Crystal structure of poly[μ6-adipato-di­aquadi-μ2-oxalato-didysprosium(III)]

Li, Z.-F.; Zhang, Y.-C.; Hu, X.-Q.; Wang, C.-X.

doi:10.1107/S1600536814024544

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 12| December 2014| Pages m399-m400

doi:10.1107/S1600536814024544

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Crystal structure of poly[μ₆-adipato-diaquadi-μ₂-oxalato-didysprosium(III)]

Zhi-Feng Li,^a ^* Yi-Chao Zhang,^a Xiao-Qin Hu ^a and Chun-Xiang Wang ^a

^aSchool of Materials Science and Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, People's Republic of China
^*Correspondence e-mail: jxlzfeng@163.com

Edited by M. Gdaniec, Adam Mickiewicz University, Poland (Received 5 November 2014; accepted 8 November 2014; online 15 November 2014)

In the title coordination polymer, [Dy₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]_n, the asymmetric unit consists of one Dy³⁺ cation, one half of an adipate anion, two halves of oxalate anions and one coordinating water molecule. The adipate and oxalate ions are located on centres of inversion. The Dy³⁺ cation has a distorted tricapped trigonal–prismatic geometry and is coordinated by nine O atoms, four belonging to three adipate anions, four to two oxalate anions and one from an aqua ligand. The cations are bridged by adipate ligands, generating a two-dimensional network parallel to (010). This network is further extended into three dimensions by coordination of the rigid oxalate ligands and is further consolidated by O—H⋯O hydrogen bonds. A part of the adipate anion is disordered over two positions in a 0.75:0.25 ratio.

Keywords: crystal structure; dysprosium(III) complex; three-dimensional coordination polymer; oxalate; adipate.

CCDC reference: 1033325

1. Related literature

For the isotypic structures of La, Sm and Gd complexes, see: Dan et al. (2005 ); Li & Wang (2010 ); Li (2011 ).

2. Experimental

2.1. Crystal data

[Dy₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]
M_r = 681.20
Triclinic, $[P \overline 1]$
a = 6.772 (2) Å
b = 6.929 (2) Å
c = 8.949 (3) Å
α = 104.916 (5)°
β = 108.069 (4)°
γ = 104.306 (4)°
V = 360.5 (2) Å³
Z = 1
Mo Kα radiation
μ = 10.37 mm⁻¹
T = 295 K
0.21 × 0.09 × 0.07 mm

2.2. Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.245, T_max = 0.531
1813 measured reflections
1234 independent reflections
1179 reflections with I > 2σ(I)
R_int = 0.014

2.3. Refinement

R[F² > 2σ(F²)] = 0.021
wR(F²) = 0.057
S = 1.05
1234 reflections
122 parameters
H-atom parameters constrained
Δρ_max = 1.41 e Å⁻³
Δρ_min = −1.45 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O3ⁱ	0.85	1.96	2.787 (4)	166
O7—H7B⋯O6ⁱⁱ	0.85	2.10	2.883 (5)	153
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x, -y+1, -z.

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

CCDC reference: 1033325

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536814024544/gk2622sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814024544/gk2622Isup2.hkl

checkCIF report

Structural commentary top

The title compound is isostructural with [M₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂] [M = La, Sm, Gd] (Dan et al., 2005; Li & Wang, 2010; Li, 2011). the asymmetric unit consists of one Dy³⁺ cation, a half of adipate anion, two half of oxalate anions and one aqua ligand (Fig. 1). The Dy atom is each coordinated by nine oxygen atoms, in which four oxygen atoms are from three adipate anions, four from two oxalate anions and one from a water molecule, to form a DyO₉ polyhedron of a distorted tricapped trigonal-prismatic geometry. In the title complex, the adipate anions are located on a centre of symmetry and atom C3 is positionally disordered (C3A and C3B sites; occupancies 0.75/0.25). The adipate ligands act in a η²,µ₃-η²,µ₃-chelating-bridging octadentate coordination modes and link the DyO₉ polyhedra into layers parallel to (010), in which the adjacent Dy···Dy distances are 4.20 (2) Å and 4.223 (9) Å, respectively. In the title complex, two symmetry independent oxalate ions are also located on centres of inversion and act as double bidentate (tetradentate) ligands in a zigzag chain along [001]. Through the oxalate and adipate ligands bridging interactions, the Dy atoms build up three-dimensional framework. The aqua ligand provides hydrogen-bond donors form hydrogen bonds with oxalate atoms O3 and O6.

The structure of the title complex is similar to that of other lanthanide (gadolinium, samarium and lanthanum) coordination polymers with adipate and oxalate ligands, and the mean Dy—O distance in the title complex of 2.438 Å is shorter than that of Ga—O (2.463 Å), Sm—O (2.482 Å) and La—O (2.566 Å).

Synthesis and crystallization top

A mixture of DyCl₃·6H₂O(1.00 mmol, 0.38 g), oxalic acid (0.50 mmol, 0.05 g), adipic acid (0.50 mmol, 0.07 g), NaOH (2.00 mmol, 0.08 g) and H₂O (10.0 ml) was heated in a 23 ml stainless steel reactor with a Teflon liner at 443 K for 48 h. A small amount of colorless plate-like crystals were filtered and washed with water and acetone. Yield 5% based on Dy.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. Atom C3 of the adipate anion is positionally disordered (C3A and C3B) and these atoms were refined with occupancies of 0.75/0.25. The C-bound H atoms were included in calculated positions and treated as riding atoms: C–H = 0.97 Å and U_iso(H) = 1.2U_eq(C)]. The water H-atoms were located in difference Fourier maps and were refined with distance restraints: O—H distance of 0.85 Å and U_iso(H) = 1.5U_eq(O). The highest density peak and deepest hole are located at 0.95 Å and 0.87 Å from the Dy atom, respectively.

Related literature top

For the isotypic structures of La, Sm and Gd complexes, see: Dan et al. (2005); Li & Wang (20101); Li (2011).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig.1.The fragment of the structure of the title compounds, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. Symmetry code: (i) -x, 1 - y, 1 - z; (ii) 1 - x, 1 - y, 1 - z; (iii) -x, - y, 1- z; (iv) - x, - y, -z; (v) 1 - x, 1 - y, 2 - z.

Poly[µ₆-adipato-diaquadi-µ₂-oxalato-didysprosium(III)] top

Crystal data top

[Dy₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]	Z = 1
M_r = 681.20	F(000) = 316
Triclinic, P1	D_x = 3.138 Mg m⁻³
Hall symbol: -p 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.772 (2) Å	Cell parameters from 198 reflections
b = 6.929 (2) Å	θ = 4.6–28.3°
c = 8.949 (3) Å	µ = 10.37 mm⁻¹
α = 104.916 (5)°	T = 295 K
β = 108.069 (4)°	Plate, colorless
γ = 104.306 (4)°	0.21 × 0.09 × 0.07 mm
V = 360.5 (2) Å³

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	1234 independent reflections
Radiation source: fine-focus sealed tube	1179 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.014
ϕ and ω scans	θ_max = 25.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −8→7
T_min = 0.245, T_max = 0.531	k = −6→8
1813 measured reflections	l = −10→7

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.021	H-atom parameters constrained
wR(F²) = 0.057	w = 1/[σ²(F_o²) + (0.0422P)² + 0.1716P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max < 0.001
1234 reflections	Δρ_max = 1.41 e Å⁻³
122 parameters	Δρ_min = −1.45 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0039 (11)

Crystal data top

[Dy₂(C₆H₈O₄)(C₂O₄)₂(H₂O)₂]	γ = 104.306 (4)°
M_r = 681.20	V = 360.5 (2) Å³
Triclinic, P1	Z = 1
a = 6.772 (2) Å	Mo Kα radiation
b = 6.929 (2) Å	µ = 10.37 mm⁻¹
c = 8.949 (3) Å	T = 295 K
α = 104.916 (5)°	0.21 × 0.09 × 0.07 mm
β = 108.069 (4)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	1234 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	1179 reflections with I > 2σ(I)
T_min = 0.245, T_max = 0.531	R_int = 0.014
1813 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.021	0 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.05	Δρ_max = 1.41 e Å⁻³
1234 reflections	Δρ_min = −1.45 e Å⁻³
122 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Dy	0.15576 (3)	0.34496 (3)	0.36280 (2)	0.01182 (14)
O1	0.1519 (6)	0.5222 (6)	0.6470 (4)	0.0145 (7)
O2	0.4801 (6)	0.5972 (6)	0.6395 (4)	0.0162 (8)
O3	0.2699 (6)	0.1546 (6)	0.5391 (4)	0.0154 (8)
O4	0.1535 (6)	−0.0812 (6)	0.6512 (5)	0.0181 (8)
O5	−0.0072 (6)	0.2564 (6)	0.0712 (4)	0.0172 (8)
O6	−0.1314 (7)	0.0203 (6)	−0.1913 (5)	0.0201 (8)
O7	0.2677 (6)	0.6848 (6)	0.3381 (5)	0.0206 (8)
H7A	0.4060	0.7539	0.3786	0.031*
H7B	0.1863	0.7472	0.2931	0.031*
C1	0.3632 (9)	0.6131 (8)	0.7234 (6)	0.0135 (11)
C2	0.4635 (9)	0.7252 (9)	0.9114 (7)	0.0178 (12)
H2A	0.3960	0.8298	0.9403	0.021*
H2B	0.6211	0.8016	0.9479	0.021*
C3A	0.4334 (12)	0.5740 (12)	1.0066 (9)	0.0162 (14)	0.75
H3A1	0.2770	0.4877	0.9624	0.019*	0.75
H3A2	0.4788	0.6577	1.1245	0.019*	0.75
C3B	0.576 (4)	0.593 (4)	1.005 (3)	0.0162 (14)	0.25
H3B1	0.6770	0.5536	0.9564	0.019*	0.25
H3B2	0.6640	0.6824	1.1227	0.019*	0.25
C4	0.1215 (8)	0.0215 (7)	0.5549 (6)	0.0127 (10)
C5	−0.0395 (8)	0.0806 (8)	−0.0350 (7)	0.0150 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy	0.01277 (19)	0.01272 (18)	0.01252 (19)	0.00465 (11)	0.00650 (12)	0.00663 (11)
O1	0.0132 (17)	0.0169 (18)	0.0168 (18)	0.0054 (14)	0.0085 (15)	0.0081 (14)
O2	0.0179 (19)	0.0165 (19)	0.0181 (19)	0.0061 (15)	0.0117 (16)	0.0070 (14)
O3	0.0135 (18)	0.0175 (19)	0.0164 (18)	0.0052 (15)	0.0049 (15)	0.0093 (15)
O4	0.0134 (18)	0.022 (2)	0.0213 (19)	0.0068 (15)	0.0054 (15)	0.0131 (16)
O5	0.0220 (19)	0.0161 (19)	0.0167 (19)	0.0095 (15)	0.0092 (16)	0.0062 (15)
O6	0.027 (2)	0.022 (2)	0.014 (2)	0.0111 (17)	0.0083 (17)	0.0095 (16)
O7	0.0178 (19)	0.020 (2)	0.031 (2)	0.0080 (16)	0.0105 (17)	0.0177 (17)
C1	0.021 (3)	0.008 (2)	0.015 (3)	0.009 (2)	0.007 (2)	0.0074 (19)
C2	0.017 (3)	0.019 (3)	0.019 (3)	0.006 (2)	0.009 (2)	0.007 (2)
C3A	0.017 (3)	0.029 (4)	0.013 (3)	0.013 (3)	0.010 (3)	0.012 (3)
C3B	0.017 (3)	0.029 (4)	0.013 (3)	0.013 (3)	0.010 (3)	0.012 (3)
C4	0.018 (3)	0.008 (2)	0.015 (2)	0.0022 (19)	0.011 (2)	0.0058 (19)
C5	0.012 (2)	0.019 (3)	0.019 (3)	0.007 (2)	0.009 (2)	0.009 (2)

Geometric parameters (Å, º) top

Dy—O5	2.336 (4)	O7—H7A	0.8468
Dy—O4ⁱ	2.360 (4)	O7—H7B	0.8496
Dy—O3	2.376 (4)	C1—C2	1.501 (7)
Dy—O7	2.379 (4)	C2—C3A	1.525 (9)
Dy—O2ⁱⁱ	2.406 (3)	C2—C3B	1.57 (2)
Dy—O1ⁱⁱⁱ	2.464 (4)	C2—H2A	0.9700
Dy—O6^iv	2.535 (4)	C2—H2B	0.9700
Dy—O1	2.535 (3)	C3A—C3A^v	1.529 (14)
Dy—O2	2.552 (4)	C3A—H3A1	0.9700
O1—C1	1.279 (7)	C3A—H3A2	0.9700
O2—C1	1.255 (6)	C3B—C3B^v	1.40 (4)
O3—C4	1.256 (6)	C3B—H3B1	0.9700
O4—C4	1.253 (6)	C3B—H3B2	0.9700
O5—C5	1.256 (6)	C4—C4ⁱ	1.538 (10)
O6—C5	1.245 (7)	C5—C5^iv	1.540 (11)
O6—Dy^iv	2.535 (4)

O5—Dy—O4ⁱ	90.45 (13)	C1—O1—Dy	95.2 (3)
O5—Dy—O3	134.27 (12)	Dyⁱⁱⁱ—O1—Dy	115.28 (14)
O4ⁱ—Dy—O3	68.93 (12)	C1—O2—Dyⁱⁱ	148.4 (3)
O5—Dy—O7	78.20 (13)	C1—O2—Dy	95.1 (3)
O4ⁱ—Dy—O7	142.35 (13)	Dyⁱⁱ—O2—Dy	115.66 (13)
O3—Dy—O7	141.46 (12)	C4—O3—Dy	117.8 (3)
O5—Dy—O2ⁱⁱ	91.79 (12)	C4—O4—Dyⁱ	118.7 (3)
O4ⁱ—Dy—O2ⁱⁱ	142.20 (13)	C5—O5—Dy	123.8 (3)
O3—Dy—O2ⁱⁱ	82.95 (12)	C5—O6—Dy^iv	117.5 (3)
O7—Dy—O2ⁱⁱ	74.65 (13)	Dy—O7—H7A	116.9
O5—Dy—O1ⁱⁱⁱ	82.15 (12)	Dy—O7—H7B	128.4
O4ⁱ—Dy—O1ⁱⁱⁱ	69.07 (12)	H7A—O7—H7B	114.8
O3—Dy—O1ⁱⁱⁱ	122.91 (11)	O2—C1—O1	118.8 (5)
O7—Dy—O1ⁱⁱⁱ	73.84 (12)	O2—C1—C2	122.2 (5)
O2ⁱⁱ—Dy—O1ⁱⁱⁱ	148.49 (12)	O1—C1—C2	119.0 (4)
O5—Dy—O6^iv	65.84 (12)	O2—C1—Dy	59.8 (3)
O4ⁱ—Dy—O6^iv	70.76 (13)	O1—C1—Dy	59.1 (2)
O3—Dy—O6^iv	68.84 (12)	C2—C1—Dy	173.1 (4)
O7—Dy—O6^iv	132.07 (13)	C1—C2—C3A	113.3 (5)
O2ⁱⁱ—Dy—O6^iv	75.88 (12)	C1—C2—C3B	111.8 (9)
O1ⁱⁱⁱ—Dy—O6^iv	127.55 (12)	C1—C2—H2A	108.9
O5—Dy—O1	146.78 (12)	C3A—C2—H2A	108.9
O4ⁱ—Dy—O1	80.36 (12)	C3B—C2—H2A	134.9
O3—Dy—O1	71.64 (12)	C1—C2—H2B	108.9
O7—Dy—O1	89.76 (13)	C3A—C2—H2B	108.9
O2ⁱⁱ—Dy—O1	114.93 (11)	C3B—C2—H2B	76.5
O1ⁱⁱⁱ—Dy—O1	64.72 (14)	H2A—C2—H2B	107.7
O6^iv—Dy—O1	137.19 (12)	C2—C3A—C3A^v	113.2 (7)
O5—Dy—O2	146.25 (12)	C2—C3A—H3A1	108.9
O4ⁱ—Dy—O2	123.15 (12)	C3A^v—C3A—H3A1	108.9
O3—Dy—O2	69.30 (12)	C2—C3A—H3A2	108.9
O7—Dy—O2	72.79 (13)	C3A^v—C3A—H3A2	108.9
O2ⁱⁱ—Dy—O2	64.34 (13)	H3A1—C3A—H3A2	107.8
O1ⁱⁱⁱ—Dy—O2	105.43 (11)	C3B^v—C3B—C2	113 (2)
O6^iv—Dy—O2	124.52 (12)	C3B^v—C3B—H3B1	108.9
O1—Dy—O2	50.76 (11)	C2—C3B—H3B1	108.9
O5—Dy—C1	158.48 (13)	C3B^v—C3B—H3B2	108.9
O4ⁱ—Dy—C1	101.76 (14)	C2—C3B—H3B2	108.9
O3—Dy—C1	67.18 (13)	H3B1—C3B—H3B2	107.7
O7—Dy—C1	81.38 (14)	O4—C4—O3	125.9 (5)
O2ⁱⁱ—Dy—C1	89.29 (13)	O4—C4—C4ⁱ	116.9 (5)
O1ⁱⁱⁱ—Dy—C1	85.74 (13)	O3—C4—C4ⁱ	117.2 (5)
O6^iv—Dy—C1	134.90 (13)	O6—C5—O5	127.2 (5)
O1—Dy—C1	25.66 (13)	O6—C5—C5^iv	116.0 (6)
O2—Dy—C1	25.14 (13)	O5—C5—C5^iv	116.8 (6)
C1—O1—Dyⁱⁱⁱ	132.5 (3)

O5—Dy—O1—C1	−138.0 (3)	O1ⁱⁱⁱ—Dy—O5—C5	−135.5 (4)
O4ⁱ—Dy—O1—C1	146.2 (3)	O6^iv—Dy—O5—C5	1.9 (4)
O3—Dy—O1—C1	75.4 (3)	O1—Dy—O5—C5	−139.6 (4)
O7—Dy—O1—C1	−70.3 (3)	O2—Dy—O5—C5	118.4 (4)
O2ⁱⁱ—Dy—O1—C1	2.6 (3)	C1—Dy—O5—C5	168.2 (4)
O1ⁱⁱⁱ—Dy—O1—C1	−142.5 (4)	Dyⁱⁱ—O2—C1—O1	−171.1 (4)
O6^iv—Dy—O1—C1	98.7 (3)	Dy—O2—C1—O1	−4.5 (5)
O2—Dy—O1—C1	−2.5 (3)	Dyⁱⁱ—O2—C1—C2	5.7 (9)
O5—Dy—O1—Dyⁱⁱⁱ	4.5 (3)	Dy—O2—C1—C2	172.3 (4)
O4ⁱ—Dy—O1—Dyⁱⁱⁱ	−71.31 (15)	Dyⁱⁱ—O2—C1—Dy	−166.6 (6)
O3—Dy—O1—Dyⁱⁱⁱ	−142.17 (17)	Dyⁱⁱⁱ—O1—C1—O2	−127.1 (4)
O7—Dy—O1—Dyⁱⁱⁱ	72.19 (15)	Dy—O1—C1—O2	4.5 (5)
O2ⁱⁱ—Dy—O1—Dyⁱⁱⁱ	145.10 (14)	Dyⁱⁱⁱ—O1—C1—C2	56.0 (6)
O1ⁱⁱⁱ—Dy—O1—Dyⁱⁱⁱ	0.0	Dy—O1—C1—C2	−172.3 (4)
O6^iv—Dy—O1—Dyⁱⁱⁱ	−118.82 (18)	Dyⁱⁱⁱ—O1—C1—Dy	−131.7 (4)
O2—Dy—O1—Dyⁱⁱⁱ	139.9 (2)	O5—Dy—C1—O2	−86.1 (5)
C1—Dy—O1—Dyⁱⁱⁱ	142.5 (4)	O4ⁱ—Dy—C1—O2	150.6 (3)
O5—Dy—O2—C1	138.8 (3)	O3—Dy—C1—O2	89.7 (3)
O4ⁱ—Dy—O2—C1	−35.1 (3)	O7—Dy—C1—O2	−67.6 (3)
O3—Dy—O2—C1	−80.2 (3)	O2ⁱⁱ—Dy—C1—O2	7.0 (3)
O7—Dy—O2—C1	106.9 (3)	O1ⁱⁱⁱ—Dy—C1—O2	−141.9 (3)
O2ⁱⁱ—Dy—O2—C1	−172.2 (4)	O6^iv—Dy—C1—O2	76.1 (3)
O1ⁱⁱⁱ—Dy—O2—C1	39.7 (3)	O1—Dy—C1—O2	−175.4 (5)
O6^iv—Dy—O2—C1	−123.4 (3)	O5—Dy—C1—O1	89.3 (5)
O1—Dy—O2—C1	2.6 (3)	O4ⁱ—Dy—C1—O1	−34.1 (3)
O5—Dy—O2—Dyⁱⁱ	−49.0 (3)	O3—Dy—C1—O1	−95.0 (3)
O4ⁱ—Dy—O2—Dyⁱⁱ	137.16 (15)	O7—Dy—C1—O1	107.8 (3)
O3—Dy—O2—Dyⁱⁱ	92.06 (16)	O2ⁱⁱ—Dy—C1—O1	−177.6 (3)
O7—Dy—O2—Dyⁱⁱ	−80.87 (16)	O1ⁱⁱⁱ—Dy—C1—O1	33.5 (3)
O2ⁱⁱ—Dy—O2—Dyⁱⁱ	0.001 (1)	O6^iv—Dy—C1—O1	−108.5 (3)
O1ⁱⁱⁱ—Dy—O2—Dyⁱⁱ	−148.06 (15)	O2—Dy—C1—O1	175.4 (5)
O6^iv—Dy—O2—Dyⁱⁱ	48.8 (2)	O2—C1—C2—C3A	−110.4 (6)
O1—Dy—O2—Dyⁱⁱ	174.8 (2)	O1—C1—C2—C3A	66.3 (7)
C1—Dy—O2—Dyⁱⁱ	172.2 (4)	O2—C1—C2—C3B	−71.7 (11)
O5—Dy—O3—C4	−74.6 (4)	O1—C1—C2—C3B	105.1 (10)
O4ⁱ—Dy—O3—C4	−5.9 (3)	C1—C2—C3A—C3A^v	68.2 (9)
O7—Dy—O3—C4	145.5 (3)	C3B—C2—C3A—C3A^v	−27.2 (14)
O2ⁱⁱ—Dy—O3—C4	−160.2 (3)	C1—C2—C3B—C3B^v	−70 (2)
O1ⁱⁱⁱ—Dy—O3—C4	39.2 (4)	C3A—C2—C3B—C3B^v	29.9 (15)
O6^iv—Dy—O3—C4	−82.6 (3)	Dyⁱ—O4—C4—O3	−174.4 (4)
O1—Dy—O3—C4	80.6 (3)	Dyⁱ—O4—C4—C4ⁱ	4.9 (7)
O2—Dy—O3—C4	134.6 (4)	Dy—O3—C4—O4	−175.0 (4)
C1—Dy—O3—C4	107.6 (4)	Dy—O3—C4—C4ⁱ	5.8 (7)
O4ⁱ—Dy—O5—C5	−66.7 (4)	Dy^iv—O6—C5—O5	178.5 (4)
O3—Dy—O5—C5	−6.3 (5)	Dy^iv—O6—C5—C5^iv	−2.6 (7)
O7—Dy—O5—C5	149.5 (4)	Dy—O5—C5—O6	177.5 (4)
O2ⁱⁱ—Dy—O5—C5	75.6 (4)	Dy—O5—C5—C5^iv	−1.4 (7)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O3ⁱⁱ	0.85	1.96	2.787 (4)	166
O7—H7B···O6^vi	0.85	2.10	2.883 (5)	153

Symmetry codes: (ii) −x+1, −y+1, −z+1; (vi) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O3ⁱ	0.85	1.96	2.787 (4)	166
O7—H7B···O6ⁱⁱ	0.85	2.10	2.883 (5)	153

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (51372104), the Natural Science Foundation of Jiangxi Province (2010GQC0064), the Science and Technology Support Fundation of Jiangxi Province (2012BBE500038, 20141BBE50019) and the Jiangxi University of Science and Technology Foundation (3304000027).

References

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Volume 70| Part 12| December 2014| Pages m399-m400

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