Literature DB >> 21754674

Bis(μ-2-{[2-(1,3-benzothia-zol-2-yl)hydrazinyl-idene]meth-yl}-6-meth-oxy-phenolato)bis-[dinitratodysprosium(III)] methanol disolvate.

Xuebin Xu, Shuai Ding, Si Shen, Jinkui Tang, Zhiliang Liu.   

Abstract

In the centrosymmetric dinuclear title compound, [Dy(2)(C(15)H(12)N(3)O(2)S)(2)(NO(3))(4)]·2CH(3)OH, the two Dy(III) atoms are coordinated by two deprotonated 2-{[2-(1,3-benzothia-zol-2-yl)hydrazinyl-idene]meth-yl}-6-meth-oxy-phenol ligands and four nitrate ions, all of which are chelating. The crystal packing is stabilized by inter-molecular N-H⋯O hydrogen bonds and weak O-H⋯O inter-actions, forming a two-dimensional network parallel to (010).

Entities:  

Year:  2011        PMID: 21754674      PMCID: PMC3120308          DOI: 10.1107/S1600536811019118

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For applications of dysprosium complexes in data storage and processing, see: Lin et al. (2010 ▶). For the preparation of the 2-{[2-(1,3-benzothia­zol-2-yl)hydrazinyl­idene]meth­yl}-6-meth­oxy­phenol ligand, see: Patil et al. (2009 ▶). For related structures, see: Lin & Hong (2009 ▶); Lin et al. (2008 ▶); Xu et al. (2010 ▶).

Experimental

Crystal data

[Dy2(C15H12N3O2S)2(NO3)4]·2CH4O M = 1233.82 Triclinic, a = 9.6191 (6) Å b = 10.1002 (7) Å c = 11.6151 (8) Å α = 112.045 (1)° β = 105.065 (1)° γ = 93.154 (1)° V = 995.23 (12) Å3 Z = 1 Mo Kα radiation μ = 3.92 mm−1 T = 159 K 0.20 × 0.10 × 0.10 mm

Data collection

Rigaku Saturn CCD area-detector diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2002 ▶) T min = 0.631, T max = 0.676 5083 measured reflections 3502 independent reflections 3162 reflections with I > 2σ(I) R int = 0.016

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.057 S = 1.07 3502 reflections 292 parameters H-atom parameters constrained Δρmax = 0.83 e Å−3 Δρmin = −0.51 e Å−3 Data collection: CrystalClear (Rigaku, 2002 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2006 ▶) and XP (Siemens, 1994 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811019118/jj2083sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811019118/jj2083Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Dy2(C15H12N3O2S)2(NO3)4]·2CH4OZ = 1
Mr = 1233.82F(000) = 602
Triclinic, P1Dx = 2.059 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.6191 (6) ÅCell parameters from 3776 reflections
b = 10.1002 (7) Åθ = 2.3–25.1°
c = 11.6151 (8) ŵ = 3.92 mm1
α = 112.045 (1)°T = 159 K
β = 105.065 (1)°Block, yellow
γ = 93.154 (1)°0.20 × 0.10 × 0.10 mm
V = 995.23 (12) Å3
Rigaku Saturn CCD area-detector diffractometer3502 independent reflections
Radiation source: rotating anode3162 reflections with I > 2σ(I)
confocalRint = 0.016
Detector resolution: 7.31 pixels mm-1θmax = 25.1°, θmin = 2.0°
ω and φ scansh = −11→11
Absorption correction: multi-scan (CrystalClear; Rigaku, 2002)k = −12→7
Tmin = 0.631, Tmax = 0.676l = −13→13
5083 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.0289P)2 + 0.127P] where P = (Fo2 + 2Fc2)/3
3502 reflections(Δ/σ)max = 0.001
292 parametersΔρmax = 0.83 e Å3
0 restraintsΔρmin = −0.51 e Å3
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.
xyzUiso*/Ueq
C10.5488 (5)−0.1481 (6)1.3423 (4)0.0419 (12)
H1A0.4829−0.09891.38950.063*
H1B0.6488−0.09461.38760.063*
H1C0.5453−0.24681.33870.063*
C20.3550 (4)−0.2085 (4)1.1420 (4)0.0262 (9)
C30.2744 (5)−0.3007 (5)1.1704 (4)0.0328 (10)
H30.3194−0.33231.23630.039*
C40.1277 (5)−0.3481 (5)1.1034 (4)0.0349 (10)
H40.0711−0.41431.12080.042*
C50.0654 (4)−0.2974 (5)1.0113 (4)0.0314 (10)
H5−0.0365−0.32630.96770.038*
C60.1455 (4)−0.2054 (4)0.9789 (4)0.0259 (9)
C70.2972 (4)−0.1615 (4)1.0421 (4)0.0237 (8)
C80.0613 (4)−0.1613 (5)0.8805 (4)0.0308 (10)
H8−0.0395−0.20250.84230.037*
C90.0364 (4)0.0701 (5)0.7244 (4)0.0285 (9)
C100.1564 (4)0.2767 (4)0.7467 (4)0.0265 (9)
C110.2636 (4)0.3998 (5)0.7988 (4)0.0309 (10)
H110.35300.40750.86170.037*
C120.2378 (5)0.5099 (5)0.7573 (4)0.0335 (10)
H120.31120.59300.79040.040*
C130.1059 (5)0.5011 (5)0.6680 (4)0.0354 (10)
H130.09020.57910.64210.042*
C14−0.0026 (5)0.3818 (5)0.6163 (4)0.0335 (10)
H14−0.09300.37640.55570.040*
C150.0251 (4)0.2701 (5)0.6558 (4)0.0284 (9)
C160.2951 (6)0.3287 (6)0.4354 (5)0.0540 (14)
H16A0.25850.38620.38580.081*
H16C0.39780.36820.48620.081*
H16B0.23740.33260.49450.081*
Dy10.358298 (18)0.05304 (2)0.890365 (17)0.02346 (8)
N40.1097 (3)−0.0726 (4)0.8405 (3)0.0283 (8)
N50.1632 (3)0.1587 (4)0.7829 (3)0.0274 (8)
N60.3542 (4)0.3093 (4)1.1063 (3)0.0345 (9)
N70.3601 (4)−0.1898 (4)0.6517 (3)0.0327 (8)
N90.0038 (3)−0.0478 (4)0.7456 (3)0.0327 (8)
H9−0.0802−0.10700.70200.039*
O10.5034 (3)−0.1543 (3)1.2102 (3)0.0291 (6)
O20.3863 (3)−0.0823 (3)1.0113 (2)0.0249 (6)
O30.2717 (3)0.1897 (3)1.0724 (3)0.0340 (7)
O40.4335 (3)0.3079 (3)1.0330 (3)0.0337 (7)
O50.3585 (4)0.4152 (4)1.2012 (3)0.0574 (10)
O60.2613 (3)−0.1127 (3)0.6575 (3)0.0371 (7)
O70.3620 (4)−0.2850 (4)0.5512 (3)0.0580 (10)
O80.4579 (3)−0.1600 (3)0.7589 (3)0.0416 (8)
O90.2828 (3)0.1836 (4)0.3486 (3)0.0452 (8)
H9A0.33980.17900.30380.068*
S1−0.09430 (11)0.11034 (12)0.61321 (10)0.0315 (2)
U11U22U33U12U13U23
C10.033 (2)0.062 (3)0.028 (2)0.002 (2)0.0030 (19)0.020 (2)
C20.021 (2)0.029 (2)0.027 (2)0.0045 (17)0.0058 (17)0.0110 (18)
C30.036 (2)0.029 (2)0.033 (2)0.006 (2)0.0075 (19)0.014 (2)
C40.033 (2)0.033 (2)0.041 (3)0.002 (2)0.011 (2)0.017 (2)
C50.022 (2)0.035 (2)0.034 (2)0.0027 (18)0.0075 (18)0.011 (2)
C60.0188 (19)0.028 (2)0.030 (2)0.0037 (17)0.0051 (17)0.0118 (18)
C70.0183 (19)0.022 (2)0.028 (2)0.0031 (16)0.0038 (16)0.0095 (18)
C80.016 (2)0.037 (3)0.033 (2)0.0030 (18)0.0006 (17)0.013 (2)
C90.019 (2)0.037 (2)0.028 (2)0.0086 (18)0.0036 (17)0.013 (2)
C100.023 (2)0.032 (2)0.024 (2)0.0070 (18)0.0049 (17)0.0117 (18)
C110.022 (2)0.039 (3)0.030 (2)0.0060 (19)0.0039 (17)0.014 (2)
C120.029 (2)0.035 (2)0.032 (2)0.003 (2)0.0046 (19)0.012 (2)
C130.039 (2)0.039 (3)0.031 (2)0.011 (2)0.006 (2)0.019 (2)
C140.031 (2)0.042 (3)0.028 (2)0.012 (2)0.0021 (19)0.019 (2)
C150.020 (2)0.038 (2)0.022 (2)0.0059 (18)0.0028 (16)0.0086 (19)
C160.043 (3)0.069 (4)0.044 (3)0.009 (3)0.011 (2)0.018 (3)
Dy10.01390 (10)0.03118 (12)0.02375 (11)0.00321 (8)0.00021 (7)0.01318 (9)
N40.0175 (16)0.033 (2)0.0301 (18)−0.0005 (15)−0.0019 (14)0.0156 (16)
N50.0207 (17)0.0310 (19)0.0281 (18)0.0054 (15)0.0046 (14)0.0110 (16)
N60.033 (2)0.039 (2)0.029 (2)0.0144 (18)0.0035 (17)0.0152 (19)
N70.0199 (18)0.036 (2)0.031 (2)0.0019 (16)−0.0010 (15)0.0067 (18)
N90.0144 (16)0.045 (2)0.0347 (19)−0.0018 (16)−0.0072 (14)0.0229 (18)
O10.0195 (13)0.0415 (17)0.0277 (15)0.0034 (13)0.0010 (11)0.0199 (14)
O20.0146 (13)0.0316 (16)0.0279 (14)0.0016 (12)0.0007 (11)0.0156 (13)
O30.0291 (16)0.0430 (19)0.0312 (16)0.0091 (15)0.0063 (13)0.0177 (15)
O40.0285 (15)0.0393 (18)0.0298 (15)0.0044 (14)0.0036 (13)0.0138 (14)
O50.086 (3)0.041 (2)0.041 (2)0.021 (2)0.0250 (19)0.0073 (18)
O60.0229 (15)0.0449 (19)0.0318 (16)0.0119 (14)−0.0016 (13)0.0087 (15)
O70.0373 (19)0.066 (3)0.037 (2)0.0132 (18)−0.0008 (16)−0.0066 (19)
O80.0351 (17)0.0463 (19)0.0321 (16)0.0152 (15)−0.0033 (14)0.0117 (15)
O90.0258 (17)0.057 (2)0.046 (2)−0.0010 (16)0.0079 (14)0.0163 (18)
S10.0212 (5)0.0388 (6)0.0302 (5)0.0037 (5)−0.0020 (4)0.0161 (5)
C1—O11.459 (5)C13—H130.9500
C1—H1A0.9800C14—C151.384 (6)
C1—H1B0.9800C14—H140.9500
C1—H1C0.9800C15—S11.752 (4)
C2—C31.364 (6)C16—O91.410 (6)
C2—O11.402 (4)C16—H16A0.9800
C2—C71.410 (5)C16—H16C0.9800
C3—C41.379 (6)C16—H16B0.9800
C3—H30.9500Dy1—O22.280 (3)
C4—C51.370 (6)Dy1—O2i2.374 (2)
C4—H40.9500Dy1—O1i2.394 (3)
C5—C61.390 (5)Dy1—O42.422 (3)
C5—H50.9500Dy1—O32.433 (3)
C6—C71.412 (5)Dy1—N42.461 (3)
C6—C81.451 (5)Dy1—O62.471 (3)
C7—O21.342 (4)Dy1—N52.494 (3)
C8—N41.270 (5)Dy1—O82.530 (3)
C8—H80.9500Dy1—Dy1i3.7184 (4)
C9—N51.320 (5)N4—N91.402 (4)
C9—N91.340 (5)N6—O51.203 (5)
C9—S11.738 (4)N6—O31.273 (5)
C10—C111.395 (6)N6—O41.279 (4)
C10—C151.399 (5)N7—O71.208 (5)
C10—N51.405 (5)N7—O61.261 (4)
C11—C121.379 (6)N7—O81.266 (4)
C11—H110.9500N9—H90.8800
C12—C131.388 (6)O1—Dy1i2.394 (3)
C12—H120.9500O2—Dy1i2.374 (2)
C13—C141.376 (6)O9—H9A0.8400
O1—C1—H1A109.5O4—Dy1—O352.63 (10)
O1—C1—H1B109.5O2—Dy1—N475.53 (10)
H1A—C1—H1B109.5O2i—Dy1—N4149.07 (10)
O1—C1—H1C109.5O1i—Dy1—N4138.80 (10)
H1A—C1—H1C109.5O4—Dy1—N4121.11 (11)
H1B—C1—H1C109.5O3—Dy1—N474.17 (11)
C3—C2—O1122.0 (4)O2—Dy1—O6108.45 (10)
C3—C2—C7123.2 (4)O2i—Dy1—O6116.45 (9)
O1—C2—C7114.8 (3)O1i—Dy1—O676.95 (10)
C2—C3—C4120.1 (4)O4—Dy1—O6141.79 (10)
C2—C3—H3120.0O3—Dy1—O6139.92 (10)
C4—C3—H3120.0N4—Dy1—O669.16 (10)
C5—C4—C3118.5 (4)O2—Dy1—N5139.17 (10)
C5—C4—H4120.8O2i—Dy1—N5144.17 (10)
C3—C4—H4120.8O1i—Dy1—N581.46 (10)
C4—C5—C6122.6 (4)O4—Dy1—N579.22 (10)
C4—C5—H5118.7O3—Dy1—N579.08 (10)
C6—C5—H5118.7N4—Dy1—N566.52 (11)
C5—C6—C7119.6 (4)O6—Dy1—N572.05 (10)
C5—C6—C8115.0 (4)O2—Dy1—O877.32 (10)
C7—C6—C8125.3 (4)O2i—Dy1—O870.22 (9)
O2—C7—C2119.8 (3)O1i—Dy1—O876.42 (10)
O2—C7—C6124.3 (3)O4—Dy1—O8140.65 (10)
C2—C7—C6115.8 (3)O3—Dy1—O8153.86 (10)
N4—C8—C6126.1 (4)N4—Dy1—O898.23 (11)
N4—C8—H8117.0O6—Dy1—O850.52 (9)
C6—C8—H8117.0N5—Dy1—O8121.51 (10)
N5—C9—N9123.9 (4)O2—Dy1—Dy1i37.86 (6)
N5—C9—S1117.3 (3)O2i—Dy1—Dy1i36.10 (6)
N9—C9—S1118.8 (3)O1i—Dy1—Dy1i103.10 (6)
C11—C10—C15119.0 (4)O4—Dy1—Dy1i92.27 (7)
C11—C10—N5125.8 (3)O3—Dy1—Dy1i90.23 (7)
C15—C10—N5115.2 (4)N4—Dy1—Dy1i113.24 (8)
C12—C11—C10118.9 (4)O6—Dy1—Dy1i118.59 (7)
C12—C11—H11120.6N5—Dy1—Dy1i169.00 (8)
C10—C11—H11120.6O8—Dy1—Dy1i69.47 (6)
C11—C12—C13120.9 (4)C8—N4—N9114.2 (3)
C11—C12—H12119.5C8—N4—Dy1131.6 (3)
C13—C12—H12119.5N9—N4—Dy1114.1 (2)
C14—C13—C12121.5 (4)C9—N5—C10109.1 (3)
C14—C13—H13119.3C9—N5—Dy1113.1 (3)
C12—C13—H13119.3C10—N5—Dy1136.6 (2)
C13—C14—C15117.4 (4)O5—N6—O3122.4 (4)
C13—C14—H14121.3O5—N6—O4122.6 (4)
C15—C14—H14121.3O3—N6—O4115.0 (3)
C14—C15—C10122.3 (4)O7—N7—O6122.5 (4)
C14—C15—S1127.6 (3)O7—N7—O8122.2 (4)
C10—C15—S1109.9 (3)O6—N7—O8115.2 (3)
O9—C16—H16A109.5C9—N9—N4117.0 (3)
O9—C16—H16C109.5C9—N9—H9121.5
H16A—C16—H16C109.5N4—N9—H9121.5
O9—C16—H16B109.5C2—O1—C1114.9 (3)
H16A—C16—H16B109.5C2—O1—Dy1i116.7 (2)
H16C—C16—H16B109.5C1—O1—Dy1i127.7 (2)
O2—Dy1—O2i73.96 (10)C7—O2—Dy1136.2 (2)
O2—Dy1—O1i139.27 (9)C7—O2—Dy1i117.7 (2)
O2i—Dy1—O1i68.12 (9)Dy1—O2—Dy1i106.04 (10)
O2—Dy1—O4109.76 (9)N6—O3—Dy195.9 (2)
O2i—Dy1—O474.78 (9)N6—O4—Dy196.3 (2)
O1i—Dy1—O474.29 (10)N7—O6—Dy198.6 (2)
O2—Dy1—O376.56 (10)N7—O8—Dy195.6 (2)
O2i—Dy1—O3103.27 (9)C16—O9—H9A109.5
O1i—Dy1—O3125.83 (10)C9—S1—C1588.36 (19)
O1—C2—C3—C4178.1 (4)C8—N4—N9—C9162.8 (4)
C7—C2—C3—C4−2.5 (7)Dy1—N4—N9—C9−20.4 (4)
C2—C3—C4—C5−1.7 (6)C3—C2—O1—C1−25.7 (5)
C3—C4—C5—C62.8 (7)C7—C2—O1—C1154.9 (4)
C4—C5—C6—C70.2 (6)C3—C2—O1—Dy1i162.7 (3)
C4—C5—C6—C8−179.3 (4)C7—C2—O1—Dy1i−16.7 (4)
C3—C2—C7—O2−173.5 (4)C2—C7—O2—Dy1−167.5 (3)
O1—C2—C7—O26.0 (5)C6—C7—O2—Dy113.8 (6)
C3—C2—C7—C65.3 (6)C2—C7—O2—Dy1i7.9 (5)
O1—C2—C7—C6−175.2 (3)C6—C7—O2—Dy1i−170.8 (3)
C5—C6—C7—O2174.7 (4)O2i—Dy1—O2—C7175.7 (4)
C8—C6—C7—O2−6.0 (6)O1i—Dy1—O2—C7−162.4 (3)
C5—C6—C7—C2−4.1 (6)O4—Dy1—O2—C7108.9 (3)
C8—C6—C7—C2175.3 (4)O3—Dy1—O2—C767.4 (3)
C5—C6—C8—N4176.4 (4)N4—Dy1—O2—C7−9.4 (3)
C7—C6—C8—N4−3.0 (7)O6—Dy1—O2—C7−71.2 (3)
C15—C10—C11—C12−1.1 (6)N5—Dy1—O2—C712.5 (4)
N5—C10—C11—C12−176.9 (4)O8—Dy1—O2—C7−111.5 (3)
C10—C11—C12—C131.8 (6)Dy1i—Dy1—O2—C7175.7 (4)
C11—C12—C13—C14−1.0 (7)O2i—Dy1—O2—Dy1i0.0
C12—C13—C14—C15−0.5 (6)O1i—Dy1—O2—Dy1i21.83 (19)
C13—C14—C15—C101.2 (6)O4—Dy1—O2—Dy1i−66.82 (12)
C13—C14—C15—S1176.6 (3)O3—Dy1—O2—Dy1i−108.32 (12)
C11—C10—C15—C14−0.5 (6)N4—Dy1—O2—Dy1i174.87 (13)
N5—C10—C15—C14175.8 (4)O6—Dy1—O2—Dy1i113.12 (11)
C11—C10—C15—S1−176.5 (3)N5—Dy1—O2—Dy1i−163.24 (12)
N5—C10—C15—S1−0.2 (4)O8—Dy1—O2—Dy1i72.77 (11)
C6—C8—N4—N9−179.2 (4)O5—N6—O3—Dy1−175.9 (4)
C6—C8—N4—Dy14.8 (7)O4—N6—O3—Dy13.2 (3)
O2—Dy1—N4—C80.1 (4)O2—Dy1—O3—N6126.4 (2)
O2i—Dy1—N4—C89.7 (5)O2i—Dy1—O3—N656.8 (2)
O1i—Dy1—N4—C8153.4 (3)O1i—Dy1—O3—N6−15.6 (2)
O4—Dy1—N4—C8−104.5 (4)O4—Dy1—O3—N6−1.92 (19)
O3—Dy1—N4—C8−79.8 (4)N4—Dy1—O3—N6−155.1 (2)
O6—Dy1—N4—C8116.7 (4)O6—Dy1—O3—N6−130.8 (2)
N5—Dy1—N4—C8−164.5 (4)N5—Dy1—O3—N6−86.6 (2)
O8—Dy1—N4—C874.6 (4)O8—Dy1—O3—N6128.8 (3)
Dy1i—Dy1—N4—C83.5 (4)Dy1i—Dy1—O3—N690.8 (2)
O2—Dy1—N4—N9−176.0 (3)O5—N6—O4—Dy1175.9 (4)
O2i—Dy1—N4—N9−166.4 (2)O3—N6—O4—Dy1−3.2 (3)
O1i—Dy1—N4—N9−22.7 (3)O2—Dy1—O4—N6−52.3 (2)
O4—Dy1—N4—N979.4 (3)O2i—Dy1—O4—N6−118.6 (2)
O3—Dy1—N4—N9104.2 (3)O1i—Dy1—O4—N6170.4 (2)
O6—Dy1—N4—N9−59.4 (3)O3—Dy1—O4—N61.91 (19)
N5—Dy1—N4—N919.4 (2)N4—Dy1—O4—N632.4 (2)
O8—Dy1—N4—N9−101.4 (3)O6—Dy1—O4—N6127.8 (2)
Dy1i—Dy1—N4—N9−172.6 (2)N5—Dy1—O4—N686.3 (2)
N9—C9—N5—C10−175.2 (4)O8—Dy1—O4—N6−146.3 (2)
S1—C9—N5—C105.1 (4)Dy1i—Dy1—O4—N6−86.6 (2)
N9—C9—N5—Dy115.4 (5)O7—N7—O6—Dy1−176.6 (4)
S1—C9—N5—Dy1−164.29 (19)O8—N7—O6—Dy13.1 (4)
C11—C10—N5—C9173.0 (4)O2—Dy1—O6—N7−56.8 (2)
C15—C10—N5—C9−3.0 (5)O2i—Dy1—O6—N724.1 (3)
C11—C10—N5—Dy1−21.3 (6)O1i—Dy1—O6—N781.2 (2)
C15—C10—N5—Dy1162.7 (3)O4—Dy1—O6—N7123.1 (2)
O2—Dy1—N5—C9−40.9 (3)O3—Dy1—O6—N7−147.7 (2)
O2i—Dy1—N5—C9167.3 (2)N4—Dy1—O6—N7−122.6 (2)
O1i—Dy1—N5—C9135.7 (3)N5—Dy1—O6—N7166.3 (3)
O4—Dy1—N5—C9−148.7 (3)O8—Dy1—O6—N7−1.8 (2)
O3—Dy1—N5—C9−95.1 (3)Dy1i—Dy1—O6—N7−16.8 (2)
N4—Dy1—N5—C9−17.7 (3)O7—N7—O8—Dy1176.7 (4)
O6—Dy1—N5—C956.8 (3)O6—N7—O8—Dy1−3.0 (4)
O8—Dy1—N5—C967.5 (3)O2—Dy1—O8—N7129.1 (2)
Dy1i—Dy1—N5—C9−108.9 (4)O2i—Dy1—O8—N7−153.6 (3)
O2—Dy1—N5—C10153.8 (3)O1i—Dy1—O8—N7−82.3 (2)
O2i—Dy1—N5—C102.0 (5)O4—Dy1—O8—N7−125.1 (2)
O1i—Dy1—N5—C10−29.6 (4)O3—Dy1—O8—N7126.7 (3)
O4—Dy1—N5—C1046.0 (4)N4—Dy1—O8—N756.0 (2)
O3—Dy1—N5—C1099.6 (4)O6—Dy1—O8—N71.8 (2)
N4—Dy1—N5—C10177.0 (4)N5—Dy1—O8—N7−11.4 (3)
O6—Dy1—N5—C10−108.5 (4)Dy1i—Dy1—O8—N7167.8 (3)
O8—Dy1—N5—C10−97.8 (4)N5—C9—S1—C15−4.6 (3)
Dy1i—Dy1—N5—C1085.8 (5)N9—C9—S1—C15175.7 (4)
N5—C9—N9—N43.2 (6)C14—C15—S1—C9−173.3 (4)
S1—C9—N9—N4−177.1 (3)C10—C15—S1—C92.4 (3)
D—H···AD—HH···AD···AD—H···A
O9—H9A···O3ii0.842.643.206 (4)126
O9—H9A···O8iii0.842.243.049 (4)161
N9—H9···O9iv0.881.912.751 (4)160
Table 1

Selected bond lengths (Å)

Dy1—O22.280 (3)
Dy1—O2i2.374 (2)
Dy1—O1i2.394 (3)
Dy1—O42.422 (3)
Dy1—O32.433 (3)
Dy1—N42.461 (3)
Dy1—O62.471 (3)
Dy1—N52.494 (3)
Dy1—O82.530 (3)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O9—H9A⋯O3ii0.842.643.206 (4)126
O9—H9A⋯O8iii0.842.243.049 (4)161
N9—H9⋯O9iv0.881.912.751 (4)160

Symmetry codes: (ii) ; (iii) ; (iv) .

  4 in total

1.  A promising new route towards single-molecule magnets based on the oxalate ligand.

Authors:  Gong-Feng Xu; Qing-Lun Wang; Patrick Gamez; Yue Ma; Rodolphe Clérac; Jinkui Tang; Shi-Ping Yan; Peng Cheng; Dai-Zheng Liao
Journal:  Chem Commun (Camb)       Date:  2009-12-23       Impact factor: 6.222

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Dinuclear dysprosium(III) single-molecule magnets with a large anisotropic barrier.

Authors:  Po-Heng Lin; Tara J Burchell; Rodolphe Clérac; Muralee Murugesu
Journal:  Angew Chem Int Ed Engl       Date:  2008       Impact factor: 15.336

4.  {μ-2-[(Benzothia-zol-2-yl-2κN)hydrazonomethyl-2κN]-6-methoxy-phenolato-1:2κO,O:O}{2-[(benzo-thia-zol-2-yl-1κN)hydrazonomethyl-1κN]-6-methoxy-phenolato-1κO}(methanol-2κO)(nitrato-2κO)dicopper(II) nitrate.

Authors:  Yu-Ching Lin; Fung-E Hong
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-08-15
  4 in total

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