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Acta Crystallogr Sect E Struct Rep Online. 2010 December 1; 66(Pt 12): m1653–m1654.
Published online 2010 November 24. doi:  10.1107/S1600536810048348
PMCID: PMC3011458

Bis(2,6-dihy­droxy­benzoato-κ2 O 1,O 1′)(nitrato-κ2 O,O′)bis­(1,10-phenanthroline-κ2 N,N′)dysprosium(III)

Abstract

In the mononuclear title complex, [Dy(C7H5O4)2(NO3)(C12H8N2)2], the DyIII atom is in a distorted bicapped square-anti­prismatic geometry formed by four N atoms from two chelating 1,10-phenanthroline (phen) ligands, four O atoms from two 2,6-dihy­droxy­benzoate (DHB) ligands and two O atoms from a nitrate anion. Inter­molecular π–π stacking inter­actions between the phen and DHB ligands [centroid–centroid distances = 3.542 (4) and 3.879 (4) Å] and between the pyridine and benzene rings of adjacent phen ligands [centroid–centroid distance = 3.751 (4) Å] stabilize the crystal structure. Intra­molecular O–H(...)O hydrogen bonds are observed in the DHB ligands.

Related literature

For a related structure, see: Zheng et al. (2010 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1653-scheme1.jpg

Experimental

Crystal data

  • [Dy(C7H5O4)2(NO3)(C12H8N2)2]
  • M r = 891.14
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1653-efi1.jpg
  • a = 11.1268 (3) Å
  • b = 26.7587 (4) Å
  • c = 14.2703 (5) Å
  • β = 127.280 (2)°
  • V = 3380.72 (18) Å3
  • Z = 4
  • Cu Kα radiation
  • μ = 12.46 mm−1
  • T = 298 K
  • 0.35 × 0.32 × 0.30 mm

Data collection

  • Oxford Diffraction Gemini S Ultra CCD diffractometer
  • Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2006 [triangle]) T min = 0.097, T max = 0.118
  • 11595 measured reflections
  • 5923 independent reflections
  • 4674 reflections with I > 2σ(I)
  • R int = 0.043

Refinement

  • R[F 2 > 2σ(F 2)] = 0.051
  • wR(F 2) = 0.137
  • S = 1.00
  • 5923 reflections
  • 496 parameters
  • H-atom parameters constrained
  • Δρmax = 1.68 e Å−3
  • Δρmin = −1.16 e Å−3

Data collection: CrysAlis PRO (Oxford Diffraction, 2006 [triangle]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: DIAMOND (Brandenburg & Berndt, 1999 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810048348/hy2381sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810048348/hy2381Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors are grateful for financial support from the Natural Science Foundation of Zhejiang Province (project No. 2010 Y4100495).

supplementary crystallographic information

Comment

The description of the structure of the title compound is part of a series of papers on mononuclear complexes of the type [Ln(DHB)2(NO3)(phen)2] [Ln = Ce, Pr, Sm, Eu and Dy (this publication); DHB = 2,6-dihydroxybenzoate; phen = 1,10-phenanthroline]. All five compounds are isostructural to the previously reported Nd complex (Zheng et al. 2010).

Experimental

All reagents are commercially available and of analytical grade. Dy(NO3)3.6H2O (0.229 g, 0.5 mmol), 2,6-dihydroxybenzoic acid (0.074 g, 0.5 mmol), 1,10-phenanthroline (0.090 g, 0.5 mmol) and NaHCO3 (0.042 g, 0.5 mmol) were dissolved in a water–ethanol solution (10 ml, v/v 1:1). The solution was refluxed for 4 h and filtered after cooling to room temperature. Yellow single crystals were obtained from the filtrate in 4 days.

Refinement

H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 and O—H = 0.82 Å and Uiso(H) = 1.2Ueq(C) and 1.5Ueq(O). The highest residual electron density was found 0.90 Å from Dy1 and the deepest hole 1.61 Å from O1.

Figures

Fig. 1.
The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probablility level. H atoms have been omitted for clarity. Dashed orange lines denote intramolecular hydrogen bonds.

Crystal data

[Dy(C7H5O4)2(NO3)(C12H8N2)2]F(000) = 1772
Mr = 891.14Dx = 1.751 Mg m3
Monoclinic, P21/cCu Kα radiation, λ = 1.54184 Å
Hall symbol: -P 2ybcCell parameters from 5391 reflections
a = 11.1268 (3) Åθ = 3.3–67.5°
b = 26.7587 (4) ŵ = 12.46 mm1
c = 14.2703 (5) ÅT = 298 K
β = 127.280 (2)°Prism, yellow
V = 3380.72 (18) Å30.35 × 0.32 × 0.30 mm
Z = 4

Data collection

Oxford Diffraction Gemini S Ultra CCD diffractometer5923 independent reflections
Radiation source: Enhance (Cu) X-ray Source4674 reflections with I > 2σ(I)
graphiteRint = 0.043
Detector resolution: 15.9149 pixels mm-1θmax = 67.1°, θmin = 3.3°
ω scansh = −11→13
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2006)k = −31→31
Tmin = 0.097, Tmax = 0.118l = −16→17
11595 measured reflections

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.0774P)2] where P = (Fo2 + 2Fc2)/3
5923 reflections(Δ/σ)max < 0.001
496 parametersΔρmax = 1.68 e Å3
0 restraintsΔρmin = −1.16 e Å3

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

xyzUiso*/Ueq
Dy10.92866 (4)0.862990 (11)0.22227 (3)0.03846 (13)
O10.8450 (5)0.83886 (15)0.0261 (4)0.0522 (11)
O20.8884 (5)0.91905 (15)0.0604 (4)0.0499 (10)
O30.7499 (6)0.80195 (16)−0.1748 (4)0.0702 (15)
H270.79120.8015−0.10390.105*
O40.8352 (8)0.97830 (17)−0.1043 (5)0.087 (2)
H310.85780.9702−0.04000.131*
O50.6975 (5)0.81369 (15)0.1368 (4)0.0505 (10)
O60.6691 (5)0.89410 (16)0.1017 (4)0.0584 (12)
O70.4806 (6)0.76073 (17)0.1052 (4)0.0624 (12)
H340.57060.76710.14140.094*
O80.4205 (7)0.93749 (19)0.0292 (6)0.0822 (17)
H380.50480.93440.04610.123*
O90.9472 (5)0.80198 (15)0.3727 (4)0.0583 (12)
O100.8436 (6)0.87351 (16)0.3467 (4)0.0556 (11)
O110.8566 (7)0.8210 (3)0.4675 (5)0.0883 (19)
N11.1603 (6)0.87915 (17)0.4391 (4)0.0408 (11)
N20.9734 (6)0.95380 (16)0.2914 (4)0.0442 (12)
N31.1761 (6)0.86887 (16)0.2491 (4)0.0406 (11)
N41.0506 (6)0.78088 (18)0.2394 (4)0.0435 (11)
N50.8816 (6)0.8312 (2)0.3985 (5)0.0527 (13)
C11.2533 (8)0.8434 (2)0.5122 (6)0.0483 (14)
H11.23850.81120.48200.058*
C21.3706 (8)0.8506 (3)0.6301 (6)0.0560 (16)
H21.43310.82420.67680.067*
C31.3928 (8)0.8974 (3)0.6766 (6)0.0569 (17)
H31.46920.90300.75610.068*
C41.2998 (7)0.9369 (2)0.6037 (5)0.0463 (14)
C51.1836 (7)0.9259 (2)0.4851 (5)0.0400 (12)
C61.0847 (7)0.9650 (2)0.4065 (5)0.0416 (13)
C71.1054 (8)1.0142 (2)0.4516 (6)0.0478 (15)
C81.2255 (8)1.0234 (2)0.5743 (7)0.0583 (18)
H81.23881.05550.60440.070*
C91.3175 (9)0.9870 (3)0.6454 (7)0.0618 (19)
H91.39500.99430.72380.074*
C101.0063 (9)1.0512 (2)0.3732 (6)0.0554 (17)
H101.01691.08390.39910.066*
C110.8959 (9)1.0395 (2)0.2603 (7)0.0590 (18)
H110.82831.06380.20820.071*
C120.8835 (8)0.9907 (2)0.2220 (6)0.0521 (15)
H120.80780.98360.14320.063*
C131.2359 (8)0.9120 (2)0.2500 (6)0.0528 (15)
H131.17650.94060.22480.063*
C141.3846 (8)0.9163 (3)0.2873 (6)0.0563 (17)
H141.42280.94730.28750.068*
C151.4723 (8)0.8747 (3)0.3231 (6)0.0594 (18)
H151.57150.87720.34880.071*
C161.4132 (7)0.8282 (3)0.3211 (5)0.0489 (15)
C171.2625 (7)0.8270 (2)0.2827 (5)0.0429 (13)
C181.1934 (7)0.7804 (2)0.2724 (5)0.0413 (13)
C191.2765 (7)0.7358 (2)0.2975 (5)0.0475 (14)
C201.4291 (8)0.7381 (3)0.3411 (6)0.0588 (18)
H201.48460.70870.36200.071*
C211.4956 (8)0.7820 (3)0.3529 (6)0.0595 (18)
H211.59630.78260.38200.071*
C221.1985 (8)0.6906 (2)0.2765 (6)0.0545 (17)
H221.24620.66030.28790.065*
C231.0545 (8)0.6914 (2)0.2399 (6)0.0535 (17)
H231.00270.66170.22610.064*
C240.9842 (8)0.7374 (2)0.2232 (5)0.0491 (15)
H240.88570.73730.19940.059*
C250.8441 (7)0.8824 (2)−0.0106 (5)0.0425 (13)
C260.7959 (7)0.8895 (2)−0.1304 (5)0.0416 (13)
C270.7498 (7)0.8487 (2)−0.2084 (5)0.0482 (15)
C280.7019 (8)0.8562 (3)−0.3224 (6)0.0608 (19)
H280.67180.8292−0.37320.073*
C290.6992 (9)0.9035 (3)−0.3599 (6)0.069 (2)
H290.66610.9082−0.43670.083*
C300.7440 (10)0.9440 (3)−0.2870 (6)0.068 (2)
H300.74180.9758−0.31440.082*
C310.7926 (9)0.9375 (2)−0.1728 (6)0.0582 (18)
C320.6131 (7)0.8522 (2)0.1013 (5)0.0474 (15)
C330.4611 (7)0.8492 (2)0.0671 (5)0.0460 (14)
C340.4014 (7)0.8037 (3)0.0719 (5)0.0504 (15)
C350.2580 (7)0.8010 (3)0.0423 (5)0.0555 (17)
H350.21990.77070.04590.067*
C360.1724 (8)0.8441 (3)0.0071 (6)0.067 (2)
H360.07540.8422−0.01390.080*
C370.2255 (9)0.8898 (3)0.0021 (6)0.067 (2)
H370.16580.9183−0.02140.081*
C380.3692 (8)0.8923 (3)0.0329 (6)0.0594 (18)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Dy10.0455 (2)0.02877 (18)0.0461 (2)−0.00037 (13)0.03041 (17)−0.00158 (13)
O10.065 (3)0.039 (2)0.050 (2)−0.0029 (19)0.033 (2)0.0047 (18)
O20.066 (3)0.040 (2)0.050 (2)−0.0004 (19)0.038 (2)−0.0041 (18)
O30.083 (4)0.044 (2)0.057 (3)−0.004 (2)0.028 (3)−0.008 (2)
O40.154 (6)0.043 (2)0.066 (3)−0.019 (3)0.067 (4)−0.005 (2)
O50.046 (2)0.041 (2)0.064 (3)0.0088 (18)0.033 (2)0.0041 (19)
O60.060 (3)0.044 (2)0.075 (3)0.002 (2)0.043 (3)0.009 (2)
O70.059 (3)0.052 (2)0.075 (3)0.002 (2)0.041 (3)0.010 (2)
O80.076 (4)0.053 (3)0.110 (4)0.019 (3)0.053 (3)0.017 (3)
O90.066 (3)0.040 (2)0.069 (3)0.000 (2)0.040 (3)0.000 (2)
O100.067 (3)0.049 (2)0.070 (3)0.004 (2)0.052 (3)−0.002 (2)
O110.097 (4)0.129 (5)0.066 (3)−0.013 (4)0.063 (3)0.010 (3)
N10.053 (3)0.033 (2)0.046 (3)0.002 (2)0.035 (2)0.0000 (19)
N20.063 (3)0.029 (2)0.046 (3)0.003 (2)0.035 (3)0.0012 (19)
N30.043 (3)0.037 (2)0.050 (3)−0.006 (2)0.033 (2)−0.004 (2)
N40.051 (3)0.038 (2)0.043 (2)−0.005 (2)0.029 (2)−0.001 (2)
N50.050 (3)0.060 (3)0.052 (3)−0.006 (3)0.033 (3)−0.005 (3)
C10.061 (4)0.041 (3)0.055 (4)0.006 (3)0.042 (3)0.004 (3)
C20.053 (4)0.063 (4)0.051 (4)0.009 (3)0.031 (3)0.007 (3)
C30.047 (3)0.072 (4)0.051 (3)−0.006 (3)0.029 (3)−0.006 (3)
C40.043 (3)0.049 (3)0.053 (3)−0.007 (3)0.032 (3)−0.008 (3)
C50.045 (3)0.039 (3)0.049 (3)−0.005 (2)0.035 (3)−0.005 (2)
C60.052 (3)0.033 (3)0.053 (3)−0.006 (2)0.039 (3)−0.003 (2)
C70.064 (4)0.036 (3)0.072 (4)−0.015 (3)0.056 (4)−0.013 (3)
C80.074 (5)0.044 (3)0.083 (5)−0.021 (3)0.061 (4)−0.022 (3)
C90.063 (4)0.062 (4)0.068 (4)−0.023 (4)0.043 (4)−0.026 (4)
C100.086 (5)0.029 (3)0.081 (5)−0.004 (3)0.067 (4)−0.003 (3)
C110.084 (5)0.034 (3)0.079 (5)0.012 (3)0.060 (4)0.014 (3)
C120.068 (4)0.037 (3)0.059 (4)0.004 (3)0.042 (3)0.002 (3)
C130.061 (4)0.045 (3)0.060 (4)−0.005 (3)0.041 (3)−0.005 (3)
C140.059 (4)0.060 (4)0.064 (4)−0.023 (3)0.044 (4)−0.012 (3)
C150.053 (4)0.077 (5)0.055 (4)−0.019 (4)0.036 (3)−0.010 (3)
C160.041 (3)0.067 (4)0.040 (3)−0.006 (3)0.026 (3)−0.006 (3)
C170.045 (3)0.046 (3)0.038 (3)−0.003 (3)0.026 (3)−0.007 (2)
C180.048 (3)0.045 (3)0.034 (3)0.000 (3)0.027 (3)−0.002 (2)
C190.056 (4)0.051 (3)0.040 (3)0.012 (3)0.032 (3)0.004 (3)
C200.059 (4)0.064 (4)0.049 (4)0.016 (3)0.030 (3)0.005 (3)
C210.047 (4)0.084 (5)0.050 (4)0.007 (4)0.031 (3)0.000 (3)
C220.073 (5)0.039 (3)0.052 (4)0.012 (3)0.039 (3)0.002 (3)
C230.073 (5)0.032 (3)0.055 (4)0.000 (3)0.039 (3)−0.003 (3)
C240.051 (3)0.038 (3)0.056 (4)−0.009 (3)0.031 (3)−0.006 (3)
C250.045 (3)0.041 (3)0.046 (3)−0.001 (2)0.030 (3)−0.001 (2)
C260.044 (3)0.040 (3)0.041 (3)−0.002 (2)0.026 (3)−0.001 (2)
C270.040 (3)0.048 (3)0.047 (3)0.005 (3)0.021 (3)−0.005 (3)
C280.055 (4)0.072 (5)0.049 (4)0.000 (3)0.028 (3)−0.017 (3)
C290.078 (5)0.084 (5)0.048 (4)−0.010 (4)0.039 (4)−0.005 (4)
C300.094 (6)0.063 (4)0.059 (4)−0.010 (4)0.052 (4)0.007 (3)
C310.078 (5)0.047 (3)0.052 (4)−0.010 (3)0.040 (4)0.000 (3)
C320.050 (4)0.049 (3)0.040 (3)0.003 (3)0.026 (3)0.002 (3)
C330.041 (3)0.058 (3)0.040 (3)0.004 (3)0.025 (3)−0.002 (3)
C340.045 (3)0.067 (4)0.042 (3)0.001 (3)0.028 (3)0.000 (3)
C350.047 (4)0.079 (5)0.044 (3)−0.002 (3)0.029 (3)0.000 (3)
C360.048 (4)0.105 (6)0.049 (4)0.007 (4)0.031 (3)−0.001 (4)
C370.057 (4)0.085 (5)0.060 (4)0.029 (4)0.035 (4)0.008 (4)
C380.058 (4)0.066 (4)0.053 (4)0.015 (3)0.033 (3)0.006 (3)

Geometric parameters (Å, °)

Dy1—N12.597 (5)C9—H90.9300
Dy1—N22.556 (4)C10—C111.344 (10)
Dy1—N32.545 (5)C10—H100.9300
Dy1—N42.515 (5)C11—C121.389 (9)
Dy1—O12.442 (4)C11—H110.9300
Dy1—O22.557 (4)C12—H120.9300
Dy1—O52.458 (4)C13—C141.403 (9)
Dy1—O62.444 (5)C13—H130.9300
Dy1—O92.604 (5)C14—C151.360 (11)
Dy1—O102.482 (5)C14—H140.9300
O1—C251.274 (7)C15—C161.401 (10)
O2—C251.275 (7)C15—H150.9300
O3—C271.340 (8)C16—C171.414 (8)
O3—H270.8196C16—C211.439 (10)
O4—C311.345 (8)C17—C181.425 (8)
O4—H310.8201C18—C191.417 (8)
O5—C321.275 (7)C19—C221.410 (10)
O6—C321.281 (8)C19—C201.413 (10)
O7—C341.348 (8)C20—C211.344 (11)
O7—H340.8198C20—H200.9300
O8—C381.352 (9)C21—H210.9300
O8—H380.8190C22—C231.352 (10)
O9—N51.267 (7)C22—H220.9300
O10—N51.277 (7)C23—C241.398 (9)
O11—N51.205 (7)C23—H230.9300
N1—C11.330 (8)C24—H240.9300
N1—C51.363 (7)C25—C261.462 (8)
N2—C121.326 (8)C26—C311.411 (9)
N2—C61.363 (8)C26—C271.415 (8)
N3—C131.328 (8)C27—C281.386 (10)
N3—C171.360 (8)C28—C291.365 (11)
N4—C241.322 (8)C28—H280.9300
N4—C181.356 (8)C29—C301.371 (11)
C1—C21.382 (9)C29—H290.9300
C1—H10.9300C30—C311.383 (10)
C2—C31.367 (10)C30—H300.9300
C2—H20.9300C32—C331.452 (9)
C3—C41.402 (10)C33—C341.407 (9)
C3—H30.9300C33—C381.418 (9)
C4—C51.404 (8)C34—C351.383 (9)
C4—C91.433 (9)C35—C361.384 (11)
C5—C61.439 (8)C35—H350.9300
C6—C71.420 (8)C36—C371.379 (12)
C7—C101.398 (9)C36—H360.9300
C7—C81.442 (10)C37—C381.380 (10)
C8—C91.329 (11)C37—H370.9300
C8—H80.9300
O1—Dy1—O679.39 (17)C9—C8—H8119.4
O1—Dy1—O574.42 (15)C7—C8—H8119.4
O6—Dy1—O553.02 (13)C8—C9—C4121.4 (6)
O1—Dy1—O10143.53 (17)C8—C9—H9119.3
O6—Dy1—O1070.42 (17)C4—C9—H9119.3
O5—Dy1—O1071.23 (16)C11—C10—C7120.0 (6)
O1—Dy1—N471.90 (15)C11—C10—H10120.0
O6—Dy1—N4134.73 (16)C7—C10—H10120.0
O5—Dy1—N485.41 (15)C10—C11—C12119.4 (6)
O10—Dy1—N4116.50 (15)C10—C11—H11120.3
O1—Dy1—N379.34 (16)C12—C11—H11120.3
O6—Dy1—N3142.59 (16)N2—C12—C11123.8 (6)
O5—Dy1—N3145.01 (14)N2—C12—H12118.1
O10—Dy1—N3137.05 (16)C11—C12—H12118.1
N4—Dy1—N364.45 (15)N3—C13—C14122.9 (6)
O1—Dy1—N2122.95 (14)N3—C13—H13118.5
O6—Dy1—N279.54 (16)C14—C13—H13118.5
O5—Dy1—N2127.03 (16)C15—C14—C13119.2 (6)
O10—Dy1—N271.66 (16)C15—C14—H14120.4
N4—Dy1—N2145.66 (16)C13—C14—H14120.4
N3—Dy1—N286.76 (16)C14—C15—C16119.9 (7)
O1—Dy1—O251.87 (12)C14—C15—H15120.0
O6—Dy1—O271.26 (16)C16—C15—H15120.0
O5—Dy1—O2107.97 (14)C15—C16—C17117.4 (6)
O10—Dy1—O2130.24 (14)C15—C16—C21123.7 (7)
N4—Dy1—O2112.92 (15)C17—C16—C21118.9 (6)
N3—Dy1—O271.39 (15)N3—C17—C16122.5 (6)
N2—Dy1—O271.20 (14)N3—C17—C18117.6 (5)
O1—Dy1—N1145.48 (16)C16—C17—C18119.9 (6)
O6—Dy1—N1132.75 (16)N4—C18—C19122.9 (6)
O5—Dy1—N1131.74 (15)N4—C18—C17118.2 (5)
O10—Dy1—N170.26 (16)C19—C18—C17118.8 (6)
N4—Dy1—N186.66 (15)C22—C19—C20123.5 (6)
N3—Dy1—N166.91 (16)C22—C19—C18116.4 (6)
N2—Dy1—N163.96 (15)C20—C19—C18120.1 (6)
O2—Dy1—N1118.90 (14)C21—C20—C19121.2 (6)
O1—Dy1—O9124.35 (14)C21—C20—H20119.4
O6—Dy1—O9105.28 (16)C19—C20—H20119.4
O5—Dy1—O967.00 (15)C20—C21—C16120.9 (7)
O10—Dy1—O949.88 (15)C20—C21—H21119.5
N4—Dy1—O966.62 (16)C16—C21—H21119.5
N3—Dy1—O9112.12 (16)C23—C22—C19120.2 (6)
N2—Dy1—O9112.21 (15)C23—C22—H22119.9
O2—Dy1—O9174.91 (14)C19—C22—H22119.9
N1—Dy1—O966.19 (15)C22—C23—C24119.2 (6)
C25—O1—Dy197.6 (4)C22—C23—H23120.4
C25—O2—Dy192.2 (3)C24—C23—H23120.4
C27—O3—H27109.5N4—C24—C23123.4 (7)
C31—O4—H31109.4N4—C24—H24118.3
C32—O5—Dy193.5 (4)C23—C24—H24118.3
C32—O6—Dy194.0 (4)O1—C25—O2118.3 (5)
C34—O7—H34109.5O1—C25—C26120.4 (5)
C38—O8—H38109.5O2—C25—C26121.3 (5)
N5—O9—Dy194.6 (3)C31—C26—C27117.5 (6)
N5—O10—Dy1100.3 (4)C31—C26—C25121.1 (5)
C1—N1—C5116.9 (5)C27—C26—C25121.4 (5)
C1—N1—Dy1123.6 (4)O3—C27—C28118.1 (6)
C5—N1—Dy1119.2 (4)O3—C27—C26121.2 (6)
C12—N2—C6117.3 (5)C28—C27—C26120.7 (6)
C12—N2—Dy1122.6 (4)C29—C28—C27119.7 (6)
C6—N2—Dy1119.8 (3)C29—C28—H28120.2
C13—N3—C17118.1 (6)C27—C28—H28120.2
C13—N3—Dy1123.0 (4)C28—C29—C30121.6 (7)
C17—N3—Dy1118.1 (4)C28—C29—H29119.2
C24—N4—C18117.7 (5)C30—C29—H29119.2
C24—N4—Dy1122.8 (4)C29—C30—C31119.8 (7)
C18—N4—Dy1119.4 (4)C29—C30—H30120.1
O11—N5—O9123.8 (6)C31—C30—H30120.1
O11—N5—O10121.0 (6)O4—C31—C30117.9 (6)
O9—N5—O10115.2 (5)O4—C31—C26121.4 (6)
N1—C1—C2124.5 (6)C30—C31—C26120.7 (6)
N1—C1—H1117.8O5—C32—O6117.8 (6)
C2—C1—H1117.8O5—C32—C33121.1 (6)
C3—C2—C1118.6 (6)O6—C32—C33121.0 (6)
C3—C2—H2120.7C34—C33—C38117.3 (6)
C1—C2—H2120.7C34—C33—C32121.3 (6)
C2—C3—C4119.6 (6)C38—C33—C32121.3 (6)
C2—C3—H3120.2O7—C34—C35116.8 (6)
C4—C3—H3120.2O7—C34—C33121.8 (6)
C3—C4—C5117.7 (6)C35—C34—C33121.4 (6)
C3—C4—C9123.0 (6)C34—C35—C36118.7 (7)
C5—C4—C9119.4 (6)C34—C35—H35120.6
N1—C5—C4122.7 (5)C36—C35—H35120.6
N1—C5—C6117.4 (5)C37—C36—C35122.4 (7)
C4—C5—C6119.9 (5)C37—C36—H36118.8
N2—C6—C7122.0 (5)C35—C36—H36118.8
N2—C6—C5119.1 (5)C36—C37—C38118.5 (7)
C7—C6—C5118.9 (5)C36—C37—H37120.8
C10—C7—C6117.5 (6)C38—C37—H37120.8
C10—C7—C8123.5 (6)O8—C38—C37117.8 (7)
C6—C7—C8119.1 (6)O8—C38—C33120.6 (7)
C9—C8—C7121.3 (6)C37—C38—C33121.7 (7)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O3—H27···O10.821.862.577 (7)146
O4—H31···O20.821.862.588 (6)148
O7—H34···O50.821.912.592 (7)139
O8—H38···O60.821.842.570 (7)148

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2381).

References

  • Brandenburg, K. & Berndt, M. (1999). DIAMOND Crystal Impact GbR, Bonn, Germany.
  • Oxford Diffraction (2006). CrysAlis PRO Oxford Diffraction Ltd, Abingdon, England.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Zheng, J., Jin, H. & Ge, H. (2010). Acta Cryst. E66, m1469–m1470. [PMC free article] [PubMed]

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