Strategies for the structure determination of endohedral fullerenes applied to the example of Ba@C74·Co(octaethylporphyrin)·2C6H6

Friese, K.; Panthöfer, M.; Wu, G.; Jansen, M.

doi:10.1107/S010876810401451X

Strategies for the structure determination of endohedral fullerenes applied to the example of Ba@C₇₄·Co(octaethylporphyrin)·2C₆H₆

K. Friese, M. Panthöfer, G. Wu and M. Jansen

The structure determination of endohedral fullerenes is complicated because of the high degree of disorder which may affect the different structural components, e.g. the endohedral atom/molecule, the fullerene cage and solvent molecules. Even worse, the data-to-parameter ratio and, in particular, the scattering power is low. Different strategies are employed to deal with these problems. The observed fraction of the reciprocal lattice may be increased by means of synchrotron diffraction studies. The number of parameters may be reduced by applying rigid-body refinement strategies and by restricting the displacement parameters in the framework of the TLS approach. In the first section, we will give a short overview of the structure determinations of endohedral fullerenes from single-crystal data and discuss the severe problems one may encounter. Then we will give an example of a successful structure analysis of a metal-containing endohedral fullerene, i.e. Ba@C₇₄·Co(OEP)·2C₆H₆ (OEP = octaethylporphyrin). Several strategies of refinement, beyond the black box level, have been checked and compared, e.g. TLS, split-atom models, twin and single crystal models, anharmonic displacement parameters, and rigid-body models.

Keywords: endohedral fullerenes; disorder; reciprocal lattice; rigid-body refinement; synchrotron radiation.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810401451X/na5020sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S010876810401451X/na5020sup2.fcf Supplementary material

CCDC reference: 255078

Computing details top

Program(s) used to solve structure: SIR 97 (Altomare et al., 1997); program(s) used to refine structure: Jana2000 (Petricek and Dusek, 2000); software used to prepare material for publication: Jana2000 (Petricek and Dusek, 2000).

Figures top

endohedral Barium fullerene [74] top

Crystal data top

Ba⁻C₇₄[Co(OEP)](C6H₆)₂	F(000) = 3372
M_r = 1774.1	D_x = 1.607 (1) Mg m⁻³
Monoclinic, C2	Synchrotron radiation, λ = 0.643 Å
Hall symbol: C 2y	Cell parameters from 1000 reflections
a = 25.169 (3) Å	θ = 1–17°
b = 15.018 (3) Å	µ = 0.63 mm⁻¹
c = 19.429 (4) Å	T = 100 K
β = 93.30 (2)°	Rhombic, dark red
V = 7332 (2) Å³	0.04 × 0.04 × 0.02 mm
Z = 4

Data collection top

Huber four circle / Bruker Smart 6000 CCD diffractometer	7590 reflections with I > 3σ(I)
Radiation source: accelerator, synchroton	R_int = 0.132
Si (111) monochromator	θ_max = 17.0°, θ_min = 1.0°
ϕ scan, 0.3deg/fram, 20s/frame, ϕ = 0 – 360 deg	h = −22→22
18394 measured reflections	k = −11→13
18394 independent reflections	l = −17→17

Refinement top

Refinement on F	Weighting scheme based on measured s.u.'s w = 1/σ²(F)
R[F² > 2σ(F²)] = 0.131	(Δ/σ)_max = 0.148
wR(F²) = 0.186	Δρ_max = 1.70 e Å⁻³
S = 2.44	Δρ_min = −3.15 e Å⁻³
18394 reflections	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
97 parameters	Extinction coefficient: 0

Crystal data top

Ba⁻C₇₄[Co(OEP)](C6H₆)₂	V = 7332 (2) Å³
M_r = 1774.1	Z = 4
Monoclinic, C2	Synchrotron radiation, λ = 0.643 Å
a = 25.169 (3) Å	µ = 0.63 mm⁻¹
b = 15.018 (3) Å	T = 100 K
c = 19.429 (4) Å	0.04 × 0.04 × 0.02 mm
β = 93.30 (2)°

Data collection top

Huber four circle / Bruker Smart 6000 CCD diffractometer	7590 reflections with I > 3σ(I)
18394 measured reflections	R_int = 0.132
18394 independent reflections	θ_max = 17.0°

Refinement top

R[F² > 2σ(F²)] = 0.131	97 parameters
wR(F²) = 0.186	(Δ/σ)_max = 0.148
S = 2.44	Δρ_max = 1.70 e Å⁻³
18394 reflections	Δρ_min = −3.15 e Å⁻³

Special details top

Refinement. 1) the following - dummy - positions were part of the rigid body definition Grava C 0.2920 (3) −0.0206 (14) 0.3048 (4) Uani 0.0210 (6) 4 0 d.. . Gravb C 0.2918 (3) −0.0099 (13) 0.3103 (4) Uani 0.0210 (6) 4 0 d.. . the anisotropic displacement parameters correspond to the values obtained from TLS-refinement Grava C 0.0208 (8) 0.0279 (15) 0.0139 (6) 0.0063 (9) −0.0038 (6) −0.0014 (4) Gravb C 0.0261 (13) 0.0176 (10) 0.0204 (9) 0.0030 (4) 0.0105 (11) −0.0016 (4)

2) the y-coordinate of C91A was fixed in order to fix the origin (which is not automated in Jana2000)

3) comment on higher symmetry reported: the Co(OEP) part of the structure fulfills 2/m symmetry but the fullerene part does not. Twin refinement in C2 and testing in test in C2/m significantly prove the space group symmetry C2/m see Friese et al. Acta Cryst. B, in preparation

Validation Reply Form as proposed by CHECKCIF (checkcif@iucr.ac.uk)

_vrf_THETM01_I PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Intensities were recorded on a micro crystal using synchrotron radiation. The data quality is limited due to the ptroblems typically encountered in crystal structure analysis of this compound class.

_vrf_PLAT021_I PROBLEM: Ratio Unique / Expected Reflections too High ··· 6.01 RESPONSE: The value is due to averaging the intensity data corresponding to point group symmetry 2.

_vrf_PLAT023_I PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]···.. 17.02 Deg. RESPONSE: see above

_vrf_PLAT027_I PROBLEM: _diffrn_reflns_theta_full (too) Low ············ 17.02 Deg. RESPONSE: see above

_vrf_PLAT432_I PROBLEM: Short Inter X···Y Contact C91A.. C93A.. 2.25 A ng. RESPONSE: The limited data quality does not allow to a precise localization of the solvent molecule atoms. Anyhow, these positions should be part of the structure model and the refinement!

_vrf_PLAT773_I PROBLEM: Suspect C—C Bond in CIF: C91A –C92A.. 2.68 A ng. RESPONSE: see above

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co	0.51809 (7)	0	−0.08479 (9)	0.0153 (5)*
Baa	0.3338 (4)	0.0350 (6)	0.3147 (6)	0.195 (2)	0.383 (4)
Bab	0.3252 (2)	−0.0732 (4)	0.3017 (4)	0.195 (2)	0.617 (4)
C91a	0.5617 (10)	0.3769 (15)	−0.4732 (13)	0.074 (2)*
C91b	0.5578 (10)	−0.3595 (16)	−0.5044 (13)	0.074 (2)*
C92a	0.5294 (10)	0.3560 (15)	−0.4473 (13)	0.074 (2)*
C92b	0.5186 (10)	−0.3814 (14)	−0.4138 (12)	0.074 (2)*
C93a	0.4808 (11)	0.3609 (14)	−0.4208 (12)	0.074 (2)*
C93b	0.4647 (9)	−0.3644 (15)	−0.4572 (14)	0.074 (2)*
C94	0.6209 (7)	0.5196 (13)	−0.3178 (10)	0.074 (2)*
C95	0.6585 (7)	0.5198 (13)	−0.3602 (9)	0.074 (2)*
C96	0.7216 (7)	0.4784 (15)	−0.3345 (9)	0.074 (2)*
C97	0.7377 (6)	0.4795 (16)	−0.2754 (10)	0.074 (2)*
C98	0.6920 (6)	0.4848 (19)	−0.2158 (8)	0.074 (2)*
C99	0.6408 (6)	0.5095 (18)	−0.2377 (9)	0.074 (2)*
N81a	0.57555 (19)	−0.0050 (4)	−0.0084 (3)	0.0255 (8)
C82a	0.6006 (3)	−0.0793 (5)	0.0214 (4)	0.0293 (9)
C83a	0.6424 (3)	−0.0491 (5)	0.0714 (3)	0.0354 (11)
C84a	0.5926 (3)	−0.1713 (4)	0.0083 (4)	0.0324 (9)
C85a	0.6797 (3)	−0.1128 (5)	0.1129 (4)	0.0451 (15)
C86a	0.7248 (3)	−0.1457 (5)	0.0668 (4)	0.0507 (16)
N81/1a	0.52077 (15)	−0.1399 (5)	−0.08657 (19)	0.0262 (8)
C82/1a	0.4915 (3)	−0.1951 (5)	−0.1321 (4)	0.0305 (8)
C83/1a	0.5079 (3)	−0.2872 (5)	−0.1191 (3)	0.0382 (10)
C84/1a	0.4530 (3)	−0.1741 (4)	−0.1858 (4)	0.0324 (9)
C85/1a	0.4852 (3)	−0.3666 (5)	−0.1611 (4)	0.0495 (14)
C86/1a	0.5128 (3)	−0.3725 (5)	−0.2313 (4)	0.0546 (14)
N81/2a	0.46350 (19)	−0.0073 (4)	−0.1642 (3)	0.0255 (8)
C82/2a	0.4428 (3)	−0.0825 (5)	−0.1979 (4)	0.0293 (9)
C83/2a	0.4071 (3)	−0.0539 (5)	−0.2557 (3)	0.0353 (11)
C85/2a	0.3782 (3)	−0.1189 (5)	−0.3061 (4)	0.0450 (15)
C86/2a	0.4175 (3)	−0.1519 (5)	−0.3604 (4)	0.0501 (17)
C82/3a	0.4414 (3)	0.0671 (5)	−0.1976 (4)	0.0293 (9)
C83/3a	0.4062 (3)	0.0371 (5)	−0.2555 (3)	0.0353 (11)
C84/3a	0.4499 (3)	0.1591 (4)	−0.1851 (4)	0.0324 (9)
C85/3a	0.3762 (3)	0.1010 (5)	−0.3057 (4)	0.0450 (15)
C86/3a	0.4148 (3)	0.1365 (5)	−0.3598 (4)	0.0501 (17)
N81/4a	0.51828 (15)	0.1275 (5)	−0.08605 (19)	0.0262 (8)
C82/4a	0.4879 (3)	0.1815 (5)	−0.1313 (4)	0.0305 (8)
C83/4a	0.5026 (3)	0.2744 (5)	−0.1180 (3)	0.0382 (10)
C85/4a	0.4785 (3)	0.3529 (5)	−0.1597 (4)	0.0495 (14)
C86/4a	0.5060 (3)	0.3609 (5)	−0.2298 (4)	0.0546 (14)
C82/5a	0.5506 (3)	0.1828 (5)	−0.0442 (4)	0.0305 (8)
C83/5a	0.5408 (3)	0.2752 (5)	−0.0650 (3)	0.0383 (10)
C84/5a	0.5895 (3)	0.1619 (4)	0.0090 (4)	0.0324 (9)
C85/5a	0.5707 (3)	0.3547 (5)	−0.0316 (4)	0.0496 (14)
C86/5a	0.6268 (3)	0.3633 (5)	−0.0618 (4)	0.0549 (14)
C82/6a	0.5992 (3)	0.0703 (5)	0.0217 (4)	0.0293 (9)
C83/6a	0.6416 (3)	0.0419 (5)	0.0716 (3)	0.0354 (11)
C85/6a	0.6777 (3)	0.1071 (5)	0.1133 (4)	0.0451 (15)
C86/6a	0.7221 (3)	0.1427 (5)	0.0673 (4)	0.0507 (16)
C82/7a	0.5541 (3)	−0.1938 (5)	−0.0449 (4)	0.0305 (8)
C83/7a	0.5460 (3)	−0.2864 (5)	−0.0661 (3)	0.0383 (10)
C85/7a	0.5774 (3)	−0.3647 (5)	−0.0330 (4)	0.0496 (14)
C86/7a	0.6337 (3)	−0.3700 (5)	−0.0632 (4)	0.0549 (14)
C1a	0.2202 (3)	−0.1945 (6)	0.4247 (4)	0.148 (3)	0.470 (7)
C2a	0.2247 (3)	−0.2482 (6)	0.2405 (4)	0.152 (3)	0.470 (7)
C3a	0.2847 (3)	−0.2714 (6)	0.3683 (4)	0.152 (3)	0.470 (7)
C4a	0.1602 (3)	−0.1713 (6)	0.2969 (4)	0.148 (3)	0.470 (7)
C5a	0.1821 (3)	−0.1267 (6)	0.4176 (4)	0.144 (3)	0.470 (7)
C6a	0.2791 (3)	−0.2670 (6)	0.2409 (4)	0.150 (3)	0.470 (7)
C7a	0.3097 (3)	−0.2788 (6)	0.3061 (4)	0.150 (3)	0.470 (7)
C8a	0.1515 (3)	−0.1149 (6)	0.3525 (4)	0.144 (3)	0.470 (7)
C9a	0.1984 (3)	−0.2426 (6)	0.3045 (4)	0.156 (4)	0.470 (7)
C10a	0.2283 (3)	−0.2542 (6)	0.3681 (4)	0.156 (4)	0.470 (7)
C11a	0.2714 (3)	−0.1749 (6)	0.4599 (4)	0.140 (2)	0.470 (7)
C12a	0.2027 (3)	−0.1806 (6)	0.1935 (4)	0.141 (2)	0.470 (7)
C13a	0.3114 (3)	−0.2226 (6)	0.4249 (4)	0.141 (2)	0.470 (7)
C14a	0.1627 (3)	−0.1329 (6)	0.2285 (4)	0.140 (2)	0.470 (7)
C15a	0.2823 (3)	−0.0903 (6)	0.4910 (4)	0.133 (3)	0.470 (7)
C16a	0.2345 (3)	−0.1375 (6)	0.1450 (4)	0.136 (3)	0.470 (7)
C17a	0.3637 (3)	−0.1874 (6)	0.4199 (4)	0.136 (3)	0.470 (7)
C18a	0.1531 (3)	−0.0404 (6)	0.2162 (4)	0.133 (3)	0.470 (7)
C19a	0.2414 (3)	−0.0204 (6)	0.4846 (4)	0.133 (3)	0.470 (7)
C20a	0.2915 (3)	−0.1595 (6)	0.1450 (4)	0.136 (3)	0.470 (7)
C21a	0.3900 (3)	−0.1976 (6)	0.3547 (4)	0.136 (3)	0.470 (7)
C22a	0.1428 (3)	0.0177 (6)	0.2749 (4)	0.133 (3)	0.470 (7)
C23a	0.1922 (3)	−0.0403 (6)	0.4476 (4)	0.138 (3)	0.470 (7)
C24a	0.3125 (3)	−0.2238 (6)	0.1934 (4)	0.143 (3)	0.470 (7)
C25a	0.3622 (3)	−0.2430 (6)	0.2990 (4)	0.143 (3)	0.470 (7)
C26a	0.1425 (3)	−0.0211 (6)	0.3419 (4)	0.138 (3)	0.470 (7)
C27a	0.1670 (3)	0.0243 (6)	0.4012 (4)	0.135 (3)	0.470 (7)
C28a	0.3638 (3)	−0.2104 (6)	0.2292 (4)	0.139 (3)	0.470 (7)
C29a	0.3370 (3)	−0.0649 (6)	0.4978 (4)	0.140 (3)	0.470 (7)
C30a	0.2173 (3)	−0.0510 (6)	0.1231 (4)	0.140 (3)	0.470 (7)
C31a	0.3770 (3)	−0.1127 (6)	0.4629 (4)	0.140 (3)	0.470 (7)
C32a	0.1773 (3)	−0.0033 (6)	0.1581 (4)	0.140 (3)	0.470 (7)
C33a	0.3529 (3)	0.0281 (6)	0.5015 (4)	0.149 (3)	0.470 (7)
C34a	0.2543 (3)	0.0141 (6)	0.0980 (4)	0.149 (3)	0.470 (7)
C35a	0.4174 (3)	−0.0488 (6)	0.4451 (4)	0.149 (3)	0.470 (7)
C36a	0.1898 (3)	0.0910 (6)	0.1544 (4)	0.149 (3)	0.470 (7)
C37a	0.3137 (3)	0.0939 (6)	0.4938 (4)	0.147 (3)	0.470 (7)
C38a	0.3085 (3)	−0.0070 (6)	0.0997 (4)	0.146 (3)	0.470 (7)
C39a	0.4413 (3)	−0.0583 (6)	0.3823 (4)	0.146 (3)	0.470 (7)
C40a	0.1809 (3)	0.1452 (6)	0.2112 (4)	0.147 (3)	0.470 (7)
C41a	0.2583 (3)	0.0705 (6)	0.4859 (4)	0.140 (3)	0.470 (7)
C42a	0.3273 (3)	−0.0932 (6)	0.1224 (4)	0.140 (3)	0.470 (7)
C43a	0.4283 (3)	−0.1322 (6)	0.3373 (4)	0.140 (3)	0.470 (7)
C44a	0.1573 (3)	0.1095 (6)	0.2710 (4)	0.140 (3)	0.470 (7)
C45a	0.2330 (3)	0.1350 (6)	0.4395 (4)	0.138 (3)	0.470 (7)
C46a	0.3786 (3)	−0.0799 (6)	0.1583 (4)	0.136 (3)	0.470 (7)
C47a	0.4299 (3)	−0.0997 (6)	0.2674 (4)	0.136 (3)	0.470 (7)
C48a	0.1817 (3)	0.1548 (6)	0.3303 (4)	0.138 (3)	0.470 (7)
C49a	0.1880 (3)	0.1118 (6)	0.3955 (4)	0.134 (3)	0.470 (7)
C50a	0.3967 (3)	−0.1371 (6)	0.2131 (4)	0.134 (3)	0.470 (7)
C51a	0.2374 (3)	0.1020 (6)	0.1172 (4)	0.154 (3)	0.470 (7)
C52a	0.4027 (3)	0.0382 (6)	0.4690 (4)	0.154 (3)	0.470 (7)
C53a	0.4113 (3)	0.1142 (6)	0.4277 (4)	0.155 (3)	0.470 (7)
C54a	0.2758 (3)	0.1665 (6)	0.1395 (4)	0.155 (3)	0.470 (7)
C55a	0.3702 (3)	0.1808 (6)	0.4185 (4)	0.151 (3)	0.470 (7)
C56a	0.3316 (3)	0.1437 (6)	0.1427 (4)	0.148 (3)	0.470 (7)
C57a	0.4347 (3)	0.1039 (6)	0.3621 (4)	0.148 (3)	0.470 (7)
C58a	0.2671 (3)	0.2206 (6)	0.1991 (4)	0.151 (3)	0.470 (7)
C59a	0.3225 (3)	0.1718 (6)	0.4515 (4)	0.149 (3)	0.470 (7)
C60a	0.3479 (3)	0.0591 (6)	0.1225 (4)	0.145 (3)	0.470 (7)
C61a	0.4501 (3)	0.0197 (6)	0.3399 (4)	0.145 (3)	0.470 (7)
C62a	0.2203 (3)	0.2113 (6)	0.2340 (4)	0.149 (3)	0.470 (7)
C63a	0.2725 (3)	0.1969 (6)	0.4172 (4)	0.143 (3)	0.470 (7)
C64a	0.3912 (3)	0.0140 (6)	0.1594 (4)	0.138 (3)	0.470 (7)
C65a	0.4425 (3)	−0.0058 (6)	0.2687 (4)	0.138 (3)	0.470 (7)
C66a	0.2212 (3)	0.2167 (6)	0.3080 (4)	0.143 (3)	0.470 (7)
C67a	0.2698 (3)	0.2305 (6)	0.3483 (4)	0.138 (3)	0.470 (7)
C68a	0.4184 (3)	0.0533 (6)	0.2184 (4)	0.132 (3)	0.470 (7)
C69a	0.4008 (3)	0.1413 (6)	0.2413 (4)	0.133 (3)	0.470 (7)
C70a	0.3194 (3)	0.2384 (6)	0.3125 (4)	0.138 (3)	0.470 (7)
C71a	0.4083 (3)	0.1641 (6)	0.3125 (4)	0.140 (3)	0.470 (7)
C72a	0.3173 (3)	0.2314 (6)	0.2391 (4)	0.142 (3)	0.470 (7)
C73a	0.3682 (3)	0.2118 (6)	0.3475 (4)	0.142 (3)	0.470 (7)
C74a	0.3573 (3)	0.1837 (6)	0.2041 (4)	0.140 (3)	0.470 (7)
Grava	0.2923 (3)	−0.0127 (6)	0.3043 (4)	0.0250 (6)	0.00
C1b	0.1329 (3)	−0.0346 (6)	0.2642 (4)	0.148 (3)	0.530 (7)
C2b	0.2163 (3)	0.0133 (6)	0.1195 (4)	0.152 (3)	0.530 (7)
C3b	0.1558 (3)	0.1019 (6)	0.2186 (4)	0.152 (3)	0.530 (7)
C4b	0.1934 (3)	−0.1231 (6)	0.1650 (4)	0.148 (3)	0.530 (7)
C5b	0.1503 (3)	−0.1220 (6)	0.2761 (4)	0.144 (3)	0.530 (7)
C6b	0.2265 (3)	0.1028 (6)	0.1355 (4)	0.150 (3)	0.530 (7)
C7b	0.1957 (3)	0.1479 (6)	0.1860 (4)	0.150 (3)	0.530 (7)
C8b	0.1812 (3)	−0.1672 (6)	0.2256 (4)	0.144 (3)	0.530 (7)
C9b	0.1745 (3)	−0.0338 (6)	0.1517 (4)	0.156 (4)	0.530 (7)
C10b	0.1443 (3)	0.0103 (6)	0.2011 (4)	0.156 (4)	0.530 (7)
C11b	0.1373 (3)	0.0290 (6)	0.3206 (4)	0.140 (3)	0.530 (7)
C12b	0.2611 (3)	−0.0467 (6)	0.1128 (4)	0.141 (3)	0.530 (7)
C13b	0.1515 (3)	0.1137 (6)	0.2923 (4)	0.141 (3)	0.530 (7)
C14b	0.2469 (3)	−0.1313 (6)	0.1411 (4)	0.140 (3)	0.530 (7)
C15b	0.1556 (3)	0.0030 (6)	0.3885 (4)	0.133 (3)	0.530 (7)
C16b	0.3147 (3)	−0.0153 (6)	0.1177 (4)	0.136 (3)	0.530 (7)
C17b	0.1845 (3)	0.1752 (6)	0.3310 (4)	0.136 (3)	0.530 (7)
C18b	0.2858 (3)	−0.1875 (6)	0.1752 (4)	0.133 (3)	0.530 (7)
C19b	0.1726 (3)	−0.0897 (6)	0.4007 (4)	0.133 (3)	0.530 (7)
C20b	0.3247 (3)	0.0794 (6)	0.1329 (4)	0.136 (3)	0.530 (7)
C21b	0.2254 (3)	0.2247 (6)	0.2957 (4)	0.136 (3)	0.530 (7)
C22b	0.2719 (3)	−0.2350 (6)	0.2379 (4)	0.133 (3)	0.530 (7)
C23b	0.1697 (3)	−0.1501 (6)	0.3438 (4)	0.138 (3)	0.530 (7)
C24b	0.2801 (3)	0.1363 (6)	0.1417 (4)	0.143 (2)	0.530 (7)
C25b	0.2301 (3)	0.2095 (6)	0.2237 (4)	0.143 (2)	0.530 (7)
C26b	0.2197 (3)	−0.2233 (6)	0.2618 (4)	0.138 (3)	0.530 (7)
C27b	0.2119 (3)	−0.2135 (6)	0.3345 (4)	0.135 (3)	0.530 (7)
C28b	0.2818 (3)	0.2029 (6)	0.1955 (4)	0.139 (3)	0.530 (7)
C29b	0.1791 (3)	0.0716 (6)	0.4310 (4)	0.140 (3)	0.530 (7)
C30b	0.3542 (3)	−0.0792 (6)	0.1391 (4)	0.140 (3)	0.530 (7)
C31b	0.1933 (3)	0.1562 (6)	0.4027 (4)	0.140 (3)	0.530 (7)
C32b	0.3400 (3)	−0.1639 (6)	0.1673 (4)	0.140 (3)	0.530 (7)
C33b	0.2175 (3)	0.0515 (6)	0.4876 (4)	0.149 (4)	0.530 (7)
C34b	0.4048 (3)	−0.0526 (6)	0.1727 (4)	0.149 (4)	0.530 (7)
C35b	0.2404 (3)	0.1880 (6)	0.4421 (4)	0.149 (4)	0.530 (7)
C36b	0.3819 (3)	−0.1890 (6)	0.2182 (4)	0.149 (4)	0.530 (7)
C37b	0.2342 (3)	−0.0366 (6)	0.4976 (4)	0.147 (3)	0.530 (7)
C38b	0.4133 (3)	0.0375 (6)	0.1882 (4)	0.146 (3)	0.530 (7)
C39b	0.2795 (3)	0.2333 (6)	0.4075 (4)	0.146 (3)	0.530 (7)
C40b	0.3680 (3)	−0.2325 (6)	0.2783 (4)	0.147 (3)	0.530 (7)
C41b	0.2118 (3)	−0.1072 (6)	0.4550 (4)	0.140 (3)	0.530 (7)
C42b	0.3740 (3)	0.1035 (6)	0.1682 (4)	0.140 (3)	0.530 (7)
C43b	0.2722 (3)	0.2524 (6)	0.3350 (4)	0.140 (3)	0.530 (7)
C44b	0.3136 (3)	−0.2561 (6)	0.2883 (4)	0.140 (3)	0.530 (7)
C45b	0.2540 (3)	−0.1706 (6)	0.4457 (4)	0.138 (3)	0.530 (7)
C46b	0.3756 (3)	0.1701 (6)	0.2220 (4)	0.136 (3)	0.530 (7)
C47b	0.3239 (3)	0.2458 (6)	0.3067 (4)	0.136 (3)	0.530 (7)
C48b	0.3057 (3)	−0.2463 (6)	0.3610 (4)	0.138 (3)	0.530 (7)
C49b	0.2551 (3)	−0.2227 (6)	0.3846 (4)	0.134 (3)	0.530 (7)
C50b	0.3292 (3)	0.2188 (6)	0.2372 (4)	0.134 (3)	0.530 (7)
C51b	0.4220 (3)	−0.1204 (6)	0.2216 (4)	0.154 (4)	0.530 (7)
C52b	0.2554 (3)	0.1234 (6)	0.4946 (4)	0.154 (4)	0.530 (7)
C53b	0.3101 (3)	0.1043 (6)	0.5100 (4)	0.155 (3)	0.530 (7)
C54b	0.4465 (3)	−0.0954 (6)	0.2864 (4)	0.155 (3)	0.530 (7)
C55b	0.3273 (3)	0.0132 (6)	0.5186 (4)	0.151 (3)	0.530 (7)
C56b	0.4541 (3)	−0.0024 (6)	0.3028 (4)	0.148 (3)	0.530 (7)
C57b	0.3502 (3)	0.1496 (6)	0.4730 (4)	0.148 (3)	0.530 (7)
C58b	0.4312 (3)	−0.1389 (6)	0.3484 (4)	0.151 (3)	0.530 (7)
C59b	0.2901 (3)	−0.0562 (6)	0.5134 (4)	0.149 (3)	0.530 (7)
C60b	0.4384 (3)	0.0630 (6)	0.2545 (4)	0.145 (3)	0.530 (7)
C61b	0.3355 (3)	0.2137 (6)	0.4233 (4)	0.145 (3)	0.530 (7)
C62b	0.3931 (3)	−0.2069 (6)	0.3447 (4)	0.149 (3)	0.530 (7)
C63b	0.3026 (3)	−0.1390 (6)	0.4807 (4)	0.143 (2)	0.530 (7)
C64b	0.4147 (3)	0.1450 (6)	0.2759 (4)	0.138 (3)	0.530 (7)
C65b	0.3630 (3)	0.2206 (6)	0.3606 (4)	0.138 (3)	0.530 (7)
C66b	0.3543 (3)	−0.2147 (6)	0.3959 (4)	0.143 (2)	0.530 (7)
C67b	0.3528 (3)	−0.1527 (6)	0.4515 (4)	0.138 (2)	0.530 (7)
C68b	0.4056 (3)	0.1617 (6)	0.3466 (4)	0.132 (2)	0.530 (7)
C69b	0.4206 (3)	0.0926 (6)	0.3977 (4)	0.133 (3)	0.530 (7)
C70b	0.3917 (3)	−0.0796 (6)	0.4552 (4)	0.138 (3)	0.530 (7)
C71b	0.3921 (3)	0.0867 (6)	0.4588 (4)	0.140 (3)	0.530 (7)
C72b	0.4292 (3)	−0.0730 (6)	0.4030 (4)	0.142 (3)	0.530 (7)
C73b	0.3779 (3)	0.0021 (6)	0.4871 (4)	0.142 (3)	0.530 (7)
C74b	0.4434 (3)	0.0116 (6)	0.3748 (4)	0.140 (3)	0.530 (7)
Gravb	0.2921 (3)	−0.0019 (6)	0.3109 (4)	0.0250 (6)	0.0

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Baa	0.166 (3)	0.145 (4)	0.276 (4)	−0.087 (3)	0.043 (2)	−0.003 (3)
Bab	0.166 (3)	0.145 (4)	0.276 (4)	0.087 (3)	0.043 (2)	0.003 (3)
N81a	0.0225 (12)	0.0300 (16)	0.0248 (13)	−0.00014 (3)	0.0068 (12)	0.00010 (2)
C82a	0.0262 (12)	0.0336 (18)	0.0284 (14)	0.0020 (2)	0.0042 (13)	0.0020 (2)
C83a	0.0303 (15)	0.042 (2)	0.0331 (17)	0.0018 (2)	−0.0010 (16)	0.0017 (2)
C84a	0.0318 (13)	0.0321 (17)	0.0334 (14)	0.0043 (4)	0.0035 (14)	0.0038 (5)
C85a	0.039 (2)	0.053 (3)	0.043 (2)	0.0062 (6)	−0.008 (2)	0.0049 (6)
C86a	0.034 (2)	0.060 (3)	0.057 (3)	0.0121 (9)	−0.008 (2)	0.0032 (9)
N81/1a	0.0254 (12)	0.0265 (16)	0.0275 (13)	−0.00004 (3)	0.0077 (12)	0.00009 (2)
C82/1a	0.0316 (13)	0.0276 (16)	0.0327 (14)	−0.0018 (2)	0.0058 (14)	−0.0021 (2)
C83/1a	0.0442 (18)	0.0269 (16)	0.044 (2)	−0.0007 (2)	0.0031 (19)	−0.0026 (2)
C84/1a	0.0324 (13)	0.0319 (17)	0.0330 (14)	−0.0039 (4)	0.0036 (14)	−0.0041 (5)
C85/1a	0.061 (2)	0.0289 (16)	0.058 (3)	−0.0033 (6)	−0.002 (3)	−0.0074 (7)
C86/1a	0.069 (3)	0.0357 (17)	0.058 (3)	0.0048 (11)	−0.001 (3)	−0.0180 (12)
N81/2a	0.0225 (12)	0.0300 (16)	0.0248 (13)	−0.00014 (3)	0.0068 (12)	0.00010 (2)
C82/2a	0.0267 (12)	0.0334 (18)	0.0281 (14)	−0.0021 (2)	0.0042 (13)	−0.0020 (2)
C83/2a	0.0321 (15)	0.042 (2)	0.0315 (17)	−0.0019 (2)	−0.0008 (16)	−0.0019 (2)
C85/2a	0.043 (2)	0.052 (3)	0.039 (2)	−0.0053 (6)	−0.008 (2)	−0.0062 (6)
C86/2a	0.058 (3)	0.057 (3)	0.034 (3)	−0.0030 (9)	−0.006 (2)	−0.0116 (9)
C82/3a	0.0266 (12)	0.0335 (18)	0.0281 (14)	0.0019 (2)	0.0042 (13)	0.0021 (2)
C83/3a	0.0320 (15)	0.042 (2)	0.0315 (17)	0.0016 (2)	−0.0009 (16)	0.0019 (2)
C84/3a	0.0322 (13)	0.0321 (17)	0.0331 (14)	0.0039 (4)	0.0035 (14)	0.0041 (5)
C85/3a	0.043 (2)	0.052 (3)	0.039 (2)	0.0051 (6)	−0.008 (2)	0.0060 (6)
C86/3a	0.057 (3)	0.057 (3)	0.034 (3)	0.0031 (9)	−0.007 (2)	0.0115 (9)
N81/4a	0.0254 (12)	0.0265 (16)	0.0275 (13)	−0.00004 (3)	0.0077 (12)	0.00009 (2)
C82/4a	0.0315 (13)	0.0276 (16)	0.0327 (14)	0.0019 (2)	0.0057 (14)	0.0022 (2)
C83/4a	0.0441 (18)	0.0270 (16)	0.044 (2)	0.0013 (2)	0.0030 (19)	0.0025 (2)
C85/4a	0.061 (2)	0.0291 (16)	0.058 (3)	0.0044 (6)	−0.002 (3)	0.0071 (7)
C86/4a	0.070 (3)	0.0352 (17)	0.058 (3)	−0.0037 (11)	−0.001 (3)	0.0177 (12)
C82/5a	0.0315 (13)	0.0276 (16)	0.0328 (14)	−0.0022 (2)	0.0058 (14)	−0.0018 (2)
C83/5a	0.0440 (18)	0.0269 (16)	0.044 (2)	−0.0025 (2)	0.0031 (19)	−0.0011 (2)
C84/5a	0.0321 (13)	0.0319 (17)	0.0334 (14)	−0.0043 (4)	0.0036 (14)	−0.0037 (5)
C85/5a	0.060 (2)	0.0289 (16)	0.059 (3)	−0.0073 (6)	−0.002 (3)	−0.0040 (7)
C86/5a	0.061 (3)	0.0356 (17)	0.067 (3)	−0.0193 (12)	−0.002 (3)	0.0027 (13)
C82/6a	0.0264 (12)	0.0335 (18)	0.0284 (14)	−0.0023 (2)	0.0042 (13)	−0.0019 (2)
C83/6a	0.0305 (15)	0.042 (2)	0.0331 (17)	−0.0022 (2)	−0.0009 (16)	−0.0017 (2)
C85/6a	0.039 (2)	0.052 (3)	0.043 (2)	−0.0066 (6)	−0.008 (2)	−0.0052 (6)
C86/6a	0.035 (2)	0.059 (3)	0.057 (3)	−0.0128 (9)	−0.008 (2)	−0.0036 (9)
C82/7a	0.0313 (13)	0.0277 (16)	0.0328 (14)	0.0023 (2)	0.0057 (14)	0.0019 (2)
C83/7a	0.0438 (18)	0.0270 (16)	0.044 (2)	0.0030 (2)	0.0030 (19)	0.0010 (2)
C85/7a	0.060 (2)	0.0293 (16)	0.059 (3)	0.0083 (6)	−0.002 (3)	0.0037 (7)
C86/7a	0.060 (3)	0.0369 (17)	0.067 (3)	0.0201 (12)	−0.002 (3)	−0.0031 (13)
C1a	0.169 (6)	0.142 (4)	0.138 (6)	−0.052 (3)	0.044 (5)	0.072 (3)
C2a	0.188 (6)	0.081 (3)	0.184 (7)	−0.063 (3)	−0.019 (5)	−0.049 (3)
C3a	0.212 (6)	0.052 (3)	0.190 (7)	−0.003 (3)	0.003 (5)	0.054 (3)
C4a	0.091 (6)	0.161 (4)	0.192 (6)	−0.084 (3)	−0.004 (5)	0.001 (3)
C5a	0.115 (5)	0.189 (5)	0.136 (5)	−0.048 (4)	0.066 (4)	0.043 (3)
C6a	0.214 (5)	0.051 (4)	0.185 (6)	−0.007 (3)	0.001 (4)	−0.055 (2)
C7a	0.210 (5)	0.035 (4)	0.205 (6)	0.028 (3)	0.004 (4)	0.000 (2)
C8a	0.064 (5)	0.195 (5)	0.177 (5)	−0.055 (4)	0.037 (4)	0.020 (3)
C9a	0.163 (6)	0.098 (3)	0.206 (8)	−0.087 (4)	0.000 (6)	0.003 (3)
C10a	0.192 (6)	0.085 (3)	0.192 (8)	−0.061 (4)	0.020 (6)	0.052 (3)
C11a	0.187 (5)	0.145 (4)	0.088 (4)	−0.013 (3)	0.017 (4)	0.083 (4)
C12a	0.147 (5)	0.137 (4)	0.133 (4)	−0.061 (3)	−0.048 (4)	−0.059 (4)
C13a	0.191 (5)	0.097 (4)	0.134 (4)	0.020 (3)	−0.012 (4)	0.084 (4)
C14a	0.083 (5)	0.174 (4)	0.157 (4)	−0.063 (3)	−0.048 (4)	−0.024 (4)
C15a	0.179 (5)	0.188 (5)	0.034 (3)	−0.003 (4)	0.012 (3)	0.047 (3)
C16a	0.168 (5)	0.161 (5)	0.072 (3)	−0.029 (4)	−0.042 (3)	−0.065 (3)
C17a	0.149 (5)	0.122 (5)	0.130 (3)	0.057 (4)	−0.041 (3)	0.069 (3)
C18a	0.052 (5)	0.199 (5)	0.142 (3)	−0.013 (4)	−0.060 (3)	−0.001 (3)
C19a	0.162 (4)	0.202 (5)	0.040 (5)	0.001 (3)	0.052 (3)	0.001 (2)
C20a	0.191 (4)	0.144 (5)	0.073 (5)	0.004 (3)	0.007 (3)	−0.081 (2)
C21a	0.120 (4)	0.110 (5)	0.175 (5)	0.085 (3)	−0.021 (3)	0.032 (2)
C22a	0.028 (4)	0.198 (5)	0.170 (5)	0.027 (3)	−0.018 (3)	0.008 (2)
C23a	0.118 (4)	0.209 (6)	0.095 (5)	−0.006 (3)	0.079 (3)	0.011 (2)
C24a	0.199 (4)	0.092 (5)	0.139 (5)	0.026 (3)	0.020 (4)	−0.081 (2)
C25a	0.165 (4)	0.069 (5)	0.194 (5)	0.078 (3)	0.008 (4)	−0.006 (2)
C26a	0.035 (4)	0.209 (6)	0.173 (5)	0.003 (3)	0.034 (3)	0.005 (2)
C27a	0.075 (4)	0.200 (7)	0.137 (6)	0.029 (4)	0.070 (4)	−0.0125 (18)
C28a	0.158 (4)	0.100 (6)	0.162 (6)	0.070 (3)	0.036 (4)	−0.0525 (17)
C29a	0.176 (5)	0.204 (7)	0.033 (3)	0.008 (5)	−0.041 (3)	0.035 (3)
C30a	0.156 (5)	0.206 (7)	0.050 (3)	−0.013 (5)	−0.066 (3)	−0.020 (3)
C31a	0.141 (5)	0.184 (7)	0.087 (3)	0.036 (5)	−0.067 (3)	0.056 (3)
C32a	0.102 (5)	0.209 (7)	0.097 (3)	0.005 (5)	−0.083 (3)	0.010 (3)
C33a	0.182 (6)	0.220 (7)	0.038 (3)	−0.012 (5)	−0.056 (4)	−0.025 (3)
C34a	0.193 (6)	0.223 (7)	0.024 (3)	0.002 (5)	−0.036 (4)	0.019 (3)
C35a	0.097 (6)	0.220 (7)	0.118 (3)	0.020 (5)	−0.087 (4)	0.024 (3)
C36a	0.131 (6)	0.195 (7)	0.111 (3)	0.046 (5)	−0.076 (4)	0.056 (3)
C37a	0.203 (5)	0.190 (5)	0.047 (5)	−0.009 (4)	−0.013 (3)	−0.069 (3)
C38a	0.197 (5)	0.221 (6)	0.021 (5)	0.000 (4)	0.023 (3)	0.001 (3)
C39a	0.048 (5)	0.213 (6)	0.169 (5)	0.034 (4)	−0.055 (3)	0.019 (3)
C40a	0.115 (5)	0.153 (5)	0.167 (5)	0.080 (4)	−0.049 (3)	0.052 (3)
C41a	0.185 (5)	0.191 (5)	0.048 (6)	0.016 (3)	0.040 (3)	−0.054 (2)
C42a	0.184 (5)	0.192 (5)	0.047 (6)	0.016 (3)	0.041 (3)	−0.053 (2)
C43a	0.064 (5)	0.170 (5)	0.183 (6)	0.078 (3)	−0.017 (3)	0.017 (2)
C44a	0.065 (5)	0.168 (5)	0.183 (6)	0.079 (3)	−0.017 (3)	0.017 (2)
C45a	0.166 (4)	0.146 (6)	0.106 (6)	0.045 (3)	0.051 (4)	−0.0705 (18)
C46a	0.134 (4)	0.192 (6)	0.089 (6)	0.032 (4)	0.073 (4)	−0.0361 (17)
C47a	0.055 (4)	0.183 (6)	0.173 (6)	0.061 (4)	0.034 (4)	−0.0092 (17)
C48a	0.104 (4)	0.129 (6)	0.182 (6)	0.090 (3)	0.023 (4)	−0.0149 (18)
C49a	0.108 (3)	0.158 (7)	0.142 (7)	0.066 (4)	0.058 (4)	−0.0400 (15)
C50a	0.108 (3)	0.158 (7)	0.142 (7)	0.066 (4)	0.058 (4)	−0.0400 (15)
C51a	0.189 (6)	0.199 (7)	0.068 (3)	0.025 (5)	−0.050 (4)	0.073 (4)
C52a	0.133 (6)	0.226 (7)	0.093 (3)	−0.025 (5)	−0.089 (4)	−0.022 (4)
C53a	0.124 (5)	0.191 (5)	0.140 (4)	−0.063 (4)	−0.071 (4)	−0.046 (4)
C54a	0.209 (5)	0.151 (5)	0.101 (4)	0.013 (4)	−0.013 (4)	0.098 (4)
C55a	0.176 (5)	0.127 (4)	0.144 (5)	−0.061 (4)	−0.041 (4)	−0.071 (4)
C56a	0.192 (5)	0.164 (4)	0.092 (5)	−0.025 (4)	0.033 (4)	0.083 (4)
C57a	0.071 (5)	0.190 (4)	0.179 (5)	−0.067 (4)	−0.040 (4)	−0.015 (4)
C58a	0.204 (5)	0.084 (4)	0.163 (5)	0.029 (4)	−0.013 (4)	0.081 (4)
C59a	0.206 (5)	0.131 (5)	0.107 (5)	−0.020 (3)	−0.016 (3)	−0.091 (3)
C60a	0.175 (5)	0.209 (5)	0.056 (5)	−0.015 (3)	0.056 (3)	0.041 (3)
C61a	0.030 (5)	0.217 (5)	0.184 (5)	−0.016 (3)	−0.025 (3)	0.003 (3)
C62a	0.169 (5)	0.089 (5)	0.185 (5)	0.075 (3)	−0.022 (3)	0.053 (3)
C63a	0.199 (4)	0.094 (5)	0.137 (5)	0.025 (3)	0.020 (4)	−0.082 (2)
C64a	0.120 (4)	0.209 (6)	0.093 (5)	−0.005 (3)	0.079 (3)	0.011 (2)
C65a	0.034 (4)	0.209 (6)	0.173 (5)	0.004 (3)	0.033 (3)	0.004 (2)
C66a	0.163 (4)	0.071 (5)	0.195 (5)	0.079 (3)	0.007 (4)	−0.004 (2)
C67a	0.191 (4)	0.046 (5)	0.177 (5)	0.032 (3)	0.010 (4)	−0.038 (2)
C68a	0.071 (5)	0.192 (5)	0.139 (5)	−0.028 (3)	0.059 (4)	0.020 (2)
C69a	0.104 (5)	0.143 (4)	0.156 (6)	−0.065 (3)	0.035 (4)	0.034 (2)
C70a	0.190 (5)	0.039 (3)	0.183 (6)	−0.022 (3)	0.000 (5)	−0.008 (2)
C71a	0.106 (5)	0.132 (3)	0.181 (6)	−0.082 (3)	−0.005 (5)	−0.001 (3)
C72a	0.194 (5)	0.058 (3)	0.174 (7)	−0.021 (3)	0.008 (5)	0.052 (3)
C73a	0.164 (5)	0.081 (3)	0.178 (7)	−0.067 (3)	−0.016 (5)	−0.030 (3)
C74a	0.165 (5)	0.114 (3)	0.144 (6)	−0.050 (3)	0.032 (5)	0.065 (3)
C1b	0.038 (4)	0.207 (7)	0.198 (5)	−0.017 (4)	−0.015 (3)	−0.018 (4)
C2b	0.175 (4)	0.217 (7)	0.056 (5)	0.011 (4)	−0.055 (3)	0.007 (4)
C3b	0.090 (4)	0.184 (7)	0.175 (5)	0.067 (4)	−0.048 (3)	0.025 (4)
C4b	0.140 (4)	0.177 (7)	0.121 (5)	−0.044 (4)	−0.050 (3)	−0.066 (4)
C5b	0.069 (4)	0.167 (5)	0.197 (4)	−0.067 (4)	0.001 (3)	−0.025 (4)
C6b	0.186 (4)	0.182 (5)	0.077 (4)	0.035 (4)	−0.041 (3)	0.061 (4)
C7b	0.152 (4)	0.150 (5)	0.143 (4)	0.069 (4)	−0.045 (3)	0.060 (4)
C8b	0.119 (4)	0.136 (5)	0.175 (4)	−0.072 (4)	−0.022 (3)	−0.055 (4)
C9b	0.125 (4)	0.222 (9)	0.111 (5)	−0.008 (4)	−0.075 (4)	−0.024 (5)
C10b	0.072 (4)	0.221 (9)	0.166 (5)	0.016 (4)	−0.064 (4)	−0.005 (5)
C11b	0.035 (5)	0.192 (5)	0.194 (5)	0.023 (3)	0.029 (3)	−0.014 (3)
C12b	0.191 (5)	0.199 (5)	0.033 (5)	−0.003 (3)	−0.010 (3)	−0.032 (3)
C13b	0.066 (5)	0.162 (5)	0.197 (5)	0.073 (3)	0.004 (3)	−0.003 (3)
C14b	0.179 (5)	0.160 (5)	0.078 (5)	−0.021 (3)	−0.016 (3)	−0.078 (3)
C15b	0.063 (5)	0.186 (5)	0.160 (4)	0.002 (3)	0.078 (4)	−0.013 (3)
C16b	0.187 (5)	0.193 (5)	0.032 (4)	0.001 (3)	0.045 (4)	−0.011 (3)
C17b	0.112 (5)	0.106 (5)	0.191 (4)	0.083 (3)	0.029 (4)	−0.019 (3)
C18b	0.183 (5)	0.103 (5)	0.116 (4)	−0.003 (3)	0.019 (4)	−0.088 (3)
C19b	0.094 (5)	0.164 (4)	0.149 (4)	−0.045 (3)	0.082 (4)	0.017 (3)
C20b	0.188 (5)	0.172 (4)	0.053 (4)	−0.011 (3)	0.053 (4)	0.046 (3)
C21b	0.162 (5)	0.053 (4)	0.193 (4)	0.068 (3)	0.014 (4)	0.009 (3)
C22b	0.183 (5)	0.047 (4)	0.170 (4)	−0.017 (3)	0.017 (4)	−0.060 (3)
C23b	0.096 (5)	0.134 (3)	0.187 (5)	−0.075 (4)	0.049 (4)	0.007 (3)
C24b	0.206 (5)	0.148 (3)	0.075 (4)	0.010 (3)	0.011 (4)	0.079 (3)
C25b	0.179 (5)	0.079 (3)	0.168 (4)	0.061 (3)	−0.009 (4)	0.061 (3)
C26b	0.159 (5)	0.067 (3)	0.187 (5)	−0.064 (4)	0.009 (4)	−0.042 (3)
C27b	0.151 (6)	0.070 (2)	0.187 (5)	−0.069 (3)	0.038 (5)	0.012 (3)
C28b	0.201 (6)	0.080 (2)	0.136 (5)	0.013 (3)	0.015 (5)	0.079 (3)
C29b	0.109 (6)	0.183 (7)	0.137 (4)	0.032 (3)	0.093 (5)	−0.039 (3)
C30b	0.169 (6)	0.185 (7)	0.074 (4)	0.018 (3)	0.078 (5)	−0.050 (3)
C31b	0.128 (6)	0.133 (7)	0.166 (4)	0.065 (3)	0.068 (5)	−0.056 (3)
C32b	0.177 (6)	0.132 (7)	0.115 (4)	0.032 (3)	0.058 (5)	−0.083 (3)
C33b	0.171 (6)	0.206 (8)	0.080 (4)	0.013 (3)	0.093 (5)	−0.038 (3)
C34b	0.123 (6)	0.204 (8)	0.129 (4)	0.020 (3)	0.105 (5)	−0.033 (3)
C35b	0.187 (6)	0.120 (8)	0.144 (4)	0.041 (3)	0.058 (5)	−0.089 (3)
C36b	0.153 (6)	0.121 (8)	0.180 (4)	0.070 (3)	0.064 (5)	−0.065 (3)
C37b	0.187 (5)	0.205 (6)	0.058 (4)	−0.011 (3)	0.081 (4)	0.018 (3)
C38b	0.109 (5)	0.200 (6)	0.139 (4)	−0.023 (3)	0.103 (4)	0.006 (3)
C39b	0.201 (5)	0.064 (6)	0.174 (4)	0.014 (3)	0.031 (4)	−0.080 (3)
C40b	0.168 (5)	0.068 (6)	0.209 (4)	0.076 (3)	0.033 (4)	−0.030 (3)
C41b	0.159 (5)	0.165 (5)	0.105 (4)	−0.037 (2)	0.086 (4)	0.046 (3)
C42b	0.157 (5)	0.165 (5)	0.107 (4)	−0.038 (2)	0.086 (4)	0.045 (3)
C43b	0.195 (5)	0.027 (5)	0.200 (4)	0.025 (2)	0.026 (4)	−0.023 (3)
C44b	0.194 (5)	0.027 (5)	0.200 (4)	0.026 (2)	0.025 (4)	−0.022 (3)
C45b	0.191 (6)	0.115 (3)	0.113 (5)	−0.026 (2)	0.051 (5)	0.075 (3)
C46b	0.150 (6)	0.109 (3)	0.154 (5)	−0.060 (2)	0.065 (5)	0.046 (3)
C47b	0.187 (6)	0.028 (3)	0.194 (5)	−0.030 (2)	0.026 (5)	0.001 (3)
C48b	0.197 (6)	0.033 (3)	0.184 (5)	0.018 (2)	0.019 (5)	0.040 (3)
C49b	0.185 (6)	0.056 (2)	0.164 (5)	−0.032 (2)	0.039 (6)	0.053 (3)
C50b	0.185 (6)	0.056 (2)	0.164 (5)	−0.032 (2)	0.039 (6)	0.053 (3)
C51b	0.102 (7)	0.182 (8)	0.187 (5)	0.063 (3)	0.082 (5)	−0.046 (3)
C52b	0.204 (7)	0.184 (8)	0.081 (5)	0.017 (3)	0.059 (5)	−0.082 (3)
C53b	0.212 (6)	0.197 (6)	0.055 (6)	−0.007 (3)	0.006 (4)	−0.074 (3)
C54b	0.057 (6)	0.195 (6)	0.216 (6)	0.063 (3)	0.040 (4)	−0.020 (3)
C55b	0.204 (5)	0.218 (6)	0.030 (5)	0.001 (3)	−0.016 (3)	−0.013 (3)
C56b	0.033 (5)	0.208 (6)	0.207 (5)	0.003 (3)	0.030 (3)	−0.014 (3)
C57b	0.182 (5)	0.157 (6)	0.102 (5)	−0.033 (3)	−0.023 (3)	−0.087 (3)
C58b	0.083 (5)	0.162 (6)	0.207 (5)	0.086 (3)	−0.009 (3)	0.008 (3)
C59b	0.212 (5)	0.203 (5)	0.033 (5)	0.001 (3)	0.025 (3)	0.036 (3)
C60b	0.062 (5)	0.191 (5)	0.188 (4)	−0.040 (3)	0.069 (4)	0.000 (3)
C61b	0.188 (5)	0.088 (5)	0.157 (4)	−0.036 (3)	0.001 (4)	−0.086 (3)
C62b	0.142 (5)	0.097 (5)	0.207 (5)	0.092 (3)	0.000 (3)	0.018 (3)
C63b	0.206 (5)	0.149 (3)	0.074 (4)	0.009 (3)	0.012 (4)	0.078 (3)
C64b	0.096 (5)	0.135 (3)	0.186 (5)	−0.074 (4)	0.050 (4)	0.008 (3)
C65b	0.160 (5)	0.066 (3)	0.187 (5)	−0.063 (4)	0.009 (4)	−0.042 (3)
C66b	0.179 (5)	0.078 (3)	0.170 (4)	0.062 (3)	−0.009 (4)	0.060 (3)
C67b	0.173 (4)	0.130 (4)	0.106 (4)	0.045 (4)	−0.026 (3)	0.070 (3)
C68b	0.100 (4)	0.116 (4)	0.180 (4)	−0.074 (4)	0.006 (3)	−0.028 (3)
C69b	0.075 (3)	0.166 (6)	0.154 (4)	−0.045 (4)	−0.034 (3)	−0.037 (4)
C70b	0.128 (3)	0.176 (6)	0.101 (4)	0.040 (3)	−0.057 (3)	0.034 (4)
C71b	0.127 (4)	0.181 (7)	0.105 (5)	−0.031 (3)	−0.054 (3)	−0.050 (4)
C72b	0.074 (4)	0.185 (7)	0.161 (5)	0.049 (3)	−0.048 (3)	0.014 (4)
C73b	0.150 (4)	0.203 (7)	0.066 (5)	0.005 (3)	−0.058 (3)	−0.006 (4)
C74b	0.043 (4)	0.196 (7)	0.177 (5)	−0.002 (3)	−0.029 (3)	−0.014 (4)

Bond lengths (Å) top

Co—N81a	2.019 (5)	C21a—C47a	2.50 (2)
Co—N81/1a	2.103 (8)	C21a—C50a	2.911 (14)
Co—N81/2a	2.009 (6)	C22a—C26a	1.428 (16)
Co—N81/3a	2.016 (6)	C22a—C27a	2.497 (12)
Co—N81/4a	1.915 (8)	C22a—C32a	2.495 (13)
Co—C82/4a	2.957 (8)	C22a—C36a	2.900 (16)
Co—N81/5a	1.88 (3)	C22a—C40a	2.50 (2)
Co—C82/5a	2.959 (8)	C22a—C44a	1.43 (3)
Co—N81/7a	2.14 (3)	C22a—C48a	2.50 (2)
Co—C64aⁱ	2.782 (8)	C22a—C49a	2.911 (18)
Co—C34bⁱ	2.780 (11)	C23a—C26a	2.359 (12)
Co—C38bⁱ	2.774 (9)	C23a—C27a	1.45 (2)
Baa—Bab	1.657 (11)	C23a—C41a	2.44 (2)
Baa—C57a	2.844 (16)	C23a—C45a	2.83 (3)
Baa—C61a	2.947 (13)	C23a—C49a	2.50 (3)
Baa—C65a	2.992 (15)	C24a—C25a	2.359 (12)
Baa—C68a	2.931 (15)	C24a—C28a	1.445 (13)
Baa—C69a	2.78 (2)	C24a—C42a	2.44 (2)
Baa—C71a	2.70 (2)	C24a—C46a	2.83 (2)
Baa—C73a	2.85 (3)	C24a—C50a	2.498 (18)
Baa—C46b	2.96 (2)	C25a—C28a	1.445 (15)
Baa—C60b	2.983 (14)	C25a—C43a	2.44 (2)
Baa—C64b	2.77 (2)	C25a—C47a	2.83 (2)
Baa—C65b	3.005 (13)	C25a—C50a	2.50 (2)
Baa—C68b	2.67 (2)	C26a—C27a	1.445 (17)
Baa—C69b	2.767 (15)	C26a—C44a	2.44 (2)
Baa—C74b	2.949 (13)	C26a—C48a	2.83 (3)
Bab—C17a	2.994 (18)	C26a—C49a	2.50 (2)
Bab—C21a	2.65 (2)	C27a—C41a	2.834 (14)
Bab—C25a	2.72 (3)	C27a—C44a	2.834 (17)
Bab—C28a	2.71 (2)	C27a—C45a	2.44 (2)
Bab—C43a	2.791 (9)	C27a—C48a	2.44 (2)
Bab—C47a	2.784 (9)	C27a—C49a	1.42 (3)
Bab—C50a	2.735 (10)	C28a—C42a	2.83 (2)
Bab—C36b	2.821 (10)	C28a—C43a	2.834 (16)
Bab—C40b	2.673 (11)	C28a—C46a	2.44 (2)
Bab—C44b	2.773 (11)	C28a—C47a	2.44 (2)
Bab—C48b	2.897 (11)	C28a—C50a	1.42 (2)
Bab—C58b	2.939 (10)	C29a—C31a	1.439 (18)
Bab—C62b	2.73 (2)	C29a—C33a	1.45 (3)
Bab—C66b	2.87 (2)	C29a—C35a	2.334 (13)
C91a—C92aⁱⁱ	2.68 (4)	C29a—C37a	2.46 (3)
C91a—C93a	2.32 (4)	C29a—C41a	2.84 (2)
C91a—C93aⁱⁱ	2.25 (4)	C29a—C52a	2.36 (2)
C91b—C92b	2.09 (3)	C30a—C32a	1.439 (18)
C91b—C92bⁱⁱ	2.45 (3)	C30a—C34a	1.45 (2)
C91b—C93b	2.57 (4)	C30a—C36a	2.33 (3)
C92a—C92aⁱⁱ	2.46 (4)	C30a—C38a	2.456 (14)
C92a—C93a	1.37 (4)	C30a—C42a	2.839 (14)
C92a—C93aⁱⁱ	2.56 (3)	C30a—C51a	2.36 (3)
C92b—C93b	1.57 (3)	C31a—C33a	2.33 (3)
C92b—C93bⁱⁱ	2.59 (4)	C31a—C35a	1.45 (2)
C93b—C93bⁱⁱ	2.50 (4)	C31a—C39a	2.456 (15)
C94—C95	1.29 (3)	C31a—C43a	2.839 (13)
C94—C96	2.63 (3)	C31a—C52a	2.36 (3)
C94—C98	2.65 (2)	C32a—C34a	2.334 (13)
C94—C99	1.61 (3)	C32a—C36a	1.45 (3)
C95—C96	1.73 (3)	C32a—C40a	2.46 (3)
C95—C97	2.59 (3)	C32a—C44a	2.84 (2)
C95—C98	2.92 (3)	C32a—C51a	2.36 (2)
C95—C99	2.46 (3)	C33a—C35a	2.318 (18)
C96—C97	1.23 (3)	C33a—C37a	1.40 (2)
C96—C98	2.48 (3)	C33a—C41a	2.469 (14)
C96—C99	2.89 (3)	C33a—C52a	1.442 (13)
C97—C98	1.68 (3)	C33a—C53a	2.476 (18)
C97—C99	2.61 (3)	C33a—C55a	2.85 (2)
C98—C99	1.36 (3)	C33a—C59a	2.47 (3)
N81a—C82a	1.40 (2)	C34a—C36a	2.318 (18)
N81a—C83a	2.322 (11)	C34a—C38a	1.399 (14)
N81a—C84a	2.55 (3)	C34a—C42a	2.47 (2)
N81a—N81/1a	2.841 (8)	C34a—C51a	1.44 (3)
N81a—N81/4a	2.840 (8)	C34a—C54a	2.48 (3)
N81a—N81/5a	2.85 (2)	C34a—C56a	2.85 (2)
N81a—C82/5a	2.97 (3)	C34a—C60a	2.471 (14)
N81a—C84/5a	2.55 (3)	C35a—C39a	1.399 (13)
N81a—C82/6a	1.40 (2)	C35a—C43a	2.469 (18)
N81a—C83/6a	2.322 (11)	C35a—C52a	1.44 (3)
N81a—C84/6a	2.55 (3)	C35a—C53a	2.48 (3)
N81a—N81/7a	2.85 (2)	C35a—C57a	2.85 (2)
N81a—C82/7a	2.97 (3)	C35a—C61a	2.471 (16)
C82a—C83a	1.465 (12)	C36a—C40a	1.40 (2)
C82a—C84a	1.42 (3)	C36a—C44a	2.469 (13)
C82a—C85a	2.634 (11)	C36a—C51a	1.442 (13)
C82a—N81/1a	2.970 (11)	C36a—C54a	2.476 (17)
C82a—C82/6a	2.247 (11)	C36a—C58a	2.85 (2)
C82a—C83/6a	2.29 (2)	C36a—C62a	2.47 (2)
C82a—N81/7a	2.970 (11)	C37a—C41a	1.439 (14)
C82a—C82/7a	2.41 (2)	C37a—C45a	2.318 (14)
C83a—C84a	2.51 (2)	C37a—C52a	2.464 (15)
C83a—C85a	1.532 (19)	C37a—C53a	2.852 (13)
C83a—C86a	2.534 (18)	C37a—C55a	2.471 (18)
C83a—C82/6a	2.29 (2)	C37a—C59a	1.45 (2)
C83a—C83/6a	1.367 (11)	C37a—C63a	2.35 (2)
C83a—C85/6a	2.62 (2)	C38a—C42a	1.44 (3)
C84a—N81/1a	2.550 (9)	C38a—C46a	2.318 (17)
C84a—N81/7a	2.550 (9)	C38a—C51a	2.46 (2)
C84a—C82/7a	1.415 (12)	C38a—C54a	2.85 (3)
C84a—C83/7a	2.51 (2)	C38a—C56a	2.47 (3)
C85a—C86a	1.565 (13)	C38a—C60a	1.45 (2)
C85a—C83/6a	2.62 (2)	C38a—C64a	2.346 (12)
C1a—C3a	2.318 (18)	C39a—C43a	1.44 (2)
C1a—C4a	2.852 (12)	C39a—C47a	2.318 (14)
C1a—C5a	1.40 (2)	C39a—C52a	2.46 (2)
C1a—C8a	2.471 (17)	C39a—C53a	2.85 (3)
C1a—C9a	2.476 (14)	C39a—C57a	2.47 (3)
C1a—C10a	1.44 (2)	C39a—C61a	1.45 (2)
C1a—C11a	1.454 (13)	C39a—C65a	2.346 (15)
C1a—C13a	2.334 (13)	C40a—C44a	1.439 (16)
C1a—C15a	2.51 (2)	C40a—C48a	2.318 (12)
C1a—C19a	2.90 (3)	C40a—C51a	2.464 (14)
C1a—C23a	2.47 (3)	C40a—C54a	2.852 (13)
C2a—C3a	2.852 (12)	C40a—C58a	2.471 (17)
C2a—C4a	2.318 (18)	C40a—C62a	1.45 (2)
C2a—C6a	1.399 (13)	C40a—C66a	2.346 (17)
C2a—C7a	2.471 (13)	C41a—C45a	1.45 (2)
C2a—C9a	1.442 (13)	C41a—C49a	2.498 (13)
C2a—C10a	2.476 (12)	C41a—C59a	2.35 (2)
C2a—C12a	1.45 (2)	C41a—C63a	2.36 (2)
C2a—C14a	2.33 (2)	C42a—C46a	1.445 (13)
C2a—C16a	2.51 (2)	C42a—C50a	2.498 (14)
C2a—C20a	2.900 (17)	C42a—C60a	2.35 (3)
C2a—C24a	2.469 (13)	C42a—C64a	2.36 (2)
C3a—C6a	2.471 (12)	C43a—C47a	1.445 (15)
C3a—C7a	1.399 (13)	C43a—C50a	2.498 (12)
C3a—C9a	2.476 (13)	C43a—C61a	2.35 (3)
C3a—C10a	1.442 (13)	C43a—C65a	2.36 (2)
C3a—C11a	2.33 (2)	C44a—C48a	1.445 (17)
C3a—C13a	1.454 (18)	C44a—C49a	2.497 (12)
C3a—C17a	2.514 (18)	C44a—C62a	2.35 (2)
C3a—C21a	2.900 (16)	C44a—C66a	2.36 (2)
C3a—C25a	2.469 (13)	C45a—C48a	2.437 (12)
C4a—C5a	2.471 (14)	C45a—C49a	1.423 (14)
C4a—C8a	1.40 (2)	C45a—C59a	2.318 (14)
C4a—C9a	1.44 (2)	C45a—C63a	1.45 (2)
C4a—C10a	2.476 (18)	C45a—C66a	2.834 (16)
C4a—C12a	2.334 (13)	C45a—C67a	2.497 (19)
C4a—C14a	1.454 (16)	C46a—C47a	2.437 (12)
C4a—C18a	2.51 (2)	C46a—C50a	1.42 (2)
C4a—C22a	2.90 (3)	C46a—C60a	2.32 (3)
C4a—C26a	2.47 (3)	C46a—C64a	1.45 (3)
C5a—C8a	1.454 (12)	C46a—C65a	2.834 (16)
C5a—C9a	2.85 (2)	C46a—C68a	2.50 (2)
C5a—C10a	2.46 (2)	C47a—C50a	1.423 (16)
C5a—C11a	2.456 (14)	C47a—C61a	2.32 (2)
C5a—C15a	2.877 (13)	C47a—C64a	2.83 (2)
C5a—C19a	2.50 (2)	C47a—C65a	1.45 (3)
C5a—C23a	1.44 (3)	C47a—C68a	2.50 (3)
C5a—C26a	2.35 (2)	C48a—C49a	1.423 (17)
C5a—C27a	2.32 (3)	C48a—C62a	2.318 (15)
C6a—C7a	1.454 (12)	C48a—C63a	2.834 (13)
C6a—C9a	2.464 (13)	C48a—C66a	1.45 (2)
C6a—C10a	2.852 (13)	C48a—C67a	2.497 (17)
C6a—C12a	2.456 (18)	C49a—C63a	2.498 (18)
C6a—C16a	2.88 (2)	C49a—C66a	2.50 (2)
C6a—C20a	2.50 (2)	C49a—C67a	2.91 (2)
C6a—C24a	1.439 (17)	C50a—C64a	2.50 (3)
C6a—C25a	2.346 (13)	C50a—C65a	2.50 (2)
C6a—C28a	2.318 (16)	C50a—C68a	2.91 (3)
C7a—C9a	2.852 (13)	C51a—C54a	1.42 (2)
C7a—C10a	2.464 (13)	C51a—C56a	2.476 (14)
C7a—C13a	2.456 (15)	C51a—C58a	2.48 (2)
C7a—C17a	2.877 (17)	C51a—C60a	2.852 (14)
C7a—C21a	2.500 (18)	C51a—C62a	2.852 (19)
C7a—C24a	2.346 (15)	C52a—C53a	1.42 (2)
C7a—C25a	1.439 (16)	C52a—C55a	2.48 (3)
C7a—C28a	2.318 (17)	C52a—C57a	2.476 (16)
C8a—C9a	2.46 (2)	C52a—C59a	2.85 (2)
C8a—C10a	2.85 (2)	C52a—C61a	2.852 (13)
C8a—C14a	2.456 (13)	C53a—C55a	1.44 (2)
C8a—C18a	2.877 (16)	C53a—C57a	1.442 (13)
C8a—C22a	2.50 (2)	C53a—C59a	2.464 (15)
C8a—C23a	2.345 (17)	C53a—C61a	2.46 (2)
C8a—C26a	1.44 (3)	C53a—C71a	2.357 (14)
C8a—C27a	2.32 (3)	C53a—C73a	2.36 (2)
C9a—C85/3aⁱⁱⁱ	3.008 (11)	C54a—C56a	1.442 (14)
C9a—C10a	1.420 (12)	C54a—C58a	1.442 (19)
C9a—C12a	2.357 (16)	C54a—C60a	2.46 (2)
C9a—C14a	2.36 (2)	C54a—C62a	2.464 (14)
C10a—C11a	2.357 (18)	C54a—C72a	2.357 (16)
C10a—C13a	2.357 (13)	C54a—C74a	2.357 (12)
C11a—C13a	1.439 (18)	C55a—C57a	2.318 (18)
C11a—C15a	1.43 (3)	C55a—C59a	1.399 (13)
C11a—C17a	2.499 (13)	C55a—C63a	2.469 (13)
C11a—C19a	2.50 (3)	C55a—C67a	2.900 (14)
C11a—C23a	2.84 (2)	C55a—C70a	2.514 (15)
C11a—C29a	2.42 (2)	C55a—C71a	2.334 (13)
C11a—C31a	2.815 (15)	C55a—C73a	1.454 (14)
C12a—C14a	1.439 (18)	C56a—C58a	2.318 (18)
C12a—C16a	1.427 (17)	C56a—C60a	1.40 (3)
C12a—C18a	2.50 (3)	C56a—C64a	2.47 (2)
C12a—C20a	2.495 (13)	C56a—C68a	2.900 (17)
C12a—C24a	2.839 (14)	C56a—C69a	2.514 (12)
C12a—C30a	2.42 (2)	C56a—C72a	2.334 (19)
C12a—C32a	2.81 (3)	C56a—C74a	1.454 (16)
C13a—C15a	2.50 (2)	C57a—C61a	1.40 (3)
C13a—C17a	1.427 (16)	C57a—C65a	2.47 (2)
C13a—C21a	2.495 (13)	C57a—C68a	2.900 (14)
C13a—C25a	2.839 (13)	C57a—C69a	2.514 (13)
C13a—C29a	2.81 (3)	C57a—C71a	1.45 (2)
C13a—C31a	2.42 (2)	C57a—C73a	2.33 (2)
C14a—C16a	2.499 (13)	C58a—C62a	1.399 (13)
C14a—C18a	1.43 (3)	C58a—C66a	2.469 (12)
C14a—C22a	2.50 (3)	C58a—C67a	2.900 (12)
C14a—C26a	2.84 (2)	C58a—C70a	2.514 (12)
C14a—C30a	2.815 (17)	C58a—C72a	1.454 (12)
C14a—C32a	2.42 (2)	C58a—C74a	2.334 (14)
C15a—C17a	2.926 (18)	C59a—C63a	1.439 (14)
C15a—C19a	1.47 (2)	C59a—C67a	2.500 (15)
C15a—C23a	2.490 (14)	C59a—C70a	2.877 (15)
C15a—C29a	1.427 (14)	C59a—C73a	2.456 (14)
C15a—C31a	2.499 (13)	C60a—C64a	1.439 (17)
C15a—C33a	2.51 (2)	C60a—C68a	2.500 (12)
C15a—C37a	2.88 (3)	C60a—C69a	2.876 (16)
C15a—C41a	2.49 (3)	C60a—C74a	2.46 (2)
C16a—C18a	2.926 (18)	C61a—C65a	1.439 (14)
C16a—C20a	1.470 (14)	C61a—C68a	2.500 (13)
C16a—C24a	2.490 (18)	C61a—C69a	2.88 (2)
C16a—C30a	1.43 (3)	C61a—C71a	2.46 (3)
C16a—C32a	2.50 (2)	C62a—C66a	1.439 (12)
C16a—C34a	2.51 (3)	C62a—C67a	2.500 (12)
C16a—C38a	2.88 (2)	C62a—C70a	2.876 (13)
C16a—C42a	2.490 (14)	C62a—C72a	2.456 (13)
C17a—C21a	1.470 (13)	C63a—C66a	2.438 (12)
C17a—C25a	2.490 (15)	C63a—C67a	1.429 (15)
C17a—C29a	2.50 (2)	C63a—C70a	2.490 (14)
C17a—C31a	1.43 (2)	C63a—C73a	2.839 (13)
C17a—C35a	2.51 (2)	C64a—C65a	2.438 (12)
C17a—C39a	2.88 (2)	C64a—C68a	1.428 (16)
C17a—C43a	2.490 (15)	C64a—C69a	2.49 (2)
C18a—C22a	1.47 (2)	C64a—C74a	2.84 (3)
C18a—C26a	2.490 (13)	C65a—C68a	1.43 (2)
C18a—C30a	2.499 (13)	C65a—C69a	2.49 (3)
C18a—C32a	1.427 (16)	C65a—C71a	2.84 (3)
C18a—C36a	2.51 (2)	C66a—C67a	1.428 (13)
C18a—C40a	2.88 (3)	C66a—C70a	2.490 (13)
C18a—C44a	2.49 (3)	C66a—C72a	2.839 (13)
C19a—C23a	1.428 (13)	C67a—C70a	1.470 (13)
C19a—C27a	2.497 (14)	C67a—C72a	2.495 (12)
C19a—C29a	2.495 (14)	C67a—C73a	2.495 (13)
C19a—C33a	2.900 (14)	C68a—C69a	1.47 (3)
C19a—C37a	2.50 (2)	C68a—C71a	2.50 (2)
C19a—C41a	1.43 (3)	C68a—C74a	2.50 (2)
C19a—C45a	2.50 (3)	C69a—C70a	2.926 (18)
C19a—C49a	2.91 (2)	C69a—C71a	1.427 (14)
C20a—C24a	1.43 (2)	C69a—C72a	2.499 (19)
C20a—C28a	2.497 (14)	C69a—C73a	2.499 (17)
C20a—C30a	2.50 (2)	C69a—C74a	1.427 (16)
C20a—C34a	2.90 (3)	C70a—C71a	2.499 (17)
C20a—C38a	2.50 (3)	C70a—C72a	1.427 (12)
C20a—C42a	1.43 (2)	C70a—C73a	1.427 (14)
C20a—C46a	2.497 (17)	C70a—C74a	2.499 (15)
C20a—C50a	2.911 (12)	C71a—C72a	2.815 (15)
C21a—C25a	1.428 (17)	C71a—C73a	1.439 (18)
C21a—C28a	2.497 (12)	C71a—C74a	2.419 (12)
C21a—C31a	2.495 (18)	C72a—C73a	2.419 (12)
C21a—C35a	2.90 (2)	C72a—C74a	1.439 (18)
C21a—C39a	2.50 (3)	C73a—C74a	2.815 (13)
C21a—C43a	1.43 (2)

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

Experimental details

Crystal data
Chemical formula	Ba⁻C₇₄[Co(OEP)](C6H₆)₂
M_r	1774.1
Crystal system, space group	Monoclinic, C2
Temperature (K)	100
a, b, c (Å)	25.169 (3), 15.018 (3), 19.429 (4)
β (°)	93.30 (2)
V (Å³)	7332 (2)
Z	4
Radiation type	Synchrotron, λ = 0.643 Å
µ (mm⁻¹)	0.63
Crystal size (mm)	0.04 × 0.04 × 0.02

Data collection
Diffractometer	Huber four circle / Bruker Smart 6000 CCD diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 3σ(I)] reflections	18394, 18394, 7590
R_int	0.132
θ_max (°)	17.0
(sin θ/λ)_max (Å⁻¹)	0.455

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.131, 0.186, 2.44
No. of reflections	18394
No. of parameters	97
No. of restraints	?
(Δ/σ)_max	0.148
Δρ_max, Δρ_min (e Å⁻³)	1.70, −3.15

Computer programs: SIR 97 (Altomare et al., 1997), Jana2000 (Petricek and Dusek, 2000).

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