Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807035738/bi2211sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807035738/bi2211Isup2.hkl |
CCDC reference: 658973
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.003 Å
- R factor = 0.025
- wR factor = 0.067
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.58 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C18 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Dy
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C64 H70 Dy1 K1 O10 Atom count from _chemical_formula_moiety: PLAT794_ALERT_5_G Check Predicted Bond Valency for Dy (2) 0.89
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related literature, see: Edelmann et al. (2007); Goldschmidt & Nagel (1930); Greenhow et al. (1953); Harcourt & O'Ferrall (1995); Meyer & Gottlieb-Billroth (1921).
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.
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).
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.
For related literature, see: Edelmann et al. (2007); Goldschmidt & Nagel (1930); Greenhow et al. (1953); Harcourt & O'Ferrall (1995); Meyer & Gottlieb-Billroth (1921).
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.
Fig. 1. The molecular structure of the title compound showing displacement ellipsoids at the 50% probability level. H atoms are omitted. |
[K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)] | Z = 2 |
Mr = 1200.80 | F(000) = 1238 |
Triclinic, P1 | Dx = 1.420 Mg m−3 |
Hall symbol: -P 1 | Melting point: 663 K |
a = 12.0798 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.0513 (2) Å | Cell parameters from 100 reflections |
c = 19.3154 (3) Å | θ = 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) Å3 | 0.60 × 0.40 × 0.30 mm |
Siemens SMART CCD diffractometer | 13639 independent reflections |
Radiation source: fine-focus sealed tube | 12598 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 29.2°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1997) | h = −13→16 |
Tmin = 0.455, Tmax = 0.641 | k = −17→17 |
19240 measured reflections | l = −26→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H-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 parameters | Δρmax = 1.31 e Å−3 |
0 restraints | Δρmin = −1.40 e Å−3 |
[K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)] | γ = 74.5617 (8)° |
Mr = 1200.80 | V = 2809.20 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 12.0798 (2) Å | Mo Kα radiation |
b = 13.0513 (2) Å | µ = 1.46 mm−1 |
c = 19.3154 (3) Å | T = 173 K |
α = 85.1700 (8)° | 0.60 × 0.40 × 0.30 mm |
β = 73.1480 (7)° |
Siemens SMART CCD diffractometer | 13639 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1997) | 12598 reflections with I > 2σ(I) |
Tmin = 0.455, Tmax = 0.641 | Rint = 0.020 |
19240 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.067 | H-atom parameters constrained |
S = 1.02 | Δρmax = 1.31 e Å−3 |
13639 reflections | Δρmin = −1.40 e Å−3 |
691 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
K | 0.48016 (4) | 0.52461 (3) | 0.25229 (2) | 0.02541 (8) | |
O1 | 0.59368 (13) | 0.67575 (13) | 0.17793 (8) | 0.0329 (3) | |
O2 | 0.46758 (14) | 0.58350 (13) | 0.10802 (9) | 0.0376 (4) | |
O3 | 0.32065 (15) | 0.46039 (13) | 0.19874 (10) | 0.0392 (4) | |
O4 | 0.36303 (13) | 0.37716 (12) | 0.32869 (9) | 0.0337 (3) | |
O5 | 0.49545 (14) | 0.46832 (12) | 0.39557 (8) | 0.0321 (3) | |
O6 | 0.65250 (14) | 0.58081 (12) | 0.30114 (8) | 0.0325 (3) | |
O7 | 0.64954 (16) | 0.33991 (13) | 0.20525 (11) | 0.0477 (4) | |
O8 | 0.30420 (16) | 0.71086 (13) | 0.29797 (10) | 0.0444 (4) | |
C1 | 0.5992 (2) | 0.6930 (2) | 0.10353 (12) | 0.0400 (5) | |
H1A | 0.6649 | 0.6377 | 0.0739 | 0.0452 (16)* | |
H1B | 0.6147 | 0.7633 | 0.0878 | 0.0452 (16)* | |
C2 | 0.4818 (2) | 0.6886 (2) | 0.09360 (14) | 0.0428 (6) | |
H2A | 0.4155 | 0.7389 | 0.1270 | 0.0452 (16)* | |
H2B | 0.4797 | 0.7094 | 0.0434 | 0.0452 (16)* | |
C3 | 0.3584 (2) | 0.5744 (2) | 0.09790 (16) | 0.0480 (6) | |
H3A | 0.3612 | 0.5844 | 0.0461 | 0.0452 (16)* | |
H3B | 0.2909 | 0.6302 | 0.1257 | 0.0452 (16)* | |
C4 | 0.3399 (3) | 0.4670 (2) | 0.12292 (15) | 0.0458 (6) | |
H4A | 0.2699 | 0.4566 | 0.1103 | 0.0452 (16)* | |
H4B | 0.4112 | 0.4110 | 0.0990 | 0.0452 (16)* | |
C5 | 0.2871 (2) | 0.36662 (18) | 0.23024 (15) | 0.0405 (5) | |
H5A | 0.3537 | 0.3032 | 0.2129 | 0.0452 (16)* | |
H5B | 0.2168 | 0.3596 | 0.2163 | 0.0452 (16)* | |
C6 | 0.2575 (2) | 0.37470 (18) | 0.31050 (15) | 0.0396 (5) | |
H6A | 0.1939 | 0.4402 | 0.3275 | 0.0452 (16)* | |
H6B | 0.2283 | 0.3129 | 0.3341 | 0.0452 (16)* | |
C7 | 0.3468 (2) | 0.37626 (19) | 0.40446 (13) | 0.0395 (5) | |
H7A | 0.3170 | 0.3142 | 0.4270 | 0.0452 (16)* | |
H7B | 0.2876 | 0.4417 | 0.4263 | 0.0452 (16)* | |
C8 | 0.4653 (2) | 0.37009 (18) | 0.41659 (13) | 0.0393 (5) | |
H8A | 0.4610 | 0.3555 | 0.4683 | 0.0452 (16)* | |
H8B | 0.5273 | 0.3116 | 0.3877 | 0.0452 (16)* | |
C9 | 0.6100 (2) | 0.46734 (19) | 0.40246 (13) | 0.0368 (5) | |
H9A | 0.6718 | 0.4091 | 0.3732 | 0.0452 (16)* | |
H9B | 0.6106 | 0.4552 | 0.4536 | 0.0452 (16)* | |
C10 | 0.6367 (2) | 0.57188 (18) | 0.37680 (12) | 0.0343 (4) | |
H10A | 0.5699 | 0.6307 | 0.4018 | 0.0452 (16)* | |
H10B | 0.7103 | 0.5765 | 0.3879 | 0.0452 (16)* | |
C11 | 0.6827 (2) | 0.67701 (17) | 0.27198 (13) | 0.0341 (4) | |
H11A | 0.7559 | 0.6820 | 0.2833 | 0.0452 (16)* | |
H11B | 0.6169 | 0.7389 | 0.2936 | 0.0452 (16)* | |
C12 | 0.70304 (18) | 0.67746 (18) | 0.19195 (13) | 0.0333 (4) | |
H12A | 0.7281 | 0.7420 | 0.1703 | 0.0452 (16)* | |
H12B | 0.7670 | 0.6144 | 0.1704 | 0.0452 (16)* | |
C13 | 0.7340 (2) | 0.3667 (2) | 0.14170 (18) | 0.0533 (7) | |
H13A | 0.8074 | 0.3700 | 0.1536 | 0.083 (3)* | |
H13B | 0.6993 | 0.4372 | 0.1229 | 0.083 (3)* | |
C14 | 0.7642 (3) | 0.2830 (3) | 0.08531 (18) | 0.0694 (9) | |
H14A | 0.8448 | 0.2353 | 0.0805 | 0.083 (3)* | |
H14B | 0.7602 | 0.3155 | 0.0376 | 0.083 (3)* | |
C15 | 0.6671 (3) | 0.2232 (3) | 0.11543 (18) | 0.0608 (8) | |
H15A | 0.5958 | 0.2553 | 0.0981 | 0.083 (3)* | |
H15B | 0.6971 | 0.1473 | 0.1017 | 0.083 (3)* | |
C16 | 0.6390 (2) | 0.23608 (19) | 0.19600 (15) | 0.0442 (6) | |
H16A | 0.5571 | 0.2295 | 0.2207 | 0.083 (3)* | |
H16B | 0.6964 | 0.1816 | 0.2159 | 0.083 (3)* | |
C17 | 0.2078 (3) | 0.7031 (3) | 0.35854 (19) | 0.0627 (9) | |
H17A | 0.2008 | 0.6288 | 0.3657 | 0.083 (3)* | |
H17B | 0.1318 | 0.7490 | 0.3519 | 0.083 (3)* | |
C18 | 0.2349 (4) | 0.7394 (3) | 0.42263 (18) | 0.0727 (10) | |
H18A | 0.2747 | 0.6781 | 0.4481 | 0.083 (3)* | |
H18B | 0.1608 | 0.7792 | 0.4572 | 0.083 (3)* | |
C19 | 0.3177 (3) | 0.8110 (2) | 0.38960 (15) | 0.0459 (6) | |
H19A | 0.3954 | 0.7842 | 0.4008 | 0.083 (3)* | |
H19B | 0.2813 | 0.8846 | 0.4077 | 0.083 (3)* | |
C20 | 0.3334 (2) | 0.80660 (17) | 0.30879 (14) | 0.0383 (5) | |
H20A | 0.2793 | 0.8693 | 0.2930 | 0.083 (3)* | |
H20B | 0.4169 | 0.8049 | 0.2811 | 0.083 (3)* | |
Dy | 0.136270 (7) | 0.070125 (6) | 0.128562 (4) | 0.02123 (3) | |
O31 | 0.00368 (12) | 0.22074 (10) | 0.16913 (7) | 0.0233 (3) | |
O36 | 0.20241 (12) | 0.08247 (11) | 0.22062 (7) | 0.0266 (3) | |
C21 | 0.1169 (3) | −0.12320 (19) | 0.18210 (15) | 0.0455 (6) | |
H21 | 0.1679 | −0.1568 | 0.2112 | 0.061 (3)* | |
C22 | 0.1438 (2) | −0.13181 (17) | 0.10779 (14) | 0.0396 (5) | |
H22 | 0.2167 | −0.1719 | 0.0772 | 0.061 (3)* | |
C23 | 0.0467 (2) | −0.07224 (18) | 0.08566 (14) | 0.0392 (5) | |
H23 | 0.0414 | −0.0648 | 0.0373 | 0.061 (3)* | |
C24 | −0.0422 (2) | −0.02476 (19) | 0.14642 (18) | 0.0473 (6) | |
H24 | −0.1183 | 0.0206 | 0.1469 | 0.061 (3)* | |
C25 | 0.0021 (3) | −0.0567 (2) | 0.20691 (15) | 0.0505 (7) | |
H25 | −0.0387 | −0.0367 | 0.2557 | 0.061 (3)* | |
C26 | 0.3442 (2) | 0.1093 (3) | 0.05106 (13) | 0.0459 (6) | |
H26 | 0.4046 | 0.0992 | 0.0751 | 0.061 (3)* | |
C27 | 0.3277 (2) | 0.0325 (2) | 0.01099 (14) | 0.0502 (6) | |
H27 | 0.3743 | −0.0388 | 0.0034 | 0.061 (3)* | |
C28 | 0.2296 (2) | 0.0806 (2) | −0.01572 (12) | 0.0449 (6) | |
H28 | 0.1981 | 0.0473 | −0.0449 | 0.061 (3)* | |
C29 | 0.1866 (2) | 0.1847 (2) | 0.00774 (12) | 0.0407 (5) | |
H29 | 0.1206 | 0.2352 | −0.0028 | 0.061 (3)* | |
C30 | 0.2561 (2) | 0.2034 (2) | 0.04943 (12) | 0.0397 (5) | |
H30 | 0.2456 | 0.2681 | 0.0725 | 0.061 (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 | −0.2269 | 0.2398 | 0.3069 | 0.038 (3)* | |
C33 | −0.20713 (19) | 0.13260 (17) | 0.38785 (12) | 0.0315 (4) | |
H33 | −0.2900 | 0.1380 | 0.4088 | 0.038 (3)* | |
C34 | −0.1237 (2) | 0.06409 (17) | 0.41735 (12) | 0.0321 (4) | |
H34 | −0.1490 | 0.0229 | 0.4590 | 0.038 (3)* | |
C35 | −0.00246 (19) | 0.05567 (15) | 0.38580 (11) | 0.0270 (4) | |
H35 | 0.0545 | 0.0068 | 0.4056 | 0.038 (3)* | |
C36 | 0.03767 (17) | 0.11766 (14) | 0.32550 (10) | 0.0210 (3) | |
C37 | −0.01876 (15) | 0.26107 (14) | 0.23298 (9) | 0.0196 (3) | |
C38 | 0.16958 (17) | 0.09984 (14) | 0.29021 (10) | 0.0211 (3) | |
C41 | 0.13554 (19) | 0.16799 (15) | 0.45819 (11) | 0.0271 (4) | |
H41 | 0.0588 | 0.1889 | 0.4499 | 0.037 (2)* | |
C42 | 0.1486 (2) | 0.18555 (16) | 0.52531 (11) | 0.0316 (4) | |
H42 | 0.0800 | 0.2176 | 0.5627 | 0.037 (2)* | |
C43 | 0.2601 (2) | 0.15705 (16) | 0.53864 (12) | 0.0353 (5) | |
H43 | 0.2670 | 0.1690 | 0.5849 | 0.037 (2)* | |
C44 | 0.3608 (2) | 0.11125 (16) | 0.48450 (12) | 0.0325 (4) | |
H44 | 0.4373 | 0.0925 | 0.4931 | 0.037 (2)* | |
C45 | 0.56362 (19) | 0.01110 (17) | 0.33670 (13) | 0.0329 (4) | |
H45 | 0.6014 | 0.0093 | 0.3738 | 0.037 (2)* | |
C46 | 0.6306 (2) | −0.02579 (18) | 0.26798 (13) | 0.0365 (5) | |
H46 | 0.7147 | −0.0533 | 0.2579 | 0.037 (2)* | |
C47 | 0.57487 (19) | −0.02271 (17) | 0.21366 (12) | 0.0337 (4) | |
H47 | 0.6218 | −0.0482 | 0.1669 | 0.037 (2)* | |
C48 | 0.45198 (18) | 0.01696 (16) | 0.22662 (11) | 0.0277 (4) | |
H48 | 0.4152 | 0.0191 | 0.1890 | 0.037 (2)* | |
C49 | 0.25310 (17) | 0.09335 (14) | 0.32737 (10) | 0.0219 (3) | |
C50 | 0.23571 (18) | 0.11955 (14) | 0.40321 (10) | 0.0233 (4) | |
C51 | 0.34947 (19) | 0.09260 (14) | 0.41686 (11) | 0.0258 (4) | |
C52 | 0.44031 (18) | 0.05074 (15) | 0.35057 (11) | 0.0259 (4) | |
C53 | 0.38291 (17) | 0.05385 (14) | 0.29597 (10) | 0.0233 (4) | |
C61 | −0.07294 (17) | 0.38101 (14) | 0.38571 (10) | 0.0225 (3) | |
H61 | −0.0829 | 0.3112 | 0.3970 | 0.032 (2)* | |
C62 | −0.08552 (18) | 0.44884 (16) | 0.44059 (11) | 0.0265 (4) | |
H62 | −0.1029 | 0.4242 | 0.4893 | 0.032 (2)* | |
C63 | −0.07322 (19) | 0.55228 (16) | 0.42597 (11) | 0.0275 (4) | |
H63 | −0.0824 | 0.5974 | 0.4645 | 0.032 (2)* | |
C64 | −0.04756 (18) | 0.58916 (15) | 0.35525 (11) | 0.0254 (4) | |
H64 | −0.0397 | 0.6598 | 0.3449 | 0.032 (2)* | |
C65 | 0.01487 (18) | 0.63022 (15) | 0.18095 (11) | 0.0271 (4) | |
H65 | 0.0115 | 0.6928 | 0.2041 | 0.032 (2)* | |
C66 | 0.0401 (2) | 0.62683 (17) | 0.10631 (12) | 0.0307 (4) | |
H66 | 0.0539 | 0.6877 | 0.0780 | 0.032 (2)* | |
C67 | 0.0454 (2) | 0.53472 (17) | 0.07253 (11) | 0.0309 (4) | |
H67 | 0.0632 | 0.5336 | 0.0213 | 0.032 (2)* | |
C68 | 0.02505 (18) | 0.44395 (15) | 0.11257 (10) | 0.0255 (4) | |
H68 | 0.0284 | 0.3818 | 0.0889 | 0.032 (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) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K | 0.02496 (19) | 0.02416 (18) | 0.02657 (19) | −0.00700 (15) | −0.00607 (15) | 0.00129 (15) |
O1 | 0.0241 (7) | 0.0446 (9) | 0.0315 (8) | −0.0146 (6) | −0.0076 (6) | 0.0109 (6) |
O2 | 0.0318 (8) | 0.0444 (9) | 0.0414 (9) | −0.0120 (7) | −0.0183 (7) | 0.0114 (7) |
O3 | 0.0391 (9) | 0.0347 (8) | 0.0537 (10) | −0.0167 (7) | −0.0237 (8) | 0.0076 (7) |
O4 | 0.0248 (7) | 0.0359 (8) | 0.0381 (8) | −0.0092 (6) | −0.0057 (6) | 0.0068 (6) |
O5 | 0.0334 (8) | 0.0288 (7) | 0.0322 (8) | −0.0058 (6) | −0.0097 (6) | 0.0057 (6) |
O6 | 0.0355 (8) | 0.0318 (7) | 0.0331 (8) | −0.0102 (6) | −0.0128 (6) | 0.0015 (6) |
O7 | 0.0413 (10) | 0.0317 (8) | 0.0615 (12) | −0.0077 (7) | 0.0001 (9) | −0.0098 (8) |
O8 | 0.0408 (9) | 0.0282 (8) | 0.0580 (11) | −0.0088 (7) | −0.0015 (8) | −0.0093 (7) |
C1 | 0.0375 (12) | 0.0509 (14) | 0.0314 (11) | −0.0190 (11) | −0.0066 (9) | 0.0153 (10) |
C2 | 0.0456 (14) | 0.0489 (14) | 0.0377 (12) | −0.0160 (11) | −0.0189 (11) | 0.0172 (11) |
C3 | 0.0440 (14) | 0.0561 (15) | 0.0557 (16) | −0.0163 (12) | −0.0331 (13) | 0.0155 (13) |
C4 | 0.0445 (14) | 0.0477 (14) | 0.0567 (16) | −0.0143 (12) | −0.0303 (12) | 0.0038 (12) |
C5 | 0.0322 (11) | 0.0290 (10) | 0.0687 (17) | −0.0121 (9) | −0.0246 (11) | 0.0055 (11) |
C6 | 0.0247 (10) | 0.0305 (11) | 0.0638 (16) | −0.0115 (9) | −0.0106 (10) | 0.0072 (10) |
C7 | 0.0413 (12) | 0.0315 (11) | 0.0367 (12) | −0.0121 (9) | 0.0041 (10) | 0.0046 (9) |
C8 | 0.0566 (15) | 0.0299 (11) | 0.0305 (11) | −0.0107 (10) | −0.0132 (10) | 0.0081 (9) |
C9 | 0.0360 (11) | 0.0384 (11) | 0.0348 (11) | −0.0018 (9) | −0.0156 (9) | 0.0023 (9) |
C10 | 0.0318 (11) | 0.0396 (11) | 0.0331 (11) | −0.0045 (9) | −0.0149 (9) | −0.0024 (9) |
C11 | 0.0279 (10) | 0.0320 (10) | 0.0450 (12) | −0.0092 (8) | −0.0133 (9) | 0.0010 (9) |
C12 | 0.0213 (9) | 0.0352 (11) | 0.0434 (12) | −0.0110 (8) | −0.0069 (8) | 0.0041 (9) |
C13 | 0.0325 (12) | 0.0431 (14) | 0.075 (2) | −0.0077 (11) | −0.0033 (13) | 0.0038 (13) |
C14 | 0.069 (2) | 0.082 (2) | 0.0484 (17) | −0.0144 (19) | −0.0091 (16) | 0.0017 (16) |
C15 | 0.066 (2) | 0.0591 (18) | 0.064 (2) | −0.0085 (16) | −0.0333 (17) | −0.0094 (15) |
C16 | 0.0425 (13) | 0.0336 (12) | 0.0571 (16) | −0.0090 (10) | −0.0146 (12) | −0.0032 (11) |
C17 | 0.0485 (16) | 0.0518 (16) | 0.082 (2) | −0.0283 (14) | 0.0079 (15) | −0.0103 (15) |
C18 | 0.096 (3) | 0.072 (2) | 0.0519 (18) | −0.049 (2) | −0.0002 (18) | 0.0077 (16) |
C19 | 0.0481 (14) | 0.0371 (12) | 0.0525 (15) | −0.0109 (11) | −0.0144 (12) | 0.0016 (11) |
C20 | 0.0338 (11) | 0.0263 (10) | 0.0512 (14) | −0.0077 (9) | −0.0061 (10) | −0.0011 (9) |
Dy | 0.02097 (5) | 0.02315 (5) | 0.01945 (5) | −0.00487 (3) | −0.00488 (3) | −0.00452 (3) |
O31 | 0.0272 (7) | 0.0204 (6) | 0.0210 (6) | −0.0025 (5) | −0.0074 (5) | −0.0026 (5) |
O36 | 0.0258 (7) | 0.0332 (7) | 0.0206 (6) | −0.0055 (6) | −0.0072 (5) | −0.0038 (5) |
C21 | 0.0659 (17) | 0.0322 (11) | 0.0546 (15) | −0.0230 (12) | −0.0359 (14) | 0.0131 (11) |
C22 | 0.0425 (13) | 0.0227 (10) | 0.0536 (14) | −0.0033 (9) | −0.0155 (11) | −0.0085 (9) |
C23 | 0.0509 (14) | 0.0334 (11) | 0.0451 (13) | −0.0156 (10) | −0.0268 (11) | −0.0014 (10) |
C24 | 0.0300 (11) | 0.0313 (11) | 0.085 (2) | −0.0097 (9) | −0.0183 (12) | −0.0086 (12) |
C25 | 0.0702 (19) | 0.0479 (14) | 0.0388 (13) | −0.0419 (14) | 0.0038 (12) | −0.0096 (11) |
C26 | 0.0253 (10) | 0.0837 (19) | 0.0298 (11) | −0.0217 (12) | −0.0061 (9) | 0.0130 (12) |
C27 | 0.0368 (13) | 0.0538 (15) | 0.0413 (13) | −0.0002 (11) | 0.0092 (11) | −0.0059 (11) |
C28 | 0.0406 (13) | 0.0729 (18) | 0.0215 (10) | −0.0209 (12) | 0.0002 (9) | −0.0119 (10) |
C29 | 0.0305 (11) | 0.0603 (15) | 0.0253 (10) | −0.0116 (11) | −0.0015 (8) | 0.0103 (10) |
C30 | 0.0410 (13) | 0.0514 (14) | 0.0272 (10) | −0.0244 (11) | 0.0006 (9) | 0.0032 (9) |
C31 | 0.0235 (8) | 0.0165 (7) | 0.0207 (8) | −0.0049 (6) | −0.0064 (7) | −0.0019 (6) |
C32 | 0.0228 (9) | 0.0262 (9) | 0.0284 (9) | −0.0067 (7) | −0.0067 (7) | −0.0024 (7) |
C33 | 0.0277 (10) | 0.0324 (10) | 0.0345 (11) | −0.0135 (8) | −0.0026 (8) | −0.0029 (8) |
C34 | 0.0390 (11) | 0.0276 (10) | 0.0303 (10) | −0.0157 (9) | −0.0054 (9) | 0.0048 (8) |
C35 | 0.0342 (10) | 0.0205 (8) | 0.0270 (9) | −0.0076 (8) | −0.0097 (8) | 0.0030 (7) |
C36 | 0.0261 (9) | 0.0178 (8) | 0.0203 (8) | −0.0058 (7) | −0.0076 (7) | −0.0012 (6) |
C37 | 0.0168 (7) | 0.0208 (8) | 0.0212 (8) | −0.0037 (6) | −0.0062 (6) | 0.0002 (6) |
C38 | 0.0250 (9) | 0.0171 (7) | 0.0215 (8) | −0.0039 (6) | −0.0080 (7) | 0.0001 (6) |
C41 | 0.0359 (11) | 0.0188 (8) | 0.0264 (9) | −0.0021 (7) | −0.0127 (8) | −0.0008 (7) |
C42 | 0.0470 (12) | 0.0217 (9) | 0.0251 (9) | −0.0051 (8) | −0.0111 (9) | −0.0025 (7) |
C43 | 0.0578 (15) | 0.0251 (9) | 0.0283 (10) | −0.0077 (9) | −0.0226 (10) | −0.0003 (8) |
C44 | 0.0421 (12) | 0.0280 (10) | 0.0348 (11) | −0.0077 (9) | −0.0235 (9) | 0.0018 (8) |
C45 | 0.0290 (10) | 0.0306 (10) | 0.0438 (12) | −0.0081 (8) | −0.0185 (9) | 0.0064 (9) |
C46 | 0.0240 (10) | 0.0347 (11) | 0.0486 (13) | −0.0058 (8) | −0.0100 (9) | 0.0062 (10) |
C47 | 0.0274 (10) | 0.0317 (10) | 0.0365 (11) | −0.0057 (8) | −0.0031 (8) | 0.0021 (9) |
C48 | 0.0277 (10) | 0.0265 (9) | 0.0277 (9) | −0.0056 (8) | −0.0075 (8) | 0.0008 (7) |
C49 | 0.0254 (9) | 0.0177 (8) | 0.0223 (8) | −0.0027 (7) | −0.0087 (7) | 0.0001 (6) |
C50 | 0.0304 (9) | 0.0160 (8) | 0.0251 (9) | −0.0041 (7) | −0.0124 (7) | 0.0015 (7) |
C51 | 0.0333 (10) | 0.0176 (8) | 0.0295 (9) | −0.0046 (7) | −0.0154 (8) | 0.0015 (7) |
C52 | 0.0294 (10) | 0.0195 (8) | 0.0321 (10) | −0.0060 (7) | −0.0147 (8) | 0.0033 (7) |
C53 | 0.0244 (9) | 0.0186 (8) | 0.0275 (9) | −0.0043 (7) | −0.0098 (7) | 0.0013 (7) |
C61 | 0.0237 (9) | 0.0208 (8) | 0.0241 (9) | −0.0044 (7) | −0.0095 (7) | 0.0005 (7) |
C62 | 0.0294 (10) | 0.0274 (9) | 0.0236 (9) | −0.0038 (8) | −0.0111 (7) | −0.0024 (7) |
C63 | 0.0319 (10) | 0.0270 (9) | 0.0265 (9) | −0.0060 (8) | −0.0118 (8) | −0.0072 (7) |
C64 | 0.0268 (9) | 0.0209 (8) | 0.0309 (10) | −0.0063 (7) | −0.0105 (8) | −0.0033 (7) |
C65 | 0.0271 (9) | 0.0232 (9) | 0.0342 (10) | −0.0098 (7) | −0.0112 (8) | 0.0026 (8) |
C66 | 0.0330 (10) | 0.0289 (10) | 0.0349 (11) | −0.0144 (8) | −0.0140 (9) | 0.0113 (8) |
C67 | 0.0354 (11) | 0.0366 (11) | 0.0259 (10) | −0.0147 (9) | −0.0138 (8) | 0.0084 (8) |
C68 | 0.0285 (9) | 0.0261 (9) | 0.0252 (9) | −0.0090 (7) | −0.0108 (7) | 0.0013 (7) |
C69 | 0.0200 (8) | 0.0203 (8) | 0.0210 (8) | −0.0045 (6) | −0.0073 (6) | −0.0001 (6) |
C70 | 0.0176 (8) | 0.0190 (8) | 0.0232 (8) | −0.0027 (6) | −0.0075 (6) | −0.0020 (6) |
C71 | 0.0197 (8) | 0.0200 (8) | 0.0254 (9) | −0.0043 (6) | −0.0084 (7) | −0.0011 (7) |
C72 | 0.0194 (8) | 0.0215 (8) | 0.0255 (9) | −0.0060 (7) | −0.0085 (7) | 0.0012 (7) |
C73 | 0.0197 (8) | 0.0192 (8) | 0.0235 (8) | −0.0050 (6) | −0.0083 (7) | 0.0008 (6) |
K—O7 | 2.7364 (18) | Dy—C25 | 2.691 (2) |
K—O3 | 2.7652 (16) | Dy—C28 | 2.693 (2) |
K—O4 | 2.7649 (15) | Dy—C27 | 2.699 (2) |
K—O1 | 2.7669 (15) | O31—C37 | 1.308 (2) |
K—O8 | 2.7800 (18) | O36—C38 | 1.308 (2) |
K—O6 | 2.7983 (15) | C21—C22 | 1.384 (4) |
K—O5 | 2.8488 (15) | C21—C25 | 1.397 (4) |
K—O2 | 2.8638 (16) | C21—H21 | 0.950 |
K—C13 | 3.434 (3) | C22—C23 | 1.383 (3) |
O1—C1 | 1.421 (3) | C22—H22 | 0.950 |
O1—C12 | 1.429 (2) | C23—C24 | 1.397 (4) |
O2—C2 | 1.422 (3) | C23—H23 | 0.950 |
O2—C3 | 1.424 (3) | C24—C25 | 1.410 (4) |
O3—C4 | 1.414 (3) | C24—H24 | 0.950 |
O3—C5 | 1.424 (3) | C25—H25 | 0.950 |
O4—C7 | 1.419 (3) | C26—C30 | 1.399 (4) |
O4—C6 | 1.426 (3) | C26—C27 | 1.403 (4) |
O5—C8 | 1.420 (3) | C26—H26 | 0.950 |
O5—C9 | 1.424 (3) | C27—C28 | 1.403 (4) |
O6—C10 | 1.417 (3) | C27—H27 | 0.950 |
O6—C11 | 1.425 (3) | C28—C29 | 1.384 (4) |
O7—C16 | 1.425 (3) | C28—H28 | 0.950 |
O7—C13 | 1.436 (3) | C29—C30 | 1.395 (3) |
O8—C17 | 1.410 (3) | C29—H29 | 0.950 |
O8—C20 | 1.432 (3) | C30—H30 | 0.950 |
C1—C2 | 1.501 (3) | C31—C32 | 1.396 (3) |
C1—H1A | 0.990 | C31—C36 | 1.406 (2) |
C1—H1B | 0.990 | C31—C37 | 1.506 (2) |
C2—H2A | 0.990 | C32—C33 | 1.390 (3) |
C2—H2B | 0.990 | C32—H32 | 0.950 |
C3—C4 | 1.496 (4) | C33—C34 | 1.381 (3) |
C3—H3A | 0.990 | C33—H33 | 0.950 |
C3—H3B | 0.990 | C34—C35 | 1.392 (3) |
C4—H4A | 0.990 | C34—H34 | 0.950 |
C4—H4B | 0.990 | C35—C36 | 1.403 (2) |
C5—C6 | 1.493 (4) | C35—H35 | 0.950 |
C5—H5A | 0.990 | C36—C38 | 1.502 (3) |
C5—H5B | 0.990 | C37—C69 | 1.373 (2) |
C6—H6A | 0.990 | C38—C49 | 1.380 (2) |
C6—H6B | 0.990 | C41—C42 | 1.395 (3) |
C7—C8 | 1.497 (4) | C41—C50 | 1.397 (3) |
C7—H7A | 0.990 | C41—H41 | 0.950 |
C7—H7B | 0.990 | C42—C43 | 1.392 (3) |
C8—H8A | 0.990 | C42—H42 | 0.950 |
C8—H8B | 0.990 | C43—C44 | 1.382 (3) |
C9—C10 | 1.497 (3) | C43—H43 | 0.950 |
C9—H9A | 0.990 | C44—C51 | 1.400 (3) |
C9—H9B | 0.990 | C44—H44 | 0.950 |
C10—H10A | 0.990 | C45—C46 | 1.388 (3) |
C10—H10B | 0.990 | C45—C52 | 1.393 (3) |
C11—C12 | 1.493 (3) | C45—H45 | 0.950 |
C11—H11A | 0.990 | C46—C47 | 1.394 (3) |
C11—H11B | 0.990 | C46—H46 | 0.950 |
C12—H12A | 0.990 | C47—C48 | 1.390 (3) |
C12—H12B | 0.990 | C47—H47 | 0.950 |
C13—C14 | 1.507 (5) | C48—C53 | 1.403 (3) |
C13—H13A | 0.990 | C48—H48 | 0.950 |
C13—H13B | 0.990 | C49—C53 | 1.471 (3) |
C14—C15 | 1.529 (5) | C49—C50 | 1.475 (3) |
C14—H14A | 0.990 | C50—C51 | 1.421 (3) |
C14—H14B | 0.990 | C51—C52 | 1.458 (3) |
C15—C16 | 1.508 (4) | C52—C53 | 1.413 (3) |
C15—H15A | 0.990 | C61—C62 | 1.387 (3) |
C15—H15B | 0.990 | C61—C70 | 1.402 (2) |
C16—H16A | 0.990 | C61—H61 | 0.950 |
C16—H16B | 0.990 | C62—C63 | 1.394 (3) |
C17—C18 | 1.510 (5) | C62—H62 | 0.950 |
C17—H17A | 0.990 | C63—C64 | 1.385 (3) |
C17—H17B | 0.990 | C63—H63 | 0.950 |
C18—C19 | 1.520 (4) | C64—C71 | 1.394 (3) |
C18—H18A | 0.990 | C64—H64 | 0.950 |
C18—H18B | 0.990 | C65—C66 | 1.387 (3) |
C19—C20 | 1.521 (4) | C65—C72 | 1.394 (3) |
C19—H19A | 0.990 | C65—H65 | 0.950 |
C19—H19B | 0.990 | C66—C67 | 1.394 (3) |
C20—H20A | 0.990 | C66—H66 | 0.950 |
C20—H20B | 0.990 | C67—C68 | 1.397 (3) |
Dy—O36 | 2.1832 (13) | C67—H67 | 0.950 |
Dy—O31 | 2.2134 (13) | C68—C73 | 1.397 (3) |
Dy—C30 | 2.658 (2) | C68—H68 | 0.950 |
Dy—C29 | 2.670 (2) | C69—C73 | 1.471 (2) |
Dy—C22 | 2.673 (2) | C69—C70 | 1.471 (2) |
Dy—C23 | 2.675 (2) | C70—C71 | 1.422 (2) |
Dy—C26 | 2.680 (2) | C71—C72 | 1.458 (3) |
Dy—C24 | 2.687 (2) | C72—C73 | 1.418 (2) |
Dy—C21 | 2.688 (2) | ||
O7—K—O3 | 90.26 (6) | C30—Dy—C24 | 146.66 (9) |
O7—K—O4 | 79.66 (5) | C29—Dy—C24 | 116.67 (9) |
O3—K—O4 | 60.37 (5) | C22—Dy—C24 | 49.80 (8) |
O7—K—O1 | 101.60 (5) | C23—Dy—C24 | 30.21 (8) |
O3—K—O1 | 119.84 (5) | C26—Dy—C24 | 151.47 (9) |
O4—K—O1 | 178.69 (5) | O36—Dy—C21 | 85.56 (6) |
O7—K—O8 | 178.42 (6) | O31—Dy—C21 | 124.28 (8) |
O3—K—O8 | 88.18 (5) | C30—Dy—C21 | 153.13 (9) |
O4—K—O8 | 99.79 (5) | C29—Dy—C21 | 144.81 (9) |
O1—K—O8 | 78.96 (5) | C22—Dy—C21 | 29.92 (8) |
O7—K—O6 | 86.54 (5) | C23—Dy—C21 | 49.48 (7) |
O3—K—O6 | 176.62 (5) | C26—Dy—C21 | 123.02 (9) |
O4—K—O6 | 119.97 (5) | C24—Dy—C21 | 49.83 (8) |
O1—K—O6 | 59.89 (4) | O36—Dy—C25 | 90.05 (7) |
O8—K—O6 | 95.01 (5) | O31—Dy—C25 | 95.24 (8) |
O7—K—O5 | 88.51 (5) | C30—Dy—C25 | 176.30 (9) |
O3—K—O5 | 120.51 (5) | C29—Dy—C25 | 147.02 (8) |
O4—K—O5 | 60.96 (5) | C22—Dy—C25 | 49.69 (8) |
O1—K—O5 | 118.58 (5) | C23—Dy—C25 | 49.81 (8) |
O8—K—O5 | 92.51 (5) | C26—Dy—C25 | 153.07 (10) |
O6—K—O5 | 60.55 (4) | C24—Dy—C25 | 30.39 (9) |
O7—K—O2 | 91.62 (6) | C21—Dy—C25 | 30.10 (9) |
O3—K—O2 | 60.48 (5) | O36—Dy—C28 | 133.37 (7) |
O4—K—O2 | 120.04 (5) | O31—Dy—C28 | 110.54 (7) |
O1—K—O2 | 60.43 (5) | C30—Dy—C28 | 49.93 (8) |
O8—K—O2 | 87.38 (5) | C29—Dy—C28 | 29.91 (8) |
O6—K—O2 | 118.47 (5) | C22—Dy—C28 | 86.15 (8) |
O5—K—O2 | 179.00 (5) | C23—Dy—C28 | 79.85 (8) |
O7—K—C13 | 23.63 (6) | C26—Dy—C28 | 49.77 (7) |
O3—K—C13 | 96.02 (7) | C24—Dy—C28 | 104.90 (9) |
O4—K—C13 | 102.42 (6) | C21—Dy—C28 | 115.57 (9) |
O1—K—C13 | 78.87 (6) | C25—Dy—C28 | 129.56 (8) |
O8—K—C13 | 156.45 (6) | O36—Dy—C27 | 106.91 (8) |
O6—K—C13 | 80.61 (6) | O31—Dy—C27 | 130.21 (7) |
O5—K—C13 | 105.02 (6) | C30—Dy—C27 | 50.12 (9) |
O2—K—C13 | 74.82 (6) | C29—Dy—C27 | 49.72 (8) |
C1—O1—C12 | 111.96 (16) | C22—Dy—C27 | 82.24 (9) |
C1—O1—K | 118.11 (13) | C23—Dy—C27 | 91.29 (9) |
C12—O1—K | 116.56 (11) | C26—Dy—C27 | 30.24 (9) |
C2—O2—C3 | 111.57 (18) | C24—Dy—C27 | 121.31 (9) |
C2—O2—K | 108.88 (13) | C21—Dy—C27 | 105.07 (9) |
C3—O2—K | 111.25 (14) | C25—Dy—C27 | 131.83 (9) |
C4—O3—C5 | 113.67 (19) | C28—Dy—C27 | 30.16 (8) |
C4—O3—K | 116.46 (14) | C37—O31—Dy | 125.31 (11) |
C5—O3—K | 116.24 (13) | C38—O36—Dy | 143.67 (12) |
C7—O4—C6 | 112.76 (18) | C22—C21—C25 | 108.3 (2) |
C7—O4—K | 114.76 (13) | C22—C21—Dy | 74.44 (13) |
C6—O4—K | 114.96 (12) | C25—C21—Dy | 75.08 (13) |
C8—O5—C9 | 112.41 (17) | C22—C21—H21 | 125.9 |
C8—O5—K | 110.42 (12) | C25—C21—H21 | 125.9 |
C9—O5—K | 111.21 (12) | Dy—C21—H21 | 116.7 |
C10—O6—C11 | 112.36 (17) | C23—C22—C21 | 108.4 (2) |
C10—O6—K | 115.49 (12) | C23—C22—Dy | 75.12 (13) |
C11—O6—K | 115.85 (12) | C21—C22—Dy | 75.64 (13) |
C16—O7—C13 | 108.1 (2) | C23—C22—H22 | 125.8 |
C16—O7—K | 131.44 (15) | C21—C22—H22 | 125.8 |
C13—O7—K | 106.58 (14) | Dy—C22—H22 | 115.6 |
C17—O8—C20 | 104.91 (19) | C22—C23—C24 | 108.5 (2) |
C17—O8—K | 116.98 (16) | C22—C23—Dy | 74.91 (13) |
C20—O8—K | 121.67 (14) | C24—C23—Dy | 75.35 (13) |
O1—C1—C2 | 108.38 (18) | C22—C23—H23 | 125.7 |
O1—C1—H1A | 110.0 | C24—C23—H23 | 125.7 |
C2—C1—H1A | 110.0 | Dy—C23—H23 | 116.1 |
O1—C1—H1B | 110.0 | C23—C24—C25 | 107.2 (2) |
C2—C1—H1B | 110.0 | C23—C24—Dy | 74.44 (13) |
H1A—C1—H1B | 108.4 | C25—C24—Dy | 74.97 (13) |
O2—C2—C1 | 109.29 (19) | C23—C24—H24 | 126.4 |
O2—C2—H2A | 109.8 | C25—C24—H24 | 126.4 |
C1—C2—H2A | 109.8 | Dy—C24—H24 | 116.4 |
O2—C2—H2B | 109.8 | C21—C25—C24 | 107.5 (2) |
C1—C2—H2B | 109.8 | C21—C25—Dy | 74.82 (14) |
H2A—C2—H2B | 108.3 | C24—C25—Dy | 74.64 (14) |
O2—C3—C4 | 109.51 (19) | C21—C25—H25 | 126.2 |
O2—C3—H3A | 109.8 | C24—C25—H25 | 126.2 |
C4—C3—H3A | 109.8 | Dy—C25—H25 | 116.5 |
O2—C3—H3B | 109.8 | C30—C26—C27 | 108.2 (2) |
C4—C3—H3B | 109.8 | C30—C26—Dy | 73.93 (13) |
H3A—C3—H3B | 108.2 | C27—C26—Dy | 75.61 (14) |
O3—C4—C3 | 108.5 (2) | C30—C26—H26 | 125.9 |
O3—C4—H4A | 110.0 | C27—C26—H26 | 125.9 |
C3—C4—H4A | 110.0 | Dy—C26—H26 | 116.6 |
O3—C4—H4B | 110.0 | C28—C27—C26 | 107.4 (2) |
C3—C4—H4B | 110.0 | C28—C27—Dy | 74.70 (14) |
H4A—C4—H4B | 108.4 | C26—C27—Dy | 74.15 (14) |
O3—C5—C6 | 108.22 (19) | C28—C27—H27 | 126.3 |
O3—C5—H5A | 110.1 | C26—C27—H27 | 126.3 |
C6—C5—H5A | 110.1 | Dy—C27—H27 | 117.0 |
O3—C5—H5B | 110.1 | C29—C28—C27 | 108.2 (2) |
C6—C5—H5B | 110.1 | C29—C28—Dy | 74.11 (13) |
H5A—C5—H5B | 108.4 | C27—C28—Dy | 75.14 (14) |
O4—C6—C5 | 108.32 (19) | C29—C28—H28 | 125.9 |
O4—C6—H6A | 110.0 | C27—C28—H28 | 125.9 |
C5—C6—H6A | 110.0 | Dy—C28—H28 | 116.9 |
O4—C6—H6B | 110.0 | C28—C29—C30 | 108.7 (2) |
C5—C6—H6B | 110.0 | C28—C29—Dy | 75.98 (14) |
H6A—C6—H6B | 108.4 | C30—C29—Dy | 74.35 (12) |
O4—C7—C8 | 107.72 (18) | C28—C29—H29 | 125.6 |
O4—C7—H7A | 110.2 | C30—C29—H29 | 125.6 |
C8—C7—H7A | 110.2 | Dy—C29—H29 | 116.1 |
O4—C7—H7B | 110.2 | C29—C30—C26 | 107.5 (2) |
C8—C7—H7B | 110.2 | C29—C30—Dy | 75.29 (13) |
H7A—C7—H7B | 108.5 | C26—C30—Dy | 75.69 (13) |
O5—C8—C7 | 108.91 (18) | C29—C30—H30 | 126.2 |
O5—C8—H8A | 109.9 | C26—C30—H30 | 126.2 |
C7—C8—H8A | 109.9 | Dy—C30—H30 | 115.1 |
O5—C8—H8B | 109.9 | C32—C31—C36 | 119.63 (17) |
C7—C8—H8B | 109.9 | C32—C31—C37 | 116.15 (16) |
H8A—C8—H8B | 108.3 | C36—C31—C37 | 124.22 (16) |
O5—C9—C10 | 109.02 (17) | C33—C32—C31 | 121.17 (18) |
O5—C9—H9A | 109.9 | C33—C32—H32 | 119.4 |
C10—C9—H9A | 109.9 | C31—C32—H32 | 119.4 |
O5—C9—H9B | 109.9 | C34—C33—C32 | 119.69 (19) |
C10—C9—H9B | 109.9 | C34—C33—H33 | 120.2 |
H9A—C9—H9B | 108.3 | C32—C33—H33 | 120.2 |
O6—C10—C9 | 108.91 (18) | C33—C34—C35 | 119.73 (19) |
O6—C10—H10A | 109.9 | C33—C34—H34 | 120.1 |
C9—C10—H10A | 109.9 | C35—C34—H34 | 120.1 |
O6—C10—H10B | 109.9 | C34—C35—C36 | 121.53 (18) |
C9—C10—H10B | 109.9 | C34—C35—H35 | 119.2 |
H10A—C10—H10B | 108.3 | C36—C35—H35 | 119.2 |
O6—C11—C12 | 108.73 (18) | C35—C36—C31 | 118.21 (17) |
O6—C11—H11A | 109.9 | C35—C36—C38 | 119.36 (16) |
C12—C11—H11A | 109.9 | C31—C36—C38 | 122.18 (16) |
O6—C11—H11B | 109.9 | O31—C37—C69 | 123.84 (16) |
C12—C11—H11B | 109.9 | O31—C37—C31 | 115.80 (15) |
H11A—C11—H11B | 108.3 | C69—C37—C31 | 120.25 (15) |
O1—C12—C11 | 108.16 (17) | O36—C38—C49 | 121.02 (17) |
O1—C12—H12A | 110.1 | O36—C38—C36 | 114.67 (15) |
C11—C12—H12A | 110.1 | C49—C38—C36 | 124.12 (16) |
O1—C12—H12B | 110.1 | C42—C41—C50 | 119.7 (2) |
C11—C12—H12B | 110.1 | C42—C41—H41 | 120.1 |
H12A—C12—H12B | 108.4 | C50—C41—H41 | 120.1 |
O7—C13—C14 | 108.6 (2) | C43—C42—C41 | 121.4 (2) |
O7—C13—K | 49.80 (11) | C43—C42—H42 | 119.3 |
C14—C13—K | 137.2 (2) | C41—C42—H42 | 119.3 |
O7—C13—H13A | 110.0 | C44—C43—C42 | 119.90 (19) |
C14—C13—H13A | 110.0 | C44—C43—H43 | 120.0 |
K—C13—H13A | 112.4 | C42—C43—H43 | 120.0 |
O7—C13—H13B | 110.0 | C43—C44—C51 | 119.6 (2) |
C14—C13—H13B | 110.0 | C43—C44—H44 | 120.2 |
K—C13—H13B | 62.1 | C51—C44—H44 | 120.2 |
H13A—C13—H13B | 108.3 | C46—C45—C52 | 119.1 (2) |
C13—C14—C15 | 102.7 (3) | C46—C45—H45 | 120.5 |
C13—C14—H14A | 111.2 | C52—C45—H45 | 120.5 |
C15—C14—H14A | 111.2 | C45—C46—C47 | 120.3 (2) |
C13—C14—H14B | 111.2 | C45—C46—H46 | 119.9 |
C15—C14—H14B | 111.2 | C47—C46—H46 | 119.9 |
H14A—C14—H14B | 109.1 | C48—C47—C46 | 121.3 (2) |
C16—C15—C14 | 102.8 (2) | C48—C47—H47 | 119.4 |
C16—C15—H15A | 111.2 | C46—C47—H47 | 119.4 |
C14—C15—H15A | 111.2 | C47—C48—C53 | 119.14 (19) |
C16—C15—H15B | 111.2 | C47—C48—H48 | 120.4 |
C14—C15—H15B | 111.2 | C53—C48—H48 | 120.4 |
H15A—C15—H15B | 109.1 | C38—C49—C53 | 124.13 (17) |
O7—C16—C15 | 105.3 (2) | C38—C49—C50 | 129.77 (18) |
O7—C16—H16A | 110.7 | C53—C49—C50 | 106.08 (15) |
C15—C16—H16A | 110.7 | C41—C50—C51 | 118.51 (17) |
O7—C16—H16B | 110.7 | C41—C50—C49 | 133.20 (17) |
C15—C16—H16B | 110.7 | C51—C50—C49 | 108.18 (17) |
H16A—C16—H16B | 108.8 | C44—C51—C50 | 120.9 (2) |
O8—C17—C18 | 106.2 (2) | C44—C51—C52 | 130.50 (19) |
O8—C17—H17A | 110.5 | C50—C51—C52 | 108.56 (16) |
C18—C17—H17A | 110.5 | C45—C52—C53 | 121.1 (2) |
O8—C17—H17B | 110.5 | C45—C52—C51 | 130.64 (19) |
C18—C17—H17B | 110.5 | C53—C52—C51 | 108.27 (17) |
H17A—C17—H17B | 108.7 | C48—C53—C52 | 119.12 (18) |
C17—C18—C19 | 104.1 (2) | C48—C53—C49 | 131.99 (17) |
C17—C18—H18A | 110.9 | C52—C53—C49 | 108.81 (17) |
C19—C18—H18A | 110.9 | C62—C61—C70 | 119.77 (17) |
C17—C18—H18B | 110.9 | C62—C61—H61 | 120.1 |
C19—C18—H18B | 110.9 | C70—C61—H61 | 120.1 |
H18A—C18—H18B | 109.0 | C61—C62—C63 | 121.54 (18) |
C18—C19—C20 | 103.9 (2) | C61—C62—H62 | 119.2 |
C18—C19—H19A | 111.0 | C63—C62—H62 | 119.2 |
C20—C19—H19A | 111.0 | C64—C63—C62 | 119.87 (18) |
C18—C19—H19B | 111.0 | C64—C63—H63 | 120.1 |
C20—C19—H19B | 111.0 | C62—C63—H63 | 120.1 |
H19A—C19—H19B | 109.0 | C63—C64—C71 | 119.31 (17) |
O8—C20—C19 | 105.66 (19) | C63—C64—H64 | 120.3 |
O8—C20—H20A | 110.6 | C71—C64—H64 | 120.3 |
C19—C20—H20A | 110.6 | C66—C65—C72 | 118.80 (18) |
O8—C20—H20B | 110.6 | C66—C65—H65 | 120.6 |
C19—C20—H20B | 110.6 | C72—C65—H65 | 120.6 |
H20A—C20—H20B | 108.7 | C65—C66—C67 | 120.44 (18) |
O36—Dy—O31 | 84.77 (5) | C65—C66—H66 | 119.8 |
O36—Dy—C30 | 92.15 (7) | C67—C66—H66 | 119.8 |
O31—Dy—C30 | 82.00 (7) | C66—C67—C68 | 121.24 (19) |
O36—Dy—C29 | 122.30 (7) | C66—C67—H67 | 119.4 |
O31—Dy—C29 | 82.68 (7) | C68—C67—H67 | 119.4 |
C30—Dy—C29 | 30.36 (7) | C73—C68—C67 | 119.14 (18) |
O36—Dy—C22 | 110.75 (7) | C73—C68—H68 | 120.4 |
O31—Dy—C22 | 139.57 (7) | C67—C68—H68 | 120.4 |
C30—Dy—C22 | 131.84 (8) | C37—C69—C73 | 126.39 (16) |
C29—Dy—C22 | 114.91 (8) | C37—C69—C70 | 127.37 (16) |
O36—Dy—C23 | 134.82 (6) | C73—C69—C70 | 106.16 (15) |
O31—Dy—C23 | 114.59 (7) | C61—C70—C71 | 118.11 (16) |
C30—Dy—C23 | 129.23 (8) | C61—C70—C69 | 133.47 (16) |
C29—Dy—C23 | 101.20 (8) | C71—C70—C69 | 108.42 (15) |
C22—Dy—C23 | 29.97 (7) | C64—C71—C70 | 121.39 (17) |
O36—Dy—C26 | 83.65 (6) | C64—C71—C72 | 130.18 (17) |
O31—Dy—C26 | 110.14 (8) | C70—C71—C72 | 108.43 (15) |
C30—Dy—C26 | 30.38 (8) | C65—C72—C73 | 121.37 (17) |
C29—Dy—C26 | 49.84 (7) | C65—C72—C71 | 130.35 (18) |
C22—Dy—C26 | 108.58 (9) | C73—C72—C71 | 108.28 (15) |
C23—Dy—C26 | 121.53 (9) | C68—C73—C72 | 119.00 (16) |
O36—Dy—C24 | 119.37 (8) | C68—C73—C69 | 132.30 (17) |
O31—Dy—C24 | 89.86 (7) | C72—C73—C69 | 108.70 (15) |
O7—K—O1—C1 | 77.07 (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—Dy | 68.21 (16) |
O6—K—O1—C1 | 156.11 (17) | O36—Dy—C24—C23 | −129.87 (15) |
O5—K—O1—C1 | 171.75 (15) | O31—Dy—C24—C23 | 146.21 (15) |
O2—K—O1—C1 | −8.15 (15) | C30—Dy—C24—C23 | 71.1 (2) |
C13—K—O1—C1 | 70.59 (16) | C29—Dy—C24—C23 | 64.49 (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—C23 | 10.4 (3) |
O8—K—O1—C12 | 120.77 (15) | C21—Dy—C24—C23 | −76.13 (16) |
O6—K—O1—C12 | 18.30 (14) | C25—Dy—C24—C23 | −113.1 (2) |
O5—K—O1—C12 | 33.94 (16) | C28—Dy—C24—C23 | 34.96 (17) |
O2—K—O1—C12 | −145.96 (16) | C27—Dy—C24—C23 | 7.26 (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—C2 | 142.16 (16) | C30—Dy—C24—C25 | −175.76 (16) |
O4—K—O2—C2 | 152.56 (14) | C29—Dy—C24—C25 | 177.63 (16) |
O1—K—O2—C2 | −26.03 (14) | C22—Dy—C24—C25 | 76.52 (17) |
O8—K—O2—C2 | 52.77 (15) | C23—Dy—C24—C25 | 113.1 (2) |
O6—K—O2—C2 | −41.51 (16) | C26—Dy—C24—C25 | 123.6 (2) |
C13—K—O2—C2 | −111.67 (15) | C21—Dy—C24—C25 | 37.02 (16) |
O7—K—O2—C3 | 108.18 (17) | C28—Dy—C24—C25 | 148.10 (17) |
O3—K—O2—C3 | 18.80 (16) | C27—Dy—C24—C25 | 120.40 (18) |
O4—K—O2—C3 | 29.20 (18) | C22—C21—C25—C24 | 0.4 (3) |
O1—K—O2—C3 | −149.39 (18) | Dy—C21—C25—C24 | 68.06 (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—C3 | 124.97 (17) | Dy—C24—C25—C21 | −68.18 (16) |
O7—K—O3—C4 | −75.56 (16) | C23—C24—C25—Dy | 68.03 (16) |
O4—K—O3—C4 | −153.48 (17) | O36—Dy—C25—C21 | −81.04 (15) |
O1—K—O3—C4 | 28.00 (18) | O31—Dy—C25—C21 | −165.79 (15) |
O8—K—O3—C4 | 104.18 (16) | C29—Dy—C25—C21 | 109.6 (2) |
O5—K—O3—C4 | −163.98 (15) | C22—Dy—C25—C21 | 36.60 (14) |
O2—K—O3—C4 | 16.16 (15) | C23—Dy—C25—C21 | 76.20 (16) |
C13—K—O3—C4 | −52.60 (17) | C26—Dy—C25—C21 | −5.1 (3) |
O7—K—O3—C5 | 62.62 (17) | C24—Dy—C25—C21 | 113.5 (2) |
O4—K—O3—C5 | −15.30 (16) | C28—Dy—C25—C21 | 72.0 (2) |
O1—K—O3—C5 | 166.18 (16) | C27—Dy—C25—C21 | 32.0 (2) |
O8—K—O3—C5 | −117.64 (17) | O36—Dy—C25—C24 | 165.48 (16) |
O5—K—O3—C5 | −25.80 (18) | O31—Dy—C25—C24 | 80.72 (16) |
O2—K—O3—C5 | 154.34 (18) | C29—Dy—C25—C24 | −3.9 (3) |
C13—K—O3—C5 | 85.58 (17) | C22—Dy—C25—C24 | −76.89 (16) |
O7—K—O4—C7 | 111.16 (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—C7 | 31.30 (16) | C28—Dy—C25—C24 | −41.5 (2) |
O5—K—O4—C7 | 17.09 (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—C7 | 117.53 (15) | O31—Dy—C26—C30 | −23.29 (16) |
O7—K—O4—C6 | −115.64 (16) | C29—Dy—C26—C30 | 37.55 (14) |
O3—K—O4—C6 | −19.38 (15) | C22—Dy—C26—C30 | 144.87 (15) |
O8—K—O4—C6 | 62.86 (16) | C23—Dy—C26—C30 | 114.86 (16) |
O6—K—O4—C6 | 164.50 (14) | C24—Dy—C26—C30 | 108.7 (2) |
O5—K—O4—C6 | 150.28 (16) | C21—Dy—C26—C30 | 174.18 (14) |
O2—K—O4—C6 | −29.79 (17) | C25—Dy—C26—C30 | 177.21 (16) |
C13—K—O4—C6 | −109.28 (16) | C28—Dy—C26—C30 | 77.04 (16) |
O7—K—O5—C8 | −59.85 (15) | C27—Dy—C26—C30 | 114.1 (2) |
O3—K—O5—C8 | 29.57 (16) | O36—Dy—C26—C27 | 140.54 (17) |
O4—K—O5—C8 | 19.14 (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—C8 | 118.94 (15) | C29—Dy—C26—C27 | −76.58 (17) |
O6—K—O5—C8 | −146.72 (16) | C22—Dy—C26—C27 | 30.74 (18) |
C13—K—O5—C8 | −76.93 (15) | C23—Dy—C26—C27 | 0.73 (19) |
O7—K—O5—C9 | 65.65 (14) | C24—Dy—C26—C27 | −5.4 (3) |
O3—K—O5—C9 | 155.07 (13) | C21—Dy—C26—C27 | 60.05 (18) |
O4—K—O5—C9 | 144.64 (14) | C25—Dy—C26—C27 | 63.1 (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—C28 | 0.5 (3) |
O6—K—O5—C9 | −21.22 (13) | Dy—C26—C27—C28 | 67.89 (17) |
C13—K—O5—C9 | 48.57 (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—C10 | 150.39 (15) | C30—Dy—C27—C28 | −76.59 (18) |
O8—K—O6—C10 | 76.23 (14) | C29—Dy—C27—C28 | −36.57 (16) |
O5—K—O6—C10 | −13.83 (13) | C22—Dy—C27—C28 | 95.71 (18) |
O2—K—O6—C10 | 165.96 (13) | C23—Dy—C27—C28 | 67.06 (17) |
C13—K—O6—C10 | −127.10 (14) | C26—Dy—C27—C28 | −113.6 (2) |
O7—K—O6—C11 | 121.56 (15) | C24—Dy—C27—C28 | 63.41 (19) |
O4—K—O6—C11 | −162.47 (14) | C21—Dy—C27—C28 | 115.23 (17) |
O1—K—O6—C11 | 16.02 (14) | C25—Dy—C27—C28 | 99.26 (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—C26 | 56.29 (19) |
O2—K—O6—C11 | 31.59 (16) | C30—Dy—C27—C26 | 36.98 (15) |
C13—K—O6—C11 | 98.53 (15) | C29—Dy—C27—C26 | 77.00 (17) |
O3—K—O7—C16 | −29.6 (2) | C22—Dy—C27—C26 | −150.73 (17) |
O4—K—O7—C16 | 30.2 (2) | C23—Dy—C27—C26 | −179.37 (16) |
O1—K—O7—C16 | −150.2 (2) | C24—Dy—C27—C26 | 176.98 (15) |
O6—K—O7—C16 | 151.5 (2) | C21—Dy—C27—C26 | −131.21 (16) |
O5—K—O7—C16 | 90.9 (2) | C25—Dy—C27—C26 | −147.18 (16) |
O2—K—O7—C16 | −90.1 (2) | C28—Dy—C27—C26 | 113.6 (2) |
C13—K—O7—C16 | −134.1 (3) | C26—C27—C28—C29 | −0.2 (3) |
O3—K—O7—C13 | 104.55 (17) | Dy—C27—C28—C29 | 67.34 (16) |
O4—K—O7—C13 | 164.33 (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—C29 | 22.40 (16) |
O5—K—O7—C13 | −134.93 (17) | C30—Dy—C28—C29 | −36.98 (14) |
O2—K—O7—C13 | 44.08 (17) | C22—Dy—C28—C29 | 164.54 (15) |
O3—K—O8—C17 | 73.3 (2) | C23—Dy—C28—C29 | 135.00 (16) |
O4—K—O8—C17 | 13.8 (2) | C26—Dy—C28—C29 | −77.08 (17) |
O1—K—O8—C17 | −165.8 (2) | C24—Dy—C28—C29 | 117.97 (15) |
O6—K—O8—C17 | −107.8 (2) | C21—Dy—C28—C29 | 170.18 (14) |
O5—K—O8—C17 | −47.1 (2) | C25—Dy—C28—C29 | 138.25 (16) |
O2—K—O8—C17 | 133.8 (2) | C27—Dy—C28—C29 | −114.3 (2) |
C13—K—O8—C17 | 174.3 (2) | O36—Dy—C28—C27 | 34.0 (2) |
O3—K—O8—C20 | −155.90 (17) | O31—Dy—C28—C27 | 136.68 (16) |
O4—K—O8—C20 | 144.59 (17) | C30—Dy—C28—C27 | 77.30 (18) |
O1—K—O8—C20 | −35.00 (17) | C29—Dy—C28—C27 | 114.3 (2) |
O6—K—O8—C20 | 22.98 (17) | C22—Dy—C28—C27 | −81.18 (18) |
O5—K—O8—C20 | 83.63 (17) | C23—Dy—C28—C27 | −110.72 (18) |
O2—K—O8—C20 | −95.37 (17) | C26—Dy—C28—C27 | 37.20 (17) |
C13—K—O8—C20 | −55.0 (3) | C24—Dy—C28—C27 | −127.76 (17) |
C12—O1—C1—C2 | 179.31 (19) | C21—Dy—C28—C27 | −75.54 (18) |
K—O1—C1—C2 | 39.7 (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—C1 | 58.0 (2) | Dy—C28—C29—C30 | 67.78 (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—C28 | 122.03 (14) |
K—O2—C3—C4 | −50.8 (3) | O31—Dy—C29—C28 | −158.92 (15) |
C5—O3—C4—C3 | 172.6 (2) | C30—Dy—C29—C28 | 114.4 (2) |
K—O3—C4—C3 | −48.2 (2) | C22—Dy—C29—C28 | −17.05 (17) |
O2—C3—C4—O3 | 67.0 (3) | C23—Dy—C29—C28 | −45.20 (16) |
C4—O3—C5—C6 | −174.27 (19) | C26—Dy—C29—C28 | 76.84 (17) |
K—O3—C5—C6 | 46.4 (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—C5 | 50.6 (2) | C25—Dy—C29—C28 | −70.6 (2) |
O3—C5—C6—O4 | −63.7 (2) | C27—Dy—C29—C28 | 36.89 (15) |
C6—O4—C7—C8 | 175.49 (18) | O36—Dy—C29—C30 | 7.62 (18) |
K—O4—C7—C8 | −50.3 (2) | O31—Dy—C29—C30 | 86.67 (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—O5 | 70.3 (2) | C26—Dy—C29—C30 | −37.58 (16) |
C8—O5—C9—C10 | 177.95 (19) | C24—Dy—C29—C30 | 172.81 (15) |
K—O5—C9—C10 | 53.6 (2) | C21—Dy—C29—C30 | −129.90 (18) |
C11—O6—C10—C9 | −177.89 (18) | C25—Dy—C29—C30 | 175.01 (16) |
K—O6—C10—C9 | 46.2 (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—C12 | 177.42 (17) | C28—C29—C30—C26 | 0.6 (3) |
K—O6—C11—C12 | −46.8 (2) | Dy—C29—C30—C26 | 69.45 (15) |
C1—O1—C12—C11 | 170.67 (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—O1 | 62.6 (2) | Dy—C26—C30—C29 | −69.18 (15) |
C16—O7—C13—C14 | 8.8 (3) | C27—C26—C30—Dy | 68.48 (17) |
K—O7—C13—C14 | −136.7 (2) | O36—Dy—C30—C29 | −173.56 (15) |
C16—O7—C13—K | 145.5 (2) | O31—Dy—C30—C29 | −89.15 (15) |
O3—K—C13—O7 | −76.72 (17) | C22—Dy—C30—C29 | 65.81 (19) |
O4—K—C13—O7 | −15.79 (18) | C23—Dy—C30—C29 | 26.2 (2) |
O1—K—C13—O7 | 163.98 (17) | C26—Dy—C30—C29 | 112.9 (2) |
O8—K—C13—O7 | −176.05 (15) | C24—Dy—C30—C29 | −11.7 (2) |
O6—K—C13—O7 | 103.04 (17) | C21—Dy—C30—C29 | 102.0 (2) |
O5—K—C13—O7 | 47.12 (17) | C28—Dy—C30—C29 | 36.39 (15) |
O2—K—C13—O7 | −133.90 (17) | C27—Dy—C30—C29 | 76.08 (17) |
O7—K—C13—C14 | 72.8 (3) | O36—Dy—C30—C26 | 73.57 (15) |
O3—K—C13—C14 | −3.9 (3) | O31—Dy—C30—C26 | 157.98 (15) |
O4—K—C13—C14 | 57.0 (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—C14 | 175.8 (3) | C24—Dy—C30—C26 | −124.62 (18) |
O5—K—C13—C14 | 119.9 (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—C15 | 13.6 (3) | C27—Dy—C30—C26 | −36.79 (15) |
K—C13—C14—C15 | −36.8 (4) | C36—C31—C32—C33 | 1.7 (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—C15 | 105.6 (2) | C32—C33—C34—C35 | −0.8 (3) |
C14—C15—C16—O7 | 35.8 (3) | C33—C34—C35—C36 | 1.8 (3) |
C20—O8—C17—C18 | −39.0 (3) | C34—C35—C36—C31 | −1.1 (3) |
K—O8—C17—C18 | 99.2 (2) | C34—C35—C36—C38 | −175.57 (18) |
O8—C17—C18—C19 | 24.5 (4) | C32—C31—C36—C35 | −0.6 (3) |
C17—C18—C19—C20 | −1.6 (3) | C37—C31—C36—C35 | 178.66 (16) |
C17—O8—C20—C19 | 37.8 (3) | C32—C31—C36—C38 | 173.66 (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—C69 | 130.86 (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—O31 | 87.7 (2) |
C22—Dy—O31—C37 | 102.26 (16) | C32—C31—C37—C69 | 83.3 (2) |
C23—Dy—O31—C37 | 123.52 (14) | C36—C31—C37—C69 | −96.0 (2) |
C26—Dy—O31—C37 | −95.19 (14) | Dy—O36—C38—C49 | 176.34 (14) |
C24—Dy—O31—C37 | 105.59 (15) | Dy—O36—C38—C36 | 1.1 (3) |
C21—Dy—O31—C37 | 67.07 (15) | C35—C36—C38—O36 | 126.44 (18) |
C25—Dy—O31—C37 | 75.64 (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—C49 | 137.18 (18) |
O31—Dy—O36—C38 | 48.1 (2) | C50—C41—C42—C43 | 0.9 (3) |
C30—Dy—O36—C38 | 129.9 (2) | C41—C42—C43—C44 | 0.6 (3) |
C29—Dy—O36—C38 | 126.0 (2) | C42—C43—C44—C51 | −0.9 (3) |
C22—Dy—O36—C38 | −93.4 (2) | C52—C45—C46—C47 | 0.2 (3) |
C23—Dy—O36—C38 | −71.8 (2) | C45—C46—C47—C48 | 0.0 (3) |
C26—Dy—O36—C38 | 159.1 (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—C53 | 166.44 (16) |
C25—Dy—O36—C38 | −47.2 (2) | O36—C38—C49—C50 | 173.43 (17) |
C28—Dy—O36—C38 | 161.6 (2) | C36—C38—C49—C50 | −11.8 (3) |
C27—Dy—O36—C38 | 178.6 (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—C22 | 131.50 (15) | C38—C49—C50—C41 | −7.8 (3) |
C30—Dy—C21—C22 | −61.9 (2) | C53—C49—C50—C41 | 173.65 (19) |
C29—Dy—C21—C22 | −2.8 (2) | C38—C49—C50—C51 | 176.21 (18) |
C23—Dy—C21—C22 | 36.91 (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—C22 | 76.90 (17) | C43—C44—C51—C52 | 176.7 (2) |
C25—Dy—C21—C22 | 114.3 (2) | C41—C50—C51—C44 | 1.8 (3) |
C28—Dy—C21—C22 | −11.33 (18) | C49—C50—C51—C44 | 178.47 (17) |
C27—Dy—C21—C22 | −41.58 (17) | C41—C50—C51—C52 | −175.86 (16) |
O36—Dy—C21—C25 | 97.79 (16) | C49—C50—C51—C52 | 0.8 (2) |
O31—Dy—C21—C25 | 17.20 (18) | C46—C45—C52—C53 | 0.0 (3) |
C30—Dy—C21—C25 | −176.22 (16) | C46—C45—C52—C51 | 179.1 (2) |
C29—Dy—C21—C25 | −117.14 (19) | C44—C51—C52—C45 | 4.6 (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—C25 | 177.26 (15) | C50—C51—C52—C53 | 1.1 (2) |
C24—Dy—C21—C25 | −37.39 (16) | C47—C48—C53—C52 | 0.7 (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—C49 | 176.67 (17) |
C25—C21—C22—Dy | 68.06 (16) | C51—C52—C53—C49 | −2.6 (2) |
O36—Dy—C22—C23 | 148.43 (15) | C38—C49—C53—C48 | 1.0 (3) |
O31—Dy—C22—C23 | 41.3 (2) | C50—C49—C53—C48 | 179.65 (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—C52 | 3.03 (19) |
C26—Dy—C22—C23 | −121.42 (16) | C70—C61—C62—C63 | 1.0 (3) |
C24—Dy—C22—C23 | 36.93 (16) | C61—C62—C63—C64 | −0.2 (3) |
C21—Dy—C22—C23 | 113.9 (2) | C62—C63—C64—C71 | −0.5 (3) |
C25—Dy—C22—C23 | 77.11 (18) | C72—C65—C66—C67 | −0.2 (3) |
C28—Dy—C22—C23 | −76.30 (17) | C65—C66—C67—C68 | 0.3 (3) |
C27—Dy—C22—C23 | −106.36 (17) | C66—C67—C68—C73 | −0.4 (3) |
O36—Dy—C22—C21 | 34.49 (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—C21 | 147.64 (16) | O31—C37—C69—C70 | −178.60 (17) |
C29—Dy—C22—C21 | 178.19 (15) | C31—C37—C69—C70 | 5.4 (3) |
C23—Dy—C22—C21 | −113.9 (2) | C62—C61—C70—C71 | −1.1 (3) |
C26—Dy—C22—C21 | 124.64 (16) | C62—C61—C70—C69 | 178.18 (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—C61 | 179.44 (19) |
C28—Dy—C22—C21 | 169.76 (17) | C37—C69—C70—C71 | 175.59 (17) |
C27—Dy—C22—C21 | 139.70 (17) | C73—C69—C70—C71 | −1.23 (19) |
C21—C22—C23—C24 | 0.5 (3) | C63—C64—C71—C70 | 0.4 (3) |
Dy—C22—C23—C24 | −68.50 (16) | C63—C64—C71—C72 | −179.41 (19) |
C21—C22—C23—Dy | 68.96 (16) | C61—C70—C71—C64 | 0.4 (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—C22 | 107.94 (17) | C69—C70—C71—C72 | 0.8 (2) |
C29—Dy—C23—C22 | 121.08 (16) | C66—C65—C72—C73 | 0.2 (3) |
C26—Dy—C23—C22 | 71.61 (17) | C66—C65—C72—C71 | 179.97 (19) |
C24—Dy—C23—C22 | −114.2 (2) | C64—C71—C72—C65 | 0.0 (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—C73 | 179.78 (19) |
C28—Dy—C23—C22 | 100.01 (17) | C70—C71—C72—C73 | −0.1 (2) |
C27—Dy—C23—C22 | 71.98 (17) | C67—C68—C73—C72 | 0.5 (3) |
O36—Dy—C23—C24 | 70.57 (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—C68 | 179.83 (16) |
C29—Dy—C23—C24 | −124.70 (16) | C65—C72—C73—C69 | 179.05 (17) |
C22—Dy—C23—C24 | 114.2 (2) | C71—C72—C73—C69 | −0.7 (2) |
C26—Dy—C23—C24 | −174.17 (15) | C37—C69—C73—C68 | 3.7 (3) |
C21—Dy—C23—C24 | 77.37 (18) | C70—C69—C73—C68 | −179.46 (19) |
C25—Dy—C23—C24 | 37.52 (16) | C37—C69—C73—C72 | −175.67 (17) |
C28—Dy—C23—C24 | −145.77 (17) | C70—C69—C73—C72 | 1.20 (19) |
C27—Dy—C23—C24 | −173.80 (16) |
Experimental details
Crystal data | |
Chemical formula | [K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)] |
Mr | 1200.80 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 12.0798 (2), 13.0513 (2), 19.3154 (3) |
α, β, γ (°) | 85.1700 (8), 73.1480 (7), 74.5617 (8) |
V (Å3) | 2809.20 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.46 |
Crystal size (mm) | 0.60 × 0.40 × 0.30 |
Data collection | |
Diffractometer | Siemens SMART CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1997) |
Tmin, Tmax | 0.455, 0.641 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 19240, 13639, 12598 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.686 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.067, 1.02 |
No. of reflections | 13639 |
No. of parameters | 691 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.31, −1.40 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.
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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.