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Acta Crystallogr Sect E Struct Rep Online. 2010 February 1; 66(Pt 2): m107.
Published online 2010 January 9. doi:  10.1107/S1600536809055184
PMCID: PMC2979913

[N,N′-Bis(3-meth­oxy-2-oxidobenzyl­idene)ethane-1,2-diaminium-κ4 O,O′,O′′,O′′′]tris­(nitrato-κ2 O,O′)erbium(III)

Abstract

In the mononuclear salen-type complex, [Er(NO3)3(C18H20N2O4)], the ErIII ion is ten-coordinated in a distorted hexa­deca­hedral geometry by six O atoms of three nitrate anions and four O atoms of the salen-like ligand. Inter­molecular N—H(...)O hydrogen bonds occur. The crystal structure is stabilized by inter­molecular C—H(...)O hydrogen bonds.

Related literature

For similar lanthanide complexes of the same salen-like ligand, see: Gao et al. (2008 [triangle], 2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m107-scheme1.jpg

Experimental

Crystal data

  • [Er(NO3)3(C18H20N2O4)]
  • M r = 681.65
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m107-efi1.jpg
  • a = 14.098 (3) Å
  • b = 11.865 (2) Å
  • c = 14.571 (3) Å
  • β = 103.98 (3)°
  • V = 2365.1 (8) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 3.63 mm−1
  • T = 291 K
  • 0.37 × 0.36 × 0.34 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.344, T max = 0.368
  • 21792 measured reflections
  • 5358 independent reflections
  • 4748 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.022
  • wR(F 2) = 0.049
  • S = 1.04
  • 5358 reflections
  • 344 parameters
  • 2 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.97 e Å−3
  • Δρmin = −0.32 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 [triangle]); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809055184/pk2218sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809055184/pk2218Isup2.hkl

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

Acknowledgments

The authors gratefully acknowledge financial support from the National Natural Science Foundation of China (Nos. 20672032 and 20872030), the Key Laboratory of Heilongjiang Province and the Education Department of Heilongjiang Province (Nos. ZJG0504, JC200605, 1152GZD02, GZ08A401, 11531284, 2006FRFLXG031 and 2007RFQXG096) and Heilongjiang University.

supplementary crystallographic information

Comment

In continuation of our studies of salen-type lanthanide complexes (Gao et al., 2008, 2009), we present here the crystal structure of the title compound. As shown in Fig. 1, the ten-coordinate ErIII ion adopts a hexadecahedral geometry provided by the O atoms of three bidentate nitrate anions and by one ligand that utilizes two hydroxyl and two methoxy oxygen atoms, while the protonated nitrogen atoms remain uncoordinated. This compound is isostructural with the corresponding Nd, Eu, Tb and Dy complexes (Gao et al., 2008, 2009). The Er—O bond distances range from 2.2462 (19) to 2.682 (2) Å, with the shorter bonds involving the O1 and O3 deprotonated phenol oxygen atoms. The crystal structure is stabilized by intra- and intermolecular N—H···O and C—H···O hydrogen bonds (Table 1).

Experimental

The title complex was obtained by the treatment of erbium (III) nitrate hexahydrate (0.114 g, 0.25 mmol) with the salen-type ligand (0.083 g, 0.25 mmol) in acetonitrile/methanol (10 ml/10 ml). The mixture was stirred for 3 h. The reaction mixture was filtered; diethyl ether was allowed to diffuse slowly into the solution of the filtrate. Single crystals were obtained after several days. Analysis calculated for for C18H20Er1N5O13: C 31.72, H 2.96, N 10.27%; found: C 32.08, H 3.00, N 10.38%.

Refinement

H atoms bound to C atoms were placed in calculated positions and treated as riding on their parent atoms, with C—H = 0.93 Å (aromatic C), C—H = 0.97Å (methylene C), and with Uiso(H) = 1.2Ueq(C) or C—H = 0.96 Å (methyl C) and with Uiso(H) = 1.5Ueq(C). The N-bound H atoms were initially located in a difference Fourier map and they were refined with the N—H bond distance restrained to 0.85 Å.

Figures

Fig. 1.
The molecular structure of the the title compound, showing 30% probability displacement ellipsoids.

Crystal data

[Er(NO3)3(C18H20N2O4)]F(000) = 1340
Mr = 681.65Dx = 1.914 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 19557 reflections
a = 14.098 (3) Åθ = 6.7–55.0°
b = 11.865 (2) ŵ = 3.63 mm1
c = 14.571 (3) ÅT = 291 K
β = 103.98 (3)°Block, brown
V = 2365.1 (8) Å30.37 × 0.36 × 0.34 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer5358 independent reflections
Radiation source: fine-focus sealed tube4748 reflections with I > 2σ(I)
graphiteRint = 0.024
Detector resolution: 10.000 pixels mm-1θmax = 27.5°, θmin = 3.4°
ω scansh = −18→18
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)k = −15→13
Tmin = 0.344, Tmax = 0.368l = −18→18
21792 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)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.049H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0212P)2 + 1.495P] where P = (Fo2 + 2Fc2)/3
5358 reflections(Δ/σ)max = 0.002
344 parametersΔρmax = 0.97 e Å3
2 restraintsΔρmin = −0.32 e Å3

Special details

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)

xyzUiso*/Ueq
C11.11705 (18)0.8605 (2)0.45224 (18)0.0382 (5)
C21.20341 (19)0.8854 (2)0.42275 (19)0.0407 (5)
C31.28633 (19)0.9208 (2)0.4865 (2)0.0473 (6)
H31.34340.93340.46670.057*
C41.2851 (2)0.9379 (2)0.5812 (2)0.0514 (7)
H41.34160.96180.62410.062*
C51.2025 (2)0.9199 (2)0.6108 (2)0.0482 (6)
H51.20210.93380.67360.058*
C61.11664 (18)0.8802 (2)0.54721 (17)0.0398 (5)
C71.03136 (19)0.8571 (2)0.57937 (18)0.0419 (6)
H71.03400.86610.64330.050*
C80.8585 (2)0.8013 (2)0.5501 (2)0.0476 (6)
H8A0.81900.86920.54240.057*
H8B0.87210.77910.61610.057*
C90.8026 (2)0.7084 (2)0.4892 (2)0.0463 (6)
H9A0.83840.63810.50290.056*
H9B0.73950.69850.50380.056*
C100.71313 (18)0.7852 (2)0.33653 (19)0.0405 (6)
H100.65850.79630.36070.049*
C110.70956 (17)0.8234 (2)0.24387 (18)0.0378 (5)
C120.62437 (19)0.8736 (2)0.1881 (2)0.0487 (6)
H120.56900.87990.21180.058*
C130.6223 (2)0.9123 (3)0.1009 (2)0.0562 (8)
H130.56520.94420.06470.067*
C140.7057 (2)0.9052 (2)0.0634 (2)0.0509 (7)
H140.70330.93190.00290.061*
C150.78977 (18)0.8588 (2)0.11660 (18)0.0393 (5)
C160.79432 (17)0.8157 (2)0.20754 (18)0.0353 (5)
C170.8799 (3)0.8857 (3)−0.0015 (2)0.0660 (9)
H150.82870.8495−0.04750.099*
H160.94200.8669−0.01350.099*
H170.87080.9659−0.00560.099*
C181.2751 (3)0.8925 (4)0.2892 (3)0.0813 (12)
H181.29670.96850.30430.122*
H191.25670.88350.22170.122*
H201.32700.84110.31580.122*
Er11.027172 (8)0.791612 (9)0.235283 (7)0.03487 (4)
H10.954 (2)0.824 (3)0.4667 (10)0.055 (9)*
H20.8358 (18)0.723 (3)0.364 (2)0.065 (10)*
N10.95017 (17)0.8241 (2)0.52382 (16)0.0431 (5)
N20.78847 (16)0.7357 (2)0.38932 (16)0.0410 (5)
N31.0155 (2)1.0328 (2)0.1988 (2)0.0662 (7)
N41.07427 (19)0.6872 (2)0.07369 (18)0.0498 (6)
N51.08572 (16)0.57223 (19)0.31635 (15)0.0422 (5)
O11.04131 (13)0.82028 (18)0.39117 (13)0.0500 (5)
O21.19230 (13)0.86931 (18)0.32755 (13)0.0500 (5)
O30.87510 (12)0.77016 (15)0.25531 (12)0.0393 (4)
O40.87710 (14)0.84819 (17)0.09111 (13)0.0485 (4)
O50.97238 (19)0.9849 (2)0.25442 (16)0.0729 (7)
O61.0101 (3)1.1337 (2)0.1861 (3)0.1093 (11)
O71.06391 (17)0.96856 (19)0.15897 (16)0.0613 (6)
O81.12293 (19)0.7666 (2)0.11639 (19)0.0714 (7)
O91.0911 (2)0.6461 (2)0.00302 (18)0.0794 (7)
O101.00528 (15)0.6536 (2)0.10706 (16)0.0615 (6)
O111.14616 (13)0.64176 (18)0.29752 (16)0.0543 (5)
O121.11095 (15)0.48027 (17)0.35168 (15)0.0566 (5)
O130.99850 (14)0.60343 (17)0.29684 (16)0.0547 (5)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.0425 (13)0.0366 (14)0.0352 (13)−0.0009 (10)0.0089 (10)0.0014 (10)
C20.0466 (14)0.0346 (13)0.0415 (14)−0.0049 (10)0.0119 (10)−0.0005 (11)
C30.0432 (14)0.0371 (14)0.0607 (18)−0.0041 (11)0.0111 (12)−0.0004 (13)
C40.0519 (16)0.0423 (16)0.0522 (17)−0.0049 (12)−0.0025 (12)−0.0064 (13)
C50.0614 (17)0.0391 (15)0.0390 (15)0.0005 (12)0.0023 (12)−0.0049 (11)
C60.0511 (14)0.0329 (13)0.0347 (13)0.0027 (10)0.0092 (10)−0.0002 (10)
C70.0570 (16)0.0376 (14)0.0321 (13)0.0075 (11)0.0127 (11)−0.0027 (10)
C80.0512 (15)0.0602 (18)0.0377 (14)0.0090 (12)0.0229 (11)0.0051 (12)
C90.0495 (15)0.0522 (16)0.0425 (15)0.0046 (11)0.0217 (11)0.0143 (12)
C100.0382 (13)0.0407 (14)0.0461 (15)−0.0002 (10)0.0170 (10)−0.0042 (11)
C110.0364 (12)0.0369 (13)0.0406 (14)0.0045 (9)0.0102 (10)−0.0024 (10)
C120.0402 (14)0.0496 (16)0.0546 (17)0.0106 (11)0.0084 (11)−0.0028 (13)
C130.0496 (16)0.0533 (18)0.0577 (19)0.0179 (13)−0.0027 (13)0.0056 (14)
C140.0638 (18)0.0448 (16)0.0390 (15)0.0085 (12)0.0022 (12)0.0072 (12)
C150.0460 (14)0.0371 (14)0.0347 (13)0.0039 (10)0.0094 (10)0.0018 (10)
C160.0378 (12)0.0328 (13)0.0353 (13)0.0031 (9)0.0091 (9)0.0009 (9)
C170.081 (2)0.084 (2)0.0378 (16)0.0008 (18)0.0249 (15)0.0118 (16)
C180.068 (2)0.121 (3)0.066 (2)−0.041 (2)0.0381 (18)−0.012 (2)
Er10.03856 (7)0.04067 (7)0.02990 (6)−0.00224 (4)0.01707 (4)0.00026 (4)
N10.0496 (13)0.0531 (14)0.0309 (12)0.0030 (10)0.0181 (9)0.0011 (10)
N20.0410 (12)0.0482 (13)0.0382 (12)0.0027 (9)0.0183 (9)0.0038 (9)
N30.107 (2)0.0498 (17)0.0492 (15)−0.0087 (14)0.0328 (15)−0.0004 (13)
N40.0628 (15)0.0502 (15)0.0439 (13)0.0119 (11)0.0270 (11)0.0006 (11)
N50.0452 (12)0.0476 (13)0.0352 (11)0.0032 (9)0.0124 (9)0.0028 (9)
O10.0430 (10)0.0761 (14)0.0332 (10)−0.0144 (9)0.0136 (8)−0.0086 (9)
O20.0476 (10)0.0648 (13)0.0430 (11)−0.0166 (9)0.0215 (8)−0.0047 (9)
O30.0348 (9)0.0484 (11)0.0360 (9)0.0081 (7)0.0109 (7)0.0099 (7)
O40.0574 (11)0.0581 (12)0.0335 (10)0.0032 (9)0.0179 (8)0.0075 (8)
O50.127 (2)0.0497 (14)0.0611 (15)−0.0098 (12)0.0588 (15)−0.0098 (10)
O60.192 (3)0.0431 (16)0.116 (3)0.0054 (17)0.082 (2)0.0152 (16)
O70.0805 (15)0.0568 (13)0.0560 (13)−0.0025 (11)0.0344 (11)0.0099 (11)
O80.0880 (17)0.0701 (16)0.0739 (17)−0.0253 (13)0.0539 (14)−0.0199 (13)
O90.118 (2)0.0705 (17)0.0685 (16)0.0085 (14)0.0590 (15)−0.0145 (13)
O100.0520 (12)0.0793 (16)0.0589 (14)−0.0083 (10)0.0245 (10)−0.0197 (11)
O110.0397 (10)0.0558 (13)0.0686 (14)−0.0013 (8)0.0151 (9)0.0030 (10)
O120.0679 (13)0.0489 (12)0.0524 (12)0.0159 (9)0.0132 (9)0.0122 (10)
O130.0414 (10)0.0518 (12)0.0753 (14)0.0058 (8)0.0225 (9)0.0181 (10)

Geometric parameters (Å, °)

C1—O11.304 (3)C15—C161.407 (3)
C1—C61.405 (3)C16—O31.300 (3)
C1—C21.417 (3)C17—O41.430 (3)
C2—C31.371 (4)C17—H150.9600
C2—O21.371 (3)C17—H160.9600
C3—C41.399 (4)C17—H170.9600
C3—H30.9300C18—O21.437 (3)
C4—C51.354 (4)C18—H180.9600
C4—H40.9300C18—H190.9600
C5—C61.416 (4)C18—H200.9600
C5—H50.9300Er1—O32.2469 (17)
C6—C71.419 (4)Er1—O12.2576 (19)
C7—N11.293 (3)Er1—O102.447 (2)
C7—H70.9300Er1—O52.458 (2)
C8—N11.460 (3)Er1—O82.458 (2)
C8—C91.512 (4)Er1—O112.462 (2)
C8—H8A0.9700Er1—O132.476 (2)
C8—H8B0.9700Er1—O72.488 (2)
C9—N21.457 (3)Er1—O22.562 (2)
C9—H9A0.9700Er1—O42.682 (2)
C9—H9B0.9700Er1—N42.877 (2)
C10—N21.292 (3)Er1—N52.895 (2)
C10—C111.413 (4)N1—H10.846 (10)
C10—H100.9300N2—H20.847 (10)
C11—C121.409 (4)N3—O61.211 (4)
C11—C161.422 (3)N3—O71.255 (3)
C12—C131.344 (4)N3—O51.260 (3)
C12—H120.9300N4—O91.213 (3)
C13—C141.413 (4)N4—O81.241 (3)
C13—H130.9300N4—O101.253 (3)
C14—C151.365 (4)N5—O121.222 (3)
C14—H140.9300N5—O131.249 (3)
C15—O41.375 (3)N5—O111.263 (3)
O1—C1—C6122.4 (2)O8—Er1—O13108.19 (8)
O1—C1—C2119.4 (2)O11—Er1—O1351.07 (6)
C6—C1—C2118.2 (2)O3—Er1—O7117.50 (7)
C3—C2—O2126.7 (2)O1—Er1—O7110.20 (8)
C3—C2—C1120.9 (2)O10—Er1—O7103.00 (8)
O2—C2—C1112.4 (2)O5—Er1—O750.82 (7)
C2—C3—C4120.1 (3)O8—Er1—O765.02 (8)
C2—C3—H3120.0O11—Er1—O7125.25 (7)
C4—C3—H3120.0O13—Er1—O7173.13 (7)
C5—C4—C3120.6 (3)O3—Er1—O2138.34 (6)
C5—C4—H4119.7O1—Er1—O264.51 (6)
C3—C4—H4119.7O10—Er1—O2124.92 (7)
C4—C5—C6120.6 (3)O5—Er1—O282.83 (8)
C4—C5—H5119.7O8—Er1—O280.16 (8)
C6—C5—H5119.7O11—Er1—O267.34 (7)
C1—C6—C5119.6 (2)O13—Er1—O2109.97 (7)
C1—C6—C7119.9 (2)O7—Er1—O270.74 (7)
C5—C6—C7120.4 (2)O3—Er1—O462.17 (6)
N1—C7—C6123.0 (2)O1—Er1—O4127.71 (7)
N1—C7—H7118.5O10—Er1—O468.86 (7)
C6—C7—H7118.5O5—Er1—O469.22 (8)
N1—C8—C9110.5 (2)O8—Er1—O486.66 (8)
N1—C8—H8A109.6O11—Er1—O4143.86 (7)
C9—C8—H8A109.6O13—Er1—O4110.04 (7)
N1—C8—H8B109.6O7—Er1—O469.43 (7)
C9—C8—H8B109.6O2—Er1—O4139.98 (7)
H8A—C8—H8B108.1O3—Er1—N4118.27 (8)
N2—C9—C8110.5 (2)O1—Er1—N4155.06 (7)
N2—C9—H9A109.5O10—Er1—N425.63 (7)
C8—C9—H9A109.5O5—Er1—N4129.48 (7)
N2—C9—H9B109.5O8—Er1—N425.37 (7)
C8—C9—H9B109.5O11—Er1—N473.69 (7)
H9A—C9—H9B108.1O13—Er1—N489.91 (7)
N2—C10—C11123.3 (2)O7—Er1—N483.31 (7)
N2—C10—H10118.4O2—Er1—N4102.96 (7)
C11—C10—H10118.4O4—Er1—N476.17 (7)
C12—C11—C10121.0 (2)O3—Er1—N591.84 (6)
C12—C11—C16119.2 (2)O1—Er1—N577.16 (7)
C10—C11—C16119.7 (2)O10—Er1—N571.38 (8)
C13—C12—C11120.7 (3)O5—Er1—N5149.24 (7)
C13—C12—H12119.7O8—Er1—N591.62 (8)
C11—C12—H12119.7O11—Er1—N525.67 (6)
C12—C13—C14121.0 (2)O13—Er1—N525.39 (6)
C12—C13—H13119.5O7—Er1—N5150.63 (7)
C14—C13—H13119.5O2—Er1—N588.63 (7)
C15—C14—C13119.6 (3)O4—Er1—N5129.63 (6)
C15—C14—H14120.2N4—Er1—N581.22 (7)
C13—C14—H14120.2C7—N1—C8126.7 (2)
C14—C15—O4126.5 (2)C7—N1—H1111 (2)
C14—C15—C16121.1 (2)C8—N1—H1122 (2)
O4—C15—C16112.4 (2)C10—N2—C9126.2 (2)
O3—C16—C15119.3 (2)C10—N2—H2116 (2)
O3—C16—C11122.2 (2)C9—N2—H2117 (2)
C15—C16—C11118.4 (2)O6—N3—O7123.4 (3)
O4—C17—H15109.5O6—N3—O5121.5 (3)
O4—C17—H16109.5O7—N3—O5115.1 (3)
H15—C17—H16109.5O6—N3—Er1178.1 (2)
O4—C17—H17109.5O7—N3—Er158.24 (15)
H15—C17—H17109.5O5—N3—Er156.87 (16)
H16—C17—H17109.5O9—N4—O8122.3 (3)
O2—C18—H18109.5O9—N4—O10122.0 (3)
O2—C18—H19109.5O8—N4—O10115.7 (2)
H18—C18—H19109.5O9—N4—Er1177.1 (2)
O2—C18—H20109.5O8—N4—Er158.09 (13)
H18—C18—H20109.5O10—N4—Er157.67 (14)
H19—C18—H20109.5O12—N5—O13122.0 (2)
O3—Er1—O175.02 (7)O12—N5—O11122.1 (2)
O3—Er1—O1094.30 (7)O13—N5—O11115.8 (2)
O1—Er1—O10146.42 (8)O12—N5—Er1179.17 (19)
O3—Er1—O575.82 (7)O13—N5—Er158.18 (13)
O1—Er1—O572.48 (8)O11—N5—Er157.65 (13)
O10—Er1—O5136.56 (9)C1—O1—Er1126.89 (16)
O3—Er1—O8141.41 (8)C2—O2—C18117.5 (2)
O1—Er1—O8142.88 (8)C2—O2—Er1116.64 (14)
O10—Er1—O851.00 (7)C18—O2—Er1125.79 (19)
O5—Er1—O8115.70 (8)C16—O3—Er1128.54 (15)
O3—Er1—O11117.19 (6)C15—O4—C17117.2 (2)
O1—Er1—O1181.46 (8)C15—O4—Er1113.57 (14)
O10—Er1—O1175.35 (8)C17—O4—Er1128.36 (18)
O5—Er1—O11146.82 (8)N3—O5—Er197.71 (18)
O8—Er1—O1174.41 (9)N3—O7—Er196.36 (16)
O3—Er1—O1366.82 (6)N4—O8—Er196.54 (16)
O1—Er1—O1375.74 (8)N4—O10—Er196.69 (17)
O10—Er1—O1370.83 (8)N5—O11—Er196.68 (14)
O5—Er1—O13135.84 (7)N5—O13—Er196.42 (15)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N2—H2···O30.85 (1)1.89 (3)2.574 (3)137 (3)
N1—H1···O10.85 (1)1.84 (2)2.567 (3)143 (3)
C7—H7···O5i0.932.333.073 (3)137
C9—H9A···O12ii0.972.503.241 (3)133
C10—H10···O9iii0.932.573.395 (4)148
C14—H14···O12iv0.932.503.341 (4)150

Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+2, −y+1, −z+1; (iii) x−1/2, −y+3/2, z+1/2; (iv) x−1/2, −y+3/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PK2218).

References

  • Gao, T., Li, G.-M., Gao, P., Yan, P.-F. & Hou, G.-F. (2009). Acta Cryst. E65, m1585. [PMC free article] [PubMed]
  • Gao, T., Yan, P. F., Li, G. M., Hou, G. F. & Gao, J. S. (2008). Inorg. Chim. Acta, 361, 2051–2058.
  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Rigaku (1998). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  • Rigaku/MSC (2002). CrystalClear Rigaku/MSC Inc., The Woodlands, Texas, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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