metal-organic compounds
Bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-κ2N)imidazoline-1-oxyl 3-oxide-κO]tris(nitrato-κ2O,O′)terbium(III)
aChemical Institute, Linyi University, Linyi Shandong 276005, People's Republic of China
*Correspondence e-mail: lidongjiao@lyu.edu.cn
The title compound, [Tb(NO3)3(C12H16N3O2)2], was prepared from the nitroxide radical ligand 4,4,5,5-tetramethyl-2-(pyridin-2-yl)-imidazoline-1-oxyl-3-oxide and TbIII nitrate. The TbIII ion adopts a doubly-capped square-antiprismatic coordination environment defined by three chelating nitrate anions and two N,O-bidentate nitronyl nitroxide radical ligands. Weak C—H⋯O hydrogen bonds connect the molecules into a three-dimensional framework. The title structure is isotypic with the Ho analogue [Li (2012). Acta Cryst. E68, 550].
Related literature
For background to the use of rare earth complexes with nitroxide radicals in coordination chemistry, see: Sutter et al. (1998); Kahn et al. (2000); Lescop et al. (2000). For the structures of related complexes, see: Li et al. (2004a,b, 2005); Li (2012).
Experimental
Crystal data
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Refinement
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Data collection: CrystalClear (Rigaku, 2008); cell CrystalClear; data reduction: CrystalClear; 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
10.1107/S1600536812040287/mw2078sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812040287/mw2078Isup2.hkl
The compound was synthesized by the following procedure. Tb(NO3)3.6H2O (0.045 g, 0.2 mmol) and NIT2Py (0.047 g, 0.2 mmol) were dissolved in 10 mL of anhydrous THF. The mixture was stirred at room temperature for four hours and then filtered. The dark brown filtrate was allowed to stand in the dark for one week. Dark brown crystals were obtained.
Hydrogen atoms were placed in calculated positions (C—H = 0.93–0.96 Å) and refined using a riding model with Uiso(H) = 1.2Ueq(Caromatic) and 1.5Ueq(Cmethyl).
Data collection: CrystalClear (Rigaku, 2008); cell
CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); 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).Fig. 1. The molecular structure of the title compound drawn with 30% ellipsoidal probability. | |
Fig. 2. The three-dimensional framework of the structure connected through intermolecular hydrogen bonds. |
[Tb(NO3)3(C12H16N3O2)2] | F(000) = 1632 |
Mr = 813.51 | Dx = 1.718 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9251 reflections |
a = 12.292 (3) Å | θ = 3.0–27.9° |
b = 11.114 (2) Å | µ = 2.33 mm−1 |
c = 23.264 (5) Å | T = 293 K |
β = 98.37 (3)° | Prism, colorless |
V = 3144.6 (11) Å3 | 0.20 × 0.20 × 0.20 mm |
Z = 4 |
Rigaku Saturn CCD area-detector diffractometer | 5554 independent reflections |
Radiation source: fine-focus sealed tube | 4726 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.059 |
ω–θ scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | h = −14→14 |
Tmin = 0.581, Tmax = 1.000 | k = −13→13 |
25443 measured reflections | l = −27→27 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.071 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0354P)2] where P = (Fo2 + 2Fc2)/3 |
5554 reflections | (Δ/σ)max = 0.001 |
432 parameters | Δρmax = 0.89 e Å−3 |
0 restraints | Δρmin = −0.95 e Å−3 |
[Tb(NO3)3(C12H16N3O2)2] | V = 3144.6 (11) Å3 |
Mr = 813.51 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.292 (3) Å | µ = 2.33 mm−1 |
b = 11.114 (2) Å | T = 293 K |
c = 23.264 (5) Å | 0.20 × 0.20 × 0.20 mm |
β = 98.37 (3)° |
Rigaku Saturn CCD area-detector diffractometer | 5554 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 4726 reflections with I > 2σ(I) |
Tmin = 0.581, Tmax = 1.000 | Rint = 0.059 |
25443 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.071 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.89 e Å−3 |
5554 reflections | Δρmin = −0.95 e Å−3 |
432 parameters |
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. |
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. |
x | y | z | Uiso*/Ueq | ||
Tb1 | 0.179699 (13) | 0.838779 (16) | 0.103896 (7) | 0.02337 (7) | |
C1 | 0.5499 (3) | 1.0194 (4) | 0.21909 (17) | 0.0512 (12) | |
H1A | 0.5285 | 1.0905 | 0.2381 | 0.077* | |
H1B | 0.6286 | 1.0143 | 0.2239 | 0.077* | |
H1C | 0.5209 | 0.9497 | 0.2360 | 0.077* | |
C2 | 0.5046 (3) | 1.0251 (4) | 0.15437 (16) | 0.0342 (9) | |
C3 | 0.5415 (3) | 0.9164 (4) | 0.12280 (18) | 0.0470 (11) | |
H3A | 0.5285 | 0.8446 | 0.1437 | 0.071* | |
H3B | 0.6186 | 0.9232 | 0.1204 | 0.071* | |
H3C | 0.5009 | 0.9127 | 0.0843 | 0.071* | |
C4 | 0.6215 (3) | 1.2196 (5) | 0.1523 (2) | 0.0620 (14) | |
H4A | 0.6208 | 1.2973 | 0.1342 | 0.093* | |
H4B | 0.6869 | 1.1771 | 0.1462 | 0.093* | |
H4C | 0.6204 | 1.2292 | 0.1932 | 0.093* | |
C5 | 0.5205 (3) | 1.1483 (4) | 0.12557 (18) | 0.0366 (10) | |
C6 | 0.5140 (3) | 1.1439 (4) | 0.05979 (18) | 0.0506 (12) | |
H6A | 0.4485 | 1.1020 | 0.0434 | 0.076* | |
H6B | 0.5772 | 1.1026 | 0.0498 | 0.076* | |
H6C | 0.5122 | 1.2244 | 0.0447 | 0.076* | |
C7 | 0.3375 (3) | 1.1328 (3) | 0.14343 (15) | 0.0273 (8) | |
C8 | 0.2205 (3) | 1.1605 (3) | 0.13872 (15) | 0.0264 (8) | |
C9 | 0.1869 (3) | 1.2733 (4) | 0.15514 (17) | 0.0392 (10) | |
H9 | 0.2375 | 1.3287 | 0.1731 | 0.047* | |
C10 | 0.0755 (3) | 1.3009 (4) | 0.1439 (2) | 0.0516 (12) | |
H10 | 0.0498 | 1.3752 | 0.1546 | 0.062* | |
C11 | 0.0038 (4) | 1.2166 (4) | 0.11684 (19) | 0.0496 (12) | |
H11 | −0.0707 | 1.2341 | 0.1075 | 0.060* | |
C12 | 0.0440 (3) | 1.1056 (4) | 0.10369 (16) | 0.0342 (9) | |
H12 | −0.0054 | 1.0489 | 0.0858 | 0.041* | |
C13 | −0.0898 (3) | 0.5854 (4) | 0.02645 (19) | 0.0527 (13) | |
H13A | −0.0490 | 0.6257 | 0.0000 | 0.079* | |
H13B | −0.1357 | 0.5247 | 0.0060 | 0.079* | |
H13C | −0.0397 | 0.5485 | 0.0569 | 0.079* | |
C14 | −0.2299 (3) | 0.7483 (4) | 0.00525 (17) | 0.0502 (12) | |
H14A | −0.2748 | 0.8043 | 0.0227 | 0.075* | |
H14B | −0.2760 | 0.6949 | −0.0200 | 0.075* | |
H14C | −0.1824 | 0.7915 | −0.0168 | 0.075* | |
C15 | −0.1608 (3) | 0.6758 (3) | 0.05252 (15) | 0.0276 (8) | |
C16 | −0.2276 (3) | 0.6246 (3) | 0.09918 (16) | 0.0282 (8) | |
C17 | −0.3508 (3) | 0.6170 (4) | 0.08142 (19) | 0.0464 (11) | |
H17A | −0.3841 | 0.5853 | 0.1131 | 0.070* | |
H17B | −0.3668 | 0.5649 | 0.0483 | 0.070* | |
H17C | −0.3795 | 0.6958 | 0.0716 | 0.070* | |
C18 | −0.1832 (4) | 0.5038 (4) | 0.12504 (19) | 0.0554 (12) | |
H18A | −0.1054 | 0.5102 | 0.1373 | 0.083* | |
H18B | −0.1974 | 0.4420 | 0.0961 | 0.083* | |
H18C | −0.2191 | 0.4840 | 0.1578 | 0.083* | |
C19 | −0.1140 (3) | 0.7868 (3) | 0.13971 (14) | 0.0248 (8) | |
C20 | −0.0612 (3) | 0.8733 (3) | 0.18217 (15) | 0.0267 (8) | |
C21 | −0.1226 (3) | 0.9372 (4) | 0.21670 (16) | 0.0403 (10) | |
H21 | −0.1983 | 0.9263 | 0.2131 | 0.048* | |
C22 | −0.0699 (3) | 1.0181 (4) | 0.25706 (17) | 0.0482 (12) | |
H22 | −0.1099 | 1.0657 | 0.2794 | 0.058* | |
C23 | 0.0425 (3) | 1.0260 (4) | 0.26313 (17) | 0.0444 (11) | |
H23 | 0.0809 | 1.0750 | 0.2915 | 0.053* | |
C24 | 0.0971 (3) | 0.9599 (3) | 0.22643 (15) | 0.0325 (9) | |
H24 | 0.1732 | 0.9670 | 0.2306 | 0.039* | |
N1 | 0.4181 (2) | 1.2129 (3) | 0.13688 (14) | 0.0360 (8) | |
N2 | 0.3810 (2) | 1.0241 (3) | 0.15072 (12) | 0.0269 (7) | |
N3 | 0.1495 (2) | 1.0751 (3) | 0.11510 (12) | 0.0269 (7) | |
N4 | −0.2016 (2) | 0.7157 (3) | 0.14721 (12) | 0.0272 (7) | |
N5 | −0.0869 (2) | 0.7638 (3) | 0.08801 (11) | 0.0224 (6) | |
N6 | 0.0488 (2) | 0.8867 (3) | 0.18532 (12) | 0.0281 (7) | |
N7 | 0.2135 (2) | 0.9484 (3) | −0.00603 (13) | 0.0334 (8) | |
N8 | 0.2955 (3) | 0.6582 (3) | 0.04797 (18) | 0.0544 (11) | |
N9 | 0.1719 (3) | 0.6418 (3) | 0.18668 (15) | 0.0360 (8) | |
O1 | 0.4056 (3) | 1.3255 (3) | 0.12888 (16) | 0.0603 (9) | |
O2 | 0.33022 (18) | 0.9255 (2) | 0.16160 (10) | 0.0279 (6) | |
O3 | 0.2273 (2) | 0.9783 (3) | −0.05526 (11) | 0.0507 (8) | |
O4 | 0.29363 (19) | 0.9350 (2) | 0.03460 (11) | 0.0364 (7) | |
O5 | 0.11923 (18) | 0.9293 (3) | 0.00678 (10) | 0.0352 (6) | |
O6 | 0.3472 (3) | 0.5873 (4) | 0.02285 (18) | 0.1058 (16) | |
O7 | 0.3335 (2) | 0.7016 (3) | 0.09700 (13) | 0.0468 (8) | |
O8 | 0.1999 (2) | 0.6941 (3) | 0.02583 (13) | 0.0475 (8) | |
O9 | 0.1640 (2) | 0.5585 (3) | 0.22000 (13) | 0.0593 (9) | |
O10 | 0.2374 (2) | 0.7298 (3) | 0.19933 (11) | 0.0395 (7) | |
O11 | 0.1141 (2) | 0.6446 (2) | 0.13669 (12) | 0.0393 (7) | |
O12 | −0.00934 (19) | 0.8177 (2) | 0.06566 (10) | 0.0284 (6) | |
O13 | −0.2481 (2) | 0.7132 (3) | 0.19264 (11) | 0.0446 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tb1 | 0.02218 (11) | 0.02498 (12) | 0.02300 (11) | −0.00103 (8) | 0.00341 (7) | −0.00178 (7) |
C1 | 0.027 (2) | 0.080 (4) | 0.044 (3) | 0.002 (2) | −0.0055 (19) | −0.003 (2) |
C2 | 0.0182 (18) | 0.048 (3) | 0.036 (2) | 0.0018 (18) | 0.0017 (16) | −0.0084 (19) |
C3 | 0.035 (2) | 0.048 (3) | 0.058 (3) | 0.009 (2) | 0.008 (2) | −0.009 (2) |
C4 | 0.032 (2) | 0.064 (4) | 0.089 (4) | −0.021 (2) | 0.008 (2) | −0.014 (3) |
C5 | 0.024 (2) | 0.039 (3) | 0.046 (2) | −0.0066 (18) | 0.0044 (18) | −0.0090 (19) |
C6 | 0.037 (2) | 0.072 (4) | 0.046 (3) | 0.002 (2) | 0.015 (2) | 0.003 (2) |
C7 | 0.029 (2) | 0.025 (2) | 0.0274 (19) | 0.0000 (16) | 0.0047 (16) | −0.0067 (16) |
C8 | 0.0275 (19) | 0.030 (2) | 0.0213 (18) | 0.0013 (17) | 0.0017 (15) | −0.0027 (16) |
C9 | 0.039 (2) | 0.036 (3) | 0.041 (2) | 0.006 (2) | −0.0012 (19) | −0.0101 (19) |
C10 | 0.044 (3) | 0.042 (3) | 0.068 (3) | 0.017 (2) | 0.006 (2) | −0.016 (2) |
C11 | 0.037 (2) | 0.048 (3) | 0.063 (3) | 0.011 (2) | 0.002 (2) | 0.000 (2) |
C12 | 0.032 (2) | 0.035 (2) | 0.035 (2) | 0.0023 (19) | 0.0012 (18) | 0.0041 (18) |
C13 | 0.055 (3) | 0.047 (3) | 0.062 (3) | −0.014 (2) | 0.029 (2) | −0.029 (2) |
C14 | 0.052 (3) | 0.058 (3) | 0.036 (2) | −0.016 (2) | −0.009 (2) | 0.011 (2) |
C15 | 0.0285 (19) | 0.027 (2) | 0.028 (2) | −0.0079 (16) | 0.0075 (16) | −0.0056 (16) |
C16 | 0.0277 (19) | 0.026 (2) | 0.032 (2) | −0.0048 (16) | 0.0066 (16) | −0.0013 (16) |
C17 | 0.031 (2) | 0.060 (3) | 0.049 (3) | −0.008 (2) | 0.008 (2) | −0.017 (2) |
C18 | 0.075 (3) | 0.037 (3) | 0.056 (3) | −0.001 (2) | 0.017 (3) | 0.009 (2) |
C19 | 0.0203 (18) | 0.028 (2) | 0.0268 (19) | −0.0005 (16) | 0.0058 (15) | 0.0018 (16) |
C20 | 0.0258 (19) | 0.027 (2) | 0.0267 (19) | −0.0001 (16) | 0.0033 (16) | −0.0018 (16) |
C21 | 0.029 (2) | 0.053 (3) | 0.041 (2) | −0.001 (2) | 0.0114 (18) | −0.013 (2) |
C22 | 0.050 (3) | 0.052 (3) | 0.046 (3) | 0.000 (2) | 0.018 (2) | −0.022 (2) |
C23 | 0.052 (3) | 0.046 (3) | 0.036 (2) | −0.011 (2) | 0.008 (2) | −0.016 (2) |
C24 | 0.030 (2) | 0.037 (2) | 0.030 (2) | −0.0058 (18) | 0.0021 (17) | −0.0068 (18) |
N1 | 0.0300 (17) | 0.0256 (19) | 0.053 (2) | −0.0054 (15) | 0.0079 (16) | −0.0078 (16) |
N2 | 0.0204 (15) | 0.033 (2) | 0.0263 (16) | −0.0030 (14) | 0.0013 (13) | −0.0074 (14) |
N3 | 0.0245 (15) | 0.0304 (19) | 0.0256 (16) | 0.0010 (14) | 0.0025 (13) | −0.0008 (14) |
N4 | 0.0262 (16) | 0.0329 (19) | 0.0233 (16) | −0.0043 (14) | 0.0068 (13) | −0.0005 (14) |
N5 | 0.0195 (14) | 0.0236 (17) | 0.0245 (15) | −0.0018 (13) | 0.0046 (12) | 0.0007 (13) |
N6 | 0.0255 (16) | 0.0309 (18) | 0.0274 (16) | −0.0010 (14) | 0.0025 (13) | −0.0003 (14) |
N7 | 0.0307 (18) | 0.041 (2) | 0.0296 (18) | −0.0005 (15) | 0.0072 (15) | 0.0003 (15) |
N8 | 0.054 (3) | 0.044 (3) | 0.068 (3) | 0.000 (2) | 0.019 (2) | −0.018 (2) |
N9 | 0.0303 (18) | 0.038 (2) | 0.041 (2) | 0.0093 (16) | 0.0062 (16) | 0.0095 (17) |
O1 | 0.057 (2) | 0.0310 (19) | 0.095 (3) | −0.0057 (15) | 0.0164 (19) | −0.0009 (17) |
O2 | 0.0255 (13) | 0.0275 (15) | 0.0287 (13) | 0.0003 (12) | −0.0025 (11) | −0.0024 (11) |
O3 | 0.0464 (17) | 0.078 (2) | 0.0306 (15) | −0.0007 (16) | 0.0160 (13) | 0.0132 (15) |
O4 | 0.0244 (13) | 0.0506 (19) | 0.0336 (15) | −0.0066 (13) | 0.0023 (12) | −0.0005 (13) |
O5 | 0.0211 (13) | 0.0544 (19) | 0.0299 (14) | −0.0065 (13) | 0.0032 (11) | 0.0036 (13) |
O6 | 0.086 (3) | 0.106 (4) | 0.126 (4) | 0.028 (3) | 0.020 (3) | −0.078 (3) |
O7 | 0.0440 (17) | 0.0422 (18) | 0.0526 (19) | 0.0099 (14) | 0.0009 (15) | −0.0186 (15) |
O8 | 0.0453 (18) | 0.0449 (19) | 0.0511 (19) | −0.0009 (15) | 0.0031 (15) | −0.0186 (15) |
O9 | 0.060 (2) | 0.056 (2) | 0.061 (2) | −0.0014 (17) | 0.0051 (16) | 0.0338 (18) |
O10 | 0.0340 (15) | 0.0411 (19) | 0.0404 (16) | 0.0008 (14) | −0.0043 (13) | 0.0035 (14) |
O11 | 0.0405 (16) | 0.0327 (17) | 0.0417 (17) | −0.0021 (13) | −0.0035 (14) | 0.0055 (13) |
O12 | 0.0236 (13) | 0.0353 (16) | 0.0272 (13) | −0.0062 (11) | 0.0071 (11) | 0.0011 (11) |
O13 | 0.0435 (16) | 0.061 (2) | 0.0340 (16) | −0.0152 (15) | 0.0210 (13) | −0.0046 (14) |
Tb1—O2 | 2.331 (2) | C13—H13B | 0.9600 |
Tb1—O12 | 2.376 (2) | C13—H13C | 0.9600 |
Tb1—O7 | 2.452 (3) | C14—C15 | 1.519 (5) |
Tb1—O11 | 2.463 (3) | C14—H14A | 0.9600 |
Tb1—O8 | 2.465 (3) | C14—H14B | 0.9600 |
Tb1—O5 | 2.486 (2) | C14—H14C | 0.9600 |
Tb1—O4 | 2.522 (2) | C15—N5 | 1.499 (4) |
Tb1—O10 | 2.538 (3) | C15—C16 | 1.561 (5) |
Tb1—N3 | 2.671 (3) | C16—N4 | 1.507 (5) |
Tb1—N6 | 2.711 (3) | C16—C17 | 1.513 (5) |
C1—C2 | 1.529 (5) | C16—C18 | 1.538 (5) |
C1—H1A | 0.9600 | C17—H17A | 0.9600 |
C1—H1B | 0.9600 | C17—H17B | 0.9600 |
C1—H1C | 0.9600 | C17—H17C | 0.9600 |
C2—N2 | 1.509 (4) | C18—H18A | 0.9600 |
C2—C3 | 1.518 (5) | C18—H18B | 0.9600 |
C2—C5 | 1.549 (5) | C18—H18C | 0.9600 |
C3—H3A | 0.9600 | C19—N5 | 1.319 (4) |
C3—H3B | 0.9600 | C19—N4 | 1.367 (4) |
C3—H3C | 0.9600 | C19—C20 | 1.461 (5) |
C4—C5 | 1.527 (5) | C20—N6 | 1.352 (4) |
C4—H4A | 0.9600 | C20—C21 | 1.376 (5) |
C4—H4B | 0.9600 | C21—C22 | 1.390 (5) |
C4—H4C | 0.9600 | C21—H21 | 0.9300 |
C5—N1 | 1.505 (5) | C22—C23 | 1.371 (5) |
C5—C6 | 1.521 (5) | C22—H22 | 0.9300 |
C6—H6A | 0.9600 | C23—C24 | 1.373 (5) |
C6—H6B | 0.9600 | C23—H23 | 0.9300 |
C6—H6C | 0.9600 | C24—N6 | 1.328 (4) |
C7—N2 | 1.321 (4) | C24—H24 | 0.9300 |
C7—N1 | 1.358 (5) | N1—O1 | 1.271 (4) |
C7—C8 | 1.459 (5) | N2—O2 | 1.305 (4) |
C8—N3 | 1.351 (4) | N4—O13 | 1.273 (3) |
C8—C9 | 1.391 (5) | N5—O12 | 1.297 (3) |
C9—C10 | 1.392 (5) | N7—O3 | 1.228 (4) |
C9—H9 | 0.9300 | N7—O5 | 1.256 (3) |
C10—C11 | 1.375 (6) | N7—O4 | 1.271 (4) |
C10—H10 | 0.9300 | N8—O6 | 1.214 (4) |
C11—C12 | 1.380 (6) | N8—O7 | 1.263 (5) |
C11—H11 | 0.9300 | N8—O8 | 1.277 (5) |
C12—N3 | 1.329 (4) | N9—O9 | 1.220 (4) |
C12—H12 | 0.9300 | N9—O11 | 1.272 (4) |
C13—C15 | 1.514 (5) | N9—O10 | 1.274 (4) |
C13—H13A | 0.9600 | ||
O2—Tb1—O12 | 155.19 (8) | C10—C11—H11 | 120.5 |
O2—Tb1—O7 | 74.92 (9) | C12—C11—H11 | 120.5 |
O12—Tb1—O7 | 129.47 (9) | N3—C12—C11 | 123.7 (4) |
O2—Tb1—O11 | 116.88 (9) | N3—C12—H12 | 118.2 |
O12—Tb1—O11 | 71.54 (9) | C11—C12—H12 | 118.2 |
O7—Tb1—O11 | 76.45 (10) | C15—C13—H13A | 109.5 |
O2—Tb1—O8 | 122.52 (9) | C15—C13—H13B | 109.5 |
O12—Tb1—O8 | 81.82 (9) | H13A—C13—H13B | 109.5 |
O7—Tb1—O8 | 52.04 (10) | C15—C13—H13C | 109.5 |
O11—Tb1—O8 | 74.29 (10) | H13A—C13—H13C | 109.5 |
O2—Tb1—O5 | 117.61 (8) | H13B—C13—H13C | 109.5 |
O12—Tb1—O5 | 63.44 (8) | C15—C14—H14A | 109.5 |
O7—Tb1—O5 | 108.89 (9) | C15—C14—H14B | 109.5 |
O11—Tb1—O5 | 124.61 (9) | H14A—C14—H14B | 109.5 |
O8—Tb1—O5 | 69.11 (10) | C15—C14—H14C | 109.5 |
O2—Tb1—O4 | 74.03 (8) | H14A—C14—H14C | 109.5 |
O12—Tb1—O4 | 113.97 (8) | H14B—C14—H14C | 109.5 |
O7—Tb1—O4 | 73.55 (10) | N5—C15—C13 | 108.4 (3) |
O11—Tb1—O4 | 143.77 (9) | N5—C15—C14 | 106.4 (3) |
O8—Tb1—O4 | 71.39 (9) | C13—C15—C14 | 110.8 (3) |
O5—Tb1—O4 | 50.79 (8) | N5—C15—C16 | 101.1 (3) |
O2—Tb1—O10 | 66.18 (9) | C13—C15—C16 | 115.4 (3) |
O12—Tb1—O10 | 114.46 (8) | C14—C15—C16 | 113.7 (3) |
O7—Tb1—O10 | 68.94 (10) | N4—C16—C17 | 109.6 (3) |
O11—Tb1—O10 | 51.20 (9) | N4—C16—C18 | 105.8 (3) |
O8—Tb1—O10 | 106.73 (10) | C17—C16—C18 | 110.0 (3) |
O5—Tb1—O10 | 175.35 (9) | N4—C16—C15 | 101.2 (3) |
O4—Tb1—O10 | 130.63 (8) | C17—C16—C15 | 115.9 (3) |
O2—Tb1—N3 | 69.33 (8) | C18—C16—C15 | 113.5 (3) |
O12—Tb1—N3 | 89.49 (8) | C16—C17—H17A | 109.5 |
O7—Tb1—N3 | 137.51 (9) | C16—C17—H17B | 109.5 |
O11—Tb1—N3 | 140.80 (9) | H17A—C17—H17B | 109.5 |
O8—Tb1—N3 | 138.05 (10) | C16—C17—H17C | 109.5 |
O5—Tb1—N3 | 70.31 (9) | H17A—C17—H17C | 109.5 |
O4—Tb1—N3 | 75.13 (9) | H17B—C17—H17C | 109.5 |
O10—Tb1—N3 | 114.14 (9) | C16—C18—H18A | 109.5 |
O2—Tb1—N6 | 91.06 (8) | C16—C18—H18B | 109.5 |
O12—Tb1—N6 | 68.48 (8) | H18A—C18—H18B | 109.5 |
O7—Tb1—N6 | 135.20 (10) | C16—C18—H18C | 109.5 |
O11—Tb1—N6 | 72.62 (9) | H18A—C18—H18C | 109.5 |
O8—Tb1—N6 | 140.94 (10) | H18B—C18—H18C | 109.5 |
O5—Tb1—N6 | 115.22 (8) | N5—C19—N4 | 108.2 (3) |
O4—Tb1—N6 | 143.59 (9) | N5—C19—C20 | 126.7 (3) |
O10—Tb1—N6 | 66.49 (9) | N4—C19—C20 | 125.1 (3) |
N3—Tb1—N6 | 68.51 (9) | N6—C20—C21 | 122.7 (3) |
C2—C1—H1A | 109.5 | N6—C20—C19 | 116.8 (3) |
C2—C1—H1B | 109.5 | C21—C20—C19 | 120.5 (3) |
H1A—C1—H1B | 109.5 | C20—C21—C22 | 119.1 (4) |
C2—C1—H1C | 109.5 | C20—C21—H21 | 120.4 |
H1A—C1—H1C | 109.5 | C22—C21—H21 | 120.4 |
H1B—C1—H1C | 109.5 | C23—C22—C21 | 118.3 (4) |
N2—C2—C3 | 109.7 (3) | C23—C22—H22 | 120.8 |
N2—C2—C1 | 105.9 (3) | C21—C22—H22 | 120.8 |
C3—C2—C1 | 110.6 (3) | C22—C23—C24 | 118.6 (4) |
N2—C2—C5 | 99.9 (3) | C22—C23—H23 | 120.7 |
C3—C2—C5 | 115.4 (3) | C24—C23—H23 | 120.7 |
C1—C2—C5 | 114.4 (3) | N6—C24—C23 | 124.6 (4) |
C2—C3—H3A | 109.5 | N6—C24—H24 | 117.7 |
C2—C3—H3B | 109.5 | C23—C24—H24 | 117.7 |
H3A—C3—H3B | 109.5 | O1—N1—C7 | 126.0 (3) |
C2—C3—H3C | 109.5 | O1—N1—C5 | 122.1 (3) |
H3A—C3—H3C | 109.5 | C7—N1—C5 | 110.4 (3) |
H3B—C3—H3C | 109.5 | O2—N2—C7 | 126.6 (3) |
C5—C4—H4A | 109.5 | O2—N2—C2 | 120.1 (3) |
C5—C4—H4B | 109.5 | C7—N2—C2 | 112.7 (3) |
H4A—C4—H4B | 109.5 | C12—N3—C8 | 117.2 (3) |
C5—C4—H4C | 109.5 | C12—N3—Tb1 | 112.1 (3) |
H4A—C4—H4C | 109.5 | C8—N3—Tb1 | 129.8 (2) |
H4B—C4—H4C | 109.5 | O13—N4—C19 | 125.1 (3) |
N1—C5—C6 | 105.6 (3) | O13—N4—C16 | 121.9 (3) |
N1—C5—C4 | 109.4 (3) | C19—N4—C16 | 112.3 (3) |
C6—C5—C4 | 110.2 (3) | O12—N5—C19 | 125.1 (3) |
N1—C5—C2 | 100.6 (3) | O12—N5—C15 | 120.2 (3) |
C6—C5—C2 | 114.6 (3) | C19—N5—C15 | 114.5 (3) |
C4—C5—C2 | 115.4 (4) | C24—N6—C20 | 116.4 (3) |
C5—C6—H6A | 109.5 | C24—N6—Tb1 | 112.0 (2) |
C5—C6—H6B | 109.5 | C20—N6—Tb1 | 129.2 (2) |
H6A—C6—H6B | 109.5 | O3—N7—O5 | 121.6 (3) |
C5—C6—H6C | 109.5 | O3—N7—O4 | 121.9 (3) |
H6A—C6—H6C | 109.5 | O5—N7—O4 | 116.5 (3) |
H6B—C6—H6C | 109.5 | O6—N8—O7 | 122.1 (4) |
N2—C7—N1 | 109.0 (3) | O6—N8—O8 | 121.6 (4) |
N2—C7—C8 | 125.4 (3) | O7—N8—O8 | 116.3 (3) |
N1—C7—C8 | 125.5 (3) | O9—N9—O11 | 121.0 (4) |
N3—C8—C9 | 123.0 (3) | O9—N9—O10 | 122.8 (4) |
N3—C8—C7 | 117.0 (3) | O11—N9—O10 | 116.2 (3) |
C9—C8—C7 | 119.9 (3) | N2—O2—Tb1 | 126.72 (19) |
C8—C9—C10 | 118.1 (4) | N7—O4—Tb1 | 94.75 (18) |
C8—C9—H9 | 120.9 | N7—O5—Tb1 | 96.88 (19) |
C10—C9—H9 | 120.9 | N8—O7—Tb1 | 96.3 (2) |
C11—C10—C9 | 118.9 (4) | N8—O8—Tb1 | 95.3 (2) |
C11—C10—H10 | 120.5 | N9—O10—Tb1 | 94.5 (2) |
C9—C10—H10 | 120.5 | N9—O11—Tb1 | 98.1 (2) |
C10—C11—C12 | 119.0 (4) | N5—O12—Tb1 | 129.14 (19) |
N2—C2—C5—N1 | 24.8 (3) | C19—C20—N6—Tb1 | 23.2 (5) |
C3—C2—C5—N1 | 142.3 (3) | O2—Tb1—N6—C24 | 11.2 (3) |
C1—C2—C5—N1 | −87.8 (4) | O12—Tb1—N6—C24 | −154.4 (3) |
N2—C2—C5—C6 | −87.9 (3) | O7—Tb1—N6—C24 | 80.7 (3) |
C3—C2—C5—C6 | 29.6 (5) | O11—Tb1—N6—C24 | 129.1 (3) |
C1—C2—C5—C6 | 159.5 (3) | O8—Tb1—N6—C24 | 162.4 (2) |
N2—C2—C5—C4 | 142.4 (3) | O5—Tb1—N6—C24 | −110.2 (3) |
C3—C2—C5—C4 | −100.1 (4) | O4—Tb1—N6—C24 | −52.8 (3) |
C1—C2—C5—C4 | 29.8 (5) | O10—Tb1—N6—C24 | 74.6 (3) |
N2—C7—C8—N3 | −30.5 (5) | N3—Tb1—N6—C24 | −56.0 (3) |
N1—C7—C8—N3 | 144.5 (4) | O2—Tb1—N6—C20 | 172.7 (3) |
N2—C7—C8—C9 | 153.1 (4) | O12—Tb1—N6—C20 | 7.1 (3) |
N1—C7—C8—C9 | −31.9 (6) | O7—Tb1—N6—C20 | −117.8 (3) |
N3—C8—C9—C10 | −3.3 (6) | O11—Tb1—N6—C20 | −69.4 (3) |
C7—C8—C9—C10 | 172.9 (4) | O8—Tb1—N6—C20 | −36.1 (4) |
C8—C9—C10—C11 | −0.6 (7) | O5—Tb1—N6—C20 | 51.3 (3) |
C9—C10—C11—C12 | 2.5 (7) | O4—Tb1—N6—C20 | 108.7 (3) |
C10—C11—C12—N3 | −0.9 (7) | O10—Tb1—N6—C20 | −123.9 (3) |
N5—C15—C16—N4 | 14.8 (3) | N3—Tb1—N6—C20 | 105.5 (3) |
C13—C15—C16—N4 | 131.5 (3) | C7—N2—O2—Tb1 | 59.6 (4) |
C14—C15—C16—N4 | −98.8 (3) | C2—N2—O2—Tb1 | −129.8 (3) |
N5—C15—C16—C17 | 133.3 (3) | O12—Tb1—O2—N2 | −79.2 (3) |
C13—C15—C16—C17 | −110.0 (4) | O7—Tb1—O2—N2 | 110.4 (2) |
C14—C15—C16—C17 | 19.7 (5) | O11—Tb1—O2—N2 | 176.3 (2) |
N5—C15—C16—C18 | −98.0 (3) | O8—Tb1—O2—N2 | 88.4 (3) |
C13—C15—C16—C18 | 18.7 (5) | O5—Tb1—O2—N2 | 6.7 (3) |
C14—C15—C16—C18 | 148.3 (4) | O4—Tb1—O2—N2 | 33.6 (2) |
N5—C19—C20—N6 | −35.5 (6) | O10—Tb1—O2—N2 | −176.3 (3) |
N4—C19—C20—N6 | 144.9 (3) | N3—Tb1—O2—N2 | −46.2 (2) |
N5—C19—C20—C21 | 144.4 (4) | N6—Tb1—O2—N2 | −112.7 (2) |
N4—C19—C20—C21 | −35.2 (6) | O3—N7—O4—Tb1 | −169.6 (3) |
N6—C20—C21—C22 | −0.7 (6) | O5—N7—O4—Tb1 | 10.4 (3) |
C19—C20—C21—C22 | 179.4 (4) | O2—Tb1—O4—N7 | −154.9 (2) |
C20—C21—C22—C23 | −3.7 (7) | O12—Tb1—O4—N7 | 0.1 (2) |
C21—C22—C23—C24 | 4.4 (7) | O7—Tb1—O4—N7 | 126.5 (2) |
C22—C23—C24—N6 | −0.9 (7) | O11—Tb1—O4—N7 | 91.3 (2) |
N2—C7—N1—O1 | 179.9 (4) | O8—Tb1—O4—N7 | 71.8 (2) |
C8—C7—N1—O1 | 4.2 (6) | O5—Tb1—O4—N7 | −6.03 (18) |
N2—C7—N1—C5 | 13.8 (4) | O10—Tb1—O4—N7 | 168.19 (18) |
C8—C7—N1—C5 | −161.8 (3) | N3—Tb1—O4—N7 | −82.5 (2) |
C6—C5—N1—O1 | −72.5 (4) | N6—Tb1—O4—N7 | −85.7 (2) |
C4—C5—N1—O1 | 46.2 (5) | O3—N7—O5—Tb1 | 169.4 (3) |
C2—C5—N1—O1 | 168.1 (4) | O4—N7—O5—Tb1 | −10.6 (3) |
C6—C5—N1—C7 | 94.2 (4) | O2—Tb1—O5—N7 | 40.3 (2) |
C4—C5—N1—C7 | −147.2 (4) | O12—Tb1—O5—N7 | −167.6 (2) |
C2—C5—N1—C7 | −25.2 (4) | O7—Tb1—O5—N7 | −42.2 (2) |
N1—C7—N2—O2 | 175.9 (3) | O11—Tb1—O5—N7 | −128.4 (2) |
C8—C7—N2—O2 | −8.4 (6) | O8—Tb1—O5—N7 | −76.4 (2) |
N1—C7—N2—C2 | 4.7 (4) | O4—Tb1—O5—N7 | 6.13 (19) |
C8—C7—N2—C2 | −179.6 (3) | N3—Tb1—O5—N7 | 92.7 (2) |
C3—C2—N2—O2 | 46.7 (4) | N6—Tb1—O5—N7 | 145.9 (2) |
C1—C2—N2—O2 | −72.7 (4) | O6—N8—O7—Tb1 | 175.6 (4) |
C5—C2—N2—O2 | 168.3 (3) | O8—N8—O7—Tb1 | −3.7 (4) |
C3—C2—N2—C7 | −141.5 (3) | O2—Tb1—O7—N8 | −154.2 (3) |
C1—C2—N2—C7 | 99.2 (4) | O12—Tb1—O7—N8 | 31.0 (3) |
C5—C2—N2—C7 | −19.8 (4) | O11—Tb1—O7—N8 | 82.7 (2) |
C11—C12—N3—C8 | −2.8 (5) | O8—Tb1—O7—N8 | 2.2 (2) |
C11—C12—N3—Tb1 | 167.1 (3) | O5—Tb1—O7—N8 | −39.7 (3) |
C9—C8—N3—C12 | 4.9 (5) | O4—Tb1—O7—N8 | −76.8 (2) |
C7—C8—N3—C12 | −171.4 (3) | O10—Tb1—O7—N8 | 135.9 (3) |
C9—C8—N3—Tb1 | −162.9 (3) | N3—Tb1—O7—N8 | −120.9 (2) |
C7—C8—N3—Tb1 | 20.9 (4) | N6—Tb1—O7—N8 | 129.9 (2) |
O2—Tb1—N3—C12 | −159.6 (3) | O6—N8—O8—Tb1 | −175.6 (4) |
O12—Tb1—N3—C12 | 7.2 (2) | O7—N8—O8—Tb1 | 3.7 (4) |
O7—Tb1—N3—C12 | 165.9 (2) | O2—Tb1—O8—N8 | 25.2 (3) |
O11—Tb1—N3—C12 | −52.0 (3) | O12—Tb1—O8—N8 | −160.0 (3) |
O8—Tb1—N3—C12 | 84.3 (3) | O7—Tb1—O8—N8 | −2.1 (2) |
O5—Tb1—N3—C12 | 69.1 (2) | O11—Tb1—O8—N8 | −87.0 (2) |
O4—Tb1—N3—C12 | 122.2 (2) | O5—Tb1—O8—N8 | 135.3 (3) |
O10—Tb1—N3—C12 | −109.5 (2) | O4—Tb1—O8—N8 | 81.2 (2) |
N6—Tb1—N3—C12 | −59.8 (2) | O10—Tb1—O8—N8 | −46.9 (3) |
O2—Tb1—N3—C8 | 8.7 (3) | N3—Tb1—O8—N8 | 119.9 (2) |
O12—Tb1—N3—C8 | 175.4 (3) | N6—Tb1—O8—N8 | −120.0 (2) |
O7—Tb1—N3—C8 | −25.9 (3) | O9—N9—O10—Tb1 | −178.7 (3) |
O11—Tb1—N3—C8 | 116.2 (3) | O11—N9—O10—Tb1 | 1.4 (3) |
O8—Tb1—N3—C8 | −107.4 (3) | O2—Tb1—O10—N9 | −172.4 (2) |
O5—Tb1—N3—C8 | −122.7 (3) | O12—Tb1—O10—N9 | 34.8 (2) |
O4—Tb1—N3—C8 | −69.5 (3) | O7—Tb1—O10—N9 | −90.1 (2) |
O10—Tb1—N3—C8 | 58.7 (3) | O11—Tb1—O10—N9 | −0.85 (18) |
N6—Tb1—N3—C8 | 108.5 (3) | O8—Tb1—O10—N9 | −53.7 (2) |
N5—C19—N4—O13 | 178.9 (3) | N3—Tb1—O10—N9 | 135.97 (19) |
C20—C19—N4—O13 | −1.5 (6) | N6—Tb1—O10—N9 | 85.2 (2) |
N5—C19—N4—C16 | 7.9 (4) | O9—N9—O11—Tb1 | 178.6 (3) |
C20—C19—N4—C16 | −172.4 (3) | O10—N9—O11—Tb1 | −1.5 (3) |
C17—C16—N4—O13 | 50.9 (5) | O2—Tb1—O11—N9 | 9.5 (2) |
C18—C16—N4—O13 | −67.6 (4) | O12—Tb1—O11—N9 | −145.1 (2) |
C15—C16—N4—O13 | 173.8 (3) | O7—Tb1—O11—N9 | 74.6 (2) |
C17—C16—N4—C19 | −137.8 (3) | O8—Tb1—O11—N9 | 128.4 (2) |
C18—C16—N4—C19 | 103.7 (3) | O5—Tb1—O11—N9 | 178.35 (18) |
C15—C16—N4—C19 | −14.9 (4) | O4—Tb1—O11—N9 | 109.3 (2) |
N4—C19—N5—O12 | 177.7 (3) | O10—Tb1—O11—N9 | 0.86 (18) |
C20—C19—N5—O12 | −1.9 (6) | N3—Tb1—O11—N9 | −80.2 (2) |
N4—C19—N5—C15 | 3.4 (4) | N6—Tb1—O11—N9 | −72.6 (2) |
C20—C19—N5—C15 | −176.3 (3) | C19—N5—O12—Tb1 | 55.5 (4) |
C13—C15—N5—O12 | 51.4 (4) | C15—N5—O12—Tb1 | −130.4 (3) |
C14—C15—N5—O12 | −67.9 (4) | O2—Tb1—O12—N5 | −82.1 (3) |
C16—C15—N5—O12 | 173.1 (3) | O7—Tb1—O12—N5 | 85.8 (3) |
C13—C15—N5—C19 | −134.0 (3) | O11—Tb1—O12—N5 | 32.3 (2) |
C14—C15—N5—C19 | 106.7 (4) | O8—Tb1—O12—N5 | 108.4 (3) |
C16—C15—N5—C19 | −12.3 (4) | O5—Tb1—O12—N5 | 179.1 (3) |
C23—C24—N6—C20 | −3.4 (6) | O4—Tb1—O12—N5 | 173.8 (2) |
C23—C24—N6—Tb1 | 160.7 (3) | O10—Tb1—O12—N5 | 3.7 (3) |
C21—C20—N6—C24 | 4.1 (5) | N3—Tb1—O12—N5 | −112.8 (3) |
C19—C20—N6—C24 | −176.0 (3) | N6—Tb1—O12—N5 | −45.8 (2) |
C21—C20—N6—Tb1 | −156.7 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C22—H22···O13i | 0.93 | 2.55 | 3.440 (5) | 161 |
C17—H17B···O6ii | 0.96 | 2.40 | 3.327 (5) | 161 |
C6—H6B···O3iii | 0.96 | 2.55 | 3.473 (5) | 161 |
C24—H24···O9iv | 0.93 | 2.38 | 3.211 (5) | 148 |
Symmetry codes: (i) −x−1/2, y+1/2, −z+1/2; (ii) −x, −y+1, −z; (iii) −x+1, −y+2, −z; (iv) −x+1/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Tb(NO3)3(C12H16N3O2)2] |
Mr | 813.51 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 12.292 (3), 11.114 (2), 23.264 (5) |
β (°) | 98.37 (3) |
V (Å3) | 3144.6 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.33 |
Crystal size (mm) | 0.20 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Rigaku Saturn CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.581, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25443, 5554, 4726 |
Rint | 0.059 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.071, 1.01 |
No. of reflections | 5554 |
No. of parameters | 432 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.89, −0.95 |
Computer programs: CrystalClear (Rigaku, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
C22—H22···O13i | 0.93 | 2.55 | 3.440 (5) | 161 |
C17—H17B···O6ii | 0.96 | 2.40 | 3.327 (5) | 161 |
C6—H6B···O3iii | 0.96 | 2.55 | 3.473 (5) | 161 |
C24—H24···O9iv | 0.93 | 2.38 | 3.211 (5) | 148 |
Symmetry codes: (i) −x−1/2, y+1/2, −z+1/2; (ii) −x, −y+1, −z; (iii) −x+1, −y+2, −z; (iv) −x+1/2, y+1/2, −z+1/2. |
Acknowledgements
The author thanks the Chemical Institute of Linyi University for supporting this work.
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As a continuation of our work on complexes containing nitroxide radicals as the ligand, the title Tb complex is reported. An ORTEP drawing of [TbIII(NIT2Py)2(NO3)3] is illustrated in Fig. 1. The TbIII ion is ten-coordinated by three η2-nitrato anions and two NIT2Py radicals which bind via one oxygen atom of the nitronyl nitroxide moiety and one nitrogen atom of the pyridine substituent. The complex is further connected by weak C—H···O H-bonds into a three-dimensional framework as shown in Fig. 2.