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The title compound, [Dy2(C8H7O2)6(C12H8N2)2], forms binuclear complexes, viz. di-μ-4-methyl­benzoato-κ4O:O′-bis[bis(4-methyl­benzoato-κ2O,O′)(1,10-phenanthroline-κ2N,N′)dyspros­ium(III)] tetra-μ-4-methyl­benzoato-κ8O:O′-bis[(4-methyl­benzoato-κ2O,O′)(1,10-phenanthroline-κ2N,N′)dyspros­ium(III)]. There are two independent binuclear com­plexes in the asymmetric unit, both of which are centrosymmetric. In one, the DyIII ions are linked by two bridging 4-­methyl­benzoate groups, while in the other, the DyIII ions are linked by four bridging 4-methyl­benzoate groups. The remaining 4-methyl­benzoate groups and 1,10-phenanthroline units coordinate to just one metal ion in bidentate modes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104032585/gd1354sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104032585/gd1354Isup2.hkl
Contains datablock I

CCDC reference: 241324

Comment top

Lanthanide carboxylate complexes containing 1,10-phenanthroline (phen) or 2,2'-bipyridine (2,2'-bipy) have been widely studied. Complexes of this type display a variety of structural types, with high stability and intense fluorescence. We have synthesized the title novel complex, [Dy(4—CH3C6H4COO)3.phen]2, (I), using 4-methylbenzoic acid and 1,10-phenanthroline (phen) as ligands with dysprosium(III) via a conventional solution reaction method. Two kinds of constitution exist in the complex. Here, we report the crystal structure of (I).

The structure of (I) contains two independent centrosymmtric dimers (Fig. 1), unlike lanthanide complexes of 4-methylbenzoic acid, such as the one-dimensional polymer Eu(4—CH3C6H4COO)3 (Jin et al., 2001), but similar to the binuclear complex Sm2(C8H7O2)6·(C10H8N2)2 (C10H8N2 is 2,2'-bipyridine; Li & Zou, 2003).

Each Dy1 ion is coordinated by two O atoms from two bridging 4-methylbenzoate groups, four O atoms from two chelating 4-methylbenzoate groups and two N atoms from one 1,10-phenanthroline (Fig. 1a), and each Dy2 ion is coordinated by four O atoms from four bridging 4-methylbenzoate groups, two O atoms from one chelating 4-methylbenzoate group and two N atoms from one 1,10-phenanthroline (Fig. 1b). The coordination number of each type of Dy ion is 8, but their coordination environments are different. The coordinated polyhedron of Dy1 is an irregular dodecahedron (Fig. 2a), while that of Dy2 is a square antiprism (Fig. 2 b).

Two carboxylate groups rarely link to the same central ion in chelating coordination mode. The complex containing Dy2, however, is typical of lanthanide carboxylate complexes. For example, Sm2(C8H7O2)6·(C10H8N2)2, [Eu(3—CH3C6H4COO)3.phen](H2O) (Jin et al., 1993) and Eu2(3,4-DMBA)6.(phen)2 (3,4-DMBA is 3,4-dimethylbenzoate; Wang et al., 1999) are of this type.

The Dy1—O distances in (I) range from 2.256 (5) to 2.433 (5) Å, with an average of 2.278 (5) Å. The Dy1—N distances are 2.529 (6) and 2.547 (6) Å, and the distance between two Dy ions is 5.305%A. The Dy2—O distances range from 2.276 (5) to 2.471 (5) Å, with an average of 2.3555 Å. The Dy2—N distances are 2.576 (6) and 2.579 (6) Å, and the distance between the two Dy ions is 4.200 Å.

The Dy—O or Dy—N distances involving Dy1 and Dy2 differ only slightly between the two metal sites, but the Dy—Dy distances are significantly different. The Dy1—Dy1 distance is longer than Dy2—Dy2 because of the different numbers of bridging ligands. The molecular structure and coordination environment of the title complex are quite similar to that observed for the dimer Eu(4—CH3C6H4COO)3.phen (Jin et al., 1994).

Experimental top

4-Methylbenzoic acid (1.5 mmol, 204 mg) was dissolved in ethanol (20 ml) and the pH of the solution was adjusted to be in the range 5–6 using 2M NaOH. Ethanol solutions of 1,10-phenanthroline (0.5 mmol, 90 mg) and DyCl3·6H2O (0.5 mmol, 189 mg) were successively added. The mixture was heated under reflux with stirring for 2 h and then kept at ambient temperature for 6 d. Crystals of (I) were obtained and used for IR and X-ray diffraction analyses. Analysis calculated: C 57.8, N 3.7, H 3.9%; found: C 58.0, N 3.6, H 3.9%.

Refinement top

All H atoms were initially located in a difference Fourier map. The methyl H atoms were then constrained to an ideal geometry, with C—H distances of 0.97 Å 0.96 Å in CIF? and Uiso(H) = 1.5Ueq(C), but each group was allowed to rotate freely about its C—C bond. All other H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C—H distances in the range 0.93–?? Å and Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); 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. Views of the title complex. Displacement ellipsoids are drawn at the 30% probability level and H atoms have been omitted for clarity. [Symmetry codes: (A) 1 − x, 1 − y, 1 − z; (B) 1 − x, 1 − y, −z.]
[Figure 2] Fig. 2. Schematic representations of the coordination geometry of the two independent Dy ions in (I) [symmetry codes: (A) 1 − x, 1 − y, 1 − z); (B) 1 − x, 1 − y, −z].
di-µ-4-methylbenzoato-κ4O:O'-bis[bis(4-methylbenzoato- κ2O,O')(1,10-phenanthroline-κ2N,N')dysprosium(III)] tetra-µ-4-methylbenzoato-κ8O:O'-bis[(4-methylbenzoato- κ2O,O')(1,10-phenanthroline-κ2N,N')dysprosium(III)] top
Crystal data top
[Dy2(C8H7O2)6(C12H8N2)2]Z = 2
Mr = 1496.22F(000) = 1492
Triclinic, P1Dx = 1.559 Mg m3
a = 12.760 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.346 (9) ÅCell parameters from 987 reflections
c = 19.758 (13) Åθ = 3.1–23.7°
α = 91.619 (12)°µ = 2.39 mm1
β = 97.925 (11)°T = 293 K
γ = 106.44 (1)°Prism, yellow
V = 3188 (4) Å30.22 × 0.18 × 0.12 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
11165 independent reflections
Radiation source: fine-focus sealed tube7695 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ϕ and ω scansθmax = 25.0°, θmin = 1.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1514
Tmin = 0.541, Tmax = 0.750k = 1315
16586 measured reflectionsl = 2023
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0549P)2 + 0.0276P]
where P = (Fo2 + 2Fc2)/3
11165 reflections(Δ/σ)max = 0.003
811 parametersΔρmax = 0.86 e Å3
18 restraintsΔρmin = 0.96 e Å3
Crystal data top
[Dy2(C8H7O2)6(C12H8N2)2]γ = 106.44 (1)°
Mr = 1496.22V = 3188 (4) Å3
Triclinic, P1Z = 2
a = 12.760 (8) ÅMo Kα radiation
b = 13.346 (9) ŵ = 2.39 mm1
c = 19.758 (13) ÅT = 293 K
α = 91.619 (12)°0.22 × 0.18 × 0.12 mm
β = 97.925 (11)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
11165 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
7695 reflections with I > 2σ(I)
Tmin = 0.541, Tmax = 0.750Rint = 0.033
16586 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04318 restraints
wR(F2) = 0.121H-atom parameters constrained
S = 1.11Δρmax = 0.86 e Å3
11165 reflectionsΔρmin = 0.96 e Å3
811 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
Dy10.71642 (3)0.54410 (3)0.501141 (17)0.03106 (12)
Dy20.38941 (3)0.54073 (3)0.057315 (16)0.02815 (11)
O10.8536 (5)0.6978 (4)0.4823 (3)0.0578 (18)
O20.8443 (4)0.6669 (4)0.5892 (3)0.0496 (15)
O30.8172 (5)0.4305 (5)0.5402 (3)0.0532 (16)
O40.6976 (4)0.4510 (4)0.6049 (3)0.0411 (13)
O50.5737 (4)0.4021 (4)0.4615 (3)0.0471 (15)
O60.3962 (5)0.3712 (4)0.4604 (3)0.0486 (15)
O70.3537 (4)0.3629 (4)0.0258 (2)0.0312 (12)
O80.4491 (4)0.3264 (4)0.0537 (3)0.0437 (14)
O90.3156 (4)0.6863 (4)0.0381 (3)0.0401 (13)
O100.3911 (4)0.6790 (4)0.1436 (2)0.0383 (13)
O110.5110 (4)0.4881 (4)0.1375 (2)0.0359 (13)
O120.6053 (4)0.4573 (4)0.0573 (2)0.0369 (13)
N10.6412 (5)0.5955 (5)0.3863 (3)0.0323 (15)
N20.8044 (5)0.4993 (5)0.4006 (3)0.0351 (15)
N30.1812 (5)0.4600 (5)0.0148 (3)0.0320 (14)
N40.2708 (5)0.4507 (5)0.1463 (3)0.0359 (15)
C10.5529 (7)0.6309 (6)0.3770 (4)0.044 (2)
H1A0.51120.62790.41240.053*
C20.5209 (7)0.6721 (7)0.3164 (4)0.049 (2)
H2A0.45780.69460.31110.058*
C30.5824 (7)0.6790 (6)0.2653 (4)0.048 (2)
H3A0.56280.70830.22510.058*
C40.6766 (6)0.6420 (6)0.2727 (4)0.040 (2)
C50.7461 (8)0.6430 (7)0.2212 (4)0.057 (3)
H5A0.73380.67590.18130.069*
C60.8274 (7)0.5984 (8)0.2289 (4)0.060 (3)
H6A0.87090.60140.19450.072*
C70.8498 (6)0.5457 (7)0.2890 (4)0.046 (2)
C80.9287 (7)0.4914 (8)0.2959 (5)0.061 (3)
H8A0.97050.48860.26120.074*
C90.9431 (7)0.4432 (8)0.3536 (5)0.060 (3)
H9A0.99520.40620.35920.071*
C100.8803 (7)0.4485 (7)0.4048 (4)0.048 (2)
H10A0.89210.41440.44430.058*
C110.7873 (6)0.5477 (6)0.3426 (3)0.0324 (18)
C120.7013 (6)0.5969 (6)0.3348 (4)0.0320 (18)
C130.8858 (6)0.7240 (6)0.5460 (4)0.041 (2)
C140.9718 (7)0.8250 (6)0.5659 (4)0.045 (2)
C151.0428 (8)0.8727 (8)0.5205 (5)0.070 (3)
H15A1.03430.84130.47670.084*
C161.1247 (9)0.9651 (9)0.5394 (7)0.092 (4)
H16A1.17210.99550.50900.110*
C171.1356 (10)1.0120 (8)0.6045 (8)0.095 (5)
C181.0641 (10)0.9649 (8)0.6495 (6)0.085 (4)
H18A1.07120.99680.69300.102*
C190.9842 (8)0.8726 (7)0.6304 (5)0.062 (3)
H19A0.93770.84170.66110.074*
C201.2277 (11)1.1152 (10)0.6212 (7)0.130 (5)
H20A1.22901.14120.66720.194*
H20B1.21441.16560.58990.194*
H20C1.29751.10370.61700.194*
C210.7734 (7)0.4141 (7)0.5937 (4)0.041 (2)
C220.8140 (7)0.3464 (7)0.6433 (4)0.044 (2)
C230.7888 (7)0.3412 (7)0.7093 (4)0.046 (2)
H23A0.74410.37980.72290.055*
C240.8285 (8)0.2802 (8)0.7551 (4)0.057 (3)
H24A0.81070.27930.79920.069*
C250.8927 (9)0.2214 (8)0.7379 (5)0.066 (3)
C260.9180 (9)0.2251 (8)0.6724 (5)0.075 (3)
H26A0.96110.18450.65910.090*
C270.8806 (8)0.2883 (8)0.6255 (5)0.066 (3)
H27A0.90080.29100.58200.080*
C280.9302 (11)0.1478 (10)0.7872 (6)0.106 (4)
H28A0.90490.15470.83020.159*
H28B1.00940.16560.79440.159*
H28C0.89970.07690.76810.159*
C290.4787 (6)0.3427 (6)0.4532 (3)0.0300 (17)
C300.4641 (6)0.2290 (5)0.4342 (3)0.0297 (17)
C310.5535 (7)0.1916 (6)0.4397 (4)0.048 (2)
H31A0.62430.23610.45420.057*
C320.5373 (10)0.0855 (8)0.4234 (5)0.070 (3)
H32A0.59830.05980.42800.084*
C330.4353 (12)0.0181 (7)0.4008 (5)0.074 (3)
C340.3485 (10)0.0575 (8)0.3947 (6)0.084 (4)
H34A0.27810.01320.37910.100*
C350.3613 (7)0.1623 (7)0.4111 (5)0.062 (3)
H35A0.29990.18740.40630.074*
C360.4197 (12)0.0962 (9)0.3833 (6)0.103 (4)
H36A0.49000.11010.39120.155*
H36B0.38790.11360.33610.155*
H36C0.37130.13770.41170.155*
C370.1376 (6)0.4589 (6)0.0504 (4)0.040 (2)
H37A0.18300.49330.08070.048*
C380.0274 (7)0.4088 (7)0.0754 (4)0.051 (2)
H38A0.00070.40850.12160.062*
C390.0401 (6)0.3609 (7)0.0322 (4)0.047 (2)
H39A0.11440.32820.04850.057*
C400.0010 (6)0.3598 (6)0.0374 (4)0.040 (2)
C410.0654 (7)0.3165 (7)0.0870 (5)0.057 (3)
H41A0.14100.28650.07370.068*
C420.0220 (7)0.3178 (7)0.1523 (5)0.053 (2)
H42A0.06870.29090.18380.064*
C430.0937 (7)0.3589 (6)0.1757 (4)0.044 (2)
C440.1441 (8)0.3569 (7)0.2425 (4)0.055 (2)
H44A0.10090.32720.27510.066*
C450.2534 (8)0.3966 (7)0.2609 (4)0.052 (2)
H45A0.28770.39310.30510.062*
C460.3124 (7)0.4431 (7)0.2110 (4)0.047 (2)
H46A0.38830.47180.22360.056*
C470.1600 (6)0.4074 (6)0.1290 (4)0.0336 (18)
C480.1148 (6)0.4097 (6)0.0584 (4)0.0313 (17)
C490.3662 (6)0.3070 (6)0.0229 (4)0.0294 (17)
C500.2742 (6)0.2086 (6)0.0483 (4)0.0324 (17)
C510.2854 (7)0.1372 (7)0.0961 (4)0.050 (2)
H51A0.35230.14690.11250.060*
C520.1949 (9)0.0488 (7)0.1202 (5)0.067 (3)
H52A0.20350.00010.15190.081*
C530.0965 (8)0.0337 (7)0.0983 (5)0.052 (2)
C540.0861 (7)0.1048 (6)0.0507 (5)0.052 (2)
H54A0.01850.09550.03540.063*
C550.1739 (6)0.1904 (6)0.0248 (4)0.0375 (19)
H55A0.16530.23640.00880.045*
C560.0010 (8)0.0601 (7)0.1268 (6)0.082 (4)
H56A0.02420.10060.15960.124*
H56B0.05910.03700.14870.124*
H56C0.02270.10260.09020.124*
C570.3539 (6)0.7291 (6)0.0987 (4)0.0341 (18)
C580.3514 (6)0.8395 (6)0.1140 (4)0.0350 (18)
C590.3059 (8)0.8935 (7)0.0658 (4)0.056 (2)
H59A0.27800.86220.02190.067*
C600.3010 (8)0.9938 (7)0.0813 (5)0.064 (3)
H60A0.26901.02840.04790.076*
C610.3429 (7)1.0426 (7)0.1455 (5)0.057 (3)
C620.3866 (8)0.9884 (7)0.1935 (5)0.059 (3)
H62A0.41341.01940.23760.071*
C630.3921 (7)0.8892 (7)0.1784 (4)0.052 (2)
H63A0.42380.85500.21210.062*
C640.3328 (10)1.1510 (7)0.1634 (6)0.084 (4)
H64A0.36511.17260.21020.127*
H64B0.25621.14860.15730.127*
H64C0.37081.20000.13400.127*
C650.5720 (6)0.4423 (6)0.1155 (4)0.0323 (18)
C660.6086 (5)0.3625 (6)0.1573 (4)0.0323 (18)
C670.6465 (7)0.2871 (7)0.1281 (5)0.054 (2)
H67A0.65160.28540.08160.065*
C680.6769 (8)0.2140 (8)0.1684 (6)0.073 (3)
H68A0.70230.16320.14850.088*
C690.6705 (8)0.2147 (9)0.2370 (6)0.073 (3)
C700.6307 (7)0.2876 (8)0.2649 (5)0.059 (3)
H70A0.62460.28770.31130.071*
C710.5991 (6)0.3611 (7)0.2268 (4)0.043 (2)
H71A0.57140.40990.24720.051*
C720.7088 (11)0.1354 (10)0.2794 (6)0.108 (4)
H72A0.70010.14660.32630.162*
H72B0.78530.14330.27680.162*
H72C0.66530.06600.26220.162*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.0323 (2)0.0303 (2)0.0294 (2)0.00754 (17)0.00397 (16)0.00138 (16)
Dy20.02508 (19)0.0355 (2)0.0242 (2)0.00896 (16)0.00428 (15)0.00333 (15)
O10.067 (4)0.046 (4)0.039 (3)0.016 (3)0.002 (3)0.002 (3)
O20.050 (3)0.046 (4)0.039 (3)0.005 (3)0.001 (3)0.008 (3)
O30.061 (4)0.075 (5)0.043 (4)0.042 (3)0.020 (3)0.024 (3)
O40.041 (3)0.046 (4)0.043 (3)0.017 (3)0.015 (3)0.010 (3)
O50.044 (3)0.032 (3)0.057 (4)0.000 (3)0.004 (3)0.004 (3)
O60.045 (3)0.048 (4)0.057 (4)0.022 (3)0.007 (3)0.012 (3)
O70.028 (3)0.029 (3)0.033 (3)0.005 (2)0.002 (2)0.000 (2)
O80.034 (3)0.047 (4)0.050 (3)0.008 (3)0.014 (3)0.001 (3)
O90.040 (3)0.046 (3)0.035 (3)0.017 (3)0.002 (2)0.001 (3)
O100.050 (3)0.043 (3)0.029 (3)0.024 (3)0.008 (2)0.005 (2)
O110.032 (3)0.052 (4)0.028 (3)0.019 (3)0.005 (2)0.006 (2)
O120.041 (3)0.044 (3)0.028 (3)0.013 (3)0.005 (2)0.010 (2)
N10.028 (3)0.033 (4)0.033 (4)0.005 (3)0.002 (3)0.001 (3)
N20.032 (3)0.043 (4)0.032 (4)0.017 (3)0.002 (3)0.001 (3)
N30.025 (3)0.043 (4)0.031 (3)0.014 (3)0.006 (3)0.002 (3)
N40.041 (4)0.037 (4)0.030 (4)0.010 (3)0.011 (3)0.002 (3)
C10.043 (5)0.045 (5)0.041 (5)0.009 (4)0.001 (4)0.000 (4)
C20.044 (5)0.047 (6)0.052 (6)0.015 (4)0.006 (4)0.004 (4)
C30.054 (5)0.039 (5)0.039 (5)0.008 (4)0.024 (4)0.003 (4)
C40.036 (4)0.041 (5)0.030 (4)0.003 (4)0.008 (4)0.002 (4)
C50.069 (6)0.064 (7)0.028 (5)0.005 (5)0.002 (4)0.013 (4)
C60.045 (5)0.101 (8)0.030 (5)0.011 (6)0.014 (4)0.011 (5)
C70.036 (5)0.062 (6)0.029 (4)0.000 (4)0.003 (4)0.007 (4)
C80.041 (5)0.103 (9)0.045 (6)0.029 (5)0.010 (4)0.006 (5)
C90.050 (6)0.080 (8)0.054 (6)0.032 (5)0.000 (5)0.006 (5)
C100.051 (5)0.066 (6)0.034 (5)0.029 (5)0.001 (4)0.002 (4)
C110.025 (4)0.043 (5)0.021 (4)0.001 (3)0.003 (3)0.004 (3)
C120.029 (4)0.027 (4)0.031 (4)0.002 (3)0.006 (3)0.001 (3)
C130.035 (4)0.039 (5)0.043 (5)0.011 (4)0.006 (4)0.007 (4)
C140.042 (5)0.041 (5)0.047 (5)0.013 (4)0.008 (4)0.001 (4)
C150.073 (7)0.053 (7)0.070 (7)0.005 (5)0.016 (6)0.009 (5)
C160.069 (7)0.053 (7)0.130 (11)0.021 (6)0.012 (7)0.025 (7)
C170.076 (8)0.029 (6)0.149 (13)0.002 (6)0.060 (8)0.005 (7)
C180.108 (9)0.043 (7)0.079 (8)0.009 (7)0.040 (7)0.014 (6)
C190.074 (7)0.043 (6)0.057 (6)0.011 (5)0.016 (5)0.011 (5)
C200.118 (8)0.093 (8)0.151 (9)0.006 (7)0.020 (7)0.008 (7)
C210.046 (5)0.045 (5)0.033 (5)0.014 (4)0.005 (4)0.008 (4)
C220.045 (5)0.051 (6)0.038 (5)0.014 (4)0.007 (4)0.009 (4)
C230.047 (5)0.053 (6)0.035 (5)0.009 (4)0.011 (4)0.009 (4)
C240.060 (6)0.074 (7)0.036 (5)0.013 (5)0.010 (4)0.021 (5)
C250.077 (7)0.072 (8)0.053 (6)0.029 (6)0.006 (5)0.032 (5)
C260.097 (8)0.084 (8)0.072 (7)0.069 (7)0.019 (6)0.016 (6)
C270.093 (8)0.091 (8)0.040 (5)0.060 (7)0.019 (5)0.026 (5)
C280.131 (11)0.112 (11)0.094 (9)0.067 (9)0.008 (8)0.049 (8)
C290.041 (5)0.026 (4)0.020 (4)0.009 (4)0.001 (3)0.001 (3)
C300.035 (4)0.026 (4)0.027 (4)0.006 (3)0.007 (3)0.001 (3)
C310.060 (6)0.036 (5)0.050 (5)0.021 (4)0.005 (4)0.004 (4)
C320.105 (9)0.052 (7)0.063 (7)0.039 (6)0.014 (6)0.002 (5)
C330.140 (11)0.030 (6)0.052 (6)0.019 (7)0.027 (7)0.006 (5)
C340.097 (9)0.037 (6)0.101 (9)0.012 (6)0.032 (7)0.023 (6)
C350.047 (5)0.046 (6)0.080 (7)0.002 (5)0.010 (5)0.022 (5)
C360.153 (9)0.062 (6)0.093 (7)0.027 (6)0.024 (7)0.009 (6)
C370.025 (4)0.054 (6)0.043 (5)0.014 (4)0.006 (4)0.004 (4)
C380.038 (5)0.074 (7)0.043 (5)0.023 (5)0.005 (4)0.007 (5)
C390.023 (4)0.053 (6)0.065 (6)0.012 (4)0.004 (4)0.006 (5)
C400.024 (4)0.048 (5)0.052 (5)0.013 (4)0.011 (4)0.002 (4)
C410.028 (4)0.057 (6)0.085 (7)0.004 (4)0.025 (5)0.003 (5)
C420.043 (5)0.052 (6)0.070 (7)0.010 (4)0.035 (5)0.006 (5)
C430.046 (5)0.037 (5)0.052 (6)0.008 (4)0.028 (4)0.001 (4)
C440.075 (7)0.055 (6)0.038 (5)0.015 (5)0.032 (5)0.001 (4)
C450.074 (7)0.056 (6)0.026 (4)0.018 (5)0.013 (4)0.004 (4)
C460.054 (5)0.051 (6)0.031 (5)0.009 (4)0.008 (4)0.002 (4)
C470.032 (4)0.038 (5)0.034 (4)0.013 (4)0.012 (3)0.002 (3)
C480.027 (4)0.034 (4)0.038 (4)0.013 (3)0.013 (3)0.000 (3)
C490.029 (4)0.025 (4)0.033 (4)0.008 (3)0.002 (3)0.009 (3)
C500.036 (4)0.027 (4)0.033 (4)0.007 (3)0.005 (3)0.001 (3)
C510.050 (5)0.045 (6)0.056 (6)0.015 (4)0.013 (4)0.002 (4)
C520.101 (9)0.036 (6)0.057 (6)0.017 (6)0.004 (6)0.012 (5)
C530.053 (6)0.032 (5)0.063 (6)0.004 (4)0.001 (5)0.010 (4)
C540.037 (5)0.033 (5)0.083 (7)0.004 (4)0.009 (5)0.011 (5)
C550.033 (4)0.027 (4)0.051 (5)0.005 (3)0.009 (4)0.003 (4)
C560.080 (7)0.036 (6)0.104 (9)0.007 (5)0.025 (6)0.000 (6)
C570.026 (4)0.044 (5)0.035 (4)0.010 (4)0.014 (3)0.006 (4)
C580.037 (4)0.027 (4)0.040 (5)0.007 (3)0.005 (4)0.000 (3)
C590.072 (6)0.050 (6)0.040 (5)0.019 (5)0.009 (5)0.002 (4)
C600.078 (7)0.035 (6)0.072 (7)0.016 (5)0.010 (6)0.014 (5)
C610.056 (6)0.032 (5)0.079 (7)0.009 (4)0.004 (5)0.007 (5)
C620.079 (7)0.042 (6)0.051 (6)0.016 (5)0.005 (5)0.011 (4)
C630.066 (6)0.052 (6)0.035 (5)0.018 (5)0.003 (4)0.006 (4)
C640.105 (9)0.034 (6)0.110 (9)0.019 (6)0.005 (7)0.003 (6)
C650.028 (4)0.042 (5)0.023 (4)0.005 (4)0.002 (3)0.003 (3)
C660.019 (4)0.040 (5)0.037 (4)0.003 (3)0.010 (3)0.014 (4)
C670.065 (6)0.063 (6)0.052 (6)0.033 (5)0.029 (5)0.021 (5)
C680.076 (7)0.082 (8)0.096 (8)0.057 (6)0.048 (6)0.049 (7)
C690.062 (6)0.094 (9)0.081 (8)0.038 (6)0.025 (6)0.065 (7)
C700.058 (6)0.077 (7)0.045 (6)0.026 (5)0.002 (5)0.027 (5)
C710.049 (5)0.050 (6)0.031 (4)0.018 (4)0.000 (4)0.011 (4)
C720.123 (8)0.113 (8)0.110 (8)0.060 (6)0.027 (6)0.062 (6)
Geometric parameters (Å, º) top
Dy1—O52.256 (5)C26—C271.396 (12)
Dy1—O6i2.257 (6)C26—H26A0.9300
Dy1—O32.332 (6)C27—H27A0.9300
Dy1—O12.367 (5)C28—H28A0.9600
Dy1—O42.431 (5)C28—H28B0.9600
Dy1—O22.433 (5)C28—H28C0.9600
Dy1—N12.529 (6)C29—C301.506 (10)
Dy1—N22.547 (6)C30—C311.361 (11)
Dy1—C212.722 (8)C30—C351.369 (10)
Dy1—C132.763 (8)C31—C321.393 (12)
Dy2—O12ii2.276 (5)C31—H31A0.9300
Dy2—O8ii2.318 (5)C32—C331.363 (15)
Dy2—O112.328 (5)C32—H32A0.9300
Dy2—O72.335 (5)C33—C341.347 (15)
Dy2—O92.405 (5)C33—C361.505 (14)
Dy2—O102.471 (5)C34—C351.384 (13)
Dy2—N32.576 (6)C34—H34A0.9300
Dy2—N42.579 (6)C35—H35A0.9300
Dy2—C572.798 (8)C36—H36A0.9600
O1—C131.276 (9)C36—H36B0.9600
O2—C131.234 (9)C36—H36C0.9600
O3—C211.259 (9)C37—C381.387 (10)
O4—C211.245 (9)C37—H37A0.9300
O5—C291.232 (8)C38—C391.341 (11)
O6—C291.240 (9)C38—H38A0.9300
O6—Dy1i2.257 (6)C39—C401.405 (11)
O7—C491.257 (8)C39—H39A0.9300
O8—C491.259 (8)C40—C481.412 (10)
O8—Dy2ii2.318 (5)C40—C411.414 (11)
O9—C571.281 (8)C41—C421.330 (12)
O10—C571.248 (8)C41—H41A0.9300
O11—C651.231 (9)C42—C431.427 (11)
O12—C651.281 (8)C42—H42A0.9300
O12—Dy2ii2.276 (5)C43—C471.387 (10)
N1—C11.333 (10)C43—C441.391 (12)
N1—C121.354 (9)C44—C451.337 (12)
N2—C101.326 (10)C44—H44A0.9300
N2—C111.354 (9)C45—C461.379 (11)
N3—C371.329 (9)C45—H45A0.9300
N3—C481.350 (9)C46—H46A0.9300
N4—C461.332 (9)C47—C481.439 (10)
N4—C471.357 (9)C49—C501.511 (9)
C1—C21.390 (11)C50—C511.372 (11)
C1—H1A0.9300C50—C551.381 (10)
C2—C31.352 (11)C51—C521.414 (12)
C2—H2A0.9300C51—H51A0.9300
C3—C41.414 (11)C52—C531.348 (13)
C3—H3A0.9300C52—H52A0.9300
C4—C121.417 (10)C53—C541.362 (12)
C4—C51.436 (12)C53—C561.509 (11)
C5—C61.330 (13)C54—C551.381 (10)
C5—H5A0.9300C54—H54A0.9300
C6—C71.431 (12)C55—H55A0.9300
C6—H6A0.9300C56—H56A0.9600
C7—C81.392 (12)C56—H56B0.9600
C7—C111.414 (10)C56—H56C0.9600
C8—C91.340 (12)C57—C581.505 (10)
C8—H8A0.9300C58—C591.374 (11)
C9—C101.387 (12)C58—C631.381 (10)
C9—H9A0.9300C59—C601.385 (12)
C10—H10A0.9300C59—H59A0.9300
C11—C121.424 (11)C60—C611.376 (12)
C13—C141.480 (11)C60—H60A0.9300
C14—C191.376 (12)C61—C621.362 (12)
C14—C151.401 (12)C61—C641.525 (12)
C15—C161.374 (13)C62—C631.371 (12)
C15—H15A0.9300C62—H62A0.9300
C16—C171.386 (17)C63—H63A0.9300
C16—H16A0.9300C64—H64A0.9600
C17—C181.397 (17)C64—H64B0.9600
C17—C201.529 (15)C64—H64C0.9600
C18—C191.362 (13)C65—C661.502 (10)
C18—H18A0.9300C66—C671.378 (11)
C19—H19A0.9300C66—C711.396 (10)
C20—H20A0.9600C67—C681.382 (12)
C20—H20B0.9600C67—H67A0.9300
C20—H20C0.9600C68—C691.368 (14)
C21—C221.491 (11)C68—H68A0.9300
C22—C271.374 (12)C69—C701.355 (14)
C22—C231.383 (10)C69—C721.514 (13)
C23—C241.374 (12)C70—C711.369 (11)
C23—H23A0.9300C70—H70A0.9300
C24—C251.351 (14)C71—H71A0.9300
C24—H24A0.9300C72—H72A0.9600
C25—C261.375 (13)C72—H72B0.9600
C25—C281.528 (13)C72—H72C0.9600
O5—Dy1—O6i92.3 (2)O4—C21—Dy163.3 (4)
O5—Dy1—O388.1 (2)O3—C21—Dy158.8 (4)
O6i—Dy1—O3139.1 (2)C22—C21—Dy1175.3 (6)
O5—Dy1—O1150.90 (19)C27—C22—C23117.3 (8)
O6i—Dy1—O195.3 (2)C27—C22—C21120.8 (8)
O3—Dy1—O1103.9 (2)C23—C22—C21121.8 (8)
O5—Dy1—O479.63 (19)C24—C23—C22121.4 (9)
O6i—Dy1—O485.2 (2)C24—C23—H23A119.3
O3—Dy1—O454.66 (18)C22—C23—H23A119.3
O1—Dy1—O4128.94 (18)C25—C24—C23121.9 (9)
O5—Dy1—O2155.07 (19)C25—C24—H24A119.1
O6i—Dy1—O278.9 (2)C23—C24—H24A119.1
O3—Dy1—O283.7 (2)C24—C25—C26117.6 (9)
O1—Dy1—O253.94 (18)C24—C25—C28121.9 (10)
O4—Dy1—O276.43 (18)C26—C25—C28120.5 (10)
O5—Dy1—N176.99 (19)C25—C26—C27121.5 (9)
O6i—Dy1—N182.7 (2)C25—C26—H26A119.2
O3—Dy1—N1136.7 (2)C27—C26—H26A119.2
O1—Dy1—N176.20 (19)C22—C27—C26120.3 (9)
O4—Dy1—N1153.11 (18)C22—C27—H27A119.8
O2—Dy1—N1124.11 (19)C26—C27—H27A119.8
O5—Dy1—N285.6 (2)C25—C28—H28A109.5
O6i—Dy1—N2147.3 (2)C25—C28—H28B109.5
O3—Dy1—N273.6 (2)H28A—C28—H28B109.5
O1—Dy1—N272.9 (2)C25—C28—H28C109.5
O4—Dy1—N2126.2 (2)H28A—C28—H28C109.5
O2—Dy1—N2114.3 (2)H28B—C28—H28C109.5
N1—Dy1—N265.0 (2)O5—C29—O6123.9 (7)
O5—Dy1—C2184.2 (2)O5—C29—C30117.1 (7)
O6i—Dy1—C21111.9 (2)O6—C29—C30119.1 (7)
O3—Dy1—C2127.5 (2)C31—C30—C35119.3 (8)
O1—Dy1—C21118.4 (2)C31—C30—C29120.1 (7)
O4—Dy1—C2127.2 (2)C35—C30—C29120.5 (7)
O2—Dy1—C2177.7 (2)C30—C31—C32118.9 (9)
N1—Dy1—C21156.7 (2)C30—C31—H31A120.6
N2—Dy1—C21100.4 (2)C32—C31—H31A120.6
O5—Dy1—C13177.2 (2)C33—C32—C31122.4 (10)
O6i—Dy1—C1386.0 (2)C33—C32—H32A118.8
O3—Dy1—C1394.7 (2)C31—C32—H32A118.8
O1—Dy1—C1327.4 (2)C34—C33—C32117.5 (10)
O4—Dy1—C13102.5 (2)C34—C33—C36121.1 (12)
O2—Dy1—C1326.5 (2)C32—C33—C36121.4 (12)
N1—Dy1—C13100.5 (2)C33—C34—C35121.8 (10)
N2—Dy1—C1394.6 (2)C33—C34—H34A119.1
C21—Dy1—C1398.6 (2)C35—C34—H34A119.1
O12ii—Dy2—O8ii78.43 (18)C30—C35—C34120.1 (10)
O12ii—Dy2—O11125.54 (18)C30—C35—H35A120.0
O8ii—Dy2—O1179.83 (19)C34—C35—H35A120.0
O12ii—Dy2—O778.31 (17)C33—C36—H36A109.5
O8ii—Dy2—O7127.43 (18)C33—C36—H36B109.5
O11—Dy2—O776.68 (17)H36A—C36—H36B109.5
O12ii—Dy2—O983.15 (18)C33—C36—H36C109.5
O8ii—Dy2—O979.76 (19)H36A—C36—H36C109.5
O11—Dy2—O9139.83 (18)H36B—C36—H36C109.5
O7—Dy2—O9141.94 (16)N3—C37—C38123.0 (8)
O12ii—Dy2—O10131.68 (18)N3—C37—H37A118.5
O8ii—Dy2—O1074.40 (18)C38—C37—H37A118.5
O11—Dy2—O1087.87 (18)C39—C38—C37119.5 (8)
O7—Dy2—O10148.95 (17)C39—C38—H38A120.3
O9—Dy2—O1053.35 (17)C37—C38—H38A120.3
O12ii—Dy2—N381.72 (18)C38—C39—C40120.2 (7)
O8ii—Dy2—N3148.82 (19)C38—C39—H39A119.9
O11—Dy2—N3131.34 (19)C40—C39—H39A119.9
O7—Dy2—N370.48 (18)C39—C40—C48117.0 (7)
O9—Dy2—N374.18 (18)C39—C40—C41123.9 (7)
O10—Dy2—N3102.34 (18)C48—C40—C41119.1 (8)
O12ii—Dy2—N4142.40 (18)C42—C41—C40121.3 (8)
O8ii—Dy2—N4139.13 (19)C42—C41—H41A119.3
O11—Dy2—N475.01 (19)C40—C41—H41A119.3
O7—Dy2—N477.03 (18)C41—C42—C43122.2 (8)
O9—Dy2—N499.51 (19)C41—C42—H42A118.9
O10—Dy2—N472.99 (19)C43—C42—H42A118.9
N3—Dy2—N463.47 (19)C47—C43—C44117.8 (8)
O12ii—Dy2—C57106.9 (2)C47—C43—C42117.6 (8)
O8ii—Dy2—C5772.5 (2)C44—C43—C42124.6 (8)
O11—Dy2—C57113.0 (2)C45—C44—C43121.5 (8)
O7—Dy2—C57159.96 (18)C45—C44—H44A119.3
O9—Dy2—C5727.20 (18)C43—C44—H44A119.3
O10—Dy2—C5726.47 (18)C44—C45—C46116.5 (8)
N3—Dy2—C5790.8 (2)C44—C45—H45A121.7
N4—Dy2—C5788.3 (2)C46—C45—H45A121.7
C13—O1—Dy193.8 (5)N4—C46—C45126.0 (8)
C13—O2—Dy191.8 (5)N4—C46—H46A117.0
C21—O3—Dy193.7 (5)C45—C46—H46A117.0
C21—O4—Dy189.5 (5)N4—C47—C43122.3 (7)
C29—O5—Dy1158.2 (5)N4—C47—C48116.5 (6)
C29—O6—Dy1i162.4 (5)C43—C47—C48121.1 (7)
C49—O7—Dy2138.1 (5)N3—C48—C40122.2 (7)
C49—O8—Dy2ii139.3 (5)N3—C48—C47119.5 (6)
C57—O9—Dy293.7 (4)C40—C48—C47118.3 (7)
C57—O10—Dy291.5 (4)O7—C49—O8125.6 (7)
C65—O11—Dy2117.2 (5)O7—C49—C50118.2 (6)
C65—O12—Dy2ii162.9 (4)O8—C49—C50116.3 (7)
C1—N1—C12119.5 (7)C51—C50—C55118.2 (7)
C1—N1—Dy1122.8 (5)C51—C50—C49122.1 (7)
C12—N1—Dy1117.3 (5)C55—C50—C49119.6 (7)
C10—N2—C11117.5 (7)C50—C51—C52119.7 (8)
C10—N2—Dy1124.8 (5)C50—C51—H51A120.2
C11—N2—Dy1116.5 (5)C52—C51—H51A120.2
C37—N3—C48118.1 (6)C53—C52—C51121.4 (9)
C37—N3—Dy2122.1 (5)C53—C52—H52A119.3
C48—N3—Dy2119.6 (4)C51—C52—H52A119.3
C46—N4—C47115.9 (7)C52—C53—C54118.5 (8)
C46—N4—Dy2123.3 (5)C52—C53—C56119.8 (9)
C47—N4—Dy2120.8 (5)C54—C53—C56121.7 (9)
N1—C1—C2122.4 (8)C53—C54—C55121.4 (8)
N1—C1—H1A118.8C53—C54—H54A119.3
C2—C1—H1A118.8C55—C54—H54A119.3
C3—C2—C1119.3 (8)C54—C55—C50120.8 (8)
C3—C2—H2A120.3C54—C55—H55A119.6
C1—C2—H2A120.3C50—C55—H55A119.6
C2—C3—C4120.3 (8)C53—C56—H56A109.5
C2—C3—H3A119.8C53—C56—H56B109.5
C4—C3—H3A119.8H56A—C56—H56B109.5
C3—C4—C12117.1 (8)C53—C56—H56C109.5
C3—C4—C5125.0 (8)H56A—C56—H56C109.5
C12—C4—C5117.9 (8)H56B—C56—H56C109.5
C6—C5—C4122.0 (8)O10—C57—O9120.0 (7)
C6—C5—H5A119.0O10—C57—C58121.6 (7)
C4—C5—H5A119.0O9—C57—C58118.5 (7)
C5—C6—C7121.6 (8)O10—C57—Dy262.0 (4)
C5—C6—H6A119.2O9—C57—Dy259.1 (4)
C7—C6—H6A119.2C58—C57—Dy2169.7 (5)
C8—C7—C11119.1 (8)C59—C58—C63117.3 (8)
C8—C7—C6122.6 (8)C59—C58—C57122.0 (7)
C11—C7—C6118.3 (8)C63—C58—C57120.7 (7)
C9—C8—C7118.6 (9)C58—C59—C60121.3 (8)
C9—C8—H8A120.7C58—C59—H59A119.3
C7—C8—H8A120.7C60—C59—H59A119.3
C8—C9—C10119.9 (9)C61—C60—C59120.6 (9)
C8—C9—H9A120.1C61—C60—H60A119.7
C10—C9—H9A120.1C59—C60—H60A119.7
N2—C10—C9123.8 (8)C62—C61—C60118.0 (9)
N2—C10—H10A118.1C62—C61—C64121.4 (9)
C9—C10—H10A118.1C60—C61—C64120.5 (9)
N2—C11—C7121.1 (7)C61—C62—C63121.7 (8)
N2—C11—C12118.8 (7)C61—C62—H62A119.2
C7—C11—C12120.1 (7)C63—C62—H62A119.2
N1—C12—C4121.2 (7)C62—C63—C58121.1 (8)
N1—C12—C11118.7 (6)C62—C63—H63A119.4
C4—C12—C11120.0 (7)C58—C63—H63A119.4
O2—C13—O1120.3 (7)C61—C64—H64A109.5
O2—C13—C14121.6 (7)C61—C64—H64B109.5
O1—C13—C14118.0 (7)H64A—C64—H64B109.5
O2—C13—Dy161.7 (4)C61—C64—H64C109.5
O1—C13—Dy158.7 (4)H64A—C64—H64C109.5
C14—C13—Dy1175.2 (6)H64B—C64—H64C109.5
C19—C14—C15119.0 (8)O11—C65—O12123.5 (7)
C19—C14—C13120.0 (8)O11—C65—C66119.5 (7)
C15—C14—C13121.0 (8)O12—C65—C66117.0 (7)
C16—C15—C14121.3 (10)C67—C66—C71118.7 (8)
C16—C15—H15A119.4C67—C66—C65121.8 (7)
C14—C15—H15A119.4C71—C66—C65119.4 (7)
C15—C16—C17118.9 (11)C66—C67—C68119.6 (9)
C15—C16—H16A120.6C66—C67—H67A120.2
C17—C16—H16A120.6C68—C67—H67A120.2
C16—C17—C18119.8 (10)C69—C68—C67121.5 (10)
C16—C17—C20115.7 (14)C69—C68—H68A119.2
C18—C17—C20124.5 (13)C67—C68—H68A119.2
C19—C18—C17120.7 (11)C70—C69—C68118.5 (9)
C19—C18—H18A119.6C70—C69—C72122.0 (10)
C17—C18—H18A119.6C68—C69—C72119.4 (11)
C18—C19—C14120.4 (10)C69—C70—C71121.9 (9)
C18—C19—H19A119.8C69—C70—H70A119.1
C14—C19—H19A119.8C71—C70—H70A119.1
C17—C20—H20A109.5C70—C71—C66119.7 (9)
C17—C20—H20B109.5C70—C71—H71A120.1
H20A—C20—H20B109.5C66—C71—H71A120.1
C17—C20—H20C109.5C69—C72—H72A109.5
H20A—C20—H20C109.5C69—C72—H72B109.5
H20B—C20—H20C109.5H72A—C72—H72B109.5
O4—C21—O3121.9 (8)C69—C72—H72C109.5
O4—C21—C22120.5 (7)H72A—C72—H72C109.5
O3—C21—C22117.5 (8)H72B—C72—H72C109.5
O5—Dy1—O1—C13175.2 (5)O4—Dy1—C13—C14146 (8)
O6i—Dy1—O1—C1370.6 (5)O2—Dy1—C13—C14134 (8)
O3—Dy1—O1—C1372.9 (5)N1—Dy1—C13—C1420 (8)
O4—Dy1—O1—C1317.4 (6)N2—Dy1—C13—C1486 (8)
O2—Dy1—O1—C131.5 (5)C21—Dy1—C13—C14173 (8)
N1—Dy1—O1—C13151.8 (5)O2—C13—C14—C1919.6 (13)
N2—Dy1—O1—C13140.6 (5)O1—C13—C14—C19159.1 (8)
C21—Dy1—O1—C1347.8 (6)Dy1—C13—C14—C19113 (7)
O5—Dy1—O2—C13174.6 (5)O2—C13—C14—C15159.3 (9)
O6i—Dy1—O2—C13103.5 (5)O1—C13—C14—C1522.0 (12)
O3—Dy1—O2—C13113.7 (5)Dy1—C13—C14—C1568 (8)
O1—Dy1—O2—C131.5 (5)C19—C14—C15—C160.7 (15)
O4—Dy1—O2—C13168.8 (5)C13—C14—C15—C16178.2 (10)
N1—Dy1—O2—C1330.3 (6)C14—C15—C16—C170.9 (18)
N2—Dy1—O2—C1344.9 (5)C15—C16—C17—C180.4 (18)
C21—Dy1—O2—C13140.9 (5)C15—C16—C17—C20179.2 (11)
O5—Dy1—O3—C2181.0 (5)C16—C17—C18—C190.5 (18)
O6i—Dy1—O3—C2110.4 (6)C20—C17—C18—C19180.0 (11)
O1—Dy1—O3—C21125.8 (5)C17—C18—C19—C140.7 (16)
O4—Dy1—O3—C212.4 (4)C15—C14—C19—C180.1 (14)
O2—Dy1—O3—C2175.4 (5)C13—C14—C19—C18179.1 (9)
N1—Dy1—O3—C21149.7 (5)Dy1—O4—C21—O34.3 (8)
N2—Dy1—O3—C21167.0 (5)Dy1—O4—C21—C22176.9 (7)
C13—Dy1—O3—C2199.6 (5)Dy1—O3—C21—O44.5 (8)
O5—Dy1—O4—C2197.5 (5)Dy1—O3—C21—C22176.7 (6)
O6i—Dy1—O4—C21169.3 (5)O5—Dy1—C21—O478.6 (5)
O3—Dy1—O4—C212.4 (4)O6i—Dy1—C21—O411.5 (5)
O1—Dy1—O4—C2176.3 (5)O3—Dy1—C21—O4175.8 (8)
O2—Dy1—O4—C2189.5 (5)O1—Dy1—C21—O4120.8 (4)
N1—Dy1—O4—C21127.4 (5)O2—Dy1—C21—O484.1 (5)
N2—Dy1—O4—C2120.8 (5)N1—Dy1—C21—O4114.5 (6)
C13—Dy1—O4—C2184.5 (5)N2—Dy1—C21—O4163.1 (4)
O6i—Dy1—O5—C2912.5 (14)C13—Dy1—C21—O4100.6 (5)
O3—Dy1—O5—C29126.5 (14)O5—Dy1—C21—O397.1 (5)
O1—Dy1—O5—C29117.8 (14)O6i—Dy1—C21—O3172.7 (4)
O4—Dy1—O5—C2972.1 (14)O1—Dy1—C21—O363.4 (5)
O2—Dy1—O5—C2955.8 (16)O4—Dy1—C21—O3175.8 (8)
N1—Dy1—O5—C2994.5 (14)O2—Dy1—C21—O3100.1 (5)
N2—Dy1—O5—C29159.8 (14)N1—Dy1—C21—O361.3 (8)
C21—Dy1—O5—C2999.2 (14)N2—Dy1—C21—O312.7 (5)
C13—Dy1—O5—C2966 (5)C13—Dy1—C21—O383.6 (5)
O12ii—Dy2—O7—C4919.3 (6)O5—Dy1—C21—C22136 (7)
O8ii—Dy2—O7—C4946.1 (7)O6i—Dy1—C21—C22134 (7)
O11—Dy2—O7—C49112.0 (7)O3—Dy1—C21—C2239 (7)
O9—Dy2—O7—C4981.8 (7)O1—Dy1—C21—C2225 (8)
O10—Dy2—O7—C49174.1 (6)O4—Dy1—C21—C22146 (8)
N3—Dy2—O7—C49104.5 (7)O2—Dy1—C21—C2262 (7)
N4—Dy2—O7—C49170.6 (7)N1—Dy1—C21—C22100 (7)
C57—Dy2—O7—C49126.6 (8)N2—Dy1—C21—C2251 (7)
O12ii—Dy2—O9—C57150.9 (4)C13—Dy1—C21—C2245 (7)
O8ii—Dy2—O9—C5771.5 (4)O4—C21—C22—C27166.6 (9)
O11—Dy2—O9—C5711.0 (5)O3—C21—C22—C2712.3 (12)
O7—Dy2—O9—C57148.1 (4)Dy1—C21—C22—C2749 (8)
O10—Dy2—O9—C576.6 (4)O4—C21—C22—C2314.9 (12)
N3—Dy2—O9—C57125.8 (4)O3—C21—C22—C23166.2 (8)
N4—Dy2—O9—C5767.0 (4)Dy1—C21—C22—C23129 (7)
O12ii—Dy2—O10—C5723.7 (5)C27—C22—C23—C240.1 (13)
O8ii—Dy2—O10—C5781.9 (4)C21—C22—C23—C24178.7 (8)
O11—Dy2—O10—C57162.0 (4)C22—C23—C24—C250.9 (14)
O7—Dy2—O10—C57138.6 (4)C23—C24—C25—C260.4 (15)
O9—Dy2—O10—C576.8 (4)C23—C24—C25—C28175.7 (10)
N3—Dy2—O10—C5766.1 (4)C24—C25—C26—C271.0 (17)
N4—Dy2—O10—C57123.1 (4)C28—C25—C26—C27177.2 (11)
O12ii—Dy2—O11—C6512.1 (6)C23—C22—C27—C261.5 (15)
O8ii—Dy2—O11—C6579.9 (5)C21—C22—C27—C26179.9 (9)
O7—Dy2—O11—C6552.7 (5)C25—C26—C27—C222.0 (17)
O9—Dy2—O11—C65140.4 (5)Dy1—O5—C29—O623.8 (19)
O10—Dy2—O11—C65154.4 (5)Dy1—O5—C29—C30155.3 (11)
N3—Dy2—O11—C65101.0 (5)Dy1i—O6—C29—O535 (2)
N4—Dy2—O11—C65132.6 (6)Dy1i—O6—C29—C30144.3 (15)
C57—Dy2—O11—C65145.8 (5)O5—C29—C30—C3112.7 (10)
O5—Dy1—N1—C180.5 (6)O6—C29—C30—C31166.4 (7)
O6i—Dy1—N1—C113.6 (6)O5—C29—C30—C35167.1 (8)
O3—Dy1—N1—C1153.4 (5)O6—C29—C30—C3513.7 (11)
O1—Dy1—N1—C1110.9 (6)C35—C30—C31—C321.7 (12)
O4—Dy1—N1—C150.3 (8)C29—C30—C31—C32178.5 (7)
O2—Dy1—N1—C184.9 (6)C30—C31—C32—C331.2 (14)
N2—Dy1—N1—C1171.7 (6)C31—C32—C33—C340.1 (16)
C21—Dy1—N1—C1117.2 (7)C31—C32—C33—C36179.9 (9)
C13—Dy1—N1—C198.1 (6)C32—C33—C34—C350.4 (17)
O5—Dy1—N1—C12106.6 (5)C36—C33—C34—C35179.5 (10)
O6i—Dy1—N1—C12159.3 (5)C31—C30—C35—C341.2 (14)
O3—Dy1—N1—C1233.7 (6)C29—C30—C35—C34179.0 (8)
O1—Dy1—N1—C1261.9 (5)C33—C34—C35—C300.1 (17)
O4—Dy1—N1—C12136.9 (5)C48—N3—C37—C380.2 (12)
O2—Dy1—N1—C1288.0 (5)Dy2—N3—C37—C38174.9 (6)
N2—Dy1—N1—C1215.4 (5)N3—C37—C38—C391.6 (14)
C21—Dy1—N1—C1269.9 (8)C37—C38—C39—C401.2 (13)
C13—Dy1—N1—C1274.8 (5)C38—C39—C40—C480.8 (12)
O5—Dy1—N2—C1099.1 (7)C38—C39—C40—C41176.2 (8)
O6i—Dy1—N2—C10173.4 (6)C39—C40—C41—C42179.9 (9)
O3—Dy1—N2—C109.8 (6)C48—C40—C41—C423.0 (14)
O1—Dy1—N2—C10100.8 (7)C40—C41—C42—C432.5 (15)
O4—Dy1—N2—C1025.4 (7)C41—C42—C43—C476.0 (14)
O2—Dy1—N2—C1065.3 (7)C41—C42—C43—C44176.2 (9)
N1—Dy1—N2—C10176.8 (7)C47—C43—C44—C452.5 (14)
C21—Dy1—N2—C1015.9 (7)C42—C43—C44—C45179.8 (9)
C13—Dy1—N2—C1083.7 (7)C43—C44—C45—C462.4 (14)
O5—Dy1—N2—C1193.7 (5)C47—N4—C46—C450.6 (13)
O6i—Dy1—N2—C116.2 (7)Dy2—N4—C46—C45179.6 (7)
O3—Dy1—N2—C11177.0 (5)C44—C45—C46—N40.9 (14)
O1—Dy1—N2—C1166.4 (5)C46—N4—C47—C430.5 (11)
O4—Dy1—N2—C11167.4 (4)Dy2—N4—C47—C43179.6 (6)
O2—Dy1—N2—C11101.9 (5)C46—N4—C47—C48176.5 (7)
N1—Dy1—N2—C1116.0 (5)Dy2—N4—C47—C483.3 (9)
C21—Dy1—N2—C11176.9 (5)C44—C43—C47—N40.9 (12)
C13—Dy1—N2—C1183.5 (5)C42—C43—C47—N4178.8 (7)
O12ii—Dy2—N3—C3710.7 (6)C44—C43—C47—C48177.9 (8)
O8ii—Dy2—N3—C3740.1 (8)C42—C43—C47—C484.2 (12)
O11—Dy2—N3—C37141.6 (6)C37—N3—C48—C402.3 (11)
O7—Dy2—N3—C3791.2 (6)Dy2—N3—C48—C40177.1 (6)
O9—Dy2—N3—C3774.5 (6)C37—N3—C48—C47178.6 (7)
O10—Dy2—N3—C37120.3 (6)Dy2—N3—C48—C473.8 (9)
N4—Dy2—N3—C37176.1 (7)C39—C40—C48—N32.6 (12)
C57—Dy2—N3—C3796.2 (6)C41—C40—C48—N3174.6 (7)
O12ii—Dy2—N3—C48163.9 (6)C39—C40—C48—C47178.3 (7)
O8ii—Dy2—N3—C48145.3 (5)C41—C40—C48—C474.5 (11)
O11—Dy2—N3—C4833.0 (6)N4—C47—C48—N34.6 (11)
O7—Dy2—N3—C4883.4 (5)C43—C47—C48—N3178.2 (7)
O9—Dy2—N3—C48110.9 (5)N4—C47—C48—C40176.2 (7)
O10—Dy2—N3—C4865.1 (5)C43—C47—C48—C400.9 (11)
N4—Dy2—N3—C481.5 (5)Dy2—O7—C49—O839.6 (11)
C57—Dy2—N3—C4889.2 (5)Dy2—O7—C49—C50139.5 (5)
O12ii—Dy2—N4—C46154.5 (6)Dy2ii—O8—C49—O76.9 (12)
O8ii—Dy2—N4—C4629.1 (8)Dy2ii—O8—C49—C50172.2 (5)
O11—Dy2—N4—C4624.9 (6)O7—C49—C50—C51172.8 (7)
O7—Dy2—N4—C46104.3 (6)O8—C49—C50—C518.0 (11)
O9—Dy2—N4—C46114.4 (6)O7—C49—C50—C559.4 (10)
O10—Dy2—N4—C4667.5 (6)O8—C49—C50—C55169.8 (7)
N3—Dy2—N4—C46178.8 (7)C55—C50—C51—C520.7 (12)
C57—Dy2—N4—C4689.5 (6)C49—C50—C51—C52177.2 (7)
O12ii—Dy2—N4—C4725.3 (7)C50—C51—C52—C531.3 (14)
O8ii—Dy2—N4—C47151.1 (5)C51—C52—C53—C541.4 (14)
O11—Dy2—N4—C47154.9 (6)C51—C52—C53—C56178.3 (8)
O7—Dy2—N4—C4775.5 (6)C52—C53—C54—C550.3 (14)
O9—Dy2—N4—C4765.8 (6)C56—C53—C54—C55179.9 (8)
O10—Dy2—N4—C47112.7 (6)C53—C54—C55—C502.3 (13)
N3—Dy2—N4—C471.0 (5)C51—C50—C55—C542.4 (12)
C57—Dy2—N4—C4790.7 (6)C49—C50—C55—C54175.5 (7)
C12—N1—C1—C21.6 (11)Dy2—O10—C57—O911.9 (7)
Dy1—N1—C1—C2171.2 (6)Dy2—O10—C57—C58168.8 (6)
N1—C1—C2—C31.5 (12)Dy2—O9—C57—O1012.2 (7)
C1—C2—C3—C41.8 (12)Dy2—O9—C57—C58168.5 (6)
C2—C3—C4—C120.8 (11)O12ii—Dy2—C57—O10161.7 (4)
C2—C3—C4—C5178.4 (8)O8ii—Dy2—C57—O1090.1 (4)
C3—C4—C5—C6173.7 (9)O11—Dy2—C57—O1019.6 (5)
C12—C4—C5—C63.8 (13)O7—Dy2—C57—O1095.9 (7)
C4—C5—C6—C70.6 (15)O9—Dy2—C57—O10168.0 (7)
C5—C6—C7—C8174.8 (9)N3—Dy2—C57—O10116.7 (4)
C5—C6—C7—C113.9 (13)N4—Dy2—C57—O1053.3 (4)
C11—C7—C8—C90.4 (13)O12ii—Dy2—C57—O930.3 (4)
C6—C7—C8—C9179.1 (9)O8ii—Dy2—C57—O9101.9 (4)
C7—C8—C9—C100.2 (14)O11—Dy2—C57—O9172.3 (4)
C11—N2—C10—C90.6 (12)O7—Dy2—C57—O972.1 (7)
Dy1—N2—C10—C9166.4 (7)O10—Dy2—C57—O9168.0 (7)
C8—C9—C10—N20.1 (14)N3—Dy2—C57—O951.3 (4)
C10—N2—C11—C71.2 (10)N4—Dy2—C57—O9114.7 (4)
Dy1—N2—C11—C7166.9 (5)O12ii—Dy2—C57—C5849 (3)
C10—N2—C11—C12175.8 (7)O8ii—Dy2—C57—C5823 (3)
Dy1—N2—C11—C1216.0 (8)O11—Dy2—C57—C5893 (3)
C8—C7—C11—N21.1 (11)O7—Dy2—C57—C58151 (3)
C6—C7—C11—N2179.9 (7)O9—Dy2—C57—C5879 (3)
C8—C7—C11—C12175.9 (7)O10—Dy2—C57—C58113 (3)
C6—C7—C11—C122.9 (11)N3—Dy2—C57—C58131 (3)
C1—N1—C12—C44.4 (10)N4—Dy2—C57—C58166 (3)
Dy1—N1—C12—C4168.8 (5)O10—C57—C58—C59176.9 (7)
C1—N1—C12—C11172.7 (7)O9—C57—C58—C592.4 (11)
Dy1—N1—C12—C1114.2 (8)Dy2—C57—C58—C5976 (3)
C3—C4—C12—N14.0 (10)O10—C57—C58—C631.0 (11)
C5—C4—C12—N1178.3 (7)O9—C57—C58—C63179.7 (7)
C3—C4—C12—C11173.0 (6)Dy2—C57—C58—C63106 (3)
C5—C4—C12—C114.7 (10)C63—C58—C59—C600.2 (14)
N2—C11—C12—N11.4 (10)C57—C58—C59—C60177.8 (8)
C7—C11—C12—N1178.5 (7)C58—C59—C60—C610.8 (15)
N2—C11—C12—C4175.7 (6)C59—C60—C61—C621.6 (15)
C7—C11—C12—C41.4 (10)C59—C60—C61—C64177.3 (10)
Dy1—O2—C13—O12.7 (8)C60—C61—C62—C631.8 (15)
Dy1—O2—C13—C14176.0 (7)C64—C61—C62—C63177.5 (9)
Dy1—O1—C13—O22.8 (9)C61—C62—C63—C581.3 (15)
Dy1—O1—C13—C14176.0 (6)C59—C58—C63—C620.4 (13)
O5—Dy1—C13—O2127 (4)C57—C58—C63—C62177.7 (8)
O6i—Dy1—C13—O273.0 (5)Dy2—O11—C65—O1228.8 (9)
O3—Dy1—C13—O265.9 (5)Dy2—O11—C65—C66149.8 (5)
O1—Dy1—C13—O2177.3 (9)Dy2ii—O12—C65—O1169 (2)
O4—Dy1—C13—O211.1 (5)Dy2ii—O12—C65—C66109.2 (17)
N1—Dy1—C13—O2154.8 (5)O11—C65—C66—C67159.6 (7)
N2—Dy1—C13—O2139.8 (5)O12—C65—C66—C6719.1 (10)
C21—Dy1—C13—O238.5 (5)O11—C65—C66—C7117.3 (10)
O5—Dy1—C13—O156 (5)O12—C65—C66—C71164.0 (6)
O6i—Dy1—C13—O1109.7 (5)C71—C66—C67—C681.7 (13)
O3—Dy1—C13—O1111.4 (5)C65—C66—C67—C68178.6 (8)
O4—Dy1—C13—O1166.2 (5)C66—C67—C68—C690.1 (15)
O2—Dy1—C13—O1177.3 (9)C67—C68—C69—C701.7 (16)
N1—Dy1—C13—O127.9 (5)C67—C68—C69—C72177.8 (10)
N2—Dy1—C13—O137.5 (5)C68—C69—C70—C711.4 (16)
C21—Dy1—C13—O1138.8 (5)C72—C69—C70—C71178.1 (9)
O5—Dy1—C13—C148 (11)C69—C70—C71—C660.5 (14)
O6i—Dy1—C13—C1461 (8)C67—C66—C71—C702.0 (12)
O3—Dy1—C13—C14160 (8)C65—C66—C71—C70179.0 (7)
O1—Dy1—C13—C1448 (7)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Dy2(C8H7O2)6(C12H8N2)2]
Mr1496.22
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)12.760 (8), 13.346 (9), 19.758 (13)
α, β, γ (°)91.619 (12), 97.925 (11), 106.44 (1)
V3)3188 (4)
Z2
Radiation typeMo Kα
µ (mm1)2.39
Crystal size (mm)0.22 × 0.18 × 0.12
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.541, 0.750
No. of measured, independent and
observed [I > 2σ(I)] reflections
16586, 11165, 7695
Rint0.033
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.121, 1.11
No. of reflections11165
No. of parameters811
No. of restraints18
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.86, 0.96

Computer programs: SMART (Bruker, 1997), SMART, SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.

 

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