A new alkaline earth metal tetra­fluoro­terephthalate: [Ba(tfBDC)(DMF)(EtOH)]

Smets, D.; Sobieray, M.; Ruschewitz, U.

doi:10.1107/S2414314616014097

metal-organic compounds

IUCrDATA

ISSN: 2414-3146

Volume 1| Part 9| September 2016| x161409

doi:10.1107/S2414314616014097

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A new alkaline earth metal tetrafluoroterephthalate: [Ba(tfBDC)(DMF)(EtOH)]

Daniel Smets,^a Miriam Sobieray ^a and Uwe Ruschewitz ^a ^*

^aUniversity of Cologne, Greinstrasse 6, D-50939 Cologne, Germany
^*Correspondence e-mail: uwe.ruschewitz@uni-koeln.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 27 August 2016; accepted 4 September 2016; online 13 September 2016)

[Ba(C₈F₄O₄)(C₃H₇NO)(C₂H₅OH)] or [Ba(tfBDC)(DMF)(EtOH)], where tfBDC²⁻ = tetrafluoroterephthalate, DMF = dimethylformamide, EtOH = ethanol, systematic name poly[(dimethylformamide-1κO)(ethanol-1κO)(μ₅-2,3,5,6-tetrafluorobenzenedicarboxylato-1:2κ²O¹;1:3κ²O^1′;4κO⁴;5κO^4′)barium(II)], has been synthesized by a diffusion controlled synthesis from an EtOH/DMF solution. In the crystal structure two crystallographically independent Ba²⁺ cations are linked by two crystallographically distinct tfBDC²⁻ anions to form a three-dimensional network structure. The coordination spheres of the first (CN = 8) and second (CN = 8) independent Ba cations are completed by the O atoms of DMF and EtOH molecules, with both EtOH molecules being disordered over two sets of sites (occupancy ratio 0.7:0.3 and 0.6:0.4, respectively).

Keywords: barium; coordination polymer; crystal structure; tetrafluoroterephthalate.

CCDC reference: 1502501

Structure description

Despite the high interest in coordination polymers with tetrafluoroterephthalate (tfBDC²⁻) as a bridging ligand, only few alkaline earth metal tetrafluoroterephthalates have been reported up to now. Only in 2014, three calcium-based tetrafluoroterephthalates were published, one of them crystallizing in the chiral space group P4₁2₁2 (Chen et al., 2014 ). Interesting pyrotechnical effects have been observed in several alkali and alkaline earth metal tetrafluoroterephthalates, and some of their crystal structures were examined (Blair et al., 2015 ). Ca(tfBDC)·4H₂O and Sr(tfBDC)·4H₂O were synthesized mechanochemically and their crystal structures were solved and refined from X-ray powder diffraction data (Al-Terkawi et al., 2016 ). Here we report the first barium-containing coordination polymer with tfBDC²⁻ as bridging ligand.

The asymmetric unit of [Ba(tfBDC)(DMF)(EtOH)] contains two crystallographically independent Ba²⁺ cations, two symmetry-independent tfBDC²⁻ anions, two dimethylformamide (DMF) and two ethanol (EtOH) molecules. Each Ba²⁺ cation forms a BaO₈ polyhedron with six oxygen atoms stemming from five different tfBDC²⁻ ligands (Figs. 1 and 2). The coordination spheres are completed by one DMF and one EtOH molecule for each polyhedron [Ba1—O = 2.677 (4)-2.886 (3) Å; Ba2—O = 2.603 (17)-2.867 (3) Å]. The two independent EtOH molecules are each disordered over two sets of sites, and only one of the two positions is shown in the figures. The observed Ba—O distances are in good agreement with those in comparable Ba²⁺ coordination polymers (Blair et al., 2015; Lo et al., 1998 ).

Figure 1
ORTEP plot of the coordination sphere around Ba1, drawn with displacement parameters at the 50% probability level. The BaO₈ polyhedron is highlighted in dark blue. Only one position of the disordered EtOH molecule is shown. Colour code: Ba (silver), O (red), N (dark blue), F (green), C (dark grey), H (white). [Symmetry code: (i) −x + 1, y + $[{1\over 2}]$ , −z + $[{3\over 2}]$ .]

Figure 2
ORTEP plot of the coordination sphere around Ba2, drawn with displacement parameters at the 50% probability level. The BaO₈ polyhedron is highlighted in light blue. Only one position of the disordered EtOH molecule is shown. Colour code: see Fig. 1

. [Symmetry codes: (i) −x + 1, y + $[{1\over 2}]$ , −z + $[{3\over 2}]$ ; (iii) x, −y + $[{3\over 2}]$ , z − $[{1\over 2}]$ ; (iv) x, y + 1, z; (v) −x, −y + 1, −z + 1; (vi) −x, y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (viii) −x + 1, −y + 1, −z + 1.]

The BaO₈ polyhedra are connected via common edges to form zigzag chains along [010]. These chains are shown in Fig. 3. Each chain contains only Ba1 or Ba2, respectively, as highlighted in Fig. 3. The Ba1—O and Ba2—O chains are very similar, but have a different orientation, as shown in Fig. 4. The arrangement of the Ba—O chains resembles the motif of a hexagonal rod packing. The tfBDC²⁻ ligands interconnect these chains in the (010) plane so that a three-dimensional network structure is formed. The shortest Ba—Ba separations within the chains are Ba1—Ba1 = 4.5122 (3) Å and Ba2—Ba2 = 4.4999 (3) Å. The distances between Ba²⁺ cations of different chains exceed 9.5 Å.

Figure 3
View along [001] highlighting the zigzag chains of connected BaO₈ polyhedra extending in the [010] direction. Only tfbdc²⁻ ligands are shown and given in a wires/sticks representation. Colour code: see Fig. 1

Figure 4
View along [010] in direction of the Ba–O zigzag chains. tfbdc²⁻ ligands are shown in a wires/sticks representation, EtOH and DMF as ball and sticks. Colour code: see Fig. 1

Each tfBDC²⁻ linker coordinates to five Ba²⁺ cations. One carboxylate group of each tfBDC²⁻ linker (O19—C18—O18 and O1—C1—O2) bridges two Ba²⁺ cations in a monodentate fashion, whereas the other carboxylate groups (O11—C11—O12 and O9—C9—O10) bridge three Ba²⁺ cations in a bis-monodentate and chelating fashion. As found in many other tetrafluoroterephthalates, the tfBDC²⁻ linker is not planar, with the carboxylate groups twisted out of the plane of the benzene rings (Seidel et al., 2011 ). The respective torsion angles are 51.3 (3)° / 64.4 (2)° for linker I (C1–C9) and 35.4 (2)° / 48.8 (2)° for linker II (C11–C18). Both ethanol molecules are involved in hydrogen bonds, as indicated by the short O⋯O distances: O50⋯O1 = 2.68 (1) Å, O40′⋯O30 = 2.55 (3) Å, O40⋯O19 = 2.759 (8) Å. Since these hydrogen bonds only connect ethanol molecules to other oxygen atoms within the same BaO₈ coordination polyhedron, the three-dimensional network structure of [Ba(tfBDC)(DMF)(EtOH)] is entirely held together by coordinating bonds.

Synthesis and crystallization

In a snap-cap tube 61.4 mg (0.15 mmol, 1 eq.) BaI₂·H₂O and 35.6 mg (0.15 mmol, 1 eq.) H₂tfBDC (tetrafluoroterephthalic acid) were dissolved in 1.1 ml of a mixture of EtOH/DMF (3:1, v/v). The tube was closed with a cap and the latter was perforated once. This tube was then placed in a bigger one, which contained the same solvent mixture and an additional amount of 1.25 ml triethylamine. The bigger tube was closed with a non-perforated cap. After three weeks, rod-shaped colourless crystals were obtained, which are very sensitive, obviously due to an easy loss of solvent molecules. Therefore a single-crystal was isolated in perfluorinated oil for the diffraction experiment and cooled down to 170 K immediately.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1. The two crystallographically independent ethanol molecules are disordered and were refined using a split model with restraints and occupancies of 70:30 (O40/C40/C41/O40′/C40′/C41′) and 60:40 (C50/C51/C50′/C51′), respectively. The displacement parameters of the disordered atoms were refined isotropically and their bond lengths were set to ideal values by using the restraint command DFIX. The hydroxy H atoms of the disordered ethanol molecules could not be located in the final difference Fourier maps and were thus omitted in the final refinement.

Table 1
Experimental details

Crystal data
Chemical formula	[Ba(C₈F₄O₄)(C₃H₇NO)(C₂H₆O)]
M_r	492.58
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	21.4745 (8), 7.4295 (2), 26.1730 (11)
β (°)	127.366 (2)
V (Å³)	3318.8 (2)
Z	8
Radiation type	Mo Kα
μ (mm⁻¹)	2.47
Crystal size (mm)	0.35 × 0.2 × 0.1

Data collection
Diffractometer	STOE IPDS 2T
Absorption correction	Numerical (X-RED-32 and X-SHAPE; Stoe & Cie, 2002)
T_min, T_max	0.589, 0.808
No. of measured, independent and observed [I > 2σ(I)] reflections	39756, 7048, 5576
R_int	0.075
(sin θ/λ)_max (Å⁻¹)	0.634

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.099, 1.04
No. of reflections	7048
No. of parameters	436
No. of restraints	10
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.82, −1.18
Computer programs: X-AREA (Stoe, 2002 ), SIR92 (Altomare et al., 1994 ), SHELXL2013 (Sheldrick, 2015 ), DIAMOND (Brandenburg, 1999 ) and publCIF (Westrip, 2010 ).

Structural data

CCDC reference: 1502501

Crystal structure: contains datablock I. DOI: 10.1107/S2414314616014097/wm4024sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2414314616014097/wm4024Isup2.hkl

Supporting information file. DOI: 10.1107/S2414314616014097/wm4024Isup3.mol

checkCIF report

Computing details top

Data collection: X-AREA (Stoe, 2002); cell refinement: X-AREA (Stoe, 2002); data reduction: X-AREA (Stoe, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Poly[(dimethylformamide-1κO)(ethanol-1κO)(µ₅-2,3,5,6-tetrafluorobenzenedicarboxylato-1:2κ²O¹;1:3κ²O^1';4κO⁴;5κO^4')barium(II)] top

Crystal data top

[Ba(C₈F₄O₄)(C₃H₇NO)(C₂H₆O)]	F(000) = 1896
M_r = 492.58	D_x = 1.968 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 21.4745 (8) Å	Cell parameters from 19777 reflections
b = 7.4295 (2) Å	θ = 2.0–26.8°
c = 26.1730 (11) Å	µ = 2.47 mm⁻¹
β = 127.366 (2)°	T = 293 K
V = 3318.8 (2) Å³	Rod, colourless
Z = 8	0.35 × 0.2 × 0.1 mm

Data collection top

STOE IPDS 2T diffractometer	5576 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.075
Absorption correction: numerical (XRED-32 and XSHAPE; Stoe & Cie, 2002)	θ_max = 26.8°, θ_min = 2.0°
T_min = 0.589, T_max = 0.808	h = −27→27
39756 measured reflections	k = −9→9
7048 independent reflections	l = −33→33

Refinement top

Refinement on F²	10 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.038	H-atom parameters constrained
wR(F²) = 0.099	w = 1/[σ²(F_o²) + (0.0579P)² + 2.4924P] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max = 0.001
7048 reflections	Δρ_max = 1.82 e Å⁻³
436 parameters	Δρ_min = −1.18 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ba1	0.54553 (2)	0.20736 (4)	0.73378 (2)	0.02214 (9)
Ba2	0.04870 (2)	0.97090 (4)	0.31093 (2)	0.02406 (9)
F3	0.35904 (18)	0.4686 (6)	0.51315 (16)	0.0507 (10)
F4	0.23839 (19)	0.4857 (5)	0.38998 (15)	0.0469 (9)
F6	0.06587 (17)	0.4292 (5)	0.44316 (15)	0.0426 (8)
F7	0.18585 (18)	0.4252 (5)	0.56698 (15)	0.0433 (8)
F13	0.27083 (19)	0.1178 (5)	0.65661 (16)	0.0445 (8)
F14	0.14422 (18)	0.1505 (6)	0.64894 (17)	0.0505 (9)
F16	0.2977 (2)	0.3578 (6)	0.86381 (18)	0.0506 (9)
F17	0.42256 (19)	0.3398 (5)	0.86864 (17)	0.0475 (9)
O1	0.4015 (2)	0.3431 (6)	0.63339 (17)	0.0402 (9)
O2	0.6559 (2)	0.0624 (6)	0.85008 (19)	0.0424 (9)
O9	0.0705 (2)	0.6121 (5)	0.31403 (17)	0.0341 (8)
O10	0.0356 (2)	0.3338 (5)	0.31744 (16)	0.0291 (7)
O11	0.53018 (19)	−0.1568 (5)	0.71318 (17)	0.0265 (7)
O12	0.4348 (2)	0.0661 (5)	0.7489 (2)	0.0338 (8)
O18	0.1380 (3)	0.3946 (6)	0.7816 (3)	0.0572 (12)
O19	0.0914 (2)	0.1469 (6)	0.7214 (2)	0.0476 (10)
O20	0.6787 (2)	0.2181 (6)	0.7461 (2)	0.0463 (10)
O30	0.1902 (5)	0.9587 (10)	0.4261 (4)	0.095 (2)*
O50	0.5090 (3)	0.2685 (8)	0.6153 (3)	0.0698 (14)*
N20	0.8055 (3)	0.2099 (7)	0.7848 (3)	0.0401 (11)
N30	0.3132 (3)	0.9290 (8)	0.5129 (3)	0.0528 (14)
C1	0.3478 (3)	0.4508 (7)	0.6164 (2)	0.0316 (11)
C2	0.2774 (3)	0.4472 (7)	0.5454 (2)	0.0273 (10)
C3	0.2869 (3)	0.4590 (8)	0.4973 (2)	0.0325 (11)
C4	0.2242 (3)	0.4672 (7)	0.4335 (2)	0.0300 (11)
C5	0.1482 (3)	0.4571 (6)	0.4125 (2)	0.0253 (10)
C6	0.1387 (3)	0.4392 (7)	0.4600 (2)	0.0289 (10)
C7	0.2010 (3)	0.4382 (7)	0.5242 (2)	0.0286 (10)
C9	0.0792 (3)	0.4689 (6)	0.3426 (2)	0.0249 (10)
C11	0.4248 (3)	0.2118 (6)	0.7664 (2)	0.0256 (10)
C12	0.3519 (3)	0.2282 (6)	0.7632 (3)	0.0269 (10)
C13	0.2790 (3)	0.1794 (7)	0.7083 (3)	0.0309 (11)
C14	0.2127 (3)	0.1936 (7)	0.7053 (3)	0.0345 (12)
C15	0.2145 (3)	0.2545 (7)	0.7562 (3)	0.0334 (12)
C16	0.2878 (3)	0.3020 (7)	0.8108 (3)	0.0330 (12)
C17	0.3543 (3)	0.2916 (7)	0.8135 (3)	0.0322 (11)
C18	0.1413 (3)	0.2670 (8)	0.7535 (3)	0.0363 (12)
C20	0.7486 (3)	0.1856 (8)	0.7900 (3)	0.0405 (13)
H20	0.7617	0.1416	0.8287	0.049*
C21	0.8862 (4)	0.1656 (11)	0.8383 (4)	0.062 (2)
H21A	0.9197	0.1913	0.8264	0.093*
H21B	0.8897	0.0401	0.8484	0.093*
H21C	0.9022	0.2363	0.8751	0.093*
C22	0.7904 (4)	0.2747 (9)	0.7264 (3)	0.0477 (15)
H22A	0.8389	0.2834	0.7321	0.072*
H22B	0.7663	0.3913	0.7161	0.072*
H22C	0.7560	0.1926	0.6920	0.072*
C30	0.2595 (5)	0.9333 (13)	0.4528 (4)	0.074 (2)
H30	0.2745	0.9152	0.4266	0.089*
C31	0.2971 (7)	0.9511 (12)	0.5589 (5)	0.087 (3)
H31A	0.3453	0.9446	0.6017	0.131*
H31B	0.2625	0.8574	0.5529	0.131*
H31C	0.2730	1.0661	0.5526	0.131*
C32	0.3949 (6)	0.898 (2)	0.5417 (7)	0.147 (6)
H32A	0.4252	0.9009	0.5877	0.220*
H32B	0.4132	0.9896	0.5279	0.220*
H32C	0.4005	0.7820	0.5286	0.220*
O40	0.0241 (5)	0.9520 (11)	0.4043 (4)	0.069 (2)*	0.7
C40	0.0647 (8)	1.0064 (15)	0.4708 (5)	0.077 (3)*	0.7
H40A	0.0353	1.0945	0.4757	0.092*	0.7
H40B	0.1170	1.0515	0.4899	0.092*	0.7
C41	0.0660 (10)	0.8223 (17)	0.4973 (8)	0.087 (4)*	0.7
H41A	0.0918	0.8319	0.5426	0.131*	0.7
H41B	0.0939	0.7384	0.4900	0.131*	0.7
H41C	0.0133	0.7809	0.4760	0.131*	0.7
C50'	0.5375 (7)	0.2571 (14)	0.5775 (6)	0.058 (3)*	0.6
H50A	0.4951	0.2311	0.5328	0.069*	0.6
H50B	0.5774	0.1649	0.5941	0.069*	0.6
C51'	0.5713 (8)	0.4427 (15)	0.5848 (7)	0.072 (4)*	0.6
H51A	0.5919	0.4485	0.5609	0.107*	0.6
H51B	0.6126	0.4656	0.6294	0.107*	0.6
H51C	0.5309	0.5314	0.5687	0.107*	0.6
O40'	0.0662 (12)	0.969 (2)	0.4185 (9)	0.062 (5)*	0.3
C40'	0.0422 (14)	0.844 (4)	0.4449 (9)	0.076 (8)*	0.3
H40C	0.0400	0.7231	0.4300	0.091*	0.3
H40D	−0.0092	0.8756	0.4324	0.091*	0.3
C41'	0.1047 (13)	0.856 (3)	0.5193 (9)	0.044 (5)*	0.3
H41D	0.0912	0.7736	0.5395	0.067*	0.3
H41E	0.1061	0.9762	0.5333	0.067*	0.3
H41F	0.1552	0.8250	0.5309	0.067*	0.3
C50	0.5493 (10)	0.375 (2)	0.5953 (8)	0.057 (4)*	0.4
H50C	0.6043	0.3917	0.6308	0.068*	0.4
H50D	0.5248	0.4915	0.5785	0.068*	0.4
C51	0.5390 (18)	0.256 (4)	0.5426 (12)	0.113 (9)*	0.4
H51D	0.5629	0.3141	0.5256	0.170*	0.4
H51E	0.4842	0.2389	0.5088	0.170*	0.4
H51F	0.5635	0.1417	0.5605	0.170*	0.4

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.01810 (14)	0.02236 (14)	0.02548 (15)	0.00131 (10)	0.01298 (12)	0.00198 (11)
Ba2	0.01982 (15)	0.02342 (15)	0.02311 (15)	−0.00225 (10)	0.01000 (12)	0.00058 (11)
F3	0.0188 (15)	0.093 (3)	0.0347 (17)	0.0036 (16)	0.0132 (14)	0.0115 (18)
F4	0.0343 (18)	0.079 (3)	0.0306 (16)	0.0061 (17)	0.0214 (15)	0.0093 (17)
F6	0.0188 (15)	0.071 (2)	0.0307 (16)	−0.0013 (15)	0.0113 (13)	0.0017 (16)
F7	0.0295 (16)	0.072 (2)	0.0278 (15)	0.0013 (16)	0.0172 (14)	0.0036 (16)
F13	0.0337 (17)	0.061 (2)	0.0418 (18)	−0.0033 (16)	0.0247 (15)	−0.0107 (17)
F14	0.0227 (16)	0.079 (3)	0.0448 (19)	−0.0064 (16)	0.0177 (15)	−0.0097 (19)
F16	0.045 (2)	0.069 (2)	0.055 (2)	−0.0086 (18)	0.0383 (18)	−0.0189 (19)
F17	0.0314 (17)	0.067 (2)	0.0470 (19)	−0.0147 (16)	0.0251 (16)	−0.0211 (18)
O1	0.0225 (19)	0.057 (3)	0.0282 (19)	0.0068 (18)	0.0089 (16)	0.0045 (18)
O2	0.034 (2)	0.048 (2)	0.032 (2)	0.0015 (18)	0.0134 (18)	0.0079 (18)
O9	0.0319 (19)	0.0285 (19)	0.0265 (18)	0.0031 (15)	0.0096 (16)	0.0035 (15)
O10	0.0300 (19)	0.0248 (17)	0.0262 (17)	−0.0022 (14)	0.0138 (16)	−0.0028 (14)
O11	0.0247 (17)	0.0253 (17)	0.0345 (18)	0.0024 (14)	0.0206 (16)	−0.0007 (15)
O12	0.0314 (19)	0.0242 (17)	0.056 (2)	0.0022 (15)	0.0316 (19)	0.0009 (17)
O18	0.054 (3)	0.048 (3)	0.102 (4)	0.004 (2)	0.064 (3)	−0.002 (3)
O19	0.031 (2)	0.060 (3)	0.057 (3)	−0.006 (2)	0.029 (2)	0.001 (2)
O20	0.031 (2)	0.053 (3)	0.059 (3)	0.0053 (19)	0.029 (2)	0.009 (2)
N20	0.028 (2)	0.040 (3)	0.053 (3)	−0.002 (2)	0.025 (2)	−0.006 (2)
N30	0.032 (3)	0.058 (3)	0.037 (3)	−0.005 (2)	0.004 (2)	0.003 (3)
C1	0.023 (3)	0.039 (3)	0.024 (2)	−0.002 (2)	0.010 (2)	0.000 (2)
C2	0.025 (3)	0.028 (3)	0.025 (2)	0.000 (2)	0.013 (2)	−0.001 (2)
C3	0.018 (2)	0.044 (3)	0.027 (2)	0.001 (2)	0.009 (2)	0.003 (2)
C4	0.025 (3)	0.040 (3)	0.024 (2)	0.002 (2)	0.013 (2)	0.002 (2)
C5	0.023 (2)	0.023 (2)	0.019 (2)	0.0008 (19)	0.007 (2)	0.0013 (18)
C6	0.020 (2)	0.033 (3)	0.026 (2)	−0.002 (2)	0.010 (2)	−0.001 (2)
C7	0.024 (2)	0.037 (3)	0.020 (2)	0.003 (2)	0.011 (2)	0.002 (2)
C9	0.022 (2)	0.025 (2)	0.023 (2)	0.0013 (19)	0.012 (2)	−0.002 (2)
C11	0.022 (2)	0.026 (2)	0.033 (3)	0.0037 (19)	0.019 (2)	0.005 (2)
C12	0.026 (2)	0.023 (2)	0.041 (3)	0.0009 (19)	0.025 (2)	0.000 (2)
C13	0.032 (3)	0.030 (3)	0.040 (3)	0.000 (2)	0.027 (2)	0.001 (2)
C14	0.022 (3)	0.036 (3)	0.043 (3)	−0.002 (2)	0.018 (2)	0.001 (2)
C15	0.029 (3)	0.028 (3)	0.052 (3)	0.000 (2)	0.029 (3)	0.004 (2)
C16	0.034 (3)	0.033 (3)	0.045 (3)	−0.004 (2)	0.030 (3)	−0.007 (2)
C17	0.027 (3)	0.033 (3)	0.038 (3)	−0.003 (2)	0.020 (2)	−0.005 (2)
C18	0.031 (3)	0.035 (3)	0.053 (3)	0.005 (2)	0.031 (3)	0.010 (3)
C20	0.031 (3)	0.039 (3)	0.049 (3)	0.000 (2)	0.022 (3)	0.000 (3)
C21	0.025 (3)	0.076 (5)	0.068 (5)	0.000 (3)	0.020 (3)	−0.024 (4)
C22	0.045 (4)	0.041 (3)	0.072 (4)	−0.003 (3)	0.044 (4)	0.002 (3)
C30	0.053 (5)	0.082 (6)	0.064 (5)	−0.011 (4)	0.023 (4)	0.007 (4)
C31	0.123 (8)	0.058 (5)	0.073 (6)	−0.012 (5)	0.056 (6)	0.001 (4)
C32	0.043 (6)	0.158 (13)	0.173 (13)	−0.012 (7)	0.031 (7)	−0.037 (11)

Geometric parameters (Å, º) top

Ba1—O20	2.677 (4)	C2—C7	1.378 (7)
Ba1—O12ⁱ	2.694 (4)	C2—C3	1.394 (7)
Ba1—O2	2.699 (4)	C3—C4	1.371 (7)
Ba1—O50	2.737 (5)	C4—C5	1.373 (7)
Ba1—O11	2.739 (3)	C5—C6	1.385 (7)
Ba1—O1	2.761 (4)	C5—C9	1.503 (6)
Ba1—O12	2.837 (3)	C6—C7	1.372 (7)
Ba1—O11ⁱ	2.886 (3)	C9—Ba2^vii	3.209 (5)
Ba1—C11	3.183 (4)	C11—O11ⁱ	1.243 (6)
Ba1—Ba1ⁱⁱ	4.5122 (3)	C11—C12	1.522 (6)
Ba1—Ba1ⁱ	4.5122 (3)	C12—C17	1.369 (7)
Ba2—O40'	2.603 (17)	C12—C13	1.385 (8)
Ba2—O18ⁱⁱⁱ	2.654 (4)	C13—C14	1.381 (7)
Ba2—O30	2.685 (8)	C14—C15	1.385 (8)
Ba2—O9	2.699 (4)	C15—C16	1.384 (8)
Ba2—O10^iv	2.727 (4)	C15—C18	1.532 (7)
Ba2—O19^v	2.728 (4)	C16—C17	1.387 (7)
Ba2—O40	2.799 (8)	C20—H20	0.9300
Ba2—O9^vi	2.862 (4)	C21—H21A	0.9600
Ba2—O10^vi	2.867 (3)	C21—H21B	0.9600
Ba2—C9^vi	3.209 (5)	C21—H21C	0.9600
Ba2—Ba2^vi	4.4999 (3)	C22—H22A	0.9600
Ba2—Ba2^vii	4.4999 (3)	C22—H22B	0.9600
F3—C3	1.340 (6)	C22—H22C	0.9600
F4—C4	1.352 (6)	C30—H30	0.9300
F6—C6	1.345 (6)	C31—H31A	0.9600
F7—C7	1.346 (6)	C31—H31B	0.9600
F13—C13	1.335 (6)	C31—H31C	0.9600
F14—C14	1.345 (6)	C32—H32A	0.9600
F16—C16	1.336 (6)	C32—H32B	0.9600
F17—C17	1.339 (6)	C32—H32C	0.9600
O1—C1	1.243 (6)	O40—C40	1.454 (9)
O2—C1ⁱⁱ	1.246 (7)	C40—C41	1.526 (9)
O9—C9	1.248 (6)	C40—H40A	0.9700
O9—Ba2^vii	2.862 (4)	C40—H40B	0.9700
O10—C9	1.252 (6)	C41—H41A	0.9600
O10—Ba2^viii	2.727 (3)	C41—H41B	0.9600
O10—Ba2^vii	2.867 (3)	C41—H41C	0.9600
O11—C11ⁱⁱ	1.243 (6)	C50'—C51'	1.516 (9)
O11—Ba1ⁱⁱ	2.886 (3)	C50'—H50A	0.9700
O12—C11	1.244 (6)	C50'—H50B	0.9700
O12—Ba1ⁱⁱ	2.694 (4)	C51'—H51A	0.9600
O18—C18	1.230 (7)	C51'—H51B	0.9600
O18—Ba2^ix	2.654 (4)	C51'—H51C	0.9600
O19—C18	1.248 (7)	O40'—C40'	1.430 (10)
O19—Ba2^v	2.728 (4)	C40'—C41'	1.558 (10)
O20—C20	1.240 (7)	C40'—H40C	0.9700
O30—C30	1.214 (10)	C40'—H40D	0.9700
O50—C50'	1.447 (8)	C41'—H41D	0.9600
O50—C50	1.481 (9)	C41'—H41E	0.9600
N20—C20	1.320 (7)	C41'—H41F	0.9600
N20—C22	1.441 (8)	C50—C51	1.535 (10)
N20—C21	1.458 (8)	C50—H50C	0.9700
N30—C30	1.267 (10)	C50—H50D	0.9700
N30—C32	1.448 (11)	C51—H51D	0.9600
N30—C31	1.448 (11)	C51—H51E	0.9600
C1—O2ⁱ	1.246 (7)	C51—H51F	0.9600
C1—C2	1.526 (7)

O20—Ba1—O12ⁱ	84.46 (12)	C20—N20—C22	121.9 (5)
O20—Ba1—O2	74.51 (13)	C20—N20—C21	120.4 (6)
O12ⁱ—Ba1—O2	105.31 (13)	C22—N20—C21	117.7 (5)
O20—Ba1—O50	71.47 (15)	C30—N30—C32	123.6 (9)
O12ⁱ—Ba1—O50	86.25 (15)	C30—N30—C31	122.2 (8)
O2—Ba1—O50	142.71 (15)	C32—N30—C31	114.2 (9)
O20—Ba1—O11	92.61 (12)	O1—C1—O2ⁱ	128.2 (5)
O12ⁱ—Ba1—O11	176.68 (10)	O1—C1—C2	116.3 (5)
O2—Ba1—O11	75.31 (12)	O2ⁱ—C1—C2	115.5 (5)
O50—Ba1—O11	91.34 (14)	C7—C2—C3	115.5 (4)
O20—Ba1—O1	126.98 (13)	C7—C2—C1	123.2 (4)
O12ⁱ—Ba1—O1	76.67 (12)	C3—C2—C1	121.2 (4)
O2—Ba1—O1	158.26 (12)	F3—C3—C4	118.1 (5)
O50—Ba1—O1	58.39 (14)	F3—C3—C2	119.9 (4)
O11—Ba1—O1	104.00 (12)	C4—C3—C2	122.0 (5)
O20—Ba1—O12	156.67 (12)	F4—C4—C3	118.4 (4)
O12ⁱ—Ba1—O12	113.66 (8)	F4—C4—C5	119.3 (4)
O2—Ba1—O12	86.11 (12)	C3—C4—C5	122.4 (5)
O50—Ba1—O12	122.10 (14)	C4—C5—C6	115.7 (4)
O11—Ba1—O12	69.58 (10)	C4—C5—C9	122.6 (4)
O1—Ba1—O12	73.64 (12)	C6—C5—C9	121.6 (4)
O20—Ba1—O11ⁱ	143.49 (12)	F6—C6—C7	118.5 (4)
O12ⁱ—Ba1—O11ⁱ	69.47 (10)	F6—C6—C5	119.1 (4)
O2—Ba1—O11ⁱ	87.86 (11)	C7—C6—C5	122.3 (5)
O50—Ba1—O11ⁱ	129.03 (14)	F7—C7—C6	118.0 (4)
O11—Ba1—O11ⁱ	113.85 (8)	F7—C7—C2	119.9 (4)
O1—Ba1—O11ⁱ	72.39 (11)	C6—C7—C2	122.1 (5)
O12—Ba1—O11ⁱ	45.42 (10)	O9—C9—O10	125.2 (4)
O20—Ba1—C11	162.04 (14)	O9—C9—C5	117.2 (4)
O12ⁱ—Ba1—C11	90.82 (11)	O10—C9—C5	117.6 (4)
O2—Ba1—C11	90.16 (12)	O9—C9—Ba2^vii	62.8 (2)
O50—Ba1—C11	125.61 (15)	O10—C9—Ba2^vii	63.0 (2)
O11—Ba1—C11	92.45 (11)	C5—C9—Ba2^vii	170.6 (3)
O1—Ba1—C11	68.11 (12)	O11ⁱ—C11—O12	125.4 (4)
O12—Ba1—C11	22.93 (11)	O11ⁱ—C11—C12	117.8 (4)
O11ⁱ—Ba1—C11	22.97 (11)	O12—C11—C12	116.8 (4)
O20—Ba1—Ba1ⁱⁱ	123.72 (10)	O11ⁱ—C11—Ba1	65.0 (2)
O12ⁱ—Ba1—Ba1ⁱⁱ	145.52 (7)	O12—C11—Ba1	62.7 (2)
O2—Ba1—Ba1ⁱⁱ	69.13 (9)	C12—C11—Ba1	164.7 (3)
O50—Ba1—Ba1ⁱⁱ	119.42 (12)	C17—C12—C13	116.5 (4)
O11—Ba1—Ba1ⁱⁱ	37.79 (6)	C17—C12—C11	122.6 (5)
O1—Ba1—Ba1ⁱⁱ	96.70 (9)	C13—C12—C11	120.9 (4)
O12—Ba1—Ba1ⁱⁱ	34.29 (7)	F13—C13—C14	118.2 (5)
O11ⁱ—Ba1—Ba1ⁱⁱ	76.25 (7)	F13—C13—C12	120.8 (4)
C11—Ba1—Ba1ⁱⁱ	56.06 (9)	C14—C13—C12	121.1 (5)
O20—Ba1—Ba1ⁱ	120.38 (10)	F14—C14—C13	116.5 (5)
O12ⁱ—Ba1—Ba1ⁱ	36.40 (7)	F14—C14—C15	120.4 (5)
O2—Ba1—Ba1ⁱ	107.49 (9)	C13—C14—C15	123.0 (5)
O50—Ba1—Ba1ⁱ	102.58 (12)	C16—C15—C14	115.2 (5)
O11—Ba1—Ba1ⁱ	146.72 (6)	C16—C15—C18	121.6 (5)
O1—Ba1—Ba1ⁱ	61.01 (9)	C14—C15—C18	123.1 (5)
O12—Ba1—Ba1ⁱ	77.45 (7)	F16—C16—C15	121.0 (4)
O11ⁱ—Ba1—Ba1ⁱ	35.57 (7)	F16—C16—C17	117.0 (5)
C11—Ba1—Ba1ⁱ	54.87 (9)	C15—C16—C17	122.0 (5)
Ba1ⁱⁱ—Ba1—Ba1ⁱ	110.827 (11)	F17—C17—C12	120.4 (4)
O40'—Ba2—O18ⁱⁱⁱ	131.2 (5)	F17—C17—C16	117.4 (5)
O40'—Ba2—O30	57.6 (5)	C12—C17—C16	122.2 (5)
O18ⁱⁱⁱ—Ba2—O30	79.2 (2)	O18—C18—O19	128.0 (5)
O40'—Ba2—O9	93.1 (4)	O18—C18—C15	116.8 (5)
O18ⁱⁱⁱ—Ba2—O9	103.75 (13)	O19—C18—C15	115.2 (5)
O30—Ba2—O9	82.84 (17)	O20—C20—N20	123.6 (6)
O40'—Ba2—O10^iv	83.7 (4)	O20—C20—H20	118.2
O18ⁱⁱⁱ—Ba2—O10^iv	76.45 (12)	N20—C20—H20	118.2
O30—Ba2—O10^iv	93.01 (17)	N20—C21—H21A	109.5
O9—Ba2—O10^iv	175.70 (10)	N20—C21—H21B	109.5
O40'—Ba2—O19^v	75.1 (5)	H21A—C21—H21B	109.5
O18ⁱⁱⁱ—Ba2—O19^v	152.23 (16)	N20—C21—H21C	109.5
O30—Ba2—O19^v	128.43 (18)	H21A—C21—H21C	109.5
O9—Ba2—O19^v	80.29 (13)	H21B—C21—H21C	109.5
O10^iv—Ba2—O19^v	101.56 (12)	N20—C22—H22A	109.5
O18ⁱⁱⁱ—Ba2—O40	145.4 (2)	N20—C22—H22B	109.5
O30—Ba2—O40	72.7 (2)	H22A—C22—H22B	109.5
O9—Ba2—O40	92.61 (19)	N20—C22—H22C	109.5
O10^iv—Ba2—O40	85.06 (19)	H22A—C22—H22C	109.5
O19^v—Ba2—O40	59.9 (2)	H22B—C22—H22C	109.5
O40'—Ba2—O9^vi	132.8 (4)	O30—C30—N30	126.4 (10)
O18ⁱⁱⁱ—Ba2—O9^vi	80.44 (14)	O30—C30—H30	116.8
O30—Ba2—O9^vi	155.96 (17)	N30—C30—H30	116.8
O9—Ba2—O9^vi	114.53 (9)	N30—C31—H31A	109.5
O10^iv—Ba2—O9^vi	69.77 (10)	N30—C31—H31B	109.5
O19^v—Ba2—O9^vi	73.11 (12)	H31A—C31—H31B	109.5
O40—Ba2—O9^vi	120.3 (2)	N30—C31—H31C	109.5
O40'—Ba2—O10^vi	147.1 (4)	H31A—C31—H31C	109.5
O18ⁱⁱⁱ—Ba2—O10^vi	81.28 (14)	H31B—C31—H31C	109.5
O30—Ba2—O10^vi	141.53 (17)	N30—C32—H32A	109.5
O9—Ba2—O10^vi	70.06 (10)	N30—C32—H32B	109.5
O10^iv—Ba2—O10^vi	114.13 (8)	H32A—C32—H32B	109.5
O19^v—Ba2—O10^vi	74.28 (12)	N30—C32—H32C	109.5
O40—Ba2—O10^vi	133.3 (2)	H32A—C32—H32C	109.5
O9^vi—Ba2—O10^vi	45.60 (10)	H32B—C32—H32C	109.5
O40'—Ba2—C9^vi	143.7 (5)	C40—O40—Ba2	137.5 (7)
O18ⁱⁱⁱ—Ba2—C9^vi	81.90 (15)	O40—C40—C41	97.3 (9)
O30—Ba2—C9^vi	158.58 (18)	O40—C40—H40A	112.3
O9—Ba2—C9^vi	91.95 (11)	C41—C40—H40A	112.3
O10^iv—Ba2—C9^vi	92.33 (11)	O40—C40—H40B	112.3
O19^v—Ba2—C9^vi	70.44 (13)	C41—C40—H40B	112.3
O40—Ba2—C9^vi	128.4 (2)	H40A—C40—H40B	109.9
O9^vi—Ba2—C9^vi	22.82 (11)	C40—C41—H41A	109.5
O10^vi—Ba2—C9^vi	22.91 (11)	C40—C41—H41B	109.5
O40'—Ba2—Ba2^vi	118.1 (4)	H41A—C41—H41B	109.5
O18ⁱⁱⁱ—Ba2—Ba2^vi	65.86 (11)	C40—C41—H41C	109.5
O30—Ba2—Ba2^vi	123.09 (16)	H41A—C41—H41C	109.5
O9—Ba2—Ba2^vi	146.52 (7)	H41B—C41—H41C	109.5
O10^iv—Ba2—Ba2^vi	37.52 (7)	O50—C50'—C51'	103.3 (7)
O19^v—Ba2—Ba2^vi	95.39 (10)	O50—C50'—H50A	111.1
O40—Ba2—Ba2^vi	114.04 (18)	C51'—C50'—H50A	111.1
O9^vi—Ba2—Ba2^vi	34.78 (7)	O50—C50'—H50B	111.1
O10^vi—Ba2—Ba2^vi	76.78 (7)	C51'—C50'—H50B	111.1
C9^vi—Ba2—Ba2^vi	55.93 (9)	H50A—C50'—H50B	109.1
O40'—Ba2—Ba2^vii	117.5 (4)	C50'—C51'—H51A	109.5
O18ⁱⁱⁱ—Ba2—Ba2^vii	102.27 (11)	C50'—C51'—H51B	109.5
O30—Ba2—Ba2^vii	119.36 (16)	H51A—C51'—H51B	109.5
O9—Ba2—Ba2^vii	37.21 (7)	C50'—C51'—H51C	109.5
O10^iv—Ba2—Ba2^vii	147.07 (7)	H51A—C51'—H51C	109.5
O19^v—Ba2—Ba2^vii	64.18 (10)	H51B—C51'—H51C	109.5
O40—Ba2—Ba2^vii	108.93 (18)	C40'—O40'—Ba2	132.0 (14)
O9^vi—Ba2—Ba2^vii	77.53 (7)	O40'—C40'—C41'	106.2 (17)
O10^vi—Ba2—Ba2^vii	35.40 (7)	O40'—C40'—H40C	110.5
C9^vi—Ba2—Ba2^vii	55.40 (9)	C41'—C40'—H40C	110.5
Ba2^vi—Ba2—Ba2^vii	111.282 (12)	O40'—C40'—H40D	110.5
C1—O1—Ba1	146.7 (3)	C41'—C40'—H40D	110.5
C1ⁱⁱ—O2—Ba1	132.2 (3)	H40C—C40'—H40D	108.7
C9—O9—Ba2	145.1 (3)	C40'—C41'—H41D	109.5
C9—O9—Ba2^vii	94.4 (3)	C40'—C41'—H41E	109.5
Ba2—O9—Ba2^vii	108.01 (12)	H41D—C41'—H41E	109.5
C9—O10—Ba2^viii	138.8 (3)	C40'—C41'—H41F	109.5
C9—O10—Ba2^vii	94.0 (3)	H41D—C41'—H41F	109.5
Ba2^viii—O10—Ba2^vii	107.08 (11)	H41E—C41'—H41F	109.5
C11ⁱⁱ—O11—Ba1	136.2 (3)	O50—C50—C51	102.4 (8)
C11ⁱⁱ—O11—Ba1ⁱⁱ	92.1 (3)	O50—C50—H50C	111.3
Ba1—O11—Ba1ⁱⁱ	106.64 (10)	C51—C50—H50C	111.3
C11—O12—Ba1ⁱⁱ	147.5 (3)	O50—C50—H50D	111.3
C11—O12—Ba1	94.4 (3)	C51—C50—H50D	111.3
Ba1ⁱⁱ—O12—Ba1	109.31 (11)	H50C—C50—H50D	109.2
C18—O18—Ba2^ix	141.2 (4)	C50—C51—H51D	109.5
C18—O19—Ba2^v	140.7 (4)	C50—C51—H51E	109.5
C20—O20—Ba1	135.2 (4)	H51D—C51—H51E	109.5
C30—O30—Ba2	143.9 (7)	C50—C51—H51F	109.5
C50'—O50—Ba1	144.7 (6)	H51D—C51—H51F	109.5
C50—O50—Ba1	131.4 (7)	H51E—C51—H51F	109.5

Ba1—O1—C1—O2ⁱ	2.1 (11)	O12—C11—C12—C17	131.3 (5)
Ba1—O1—C1—C2	−178.1 (4)	Ba1—C11—C12—C17	−144.3 (11)
O1—C1—C2—C7	130.7 (6)	O11ⁱ—C11—C12—C13	131.9 (5)
O2ⁱ—C1—C2—C7	−49.5 (7)	O12—C11—C12—C13	−49.0 (7)
O1—C1—C2—C3	−51.4 (7)	Ba1—C11—C12—C13	35.5 (15)
O2ⁱ—C1—C2—C3	128.4 (6)	C17—C12—C13—F13	179.4 (5)
C7—C2—C3—F3	179.9 (5)	C11—C12—C13—F13	−0.4 (8)
C1—C2—C3—F3	1.9 (8)	C17—C12—C13—C14	−0.4 (8)
C7—C2—C3—C4	2.2 (8)	C11—C12—C13—C14	179.8 (5)
C1—C2—C3—C4	−175.9 (5)	F13—C13—C14—F14	−2.7 (8)
F3—C3—C4—F4	−0.4 (8)	C12—C13—C14—F14	177.1 (5)
C2—C3—C4—F4	177.4 (5)	F13—C13—C14—C15	179.5 (5)
F3—C3—C4—C5	179.5 (5)	C12—C13—C14—C15	−0.7 (8)
C2—C3—C4—C5	−2.7 (9)	F14—C14—C15—C16	−177.3 (5)
F4—C4—C5—C6	−179.7 (5)	C13—C14—C15—C16	0.4 (8)
C3—C4—C5—C6	0.4 (8)	F14—C14—C15—C18	3.5 (8)
F4—C4—C5—C9	−1.0 (8)	C13—C14—C15—C18	−178.8 (5)
C3—C4—C5—C9	179.1 (5)	C14—C15—C16—F16	−178.0 (5)
C4—C5—C6—F6	179.7 (5)	C18—C15—C16—F16	1.2 (8)
C9—C5—C6—F6	1.1 (7)	C14—C15—C16—C17	1.0 (8)
C4—C5—C6—C7	2.3 (8)	C18—C15—C16—C17	−179.8 (5)
C9—C5—C6—C7	−176.4 (5)	C13—C12—C17—F17	179.2 (5)
F6—C6—C7—F7	0.7 (8)	C11—C12—C17—F17	−1.0 (8)
C5—C6—C7—F7	178.2 (5)	C13—C12—C17—C16	1.8 (8)
F6—C6—C7—C2	179.7 (5)	C11—C12—C17—C16	−178.4 (5)
C5—C6—C7—C2	−2.8 (9)	F16—C16—C17—F17	−0.6 (8)
C3—C2—C7—F7	179.5 (5)	C15—C16—C17—F17	−179.7 (5)
C1—C2—C7—F7	−2.5 (8)	F16—C16—C17—C12	176.8 (5)
C3—C2—C7—C6	0.5 (8)	C15—C16—C17—C12	−2.2 (9)
C1—C2—C7—C6	178.5 (5)	Ba2^ix—O18—C18—O19	5.6 (12)
Ba2—O9—C9—O10	121.2 (5)	Ba2^ix—O18—C18—C15	−176.2 (4)
Ba2^vii—O9—C9—O10	−9.5 (5)	Ba2^v—O19—C18—O18	−5.4 (11)
Ba2—O9—C9—C5	−59.9 (7)	Ba2^v—O19—C18—C15	176.4 (4)
Ba2^vii—O9—C9—C5	169.4 (4)	C16—C15—C18—O18	36.9 (8)
Ba2—O9—C9—Ba2^vii	130.7 (5)	C14—C15—C18—O18	−143.9 (6)
Ba2^viii—O10—C9—O9	131.3 (4)	C16—C15—C18—O19	−144.6 (6)
Ba2^vii—O10—C9—O9	9.4 (5)	C14—C15—C18—O19	34.5 (8)
Ba2^viii—O10—C9—C5	−47.6 (7)	Ba1—O20—C20—N20	−176.7 (4)
Ba2^vii—O10—C9—C5	−169.4 (4)	C22—N20—C20—O20	−1.0 (9)
Ba2^viii—O10—C9—Ba2^vii	121.9 (4)	C21—N20—C20—O20	−179.0 (6)
C4—C5—C9—O9	−62.6 (7)	Ba2—O30—C30—N30	−175.7 (6)
C6—C5—C9—O9	116.0 (5)	C32—N30—C30—O30	179.9 (11)
C4—C5—C9—O10	116.4 (6)	C31—N30—C30—O30	1.4 (15)
C6—C5—C9—O10	−65.1 (6)	Ba2—O40—C40—C41	−125.3 (10)
Ba1ⁱⁱ—O12—C11—O11ⁱ	119.3 (6)	C50—O50—C50'—C51'	−0.8 (14)
Ba1—O12—C11—O11ⁱ	−18.1 (5)	Ba1—O50—C50'—C51'	−93.6 (11)
Ba1ⁱⁱ—O12—C11—C12	−59.7 (8)	Ba2—O40'—C40'—C41'	149.4 (16)
Ba1—O12—C11—C12	162.8 (4)	C50'—O50—C50—C51	11.1 (17)
Ba1ⁱⁱ—O12—C11—Ba1	137.5 (6)	Ba1—O50—C50—C51	140.7 (14)
O11ⁱ—C11—C12—C17	−47.8 (7)

Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) −x+1, y−1/2, −z+3/2; (iii) x, −y+3/2, z−1/2; (iv) x, y+1, z; (v) −x, −y+1, −z+1; (vi) −x, y+1/2, −z+1/2; (vii) −x, y−1/2, −z+1/2; (viii) x, y−1, z; (ix) x, −y+3/2, z+1/2.

Acknowledgements

We thank Dr Ingo Pantenburg and Silke Kremer for collecting single-crystal X-ray diffraction data as well as for many helpful discussions.

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