Perchlorophenalenyl radical, C13Cl9: a modulated structure with nine threefold-symmetric molecules in the asymmetric unit

Koutentis, P.A.; Haddon, R.C.; Oakley, R.T.; Cordes, A.W.; Brock, C.P.

doi:10.1107/S0108768101011193

Perchlorophenalenyl radical, C₁₃Cl₉: a modulated structure with nine threefold-symmetric molecules in the asymmetric unit

P. A. Koutentis, R. C. Haddon, R. T. Oakley, A. W. Cordes and C. P. Brock

The odd-alternant perchlorophenalenyl radical, C₁₃Cl₉, forms molecular stacks centered on crystallographic threefold rotation axes, but the spacing within the stacks (3.78 Å) is too large to allow good overlap of the orbitals in which the spin density is localized. The radical is ruffled because of the intramolecular repulsions between α Cl atoms (the Cl

Cl peri interactions); the average displacement of an α Cl atom from the molecular plane is ∼0.7 Å. The deviations from molecular planarity do not, however, determine the spacing within the stacks, which is determined instead by interactions between stacks. The modulations found in the P3c1 superstructure are a response to the short interstack contacts that would occur in the average pseudocell structure (R $\bar 3$ m, c′ = c/6). The primary modulation is a pattern of enantiomeric alternation; a secondary modulation involves small rotations of the molecules around their threefold axes. The number (9) of independent molecules in the true cell is exceptionally large because of the conflict between the preference within the molecular stacks for threefold rotational symmetry and the preference in directions perpendicular to the stack axes for twofold alternation of enantiomers. The structural complexity reduces the precision of the distances and angles determined, but the average values found are in excellent agreement with those calculated by density functional theory.

Keywords: perchlorophenalenyl radical; modulated structure; symmetry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101011193/bs0014sup1.cif Contains datablocks I, pseudor3
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101011193/bs0014Isup2.hkl Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768101011193/bs0014IIsup3.hkl Contains datablock II
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768101011193/bs0014sup4.pdf Supplementary material

Computing details top

For both compounds, data collection: COLLECT software (Nonius, 1998); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori & Camalli, 1994) in maXus (Mackay, Gilmore, Edwards, Tremayne, Stewart & Shankland, 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL PC (Sheldrick, 1990).

Figures top

(I) perchlorophenalenyl radical top

Crystal data top

C₁₃Cl₉	Melting point: 160_C(dec) in air; 248_C under Ar. K
M_r = 475.18	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3c1	Cell parameters from 63143 reflections
a = 18.704 (3) Å	θ = 1.3–27.5°
c = 22.675 (4) Å	µ = 1.64 mm⁻¹
V = 6870 (2) Å³	T = 299 K
Z = 18	Prisms. The a prism axis is c. The six major faces belong to the form {1 1 -2 0}., black
F(000) = 4158	0.40 × 0.10 × 0.10 mm
D_x = 2.067 Mg m⁻³

Data collection top

Nonius Kappa-CCD diffractometer	10524 independent reflections
Radiation source: fine-focus sealed tube	6178 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.033
Detector resolution: 18 pixels mm^-1	θ_max = 27.5°, θ_min = 1.3°
ϕ and ω scans with 1.0° steps	h = 0→24
Absorption correction: multi-scan DENZO-SMN (Otwinowski & Minor, 1997)	k = −21→0
T_min = 0.79, T_max = 0.85	l = −29→29
40131 measured reflections

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)] = 0.094	w = 1/[σ²(F_o²) + (0.03P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.174	(Δ/σ)_max = 0.001
S = 2.15	Δρ_max = 0.55 e Å⁻³
10524 reflections	Δρ_min = −0.44 e Å⁻³
448 parameters	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
759 restraints	Absolute structure parameter: 0.25 (9)

Crystal data top

C₁₃Cl₉	Z = 18
M_r = 475.18	Mo Kα radiation
Trigonal, P3c1	µ = 1.64 mm⁻¹
a = 18.704 (3) Å	T = 299 K
c = 22.675 (4) Å	0.40 × 0.10 × 0.10 mm
V = 6870 (2) Å³

Data collection top

Nonius Kappa-CCD diffractometer	10524 independent reflections
Absorption correction: multi-scan DENZO-SMN (Otwinowski & Minor, 1997)	6178 reflections with I > 2σ(I)
T_min = 0.79, T_max = 0.85	R_int = 0.033
40131 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.094	759 restraints
wR(F²) = 0.174	Δρ_max = 0.55 e Å⁻³
S = 2.15	Δρ_min = −0.44 e Å⁻³
10524 reflections	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
448 parameters	Absolute structure parameter: 0.25 (9)

Special details top

Experimental. The crystal-to-detector distance was 40 mm. Each frame was measured for 120 s. The number of scan sets measured was 13; the total number of frames measured was 1475.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cl1A	0.08999 (11)	0.56739 (14)	0.25513 (8)	0.0547 (5)
Cl2A	0.10122 (12)	0.41511 (12)	0.28623 (9)	0.0601 (5)
Cl3A	0.26629 (13)	0.42849 (10)	0.31604 (8)	0.0521 (5)
C01A	0.1827 (4)	0.5774 (4)	0.2780 (2)	0.0369 (8)
C02A	0.1875 (3)	0.5071 (3)	0.2857 (3)	0.0348 (7)
C03A	0.2651 (4)	0.5157 (3)	0.2908 (2)	0.0325 (8)
C04A	0.3389 (3)	0.5920 (3)	0.2868 (2)	0.0244 (6)
C05A	0.3333	0.6667	0.2840 (4)	0.0240 (5)
Cl1B	0.08682 (15)	0.55009 (16)	0.42405 (11)	0.0519 (7)	0.7613 (9)
Cl2B	0.11564 (15)	0.40905 (13)	0.45190 (11)	0.0531 (7)	0.7613 (9)
Cl3B	0.28448 (16)	0.43259 (14)	0.48028 (11)	0.0513 (7)	0.7613 (9)
C01B	0.1854 (5)	0.5752 (5)	0.4466 (3)	0.0369 (8)	0.7613 (9)
C02B	0.1987 (4)	0.5056 (4)	0.4542 (3)	0.0348 (7)	0.7613 (9)
C03B	0.2725 (5)	0.5134 (4)	0.4566 (3)	0.0325 (8)	0.7613 (9)
C04B	0.3464 (4)	0.5964 (4)	0.4518 (3)	0.0244 (6)	0.7613 (9)
C05B	0.3333	0.6667	0.4546 (5)	0.0240 (5)	0.7613 (9)
Cl1C	0.41434 (16)	0.90738 (11)	0.58813 (8)	0.0664 (7)
Cl2C	0.57342 (13)	0.91056 (13)	0.62365 (9)	0.0793 (8)
Cl3C	0.57568 (12)	0.75289 (15)	0.64730 (9)	0.0762 (7)
C01C	0.4115 (4)	0.8173 (3)	0.6113 (2)	0.0335 (8)
C02C	0.4810 (3)	0.8157 (4)	0.6200 (3)	0.0419 (8)
C03C	0.4861 (4)	0.7419 (4)	0.6255 (2)	0.0340 (8)
C04C	0.4102 (3)	0.6690 (4)	0.6181 (2)	0.0353 (7)
C05C	0.3333	0.6667	0.6187 (4)	0.0240 (5)
Cl1D	0.77214 (14)	0.57785 (11)	0.14435 (8)	0.0608 (6)
Cl2D	0.92106 (12)	0.56070 (13)	0.17416 (8)	0.0592 (6)
Cl3D	0.90290 (11)	0.39338 (14)	0.20401 (8)	0.0559 (5)
C01D	0.7529 (4)	0.4844 (3)	0.1677 (3)	0.0335 (8)
C02D	0.8240 (4)	0.4743 (4)	0.1746 (3)	0.0419 (8)
C03D	0.8189 (4)	0.3990 (4)	0.1818 (2)	0.0340 (8)
C04D	0.7399 (4)	0.3244 (4)	0.1757 (2)	0.0353 (7)
C05D	0.6667	0.3333	0.1771 (3)	0.0240 (5)
Cl1F	0.42632 (11)	0.24758 (14)	0.47622 (8)	0.0580 (6)
Cl2F	0.42554 (13)	0.08959 (13)	0.51044 (8)	0.0675 (6)
Cl3F	0.58670 (14)	0.09276 (10)	0.53739 (8)	0.0600 (6)
C01F	0.5172 (4)	0.2591 (4)	0.4993 (2)	0.0369 (8)
C02F	0.5152 (4)	0.1797 (3)	0.5083 (2)	0.0348 (7)
C03F	0.5893 (4)	0.1853 (3)	0.5148 (2)	0.0325 (8)
C04F	0.6681 (3)	0.2579 (3)	0.5093 (2)	0.0244 (6)
C05F	0.6667	0.3333	0.5108 (4)	0.0240 (5)
Cl1G	0.75564 (10)	−0.11114 (14)	0.03330 (8)	0.0580 (6)
Cl2G	0.77584 (12)	−0.25933 (12)	0.06381 (9)	0.0628 (6)
Cl3G	0.94543 (14)	−0.23431 (11)	0.09154 (8)	0.0591 (6)
C01G	0.8511 (4)	−0.0938 (4)	0.0554 (3)	0.0369 (8)
C02G	0.8607 (3)	−0.1596 (3)	0.0622 (3)	0.0348 (7)
C03G	0.9431 (4)	−0.1478 (3)	0.0714 (2)	0.0325 (8)
C04G	1.0108 (3)	−0.0697 (3)	0.0625 (2)	0.0244 (6)
C05G	1.0000	0.0000	0.0632 (4)	0.0240 (5)
Cl1H	1.07458 (18)	0.23985 (15)	0.19962 (13)	0.0639 (9)	0.7613 (9)
Cl2H	1.23650 (16)	0.24843 (15)	0.23517 (11)	0.0669 (9)	0.7613 (9)
Cl3H	1.24226 (15)	0.09024 (19)	0.25870 (11)	0.0680 (9)	0.7613 (9)
C01H	1.0717 (5)	0.1522 (4)	0.2207 (3)	0.0335 (8)	0.7613 (9)
C02H	1.1491 (4)	0.1557 (4)	0.2298 (3)	0.0419 (8)	0.7613 (9)
C03H	1.1520 (5)	0.0864 (5)	0.2392 (3)	0.0340 (8)	0.7613 (9)
C04H	1.0790 (4)	0.0023 (5)	0.2307 (3)	0.0353 (7)	0.7613 (9)
C05H	1.0000	0.0000	0.2304 (5)	0.0240 (5)	0.7613 (9)
Cl1J	1.09432 (14)	0.24303 (11)	0.36582 (8)	0.0583 (6)
Cl2J	1.24842 (13)	0.23604 (13)	0.39845 (9)	0.0651 (6)
Cl3J	1.23854 (12)	0.07224 (15)	0.42688 (8)	0.0618 (6)
C01J	1.0819 (4)	0.1498 (3)	0.3897 (3)	0.0335 (8)
C02J	1.1507 (4)	0.1440 (4)	0.3962 (3)	0.0419 (8)
C03J	1.1502 (4)	0.0679 (4)	0.4071 (2)	0.0340 (8)
C04J	1.0735 (4)	−0.0043 (4)	0.3949 (2)	0.0353 (7)
C05J	1.0000	0.0000	0.3943 (4)	0.0240 (5)
Cl1E	0.7885 (3)	0.5778 (3)	0.3103 (2)	0.0550 (14)	0.50
Cl2E	0.9309 (2)	0.5513 (2)	0.34349 (17)	0.0520 (10)	0.50
Cl3E	0.8990 (2)	0.3786 (2)	0.36894 (16)	0.0478 (10)	0.50
C05E	0.6667	0.3333	0.3322 (7)	0.0240 (5)	0.50
C01E	0.7647 (3)	0.48135 (8)	0.3332 (6)	0.0335 (8)	0.50
C02E	0.8294 (2)	0.4680 (3)	0.3414 (3)	0.0419 (8)	0.50
C03E	0.81388 (15)	0.3874 (4)	0.3433 (4)	0.0340 (8)	0.50
C04E	0.7339 (2)	0.3200 (3)	0.3475 (4)	0.0353 (7)	0.50
Cl4E	0.4285 (3)	0.2608 (4)	0.3118 (2)	0.0792 (19)	0.50
Cl5E	0.4165 (3)	0.0985 (3)	0.34562 (18)	0.0839 (16)	0.50
Cl6E	0.5711 (3)	0.0908 (2)	0.37014 (17)	0.0788 (16)	0.50
C10E	0.6667	0.3333	0.3402 (7)	0.0240 (5)	0.50
C06E	0.51686 (3)	0.2652 (4)	0.3372 (6)	0.0369 (8)	0.50
C07E	0.5103 (2)	0.1896 (3)	0.3446 (4)	0.0348 (7)	0.50
C08E	0.5819 (4)	0.18561 (16)	0.3516 (4)	0.0325 (8)	0.50
C09E	0.6600 (3)	0.25347 (12)	0.3411 (4)	0.0244 (6)	0.50
C10B	0.3333	0.6667	0.4352 (6)	0.0240 (5)	0.24
Cl4B	0.4089 (4)	0.90709 (10)	0.4216 (3)	0.0664 (7)	0.24
Cl5B	0.5688 (3)	0.9133 (2)	0.4570 (3)	0.0793 (8)	0.24
Cl6B	0.5747 (2)	0.7563 (4)	0.4809 (4)	0.0762 (7)	0.24
C06B	0.4122 (2)	0.81614 (4)	0.4264 (3)	0.0335 (8)	0.24
C07B	0.48075 (17)	0.81952 (15)	0.4507 (2)	0.0419 (8)	0.24
C08B	0.47779 (15)	0.7463 (2)	0.4657 (3)	0.0340 (8)	0.24
C09B	0.40391 (16)	0.6709 (2)	0.4666 (5)	0.0353 (7)	0.24
C10H	1.0000	0.0000	0.2281 (7)	0.0240 (5)	0.24
Cl4H	0.75415 (14)	−0.1267 (3)	0.2015 (4)	0.0580 (6)	0.24
Cl5H	0.7906 (3)	−0.26427 (13)	0.2296 (3)	0.0628 (6)	0.24
Cl6H	0.9656 (4)	−0.22773 (19)	0.2542 (3)	0.0591 (6)	0.24
C06H	0.85268 (5)	−0.10221 (15)	0.2236 (4)	0.0369 (8)	0.24
C07H	0.87040 (16)	−0.16466 (8)	0.2275 (2)	0.0348 (7)	0.24
C08H	0.95210 (19)	−0.14457 (5)	0.2334 (3)	0.0325 (8)	0.24
C09H	1.01744 (12)	−0.06421 (8)	0.2253 (6)	0.0244 (6)	0.24

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cl1A	0.0270 (10)	0.0614 (13)	0.0707 (12)	0.0184 (10)	−0.0046 (9)	−0.0034 (10)
Cl2A	0.0441 (12)	0.0352 (11)	0.0754 (13)	0.0005 (9)	0.0033 (10)	0.0010 (10)
Cl3A	0.0628 (13)	0.0221 (10)	0.0663 (12)	0.0174 (10)	0.0040 (10)	0.0077 (8)
C01A	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C02A	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C03A	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C04A	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)
C05A	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1B	0.0369 (14)	0.0407 (15)	0.0783 (17)	0.0196 (12)	−0.0099 (12)	0.0086 (13)
Cl2B	0.0476 (16)	0.0232 (12)	0.0707 (16)	0.0043 (12)	0.0068 (12)	−0.0076 (11)
Cl3B	0.0582 (17)	0.0288 (13)	0.0681 (17)	0.0225 (13)	0.0031 (13)	0.0123 (11)
C01B	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C02B	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C03B	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C04B	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)
C05B	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1C	0.115 (2)	0.0264 (10)	0.0569 (12)	0.0350 (12)	0.0038 (12)	0.0052 (9)
Cl2C	0.0467 (13)	0.0552 (14)	0.0758 (14)	−0.0198 (10)	0.0054 (10)	−0.0256 (11)
Cl3C	0.0394 (13)	0.0942 (18)	0.0879 (15)	0.0280 (13)	−0.0200 (11)	−0.0003 (13)
C01C	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C02C	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C03C	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C04C	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
C05C	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1D	0.0781 (15)	0.0340 (11)	0.0670 (13)	0.0255 (11)	0.0052 (11)	0.0162 (9)
Cl2D	0.0312 (10)	0.0440 (12)	0.0700 (12)	−0.0056 (9)	0.0058 (9)	0.0016 (10)
Cl3D	0.0328 (11)	0.0687 (15)	0.0677 (12)	0.0265 (11)	−0.0082 (9)	−0.0015 (10)
C01D	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C02D	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C03D	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C04D	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
C05D	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1F	0.0281 (10)	0.0691 (15)	0.0696 (13)	0.0188 (10)	−0.0079 (9)	−0.0010 (10)
Cl2F	0.0456 (13)	0.0490 (13)	0.0728 (14)	−0.0027 (10)	−0.0068 (10)	0.0096 (10)
Cl3F	0.0757 (15)	0.0183 (9)	0.0739 (14)	0.0143 (10)	0.0069 (11)	0.0079 (9)
C01F	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C02F	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C03F	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C04F	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)
C05F	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1G	0.0213 (10)	0.0635 (14)	0.0730 (12)	0.0090 (9)	−0.0071 (9)	−0.0114 (11)
Cl2G	0.0474 (12)	0.0401 (12)	0.0741 (13)	0.0017 (10)	0.0033 (10)	−0.0012 (10)
Cl3G	0.0813 (16)	0.0348 (11)	0.0662 (12)	0.0326 (11)	−0.0020 (11)	0.0049 (9)
C01G	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C02G	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C03G	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C04G	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)
C05G	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1H	0.088 (2)	0.0317 (14)	0.0591 (16)	0.0201 (14)	−0.0009 (17)	0.0086 (12)
Cl2H	0.0563 (18)	0.0352 (15)	0.0645 (16)	−0.0106 (13)	0.0049 (13)	0.0014 (12)
Cl3H	0.0272 (14)	0.093 (2)	0.0750 (19)	0.0235 (15)	−0.0064 (13)	−0.0068 (15)
C01H	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C02H	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C03H	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C04H	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
C05H	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1J	0.0773 (15)	0.0260 (10)	0.0640 (12)	0.0200 (10)	0.0126 (11)	0.0110 (9)
Cl2J	0.0397 (12)	0.0472 (13)	0.0676 (12)	−0.0089 (9)	0.0024 (10)	0.0016 (10)
Cl3J	0.0469 (12)	0.0814 (16)	0.0628 (12)	0.0365 (12)	−0.0143 (10)	−0.0016 (11)
C01J	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C02J	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C03J	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C04J	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
C05J	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl1E	0.060 (4)	0.025 (2)	0.073 (3)	0.016 (2)	0.009 (3)	0.0145 (18)
Cl2E	0.0204 (17)	0.030 (2)	0.089 (3)	0.0003 (15)	−0.0002 (17)	−0.0014 (19)
Cl3E	0.030 (2)	0.045 (2)	0.074 (3)	0.0234 (18)	−0.0015 (17)	0.0074 (18)
C05E	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
C01E	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C02E	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C03E	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C04E	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
Cl4E	0.042 (3)	0.137 (6)	0.057 (3)	0.044 (4)	−0.008 (2)	−0.006 (4)
Cl5E	0.067 (3)	0.063 (3)	0.061 (3)	−0.014 (3)	0.016 (2)	−0.007 (2)
Cl6E	0.112 (4)	0.021 (2)	0.086 (3)	0.021 (2)	0.016 (3)	0.0150 (19)
C10E	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
C06E	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C07E	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C08E	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C09E	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)
C10B	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl4B	0.115 (2)	0.0264 (10)	0.0569 (12)	0.0350 (12)	0.0038 (12)	0.0052 (9)
Cl5B	0.0467 (13)	0.0552 (14)	0.0758 (14)	−0.0198 (10)	0.0054 (10)	−0.0256 (11)
Cl6B	0.0394 (13)	0.0942 (18)	0.0879 (15)	0.0280 (13)	−0.0200 (11)	−0.0003 (13)
C06B	0.0408 (19)	0.0157 (15)	0.0413 (19)	0.0123 (14)	0.0080 (14)	−0.0004 (13)
C07B	0.035 (2)	0.035 (2)	0.0359 (17)	0.0026 (15)	0.0028 (15)	−0.0017 (15)
C08B	0.0333 (19)	0.0354 (19)	0.0297 (18)	0.0145 (16)	−0.0028 (14)	−0.0033 (14)
C09B	0.0349 (19)	0.0403 (18)	0.0297 (15)	0.0180 (17)	−0.0001 (15)	−0.0006 (13)
C10H	0.0269 (7)	0.0269 (7)	0.0183 (11)	0.0134 (4)	0.000	0.000
Cl4H	0.0213 (10)	0.0635 (14)	0.0730 (12)	0.0090 (9)	−0.0071 (9)	−0.0114 (11)
Cl5H	0.0474 (12)	0.0401 (12)	0.0741 (13)	0.0017 (10)	0.0033 (10)	−0.0012 (10)
Cl6H	0.0813 (16)	0.0348 (11)	0.0662 (12)	0.0326 (11)	−0.0020 (11)	0.0049 (9)
C06H	0.0367 (19)	0.043 (2)	0.0277 (17)	0.0175 (16)	−0.0015 (14)	0.0060 (14)
C07H	0.0320 (18)	0.0245 (16)	0.0356 (17)	0.0050 (14)	0.0026 (14)	−0.0008 (13)
C08H	0.047 (2)	0.0158 (15)	0.0303 (17)	0.0127 (15)	0.0004 (14)	−0.0046 (12)
C09H	0.0291 (15)	0.0201 (15)	0.0263 (14)	0.0141 (13)	0.0011 (12)	0.0006 (12)

Geometric parameters (Å, º) top

C01A—C02A	1.372 (7)	C04A—C05A	1.452 (5)
C01B—C02B	1.452 (9)	C04B—C05B	1.454 (6)
C01C—C02C	1.331 (8)	C04C—C05C	1.416 (5)
C01D—C02D	1.442 (8)	C04D—C05D	1.461 (6)
C01E—C02E	1.367	C04E—C05E	1.442
C01F—C02F	1.481 (7)	C04F—C05F	1.425 (5)
C01G—C02G	1.339 (7)	C04G—C05G	1.416 (5)
C01H—C02H	1.432 (10)	C04H—C05H	1.456 (7)
C01J—C02J	1.354 (8)	C04J—C05J	1.416 (6)
C06B—C07B	1.367	C09B—C10B	1.467
C06E—C07E	1.367	C09E—C10E	1.436
C06H—C07H	1.367	C09H—C10H	1.394
C01A—C04Aⁱ	1.472 (7)	Cl1A—C01A	1.728 (6)
C01B—C04Bⁱ	1.360 (9)	Cl1B—C01B	1.737 (7)
C01C—C04Cⁱⁱ	1.475 (7)	Cl1C—C01C	1.740 (6)
C01D—C04Dⁱⁱⁱ	1.386 (7)	Cl1D—C01D	1.684 (5)
C01E—C04Eⁱⁱⁱ	1.484	Cl1E—C01E	1.709
C01F—C04F^iv	1.379 (7)	Cl1F—C01F	1.686 (6)
C01G—C04G^v	1.444 (7)	Cl1G—C01G	1.722 (6)
C01H—C04H^vi	1.417 (9)	Cl1H—C01H	1.682 (7)
C01J—C04J^vi	1.407 (7)	Cl1J—C01J	1.727 (5)
C06B—C09Bⁱⁱ	1.801	Cl4B—C06B	1.736
C06E—C09E^iv	1.419	Cl4E—C06E	1.712
C06H—C09H^v	1.441	Cl4H—C06H	1.736
C02A—C03A	1.384 (7)	Cl2A—C02A	1.669 (6)
C02B—C03B	1.315 (9)	Cl2B—C02B	1.694 (7)
C02C—C03C	1.435 (8)	Cl2C—C02C	1.754 (6)
C02D—C03D	1.374 (8)	Cl2D—C02D	1.724 (6)
C02E—C03E	1.386	Cl2E—C02E	1.753
C02F—C03F	1.345 (8)	Cl2F—C02F	1.682 (6)
C02G—C03G	1.460 (8)	Cl2G—C02G	1.743 (6)
C02H—C03H	1.340 (9)	Cl2H—C02H	1.691 (7)
C02J—C03J	1.439 (8)	Cl2J—C02J	1.778 (6)
C07B—C08B	1.386	Cl5B—C07B	1.709
C07E—C08E	1.386	Cl5E—C07E	1.730
C07H—C08H	1.386	Cl5H—C07H	1.709
C03A—C04A	1.408 (7)	Cl3A—C03A	1.739 (6)
C03B—C04B	1.478 (9)	Cl3B—C03B	1.721 (7)
C03C—C04C	1.402 (7)	Cl3C—C03C	1.658 (6)
C03D—C04D	1.444 (7)	Cl3D—C03D	1.703 (6)
C03E—C04E	1.396	Cl3E—C03E	1.777
C03F—C04F	1.425 (7)	Cl3F—C03F	1.782 (6)
C03G—C04G	1.388 (7)	Cl3G—C03G	1.702 (5)
C03H—C04H	1.493 (9)	Cl3H—C03H	1.712 (8)
C03J—C04J	1.422 (7)	Cl3J—C03J	1.674 (6)
C08B—C09B	1.396	Cl6B—C08B	1.760
C08E—C09E	1.396	Cl6E—C08E	1.733
C08H—C09H	1.396	Cl6H—C08H	1.760

C04Aⁱ—C01A—C02A	123.3 (5)	C02G—C01G—Cl1G	117.5 (5)
C04Bⁱ—C01B—C02B	119.9 (7)	C02H—C01H—Cl1H	117.3 (6)
C04Cⁱⁱ—C01C—C02C	120.0 (5)	C02J—C01J—Cl1J	117.5 (5)
C04Dⁱⁱⁱ—C01D—C02D	117.8 (5)	C07B—C06B—Cl4B	118.2
C04Eⁱⁱⁱ—C01E—C02E	118.8	C07E—C06E—Cl4E	114.0
C04F^iv—C01F—C02F	119.1 (5)	C07H—C06H—Cl4H	118.2
C04G^v—C01G—C02G	121.5 (5)	C01A—C02A—Cl2A	119.7 (5)
C04H^vi—C01H—C02H	118.9 (6)	C01B—C02B—Cl2B	118.3 (6)
C04J^vi—C01J—C02J	118.7 (5)	C01C—C02C—Cl2C	117.6 (5)
C09Bⁱⁱ—C06B—C07B	102.8	C01D—C02D—Cl2D	119.0 (5)
C09E^iv—C06E—C07E	122.4	C01E—C02E—Cl2E	120.3
C09H^v—C06H—C07H	120.1	C01F—C02F—Cl2F	121.4 (5)
C01A—C02A—C03A	117.8 (5)	C01G—C02G—Cl2G	121.2 (5)
C01B—C02B—C03B	123.0 (6)	C01H—C02H—Cl2H	119.5 (6)
C01C—C02C—C03C	124.8 (5)	C01J—C02J—Cl2J	118.9 (5)
C01D—C02D—C03D	123.4 (5)	C06B—C07B—Cl5B	118.7
C01E—C02E—C03E	118.7	C06E—C07E—Cl5E	122.8
C01F—C02F—C03F	115.4 (5)	C06H—C07H—Cl5H	118.7
C01G—C02G—C03G	119.6 (5)	C03A—C02A—Cl2A	122.4 (5)
C01H—C02H—C03H	120.5 (7)	C03B—C02B—Cl2B	118.2 (6)
C01J—C02J—C03J	124.2 (5)	C03C—C02C—Cl2C	117.6 (5)
C06B—C07B—C08B	118.7	C03D—C02D—Cl2D	117.6 (5)
C06E—C07E—C08E	118.7	C03E—C02E—Cl2E	120.8
C06H—C07H—C08H	118.7	C03F—C02F—Cl2F	123.2 (5)
C02A—C03A—C04A	123.5 (5)	C03G—C02G—Cl2G	119.1 (4)
C02B—C03B—C04B	119.6 (6)	C03H—C02H—Cl2H	119.7 (6)
C02C—C03C—C04C	113.7 (5)	C03J—C02J—Cl2J	116.6 (5)
C02D—C03D—C04D	119.6 (6)	C08B—C07B—Cl5B	122.4
C02E—C03E—C04E	122.1	C08E—C07E—Cl5E	118.5
C02F—C03F—C04F	126.8 (5)	C08H—C07H—Cl5H	122.4
C02G—C03G—C04G	118.5 (5)	C02A—C03A—Cl3A	115.0 (4)
C02H—C03H—C04H	122.7 (7)	C02B—C03B—Cl3B	120.3 (6)
C02J—C03J—C04J	114.2 (5)	C02C—C03C—Cl3C	117.1 (5)
C07B—C08B—C09B	122.1	C02D—C03D—Cl3D	120.3 (5)
C07E—C08E—C09E	122.1	C02E—C03E—Cl3E	113.6
C07H—C08H—C09H	122.1	C02F—C03F—Cl3F	115.4 (4)
C03A—C04A—C05A	118.3 (4)	C02G—C03G—Cl3G	114.9 (4)
C03B—C04B—C05B	117.0 (5)	C02H—C03H—Cl3H	121.0 (6)
C03C—C04C—C05C	123.2 (5)	C02J—C03J—Cl3J	118.6 (5)
C03D—C04D—C05D	116.9 (5)	C07B—C08B—Cl6B	114.4
C03E—C04E—C05E	117.4	C07E—C08E—Cl6E	117.5
C03F—C04F—C05F	114.8 (4)	C07H—C08H—Cl6H	114.3
C03G—C04G—C05G	119.5 (4)	C04A—C03A—Cl3A	120.5 (5)
C03H—C04H—C05H	114.3 (6)	C04B—C03B—Cl3B	118.8 (6)
C03J—C04J—C05J	119.7 (5)	C04C—C03C—Cl3C	128.7 (5)
C08B—C09B—C10B	117.2	C04D—C03D—Cl3D	119.9 (5)
C08E—C09E—C10E	117.0	C04E—C03E—Cl3E	119.9
C08H—C09H—C10H	117.7	C04F—C03F—Cl3F	117.7 (4)
C04Aⁱ—C05A—C04A	119.8	C04G—C03G—Cl3G	126.6 (5)
C04Bⁱ—C05B—C04B	119.8	C04H—C03H—Cl3H	116.2 (6)
C04Cⁱⁱ—C05C—C04C	120.0	C04J—C03J—Cl3J	126.9 (5)
C04Dⁱⁱⁱ—C05D—C04D	120.0	C09B—C08B—Cl6B	123.5
C04Eⁱⁱⁱ—C05E—C04E	114.4	C09E—C08E—Cl6E	120.3
C04F^iv—C05F—C04F	119.9	C09H—C08H—Cl6H	123.5
C04G^v—C05G—C04G	120.0	C01Aⁱⁱ—C04A—C03A	126.9 (5)
C04H^vi—C05H—C04H	120.0	C01Bⁱⁱ—C04B—C03B	124.0 (6)
C04J^vi—C05J—C04J	120.0	C01Cⁱ—C04C—C03C	121.1 (5)
C09Bⁱⁱ—C10B—C09B	98.4	C01D^iv—C04D—C03D	123.3 (5)
C09E^iv—C10E—C09E	120.0	C01E^iv—C04E—C03E	120.8
C09H^v—C10H—C09H	119.8	C01Fⁱⁱⁱ—C04F—C03F	124.5 (5)
C04Aⁱ—C01A—Cl1A	118.1 (4)	C01G^vi—C04G—C03G	122.9 (5)
C04Bⁱ—C01B—Cl1B	124.5 (6)	C01H^v—C04H—C03H	126.5 (7)
C04Cⁱⁱ—C01C—Cl1C	119.2 (4)	C01J^v—C04J—C03J	120.9 (5)
C04Dⁱⁱⁱ—C01D—Cl1D	126.0 (5)	C06Bⁱ—C09B—C08B	115.9
C04Eⁱⁱⁱ—C01E—Cl1E	124.6	C06Eⁱⁱⁱ—C09E—C08E	125.9
C04F^iv—C01F—Cl1F	127.6 (5)	C06H^vi—C09H—C08H	122.2
C04G^v—C01G—Cl1G	120.9 (4)	C01Aⁱⁱ—C04A—C05A	114.4 (4)
C04H^vi—C01H—Cl1H	123.8 (6)	C01Bⁱⁱ—C04B—C05B	119.0 (6)
C04J^vi—C01J—Cl1J	123.2 (5)	C01Cⁱ—C04C—C05C	115.6 (5)
C09Bⁱⁱ—C06B—Cl4B	116.1	C01D^iv—C04D—C05D	119.8 (5)
C09E^iv—C06E—Cl4E	122.9	C01E^iv—C04E—C05E	112.9
C09H^v—C06H—Cl4H	120.4	C01Fⁱⁱⁱ—C04F—C05F	120.6 (5)
C02A—C01A—Cl1A	118.5 (5)	C01G^vi—C04G—C05G	117.5 (4)
C02B—C01B—Cl1B	115.3 (6)	C01H^v—C04H—C05H	119.1 (6)
C02C—C01C—Cl1C	120.7 (5)	C01J^v—C04J—C05J	119.0 (5)
C02D—C01D—Cl1D	115.9 (5)	C06Bⁱ—C09B—C10B	95.6
C02E—C01E—Cl1E	116.6	C06H^vi—C09H—C10H	119.3
C02F—C01F—Cl1F	113.3 (5)	C06Eⁱⁱⁱ—C09E—C10E	116.8

Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) −y+1, x−y, z; (iv) −x+y+1, −x+1, z; (v) −x+y+2, −x+1, z; (vi) −y+1, x−y−1, z.

(pseudor3) perchlorophenalenyl radical top

Crystal data top

C₁₃Cl₉	Melting point: 160_C(dec) in air; 248_C under Ar. K
M_r = 475.18	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3m	Cell parameters from 63143 reflections
a = 18.704 (3) Å	θ = 1.3–27.5°
c = 3.7792 (7) Å	µ = 1.64 mm⁻¹
V = 1145.0 (3) Å³	T = 299 K
Z = 3	Prisms. The a prism axis is c. The six major faces belong to the form {1 1 -2 0}., black
F(000) = 693	0.40 × 0.10 × 0.10 mm
D_x = 2.067 Mg m⁻³

Data collection top

Nonius Kappa-CCD diffractometer	323 independent reflections
Radiation source: fine-focus sealed tube	318 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
Detector resolution: 18 pixels mm^-1	θ_max = 27.5°, θ_min = 2.2°
ϕ and ω scans with 1.0° steps	h = 0→24
Absorption correction: multi-scan DENZO-SMN (Otwinowski & Minor, 1997)	k = −21→0
T_min = 0.79, T_max = 0.85	l = −4→4
2409 measured reflections

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.045	Secondary atom site location: difference Fourier map
wR(F²) = 0.140	w = 1/[σ²(F_o²) + (0.03P)²] where P = (F_o² + 2F_c²)/3
S = 4.08	(Δ/σ)_max < 0.001
323 reflections	Δρ_max = 0.36 e Å⁻³
64 parameters	Δρ_min = −0.33 e Å⁻³

Crystal data top

C₁₃Cl₉	Z = 3
M_r = 475.18	Mo Kα radiation
Trigonal, R3m	µ = 1.64 mm⁻¹
a = 18.704 (3) Å	T = 299 K
c = 3.7792 (7) Å	0.40 × 0.10 × 0.10 mm
V = 1145.0 (3) Å³

Data collection top

Nonius Kappa-CCD diffractometer	323 independent reflections
Absorption correction: multi-scan DENZO-SMN (Otwinowski & Minor, 1997)	318 reflections with I > 2σ(I)
T_min = 0.79, T_max = 0.85	R_int = 0.034
2409 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.045	64 parameters
wR(F²) = 0.140	1 restraint
S = 4.08	Δρ_max = 0.36 e Å⁻³
323 reflections	Δρ_min = −0.33 e Å⁻³

Special details top

Experimental. The crystal-to-detector distance was 40 mm. Each frame was measured for 120 s. The number of scan sets measured was 13; the total number of frames measured was 1475.

Geometry. The distances and angles are determined for atomic positions averaged over nine independent molecules. The values are reasonably precise but very inaccurate.

Refinement. Friedel reflections were merged during refinement. Refinement with unmerged data gave a Flack parameter of 0.2 (2).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cl1	0.75782 (16)	−0.0976 (3)	0.1796 (7)	0.105 (3)	0.50
Cl2	0.7673 (2)	−0.2507 (2)	−0.0146 (12)	0.1085 (16)	0.50
Cl3	0.9320 (3)	−0.23869 (17)	−0.1771 (7)	0.0913 (12)	0.50
C01	0.8507 (4)	−0.07464 (18)	0.0412 (16)	0.0575 (18)
C02	0.8557 (7)	−0.1564 (5)	−0.003 (3)	0.055 (3)	0.50
C03	0.9368 (8)	−0.1502 (4)	−0.044 (2)	0.036 (4)	0.50
C04	1.0059 (5)	−0.0734 (4)	0.002 (2)	0.0357 (13)	0.50
C05	1.0000	0.0000	0.000 (3)	0.0271 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cl1	0.0304 (10)	0.191 (7)	0.0706 (16)	0.0397 (16)	0.0102 (9)	0.0125 (19)
Cl2	0.086 (2)	0.0671 (18)	0.0738 (16)	−0.0352 (14)	0.0096 (17)	−0.0022 (16)
Cl3	0.160 (3)	0.0365 (13)	0.0721 (19)	0.0450 (16)	0.003 (2)	−0.0086 (12)
C01	0.027 (2)	0.092 (4)	0.033 (3)	0.0133 (12)	0.0033 (19)	0.0017 (9)
C02	0.043 (5)	0.049 (5)	0.036 (3)	−0.006 (4)	0.001 (3)	−0.002 (4)
C03	0.042 (11)	0.029 (3)	0.038 (3)	0.018 (3)	0.002 (3)	0.006 (2)
C04	0.048 (3)	0.037 (3)	0.028 (3)	0.025 (3)	−0.001 (2)	0.003 (3)
C05	0.0293 (18)	0.0293 (18)	0.023 (3)	0.0147 (9)	0.000	0.000

Geometric parameters (Å, º) top

Cl1—C01	1.652 (6)	C02—C03	1.470 (15)
Cl2—C02	1.712 (8)	C03—C04	1.381 (12)
Cl3—C03	1.688 (9)	C04—C05	1.431 (5)
C01—C02	1.587 (13)	C04—C01ⁱ	1.307 (9)

C04ⁱⁱ—C01—C02	115.0 (6)	C02—C03—Cl3	114.0 (7)
C04ⁱⁱ—C01—Cl1	134.3 (4)	C04—C03—Cl3	128.4 (10)
C02—C01—Cl1	110.1 (5)	C03—C04—C05	121.1 (8)
C01—C02—C03	119.4 (5)	C01ⁱ—C04—C03	114.4 (7)
C01—C02—Cl2	120.2 (9)	C01ⁱ—C04—C05	124.5 (6)
C03—C02—Cl2	120.4 (8)	C04ⁱⁱ—C05—C04	120
C02—C03—C04	117.4 (8)

Symmetry codes: (i) −y+1, x−y−1, z; (ii) −x+y+2, −x+1, z.

Experimental details

	(I)	(pseudor3)
Crystal data
Chemical formula	C₁₃Cl₉	C₁₃Cl₉
M_r	475.18	475.18
Crystal system, space group	Trigonal, P3c1	Trigonal, R3m
Temperature (K)	299	299
a, c (Å)	18.704 (3), 22.675 (4)	18.704 (3), 3.7792 (7)
V (Å³)	6870 (2)	1145.0 (3)
Z	18	3
Radiation type	Mo Kα	Mo Kα
µ (mm⁻¹)	1.64	1.64
Crystal size (mm)	0.40 × 0.10 × 0.10	0.40 × 0.10 × 0.10

Data collection
Diffractometer	Nonius Kappa-CCD diffractometer	Nonius Kappa-CCD diffractometer
Absorption correction	Multi-scan DENZO-SMN (Otwinowski & Minor, 1997)	Multi-scan DENZO-SMN (Otwinowski & Minor, 1997)
T_min, T_max	0.79, 0.85	0.79, 0.85
No. of measured, independent and observed [I > 2σ(I)] reflections	40131, 10524, 6178	2409, 323, 318
R_int	0.033	0.034
(sin θ/λ)_max (Å⁻¹)	0.650	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.094, 0.174, 2.15	0.045, 0.140, 4.08
No. of reflections	10524	323
No. of parameters	448	64
No. of restraints	759	1
Δρ_max, Δρ_min (e Å⁻³)	0.55, −0.44	0.36, −0.33
Absolute structure	Flack H D (1983), Acta Cryst. A39, 876-881	?
Absolute structure parameter	0.25 (9)	?

Computer programs: COLLECT software (Nonius, 1998), DENZO-SMN (Otwinowski & Minor, 1997), SCALEPACK (Otwinowski & Minor, 1997), SIR92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori & Camalli, 1994) in maXus (Mackay, Gilmore, Edwards, Tremayne, Stewart & Shankland, 1998), SHELXL97 (Sheldrick, 1997), SHELXTL PC (Sheldrick, 1990).

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