Download citation
Download citation
link to html
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 η5-Cp ligands and the novel chelating ligand o-phenyl­enebis(fluorenylideneacyl­ate).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807035738/bi2211sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807035738/bi2211Isup2.hkl
Contains datablock I

CCDC reference: 658973

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](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

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).

Structure description 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.

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

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 m3
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 mm1
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)
Graphite monochromatorRint = 0.020
ω scansθmax = 29.2°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 1316
Tmin = 0.455, Tmax = 0.641k = 1717
19240 measured reflectionsl = 2623
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 Å3
0 restraintsΔρmin = 1.40 e Å3
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 mm1
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 reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.067H-atom parameters constrained
S = 1.02Δρmax = 1.31 e Å3
13639 reflectionsΔρmin = 1.40 e Å3
691 parameters
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)
H210.16790.15680.21120.061 (3)*
C220.1438 (2)0.13181 (17)0.10779 (14)0.0396 (5)
H220.21670.17190.07720.061 (3)*
C230.0467 (2)0.07224 (18)0.08566 (14)0.0392 (5)
H230.04140.06480.03730.061 (3)*
C240.0422 (2)0.02476 (19)0.14642 (18)0.0473 (6)
H240.11830.02060.14690.061 (3)*
C250.0021 (3)0.0567 (2)0.20691 (15)0.0505 (7)
H250.03870.03670.25570.061 (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)
H270.37430.03880.00340.061 (3)*
C280.2296 (2)0.0806 (2)0.01572 (12)0.0449 (6)
H280.19810.04730.04490.061 (3)*
C290.1866 (2)0.1847 (2)0.00774 (12)0.0407 (5)
H290.12060.23520.00280.061 (3)*
C300.2561 (2)0.2034 (2)0.04943 (12)0.0397 (5)
H300.24560.26810.07250.061 (3)*
C310.04811 (16)0.18802 (13)0.29644 (10)0.0201 (3)
C320.16929 (17)0.19355 (15)0.32745 (11)0.0257 (4)
H320.22690.23980.30690.038 (3)*
C330.20713 (19)0.13260 (17)0.38785 (12)0.0315 (4)
H330.29000.13800.40880.038 (3)*
C340.1237 (2)0.06409 (17)0.41735 (12)0.0321 (4)
H340.14900.02290.45900.038 (3)*
C350.00246 (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)
C370.01876 (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)
H460.71470.05330.25790.037 (2)*
C470.57487 (19)0.02271 (17)0.21366 (12)0.0337 (4)
H470.62180.04820.16690.037 (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)
C610.07294 (17)0.38101 (14)0.38571 (10)0.0225 (3)
H610.08290.31120.39700.032 (2)*
C620.08552 (18)0.44884 (16)0.44059 (11)0.0265 (4)
H620.10290.42420.48930.032 (2)*
C630.07322 (19)0.55228 (16)0.42597 (11)0.0275 (4)
H630.08240.59740.46450.032 (2)*
C640.04756 (18)0.58916 (15)0.35525 (11)0.0254 (4)
H640.03970.65980.34490.032 (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)*
C690.02338 (16)0.36481 (14)0.24407 (10)0.0202 (3)
C700.04538 (16)0.41586 (14)0.31351 (10)0.0198 (3)
C710.03333 (16)0.52160 (14)0.29937 (10)0.0213 (3)
C720.00544 (16)0.54005 (14)0.22144 (10)0.0216 (3)
C730.00025 (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, º) 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—C250.2 (3)
O3—K—O1—C120.00 (17)Dy—C23—C24—C2568.40 (16)
O8—K—O1—C1101.42 (16)C22—C23—C24—Dy68.21 (16)
O6—K—O1—C1156.11 (17)O36—Dy—C24—C23129.87 (15)
O5—K—O1—C1171.75 (15)O31—Dy—C24—C23146.21 (15)
O2—K—O1—C18.15 (15)C30—Dy—C24—C2371.1 (2)
C13—K—O1—C170.59 (16)C29—Dy—C24—C2364.49 (17)
O7—K—O1—C1260.74 (15)C22—Dy—C24—C2336.62 (14)
O3—K—O1—C12157.81 (14)C26—Dy—C24—C2310.4 (3)
O8—K—O1—C12120.77 (15)C21—Dy—C24—C2376.13 (16)
O6—K—O1—C1218.30 (14)C25—Dy—C24—C23113.1 (2)
O5—K—O1—C1233.94 (16)C28—Dy—C24—C2334.96 (17)
O2—K—O1—C12145.96 (16)C27—Dy—C24—C237.26 (19)
C13—K—O1—C1267.22 (15)O36—Dy—C24—C2516.72 (19)
O7—K—O2—C2128.46 (15)O31—Dy—C24—C25100.64 (16)
O3—K—O2—C2142.16 (16)C30—Dy—C24—C25175.76 (16)
O4—K—O2—C2152.56 (14)C29—Dy—C24—C25177.63 (16)
O1—K—O2—C226.03 (14)C22—Dy—C24—C2576.52 (17)
O8—K—O2—C252.77 (15)C23—Dy—C24—C25113.1 (2)
O6—K—O2—C241.51 (16)C26—Dy—C24—C25123.6 (2)
C13—K—O2—C2111.67 (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—C3149.39 (18)Dy—C21—C25—C2468.06 (16)
O8—K—O2—C370.59 (16)C22—C21—C25—Dy67.63 (17)
O6—K—O2—C3164.87 (16)C23—C24—C25—C210.1 (3)
C13—K—O2—C3124.97 (17)Dy—C24—C25—C2168.18 (16)
O7—K—O3—C475.56 (16)C23—C24—C25—Dy68.03 (16)
O4—K—O3—C4153.48 (17)O36—Dy—C25—C2181.04 (15)
O1—K—O3—C428.00 (18)O31—Dy—C25—C21165.79 (15)
O8—K—O3—C4104.18 (16)C29—Dy—C25—C21109.6 (2)
O5—K—O3—C4163.98 (15)C22—Dy—C25—C2136.60 (14)
O2—K—O3—C416.16 (15)C23—Dy—C25—C2176.20 (16)
C13—K—O3—C452.60 (17)C26—Dy—C25—C215.1 (3)
O7—K—O3—C562.62 (17)C24—Dy—C25—C21113.5 (2)
O4—K—O3—C515.30 (16)C28—Dy—C25—C2172.0 (2)
O1—K—O3—C5166.18 (16)C27—Dy—C25—C2132.0 (2)
O8—K—O3—C5117.64 (17)O36—Dy—C25—C24165.48 (16)
O5—K—O3—C525.80 (18)O31—Dy—C25—C2480.72 (16)
O2—K—O3—C5154.34 (18)C29—Dy—C25—C243.9 (3)
C13—K—O3—C585.58 (17)C22—Dy—C25—C2476.89 (16)
O7—K—O4—C7111.16 (15)C23—Dy—C25—C2437.28 (15)
O3—K—O4—C7152.57 (16)C26—Dy—C25—C24118.6 (2)
O8—K—O4—C770.34 (15)C21—Dy—C25—C24113.5 (2)
O6—K—O4—C731.30 (16)C28—Dy—C25—C2441.5 (2)
O5—K—O4—C717.09 (14)C27—Dy—C25—C2481.5 (2)
O2—K—O4—C7162.98 (14)O36—Dy—C26—C30105.33 (15)
C13—K—O4—C7117.53 (15)O31—Dy—C26—C3023.29 (16)
O7—K—O4—C6115.64 (16)C29—Dy—C26—C3037.55 (14)
O3—K—O4—C619.38 (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—C629.79 (17)C25—Dy—C26—C30177.21 (16)
C13—K—O4—C6109.28 (16)C28—Dy—C26—C3077.04 (16)
O7—K—O5—C859.85 (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—C27137.42 (16)
O1—K—O5—C8162.26 (14)C30—Dy—C26—C27114.1 (2)
O8—K—O5—C8118.94 (15)C29—Dy—C26—C2776.58 (17)
O6—K—O5—C8146.72 (16)C22—Dy—C26—C2730.74 (18)
C13—K—O5—C876.93 (15)C23—Dy—C26—C270.73 (19)
O7—K—O5—C965.65 (14)C24—Dy—C26—C275.4 (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—C936.76 (15)C28—Dy—C26—C2737.09 (16)
O8—K—O5—C9115.56 (14)C30—C26—C27—C280.5 (3)
O6—K—O5—C921.22 (13)Dy—C26—C27—C2867.89 (17)
C13—K—O5—C948.57 (14)C30—C26—C27—Dy67.36 (16)
O7—K—O6—C10104.07 (14)O36—Dy—C27—C28154.88 (16)
O4—K—O6—C1028.10 (15)O31—Dy—C27—C2857.3 (2)
O1—K—O6—C10150.39 (15)C30—Dy—C27—C2876.59 (18)
O8—K—O6—C1076.23 (14)C29—Dy—C27—C2836.57 (16)
O5—K—O6—C1013.83 (13)C22—Dy—C27—C2895.71 (18)
O2—K—O6—C10165.96 (13)C23—Dy—C27—C2867.06 (17)
C13—K—O6—C10127.10 (14)C26—Dy—C27—C28113.6 (2)
O7—K—O6—C11121.56 (15)C24—Dy—C27—C2863.41 (19)
O4—K—O6—C11162.47 (14)C21—Dy—C27—C28115.23 (17)
O1—K—O6—C1116.02 (14)C25—Dy—C27—C2899.26 (19)
O8—K—O6—C1158.14 (15)O36—Dy—C27—C2641.32 (17)
O5—K—O6—C11148.20 (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—C1629.6 (2)C22—Dy—C27—C26150.73 (17)
O4—K—O7—C1630.2 (2)C23—Dy—C27—C26179.37 (16)
O1—K—O7—C16150.2 (2)C24—Dy—C27—C26176.98 (15)
O6—K—O7—C16151.5 (2)C21—Dy—C27—C26131.21 (16)
O5—K—O7—C1690.9 (2)C25—Dy—C27—C26147.18 (16)
O2—K—O7—C1690.1 (2)C28—Dy—C27—C26113.6 (2)
C13—K—O7—C16134.1 (3)C26—C27—C28—C290.2 (3)
O3—K—O7—C13104.55 (17)Dy—C27—C28—C2967.34 (16)
O4—K—O7—C13164.33 (17)C26—C27—C28—Dy67.52 (17)
O1—K—O7—C1316.04 (17)O36—Dy—C28—C2980.32 (17)
O6—K—O7—C1374.35 (17)O31—Dy—C28—C2922.40 (16)
O5—K—O7—C13134.93 (17)C30—Dy—C28—C2936.98 (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—C2977.08 (17)
O1—K—O8—C17165.8 (2)C24—Dy—C28—C29117.97 (15)
O6—K—O8—C17107.8 (2)C21—Dy—C28—C29170.18 (14)
O5—K—O8—C1747.1 (2)C25—Dy—C28—C29138.25 (16)
O2—K—O8—C17133.8 (2)C27—Dy—C28—C29114.3 (2)
C13—K—O8—C17174.3 (2)O36—Dy—C28—C2734.0 (2)
O3—K—O8—C20155.90 (17)O31—Dy—C28—C27136.68 (16)
O4—K—O8—C20144.59 (17)C30—Dy—C28—C2777.30 (18)
O1—K—O8—C2035.00 (17)C29—Dy—C28—C27114.3 (2)
O6—K—O8—C2022.98 (17)C22—Dy—C28—C2781.18 (18)
O5—K—O8—C2083.63 (17)C23—Dy—C28—C27110.72 (18)
O2—K—O8—C2095.37 (17)C26—Dy—C28—C2737.20 (17)
C13—K—O8—C2055.0 (3)C24—Dy—C28—C27127.76 (17)
C12—O1—C1—C2179.31 (19)C21—Dy—C28—C2775.54 (18)
K—O1—C1—C239.7 (2)C25—Dy—C28—C27107.47 (19)
C3—O2—C2—C1178.8 (2)C27—C28—C29—C300.3 (3)
K—O2—C2—C158.0 (2)Dy—C28—C29—C3067.78 (15)
O1—C1—C2—O266.6 (3)C27—C28—C29—Dy68.03 (17)
C2—O2—C3—C4172.6 (2)O36—Dy—C29—C28122.03 (14)
K—O2—C3—C450.8 (3)O31—Dy—C29—C28158.92 (15)
C5—O3—C4—C3172.6 (2)C30—Dy—C29—C28114.4 (2)
K—O3—C4—C348.2 (2)C22—Dy—C29—C2817.05 (17)
O2—C3—C4—O367.0 (3)C23—Dy—C29—C2845.20 (16)
C4—O3—C5—C6174.27 (19)C26—Dy—C29—C2876.84 (17)
K—O3—C5—C646.4 (2)C24—Dy—C29—C2872.78 (16)
C7—O4—C6—C5175.28 (17)C21—Dy—C29—C2815.5 (2)
K—O4—C6—C550.6 (2)C25—Dy—C29—C2870.6 (2)
O3—C5—C6—O463.7 (2)C27—Dy—C29—C2836.89 (15)
C6—O4—C7—C8175.49 (18)O36—Dy—C29—C307.62 (18)
K—O4—C7—C850.3 (2)O31—Dy—C29—C3086.67 (16)
C9—O5—C8—C7177.39 (19)C22—Dy—C29—C30131.47 (16)
K—O5—C8—C752.6 (2)C23—Dy—C29—C30159.62 (16)
O4—C7—C8—O570.3 (2)C26—Dy—C29—C3037.58 (16)
C8—O5—C9—C10177.95 (19)C24—Dy—C29—C30172.81 (15)
K—O5—C9—C1053.6 (2)C21—Dy—C29—C30129.90 (18)
C11—O6—C10—C9177.89 (18)C25—Dy—C29—C30175.01 (16)
K—O6—C10—C946.2 (2)C28—Dy—C29—C30114.4 (2)
O5—C9—C10—O667.9 (2)C27—Dy—C29—C3077.53 (17)
C10—O6—C11—C12177.42 (17)C28—C29—C30—C260.6 (3)
K—O6—C11—C1246.8 (2)Dy—C29—C30—C2669.45 (15)
C1—O1—C12—C11170.67 (19)C28—C29—C30—Dy68.87 (16)
K—O1—C12—C1149.0 (2)C27—C26—C30—C290.7 (3)
O6—C11—C12—O162.6 (2)Dy—C26—C30—C2969.18 (15)
C16—O7—C13—C148.8 (3)C27—C26—C30—Dy68.48 (17)
K—O7—C13—C14136.7 (2)O36—Dy—C30—C29173.56 (15)
C16—O7—C13—K145.5 (2)O31—Dy—C30—C2989.15 (15)
O3—K—C13—O776.72 (17)C22—Dy—C30—C2965.81 (19)
O4—K—C13—O715.79 (18)C23—Dy—C30—C2926.2 (2)
O1—K—C13—O7163.98 (17)C26—Dy—C30—C29112.9 (2)
O8—K—C13—O7176.05 (15)C24—Dy—C30—C2911.7 (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—O7133.90 (17)C27—Dy—C30—C2976.08 (17)
O7—K—C13—C1472.8 (3)O36—Dy—C30—C2673.57 (15)
O3—K—C13—C143.9 (3)O31—Dy—C30—C26157.98 (15)
O4—K—C13—C1457.0 (3)C29—Dy—C30—C26112.9 (2)
O1—K—C13—C14123.2 (3)C22—Dy—C30—C2647.06 (19)
O8—K—C13—C14103.3 (3)C23—Dy—C30—C2686.70 (17)
O6—K—C13—C14175.8 (3)C24—Dy—C30—C26124.62 (18)
O5—K—C13—C14119.9 (3)C21—Dy—C30—C2610.8 (3)
O2—K—C13—C1461.1 (3)C28—Dy—C30—C2676.48 (17)
O7—C13—C14—C1513.6 (3)C27—Dy—C30—C2636.79 (15)
K—C13—C14—C1536.8 (4)C36—C31—C32—C331.7 (3)
C13—C14—C15—C1629.3 (3)C37—C31—C32—C33177.68 (17)
C13—O7—C16—C1528.1 (3)C31—C32—C33—C340.9 (3)
K—O7—C16—C15105.6 (2)C32—C33—C34—C350.8 (3)
C14—C15—C16—O735.8 (3)C33—C34—C35—C361.8 (3)
C20—O8—C17—C1839.0 (3)C34—C35—C36—C311.1 (3)
K—O8—C17—C1899.2 (2)C34—C35—C36—C38175.57 (18)
O8—C17—C18—C1924.5 (4)C32—C31—C36—C350.6 (3)
C17—C18—C19—C201.6 (3)C37—C31—C36—C35178.66 (16)
C17—O8—C20—C1937.8 (3)C32—C31—C36—C38173.66 (17)
K—O8—C20—C1998.0 (2)C37—C31—C36—C387.0 (3)
C18—C19—C20—O821.4 (3)Dy—O31—C37—C69130.86 (15)
O36—Dy—O31—C3713.93 (14)Dy—O31—C37—C3153.02 (19)
C30—Dy—O31—C37106.84 (15)C32—C31—C37—O3193.0 (2)
C29—Dy—O31—C37137.48 (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—C6996.0 (2)
C26—Dy—O31—C3795.19 (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—O3647.8 (2)
C28—Dy—O31—C37148.52 (14)C35—C36—C38—C4948.6 (3)
C27—Dy—O31—C37121.69 (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—C510.9 (3)
C22—Dy—O36—C3893.4 (2)C52—C45—C46—C470.2 (3)
C23—Dy—O36—C3871.8 (2)C45—C46—C47—C480.0 (3)
C26—Dy—O36—C38159.1 (2)C46—C47—C48—C530.4 (3)
C24—Dy—O36—C3838.8 (2)O36—C38—C49—C538.3 (3)
C21—Dy—O36—C3877.0 (2)C36—C38—C49—C53166.44 (16)
C25—Dy—O36—C3847.2 (2)O36—C38—C49—C50173.43 (17)
C28—Dy—O36—C38161.6 (2)C36—C38—C49—C5011.8 (3)
C27—Dy—O36—C38178.6 (2)C42—C41—C50—C512.0 (3)
O36—Dy—C21—C22147.92 (16)C42—C41—C50—C49177.68 (19)
O31—Dy—C21—C22131.50 (15)C38—C49—C50—C417.8 (3)
C30—Dy—C21—C2261.9 (2)C53—C49—C50—C41173.65 (19)
C29—Dy—C21—C222.8 (2)C38—C49—C50—C51176.21 (18)
C23—Dy—C21—C2236.91 (15)C53—C49—C50—C512.32 (19)
C26—Dy—C21—C2268.45 (17)C43—C44—C51—C500.4 (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—C2211.33 (18)C49—C50—C51—C44178.47 (17)
C27—Dy—C21—C2241.58 (17)C41—C50—C51—C52175.86 (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—C25176.22 (16)C46—C45—C52—C51179.1 (2)
C29—Dy—C21—C25117.14 (19)C44—C51—C52—C454.6 (3)
C22—Dy—C21—C25114.3 (2)C50—C51—C52—C45178.0 (2)
C23—Dy—C21—C2577.38 (17)C44—C51—C52—C53176.26 (19)
C26—Dy—C21—C25177.26 (15)C50—C51—C52—C531.1 (2)
C24—Dy—C21—C2537.39 (16)C47—C48—C53—C520.7 (3)
C28—Dy—C21—C25125.63 (16)C47—C48—C53—C49175.67 (19)
C27—Dy—C21—C25155.88 (16)C45—C52—C53—C480.5 (3)
C25—C21—C22—C230.5 (3)C51—C52—C53—C48179.71 (17)
Dy—C21—C22—C2368.61 (16)C45—C52—C53—C49176.67 (17)
C25—C21—C22—Dy68.06 (16)C51—C52—C53—C492.6 (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—C2398.43 (18)C38—C49—C53—C52175.60 (17)
C29—Dy—C22—C2367.87 (17)C50—C49—C53—C523.03 (19)
C26—Dy—C22—C23121.42 (16)C70—C61—C62—C631.0 (3)
C24—Dy—C22—C2336.93 (16)C61—C62—C63—C640.2 (3)
C21—Dy—C22—C23113.9 (2)C62—C63—C64—C710.5 (3)
C25—Dy—C22—C2377.11 (18)C72—C65—C66—C670.2 (3)
C28—Dy—C22—C2376.30 (17)C65—C66—C67—C680.3 (3)
C27—Dy—C22—C23106.36 (17)C66—C67—C68—C730.4 (3)
O36—Dy—C22—C2134.49 (17)O31—C37—C69—C732.4 (3)
O31—Dy—C22—C2172.63 (18)C31—C37—C69—C73178.34 (16)
C30—Dy—C22—C21147.64 (16)O31—C37—C69—C70178.60 (17)
C29—Dy—C22—C21178.19 (15)C31—C37—C69—C705.4 (3)
C23—Dy—C22—C21113.9 (2)C62—C61—C70—C711.1 (3)
C26—Dy—C22—C21124.64 (16)C62—C61—C70—C69178.18 (19)
C24—Dy—C22—C2177.01 (18)C37—C69—C70—C613.7 (3)
C25—Dy—C22—C2136.83 (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—C711.23 (19)
C21—C22—C23—C240.5 (3)C63—C64—C71—C700.4 (3)
Dy—C22—C23—C2468.50 (16)C63—C64—C71—C72179.41 (19)
C21—C22—C23—Dy68.96 (16)C61—C70—C71—C640.4 (3)
O36—Dy—C23—C2243.6 (2)C69—C70—C71—C64179.04 (17)
O31—Dy—C23—C22151.92 (15)C61—C70—C71—C72179.74 (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—C22114.2 (2)C64—C71—C72—C650.0 (3)
C21—Dy—C23—C2236.85 (16)C70—C71—C72—C65179.81 (19)
C25—Dy—C23—C2276.70 (18)C64—C71—C72—C73179.78 (19)
C28—Dy—C23—C22100.01 (17)C70—C71—C72—C730.1 (2)
C27—Dy—C23—C2271.98 (17)C67—C68—C73—C720.5 (3)
O36—Dy—C23—C2470.57 (18)C67—C68—C73—C69178.81 (19)
O31—Dy—C23—C2437.70 (17)C65—C72—C73—C680.4 (3)
C30—Dy—C23—C24137.84 (16)C71—C72—C73—C68179.83 (16)
C29—Dy—C23—C24124.70 (16)C65—C72—C73—C69179.05 (17)
C22—Dy—C23—C24114.2 (2)C71—C72—C73—C690.7 (2)
C26—Dy—C23—C24174.17 (15)C37—C69—C73—C683.7 (3)
C21—Dy—C23—C2477.37 (18)C70—C69—C73—C68179.46 (19)
C25—Dy—C23—C2437.52 (16)C37—C69—C73—C72175.67 (17)
C28—Dy—C23—C24145.77 (17)C70—C69—C73—C721.20 (19)
C27—Dy—C23—C24173.80 (16)

Experimental details

Crystal data
Chemical formula[K(C20H40O8)(C4H8O)2][Dy(C5H5)2(C34H20O2)]
Mr1200.80
Crystal system, space groupTriclinic, 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)
V3)2809.20 (8)
Z2
Radiation typeMo Kα
µ (mm1)1.46
Crystal size (mm)0.60 × 0.40 × 0.30
Data collection
DiffractometerSiemens SMART CCD
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1997)
Tmin, Tmax0.455, 0.641
No. of measured, independent and
observed [I > 2σ(I)] reflections
19240, 13639, 12598
Rint0.020
(sin θ/λ)max1)0.686
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.067, 1.02
No. of reflections13639
No. of parameters691
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.31, 1.40

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.

 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds