824 | −0.70368 | −0.72997 | 0.06260 | |
C14 | −0.32373 (16) | −0.4347 (5) | −0.7437 (2) | 0.05216 | |
H14A | −0.34730 | −0.31583 | −0.72027 | 0.06260 | |
H14B | −0.28204 | −0.37746 | −0.75818 | 0.06260 | |
H14C | −0.35837 | −0.49861 | −0.80118 | 0.06260 | |
C11 | −0.39471 (15) | −0.6343 (5) | −0.5841 (2) | 0.05216 | |
C12 | −0.33927 (15) | −0.5283 (5) | −0.49453 (16) | 0.05216 | |
H12A | −0.31642 | −0.64853 | −0.45082 | 0.06260 | |
H12B | −0.36672 | −0.42988 | −0.46700 | 0.06260 | |
C16 | −0.43204 (16) | −0.8275 (5) | −0.5501 (2) | 0.05216 | |
H16A | −0.44832 | −0.77513 | −0.49812 | 0.06260 | |
H16B | −0.47411 | −0.87580 | −0.60293 | 0.06260 | |
H16C | −0.39774 | −0.94899 | −0.52777 | 0.06260 | |
C15 | −0.45579 (16) | −0.4722 (5) | −0.6396 (2) | 0.05216 | |
H15A | −0.47228 | −0.39490 | −0.59254 | 0.06260 | |
H15B | −0.43934 | −0.36480 | −0.67726 | 0.06260 | |
H15C | −0.49556 | −0.56058 | −0.68083 | 0.06260 |
N1—C1 | 1.429 (3) | C9—H9B | 0.960 |
N2—O1 | 1.308 (5) | C9—C10 | 1.523 (4) |
N2—C10 | 1.478 (5) | C10—C13 | 1.500 (5) |
N2—C11 | 1.462 (5) | C10—C14 | 1.531 (4) |
O2—C7 | 1.201 (6) | C13—H13A | 0.960 |
O3—C7 | 1.339 (6) | C13—H13B | 0.960 |
O3—C8 | 1.437 (4) | C13—H13C | 0.960 |
C1—C2 | 1.384 (4) | C14—H14A | 0.960 |
C1—C6 | 1.393 (4) | C14—H14B | 0.960 |
C2—H2 | 0.960 | C14—H14C | 0.960 |
C2—C3 | 1.375 (4) | C11—C12 | 1.523 (3) |
C3—H3 | 0.960 | C11—C16 | 1.521 (5) |
C3—C4 | 1.403 (4) | C11—C15 | 1.530 (4) |
C4—C5 | 1.382 (4) | C12—H12A | 0.960 |
C4—C7 | 1.495 (4) | C12—H12B | 0.960 |
C5—H5 | 0.960 | C16—H16A | 0.960 |
C5—C6 | 1.376 (3) | C16—H16B | 0.960 |
C6—H6 | 0.960 | C16—H16C | 0.960 |
C8—H8 | 0.960 | C15—H15A | 0.960 |
C8—C9 | 1.521 (5) | C15—H15B | 0.960 |
C8—C12 | 1.526 (5) | C15—H15C | 0.960 |
C9—H9A | 0.960 | ||
O1—N2—C10 | 115.9 (3) | C9—C10—C13 | 106.4 (3) |
O1—N2—C11 | 115.5 (3) | C9—C10—C14 | 111.0 (3) |
C10—N2—C11 | 123.6 (3) | C13—C10—C14 | 107.7 (3) |
C7—O3—C8 | 118.1 (4) | C10—C13—H13A | 109.9 |
N1—C1—C2 | 116.4 (3) | C10—C13—H13B | 106.8 |
N1—C1—C6 | 121.8 (3) | C10—C13—H13C | 110.3 |
C2—C1—C6 | 121.7 (2) | H13A—C13—H13B | 110.1 |
C1—C2—H2 | 120.5 | H13A—C13—H13C | 109.1 |
C1—C2—C3 | 118.4 (2) | H13B—C13—H13C | 110.6 |
H2—C2—C3 | 121.1 | C10—C14—H14A | 111.8 |
C2—C3—H3 | 117.6 | C10—C14—H14B | 106.5 |
C2—C3—C4 | 120.8 (2) | C10—C14—H14C | 109.3 |
H3—C3—C4 | 121.6 | H14A—C14—H14B | 110.4 |
C3—C4—C5 | 119.6 (3) | H14A—C14—H14C | 108.7 |
C3—C4—C7 | 120.7 (3) | H14B—C14—H14C | 110.1 |
C5—C4—C7 | 119.3 (3) | N2—C11—C12 | 109.3 (3) |
C4—C5—H5 | 120.7 | N2—C11—C16 | 106.8 (3) |
C4—C5—C6 | 120.3 (2) | N2—C11—C15 | 113.0 (3) |
H5—C5—C6 | 119.0 | C12—C11—C16 | 108.0 (2) |
C1—C6—C5 | 119.2 (2) | C12—C11—C15 | 113.3 (2) |
C1—C6—H6 | 122.2 | C16—C11—C15 | 106.1 (2) |
C5—C6—H6 | 118.6 | C8—C12—C11 | 114.6 (2) |
O2—C7—O3 | 121.1 (4) | C8—C12—H12A | 109.1 |
O2—C7—C4 | 122.6 (4) | C8—C12—H12B | 107.7 |
O3—C7—C4 | 116.0 (4) | C11—C12—H12A | 107.5 |
O3—C8—H8 | 105.2 | C11—C12—H12B | 106.1 |
O3—C8—C9 | 106.9 (3) | H12A—C12—H12B | 111.9 |
O3—C8—C12 | 105.8 (3) | C11—C16—H16A | 109.0 |
H8—C8—C9 | 114.7 | C11—C16—H16B | 109.4 |
H8—C8—C12 | 112.9 | C11—C16—H16C | 109.0 |
C9—C8—C12 | 110.6 (2) | H16A—C16—H16B | 108.3 |
C8—C9—H9A | 111.6 | H16A—C16—H16C | 110.3 |
C8—C9—H9B | 107.4 | H16B—C16—H16C | 110.8 |
C8—C9—C10 | 112.6 (3) | C11—C15—H15A | 107.8 |
H9A—C9—H9B | 107.3 | C11—C15—H15B | 111.9 |
H9A—C9—C10 | 109.7 | C11—C15—H15C | 107.9 |
H9B—C9—C10 | 108.0 | H15A—C15—H15B | 109.8 |
N2—C10—C9 | 109.2 (3) | H15A—C15—H15C | 108.6 |
N2—C10—C13 | 111.6 (3) | H15B—C15—H15C | 110.7 |
N2—C10—C14 | 110.8 (3) | ||
O1—N2—C10—C9 | −160.6 (3) | H8—C8—C12—H12B | −41.5 |
O1—N2—C10—C13 | −43.2 (4) | C9—C8—C12—C11 | −53.8 (3) |
O1—N2—C10—C14 | 76.8 (4) | C9—C8—C12—H12A | 66.7 |
C11—N2—C10—C9 | 45.7 (4) | C9—C8—C12—H12B | −171.6 |
C11—N2—C10—C13 | 163.1 (3) | C8—C9—C10—N2 | −49.2 (4) |
C11—N2—C10—C14 | −76.9 (4) | C8—C9—C10—C13 | −169.9 (3) |
O1—N2—C11—C12 | 163.1 (3) | C8—C9—C10—C14 | 73.2 (3) |
O1—N2—C11—C16 | 46.5 (4) | H9A—C9—C10—N2 | −174.2 |
O1—N2—C11—C15 | −69.8 (4) | H9A—C9—C10—C13 | 65.2 |
C10—N2—C11—C12 | −43.1 (4) | H9A—C9—C10—C14 | −51.7 |
C10—N2—C11—C16 | −159.7 (3) | H9B—C9—C10—N2 | 69.2 |
C10—N2—C11—C15 | 84.0 (4) | H9B—C9—C10—C13 | −51.4 |
C8—O3—C7—O2 | 3.6 (6) | H9B—C9—C10—C14 | −168.3 |
C8—O3—C7—C4 | 177.6 (3) | N2—C10—C13—H13A | −69.4 |
C7—O3—C8—H8 | −37.9 | N2—C10—C13—H13B | 49.9 |
C7—O3—C8—C9 | 84.5 (4) | N2—C10—C13—H13C | 170.2 |
C7—O3—C8—C12 | −157.7 (3) | C9—C10—C13—H13A | 49.6 |
N1—C1—C2—H2 | −2.9 | C9—C10—C13—H13B | 169.0 |
N1—C1—C2—C3 | 176.6 (3) | C9—C10—C13—H13C | −70.7 |
C6—C1—C2—H2 | −179.4 | C14—C10—C13—H13A | 168.7 |
C6—C1—C2—C3 | 0.1 (4) | C14—C10—C13—H13B | −71.9 |
N1—C1—C6—C5 | −176.5 (3) | C14—C10—C13—H13C | 48.3 |
N1—C1—C6—H6 | 3.4 | N2—C10—C14—H14A | 64.0 |
C2—C1—C6—C5 | −0.2 (4) | N2—C10—C14—H14B | −175.3 |
C2—C1—C6—H6 | 179.7 | N2—C10—C14—H14C | −56.4 |
C1—C2—C3—H3 | −179.6 | C9—C10—C14—H14A | −57.5 |
C1—C2—C3—C4 | −0.0 (4) | C9—C10—C14—H14B | 63.1 |
H2—C2—C3—H3 | −0.1 | C9—C10—C14—H14C | −178.0 |
H2—C2—C3—C4 | 179.4 | C13—C10—C14—H14A | −173.7 |
C2—C3—C4—C5 | 0.1 (4) | C13—C10—C14—H14B | −53.0 |
C2—C3—C4—C7 | 173.5 (3) | C13—C10—C14—H14C | 65.9 |
H3—C3—C4—C5 | 179.6 | N2—C11—C12—C8 | 44.9 (3) |
H3—C3—C4—C7 | −7.0 | N2—C11—C12—H12A | −76.6 |
C3—C4—C5—H5 | −179.7 | N2—C11—C12—H12B | 163.6 |
C3—C4—C5—C6 | −0.2 (4) | C16—C11—C12—C8 | 160.7 (2) |
C7—C4—C5—H5 | 6.8 | C16—C11—C12—H12A | 39.3 |
C7—C4—C5—C6 | −173.6 (3) | C16—C11—C12—H12B | −80.6 |
C3—C4—C7—O2 | 2.6 (6) | C15—C11—C12—C8 | −82.1 (3) |
C3—C4—C7—O3 | −171.4 (3) | C15—C11—C12—H12A | 156.4 |
C5—C4—C7—O2 | 175.9 (4) | C15—C11—C12—H12B | 36.6 |
C5—C4—C7—O3 | 2.0 (5) | N2—C11—C16—H16A | 166.9 |
C4—C5—C6—C1 | 0.2 (4) | N2—C11—C16—H16B | −74.9 |
C4—C5—C6—H6 | −179.6 | N2—C11—C16—H16C | 46.5 |
H5—C5—C6—C1 | 179.8 | C12—C11—C16—H16A | 49.4 |
H5—C5—C6—H6 | −0.1 | C12—C11—C16—H16B | 167.7 |
O3—C8—C9—H9A | −65.7 | C12—C11—C16—H16C | −71.0 |
O3—C8—C9—H9B | 51.7 | C15—C11—C16—H16A | −72.3 |
O3—C8—C9—C10 | 170.4 (3) | C15—C11—C16—H16B | 46.0 |
H8—C8—C9—H9A | 50.4 | C15—C11—C16—H16C | 167.3 |
H8—C8—C9—H9B | 167.8 | N2—C11—C15—H15A | −169.8 |
H8—C8—C9—C10 | −73.4 | N2—C11—C15—H15B | −49.0 |
C12—C8—C9—H9A | 179.6 | N2—C11—C15—H15C | 73.1 |
C12—C8—C9—H9B | −63.0 | C12—C11—C15—H15A | −44.8 |
C12—C8—C9—C10 | 55.7 (3) | C12—C11—C15—H15B | 76.0 |
O3—C8—C12—C11 | −169.2 (3) | C12—C11—C15—H15C | −162.0 |
O3—C8—C12—H12A | −48.6 | C16—C11—C15—H15A | 73.4 |
O3—C8—C12—H12B | 73.1 | C16—C11—C15—H15B | −165.7 |
H8—C8—C12—C11 | 76.3 | C16—C11—C15—H15C | −43.7 |
H8—C8—C12—H12A | −163.2 |
Experimental details
Crystal data | |
Chemical formula | C32H42N4O6 |
Mr | 578.7 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 19.3355 (5), 5.9277 (2), 14.5264 (4) |
β (°) | 109.222 (1) |
V (Å3) | 1572.12 (8) |
Z | 2 |
Radiation type | Cu Kα1, λ = 1.54056 Å |
µ (mm−1) | 0.69 |
Specimen shape, size (mm) | Cylinder, 30 × 0.7 |
Data collection | |
Diffractometer | Stoe Stadi-P diffractometer |
Specimen mounting | 0.7 mm glass capillary |
Data collection mode | Transmission |
Scan method | Step |
2θ values (°) | 2θmin = 2.0 2θmax = 79.99 2θstep = 0.01 |
Refinement | |
R factors and goodness of fit | Rp = 9.336, Rwp = 8.997, Rexp = 6.772, RBragg = 0.929, χ2 = 1.329 |
No. of data points | 7700 |
No. of parameters | 114 |
No. of restraints | 59 |
H-atom treatment | H-atom parameters not refined |
Computer programs: WinXPOW (Stoe & Cie, 2004), TOPAS Academic (Coelho, 2007), DASH (David et al., 2006), Mercury (Macrae et al., 2008).