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Acta Cryst. (2007). E63, m2218    [ doi:10.1107/S1600536807035738 ]

(18-Crown-6)bis(tetrahydrofuran-[kappa]O)potassium(I) [1,2-bis(fluoren-9-ylcarbonyl)benzene(2-)]bis([eta]5-cyclopentadienyl)dysprosate(III)

A. Zaeni, F. Olbrich, S. Blaurock and F. T. Edelmann

Abstract top

The title compound, [K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)], was isolated serendipitously from a reaction of anhydrous DyCl3 and KCp (Cp = cyclopentadienyl) in tetrahydrofuran (THF), followed by addition of KFl(18-crown-6) (Fl = fluorenide). In the cation, K+ is coordinated by 18-crown-6 and two THF ligands, while the anion is an `ate' complex of DyIII, containing two [eta]5-Cp ligands and the novel chelating ligand o-phenylenebis(fluorenylideneacylate).

Comment top

As part of a research project on the synthesis and structural characterization of new lanthanide fluorenyl complexes we investigated the possibility of preparing an anionic "ate" complex of dysprosium containing two cyclopentadienyl and two fluorenyl ligands. The title compound was isolated serendipitously and in small amounts from a reaction of anhydrous DyCl3 and KCp in THF, followed by addition of KFl(18-crown-6) (Fl = fluorenide). The structure comprises discrete [K(18-crown-6)(THF)2]+ cations and unprecedented [DyCp2(C6H4(OC=C13H8)2)]- anions (Figure 1).

In the cation, K+ is coordinated by 18-crown-6 and two THF ligands. This cation is not unusual and has been observed in the potassium fluorenide derivative [K(18-crown-6)(THF)2]+Fl- (Edelmann et al., 2007). The surprising result of this reaction is the formation of the unprecedented C6H4(OC=C13H8)22- ligand in the [DyCp2(C6H4(OC=C13H8)2)]- anion. In this ligand, a central phenyl ring is substituted in ortho positions by two fluorenylideneacylate groups. While the origin of the fluorenyl group is certain, the formation of the entire ligand system remains speculative. The new ligand is coordinated as a dianion via its two acyl O atoms.The bonds C37—C69 (1.373 (2) Å) and C38—C49 (1.380 (3) Å) are clearly double bonds. Thus, the new ligand can be regarded as a chelating phenylene-1,2-bis(fluorenylideneacylate)dianion. It is well established that 9-acylfluorenes exhibit keto-enol tautomerism (Meyer & Gottlieb-Billroth (1921); Goldschmidt & Nagel (1930); Greenhow et al. (1953); Harcourt & O'Ferrall (1995)). In the title compound, the dianion of the bis-enol form is coordinated to Dy. We were unable to prepare the new ligand independently by treatment of phthalic dichloride with two equivalents of sodium fluorenide.

Related literature top

For related literature, see: Edelmann et al. (2007); Goldschmidt & Nagel (1930); Greenhow et al. (1953); Harcourt & O'Ferrall (1995); Meyer & Gottlieb-Billroth (1921).

Experimental top

0.27 g (1.0 mmol) of anhydrous DyCl3 and 0.312 g (3.0 mmol) of KCp were dissolved in 20 ml of THF under nitrogen and stirred at reflux temperature for 1 h. The yellow reaction mixture was filtered and 0.15 g (1 mmol) of KFl(18-crown-6) were added with stirring. After filtering again, the solution was carefully layered with n-hexane (10 ml). After several days a small amount of well formed dark green crystals were obtained at room temperature. M.p. 663 K.

Refinement top

H atoms were placed geometrically and refined using a riding model with C—H = 0.95–0.99 Å and with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound showing displacement ellipsoids at the 50% probability level. H atoms are omitted.
(I) top
Crystal data top
[K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)]Z = 2
Mr = 1200.80F(000) = 1238
Triclinic, P1Dx = 1.420 Mg m−3
Hall symbol: -P 1Melting point: 663 K
a = 12.0798 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.0513 (2) ÅCell parameters from 100 reflections
c = 19.3154 (3) Åθ = 1.6–29.2°
α = 85.1700 (8)°µ = 1.46 mm−1
β = 73.1480 (7)°T = 173 K
γ = 74.5617 (8)°Plate, dark green
V = 2809.20 (8) Å30.60 × 0.40 × 0.30 mm
Data collection top
Siemens SMART CCD
diffractometer		13639 independent reflections
Radiation source: fine-focus sealed tube12598 reflections with I > 2σ(I)
graphiteRint = 0.020
ω scansθmax = 29.2°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)		h = −13→16
Tmin = 0.455, Tmax = 0.641k = −17→17
19240 measured reflectionsl = −26→23
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.035P)2 + 0.3278P]
where P = (Fo2 + 2Fc2)/3
13639 reflections(Δ/σ)max = 0.001
691 parametersΔρmax = 1.31 e Å−3
0 restraintsΔρmin = −1.40 e Å−3
Crystal data top
[K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)]γ = 74.5617 (8)°
Mr = 1200.80V = 2809.20 (8) Å3
Triclinic, P1Z = 2
a = 12.0798 (2) ÅMo Kα radiation
b = 13.0513 (2) ŵ = 1.46 mm−1
c = 19.3154 (3) ÅT = 173 K
α = 85.1700 (8)°0.60 × 0.40 × 0.30 mm
β = 73.1480 (7)°
Data collection top
Siemens SMART CCD
diffractometer		13639 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)		12598 reflections with I > 2σ(I)
Tmin = 0.455, Tmax = 0.641Rint = 0.020
19240 measured reflectionsθmax = 29.2°
Refinement top
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.067Δρmax = 1.31 e Å−3
S = 1.02Δρmin = −1.40 e Å−3
13639 reflectionsAbsolute structure: ?
691 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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
xyzUiso*/Ueq
K0.48016 (4)0.52461 (3)0.25229 (2)0.02541 (8)
O10.59368 (13)0.67575 (13)0.17793 (8)0.0329 (3)
O20.46758 (14)0.58350 (13)0.10802 (9)0.0376 (4)
O30.32065 (15)0.46039 (13)0.19874 (10)0.0392 (4)
O40.36303 (13)0.37716 (12)0.32869 (9)0.0337 (3)
O50.49545 (14)0.46832 (12)0.39557 (8)0.0321 (3)
O60.65250 (14)0.58081 (12)0.30114 (8)0.0325 (3)
O70.64954 (16)0.33991 (13)0.20525 (11)0.0477 (4)
O80.30420 (16)0.71086 (13)0.29797 (10)0.0444 (4)
C10.5992 (2)0.6930 (2)0.10353 (12)0.0400 (5)
H1A0.66490.63770.07390.0452 (16)*
H1B0.61470.76330.08780.0452 (16)*
C20.4818 (2)0.6886 (2)0.09360 (14)0.0428 (6)
H2A0.41550.73890.12700.0452 (16)*
H2B0.47970.70940.04340.0452 (16)*
C30.3584 (2)0.5744 (2)0.09790 (16)0.0480 (6)
H3A0.36120.58440.04610.0452 (16)*
H3B0.29090.63020.12570.0452 (16)*
C40.3399 (3)0.4670 (2)0.12292 (15)0.0458 (6)
H4A0.26990.45660.11030.0452 (16)*
H4B0.41120.41100.09900.0452 (16)*
C50.2871 (2)0.36662 (18)0.23024 (15)0.0405 (5)
H5A0.35370.30320.21290.0452 (16)*
H5B0.21680.35960.21630.0452 (16)*
C60.2575 (2)0.37470 (18)0.31050 (15)0.0396 (5)
H6A0.19390.44020.32750.0452 (16)*
H6B0.22830.31290.33410.0452 (16)*
C70.3468 (2)0.37626 (19)0.40446 (13)0.0395 (5)
H7A0.31700.31420.42700.0452 (16)*
H7B0.28760.44170.42630.0452 (16)*
C80.4653 (2)0.37009 (18)0.41659 (13)0.0393 (5)
H8A0.46100.35550.46830.0452 (16)*
H8B0.52730.31160.38770.0452 (16)*
C90.6100 (2)0.46734 (19)0.40246 (13)0.0368 (5)
H9A0.67180.40910.37320.0452 (16)*
H9B0.61060.45520.45360.0452 (16)*
C100.6367 (2)0.57188 (18)0.37680 (12)0.0343 (4)
H10A0.56990.63070.40180.0452 (16)*
H10B0.71030.57650.38790.0452 (16)*
C110.6827 (2)0.67701 (17)0.27198 (13)0.0341 (4)
H11A0.75590.68200.28330.0452 (16)*
H11B0.61690.73890.29360.0452 (16)*
C120.70304 (18)0.67746 (18)0.19195 (13)0.0333 (4)
H12A0.72810.74200.17030.0452 (16)*
H12B0.76700.61440.17040.0452 (16)*
C130.7340 (2)0.3667 (2)0.14170 (18)0.0533 (7)
H13A0.80740.37000.15360.083 (3)*
H13B0.69930.43720.12290.083 (3)*
C140.7642 (3)0.2830 (3)0.08531 (18)0.0694 (9)
H14A0.84480.23530.08050.083 (3)*
H14B0.76020.31550.03760.083 (3)*
C150.6671 (3)0.2232 (3)0.11543 (18)0.0608 (8)
H15A0.59580.25530.09810.083 (3)*
H15B0.69710.14730.10170.083 (3)*
C160.6390 (2)0.23608 (19)0.19600 (15)0.0442 (6)
H16A0.55710.22950.22070.083 (3)*
H16B0.69640.18160.21590.083 (3)*
C170.2078 (3)0.7031 (3)0.35854 (19)0.0627 (9)
H17A0.20080.62880.36570.083 (3)*
H17B0.13180.74900.35190.083 (3)*
C180.2349 (4)0.7394 (3)0.42263 (18)0.0727 (10)
H18A0.27470.67810.44810.083 (3)*
H18B0.16080.77920.45720.083 (3)*
C190.3177 (3)0.8110 (2)0.38960 (15)0.0459 (6)
H19A0.39540.78420.40080.083 (3)*
H19B0.28130.88460.40770.083 (3)*
C200.3334 (2)0.80660 (17)0.30879 (14)0.0383 (5)
H20A0.27930.86930.29300.083 (3)*
H20B0.41690.80490.28110.083 (3)*
Dy0.136270 (7)0.070125 (6)0.128562 (4)0.02123 (3)
O310.00368 (12)0.22074 (10)0.16913 (7)0.0233 (3)
O360.20241 (12)0.08247 (11)0.22062 (7)0.0266 (3)
C210.1169 (3)−0.12320 (19)0.18210 (15)0.0455 (6)
H210.1679−0.15680.21120.061 (3)*
C220.1438 (2)−0.13181 (17)0.10779 (14)0.0396 (5)
H220.2167−0.17190.07720.061 (3)*
C230.0467 (2)−0.07224 (18)0.08566 (14)0.0392 (5)
H230.0414−0.06480.03730.061 (3)*
C24−0.0422 (2)−0.02476 (19)0.14642 (18)0.0473 (6)
H24−0.11830.02060.14690.061 (3)*
C250.0021 (3)−0.0567 (2)0.20691 (15)0.0505 (7)
H25−0.0387−0.03670.25570.061 (3)*
C260.3442 (2)0.1093 (3)0.05106 (13)0.0459 (6)
H260.40460.09920.07510.061 (3)*
C270.3277 (2)0.0325 (2)0.01099 (14)0.0502 (6)
H270.3743−0.03880.00340.061 (3)*
C280.2296 (2)0.0806 (2)−0.01572 (12)0.0449 (6)
H280.19810.0473−0.04490.061 (3)*
C290.1866 (2)0.1847 (2)0.00774 (12)0.0407 (5)
H290.12060.2352−0.00280.061 (3)*
C300.2561 (2)0.2034 (2)0.04943 (12)0.0397 (5)
H300.24560.26810.07250.061 (3)*
C31−0.04811 (16)0.18802 (13)0.29644 (10)0.0201 (3)
C32−0.16929 (17)0.19355 (15)0.32745 (11)0.0257 (4)
H32−0.22690.23980.30690.038 (3)*
C33−0.20713 (19)0.13260 (17)0.38785 (12)0.0315 (4)
H33−0.29000.13800.40880.038 (3)*
C34−0.1237 (2)0.06409 (17)0.41735 (12)0.0321 (4)
H34−0.14900.02290.45900.038 (3)*
C35−0.00246 (19)0.05567 (15)0.38580 (11)0.0270 (4)
H350.05450.00680.40560.038 (3)*
C360.03767 (17)0.11766 (14)0.32550 (10)0.0210 (3)
C37−0.01876 (15)0.26107 (14)0.23298 (9)0.0196 (3)
C380.16958 (17)0.09984 (14)0.29021 (10)0.0211 (3)
C410.13554 (19)0.16799 (15)0.45819 (11)0.0271 (4)
H410.05880.18890.44990.037 (2)*
C420.1486 (2)0.18555 (16)0.52531 (11)0.0316 (4)
H420.08000.21760.56270.037 (2)*
C430.2601 (2)0.15705 (16)0.53864 (12)0.0353 (5)
H430.26700.16900.58490.037 (2)*
C440.3608 (2)0.11125 (16)0.48450 (12)0.0325 (4)
H440.43730.09250.49310.037 (2)*
C450.56362 (19)0.01110 (17)0.33670 (13)0.0329 (4)
H450.60140.00930.37380.037 (2)*
C460.6306 (2)−0.02579 (18)0.26798 (13)0.0365 (5)
H460.7147−0.05330.25790.037 (2)*
C470.57487 (19)−0.02271 (17)0.21366 (12)0.0337 (4)
H470.6218−0.04820.16690.037 (2)*
C480.45198 (18)0.01696 (16)0.22662 (11)0.0277 (4)
H480.41520.01910.18900.037 (2)*
C490.25310 (17)0.09335 (14)0.32737 (10)0.0219 (3)
C500.23571 (18)0.11955 (14)0.40321 (10)0.0233 (4)
C510.34947 (19)0.09260 (14)0.41686 (11)0.0258 (4)
C520.44031 (18)0.05074 (15)0.35057 (11)0.0259 (4)
C530.38291 (17)0.05385 (14)0.29597 (10)0.0233 (4)
C61−0.07294 (17)0.38101 (14)0.38571 (10)0.0225 (3)
H61−0.08290.31120.39700.032 (2)*
C62−0.08552 (18)0.44884 (16)0.44059 (11)0.0265 (4)
H62−0.10290.42420.48930.032 (2)*
C63−0.07322 (19)0.55228 (16)0.42597 (11)0.0275 (4)
H63−0.08240.59740.46450.032 (2)*
C64−0.04756 (18)0.58916 (15)0.35525 (11)0.0254 (4)
H64−0.03970.65980.34490.032 (2)*
C650.01487 (18)0.63022 (15)0.18095 (11)0.0271 (4)
H650.01150.69280.20410.032 (2)*
C660.0401 (2)0.62683 (17)0.10631 (12)0.0307 (4)
H660.05390.68770.07800.032 (2)*
C670.0454 (2)0.53472 (17)0.07253 (11)0.0309 (4)
H670.06320.53360.02130.032 (2)*
C680.02505 (18)0.44395 (15)0.11257 (10)0.0255 (4)
H680.02840.38180.08890.032 (2)*
C69−0.02338 (16)0.36481 (14)0.24407 (10)0.0202 (3)
C70−0.04538 (16)0.41586 (14)0.31351 (10)0.0198 (3)
C71−0.03333 (16)0.52160 (14)0.29937 (10)0.0213 (3)
C72−0.00544 (16)0.54005 (14)0.22144 (10)0.0216 (3)
C73−0.00025 (16)0.44578 (14)0.18781 (10)0.0203 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K0.02496 (19)0.02416 (18)0.02657 (19)−0.00700 (15)−0.00607 (15)0.00129 (15)
O10.0241 (7)0.0446 (9)0.0315 (8)−0.0146 (6)−0.0076 (6)0.0109 (6)
O20.0318 (8)0.0444 (9)0.0414 (9)−0.0120 (7)−0.0183 (7)0.0114 (7)
O30.0391 (9)0.0347 (8)0.0537 (10)−0.0167 (7)−0.0237 (8)0.0076 (7)
O40.0248 (7)0.0359 (8)0.0381 (8)−0.0092 (6)−0.0057 (6)0.0068 (6)
O50.0334 (8)0.0288 (7)0.0322 (8)−0.0058 (6)−0.0097 (6)0.0057 (6)
O60.0355 (8)0.0318 (7)0.0331 (8)−0.0102 (6)−0.0128 (6)0.0015 (6)
O70.0413 (10)0.0317 (8)0.0615 (12)−0.0077 (7)0.0001 (9)−0.0098 (8)
O80.0408 (9)0.0282 (8)0.0580 (11)−0.0088 (7)−0.0015 (8)−0.0093 (7)
C10.0375 (12)0.0509 (14)0.0314 (11)−0.0190 (11)−0.0066 (9)0.0153 (10)
C20.0456 (14)0.0489 (14)0.0377 (12)−0.0160 (11)−0.0189 (11)0.0172 (11)
C30.0440 (14)0.0561 (15)0.0557 (16)−0.0163 (12)−0.0331 (13)0.0155 (13)
C40.0445 (14)0.0477 (14)0.0567 (16)−0.0143 (12)−0.0303 (12)0.0038 (12)
C50.0322 (11)0.0290 (10)0.0687 (17)−0.0121 (9)−0.0246 (11)0.0055 (11)
C60.0247 (10)0.0305 (11)0.0638 (16)−0.0115 (9)−0.0106 (10)0.0072 (10)
C70.0413 (12)0.0315 (11)0.0367 (12)−0.0121 (9)0.0041 (10)0.0046 (9)
C80.0566 (15)0.0299 (11)0.0305 (11)−0.0107 (10)−0.0132 (10)0.0081 (9)
C90.0360 (11)0.0384 (11)0.0348 (11)−0.0018 (9)−0.0156 (9)0.0023 (9)
C100.0318 (11)0.0396 (11)0.0331 (11)−0.0045 (9)−0.0149 (9)−0.0024 (9)
C110.0279 (10)0.0320 (10)0.0450 (12)−0.0092 (8)−0.0133 (9)0.0010 (9)
C120.0213 (9)0.0352 (11)0.0434 (12)−0.0110 (8)−0.0069 (8)0.0041 (9)
C130.0325 (12)0.0431 (14)0.075 (2)−0.0077 (11)−0.0033 (13)0.0038 (13)
C140.069 (2)0.082 (2)0.0484 (17)−0.0144 (19)−0.0091 (16)0.0017 (16)
C150.066 (2)0.0591 (18)0.064 (2)−0.0085 (16)−0.0333 (17)−0.0094 (15)
C160.0425 (13)0.0336 (12)0.0571 (16)−0.0090 (10)−0.0146 (12)−0.0032 (11)
C170.0485 (16)0.0518 (16)0.082 (2)−0.0283 (14)0.0079 (15)−0.0103 (15)
C180.096 (3)0.072 (2)0.0519 (18)−0.049 (2)−0.0002 (18)0.0077 (16)
C190.0481 (14)0.0371 (12)0.0525 (15)−0.0109 (11)−0.0144 (12)0.0016 (11)
C200.0338 (11)0.0263 (10)0.0512 (14)−0.0077 (9)−0.0061 (10)−0.0011 (9)
Dy0.02097 (5)0.02315 (5)0.01945 (5)−0.00487 (3)−0.00488 (3)−0.00452 (3)
O310.0272 (7)0.0204 (6)0.0210 (6)−0.0025 (5)−0.0074 (5)−0.0026 (5)
O360.0258 (7)0.0332 (7)0.0206 (6)−0.0055 (6)−0.0072 (5)−0.0038 (5)
C210.0659 (17)0.0322 (11)0.0546 (15)−0.0230 (12)−0.0359 (14)0.0131 (11)
C220.0425 (13)0.0227 (10)0.0536 (14)−0.0033 (9)−0.0155 (11)−0.0085 (9)
C230.0509 (14)0.0334 (11)0.0451 (13)−0.0156 (10)−0.0268 (11)−0.0014 (10)
C240.0300 (11)0.0313 (11)0.085 (2)−0.0097 (9)−0.0183 (12)−0.0086 (12)
C250.0702 (19)0.0479 (14)0.0388 (13)−0.0419 (14)0.0038 (12)−0.0096 (11)
C260.0253 (10)0.0837 (19)0.0298 (11)−0.0217 (12)−0.0061 (9)0.0130 (12)
C270.0368 (13)0.0538 (15)0.0413 (13)−0.0002 (11)0.0092 (11)−0.0059 (11)
C280.0406 (13)0.0729 (18)0.0215 (10)−0.0209 (12)0.0002 (9)−0.0119 (10)
C290.0305 (11)0.0603 (15)0.0253 (10)−0.0116 (11)−0.0015 (8)0.0103 (10)
C300.0410 (13)0.0514 (14)0.0272 (10)−0.0244 (11)0.0006 (9)0.0032 (9)
C310.0235 (8)0.0165 (7)0.0207 (8)−0.0049 (6)−0.0064 (7)−0.0019 (6)
C320.0228 (9)0.0262 (9)0.0284 (9)−0.0067 (7)−0.0067 (7)−0.0024 (7)
C330.0277 (10)0.0324 (10)0.0345 (11)−0.0135 (8)−0.0026 (8)−0.0029 (8)
C340.0390 (11)0.0276 (10)0.0303 (10)−0.0157 (9)−0.0054 (9)0.0048 (8)
C350.0342 (10)0.0205 (8)0.0270 (9)−0.0076 (8)−0.0097 (8)0.0030 (7)
C360.0261 (9)0.0178 (8)0.0203 (8)−0.0058 (7)−0.0076 (7)−0.0012 (6)
C370.0168 (7)0.0208 (8)0.0212 (8)−0.0037 (6)−0.0062 (6)0.0002 (6)
C380.0250 (9)0.0171 (7)0.0215 (8)−0.0039 (6)−0.0080 (7)0.0001 (6)
C410.0359 (11)0.0188 (8)0.0264 (9)−0.0021 (7)−0.0127 (8)−0.0008 (7)
C420.0470 (12)0.0217 (9)0.0251 (9)−0.0051 (8)−0.0111 (9)−0.0025 (7)
C430.0578 (15)0.0251 (9)0.0283 (10)−0.0077 (9)−0.0226 (10)−0.0003 (8)
C440.0421 (12)0.0280 (10)0.0348 (11)−0.0077 (9)−0.0235 (9)0.0018 (8)
C450.0290 (10)0.0306 (10)0.0438 (12)−0.0081 (8)−0.0185 (9)0.0064 (9)
C460.0240 (10)0.0347 (11)0.0486 (13)−0.0058 (8)−0.0100 (9)0.0062 (10)
C470.0274 (10)0.0317 (10)0.0365 (11)−0.0057 (8)−0.0031 (8)0.0021 (9)
C480.0277 (10)0.0265 (9)0.0277 (9)−0.0056 (8)−0.0075 (8)0.0008 (7)
C490.0254 (9)0.0177 (8)0.0223 (8)−0.0027 (7)−0.0087 (7)0.0001 (6)
C500.0304 (9)0.0160 (8)0.0251 (9)−0.0041 (7)−0.0124 (7)0.0015 (7)
C510.0333 (10)0.0176 (8)0.0295 (9)−0.0046 (7)−0.0154 (8)0.0015 (7)
C520.0294 (10)0.0195 (8)0.0321 (10)−0.0060 (7)−0.0147 (8)0.0033 (7)
C530.0244 (9)0.0186 (8)0.0275 (9)−0.0043 (7)−0.0098 (7)0.0013 (7)
C610.0237 (9)0.0208 (8)0.0241 (9)−0.0044 (7)−0.0095 (7)0.0005 (7)
C620.0294 (10)0.0274 (9)0.0236 (9)−0.0038 (8)−0.0111 (7)−0.0024 (7)
C630.0319 (10)0.0270 (9)0.0265 (9)−0.0060 (8)−0.0118 (8)−0.0072 (7)
C640.0268 (9)0.0209 (8)0.0309 (10)−0.0063 (7)−0.0105 (8)−0.0033 (7)
C650.0271 (9)0.0232 (9)0.0342 (10)−0.0098 (7)−0.0112 (8)0.0026 (8)
C660.0330 (10)0.0289 (10)0.0349 (11)−0.0144 (8)−0.0140 (9)0.0113 (8)
C670.0354 (11)0.0366 (11)0.0259 (10)−0.0147 (9)−0.0138 (8)0.0084 (8)
C680.0285 (9)0.0261 (9)0.0252 (9)−0.0090 (7)−0.0108 (7)0.0013 (7)
C690.0200 (8)0.0203 (8)0.0210 (8)−0.0045 (6)−0.0073 (6)−0.0001 (6)
C700.0176 (8)0.0190 (8)0.0232 (8)−0.0027 (6)−0.0075 (6)−0.0020 (6)
C710.0197 (8)0.0200 (8)0.0254 (9)−0.0043 (6)−0.0084 (7)−0.0011 (7)
C720.0194 (8)0.0215 (8)0.0255 (9)−0.0060 (7)−0.0085 (7)0.0012 (7)
C730.0197 (8)0.0192 (8)0.0235 (8)−0.0050 (6)−0.0083 (7)0.0008 (6)
Geometric parameters (Å, °) top
K—O72.7364 (18)Dy—C252.691 (2)
K—O32.7652 (16)Dy—C282.693 (2)
K—O42.7649 (15)Dy—C272.699 (2)
K—O12.7669 (15)O31—C371.308 (2)
K—O82.7800 (18)O36—C381.308 (2)
K—O62.7983 (15)C21—C221.384 (4)
K—O52.8488 (15)C21—C251.397 (4)
K—O22.8638 (16)C21—H210.950
K—C133.434 (3)C22—C231.383 (3)
O1—C11.421 (3)C22—H220.950
O1—C121.429 (2)C23—C241.397 (4)
O2—C21.422 (3)C23—H230.950
O2—C31.424 (3)C24—C251.410 (4)
O3—C41.414 (3)C24—H240.950
O3—C51.424 (3)C25—H250.950
O4—C71.419 (3)C26—C301.399 (4)
O4—C61.426 (3)C26—C271.403 (4)
O5—C81.420 (3)C26—H260.950
O5—C91.424 (3)C27—C281.403 (4)
O6—C101.417 (3)C27—H270.950
O6—C111.425 (3)C28—C291.384 (4)
O7—C161.425 (3)C28—H280.950
O7—C131.436 (3)C29—C301.395 (3)
O8—C171.410 (3)C29—H290.950
O8—C201.432 (3)C30—H300.950
C1—C21.501 (3)C31—C321.396 (3)
C1—H1A0.990C31—C361.406 (2)
C1—H1B0.990C31—C371.506 (2)
C2—H2A0.990C32—C331.390 (3)
C2—H2B0.990C32—H320.950
C3—C41.496 (4)C33—C341.381 (3)
C3—H3A0.990C33—H330.950
C3—H3B0.990C34—C351.392 (3)
C4—H4A0.990C34—H340.950
C4—H4B0.990C35—C361.403 (2)
C5—C61.493 (4)C35—H350.950
C5—H5A0.990C36—C381.502 (3)
C5—H5B0.990C37—C691.373 (2)
C6—H6A0.990C38—C491.380 (2)
C6—H6B0.990C41—C421.395 (3)
C7—C81.497 (4)C41—C501.397 (3)
C7—H7A0.990C41—H410.950
C7—H7B0.990C42—C431.392 (3)
C8—H8A0.990C42—H420.950
C8—H8B0.990C43—C441.382 (3)
C9—C101.497 (3)C43—H430.950
C9—H9A0.990C44—C511.400 (3)
C9—H9B0.990C44—H440.950
C10—H10A0.990C45—C461.388 (3)
C10—H10B0.990C45—C521.393 (3)
C11—C121.493 (3)C45—H450.950
C11—H11A0.990C46—C471.394 (3)
C11—H11B0.990C46—H460.950
C12—H12A0.990C47—C481.390 (3)
C12—H12B0.990C47—H470.950
C13—C141.507 (5)C48—C531.403 (3)
C13—H13A0.990C48—H480.950
C13—H13B0.990C49—C531.471 (3)
C14—C151.529 (5)C49—C501.475 (3)
C14—H14A0.990C50—C511.421 (3)
C14—H14B0.990C51—C521.458 (3)
C15—C161.508 (4)C52—C531.413 (3)
C15—H15A0.990C61—C621.387 (3)
C15—H15B0.990C61—C701.402 (2)
C16—H16A0.990C61—H610.950
C16—H16B0.990C62—C631.394 (3)
C17—C181.510 (5)C62—H620.950
C17—H17A0.990C63—C641.385 (3)
C17—H17B0.990C63—H630.950
C18—C191.520 (4)C64—C711.394 (3)
C18—H18A0.990C64—H640.950
C18—H18B0.990C65—C661.387 (3)
C19—C201.521 (4)C65—C721.394 (3)
C19—H19A0.990C65—H650.950
C19—H19B0.990C66—C671.394 (3)
C20—H20A0.990C66—H660.950
C20—H20B0.990C67—C681.397 (3)
Dy—O362.1832 (13)C67—H670.950
Dy—O312.2134 (13)C68—C731.397 (3)
Dy—C302.658 (2)C68—H680.950
Dy—C292.670 (2)C69—C731.471 (2)
Dy—C222.673 (2)C69—C701.471 (2)
Dy—C232.675 (2)C70—C711.422 (2)
Dy—C262.680 (2)C71—C721.458 (3)
Dy—C242.687 (2)C72—C731.418 (2)
Dy—C212.688 (2)
O7—K—O390.26 (6)C30—Dy—C24146.66 (9)
O7—K—O479.66 (5)C29—Dy—C24116.67 (9)
O3—K—O460.37 (5)C22—Dy—C2449.80 (8)
O7—K—O1101.60 (5)C23—Dy—C2430.21 (8)
O3—K—O1119.84 (5)C26—Dy—C24151.47 (9)
O4—K—O1178.69 (5)O36—Dy—C2185.56 (6)
O7—K—O8178.42 (6)O31—Dy—C21124.28 (8)
O3—K—O888.18 (5)C30—Dy—C21153.13 (9)
O4—K—O899.79 (5)C29—Dy—C21144.81 (9)
O1—K—O878.96 (5)C22—Dy—C2129.92 (8)
O7—K—O686.54 (5)C23—Dy—C2149.48 (7)
O3—K—O6176.62 (5)C26—Dy—C21123.02 (9)
O4—K—O6119.97 (5)C24—Dy—C2149.83 (8)
O1—K—O659.89 (4)O36—Dy—C2590.05 (7)
O8—K—O695.01 (5)O31—Dy—C2595.24 (8)
O7—K—O588.51 (5)C30—Dy—C25176.30 (9)
O3—K—O5120.51 (5)C29—Dy—C25147.02 (8)
O4—K—O560.96 (5)C22—Dy—C2549.69 (8)
O1—K—O5118.58 (5)C23—Dy—C2549.81 (8)
O8—K—O592.51 (5)C26—Dy—C25153.07 (10)
O6—K—O560.55 (4)C24—Dy—C2530.39 (9)
O7—K—O291.62 (6)C21—Dy—C2530.10 (9)
O3—K—O260.48 (5)O36—Dy—C28133.37 (7)
O4—K—O2120.04 (5)O31—Dy—C28110.54 (7)
O1—K—O260.43 (5)C30—Dy—C2849.93 (8)
O8—K—O287.38 (5)C29—Dy—C2829.91 (8)
O6—K—O2118.47 (5)C22—Dy—C2886.15 (8)
O5—K—O2179.00 (5)C23—Dy—C2879.85 (8)
O7—K—C1323.63 (6)C26—Dy—C2849.77 (7)
O3—K—C1396.02 (7)C24—Dy—C28104.90 (9)
O4—K—C13102.42 (6)C21—Dy—C28115.57 (9)
O1—K—C1378.87 (6)C25—Dy—C28129.56 (8)
O8—K—C13156.45 (6)O36—Dy—C27106.91 (8)
O6—K—C1380.61 (6)O31—Dy—C27130.21 (7)
O5—K—C13105.02 (6)C30—Dy—C2750.12 (9)
O2—K—C1374.82 (6)C29—Dy—C2749.72 (8)
C1—O1—C12111.96 (16)C22—Dy—C2782.24 (9)
C1—O1—K118.11 (13)C23—Dy—C2791.29 (9)
C12—O1—K116.56 (11)C26—Dy—C2730.24 (9)
C2—O2—C3111.57 (18)C24—Dy—C27121.31 (9)
C2—O2—K108.88 (13)C21—Dy—C27105.07 (9)
C3—O2—K111.25 (14)C25—Dy—C27131.83 (9)
C4—O3—C5113.67 (19)C28—Dy—C2730.16 (8)
C4—O3—K116.46 (14)C37—O31—Dy125.31 (11)
C5—O3—K116.24 (13)C38—O36—Dy143.67 (12)
C7—O4—C6112.76 (18)C22—C21—C25108.3 (2)
C7—O4—K114.76 (13)C22—C21—Dy74.44 (13)
C6—O4—K114.96 (12)C25—C21—Dy75.08 (13)
C8—O5—C9112.41 (17)C22—C21—H21125.9
C8—O5—K110.42 (12)C25—C21—H21125.9
C9—O5—K111.21 (12)Dy—C21—H21116.7
C10—O6—C11112.36 (17)C23—C22—C21108.4 (2)
C10—O6—K115.49 (12)C23—C22—Dy75.12 (13)
C11—O6—K115.85 (12)C21—C22—Dy75.64 (13)
C16—O7—C13108.1 (2)C23—C22—H22125.8
C16—O7—K131.44 (15)C21—C22—H22125.8
C13—O7—K106.58 (14)Dy—C22—H22115.6
C17—O8—C20104.91 (19)C22—C23—C24108.5 (2)
C17—O8—K116.98 (16)C22—C23—Dy74.91 (13)
C20—O8—K121.67 (14)C24—C23—Dy75.35 (13)
O1—C1—C2108.38 (18)C22—C23—H23125.7
O1—C1—H1A110.0C24—C23—H23125.7
C2—C1—H1A110.0Dy—C23—H23116.1
O1—C1—H1B110.0C23—C24—C25107.2 (2)
C2—C1—H1B110.0C23—C24—Dy74.44 (13)
H1A—C1—H1B108.4C25—C24—Dy74.97 (13)
O2—C2—C1109.29 (19)C23—C24—H24126.4
O2—C2—H2A109.8C25—C24—H24126.4
C1—C2—H2A109.8Dy—C24—H24116.4
O2—C2—H2B109.8C21—C25—C24107.5 (2)
C1—C2—H2B109.8C21—C25—Dy74.82 (14)
H2A—C2—H2B108.3C24—C25—Dy74.64 (14)
O2—C3—C4109.51 (19)C21—C25—H25126.2
O2—C3—H3A109.8C24—C25—H25126.2
C4—C3—H3A109.8Dy—C25—H25116.5
O2—C3—H3B109.8C30—C26—C27108.2 (2)
C4—C3—H3B109.8C30—C26—Dy73.93 (13)
H3A—C3—H3B108.2C27—C26—Dy75.61 (14)
O3—C4—C3108.5 (2)C30—C26—H26125.9
O3—C4—H4A110.0C27—C26—H26125.9
C3—C4—H4A110.0Dy—C26—H26116.6
O3—C4—H4B110.0C28—C27—C26107.4 (2)
C3—C4—H4B110.0C28—C27—Dy74.70 (14)
H4A—C4—H4B108.4C26—C27—Dy74.15 (14)
O3—C5—C6108.22 (19)C28—C27—H27126.3
O3—C5—H5A110.1C26—C27—H27126.3
C6—C5—H5A110.1Dy—C27—H27117.0
O3—C5—H5B110.1C29—C28—C27108.2 (2)
C6—C5—H5B110.1C29—C28—Dy74.11 (13)
H5A—C5—H5B108.4C27—C28—Dy75.14 (14)
O4—C6—C5108.32 (19)C29—C28—H28125.9
O4—C6—H6A110.0C27—C28—H28125.9
C5—C6—H6A110.0Dy—C28—H28116.9
O4—C6—H6B110.0C28—C29—C30108.7 (2)
C5—C6—H6B110.0C28—C29—Dy75.98 (14)
H6A—C6—H6B108.4C30—C29—Dy74.35 (12)
O4—C7—C8107.72 (18)C28—C29—H29125.6
O4—C7—H7A110.2C30—C29—H29125.6
C8—C7—H7A110.2Dy—C29—H29116.1
O4—C7—H7B110.2C29—C30—C26107.5 (2)
C8—C7—H7B110.2C29—C30—Dy75.29 (13)
H7A—C7—H7B108.5C26—C30—Dy75.69 (13)
O5—C8—C7108.91 (18)C29—C30—H30126.2
O5—C8—H8A109.9C26—C30—H30126.2
C7—C8—H8A109.9Dy—C30—H30115.1
O5—C8—H8B109.9C32—C31—C36119.63 (17)
C7—C8—H8B109.9C32—C31—C37116.15 (16)
H8A—C8—H8B108.3C36—C31—C37124.22 (16)
O5—C9—C10109.02 (17)C33—C32—C31121.17 (18)
O5—C9—H9A109.9C33—C32—H32119.4
C10—C9—H9A109.9C31—C32—H32119.4
O5—C9—H9B109.9C34—C33—C32119.69 (19)
C10—C9—H9B109.9C34—C33—H33120.2
H9A—C9—H9B108.3C32—C33—H33120.2
O6—C10—C9108.91 (18)C33—C34—C35119.73 (19)
O6—C10—H10A109.9C33—C34—H34120.1
C9—C10—H10A109.9C35—C34—H34120.1
O6—C10—H10B109.9C34—C35—C36121.53 (18)
C9—C10—H10B109.9C34—C35—H35119.2
H10A—C10—H10B108.3C36—C35—H35119.2
O6—C11—C12108.73 (18)C35—C36—C31118.21 (17)
O6—C11—H11A109.9C35—C36—C38119.36 (16)
C12—C11—H11A109.9C31—C36—C38122.18 (16)
O6—C11—H11B109.9O31—C37—C69123.84 (16)
C12—C11—H11B109.9O31—C37—C31115.80 (15)
H11A—C11—H11B108.3C69—C37—C31120.25 (15)
O1—C12—C11108.16 (17)O36—C38—C49121.02 (17)
O1—C12—H12A110.1O36—C38—C36114.67 (15)
C11—C12—H12A110.1C49—C38—C36124.12 (16)
O1—C12—H12B110.1C42—C41—C50119.7 (2)
C11—C12—H12B110.1C42—C41—H41120.1
H12A—C12—H12B108.4C50—C41—H41120.1
O7—C13—C14108.6 (2)C43—C42—C41121.4 (2)
O7—C13—K49.80 (11)C43—C42—H42119.3
C14—C13—K137.2 (2)C41—C42—H42119.3
O7—C13—H13A110.0C44—C43—C42119.90 (19)
C14—C13—H13A110.0C44—C43—H43120.0
K—C13—H13A112.4C42—C43—H43120.0
O7—C13—H13B110.0C43—C44—C51119.6 (2)
C14—C13—H13B110.0C43—C44—H44120.2
K—C13—H13B62.1C51—C44—H44120.2
H13A—C13—H13B108.3C46—C45—C52119.1 (2)
C13—C14—C15102.7 (3)C46—C45—H45120.5
C13—C14—H14A111.2C52—C45—H45120.5
C15—C14—H14A111.2C45—C46—C47120.3 (2)
C13—C14—H14B111.2C45—C46—H46119.9
C15—C14—H14B111.2C47—C46—H46119.9
H14A—C14—H14B109.1C48—C47—C46121.3 (2)
C16—C15—C14102.8 (2)C48—C47—H47119.4
C16—C15—H15A111.2C46—C47—H47119.4
C14—C15—H15A111.2C47—C48—C53119.14 (19)
C16—C15—H15B111.2C47—C48—H48120.4
C14—C15—H15B111.2C53—C48—H48120.4
H15A—C15—H15B109.1C38—C49—C53124.13 (17)
O7—C16—C15105.3 (2)C38—C49—C50129.77 (18)
O7—C16—H16A110.7C53—C49—C50106.08 (15)
C15—C16—H16A110.7C41—C50—C51118.51 (17)
O7—C16—H16B110.7C41—C50—C49133.20 (17)
C15—C16—H16B110.7C51—C50—C49108.18 (17)
H16A—C16—H16B108.8C44—C51—C50120.9 (2)
O8—C17—C18106.2 (2)C44—C51—C52130.50 (19)
O8—C17—H17A110.5C50—C51—C52108.56 (16)
C18—C17—H17A110.5C45—C52—C53121.1 (2)
O8—C17—H17B110.5C45—C52—C51130.64 (19)
C18—C17—H17B110.5C53—C52—C51108.27 (17)
H17A—C17—H17B108.7C48—C53—C52119.12 (18)
C17—C18—C19104.1 (2)C48—C53—C49131.99 (17)
C17—C18—H18A110.9C52—C53—C49108.81 (17)
C19—C18—H18A110.9C62—C61—C70119.77 (17)
C17—C18—H18B110.9C62—C61—H61120.1
C19—C18—H18B110.9C70—C61—H61120.1
H18A—C18—H18B109.0C61—C62—C63121.54 (18)
C18—C19—C20103.9 (2)C61—C62—H62119.2
C18—C19—H19A111.0C63—C62—H62119.2
C20—C19—H19A111.0C64—C63—C62119.87 (18)
C18—C19—H19B111.0C64—C63—H63120.1
C20—C19—H19B111.0C62—C63—H63120.1
H19A—C19—H19B109.0C63—C64—C71119.31 (17)
O8—C20—C19105.66 (19)C63—C64—H64120.3
O8—C20—H20A110.6C71—C64—H64120.3
C19—C20—H20A110.6C66—C65—C72118.80 (18)
O8—C20—H20B110.6C66—C65—H65120.6
C19—C20—H20B110.6C72—C65—H65120.6
H20A—C20—H20B108.7C65—C66—C67120.44 (18)
O36—Dy—O3184.77 (5)C65—C66—H66119.8
O36—Dy—C3092.15 (7)C67—C66—H66119.8
O31—Dy—C3082.00 (7)C66—C67—C68121.24 (19)
O36—Dy—C29122.30 (7)C66—C67—H67119.4
O31—Dy—C2982.68 (7)C68—C67—H67119.4
C30—Dy—C2930.36 (7)C73—C68—C67119.14 (18)
O36—Dy—C22110.75 (7)C73—C68—H68120.4
O31—Dy—C22139.57 (7)C67—C68—H68120.4
C30—Dy—C22131.84 (8)C37—C69—C73126.39 (16)
C29—Dy—C22114.91 (8)C37—C69—C70127.37 (16)
O36—Dy—C23134.82 (6)C73—C69—C70106.16 (15)
O31—Dy—C23114.59 (7)C61—C70—C71118.11 (16)
C30—Dy—C23129.23 (8)C61—C70—C69133.47 (16)
C29—Dy—C23101.20 (8)C71—C70—C69108.42 (15)
C22—Dy—C2329.97 (7)C64—C71—C70121.39 (17)
O36—Dy—C2683.65 (6)C64—C71—C72130.18 (17)
O31—Dy—C26110.14 (8)C70—C71—C72108.43 (15)
C30—Dy—C2630.38 (8)C65—C72—C73121.37 (17)
C29—Dy—C2649.84 (7)C65—C72—C71130.35 (18)
C22—Dy—C26108.58 (9)C73—C72—C71108.28 (15)
C23—Dy—C26121.53 (9)C68—C73—C72119.00 (16)
O36—Dy—C24119.37 (8)C68—C73—C69132.30 (17)
O31—Dy—C2489.86 (7)C72—C73—C69108.70 (15)
O7—K—O1—C177.07 (16)C22—C23—C24—C25−0.2 (3)
O3—K—O1—C1−20.00 (17)Dy—C23—C24—C25−68.40 (16)
O8—K—O1—C1−101.42 (16)C22—C23—C24—Dy68.21 (16)
O6—K—O1—C1156.11 (17)O36—Dy—C24—C23−129.87 (15)
O5—K—O1—C1171.75 (15)O31—Dy—C24—C23146.21 (15)
O2—K—O1—C1−8.15 (15)C30—Dy—C24—C2371.1 (2)
C13—K—O1—C170.59 (16)C29—Dy—C24—C2364.49 (17)
O7—K—O1—C12−60.74 (15)C22—Dy—C24—C23−36.62 (14)
O3—K—O1—C12−157.81 (14)C26—Dy—C24—C2310.4 (3)
O8—K—O1—C12120.77 (15)C21—Dy—C24—C23−76.13 (16)
O6—K—O1—C1218.30 (14)C25—Dy—C24—C23−113.1 (2)
O5—K—O1—C1233.94 (16)C28—Dy—C24—C2334.96 (17)
O2—K—O1—C12−145.96 (16)C27—Dy—C24—C237.26 (19)
C13—K—O1—C12−67.22 (15)O36—Dy—C24—C25−16.72 (19)
O7—K—O2—C2−128.46 (15)O31—Dy—C24—C25−100.64 (16)
O3—K—O2—C2142.16 (16)C30—Dy—C24—C25−175.76 (16)
O4—K—O2—C2152.56 (14)C29—Dy—C24—C25177.63 (16)
O1—K—O2—C2−26.03 (14)C22—Dy—C24—C2576.52 (17)
O8—K—O2—C252.77 (15)C23—Dy—C24—C25113.1 (2)
O6—K—O2—C2−41.51 (16)C26—Dy—C24—C25123.6 (2)
C13—K—O2—C2−111.67 (15)C21—Dy—C24—C2537.02 (16)
O7—K—O2—C3108.18 (17)C28—Dy—C24—C25148.10 (17)
O3—K—O2—C318.80 (16)C27—Dy—C24—C25120.40 (18)
O4—K—O2—C329.20 (18)C22—C21—C25—C240.4 (3)
O1—K—O2—C3−149.39 (18)Dy—C21—C25—C2468.06 (16)
O8—K—O2—C3−70.59 (16)C22—C21—C25—Dy−67.63 (17)
O6—K—O2—C3−164.87 (16)C23—C24—C25—C21−0.1 (3)
C13—K—O2—C3124.97 (17)Dy—C24—C25—C21−68.18 (16)
O7—K—O3—C4−75.56 (16)C23—C24—C25—Dy68.03 (16)
O4—K—O3—C4−153.48 (17)O36—Dy—C25—C21−81.04 (15)
O1—K—O3—C428.00 (18)O31—Dy—C25—C21−165.79 (15)
O8—K—O3—C4104.18 (16)C29—Dy—C25—C21109.6 (2)
O5—K—O3—C4−163.98 (15)C22—Dy—C25—C2136.60 (14)
O2—K—O3—C416.16 (15)C23—Dy—C25—C2176.20 (16)
C13—K—O3—C4−52.60 (17)C26—Dy—C25—C21−5.1 (3)
O7—K—O3—C562.62 (17)C24—Dy—C25—C21113.5 (2)
O4—K—O3—C5−15.30 (16)C28—Dy—C25—C2172.0 (2)
O1—K—O3—C5166.18 (16)C27—Dy—C25—C2132.0 (2)
O8—K—O3—C5−117.64 (17)O36—Dy—C25—C24165.48 (16)
O5—K—O3—C5−25.80 (18)O31—Dy—C25—C2480.72 (16)
O2—K—O3—C5154.34 (18)C29—Dy—C25—C24−3.9 (3)
C13—K—O3—C585.58 (17)C22—Dy—C25—C24−76.89 (16)
O7—K—O4—C7111.16 (15)C23—Dy—C25—C24−37.28 (15)
O3—K—O4—C7−152.57 (16)C26—Dy—C25—C24−118.6 (2)
O8—K—O4—C7−70.34 (15)C21—Dy—C25—C24−113.5 (2)
O6—K—O4—C731.30 (16)C28—Dy—C25—C24−41.5 (2)
O5—K—O4—C717.09 (14)C27—Dy—C25—C24−81.5 (2)
O2—K—O4—C7−162.98 (14)O36—Dy—C26—C30−105.33 (15)
C13—K—O4—C7117.53 (15)O31—Dy—C26—C30−23.29 (16)
O7—K—O4—C6−115.64 (16)C29—Dy—C26—C3037.55 (14)
O3—K—O4—C6−19.38 (15)C22—Dy—C26—C30144.87 (15)
O8—K—O4—C662.86 (16)C23—Dy—C26—C30114.86 (16)
O6—K—O4—C6164.50 (14)C24—Dy—C26—C30108.7 (2)
O5—K—O4—C6150.28 (16)C21—Dy—C26—C30174.18 (14)
O2—K—O4—C6−29.79 (17)C25—Dy—C26—C30177.21 (16)
C13—K—O4—C6−109.28 (16)C28—Dy—C26—C3077.04 (16)
O7—K—O5—C8−59.85 (15)C27—Dy—C26—C30114.1 (2)
O3—K—O5—C829.57 (16)O36—Dy—C26—C27140.54 (17)
O4—K—O5—C819.14 (14)O31—Dy—C26—C27−137.42 (16)
O1—K—O5—C8−162.26 (14)C30—Dy—C26—C27−114.1 (2)
O8—K—O5—C8118.94 (15)C29—Dy—C26—C27−76.58 (17)
O6—K—O5—C8−146.72 (16)C22—Dy—C26—C2730.74 (18)
C13—K—O5—C8−76.93 (15)C23—Dy—C26—C270.73 (19)
O7—K—O5—C965.65 (14)C24—Dy—C26—C27−5.4 (3)
O3—K—O5—C9155.07 (13)C21—Dy—C26—C2760.05 (18)
O4—K—O5—C9144.64 (14)C25—Dy—C26—C2763.1 (2)
O1—K—O5—C9−36.76 (15)C28—Dy—C26—C27−37.09 (16)
O8—K—O5—C9−115.56 (14)C30—C26—C27—C280.5 (3)
O6—K—O5—C9−21.22 (13)Dy—C26—C27—C2867.89 (17)
C13—K—O5—C948.57 (14)C30—C26—C27—Dy−67.36 (16)
O7—K—O6—C10−104.07 (14)O36—Dy—C27—C28−154.88 (16)
O4—K—O6—C10−28.10 (15)O31—Dy—C27—C28−57.3 (2)
O1—K—O6—C10150.39 (15)C30—Dy—C27—C28−76.59 (18)
O8—K—O6—C1076.23 (14)C29—Dy—C27—C28−36.57 (16)
O5—K—O6—C10−13.83 (13)C22—Dy—C27—C2895.71 (18)
O2—K—O6—C10165.96 (13)C23—Dy—C27—C2867.06 (17)
C13—K—O6—C10−127.10 (14)C26—Dy—C27—C28−113.6 (2)
O7—K—O6—C11121.56 (15)C24—Dy—C27—C2863.41 (19)
O4—K—O6—C11−162.47 (14)C21—Dy—C27—C28115.23 (17)
O1—K—O6—C1116.02 (14)C25—Dy—C27—C2899.26 (19)
O8—K—O6—C11−58.14 (15)O36—Dy—C27—C26−41.32 (17)
O5—K—O6—C11−148.20 (16)O31—Dy—C27—C2656.29 (19)
O2—K—O6—C1131.59 (16)C30—Dy—C27—C2636.98 (15)
C13—K—O6—C1198.53 (15)C29—Dy—C27—C2677.00 (17)
O3—K—O7—C16−29.6 (2)C22—Dy—C27—C26−150.73 (17)
O4—K—O7—C1630.2 (2)C23—Dy—C27—C26−179.37 (16)
O1—K—O7—C16−150.2 (2)C24—Dy—C27—C26176.98 (15)
O6—K—O7—C16151.5 (2)C21—Dy—C27—C26−131.21 (16)
O5—K—O7—C1690.9 (2)C25—Dy—C27—C26−147.18 (16)
O2—K—O7—C16−90.1 (2)C28—Dy—C27—C26113.6 (2)
C13—K—O7—C16−134.1 (3)C26—C27—C28—C29−0.2 (3)
O3—K—O7—C13104.55 (17)Dy—C27—C28—C2967.34 (16)
O4—K—O7—C13164.33 (17)C26—C27—C28—Dy−67.52 (17)
O1—K—O7—C13−16.04 (17)O36—Dy—C28—C29−80.32 (17)
O6—K—O7—C13−74.35 (17)O31—Dy—C28—C2922.40 (16)
O5—K—O7—C13−134.93 (17)C30—Dy—C28—C29−36.98 (14)
O2—K—O7—C1344.08 (17)C22—Dy—C28—C29164.54 (15)
O3—K—O8—C1773.3 (2)C23—Dy—C28—C29135.00 (16)
O4—K—O8—C1713.8 (2)C26—Dy—C28—C29−77.08 (17)
O1—K—O8—C17−165.8 (2)C24—Dy—C28—C29117.97 (15)
O6—K—O8—C17−107.8 (2)C21—Dy—C28—C29170.18 (14)
O5—K—O8—C17−47.1 (2)C25—Dy—C28—C29138.25 (16)
O2—K—O8—C17133.8 (2)C27—Dy—C28—C29−114.3 (2)
C13—K—O8—C17174.3 (2)O36—Dy—C28—C2734.0 (2)
O3—K—O8—C20−155.90 (17)O31—Dy—C28—C27136.68 (16)
O4—K—O8—C20144.59 (17)C30—Dy—C28—C2777.30 (18)
O1—K—O8—C20−35.00 (17)C29—Dy—C28—C27114.3 (2)
O6—K—O8—C2022.98 (17)C22—Dy—C28—C27−81.18 (18)
O5—K—O8—C2083.63 (17)C23—Dy—C28—C27−110.72 (18)
O2—K—O8—C20−95.37 (17)C26—Dy—C28—C2737.20 (17)
C13—K—O8—C20−55.0 (3)C24—Dy—C28—C27−127.76 (17)
C12—O1—C1—C2179.31 (19)C21—Dy—C28—C27−75.54 (18)
K—O1—C1—C239.7 (2)C25—Dy—C28—C27−107.47 (19)
C3—O2—C2—C1−178.8 (2)C27—C28—C29—C30−0.3 (3)
K—O2—C2—C158.0 (2)Dy—C28—C29—C3067.78 (15)
O1—C1—C2—O2−66.6 (3)C27—C28—C29—Dy−68.03 (17)
C2—O2—C3—C4−172.6 (2)O36—Dy—C29—C28122.03 (14)
K—O2—C3—C4−50.8 (3)O31—Dy—C29—C28−158.92 (15)
C5—O3—C4—C3172.6 (2)C30—Dy—C29—C28114.4 (2)
K—O3—C4—C3−48.2 (2)C22—Dy—C29—C28−17.05 (17)
O2—C3—C4—O367.0 (3)C23—Dy—C29—C28−45.20 (16)
C4—O3—C5—C6−174.27 (19)C26—Dy—C29—C2876.84 (17)
K—O3—C5—C646.4 (2)C24—Dy—C29—C28−72.78 (16)
C7—O4—C6—C5−175.28 (17)C21—Dy—C29—C28−15.5 (2)
K—O4—C6—C550.6 (2)C25—Dy—C29—C28−70.6 (2)
O3—C5—C6—O4−63.7 (2)C27—Dy—C29—C2836.89 (15)
C6—O4—C7—C8175.49 (18)O36—Dy—C29—C307.62 (18)
K—O4—C7—C8−50.3 (2)O31—Dy—C29—C3086.67 (16)
C9—O5—C8—C7−177.39 (19)C22—Dy—C29—C30−131.47 (16)
K—O5—C8—C7−52.6 (2)C23—Dy—C29—C30−159.62 (16)
O4—C7—C8—O570.3 (2)C26—Dy—C29—C30−37.58 (16)
C8—O5—C9—C10177.95 (19)C24—Dy—C29—C30172.81 (15)
K—O5—C9—C1053.6 (2)C21—Dy—C29—C30−129.90 (18)
C11—O6—C10—C9−177.89 (18)C25—Dy—C29—C30175.01 (16)
K—O6—C10—C946.2 (2)C28—Dy—C29—C30−114.4 (2)
O5—C9—C10—O6−67.9 (2)C27—Dy—C29—C30−77.53 (17)
C10—O6—C11—C12177.42 (17)C28—C29—C30—C260.6 (3)
K—O6—C11—C12−46.8 (2)Dy—C29—C30—C2669.45 (15)
C1—O1—C12—C11170.67 (19)C28—C29—C30—Dy−68.87 (16)
K—O1—C12—C11−49.0 (2)C27—C26—C30—C29−0.7 (3)
O6—C11—C12—O162.6 (2)Dy—C26—C30—C29−69.18 (15)
C16—O7—C13—C148.8 (3)C27—C26—C30—Dy68.48 (17)
K—O7—C13—C14−136.7 (2)O36—Dy—C30—C29−173.56 (15)
C16—O7—C13—K145.5 (2)O31—Dy—C30—C29−89.15 (15)
O3—K—C13—O7−76.72 (17)C22—Dy—C30—C2965.81 (19)
O4—K—C13—O7−15.79 (18)C23—Dy—C30—C2926.2 (2)
O1—K—C13—O7163.98 (17)C26—Dy—C30—C29112.9 (2)
O8—K—C13—O7−176.05 (15)C24—Dy—C30—C29−11.7 (2)
O6—K—C13—O7103.04 (17)C21—Dy—C30—C29102.0 (2)
O5—K—C13—O747.12 (17)C28—Dy—C30—C2936.39 (15)
O2—K—C13—O7−133.90 (17)C27—Dy—C30—C2976.08 (17)
O7—K—C13—C1472.8 (3)O36—Dy—C30—C2673.57 (15)
O3—K—C13—C14−3.9 (3)O31—Dy—C30—C26157.98 (15)
O4—K—C13—C1457.0 (3)C29—Dy—C30—C26−112.9 (2)
O1—K—C13—C14−123.2 (3)C22—Dy—C30—C26−47.06 (19)
O8—K—C13—C14−103.3 (3)C23—Dy—C30—C26−86.70 (17)
O6—K—C13—C14175.8 (3)C24—Dy—C30—C26−124.62 (18)
O5—K—C13—C14119.9 (3)C21—Dy—C30—C26−10.8 (3)
O2—K—C13—C14−61.1 (3)C28—Dy—C30—C26−76.48 (17)
O7—C13—C14—C1513.6 (3)C27—Dy—C30—C26−36.79 (15)
K—C13—C14—C15−36.8 (4)C36—C31—C32—C331.7 (3)
C13—C14—C15—C16−29.3 (3)C37—C31—C32—C33−177.68 (17)
C13—O7—C16—C15−28.1 (3)C31—C32—C33—C34−0.9 (3)
K—O7—C16—C15105.6 (2)C32—C33—C34—C35−0.8 (3)
C14—C15—C16—O735.8 (3)C33—C34—C35—C361.8 (3)
C20—O8—C17—C18−39.0 (3)C34—C35—C36—C31−1.1 (3)
K—O8—C17—C1899.2 (2)C34—C35—C36—C38−175.57 (18)
O8—C17—C18—C1924.5 (4)C32—C31—C36—C35−0.6 (3)
C17—C18—C19—C20−1.6 (3)C37—C31—C36—C35178.66 (16)
C17—O8—C20—C1937.8 (3)C32—C31—C36—C38173.66 (17)
K—O8—C20—C19−98.0 (2)C37—C31—C36—C38−7.0 (3)
C18—C19—C20—O8−21.4 (3)Dy—O31—C37—C69130.86 (15)
O36—Dy—O31—C37−13.93 (14)Dy—O31—C37—C31−53.02 (19)
C30—Dy—O31—C37−106.84 (15)C32—C31—C37—O31−93.0 (2)
C29—Dy—O31—C37−137.48 (15)C36—C31—C37—O3187.7 (2)
C22—Dy—O31—C37102.26 (16)C32—C31—C37—C6983.3 (2)
C23—Dy—O31—C37123.52 (14)C36—C31—C37—C69−96.0 (2)
C26—Dy—O31—C37−95.19 (14)Dy—O36—C38—C49176.34 (14)
C24—Dy—O31—C37105.59 (15)Dy—O36—C38—C361.1 (3)
C21—Dy—O31—C3767.07 (15)C35—C36—C38—O36126.44 (18)
C25—Dy—O31—C3775.64 (15)C31—C36—C38—O36−47.8 (2)
C28—Dy—O31—C37−148.52 (14)C35—C36—C38—C49−48.6 (3)
C27—Dy—O31—C37−121.69 (15)C31—C36—C38—C49137.18 (18)
O31—Dy—O36—C3848.1 (2)C50—C41—C42—C430.9 (3)
C30—Dy—O36—C38129.9 (2)C41—C42—C43—C440.6 (3)
C29—Dy—O36—C38126.0 (2)C42—C43—C44—C51−0.9 (3)
C22—Dy—O36—C38−93.4 (2)C52—C45—C46—C470.2 (3)
C23—Dy—O36—C38−71.8 (2)C45—C46—C47—C480.0 (3)
C26—Dy—O36—C38159.1 (2)C46—C47—C48—C53−0.4 (3)
C24—Dy—O36—C38−38.8 (2)O36—C38—C49—C53−8.3 (3)
C21—Dy—O36—C38−77.0 (2)C36—C38—C49—C53166.44 (16)
C25—Dy—O36—C38−47.2 (2)O36—C38—C49—C50173.43 (17)
C28—Dy—O36—C38161.6 (2)C36—C38—C49—C50−11.8 (3)
C27—Dy—O36—C38178.6 (2)C42—C41—C50—C51−2.0 (3)
O36—Dy—C21—C22−147.92 (16)C42—C41—C50—C49−177.68 (19)
O31—Dy—C21—C22131.50 (15)C38—C49—C50—C41−7.8 (3)
C30—Dy—C21—C22−61.9 (2)C53—C49—C50—C41173.65 (19)
C29—Dy—C21—C22−2.8 (2)C38—C49—C50—C51176.21 (18)
C23—Dy—C21—C2236.91 (15)C53—C49—C50—C51−2.32 (19)
C26—Dy—C21—C22−68.45 (17)C43—C44—C51—C50−0.4 (3)
C24—Dy—C21—C2276.90 (17)C43—C44—C51—C52176.7 (2)
C25—Dy—C21—C22114.3 (2)C41—C50—C51—C441.8 (3)
C28—Dy—C21—C22−11.33 (18)C49—C50—C51—C44178.47 (17)
C27—Dy—C21—C22−41.58 (17)C41—C50—C51—C52−175.86 (16)
O36—Dy—C21—C2597.79 (16)C49—C50—C51—C520.8 (2)
O31—Dy—C21—C2517.20 (18)C46—C45—C52—C530.0 (3)
C30—Dy—C21—C25−176.22 (16)C46—C45—C52—C51179.1 (2)
C29—Dy—C21—C25−117.14 (19)C44—C51—C52—C454.6 (3)
C22—Dy—C21—C25−114.3 (2)C50—C51—C52—C45−178.0 (2)
C23—Dy—C21—C25−77.38 (17)C44—C51—C52—C53−176.26 (19)
C26—Dy—C21—C25177.26 (15)C50—C51—C52—C531.1 (2)
C24—Dy—C21—C25−37.39 (16)C47—C48—C53—C520.7 (3)
C28—Dy—C21—C25−125.63 (16)C47—C48—C53—C49−175.67 (19)
C27—Dy—C21—C25−155.88 (16)C45—C52—C53—C48−0.5 (3)
C25—C21—C22—C23−0.5 (3)C51—C52—C53—C48−179.71 (17)
Dy—C21—C22—C23−68.61 (16)C45—C52—C53—C49176.67 (17)
C25—C21—C22—Dy68.06 (16)C51—C52—C53—C49−2.6 (2)
O36—Dy—C22—C23148.43 (15)C38—C49—C53—C481.0 (3)
O31—Dy—C22—C2341.3 (2)C50—C49—C53—C48179.65 (19)
C30—Dy—C22—C23−98.43 (18)C38—C49—C53—C52−175.60 (17)
C29—Dy—C22—C23−67.87 (17)C50—C49—C53—C523.03 (19)
C26—Dy—C22—C23−121.42 (16)C70—C61—C62—C631.0 (3)
C24—Dy—C22—C2336.93 (16)C61—C62—C63—C64−0.2 (3)
C21—Dy—C22—C23113.9 (2)C62—C63—C64—C71−0.5 (3)
C25—Dy—C22—C2377.11 (18)C72—C65—C66—C67−0.2 (3)
C28—Dy—C22—C23−76.30 (17)C65—C66—C67—C680.3 (3)
C27—Dy—C22—C23−106.36 (17)C66—C67—C68—C73−0.4 (3)
O36—Dy—C22—C2134.49 (17)O31—C37—C69—C73−2.4 (3)
O31—Dy—C22—C21−72.63 (18)C31—C37—C69—C73−178.34 (16)
C30—Dy—C22—C21147.64 (16)O31—C37—C69—C70−178.60 (17)
C29—Dy—C22—C21178.19 (15)C31—C37—C69—C705.4 (3)
C23—Dy—C22—C21−113.9 (2)C62—C61—C70—C71−1.1 (3)
C26—Dy—C22—C21124.64 (16)C62—C61—C70—C69178.18 (19)
C24—Dy—C22—C21−77.01 (18)C37—C69—C70—C61−3.7 (3)
C25—Dy—C22—C21−36.83 (16)C73—C69—C70—C61179.44 (19)
C28—Dy—C22—C21169.76 (17)C37—C69—C70—C71175.59 (17)
C27—Dy—C22—C21139.70 (17)C73—C69—C70—C71−1.23 (19)
C21—C22—C23—C240.5 (3)C63—C64—C71—C700.4 (3)
Dy—C22—C23—C24−68.50 (16)C63—C64—C71—C72−179.41 (19)
C21—C22—C23—Dy68.96 (16)C61—C70—C71—C640.4 (3)
O36—Dy—C23—C22−43.6 (2)C69—C70—C71—C64−179.04 (17)
O31—Dy—C23—C22−151.92 (15)C61—C70—C71—C72−179.74 (16)
C30—Dy—C23—C22107.94 (17)C69—C70—C71—C720.8 (2)
C29—Dy—C23—C22121.08 (16)C66—C65—C72—C730.2 (3)
C26—Dy—C23—C2271.61 (17)C66—C65—C72—C71179.97 (19)
C24—Dy—C23—C22−114.2 (2)C64—C71—C72—C650.0 (3)
C21—Dy—C23—C22−36.85 (16)C70—C71—C72—C65−179.81 (19)
C25—Dy—C23—C22−76.70 (18)C64—C71—C72—C73179.78 (19)
C28—Dy—C23—C22100.01 (17)C70—C71—C72—C73−0.1 (2)
C27—Dy—C23—C2271.98 (17)C67—C68—C73—C720.5 (3)
O36—Dy—C23—C2470.57 (18)C67—C68—C73—C69−178.81 (19)
O31—Dy—C23—C24−37.70 (17)C65—C72—C73—C68−0.4 (3)
C30—Dy—C23—C24−137.84 (16)C71—C72—C73—C68179.83 (16)
C29—Dy—C23—C24−124.70 (16)C65—C72—C73—C69179.05 (17)
C22—Dy—C23—C24114.2 (2)C71—C72—C73—C69−0.7 (2)
C26—Dy—C23—C24−174.17 (15)C37—C69—C73—C683.7 (3)
C21—Dy—C23—C2477.37 (18)C70—C69—C73—C68−179.46 (19)
C25—Dy—C23—C2437.52 (16)C37—C69—C73—C72−175.67 (17)
C28—Dy—C23—C24−145.77 (17)C70—C69—C73—C721.20 (19)
C27—Dy—C23—C24−173.80 (16)
Acknowledgements top

The authors thank the Otto-von-Guericke-Universität, Magdeburg, for financial support of this work.

references
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