Literature DB >> 29765761

Crystal structures of two isotypic lanthanide(III) complexes: tri-aqua-[2,6-di-acetyl-pyridine bis-(benzoyl-hydrazone)]methano-llanthanide(III) trichloride methanol disolvates (LnIII = Tb and Dy).

Chihiro Kachi-Terajima1, Norihisa Kimura1.   

Abstract

The title class="Chemical">lanthanide complexes, [class="Gene">pan class="Chemical">Ln(DAPBH2)(CH3OH)(H2O)3]Cl3·2CH3OH [LnIII = Tb and Dy; DAPBH2 = 2,6-di-acetyl-pyridine bis-(benzoyl-hydrazone), C23H21N5O2], are isotypic. The central lanthanide ions are nine-coordinate, being ligated by three N and two O atoms from the penta-dentate DAPBH2 ligand, and four O atoms from the coordinated methanol mol-ecule and three coordinated water mol-ecules. The coordination geometry of the lanthanide ion is a distorted capped square anti-prism. In the crystals, the various components are linked by O-H⋯Cl, N-H⋯Cl and O-H⋯O hydrogen bonds, forming three-dimensional supra-molecular frameworks. Within the frameworks, there are C-H⋯Cl and C-H⋯O hydrogen bonds and offset π-π inter-actions (inter-centroid distance ca 3.81 Å).

Entities:  

Keywords:  2,6-di­acetyl­pyridine bis­(benzoyl­hydrazone) ligand; crystal structure; dysprosium (III); hydrogen bonding; lanthanide(III); supra­molecular framework; terbium(II); π–π stacking

Year:  2018        PMID： 29765761      PMCID： PMC5946983          DOI： 10.1107/S2056989018004103

Source DB:  PubMed          Journal:  Acta Crystallogr E Crystallogr Commun


Chemical context

Mol­ecule-based magnets based on class="Chemical">lanthanide ions have attracted much attention because of their large magnetic moments and magnetic anisotropy. The design of building units, such as the coordination–acceptor or coordination–class="Gene">pan class="Species">donor magnetic units, is a key process in the construction of multi-dimensional magnetic materials. Some lanthanide complexes with 2,6-di­acetyl­pyridine bis­(benzoyl­hydrazone as ligand (DAPBH2) have been reported, viz. for LaIII (Thomas et al., 1979 ▸), YbIII (Pan et al., 1989 ▸), EuIII (Gao & Wang, 2012 ▸), DyIII (Batchelor et al., 2014 ▸) and for LaIII and DyIII (Gao et al., 2016 ▸). The Dy complexes having two DAPBH2 ligands (Batchelor et al., 2014 ▸) have demonstrated attractive single-mol­ecule magnet behaviour, indicating that DAPBH2 ligands are useful for constructing magnetic units. For the use of DAPBH2 complexes as building blocks, coordination active sites are needed. The DAPBH2 ligand is penta­dentate, thus it can make coordination sites in the axial positions of the lanthanide ion. These complexes have coordinated or non-coordinated nitrate ions, which can disturb the coordination of coordination–donor units. We report herein on the TbIII and DyIII complexes with the DAPBH2 ligand containing non-coordinating chloride ions as the coordination–acceptor building units.

Structural commentary

The title pan class="Chemical">TbIII and DyIII complexes are isotypic, crystallizing in the same space group (P ) with almost identical unit-cell parameters. The representative mol­ecular structure of the class="Gene">pan class="Chemical">TbIII complex is shown in Fig. 1 ▸.
Figure 1

Mol­ecular structure of the TbIII complex, showing the selected atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.

The class="Chemical">lanthanide ion is surrounded by six class="Gene">pan class="Chemical">oxygen atoms and three nitro­gen atoms, and the coordination polyhedron is a distorted capped square anti­prism. The equatorial coordin­ation site of the Ln III ion is occupied by an N3O2 atom set of a penta­dentate DAPBH2 ligand. Selected bond lengths and bond angles for both complexes are compared in Table 1 ▸. The Ln–donor bond distances are in the range of 2.321 (2)–2.596 (2) Å for the TbIII complex and 2.313 (2)–2.584 (2) Å for the DyIII complex. The bond distances for the DyIII complex are slightly shorter than those of the TbIII complex as a result of the lanthanide contraction effect. The DAPBH2 ligand is approximately planar, and the Ln III ion lies out of the mean plane (O1/N2/N3/N4/O2) by a distance of 0.5754 (3) Å for the TbIII complex and 0.5702 (3) Å for the DyIII complex. The coordination of the DAPBH2 ligand to the lanthanide ion shows a bent arrangement [bond angles O1—Ln—N4 and O2—Ln—N2 are 149.40 (6) and 152.08 (7)°, respectively, for the TbIII complex, and 149.36 (7) and 151.76 (8)°, respectively, for the DyIII complex]. These coordination features are similar to those reported for the dysprosium DAPBH2 nitrate complex (Gao et al., 2016 ▸). Three water mol­ecules and one methanol mol­ecule are involved in the coordination sphere of the Ln III ion. The asymmetric unit consists of the Ln III complex, three chlorides as counter-ions, and two methanol solvent mol­ecules.
Table 1

Selected geometric parameters (Å, °) for the TbIII and DyIII complexes

Tb1—N22.5845 (19)Dy1—N22.577 (2)
Tb1—N32.596 (2)Dy1—N32.584 (2)
Tb1—N42.5685 (19)Dy1—N42.555 (2)
Tb1—O12.3660 (16)Dy1—O12.358 (2)
Tb1—O22.4074 (17)Dy1—O22.3961 (19)
Tb1—O32.4867 (18)Dy1—O32.472 (2)
Tb1—O52.3642 (19)Dy1—O42.420 (2)
Tb1—O42.428 (2)Dy1—O52.354 (2)
Tb1—O62.321 (2)Dy1—O62.313 (2)
    
O1—Tb1—N4149.40 (6)O1—Dy1—N4149.36 (7)
O2—Tb1—N2152.08 (7)O2—Dy1—N2151.76 (8)
O6—Tb1—N474.40 (7)O6—Dy1—N474.67 (8)
O6—Tb1—O276.48 (7)O6—Dy1—O276.31 (8)
O6—Tb1—N276.97 (7)O6—Dy1—N276.91 (8)
O6—Tb1—N379.68 (7)O6—Dy1—N380.29 (8)
O6—Tb1—O176.15 (7)O6—Dy1—O175.91 (8)

Supra­molecular features

In the crystals, the class="Chemical">lanthanide complexes are connected by O—H⋯Cl, N—H⋯Cl, O—H⋯O, C—H⋯Cl and C—H⋯O class="Gene">pan class="Chemical">hydrogen bonds (Tables 2 ▸ and 3 ▸). The representative crystal structure of the TbIII complex is discussed here and the crystal packing is shown in Figs. 2 ▸ and 3 ▸. The various components are linked by O—H⋯Cl and N—H⋯Cl hydrogen bonds, forming layers parallel to (101), as illustrated in Fig. 2 ▸ (see also Table 2 ▸). Within the layers there are offset π–π inter­actions involving the benzoyl rings of neighbouring mol­ecules [Cg2⋯Cg3, = 3.813 (2) Å, α = 3.8 (1)°, inter­planar distance = 3.483 (1) Å, slippages = 1.77 and 1.55 Å; Cg2 and Cg3 are the centroids of C2–C7 and C18–C23 rings, respectively, symmetry codes: (a) x, y − 1, z; (b) x, y + 1, z]. The layers are linked by O—H⋯O, O—H⋯Cl and N—H⋯Cl hydrogen bonds, forming a three-dimensional supra­molecular framework, which is reinforced by a series of C—H⋯Cl and C—H⋯O hydrogen bonds (Fig. 3 ▸ and Table 2 ▸).
Table 2

Hydrogen-bond geometry (Å, °) for the TbIII complex

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O4—H4SA⋯Cl30.64 (4)2.61 (4)3.213 (2)159 (5)
N1—H1A⋯Cl2i 0.882.523.299 (2)148
O6—H6SA⋯Cl1i 0.73 (4)2.32 (4)3.040 (2)172 (4)
O3—H3S⋯Cl3ii 0.68 (5)2.68 (5)3.2998 (19)153 (5)
O4—H4SB⋯Cl3iii 0.81 (4)2.34 (4)3.1323 (19)169 (4)
O6—H6SB⋯Cl1iv 0.74 (4)2.32 (4)3.058 (2)176 (3)
O7—H7S⋯Cl2v 0.72 (3)2.34 (3)3.050 (2)174 (4)
O8—H8S⋯Cl3vi 0.91 (4)2.23 (4)3.110 (2)163 (4)
O5—H5SA⋯O8vi 0.77 (4)1.96 (4)2.710 (3)166 (4)
O5—H5SB⋯O7v 0.79 (4)1.88 (4)2.664 (3)168 (4)
C7—H7⋯Cl2i 0.952.743.491 (3)137
C11—H11⋯Cl1vii 0.952.803.731 (3)167
C12—H12⋯Cl1viii 0.952.803.741 (3)172
C16—H16B⋯Cl20.982.663.628 (3)170
C16—H16C⋯Cl2viii 0.982.793.621 (3)143
C19—H19⋯Cl20.952.733.515 (3)140
C26—H26A⋯Cl3ix 0.982.803.774 (3)174
C4—H4⋯O8x 0.952.593.397 (3)143

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) .

Table 3

Hydrogen-bond geometry (Å, °) for the DyIII complex

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O4—H4SA⋯Cl30.77 (4)2.45 (4)3.211 (3)170 (4)
N1—H1A⋯Cl2i 0.882.533.298 (2)147
O6—H6SA⋯Cl1i 0.77 (4)2.27 (4)3.030 (3)168 (4)
O3—H3S⋯Cl3ii 0.79 (3)2.60 (3)3.329 (2)156 (3)
O4—H4SB⋯Cl3iii 0.73 (5)2.42 (4)3.133 (3)165 (4)
O6—H6SB⋯Cl1iv 0.67 (3)2.39 (3)3.058 (3)179 (5)
O7—H7S⋯Cl2v 0.78 (4)2.29 (4)3.049 (3)165 (4)
O8—H8S⋯Cl3vi 0.77 (5)2.34 (5)3.104 (3)174 (6)
O5—H5SA⋯O8vi 0.81 (4)1.96 (4)2.702 (4)154 (4)
O5—H5SB⋯O7v 0.72 (5)1.95 (5)2.659 (3)167 (6)
C7—H7⋯Cl2i 0.952.753.494 (3)136
C11—H11⋯Cl1vii 0.952.803.730 (3)167
C12—H12⋯Cl1viii 0.952.793.734 (3)172
C16—H16B⋯Cl20.982.663.620 (3)166
C16—H16C⋯Cl2viii 0.982.773.618 (3)145
C19—H19⋯Cl20.952.743.522 (3)140
C26—H26A⋯Cl3ix 0.982.793.761 (4)171
C4—H4⋯O8x 0.952.603.406 (4)143

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) .

Figure 2

A view along the b axis of the hydrogen-bonded (dashed lines) layer structure of the TbIII complex. The Cl− ions are shown as green balls and the C-bound H atoms have been omitted for clarity.

Figure 3

A view along the a axis of the hydrogen-bonded (dashed lines) supra­molecular framework of the TbIII complex. The Cl− ions are shown as green balls and the C-bound H atoms have been omitted for clarity.

Database survey

A search of the Cambridge Structural Database (Version 5.39, update February 2018; Groom et al., 2016 ▸) for the class="Chemical">DAPBH2 ligand gave 59 hits. There are 12 class="Gene">pan class="Chemical">lanthanide nitrate DAPBH2 complexes but no complexes with halogen ions as counter-ions. A number of halides of transition metal DAPBH2 complexes have been reported, viz. Mn (Lorenzini et al., 1983 ▸), Fe (Bar et al., 2015 ▸), Co (Batchelor et al., 2011 ▸), Cu (Neto et al., 2013 ▸), and Re (Al-Shihri et al., 1993 ▸).

Synthesis and crystallization

A class="Chemical">methanol solution (15 ml) of TbCl3·6H2O (0.178 g, 0.48 mmol), 2,6-di­acetyl­pyridine (0.075 g, 0.45 mmol), and benzoyl­hydrazine (0.127 g, 0.93 mmol) was refluxed for 2 h. The resulting mixture was filtered. Vapour diffusion of class="Gene">pan class="Chemical">diethyl ether into the filtrate afforded colourless plate-like crystals of the TbIII complex (0.116 g, yield 30%). The synthetic procedure for the DyIII complex is similar, starting from dysprosium chloride (yield 43%).

Refinement

Crystal data, data collection, and structure refinement details are summarized in Table 4 ▸. The O—H class="Chemical">hydrogen atoms of the class="Gene">pan class="Chemical">water and methanol mol­ecules were located in difference-Fourier maps and were refined isotropically. The O—H distance of the coordinated methanol mol­ecule in the DyIII complex was restrained to 0.82 Å. Other hydrogen atoms were generated geometrically and refined with a riding model: N—H = 0.88 Å, C–H = 0.95–0.98 Å with U iso(H) = 1.5U eq(C-methyl, O-hydrox­yl) and 1.2 U eq(C, N) for other H atoms.
Table 4

Experimental details

 TbIII complexDyIII complex
Crystal data
Chemical formula[Tb(C23H21N5O2)(CH4O)(H2O)3)]Cl3·2CH4O[Dy(C23H21N5O2)(CH4O)(H2O)3)]Cl3·2CH4O
M r 814.89818.47
Crystal system, space groupTriclinic, P Triclinic, P
Temperature (K)100100
a, b, c (Å)8.9703 (7), 12.6433 (9), 14.4233 (11)8.9852 (7), 12.6242 (10), 14.3887 (12)
α, β, γ (°)87.004 (1), 88.752 (1), 81.980 (1)87.062 (1), 88.810 (1), 82.068 (1)
V (Å3)1617.4 (2)1614.2 (2)
Z 22
Radiation typeMo KαMo Kα
μ (mm−1)2.492.62
Crystal size (mm)0.20 × 0.15 × 0.050.25 × 0.15 × 0.10
 
Data collection
DiffractometerBruker SMART APEX CCDBruker SMART APEX CCD
Absorption correctionMulti-scan (SADABS; Bruker, 2014 ▸)Multi-scan (SADABS; Bruker, 2014 ▸)
T min, T max 0.636, 0.8860.561, 0.780
No. of measured, independent and observed [I > 2σ(I)] reflections13292, 8926, 822713359, 8915, 8062
R int 0.0210.021
(sin θ/λ)max (Å−1)0.7200.720
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.029, 0.069, 1.030.030, 0.073, 1.04
No. of reflections89268915
No. of parameters429429
No. of restraints01
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.48, −0.731.73, −0.79

Computer programs: SMART and SAINT (Bruker, 2014 ▸), SHELXT2014 (Sheldrick, 2015a ▸), SHELXL2014 (Sheldrick, 2015b ▸), SHELXTL (Sheldrick, 2008 ▸) and Mercury (Macrae et al., 2008 ▸).

Crystal structure: contains datablock(s) Tbpan class="Chemical">DAPBH2, Dyclass="Gene">pan class="Chemical">DAPBH2, global. DOI: 10.1107/S2056989018004103/su5429sup1.cif Structure factors: contains datablock(s) Tbpan class="Chemical">DAPBH2. DOI: 10.1107/S2056989018004103/su5429Tbclass="Gene">pan class="Chemical">DAPBH2sup2.hkl Structure factors: contains datablock(s) Dypan class="Chemical">DAPBH2. DOI: 10.1107/S2056989018004103/su5429Dyclass="Gene">pan class="Chemical">DAPBH2sup3.hkl CCDC references: 1828810, 1828809 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Tb(C23H21N5O2)(CH4O)(H2O)3)]Cl3·2CH4OZ = 2
Mr = 814.89F(000) = 820
Triclinic, P1Dx = 1.673 Mg m−3
a = 8.9703 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.6433 (9) ÅCell parameters from 7626 reflections
c = 14.4233 (11) Åθ = 2.3–30.4°
α = 87.004 (1)°µ = 2.49 mm−1
β = 88.752 (1)°T = 100 K
γ = 81.980 (1)°Plate, colorless
V = 1617.4 (2) Å30.20 × 0.15 × 0.05 mm
Bruker SMART APEX CCD diffractometer8926 independent reflections
Radiation source: sealed tube8227 reflections with I > 2σ(I)
Detector resolution: 8.366 pixels mm-1Rint = 0.021
phi and ω scansθmax = 30.8°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2014)h = −12→12
Tmin = 0.636, Tmax = 0.886k = −12→17
13292 measured reflectionsl = −16→20
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: mixed
wR(F2) = 0.069H atoms treated by a mixture of independent and constrained refinement
S = 1.03w = 1/[σ2(Fo2) + (0.0355P)2 + 0.3922P] where P = (Fo2 + 2Fc2)/3
8926 reflections(Δ/σ)max = 0.001
429 parametersΔρmax = 1.48 e Å−3
0 restraintsΔρmin = −0.73 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
xyzUiso*/Ueq
C10.3931 (3)−0.18034 (19)0.27986 (17)0.0141 (4)
C20.4840 (3)−0.27866 (19)0.31946 (17)0.0145 (5)
C30.6288 (3)−0.2707 (2)0.34747 (19)0.0185 (5)
H30.6690−0.20550.33650.022*
C40.7149 (3)−0.3579 (2)0.3915 (2)0.0238 (6)
H40.8137−0.35230.41130.029*
C50.6563 (3)−0.4533 (2)0.4066 (2)0.0232 (6)
H50.7154−0.51300.43670.028*
C60.5125 (3)−0.4623 (2)0.3781 (2)0.0212 (5)
H60.4733−0.52800.38830.025*
C70.4255 (3)−0.3752 (2)0.33454 (19)0.0186 (5)
H70.3266−0.38100.31510.022*
C80.0392 (3)−0.08870 (19)0.18845 (17)0.0133 (4)
C9−0.0525 (3)−0.1790 (2)0.2001 (2)0.0187 (5)
H9A−0.0136−0.22730.25210.028*
H9B−0.0461−0.21830.14310.028*
H9C−0.1578−0.15040.21290.028*
C10−0.0267 (3)0.01568 (19)0.14391 (17)0.0136 (4)
C11−0.1615 (3)0.0250 (2)0.09601 (19)0.0183 (5)
H11−0.2197−0.03230.09760.022*
C12−0.2087 (3)0.1203 (2)0.0458 (2)0.0202 (5)
H12−0.30100.12960.01340.024*
C13−0.1197 (3)0.2013 (2)0.04380 (18)0.0171 (5)
H13−0.14840.26610.00840.021*
C140.0129 (3)0.18641 (18)0.09447 (17)0.0127 (4)
C150.1148 (3)0.26892 (18)0.09226 (17)0.0127 (4)
C160.0854 (3)0.36814 (19)0.03070 (19)0.0187 (5)
H16A0.15540.3628−0.02250.028*
H16B0.09980.43020.06570.028*
H16C−0.01830.37650.00860.028*
C170.4647 (3)0.28258 (18)0.18861 (17)0.0136 (4)
C180.5814 (3)0.35476 (19)0.18763 (18)0.0162 (5)
C190.5606 (3)0.4577 (2)0.1460 (2)0.0205 (5)
H190.46900.48360.11540.025*
C200.6730 (3)0.5226 (2)0.1491 (2)0.0233 (6)
H200.65790.59320.12180.028*
C210.8076 (3)0.4835 (2)0.1924 (2)0.0237 (6)
H210.88540.52730.19380.028*
C220.8297 (3)0.3809 (2)0.2338 (2)0.0225 (5)
H220.92220.35480.26320.027*
C230.7164 (3)0.3164 (2)0.23211 (19)0.0185 (5)
H230.73080.24660.26110.022*
C240.4784 (3)0.1550 (2)0.4460 (2)0.0232 (6)
H24A0.38200.19040.46980.035*
H24B0.52820.20670.40800.035*
H24C0.54270.12680.49810.035*
C250.9063 (3)0.5147 (2)0.6159 (2)0.0274 (6)
H25A0.92430.56430.56370.041*
H25B0.86240.45440.59300.041*
H25C1.00180.48810.64630.041*
C260.1290 (3)0.7633 (2)0.5060 (2)0.0292 (6)
H26A0.15040.82870.53370.044*
H26B0.17360.75940.44350.044*
H26C0.17220.70090.54460.044*
Cl10.58645 (7)0.81886 (5)0.06470 (4)0.01793 (12)
Cl20.18932 (7)0.59026 (5)0.15256 (5)0.02071 (13)
Cl30.18676 (7)0.02722 (5)0.60038 (5)0.02070 (13)
H3S0.517 (5)0.035 (4)0.383 (3)0.059 (15)*
H7S0.804 (4)0.535 (3)0.722 (2)0.020 (9)*
H8S−0.061 (5)0.822 (3)0.462 (3)0.055 (13)*
H4SA0.179 (5)0.011 (3)0.421 (3)0.044 (14)*
H5SA0.127 (4)0.217 (3)0.377 (3)0.036 (11)*
H6SA0.445 (4)−0.021 (3)0.103 (3)0.035 (11)*
H4SB0.063 (4)0.003 (3)0.378 (3)0.034 (10)*
H5SB0.188 (4)0.283 (3)0.323 (3)0.045 (12)*
H6SB0.404 (4)0.070 (3)0.068 (3)0.021 (9)*
N10.2562 (2)−0.18805 (16)0.24489 (15)0.0153 (4)
H1A0.2202−0.24920.24330.018*
N20.1773 (2)−0.09152 (15)0.21167 (14)0.0126 (4)
N30.0574 (2)0.09586 (15)0.14648 (14)0.0124 (4)
N40.2332 (2)0.24464 (15)0.14258 (14)0.0117 (4)
N50.3365 (2)0.31596 (16)0.14172 (15)0.0152 (4)
H5A0.32000.37920.11250.018*
O10.43783 (19)−0.09181 (13)0.28311 (13)0.0153 (3)
O20.48215 (19)0.19393 (14)0.23100 (13)0.0174 (4)
O30.4522 (2)0.06898 (15)0.39042 (13)0.0160 (4)
O40.1509 (2)0.00969 (16)0.38079 (15)0.0180 (4)
O50.1709 (2)0.22339 (15)0.33114 (14)0.0178 (4)
O60.4055 (2)0.03235 (16)0.10887 (15)0.0207 (4)
O70.8055 (2)0.56858 (16)0.68054 (16)0.0266 (5)
O8−0.0300 (2)0.76493 (16)0.50082 (15)0.0250 (4)
Tb10.29292 (2)0.07670 (2)0.25062 (2)0.01026 (4)
U11U22U33U12U13U23
C10.0155 (11)0.0136 (11)0.0133 (11)−0.0022 (8)0.0007 (9)−0.0008 (8)
C20.0168 (11)0.0127 (10)0.0137 (12)−0.0008 (8)−0.0007 (9)−0.0004 (8)
C30.0171 (12)0.0157 (11)0.0225 (14)−0.0015 (9)−0.0025 (10)0.0005 (9)
C40.0174 (12)0.0234 (13)0.0302 (16)0.0006 (10)−0.0073 (11)−0.0029 (11)
C50.0251 (14)0.0204 (13)0.0223 (14)0.0033 (10)−0.0060 (11)0.0020 (10)
C60.0262 (14)0.0153 (12)0.0218 (14)−0.0034 (10)−0.0033 (11)0.0032 (10)
C70.0199 (12)0.0163 (11)0.0197 (13)−0.0038 (9)−0.0028 (10)0.0025 (9)
C80.0143 (11)0.0136 (10)0.0124 (11)−0.0031 (8)−0.0017 (9)−0.0010 (8)
C90.0161 (11)0.0159 (11)0.0251 (14)−0.0061 (9)−0.0023 (10)0.0006 (10)
C100.0119 (10)0.0148 (11)0.0138 (12)−0.0010 (8)−0.0010 (9)−0.0001 (8)
C110.0160 (12)0.0158 (11)0.0242 (14)−0.0056 (9)−0.0049 (10)0.0001 (10)
C120.0145 (11)0.0215 (12)0.0254 (14)−0.0049 (9)−0.0075 (10)0.0011 (10)
C130.0154 (11)0.0167 (11)0.0189 (13)−0.0016 (9)−0.0047 (9)0.0025 (9)
C140.0125 (10)0.0135 (10)0.0124 (11)−0.0022 (8)−0.0014 (9)−0.0003 (8)
C150.0152 (11)0.0115 (10)0.0112 (11)−0.0008 (8)−0.0004 (9)−0.0005 (8)
C160.0209 (12)0.0148 (11)0.0205 (13)−0.0038 (9)−0.0066 (10)0.0050 (9)
C170.0111 (10)0.0140 (11)0.0155 (12)−0.0014 (8)0.0023 (9)0.0006 (8)
C180.0130 (11)0.0165 (11)0.0192 (13)−0.0032 (9)0.0009 (9)−0.0004 (9)
C190.0154 (12)0.0198 (12)0.0262 (15)−0.0042 (9)0.0001 (10)0.0044 (10)
C200.0219 (13)0.0185 (12)0.0303 (16)−0.0082 (10)0.0037 (11)0.0042 (11)
C210.0206 (13)0.0243 (13)0.0289 (15)−0.0119 (10)0.0050 (11)−0.0040 (11)
C220.0157 (12)0.0260 (13)0.0267 (15)−0.0047 (10)−0.0031 (10)−0.0035 (11)
C230.0181 (12)0.0190 (12)0.0189 (13)−0.0039 (9)−0.0005 (10)−0.0004 (9)
C240.0266 (14)0.0210 (13)0.0230 (14)−0.0045 (10)−0.0070 (11)−0.0047 (10)
C250.0277 (15)0.0273 (14)0.0280 (16)−0.0054 (11)0.0015 (12)−0.0058 (12)
C260.0270 (15)0.0222 (14)0.0377 (18)−0.0024 (11)0.0050 (13)−0.0004 (12)
Cl10.0197 (3)0.0156 (3)0.0175 (3)−0.0001 (2)0.0012 (2)0.0021 (2)
Cl20.0225 (3)0.0190 (3)0.0211 (3)−0.0038 (2)−0.0071 (2)0.0001 (2)
Cl30.0164 (3)0.0262 (3)0.0203 (3)−0.0051 (2)−0.0007 (2)−0.0022 (2)
N10.0158 (10)0.0113 (9)0.0185 (11)−0.0019 (7)−0.0043 (8)0.0029 (8)
N20.0155 (9)0.0094 (9)0.0130 (10)−0.0019 (7)−0.0054 (8)0.0010 (7)
N30.0130 (9)0.0118 (9)0.0119 (10)−0.0014 (7)−0.0011 (7)0.0015 (7)
N40.0109 (9)0.0123 (9)0.0127 (10)−0.0044 (7)−0.0011 (7)0.0001 (7)
N50.0143 (10)0.0131 (9)0.0186 (11)−0.0053 (7)−0.0033 (8)0.0044 (8)
O10.0165 (8)0.0101 (8)0.0199 (9)−0.0033 (6)−0.0035 (7)−0.0004 (6)
O20.0148 (8)0.0149 (8)0.0222 (10)−0.0037 (6)−0.0032 (7)0.0061 (7)
O30.0161 (9)0.0166 (9)0.0154 (9)−0.0018 (7)−0.0042 (7)−0.0019 (7)
O40.0172 (10)0.0227 (10)0.0155 (10)−0.0082 (7)−0.0003 (8)−0.0003 (7)
O50.0225 (9)0.0137 (9)0.0164 (10)−0.0010 (7)0.0055 (8)0.0001 (7)
O60.0290 (11)0.0130 (9)0.0180 (10)0.0023 (8)0.0052 (8)0.0030 (8)
O70.0355 (12)0.0171 (9)0.0272 (12)−0.0061 (8)0.0056 (9)0.0039 (8)
O80.0275 (10)0.0252 (10)0.0230 (11)−0.0079 (8)0.0033 (8)0.0012 (8)
Tb10.01062 (6)0.00929 (6)0.01094 (6)−0.00193 (4)−0.00114 (4)0.00083 (4)
C1—O11.244 (3)C20—C211.388 (4)
C1—N11.355 (3)C20—H200.9500
C1—C21.483 (3)C21—C221.390 (4)
C2—C31.387 (4)C21—H210.9500
C2—C71.399 (3)C22—C231.390 (4)
C3—C41.388 (4)C22—H220.9500
C3—H30.9500C23—H230.9500
C4—C51.387 (4)C24—O31.432 (3)
C4—H40.9500C24—H24A0.9800
C5—C61.384 (4)C24—H24B0.9800
C5—H50.9500C24—H24C0.9800
C6—C71.388 (3)C25—O71.417 (4)
C6—H60.9500C25—H25A0.9800
C7—H70.9500C25—H25B0.9800
C8—N21.286 (3)C25—H25C0.9800
C8—C101.488 (3)C26—O81.427 (4)
C8—C91.498 (3)C26—H26A0.9800
C9—H9A0.9800C26—H26B0.9800
C9—H9B0.9800C26—H26C0.9800
C9—H9C0.9800N1—N21.390 (3)
C10—N31.348 (3)N1—H1A0.8800
C10—C111.393 (3)N2—Tb12.5845 (19)
C11—C121.390 (4)N3—Tb12.596 (2)
C11—H110.9500N4—N51.380 (3)
C12—C131.383 (4)N4—Tb12.5685 (19)
C12—H120.9500N5—H5A0.8800
C13—C141.394 (3)O1—Tb12.3660 (16)
C13—H130.9500O2—Tb12.4074 (17)
C14—N31.352 (3)O3—Tb12.4867 (18)
C14—C151.479 (3)O3—H3S0.68 (4)
C15—N41.291 (3)O4—Tb12.428 (2)
C15—C161.494 (3)O4—H4SA0.64 (5)
C16—H16A0.9800O4—H4SB0.80 (4)
C16—H16B0.9800O5—Tb12.3642 (19)
C16—H16C0.9800O5—H5SA0.78 (4)
C17—O21.240 (3)O5—H5SB0.80 (4)
C17—N51.351 (3)O6—Tb12.321 (2)
C17—C181.481 (3)O6—H6SA0.73 (4)
C18—C191.395 (3)O6—H6SB0.74 (4)
C18—C231.397 (4)O7—H7S0.72 (3)
C19—C201.389 (4)O8—H8S0.91 (4)
C19—H190.9500
O1—C1—N1120.6 (2)H24B—C24—H24C109.5
O1—C1—C2120.8 (2)O7—C25—H25A109.5
N1—C1—C2118.6 (2)O7—C25—H25B109.5
C3—C2—C7119.9 (2)H25A—C25—H25B109.5
C3—C2—C1117.5 (2)O7—C25—H25C109.5
C7—C2—C1122.4 (2)H25A—C25—H25C109.5
C2—C3—C4120.1 (2)H25B—C25—H25C109.5
C2—C3—H3120.0O8—C26—H26A109.5
C4—C3—H3120.0O8—C26—H26B109.5
C5—C4—C3119.8 (3)H26A—C26—H26B109.5
C5—C4—H4120.1O8—C26—H26C109.5
C3—C4—H4120.1H26A—C26—H26C109.5
C6—C5—C4120.5 (2)H26B—C26—H26C109.5
C6—C5—H5119.7C1—N1—N2114.57 (19)
C4—C5—H5119.7C1—N1—H1A122.7
C5—C6—C7119.9 (2)N2—N1—H1A122.7
C5—C6—H6120.0C8—N2—N1118.8 (2)
C7—C6—H6120.0C8—N2—Tb1123.18 (15)
C6—C7—C2119.7 (2)N1—N2—Tb1115.06 (14)
C6—C7—H7120.1C10—N3—C14117.6 (2)
C2—C7—H7120.1C10—N3—Tb1120.64 (15)
N2—C8—C10113.4 (2)C14—N3—Tb1121.71 (15)
N2—C8—C9126.2 (2)C15—N4—N5118.17 (19)
C10—C8—C9120.4 (2)C15—N4—Tb1126.08 (15)
C8—C9—H9A109.5N5—N4—Tb1115.71 (14)
C8—C9—H9B109.5C17—N5—N4115.84 (19)
H9A—C9—H9B109.5C17—N5—H5A122.1
C8—C9—H9C109.5N4—N5—H5A122.1
H9A—C9—H9C109.5C1—O1—Tb1126.00 (15)
H9B—C9—H9C109.5C17—O2—Tb1125.09 (15)
N3—C10—C11123.1 (2)C24—O3—Tb1128.24 (16)
N3—C10—C8116.1 (2)C24—O3—H3S112 (4)
C11—C10—C8120.6 (2)Tb1—O3—H3S108 (4)
C12—C11—C10118.4 (2)Tb1—O4—H4SA116 (4)
C12—C11—H11120.8Tb1—O4—H4SB123 (3)
C10—C11—H11120.8H4SA—O4—H4SB118 (5)
C13—C12—C11119.2 (2)Tb1—O5—H5SA123 (3)
C13—C12—H12120.4Tb1—O5—H5SB125 (3)
C11—C12—H12120.4H5SA—O5—H5SB110 (4)
C12—C13—C14119.0 (2)Tb1—O6—H6SA120 (3)
C12—C13—H13120.5Tb1—O6—H6SB124 (3)
C14—C13—H13120.5H6SA—O6—H6SB116 (4)
N3—C14—C13122.5 (2)C25—O7—H7S109 (3)
N3—C14—C15116.2 (2)C26—O8—H8S105 (3)
C13—C14—C15121.3 (2)O6—Tb1—O5142.11 (7)
N4—C15—C14114.7 (2)O6—Tb1—O176.15 (7)
N4—C15—C16123.8 (2)O5—Tb1—O1139.14 (7)
C14—C15—C16121.4 (2)O6—Tb1—O276.48 (7)
C15—C16—H16A109.5O5—Tb1—O281.03 (7)
C15—C16—H16B109.5O1—Tb1—O2102.60 (6)
H16A—C16—H16B109.5O6—Tb1—O4143.61 (7)
C15—C16—H16C109.5O5—Tb1—O471.13 (7)
H16A—C16—H16C109.5O1—Tb1—O479.33 (7)
H16B—C16—H16C109.5O2—Tb1—O4135.63 (7)
O2—C17—N5120.2 (2)O6—Tb1—O3119.22 (7)
O2—C17—C18121.8 (2)O5—Tb1—O378.63 (7)
N5—C17—C18118.1 (2)O1—Tb1—O365.79 (6)
C19—C18—C23119.8 (2)O2—Tb1—O368.37 (6)
C19—C18—C17123.0 (2)O4—Tb1—O372.66 (7)
C23—C18—C17117.2 (2)O6—Tb1—N474.40 (7)
C20—C19—C18120.3 (2)O5—Tb1—N468.22 (7)
C20—C19—H19119.8O1—Tb1—N4149.40 (6)
C18—C19—H19119.8O2—Tb1—N462.41 (6)
C21—C20—C19119.5 (2)O4—Tb1—N4130.58 (7)
C21—C20—H20120.2O3—Tb1—N4123.50 (6)
C19—C20—H20120.2O6—Tb1—N276.97 (7)
C20—C21—C22120.6 (2)O5—Tb1—N2126.12 (7)
C20—C21—H21119.7O1—Tb1—N262.47 (6)
C22—C21—H21119.7O2—Tb1—N2152.08 (7)
C23—C22—C21120.0 (3)O4—Tb1—N267.93 (7)
C23—C22—H22120.0O3—Tb1—N2118.85 (6)
C21—C22—H22120.0N4—Tb1—N2117.64 (6)
C22—C23—C18119.7 (2)O6—Tb1—N379.68 (7)
C22—C23—H23120.1O5—Tb1—N387.34 (7)
C18—C23—H23120.1O1—Tb1—N3121.25 (6)
O3—C24—H24A109.5O2—Tb1—N3122.36 (6)
O3—C24—H24B109.5O4—Tb1—N390.74 (7)
H24A—C24—H24B109.5O3—Tb1—N3160.96 (6)
O3—C24—H24C109.5N4—Tb1—N360.86 (6)
H24A—C24—H24C109.5N2—Tb1—N360.23 (6)
D—H···AD—HH···AD···AD—H···A
O4—H4SA···Cl30.64 (4)2.61 (4)3.213 (2)159 (5)
N1—H1A···Cl2i0.882.523.299 (2)148
O6—H6SA···Cl1i0.73 (4)2.32 (4)3.040 (2)172 (4)
O3—H3S···Cl3ii0.68 (5)2.68 (5)3.2998 (19)153 (5)
O4—H4SB···Cl3iii0.81 (4)2.34 (4)3.1323 (19)169 (4)
O6—H6SB···Cl1iv0.74 (4)2.32 (4)3.058 (2)176 (3)
O7—H7S···Cl2v0.72 (3)2.34 (3)3.050 (2)174 (4)
O8—H8S···Cl3vi0.91 (4)2.23 (4)3.110 (2)163 (4)
O5—H5SA···O8vi0.77 (4)1.96 (4)2.710 (3)166 (4)
O5—H5SB···O7v0.79 (4)1.88 (4)2.664 (3)168 (4)
C7—H7···Cl2i0.952.743.491 (3)137
C11—H11···Cl1vii0.952.803.731 (3)167
C12—H12···Cl1viii0.952.803.741 (3)172
C16—H16B···Cl20.982.663.628 (3)170
C16—H16C···Cl2viii0.982.793.621 (3)143
C19—H19···Cl20.952.733.515 (3)140
C26—H26A···Cl3ix0.982.803.774 (3)174
C4—H4···O8x0.952.593.397 (3)143
[Dy(C23H21N5O2)(CH4O)(H2O)3)]Cl3·2CH4OZ = 2
Mr = 818.47F(000) = 822
Triclinic, P1Dx = 1.684 Mg m−3
a = 8.9852 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.6242 (10) ÅCell parameters from 7204 reflections
c = 14.3887 (12) Åθ = 2.2–30.5°
α = 87.062 (1)°µ = 2.62 mm−1
β = 88.810 (1)°T = 100 K
γ = 82.068 (1)°Plate, colorless
V = 1614.2 (2) Å30.25 × 0.15 × 0.10 mm
Bruker SMART APEX CCD diffractometer8915 independent reflections
Radiation source: sealed tube8062 reflections with I > 2σ(I)
Detector resolution: 8.366 pixels mm-1Rint = 0.021
phi and ω scansθmax = 30.8°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2014)h = −12→9
Tmin = 0.561, Tmax = 0.780k = −17→18
13359 measured reflectionsl = −20→17
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: mixed
wR(F2) = 0.073H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0355P)2 + 0.3922P] where P = (Fo2 + 2Fc2)/3
8915 reflections(Δ/σ)max = 0.001
429 parametersΔρmax = 1.73 e Å−3
1 restraintΔρmin = −0.79 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
xyzUiso*/Ueq
C10.3923 (3)−0.1799 (2)0.27938 (19)0.0130 (5)
C20.4831 (3)−0.2781 (2)0.3189 (2)0.0138 (5)
C30.6283 (3)−0.2700 (2)0.3466 (2)0.0184 (6)
H30.6686−0.20470.33540.022*
C40.7142 (4)−0.3572 (2)0.3906 (2)0.0242 (7)
H40.8129−0.35160.41020.029*
C50.6554 (4)−0.4525 (2)0.4057 (2)0.0237 (7)
H50.7141−0.51220.43610.028*
C60.5134 (4)−0.4617 (2)0.3774 (2)0.0213 (6)
H60.4748−0.52780.38690.026*
C70.4259 (3)−0.3743 (2)0.3347 (2)0.0183 (6)
H70.3266−0.38020.31630.022*
C80.0387 (3)−0.0891 (2)0.1879 (2)0.0128 (5)
C9−0.0519 (3)−0.1800 (2)0.1998 (2)0.0192 (6)
H9A−0.0096−0.23000.24990.029*
H9B−0.0494−0.21740.14170.029*
H9C−0.1561−0.15210.21570.029*
C10−0.0273 (3)0.0146 (2)0.1440 (2)0.0137 (5)
C11−0.1621 (3)0.0250 (2)0.0962 (2)0.0191 (6)
H11−0.2207−0.03220.09790.023*
C12−0.2094 (3)0.1199 (2)0.0463 (2)0.0202 (6)
H12−0.30200.12930.01420.024*
C13−0.1196 (3)0.2009 (2)0.0437 (2)0.0178 (6)
H13−0.14740.26540.00750.021*
C140.0122 (3)0.1862 (2)0.0949 (2)0.0131 (5)
C150.1153 (3)0.2686 (2)0.09186 (19)0.0125 (5)
C160.0853 (3)0.3676 (2)0.0306 (2)0.0185 (6)
H16A0.15810.3641−0.02120.028*
H16B0.09470.43010.06660.028*
H16C−0.01670.37370.00610.028*
C170.4641 (3)0.2816 (2)0.1881 (2)0.0137 (5)
C180.5818 (3)0.3531 (2)0.1874 (2)0.0156 (5)
C190.5607 (3)0.4565 (2)0.1457 (2)0.0208 (6)
H190.46930.48240.11500.025*
C200.6734 (4)0.5213 (3)0.1491 (2)0.0241 (7)
H200.65860.59210.12200.029*
C210.8072 (4)0.4819 (3)0.1924 (2)0.0231 (7)
H210.88520.52550.19380.028*
C220.8286 (3)0.3798 (3)0.2334 (2)0.0225 (6)
H220.92120.35380.26270.027*
C230.7156 (3)0.3146 (2)0.2322 (2)0.0179 (6)
H230.72970.24500.26160.022*
C240.4765 (4)0.1551 (3)0.4457 (2)0.0251 (7)
H24A0.38060.19130.46920.038*
H24B0.52740.20640.40780.038*
H24C0.54010.12660.49820.038*
C250.9067 (4)0.5157 (3)0.6162 (3)0.0275 (7)
H25A0.92370.56490.56340.041*
H25B0.86350.45460.59400.041*
H25C1.00260.49010.64650.041*
C260.1282 (4)0.7637 (3)0.5053 (3)0.0318 (8)
H26A0.15110.82750.53500.048*
H26B0.17050.76260.44190.048*
H26C0.17210.69940.54130.048*
Cl10.58557 (8)0.81884 (5)0.06449 (5)0.01935 (14)
Cl20.18964 (8)0.58963 (6)0.15245 (5)0.02133 (15)
Cl30.18672 (8)0.02676 (6)0.60011 (6)0.02261 (15)
Dy10.29156 (2)0.07637 (2)0.24991 (2)0.01098 (4)
H3S0.525 (3)0.029 (3)0.387 (3)0.038 (12)*
H7S0.804 (4)0.539 (3)0.729 (3)0.024 (11)*
H8S−0.063 (6)0.819 (4)0.476 (4)0.058 (17)*
H4SA0.167 (5)0.019 (3)0.431 (3)0.028 (11)*
H5SA0.126 (5)0.206 (3)0.377 (3)0.034 (12)*
H6SA0.452 (4)−0.024 (3)0.106 (3)0.025 (11)*
H4SB0.069 (5)0.011 (3)0.379 (3)0.026 (11)*
H5SB0.190 (6)0.276 (4)0.327 (4)0.061 (17)*
H6SB0.406 (4)0.064 (3)0.071 (2)0.006 (9)*
N10.2557 (3)−0.18801 (18)0.24483 (17)0.0147 (5)
H1A0.2196−0.24930.24400.018*
N20.1772 (3)−0.09208 (18)0.21085 (17)0.0142 (5)
N30.0566 (3)0.09572 (18)0.14657 (17)0.0126 (4)
N40.2328 (3)0.24374 (18)0.14232 (17)0.0132 (4)
N50.3360 (3)0.31481 (19)0.14179 (18)0.0152 (5)
H5A0.31920.37840.11290.018*
O10.4364 (2)−0.09136 (15)0.28269 (15)0.0154 (4)
O20.4808 (2)0.19244 (16)0.23072 (15)0.0182 (4)
O30.4493 (2)0.06843 (16)0.38954 (15)0.0168 (4)
O40.1507 (3)0.00937 (18)0.38004 (17)0.0188 (4)
O50.1698 (3)0.22245 (18)0.33018 (16)0.0188 (4)
O60.4048 (3)0.0315 (2)0.10881 (18)0.0217 (5)
O70.8064 (3)0.56962 (18)0.6807 (2)0.0279 (5)
O8−0.0309 (3)0.7659 (2)0.50160 (19)0.0277 (5)
U11U22U33U12U13U23
C10.0137 (13)0.0129 (12)0.0126 (13)−0.0026 (10)0.0019 (10)−0.0017 (10)
C20.0163 (13)0.0100 (12)0.0150 (13)−0.0015 (10)−0.0015 (10)0.0002 (10)
C30.0185 (14)0.0142 (13)0.0232 (16)−0.0042 (11)−0.0026 (11)−0.0003 (11)
C40.0193 (15)0.0196 (15)0.0332 (19)0.0011 (12)−0.0074 (13)−0.0029 (13)
C50.0287 (17)0.0162 (14)0.0240 (17)0.0048 (12)−0.0069 (13)0.0028 (12)
C60.0265 (16)0.0132 (13)0.0242 (17)−0.0038 (11)0.0000 (12)0.0030 (12)
C70.0190 (14)0.0170 (14)0.0201 (15)−0.0067 (11)−0.0032 (11)0.0007 (11)
C80.0128 (13)0.0104 (12)0.0152 (13)−0.0015 (9)0.0006 (10)−0.0021 (10)
C90.0160 (14)0.0136 (13)0.0289 (17)−0.0064 (11)0.0007 (12)−0.0001 (12)
C100.0126 (13)0.0128 (12)0.0161 (14)−0.0031 (10)−0.0013 (10)−0.0014 (10)
C110.0167 (14)0.0154 (13)0.0261 (16)−0.0050 (11)−0.0046 (11)−0.0012 (12)
C120.0146 (14)0.0200 (14)0.0265 (17)−0.0038 (11)−0.0063 (11)0.0009 (12)
C130.0171 (14)0.0155 (13)0.0198 (15)0.0007 (11)−0.0061 (11)0.0024 (11)
C140.0142 (13)0.0105 (12)0.0146 (13)−0.0019 (10)−0.0005 (10)−0.0007 (10)
C150.0137 (13)0.0110 (12)0.0127 (13)−0.0007 (9)0.0004 (10)−0.0019 (10)
C160.0203 (15)0.0120 (13)0.0236 (16)−0.0054 (11)−0.0061 (12)0.0051 (11)
C170.0133 (13)0.0130 (12)0.0152 (14)−0.0033 (10)0.0011 (10)−0.0006 (10)
C180.0128 (13)0.0163 (13)0.0185 (14)−0.0041 (10)0.0019 (10)−0.0028 (11)
C190.0153 (14)0.0182 (14)0.0290 (17)−0.0044 (11)0.0005 (12)0.0027 (12)
C200.0238 (16)0.0179 (14)0.0315 (18)−0.0091 (12)0.0042 (13)0.0042 (13)
C210.0179 (15)0.0249 (16)0.0291 (18)−0.0110 (12)0.0078 (12)−0.0063 (13)
C220.0117 (14)0.0304 (17)0.0261 (17)−0.0046 (12)−0.0009 (11)−0.0051 (13)
C230.0151 (14)0.0179 (14)0.0214 (15)−0.0042 (11)−0.0001 (11)−0.0016 (11)
C240.0273 (17)0.0250 (16)0.0246 (17)−0.0059 (13)−0.0059 (13)−0.0078 (13)
C250.0276 (18)0.0260 (17)0.0298 (19)−0.0058 (13)0.0024 (14)−0.0051 (14)
C260.0294 (19)0.0232 (16)0.042 (2)−0.0022 (14)0.0068 (16)−0.0011 (15)
Cl10.0215 (3)0.0153 (3)0.0201 (4)0.0007 (3)0.0019 (3)0.0010 (3)
Cl20.0219 (4)0.0179 (3)0.0246 (4)−0.0033 (3)−0.0068 (3)−0.0004 (3)
Cl30.0184 (3)0.0265 (4)0.0237 (4)−0.0050 (3)0.0007 (3)−0.0035 (3)
Dy10.01102 (6)0.00864 (6)0.01337 (7)−0.00194 (4)−0.00055 (4)0.00032 (4)
N10.0149 (11)0.0099 (10)0.0194 (13)−0.0026 (8)−0.0030 (9)0.0014 (9)
N20.0167 (12)0.0105 (10)0.0154 (12)−0.0017 (9)−0.0031 (9)−0.0002 (9)
N30.0127 (11)0.0108 (10)0.0146 (12)−0.0020 (8)−0.0019 (9)−0.0013 (9)
N40.0127 (11)0.0105 (10)0.0167 (12)−0.0028 (8)−0.0008 (9)0.0009 (9)
N50.0152 (12)0.0108 (10)0.0200 (13)−0.0039 (9)−0.0041 (9)0.0027 (9)
O10.0145 (10)0.0109 (9)0.0213 (11)−0.0031 (7)−0.0029 (8)−0.0019 (8)
O20.0146 (10)0.0142 (9)0.0259 (12)−0.0034 (8)−0.0037 (8)0.0040 (8)
O30.0172 (11)0.0143 (10)0.0192 (11)−0.0022 (8)−0.0036 (8)−0.0035 (8)
O40.0186 (12)0.0211 (11)0.0181 (12)−0.0082 (9)0.0020 (9)0.0000 (9)
O50.0241 (12)0.0130 (10)0.0181 (11)−0.0004 (8)0.0071 (9)0.0016 (9)
O60.0306 (13)0.0151 (11)0.0179 (12)−0.0001 (10)0.0056 (9)0.0031 (10)
O70.0355 (14)0.0161 (11)0.0316 (15)−0.0042 (10)0.0083 (11)0.0005 (10)
O80.0306 (13)0.0260 (13)0.0272 (14)−0.0070 (10)0.0048 (10)0.0000 (11)
C1—O11.239 (3)C20—C211.384 (5)
C1—N11.352 (4)C20—H200.9500
C1—C21.481 (4)C21—C221.380 (5)
C2—C71.388 (4)C21—H210.9500
C2—C31.391 (4)C22—C231.393 (4)
C3—C41.386 (4)C22—H220.9500
C3—H30.9500C23—H230.9500
C4—C51.386 (4)C24—O31.444 (4)
C4—H40.9500C24—H24A0.9800
C5—C61.369 (5)C24—H24B0.9800
C5—H50.9500C24—H24C0.9800
C6—C71.387 (4)C25—O71.414 (4)
C6—H60.9500C25—H25A0.9800
C7—H70.9500C25—H25B0.9800
C8—N21.289 (4)C25—H25C0.9800
C8—C101.478 (4)C26—O81.427 (4)
C8—C91.497 (4)C26—H26A0.9800
C9—H9A0.9800C26—H26B0.9800
C9—H9B0.9800C26—H26C0.9800
C9—H9C0.9800Dy1—O62.313 (2)
C10—N31.355 (3)Dy1—O52.354 (2)
C10—C111.392 (4)Dy1—O12.358 (2)
C11—C121.384 (4)Dy1—O22.3961 (19)
C11—H110.9500Dy1—O42.420 (2)
C12—C131.386 (4)Dy1—O32.472 (2)
C12—H120.9500Dy1—N42.555 (2)
C13—C141.393 (4)Dy1—N22.577 (2)
C13—H130.9500Dy1—N32.584 (2)
C14—N31.348 (4)N1—N21.386 (3)
C14—C151.484 (4)N1—H1A0.8800
C15—N41.287 (4)N4—N51.376 (3)
C15—C161.488 (4)N5—H5A0.8800
C16—H16A0.9800O3—H3S0.792 (19)
C16—H16B0.9800O4—H4SA0.77 (4)
C16—H16C0.9800O4—H4SB0.73 (4)
C17—O21.246 (3)O5—H5SA0.81 (5)
C17—N51.347 (4)O5—H5SB0.73 (5)
C17—C181.481 (4)O6—H6SA0.77 (4)
C18—C231.392 (4)O6—H6SB0.66 (4)
C18—C191.398 (4)O7—H7S0.77 (4)
C19—C201.390 (4)O8—H8S0.77 (5)
C19—H190.9500
O1—C1—N1120.6 (3)H24B—C24—H24C109.5
O1—C1—C2120.9 (3)O7—C25—H25A109.5
N1—C1—C2118.4 (2)O7—C25—H25B109.5
C7—C2—C3119.5 (3)H25A—C25—H25B109.5
C7—C2—C1122.8 (3)O7—C25—H25C109.5
C3—C2—C1117.5 (2)H25A—C25—H25C109.5
C4—C3—C2120.0 (3)H25B—C25—H25C109.5
C4—C3—H3120.0O8—C26—H26A109.5
C2—C3—H3120.0O8—C26—H26B109.5
C5—C4—C3119.7 (3)H26A—C26—H26B109.5
C5—C4—H4120.1O8—C26—H26C109.5
C3—C4—H4120.1H26A—C26—H26C109.5
C6—C5—C4120.6 (3)H26B—C26—H26C109.5
C6—C5—H5119.7O6—Dy1—O5142.37 (9)
C4—C5—H5119.7O6—Dy1—O175.91 (8)
C5—C6—C7119.9 (3)O5—Dy1—O1139.05 (8)
C5—C6—H6120.0O6—Dy1—O276.31 (8)
C7—C6—H6120.0O5—Dy1—O281.41 (8)
C6—C7—C2120.2 (3)O1—Dy1—O2102.05 (7)
C6—C7—H7119.9O6—Dy1—O4143.55 (8)
C2—C7—H7119.9O5—Dy1—O471.08 (8)
N2—C8—C10113.6 (2)O1—Dy1—O479.30 (8)
N2—C8—C9125.8 (3)O2—Dy1—O4135.51 (8)
C10—C8—C9120.5 (2)O6—Dy1—O3118.98 (8)
C8—C9—H9A109.5O5—Dy1—O378.77 (8)
C8—C9—H9B109.5O1—Dy1—O365.49 (7)
H9A—C9—H9B109.5O2—Dy1—O368.35 (7)
C8—C9—H9C109.5O4—Dy1—O372.39 (8)
H9A—C9—H9C109.5O6—Dy1—N474.67 (8)
H9B—C9—H9C109.5O5—Dy1—N468.20 (8)
N3—C10—C11122.3 (3)O1—Dy1—N4149.36 (7)
N3—C10—C8116.2 (2)O2—Dy1—N462.61 (7)
C11—C10—C8121.3 (2)O4—Dy1—N4130.72 (8)
C12—C11—C10119.0 (3)O3—Dy1—N4123.55 (7)
C12—C11—H11120.5O6—Dy1—N276.91 (8)
C10—C11—H11120.5O5—Dy1—N2126.14 (8)
C11—C12—C13119.0 (3)O1—Dy1—N262.53 (7)
C11—C12—H12120.5O2—Dy1—N2151.76 (8)
C13—C12—H12120.5O4—Dy1—N268.03 (8)
C12—C13—C14119.0 (3)O3—Dy1—N2118.59 (7)
C12—C13—H13120.5N4—Dy1—N2117.86 (7)
C14—C13—H13120.5O6—Dy1—N380.29 (8)
N3—C14—C13122.5 (2)O5—Dy1—N386.94 (8)
N3—C14—C15116.2 (2)O1—Dy1—N3121.65 (7)
C13—C14—C15121.3 (3)O2—Dy1—N3122.71 (7)
N4—C15—C14114.3 (2)O4—Dy1—N390.64 (8)
N4—C15—C16124.5 (2)O3—Dy1—N3160.57 (7)
C14—C15—C16121.1 (2)N4—Dy1—N360.99 (7)
C15—C16—H16A109.5N2—Dy1—N360.48 (7)
C15—C16—H16B109.5C1—N1—N2114.6 (2)
H16A—C16—H16B109.5C1—N1—H1A122.7
C15—C16—H16C109.5N2—N1—H1A122.7
H16A—C16—H16C109.5C8—N2—N1119.1 (2)
H16B—C16—H16C109.5C8—N2—Dy1122.84 (18)
O2—C17—N5119.6 (2)N1—N2—Dy1114.88 (16)
O2—C17—C18121.6 (3)C14—N3—C10117.9 (2)
N5—C17—C18118.8 (2)C14—N3—Dy1121.69 (17)
C23—C18—C19120.2 (3)C10—N3—Dy1120.38 (18)
C23—C18—C17117.4 (3)C15—N4—N5117.9 (2)
C19—C18—C17122.4 (3)C15—N4—Dy1126.39 (18)
C20—C19—C18120.1 (3)N5—N4—Dy1115.65 (17)
C20—C19—H19120.0C17—N5—N4116.2 (2)
C18—C19—H19120.0C17—N5—H5A121.9
C21—C20—C19119.4 (3)N4—N5—H5A121.9
C21—C20—H20120.3C1—O1—Dy1125.95 (18)
C19—C20—H20120.3C17—O2—Dy1125.06 (18)
C22—C21—C20120.7 (3)C24—O3—Dy1128.33 (19)
C22—C21—H21119.7C24—O3—H3S107 (3)
C20—C21—H21119.7Dy1—O3—H3S115 (3)
C21—C22—C23120.6 (3)Dy1—O4—H4SA122 (3)
C21—C22—H22119.7Dy1—O4—H4SB122 (3)
C23—C22—H22119.7H4SA—O4—H4SB104 (4)
C18—C23—C22119.0 (3)Dy1—O5—H5SA115 (3)
C18—C23—H23120.5Dy1—O5—H5SB125 (4)
C22—C23—H23120.5H5SA—O5—H5SB116 (5)
O3—C24—H24A109.5Dy1—O6—H6SA118 (3)
O3—C24—H24B109.5Dy1—O6—H6SB126 (3)
H24A—C24—H24B109.5H6SA—O6—H6SB116 (4)
O3—C24—H24C109.5C25—O7—H7S114 (3)
H24A—C24—H24C109.5C26—O8—H8S107 (4)
D—H···AD—HH···AD···AD—H···A
O4—H4SA···Cl30.77 (4)2.45 (4)3.211 (3)170 (4)
N1—H1A···Cl2i0.882.533.298 (2)147
O6—H6SA···Cl1i0.77 (4)2.27 (4)3.030 (3)168 (4)
O3—H3S···Cl3ii0.79 (3)2.60 (3)3.329 (2)156 (3)
O4—H4SB···Cl3iii0.73 (5)2.42 (4)3.133 (3)165 (4)
O6—H6SB···Cl1iv0.67 (3)2.39 (3)3.058 (3)179 (5)
O7—H7S···Cl2v0.78 (4)2.29 (4)3.049 (3)165 (4)
O8—H8S···Cl3vi0.77 (5)2.34 (5)3.104 (3)174 (6)
O5—H5SA···O8vi0.81 (4)1.96 (4)2.702 (4)154 (4)
O5—H5SB···O7v0.72 (5)1.95 (5)2.659 (3)167 (6)
C7—H7···Cl2i0.952.753.494 (3)136
C11—H11···Cl1vii0.952.803.730 (3)167
C12—H12···Cl1viii0.952.793.734 (3)172
C16—H16B···Cl20.982.663.620 (3)166
C16—H16C···Cl2viii0.982.773.618 (3)145
C19—H19···Cl20.952.743.522 (3)140
C26—H26A···Cl3ix0.982.793.761 (4)171
C4—H4···O8x0.952.603.406 (4)143
  8 in total

1.  A short history of SHELX.

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

2.  Single-ion magnet behaviour of heptacoordinated Fe(II) complexes: on the importance of supramolecular organization.

Authors:  Arun Kumar Bar; Céline Pichon; Nayanmoni Gogoi; Carine Duhayon; S Ramasesha; Jean-Pascal Sutter
Journal:  Chem Commun (Camb)       Date:  2015-02-28       Impact factor: 6.222

3.  Chemical tuning of the magnetic relaxation in dysprosium(iii) mononuclear complexes.

Authors:  Luke J Batchelor; Irene Cimatti; Régis Guillot; Floriana Tuna; Wolfgang Wernsdorfer; Liviu Ungur; Liviu F Chibotaru; Victoria E Campbell; Talal Mallah
Journal:  Dalton Trans       Date:  2014-08-28       Impact factor: 4.390

4.  Pentanuclear cyanide-bridged complexes based on highly anisotropic Co(II) seven-coordinate building blocks: synthesis, structure, and magnetic behavior.

Authors:  Luke J Batchelor; Marco Sangalli; Régis Guillot; Nathalie Guihéry; Remi Maurice; Floriana Tuna; Talal Mallah
Journal:  Inorg Chem       Date:  2011-11-03       Impact factor: 5.165

5.  Condensed, solution and gas phase behaviour of mono- and dinuclear 2,6-diacetylpyridine (dap) hydrazone copper complexes probed by X-ray, mass spectrometry and theoretical calculations.

Authors:  Brenno A D Neto; Barbara F L Viana; Thyago S Rodrigues; Priscila M Lalli; Marcos N Eberlin; Wender A da Silva; Heibbe C B de Oliveira; Claudia C Gatto
Journal:  Dalton Trans       Date:  2013-07-08       Impact factor: 4.390

6.  SHELXT - integrated space-group and crystal-structure determination.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A Found Adv       Date:  2015-01-01       Impact factor: 2.290

7.  Crystal structure refinement with SHELXL.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr C Struct Chem       Date:  2015-01-01       Impact factor: 1.172

8.  The Cambridge Structural Database.

Authors:  Colin R Groom; Ian J Bruno; Matthew P Lightfoot; Suzanna C Ward
Journal:  Acta Crystallogr B Struct Sci Cryst Eng Mater       Date:  2016-04-01
  8 in total

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