1,6,11,16,18,24,27,36-Octa­kis(trifluoro­meth­yl)-1,6,11,16,18,24,27,36-octa­hydro­(C60–Ih)[5,6]fullerene deutero­chloro­form solvate

Shustova, N.B.; Peryshkov, D.V.; Kareev, I.E.; Boltalina, O.V.; Strauss, S.H.

doi:10.1107/S1600536807031704

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1,6,11,16,18,24,27,36-Octakis(trifluoromethyl)-1,6,11,16,18,24,27,36-octahydro(C₆₀–I_h)[5,6]fullerene deuterochloroform solvate

N. B. Shustova, D. V. Peryshkov, I. E. Kareev, O. V. Boltalina and S. H. Strauss

The title compound, C₆₈F₂₄·CDCl₃, is a solvate of one of five isomers of C₆₀(CF₃)₈ that have now been isolated. The fullerene molecule has an idealized I_h C₆₀ core with the eight CF₃ groups arranged in an asymmetric fashion on a para–para–para–meta–para–meta–para ribbon of edge-sharing C₆(CF₃)₂ hexagons. There are no cage Csp³—Csp³ bonds. There are intramolecular F

F contacts between pairs of CF₃ groups on the same hexagon, in the range 2.544 (2)–2.641 (2) Å.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031704/tk2170sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031704/tk2170Isup2.hkl Contains datablock I

CCDC reference: 657682

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.003 Å
R factor = 0.054
wR factor = 0.150
Data-to-parameter ratio = 18.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT431_ALERT_2_B Short Inter HL..A Contact  Cl2    ..  F651    ..       2.90 Ang.

Alert level C
PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound ..          ?
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT098_ALERT_2_C Minimum (Negative) Residual Density ............      -1.31 e/A   
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C69
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl1    ..  F681    ..       2.92 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl2    ..  F621    ..       3.13 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl3    ..  F672    ..       3.02 Ang.

Alert level G
CHEMS02_ALERT_1_G  Please check that you have entered the correct
            _publ_requested_category classification of your compound;
            FI or CI or EI for inorganic; FM or CM or EM for metal-organic;
            FO or CO or EO for organic.
            From the CIF: _publ_requested_category   EO
            From the CIF: _chemical_formula_sum:C69 Cl3 D1 F24
PLAT793_ALERT_1_G Check the Absolute Configuration of C6     = ...          S
PLAT793_ALERT_1_G Check the Absolute Configuration of C16    = ...          R
PLAT793_ALERT_1_G Check the Absolute Configuration of C18    = ...          R
PLAT793_ALERT_1_G Check the Absolute Configuration of C24    = ...          R
PLAT793_ALERT_1_G Check the Absolute Configuration of C27    = ...          R
PLAT793_ALERT_1_G Check the Absolute Configuration of C36    = ...          S

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   7 ALERT level G = General alerts; check

   9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

Recently reported high-temperature reactions of C₆₀ with CF₃I have yielded five C₆₀(CF₃)₈ derivatives, with thermodynamically stable addition patterns that are asymmetric as well as unprecedented in fullerene(X)_n chemistry (Kareev et al., 2005; Kareev, Lebedkin, Popov et al., 2006; Kareev, Lebedkin, Miller et al., 2006; Popov et al., 2007). A member of this set of isomers, the title compound, (I), has been prepared and we report its crystal structure here. A lower-quality structure (C—C su's 0.004–0.005 Å) of the same molecule, as a toluene solvate, has recently been reported (Goryunkov et al., 2007).

The structure of (I), Figs. 1 and 2, comprises an idealized I_h C₆₀ core with eight sp³ carbon atoms at positions 1, 6, 11, 16, 18, 24, 27, and 36 (Powell et al., 2002), each of which is attached to a CF₃ group. The core sp³ carbon atoms are not adjacent to one another. The CF₃ groups are arranged on a para-para-para-meta-para-meta-para ribbon of edge-sharing C₆(CF₃)₂ hexagons (i.e., a p³mpmp overall addition pattern; see Schlegel diagram in Fig. 3). Note that the shared edges in each ribbon of hexagons are C(sp³)-C(sp²) bonds (e.g., C16—C17, C4—C18, etc.), not C(sp²)-C(sp²) bonds. Thus, any pair of adjacent hexagons along the ribbon have a common CF₃ group. As in all other published structures of fullerene(CF₃)_n compounds, there are F···F intramolecular contacts between pairs of neighboring CF₃ groups that range from 2.544 (2) to 2.641 (2) Å.

Four of the shortest cage C—C bonds in (I) are C4—C5 1.344 (3) Å, C9—C10 1.368 (3) Å, C17—C37 1.355 (3) Å, and C25—C26 1.361 (3) Å. All four are significantly shorter than the shortest C—C bond in the most precise structure of empty C₆₀ reported to date (C₆₀^.Pt(octaethylporphyrin)), which is 1.379 (3) Å (Olmstead et al., 2003). More importantly, these bonds are pentagon-hexagon junctions, and the shortest pent-hex junction in C₆₀^.Pt(OEP) is 1.440 (3) Å (the longest pent-hex junction in C₆₀^.Pt(OEP) is 1.461 (3) Å); OEP is octaethylporphyrin).

Related literature top

For related literature, see: Goryunkov et al. (2007); Kareev et al. (2005); Kareev, Lebedkin, Miller et al. (2006); Kareev, Lebedkin, Popov et al. (2006); Olmstead et al. (2003); Popov et al. (2007); Powell et al. (2002).

Experimental top

The synthesis of (I) was carried out by heating C₆₀ in a stream of CF₃I at 460 °C as previously described (Popov et al., 2007). Crystals of the HPLC-purified compound were grown by slow evaporation of a saturated deuterochloroform solution.

Structure description top

Computing details top

Data collection: APEX2 (Bruker, 2000); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top

	Fig. 1. The molecular structure of (I). Displacement ellipsoids are shown at the 50% probability level.
	Fig. 2. The molecular structure of (I) showing the numbering scheme. Displacement ellipsoids are shown at the 50% probability level for selected atoms.
	Fig. 3. Schlegel diagram of (I) showing the location of the CF₃ groups as black circles, the IUPAC lowest-locant numbers for the cage carbon atoms to which they are attached, and the ribbons or loops of meta- and para-C₆(CF₃)₂ edge-sharing hexagons (meta-C₆(CF₃)₂ hexagons are indicated by the letter m).

1,6,11,16,18,24,27,36-Octakis(trifluoromethyl)-1,6,11,16,18,24,27,36- octahydro(C₆₀—I_h)[5,6]fullerene deuterochloroform solvate top

Crystal data top

C₆₈F₂₄·CDCl₃	F(000) = 2728
M_r = 1393.05	D_x = 2.055 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 999 reflections
a = 14.5346 (6) Å	θ = 1.7–32.6°
b = 15.5805 (7) Å	µ = 0.36 mm⁻¹
c = 20.1746 (9) Å	T = 100 K
β = 99.821 (2)°	Plate, red
V = 4501.7 (3) Å³	0.34 × 0.20 × 0.05 mm
Z = 4

Data collection top

Bruker Kappa APEXII diffractometer	16373 independent reflections
Radiation source: fine-focus sealed tube	10149 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
φ and ω scans	θ_max = 32.6°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −21→20
T_min = 0.888, T_max = 0.982	k = −21→23
99651 measured reflections	l = −30→30

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.054	Secondary atom site location: difference Fourier map
wR(F²) = 0.150	w = 1/[σ²(F_o²) + (0.0671P)² + 3.3603P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
16373 reflections	Δρ_max = 0.81 e Å⁻³
865 parameters	Δρ_min = −1.31 e Å⁻³

Crystal data top

C₆₈F₂₄·CDCl₃	V = 4501.7 (3) Å³
M_r = 1393.05	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 14.5346 (6) Å	µ = 0.36 mm⁻¹
b = 15.5805 (7) Å	T = 100 K
c = 20.1746 (9) Å	0.34 × 0.20 × 0.05 mm
β = 99.821 (2)°

Data collection top

Bruker Kappa APEXII diffractometer	16373 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2000)	10149 reflections with I > 2σ(I)
T_min = 0.888, T_max = 0.982	R_int = 0.058
99651 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.054	865 parameters
wR(F²) = 0.150	0 restraints
S = 1.03	Δρ_max = 0.81 e Å⁻³
16373 reflections	Δρ_min = −1.31 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	U_iso*/U_eq
C1	0.22954 (14)	0.51270 (13)	0.71157 (10)	0.0119 (4)
C2	0.31195 (13)	0.47443 (13)	0.75999 (10)	0.0122 (4)
C3	0.37706 (14)	0.43914 (13)	0.72152 (10)	0.0120 (4)
C4	0.33256 (14)	0.44155 (13)	0.65064 (10)	0.0124 (4)
C5	0.24620 (14)	0.47497 (13)	0.64361 (10)	0.0122 (4)
C6	0.16767 (14)	0.45221 (13)	0.58603 (10)	0.0122 (4)
C7	0.08260 (13)	0.42002 (12)	0.61501 (10)	0.0116 (4)
C8	0.06967 (13)	0.43661 (12)	0.67850 (10)	0.0119 (4)
C9	0.14044 (13)	0.47654 (12)	0.72942 (10)	0.0118 (4)
C10	0.13275 (14)	0.44108 (13)	0.79026 (10)	0.0119 (4)
C11	0.21231 (14)	0.43500 (13)	0.84895 (10)	0.0126 (4)
C12	0.30475 (14)	0.44021 (13)	0.82144 (10)	0.0126 (4)
C13	0.36336 (14)	0.37005 (13)	0.84673 (10)	0.0131 (4)
C14	0.43056 (14)	0.33913 (13)	0.81079 (10)	0.0131 (4)
C15	0.43964 (13)	0.37626 (13)	0.74774 (10)	0.0125 (4)
C16	0.48223 (14)	0.31089 (13)	0.70478 (10)	0.0138 (4)
C17	0.42311 (14)	0.30696 (13)	0.63493 (10)	0.0132 (4)
C18	0.36765 (13)	0.38418 (13)	0.59986 (10)	0.0125 (4)
C19	0.28377 (14)	0.33905 (13)	0.55855 (10)	0.0131 (4)
C20	0.19455 (14)	0.36916 (13)	0.55264 (10)	0.0129 (4)
C21	0.11890 (14)	0.30888 (13)	0.54595 (10)	0.0130 (4)
C22	0.04858 (14)	0.33898 (13)	0.58249 (10)	0.0127 (4)
C23	−0.00237 (13)	0.28128 (13)	0.61350 (10)	0.0132 (4)
C24	−0.03997 (13)	0.30422 (13)	0.67805 (10)	0.0120 (4)
C25	0.01605 (13)	0.37749 (13)	0.71364 (10)	0.0119 (4)
C26	0.05413 (14)	0.37925 (13)	0.78009 (10)	0.0121 (4)
C27	0.04584 (14)	0.30608 (13)	0.82818 (10)	0.0132 (4)
C28	0.14437 (14)	0.28551 (13)	0.86735 (10)	0.0133 (4)
C29	0.21721 (14)	0.34206 (13)	0.87615 (10)	0.0137 (4)
C30	0.31094 (14)	0.31034 (14)	0.88086 (10)	0.0138 (4)
C31	0.32936 (14)	0.22274 (14)	0.87955 (10)	0.0149 (4)
C32	0.39982 (14)	0.19058 (14)	0.84261 (10)	0.0149 (4)
C33	0.44895 (14)	0.24785 (13)	0.80846 (10)	0.0142 (4)
C34	0.46981 (13)	0.22705 (13)	0.74309 (10)	0.0136 (4)
C35	0.43829 (14)	0.15167 (13)	0.71288 (11)	0.0148 (4)
C36	0.40829 (14)	0.14344 (13)	0.63628 (11)	0.0152 (4)
C37	0.38769 (14)	0.23243 (13)	0.60682 (10)	0.0135 (4)
C38	0.30168 (14)	0.24885 (13)	0.55832 (10)	0.0137 (4)
C39	0.23019 (15)	0.19004 (13)	0.54784 (10)	0.0143 (4)
C40	0.13594 (14)	0.22051 (13)	0.54197 (10)	0.0136 (4)
C41	0.08435 (14)	0.16073 (13)	0.57607 (10)	0.0139 (4)
C42	0.01719 (14)	0.19157 (13)	0.61230 (10)	0.0137 (4)
C43	0.00952 (14)	0.15484 (13)	0.67717 (10)	0.0131 (4)
C44	−0.01543 (13)	0.22188 (13)	0.71973 (10)	0.0128 (4)
C45	0.02385 (14)	0.22293 (13)	0.78671 (10)	0.0132 (4)
C46	0.08854 (14)	0.15709 (13)	0.81393 (10)	0.0141 (4)
C47	0.16171 (14)	0.19491 (13)	0.86302 (10)	0.0143 (4)
C48	0.25307 (15)	0.16337 (14)	0.87047 (10)	0.0155 (4)
C49	0.27510 (15)	0.09381 (13)	0.82797 (11)	0.0159 (4)
C50	0.36617 (14)	0.11167 (13)	0.81069 (11)	0.0153 (4)
C52	0.31046 (15)	0.05660 (13)	0.69644 (11)	0.0160 (4)
C51	0.38363 (14)	0.09373 (13)	0.74610 (11)	0.0159 (4)
C53	0.31764 (15)	0.09096 (13)	0.63196 (11)	0.0162 (4)
C54	0.23746 (15)	0.10979 (13)	0.58680 (10)	0.0153 (4)
C55	0.14711 (15)	0.09228 (13)	0.60372 (11)	0.0154 (4)
C56	0.13946 (15)	0.05629 (13)	0.66603 (11)	0.0156 (4)
C57	0.06917 (14)	0.08813 (13)	0.70320 (10)	0.0141 (4)
C58	0.10952 (15)	0.08903 (13)	0.77358 (11)	0.0151 (4)
C59	0.20490 (15)	0.05780 (13)	0.78024 (11)	0.0156 (4)
C60	0.22246 (15)	0.03785 (13)	0.71339 (11)	0.0158 (4)
C61	0.23418 (15)	0.61124 (13)	0.70994 (11)	0.0160 (4)
C62	0.13984 (15)	0.52462 (14)	0.53379 (11)	0.0169 (4)
C63	0.20979 (15)	0.50065 (14)	0.90533 (11)	0.0169 (4)
C64	0.58647 (14)	0.33052 (14)	0.70584 (11)	0.0166 (4)
C65	0.42188 (15)	0.43631 (14)	0.55408 (11)	0.0177 (4)
C66	−0.14472 (14)	0.32420 (13)	0.66104 (10)	0.0135 (4)
C67	−0.02525 (15)	0.32071 (14)	0.87504 (10)	0.0155 (4)
C68	0.47841 (15)	0.09581 (14)	0.60102 (12)	0.0188 (4)
C69	0.68341 (18)	0.30051 (17)	0.98786 (14)	0.0290 (5)
D691	0.6858	0.3219	1.0349	0.035*
Cl1	0.62123 (6)	0.37552 (5)	0.93253 (4)	0.0537 (2)
Cl2	0.62609 (6)	0.20279 (5)	0.98064 (6)	0.0564 (2)
Cl3	0.79819 (5)	0.29047 (5)	0.97296 (4)	0.04089 (18)
F611	0.31448 (10)	0.63788 (8)	0.69331 (8)	0.0255 (3)
F612	0.22776 (10)	0.64561 (8)	0.76941 (7)	0.0252 (3)
F613	0.16494 (10)	0.64384 (9)	0.66515 (7)	0.0264 (3)
F621	0.21276 (10)	0.57120 (9)	0.52435 (7)	0.0278 (3)
F622	0.07730 (10)	0.57817 (9)	0.55216 (7)	0.0279 (3)
F623	0.10111 (11)	0.49154 (9)	0.47448 (7)	0.0278 (3)
F631	0.28373 (10)	0.49032 (9)	0.95411 (7)	0.0271 (3)
F632	0.13408 (11)	0.49217 (11)	0.93358 (8)	0.0332 (4)
F633	0.21160 (11)	0.58085 (9)	0.88351 (7)	0.0271 (3)
F641	0.62551 (9)	0.27344 (9)	0.67054 (8)	0.0265 (3)
F642	0.63347 (9)	0.32981 (10)	0.76843 (7)	0.0282 (3)
F643	0.59864 (9)	0.40800 (9)	0.68020 (8)	0.0267 (3)
F651	0.46681 (12)	0.38468 (10)	0.51812 (8)	0.0378 (4)
F652	0.48295 (10)	0.48998 (10)	0.58856 (8)	0.0323 (4)
F653	0.36383 (10)	0.48368 (10)	0.51031 (7)	0.0279 (3)
F661	−0.15923 (9)	0.39304 (8)	0.62046 (7)	0.0201 (3)
F662	−0.18186 (8)	0.34158 (9)	0.71544 (6)	0.0182 (3)
F663	−0.19178 (8)	0.25846 (8)	0.62891 (6)	0.0186 (3)
F671	−0.00442 (10)	0.38995 (9)	0.91402 (7)	0.0227 (3)
F672	−0.02650 (9)	0.25319 (9)	0.91616 (6)	0.0193 (3)
F673	−0.11104 (9)	0.33158 (9)	0.84072 (6)	0.0213 (3)
F681	0.49604 (9)	0.01739 (9)	0.62755 (7)	0.0248 (3)
F682	0.56018 (9)	0.13640 (9)	0.60644 (8)	0.0271 (3)
F683	0.44498 (10)	0.08603 (9)	0.53539 (7)	0.0259 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0119 (9)	0.0102 (8)	0.0136 (9)	−0.0004 (7)	0.0017 (7)	0.0007 (7)
C2	0.0099 (8)	0.0116 (9)	0.0146 (9)	−0.0026 (7)	0.0002 (7)	−0.0015 (7)
C3	0.0111 (9)	0.0114 (9)	0.0133 (9)	−0.0035 (7)	0.0016 (7)	0.0012 (7)
C4	0.0127 (9)	0.0109 (9)	0.0136 (9)	−0.0034 (7)	0.0023 (7)	0.0011 (7)
C5	0.0120 (9)	0.0114 (9)	0.0136 (9)	−0.0012 (7)	0.0032 (7)	0.0030 (7)
C6	0.0124 (9)	0.0127 (9)	0.0116 (9)	−0.0013 (7)	0.0018 (7)	0.0028 (7)
C7	0.0093 (8)	0.0113 (9)	0.0135 (9)	0.0008 (7)	−0.0004 (7)	0.0038 (7)
C8	0.0095 (8)	0.0107 (9)	0.0149 (9)	0.0014 (7)	0.0002 (7)	0.0015 (7)
C9	0.0099 (8)	0.0104 (9)	0.0149 (9)	0.0005 (7)	0.0012 (7)	−0.0002 (7)
C10	0.0114 (9)	0.0118 (9)	0.0123 (9)	−0.0001 (7)	0.0016 (7)	−0.0021 (7)
C11	0.0125 (9)	0.0138 (9)	0.0113 (8)	−0.0018 (7)	0.0012 (7)	−0.0017 (7)
C12	0.0117 (9)	0.0116 (9)	0.0140 (9)	−0.0037 (7)	0.0006 (7)	−0.0038 (7)
C13	0.0127 (9)	0.0141 (9)	0.0115 (9)	−0.0028 (7)	−0.0008 (7)	−0.0005 (7)
C14	0.0097 (9)	0.0138 (9)	0.0144 (9)	−0.0015 (7)	−0.0016 (7)	0.0001 (7)
C15	0.0080 (8)	0.0138 (9)	0.0154 (9)	−0.0027 (7)	0.0011 (7)	−0.0005 (7)
C16	0.0103 (9)	0.0138 (9)	0.0169 (9)	−0.0014 (7)	0.0010 (7)	0.0004 (7)
C17	0.0103 (9)	0.0152 (9)	0.0149 (9)	−0.0006 (7)	0.0039 (7)	0.0006 (7)
C18	0.0105 (9)	0.0149 (9)	0.0127 (9)	−0.0006 (7)	0.0038 (7)	0.0018 (7)
C19	0.0143 (9)	0.0169 (10)	0.0090 (8)	−0.0017 (7)	0.0041 (7)	0.0006 (7)
C20	0.0154 (9)	0.0142 (9)	0.0089 (8)	−0.0008 (7)	0.0019 (7)	0.0014 (7)
C21	0.0120 (9)	0.0185 (10)	0.0083 (8)	−0.0011 (7)	0.0007 (7)	−0.0002 (7)
C22	0.0107 (9)	0.0169 (10)	0.0096 (8)	0.0002 (7)	−0.0010 (7)	0.0007 (7)
C23	0.0090 (8)	0.0169 (10)	0.0124 (9)	−0.0008 (7)	−0.0015 (7)	0.0003 (7)
C24	0.0085 (8)	0.0126 (9)	0.0148 (9)	−0.0016 (7)	0.0016 (7)	0.0011 (7)
C25	0.0096 (8)	0.0125 (9)	0.0138 (9)	−0.0005 (7)	0.0030 (7)	0.0004 (7)
C26	0.0108 (8)	0.0137 (9)	0.0127 (9)	0.0008 (7)	0.0041 (7)	−0.0009 (7)
C27	0.0115 (9)	0.0166 (9)	0.0116 (9)	−0.0011 (7)	0.0027 (7)	0.0014 (7)
C28	0.0146 (9)	0.0171 (10)	0.0085 (8)	−0.0012 (7)	0.0029 (7)	0.0014 (7)
C29	0.0157 (9)	0.0164 (10)	0.0086 (8)	−0.0010 (8)	0.0011 (7)	−0.0005 (7)
C30	0.0134 (9)	0.0180 (10)	0.0087 (8)	−0.0018 (7)	−0.0014 (7)	0.0002 (7)
C31	0.0141 (9)	0.0180 (10)	0.0111 (9)	−0.0003 (8)	−0.0017 (7)	0.0031 (7)
C32	0.0124 (9)	0.0158 (10)	0.0149 (9)	0.0025 (7)	−0.0021 (7)	0.0038 (7)
C33	0.0098 (9)	0.0157 (9)	0.0153 (9)	0.0005 (7)	−0.0030 (7)	0.0023 (7)
C34	0.0073 (8)	0.0148 (9)	0.0181 (9)	0.0021 (7)	0.0002 (7)	0.0031 (8)
C35	0.0116 (9)	0.0143 (9)	0.0181 (10)	0.0033 (7)	0.0010 (7)	0.0010 (8)
C36	0.0131 (9)	0.0130 (9)	0.0194 (10)	0.0011 (7)	0.0027 (8)	−0.0015 (8)
C37	0.0108 (9)	0.0160 (9)	0.0145 (9)	0.0003 (7)	0.0043 (7)	−0.0005 (7)
C38	0.0136 (9)	0.0169 (9)	0.0110 (8)	0.0004 (7)	0.0037 (7)	−0.0013 (7)
C39	0.0156 (9)	0.0158 (10)	0.0121 (9)	−0.0002 (7)	0.0037 (7)	−0.0045 (7)
C40	0.0138 (9)	0.0170 (10)	0.0097 (8)	−0.0017 (7)	0.0013 (7)	−0.0020 (7)
C41	0.0117 (9)	0.0159 (9)	0.0132 (9)	−0.0036 (7)	−0.0006 (7)	−0.0031 (7)
C42	0.0099 (9)	0.0156 (9)	0.0147 (9)	−0.0034 (7)	−0.0003 (7)	−0.0033 (7)
C43	0.0101 (9)	0.0129 (9)	0.0159 (9)	−0.0040 (7)	0.0006 (7)	−0.0002 (7)
C44	0.0092 (8)	0.0136 (9)	0.0161 (9)	−0.0024 (7)	0.0034 (7)	0.0002 (7)
C45	0.0111 (9)	0.0131 (9)	0.0158 (9)	−0.0033 (7)	0.0038 (7)	0.0009 (7)
C46	0.0133 (9)	0.0142 (9)	0.0149 (9)	−0.0033 (7)	0.0031 (7)	0.0031 (7)
C47	0.0152 (9)	0.0163 (10)	0.0118 (9)	−0.0023 (8)	0.0034 (7)	0.0045 (7)
C48	0.0166 (10)	0.0171 (10)	0.0118 (9)	0.0006 (8)	0.0000 (7)	0.0067 (7)
C49	0.0171 (10)	0.0128 (9)	0.0168 (10)	0.0003 (7)	−0.0001 (8)	0.0057 (8)
C50	0.0139 (9)	0.0122 (9)	0.0184 (10)	0.0022 (7)	−0.0013 (8)	0.0057 (8)
C52	0.0159 (10)	0.0101 (9)	0.0214 (10)	0.0014 (7)	0.0015 (8)	−0.0014 (8)
C51	0.0136 (9)	0.0111 (9)	0.0220 (10)	0.0030 (7)	0.0004 (8)	0.0022 (8)
C53	0.0157 (10)	0.0109 (9)	0.0224 (10)	0.0006 (7)	0.0040 (8)	−0.0039 (8)
C54	0.0160 (10)	0.0137 (9)	0.0166 (9)	−0.0002 (7)	0.0039 (8)	−0.0049 (7)
C55	0.0152 (9)	0.0115 (9)	0.0184 (10)	−0.0021 (7)	−0.0005 (8)	−0.0043 (7)
C56	0.0162 (10)	0.0095 (9)	0.0207 (10)	−0.0030 (7)	0.0020 (8)	−0.0025 (8)
C57	0.0131 (9)	0.0106 (9)	0.0182 (10)	−0.0041 (7)	0.0017 (7)	−0.0005 (7)
C58	0.0160 (10)	0.0111 (9)	0.0181 (10)	−0.0025 (7)	0.0029 (8)	0.0040 (7)
C59	0.0153 (10)	0.0109 (9)	0.0202 (10)	−0.0007 (7)	0.0019 (8)	0.0047 (8)
C60	0.0178 (10)	0.0081 (9)	0.0211 (10)	−0.0008 (7)	0.0021 (8)	0.0000 (7)
C61	0.0149 (9)	0.0125 (9)	0.0214 (10)	−0.0003 (7)	0.0051 (8)	0.0010 (8)
C62	0.0153 (10)	0.0186 (10)	0.0162 (10)	−0.0014 (8)	0.0008 (8)	0.0056 (8)
C63	0.0169 (10)	0.0181 (10)	0.0158 (9)	−0.0022 (8)	0.0028 (8)	−0.0030 (8)
C64	0.0117 (9)	0.0157 (10)	0.0228 (10)	−0.0001 (7)	0.0040 (8)	−0.0005 (8)
C65	0.0155 (10)	0.0189 (10)	0.0196 (10)	−0.0013 (8)	0.0060 (8)	0.0025 (8)
C66	0.0101 (9)	0.0152 (9)	0.0147 (9)	−0.0012 (7)	0.0012 (7)	0.0000 (7)
C67	0.0159 (10)	0.0178 (10)	0.0131 (9)	−0.0021 (8)	0.0031 (7)	0.0013 (8)
C68	0.0162 (10)	0.0161 (10)	0.0247 (11)	0.0013 (8)	0.0049 (8)	−0.0029 (8)
C69	0.0256 (12)	0.0289 (13)	0.0322 (13)	0.0020 (10)	0.0040 (10)	0.0001 (11)
Cl1	0.0641 (5)	0.0305 (4)	0.0525 (5)	0.0121 (3)	−0.0302 (4)	−0.0050 (3)
Cl2	0.0327 (4)	0.0348 (4)	0.1032 (8)	−0.0068 (3)	0.0158 (4)	0.0022 (4)
Cl3	0.0261 (3)	0.0569 (5)	0.0438 (4)	−0.0025 (3)	0.0176 (3)	0.0046 (3)
F611	0.0221 (7)	0.0147 (6)	0.0430 (8)	−0.0057 (5)	0.0150 (6)	0.0004 (6)
F612	0.0369 (8)	0.0144 (6)	0.0260 (7)	−0.0014 (6)	0.0104 (6)	−0.0060 (5)
F613	0.0263 (7)	0.0165 (6)	0.0343 (8)	0.0046 (5)	−0.0013 (6)	0.0071 (6)
F621	0.0191 (7)	0.0282 (8)	0.0344 (8)	−0.0077 (6)	−0.0001 (6)	0.0177 (6)
F622	0.0296 (8)	0.0238 (7)	0.0313 (8)	0.0124 (6)	0.0080 (6)	0.0124 (6)
F623	0.0379 (8)	0.0251 (7)	0.0164 (6)	−0.0038 (6)	−0.0074 (6)	0.0063 (5)
F631	0.0291 (8)	0.0303 (8)	0.0177 (6)	0.0015 (6)	−0.0075 (6)	−0.0080 (6)
F632	0.0291 (8)	0.0420 (9)	0.0328 (8)	−0.0133 (7)	0.0182 (7)	−0.0217 (7)
F633	0.0440 (9)	0.0151 (6)	0.0218 (7)	0.0016 (6)	0.0045 (6)	−0.0037 (5)
F641	0.0128 (6)	0.0263 (7)	0.0421 (8)	−0.0010 (5)	0.0091 (6)	−0.0121 (6)
F642	0.0140 (6)	0.0456 (9)	0.0231 (7)	−0.0055 (6)	−0.0023 (5)	0.0012 (6)
F643	0.0161 (6)	0.0197 (7)	0.0451 (9)	−0.0042 (5)	0.0071 (6)	0.0073 (6)
F651	0.0480 (10)	0.0303 (8)	0.0457 (10)	0.0067 (7)	0.0385 (8)	0.0066 (7)
F652	0.0276 (8)	0.0387 (9)	0.0296 (8)	−0.0201 (7)	0.0017 (6)	0.0085 (7)
F653	0.0258 (7)	0.0323 (8)	0.0256 (7)	−0.0016 (6)	0.0042 (6)	0.0164 (6)
F661	0.0151 (6)	0.0218 (7)	0.0227 (7)	0.0026 (5)	0.0008 (5)	0.0084 (5)
F662	0.0120 (6)	0.0260 (7)	0.0169 (6)	0.0010 (5)	0.0039 (5)	−0.0018 (5)
F663	0.0114 (6)	0.0203 (6)	0.0226 (6)	−0.0046 (5)	−0.0008 (5)	−0.0043 (5)
F671	0.0252 (7)	0.0234 (7)	0.0219 (7)	−0.0044 (6)	0.0109 (5)	−0.0073 (5)
F672	0.0182 (6)	0.0238 (7)	0.0171 (6)	−0.0014 (5)	0.0069 (5)	0.0055 (5)
F673	0.0125 (6)	0.0342 (8)	0.0173 (6)	0.0025 (5)	0.0028 (5)	0.0042 (5)
F681	0.0211 (7)	0.0169 (6)	0.0360 (8)	0.0066 (5)	0.0036 (6)	−0.0026 (6)
F682	0.0149 (6)	0.0264 (7)	0.0425 (9)	−0.0024 (5)	0.0120 (6)	−0.0114 (6)
F683	0.0256 (7)	0.0288 (8)	0.0237 (7)	0.0048 (6)	0.0053 (6)	−0.0076 (6)

Geometric parameters (Å, º) top

C1—C9	1.511 (3)	C35—C51	1.441 (3)
C1—C2	1.532 (3)	C35—C36	1.538 (3)
C1—C61	1.537 (3)	C36—C37	1.518 (3)
C1—C5	1.548 (3)	C36—C68	1.531 (3)
C2—C12	1.370 (3)	C36—C53	1.540 (3)
C2—C3	1.432 (3)	C37—C38	1.473 (3)
C3—C15	1.379 (3)	C38—C39	1.374 (3)
C3—C4	1.466 (3)	C39—C40	1.436 (3)
C4—C5	1.344 (3)	C39—C54	1.471 (3)
C4—C18	1.512 (3)	C40—C41	1.442 (3)
C5—C6	1.525 (3)	C41—C42	1.400 (3)
C6—C7	1.539 (3)	C41—C55	1.452 (3)
C6—C20	1.540 (3)	C42—C43	1.450 (3)
C6—C62	1.550 (3)	C43—C57	1.397 (3)
C7—C8	1.351 (3)	C43—C44	1.437 (3)
C7—C22	1.469 (3)	C44—C45	1.375 (3)
C8—C9	1.463 (3)	C45—C46	1.436 (3)
C8—C25	1.465 (3)	C46—C58	1.402 (3)
C9—C10	1.368 (3)	C46—C47	1.449 (3)
C10—C26	1.482 (3)	C47—C48	1.400 (3)
C10—C11	1.510 (3)	C48—C49	1.451 (3)
C11—C63	1.535 (3)	C49—C59	1.396 (3)
C11—C12	1.541 (3)	C49—C50	1.452 (3)
C11—C29	1.546 (3)	C50—C51	1.398 (3)
C12—C13	1.426 (3)	C52—C60	1.410 (3)
C13—C14	1.398 (3)	C52—C53	1.427 (3)
C13—C30	1.449 (3)	C52—C51	1.451 (3)
C14—C15	1.424 (3)	C53—C54	1.383 (3)
C14—C33	1.449 (3)	C54—C55	1.438 (3)
C15—C16	1.535 (3)	C55—C56	1.398 (3)
C16—C17	1.521 (3)	C56—C60	1.434 (3)
C16—C64	1.542 (3)	C56—C57	1.454 (3)
C16—C34	1.544 (3)	C57—C58	1.441 (3)
C17—C37	1.355 (3)	C58—C59	1.454 (3)
C17—C18	1.550 (3)	C59—C60	1.448 (3)
C18—C19	1.526 (3)	C61—F612	1.332 (2)
C18—C65	1.544 (3)	C61—F613	1.333 (2)
C19—C20	1.365 (3)	C61—F611	1.334 (2)
C19—C38	1.429 (3)	C62—F621	1.325 (2)
C20—C21	1.435 (3)	C62—F622	1.332 (3)
C21—C40	1.404 (3)	C62—F623	1.336 (3)
C21—C22	1.437 (3)	C63—F633	1.327 (3)
C22—C23	1.381 (3)	C63—F632	1.329 (3)
C23—C42	1.427 (3)	C63—F631	1.337 (3)
C23—C24	1.538 (3)	C64—F641	1.326 (2)
C24—C25	1.511 (3)	C64—F642	1.329 (3)
C24—C66	1.534 (3)	C64—F643	1.337 (3)
C24—C44	1.542 (3)	C65—F652	1.327 (3)
C25—C26	1.361 (3)	C65—F651	1.327 (3)
C26—C27	1.515 (3)	C65—F653	1.335 (3)
C27—C67	1.532 (3)	C66—F662	1.331 (2)
C27—C45	1.546 (3)	C66—F663	1.336 (2)
C27—C28	1.547 (3)	C66—F661	1.344 (2)
C28—C29	1.366 (3)	C67—F673	1.330 (2)
C28—C47	1.439 (3)	C67—F671	1.339 (2)
C29—C30	1.437 (3)	C67—F672	1.342 (2)
C30—C31	1.392 (3)	C68—F682	1.334 (3)
C31—C48	1.432 (3)	C68—F683	1.339 (3)
C31—C32	1.455 (3)	C68—F681	1.341 (3)
C32—C33	1.396 (3)	C69—Cl2	1.730 (3)
C32—C50	1.435 (3)	C69—Cl3	1.752 (3)
C33—C34	1.440 (3)	C69—Cl1	1.756 (3)
C34—C35	1.366 (3)

C9—C1—C2	108.16 (16)	C68—C36—C35	114.22 (17)
C9—C1—C61	114.83 (16)	C37—C36—C53	110.66 (17)
C2—C1—C61	111.72 (16)	C68—C36—C53	110.32 (17)
C9—C1—C5	109.83 (16)	C35—C36—C53	101.20 (17)
C2—C1—C5	101.17 (15)	C17—C37—C38	110.38 (18)
C61—C1—C5	110.26 (16)	C17—C37—C36	125.69 (18)
C12—C2—C3	120.04 (18)	C38—C37—C36	120.48 (18)
C12—C2—C1	123.83 (18)	C39—C38—C19	121.51 (19)
C3—C2—C1	108.72 (17)	C39—C38—C37	121.35 (19)
C15—C3—C2	121.22 (18)	C19—C38—C37	107.64 (17)
C15—C3—C4	122.99 (18)	C38—C39—C40	118.56 (19)
C2—C3—C4	107.25 (17)	C38—C39—C54	120.06 (19)
C5—C4—C3	111.20 (18)	C40—C39—C54	107.80 (18)
C5—C4—C18	125.05 (18)	C21—C40—C39	119.66 (18)
C3—C4—C18	120.14 (17)	C21—C40—C41	119.67 (18)
C4—C5—C6	123.67 (18)	C39—C40—C41	108.28 (18)
C4—C5—C1	109.75 (17)	C42—C41—C40	119.53 (19)
C6—C5—C1	123.58 (17)	C42—C41—C55	119.99 (19)
C5—C6—C7	109.37 (16)	C40—C41—C55	108.30 (18)
C5—C6—C20	108.41 (16)	C41—C42—C23	120.23 (19)
C7—C6—C20	99.94 (15)	C41—C42—C43	120.22 (19)
C5—C6—C62	115.05 (17)	C23—C42—C43	108.96 (17)
C7—C6—C62	111.23 (16)	C57—C43—C44	121.31 (18)
C20—C6—C62	111.75 (16)	C57—C43—C42	119.63 (18)
C8—C7—C22	119.81 (18)	C44—C43—C42	108.57 (17)
C8—C7—C6	123.27 (18)	C45—C44—C43	119.42 (19)
C22—C7—C6	109.96 (16)	C45—C44—C24	123.01 (18)
C7—C8—C9	123.53 (18)	C43—C44—C24	109.71 (17)
C7—C8—C25	120.66 (18)	C44—C45—C46	120.17 (19)
C9—C8—C25	107.21 (17)	C44—C45—C27	123.71 (18)
C10—C9—C8	107.64 (17)	C46—C45—C27	109.29 (17)
C10—C9—C1	124.68 (18)	C58—C46—C45	120.77 (19)
C8—C9—C1	121.32 (17)	C58—C46—C47	119.84 (19)
C9—C10—C26	108.51 (17)	C45—C46—C47	109.10 (18)
C9—C10—C11	124.05 (18)	C48—C47—C28	120.70 (19)
C26—C10—C11	122.48 (17)	C48—C47—C46	120.18 (19)
C10—C11—C63	115.30 (17)	C28—C47—C46	108.95 (18)
C10—C11—C12	108.21 (16)	C47—C48—C31	119.13 (19)
C63—C11—C12	111.37 (16)	C47—C48—C49	119.98 (19)
C10—C11—C29	108.65 (16)	C31—C48—C49	108.30 (18)
C63—C11—C29	111.50 (16)	C59—C49—C48	119.92 (19)
C12—C11—C29	100.78 (16)	C59—C49—C50	120.0 (2)
C2—C12—C13	119.29 (18)	C48—C49—C50	107.51 (18)
C2—C12—C11	123.53 (18)	C51—C50—C32	119.18 (19)
C13—C12—C11	109.58 (17)	C51—C50—C49	120.23 (19)
C14—C13—C12	120.41 (18)	C32—C50—C49	108.15 (18)
C14—C13—C30	119.73 (19)	C60—C52—C53	120.63 (19)
C12—C13—C30	109.39 (18)	C60—C52—C51	120.24 (19)
C13—C14—C15	120.20 (18)	C53—C52—C51	108.71 (18)
C13—C14—C33	120.27 (18)	C50—C51—C35	120.70 (19)
C15—C14—C33	108.90 (18)	C50—C51—C52	119.68 (19)
C3—C15—C14	118.40 (18)	C35—C51—C52	109.03 (18)
C3—C15—C16	123.91 (18)	C54—C53—C52	119.7 (2)
C14—C15—C16	110.05 (17)	C54—C53—C36	122.77 (19)
C17—C16—C15	109.35 (16)	C52—C53—C36	110.03 (18)
C17—C16—C64	114.79 (17)	C53—C54—C55	120.30 (19)
C15—C16—C64	110.52 (16)	C53—C54—C39	120.53 (19)
C17—C16—C34	109.50 (16)	C55—C54—C39	107.62 (18)
C15—C16—C34	100.71 (16)	C56—C55—C54	120.36 (19)
C64—C16—C34	111.06 (16)	C56—C55—C41	119.94 (19)
C37—C17—C16	122.44 (18)	C54—C55—C41	107.99 (18)
C37—C17—C18	110.07 (17)	C55—C56—C60	119.50 (19)
C16—C17—C18	124.00 (17)	C55—C56—C57	119.84 (19)
C4—C18—C19	108.18 (16)	C60—C56—C57	108.06 (18)
C4—C18—C65	111.10 (17)	C43—C57—C58	119.03 (19)
C19—C18—C65	110.96 (16)	C43—C57—C56	120.37 (19)
C4—C18—C17	111.02 (16)	C58—C57—C56	107.93 (18)
C19—C18—C17	101.33 (16)	C46—C58—C57	119.17 (19)
C65—C18—C17	113.74 (16)	C46—C58—C59	119.87 (19)
C20—C19—C38	120.56 (19)	C57—C58—C59	108.02 (18)
C20—C19—C18	123.22 (18)	C49—C59—C60	120.29 (19)
C38—C19—C18	109.02 (17)	C49—C59—C58	120.18 (19)
C19—C20—C21	118.99 (19)	C60—C59—C58	107.61 (18)
C19—C20—C6	123.97 (18)	C52—C60—C56	119.45 (19)
C21—C20—C6	110.10 (17)	C52—C60—C59	119.52 (19)
C40—C21—C20	120.50 (18)	C56—C60—C59	108.39 (18)
C40—C21—C22	119.83 (18)	F612—C61—F613	107.26 (17)
C20—C21—C22	109.81 (18)	F612—C61—F611	107.46 (17)
C23—C22—C21	120.22 (19)	F613—C61—F611	107.62 (17)
C23—C22—C7	121.54 (18)	F612—C61—C1	111.86 (17)
C21—C22—C7	107.15 (17)	F613—C61—C1	111.36 (17)
C22—C23—C42	120.41 (19)	F611—C61—C1	111.06 (17)
C22—C23—C24	121.86 (18)	F621—C62—F622	107.31 (18)
C42—C23—C24	110.04 (17)	F621—C62—F623	107.92 (17)
C25—C24—C66	112.75 (16)	F622—C62—F623	106.71 (17)
C25—C24—C23	109.74 (16)	F621—C62—C6	111.97 (17)
C66—C24—C23	109.89 (16)	F622—C62—C6	112.22 (17)
C25—C24—C44	108.28 (16)	F623—C62—C6	110.46 (17)
C66—C24—C44	114.77 (16)	F633—C63—F632	107.49 (18)
C23—C24—C44	100.71 (16)	F633—C63—F631	107.37 (17)
C26—C25—C8	107.67 (17)	F632—C63—F631	107.01 (18)
C26—C25—C24	125.40 (18)	F633—C63—C11	112.18 (17)
C8—C25—C24	122.21 (17)	F632—C63—C11	112.20 (17)
C25—C26—C10	108.90 (17)	F631—C63—C11	110.33 (17)
C25—C26—C27	123.53 (18)	F641—C64—F642	107.87 (17)
C10—C26—C27	122.97 (17)	F641—C64—F643	107.51 (18)
C26—C27—C67	114.77 (17)	F642—C64—F643	107.14 (18)
C26—C27—C45	108.41 (16)	F641—C64—C16	111.64 (17)
C67—C27—C45	111.08 (16)	F642—C64—C16	110.86 (17)
C26—C27—C28	108.38 (16)	F643—C64—C16	111.61 (17)
C67—C27—C28	112.26 (16)	F652—C65—F651	108.73 (18)
C45—C27—C28	101.00 (16)	F652—C65—F653	106.81 (18)
C29—C28—C47	120.06 (19)	F651—C65—F653	106.74 (18)
C29—C28—C27	124.23 (18)	F652—C65—C18	112.46 (18)
C47—C28—C27	109.19 (17)	F651—C65—C18	110.93 (18)
C28—C29—C30	119.46 (19)	F653—C65—C18	110.92 (17)
C28—C29—C11	124.79 (18)	F662—C66—F663	108.05 (16)
C30—C29—C11	109.35 (17)	F662—C66—F661	107.23 (16)
C31—C30—C29	121.28 (19)	F663—C66—F661	107.58 (16)
C31—C30—C13	120.15 (19)	F662—C66—C24	112.55 (16)
C29—C30—C13	108.49 (18)	F663—C66—C24	111.05 (16)
C30—C31—C48	119.26 (19)	F661—C66—C24	110.17 (16)
C30—C31—C32	120.13 (19)	F673—C67—F671	107.52 (18)
C48—C31—C32	108.03 (18)	F673—C67—F672	108.14 (17)
C33—C32—C50	119.37 (19)	F671—C67—F672	107.09 (16)
C33—C32—C31	119.78 (19)	F673—C67—C27	111.66 (16)
C50—C32—C31	108.01 (18)	F671—C67—C27	111.94 (17)
C32—C33—C34	120.90 (19)	F672—C67—C27	110.29 (17)
C32—C33—C14	119.91 (19)	F682—C68—F683	107.64 (18)
C34—C33—C14	108.63 (18)	F682—C68—F681	107.00 (18)
C35—C34—C33	119.69 (19)	F683—C68—F681	107.66 (18)
C35—C34—C16	124.27 (19)	F682—C68—C36	112.74 (18)
C33—C34—C16	109.21 (17)	F683—C68—C36	110.89 (18)
C34—C35—C51	120.05 (19)	F681—C68—C36	110.69 (18)
C34—C35—C36	122.42 (19)	Cl2—C69—Cl3	111.47 (15)
C51—C35—C36	109.31 (18)	Cl2—C69—Cl1	110.11 (15)
C37—C36—C68	111.31 (17)	Cl3—C69—Cl1	110.62 (15)
C37—C36—C35	108.69 (17)

Experimental details

Crystal data
Chemical formula	C₆₈F₂₄·CDCl₃
M_r	1393.05
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	14.5346 (6), 15.5805 (7), 20.1746 (9)
β (°)	99.821 (2)
V (Å³)	4501.7 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.36
Crystal size (mm)	0.34 × 0.20 × 0.05

Data collection
Diffractometer	Bruker Kappa APEXII
Absorption correction	Multi-scan (SADABS; Bruker, 2000)
T_min, T_max	0.888, 0.982
No. of measured, independent and observed [I > 2σ(I)] reflections	99651, 16373, 10149
R_int	0.058
(sin θ/λ)_max (Å⁻¹)	0.758

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.054, 0.150, 1.03
No. of reflections	16373
No. of parameters	865
Δρ_max, Δρ_min (e Å⁻³)	0.81, −1.31

Computer programs: APEX2 (Bruker, 2000), APEX2, SHELXTL (Bruker, 2000), SHELXTL.

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