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The title compound, [Tb(NO3)3(C18H15OP)3]·1.5(CH3)2CO, contains discrete mol­ecules with nine-coordinate Tb atoms, all nitrate groups being bonded as symmetrical bidentate ligands; Tb—O(P) = 2.307 (4), 2.309 (4) and 2.295 (4) Å, and Tb—O(N) = 2.467 (4)-2.539 (4) Å).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680300967X/bt6278sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680300967X/bt6278Isup2.hkl
Contains datablock I

CCDC reference: 214775

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.010 Å
  • Disorder in solvent or counterion
  • R factor = 0.054
  • wR factor = 0.135
  • Data-to-parameter ratio = 14.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.111 PLAT_302 Alert C Anion/Solvent Disorder ....................... 25.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

As part of a continuing study into the solution equilibria found in lanthanide complexes of phosphine oxides, the complex [Tb(NO3)3(Ph3PO)3]·1.5Me2CO, (I), was isolated (Cousins & Hart, 1967). The crystal structure reveals a nine-coordinate terbium bonded to three bidentate nitrate groups and three phosphine oxides, with 1.5 acetone molecules in the asymmetric unit, the latter arising from a partial occupancy for one solvate molecule. The three (P)O—Tb—O(P) angles (Table 1) show that this complex may be described as mer-(pseudo)octahedral, where the nitrate ligands have been replaced conceptually by monodentate ligands. The nitrate groups are symmetrically bonded with the Oc—N—Oc angle smaller (average 116°) than the idealized value in the free D3 h NO3 anion, where Oc is a coordinated O atom. As described previously (Valle et al., 1986), the N—Oc distances are ca 0.05 Å longer than N—Ot, where Ot is the terminal O atom. The M—O—P angles are very variable among phosphine oxide complexes and in the present compound are 154.7 (3), 159.6 (3) and 173.8 (3)°.

Five other structurally characterized compounds with the same stoichiometry are known for Y (Deakin et al., 2000), La (Huang et al., 1987), Ce (Lin et al., 1994), Sm (Sakamoto & Miyake, 1993) and Eu (Valle et al., 1986) and all have a similar structure and are solvated (2Me2CO for Ce, Sm and Eu).

The Tb—O(P) and Tb—O(N) distances are a little longer than the corresponding values found in [Y(NO3)3(Ph3PO)3].xCH2Cl2 (Deakin et al., 2000), where the Y compound is again `mer' and reflecting the ionic radii [M3+ (eight-coordinate): Y 1.159 Å and Tb 1.180 Å (Shannon, 1976)].

Experimental top

Cooling a boiling acetone solution of Tb(NO3)3·6H2O and Ph3PO (1:3) gave the title compound. Suitable crystals were isolated from the reaction product.

Refinement top

The large displacement parameter values of all the atoms of one of the acetone solvate molecules suggested partial occupancy and the site-occupancy factor was set to 0.5 to bring the values close to those of the other acetone molecule. The atoms with sof of 0.5 were refined isotropically. H atoms were placed in calculated positions with a displacement parameter related to that of the bonded C atom.

Computing details top

Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976).

Figures top
[Figure 1] Fig. 1. The molecular structure of [Tb(NO3)3(Ph3PO)3], showing the atom-labelling scheme. Ellipsoids are drawn at the 50% probability level and H atoms have been omitted for clarity.
Tris(nitrato-κ2O,O')tris(triphenylphosphine oxide-κO)terbium(III) acetone solvate top
Crystal data top
[Tb(NO3)3(C18H15OP)3]·1.5C3H6OF(000) = 2576
Mr = 1266.88Dx = 1.440 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 41633 reflections
a = 11.0612 (10) Åθ = 2.9–27.5°
b = 19.180 (2) ŵ = 1.36 mm1
c = 27.641 (4) ÅT = 120 K
β = 94.895 (7)°Block, colourless
V = 5842.7 (12) Å30.16 × 0.16 × 0.10 mm
Z = 4
Data collection top
Nonius KappaCCD area-detector
diffractometer
10247 independent reflections
Radiation source: Nonius rotating anode6620 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.111
ϕ and ω scansθmax = 25.0°, θmin = 3.0°
Absorption correction: multi-scan
(SORTAV; Blessing, 1997)
h = 1312
Tmin = 0.847, Tmax = 0.873k = 2222
40261 measured reflectionsl = 3231
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.054H-atom parameters constrained
wR(F2) = 0.135 w = 1/[σ2(Fo2) + (0.0194P)2 + 9.57P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.002
10247 reflectionsΔρmax = 1.24 e Å3
711 parametersΔρmin = 0.83 e Å3
3 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00179 (16)
Crystal data top
[Tb(NO3)3(C18H15OP)3]·1.5C3H6OV = 5842.7 (12) Å3
Mr = 1266.88Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.0612 (10) ŵ = 1.36 mm1
b = 19.180 (2) ÅT = 120 K
c = 27.641 (4) Å0.16 × 0.16 × 0.10 mm
β = 94.895 (7)°
Data collection top
Nonius KappaCCD area-detector
diffractometer
10247 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1997)
6620 reflections with I > 2σ(I)
Tmin = 0.847, Tmax = 0.873Rint = 0.111
40261 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0543 restraints
wR(F2) = 0.135H-atom parameters constrained
S = 1.03Δρmax = 1.24 e Å3
10247 reflectionsΔρmin = 0.83 e Å3
711 parameters
Special details top

Experimental. Weak data with <I/sigma(I)> = 3.0 probably responsible for the high Rint.

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.

The sof of one acetone was set to 0.5 to reduce the large U values of the 3 C and 1 O atoms to values similar to the other acetone. DFIX (C—C, C—O) used on the half acetone to improve geometry.

Using AFIX 137 to obtain torsion angles for acetone Me groups failed to converge satisfactorily for C55 and for the final cycles AFIX 33 was used.

The 2theta limit was set to 50 ° as reflections at higher angles were weak and gave a poor R value. Removing these reflections had only a small effect on the final R values.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Tb11.10010 (2)0.248402 (15)0.134232 (10)0.01771 (12)
P10.76300 (14)0.25817 (8)0.11968 (6)0.0218 (4)
P21.08219 (14)0.29973 (8)0.26469 (6)0.0194 (4)
P31.11773 (14)0.29999 (8)0.00253 (6)0.0198 (4)
O10.8960 (4)0.2680 (2)0.11452 (17)0.0235 (10)
O21.0603 (4)0.2769 (2)0.21248 (15)0.0217 (10)
O31.1194 (4)0.2807 (2)0.05533 (15)0.0215 (10)
O41.0303 (5)0.1357 (2)0.16464 (18)0.0365 (12)
O51.0311 (4)0.1429 (2)0.08698 (19)0.0367 (12)
O60.9640 (5)0.0482 (2)0.1197 (2)0.0419 (14)
O71.2864 (4)0.1893 (3)0.11181 (19)0.0375 (13)
O81.2696 (4)0.1970 (2)0.18873 (18)0.0325 (11)
O91.4284 (5)0.1472 (4)0.1634 (2)0.069 (2)
O101.2590 (4)0.3379 (2)0.14605 (16)0.0223 (10)
O111.0774 (4)0.3801 (2)0.13611 (16)0.0226 (10)
O121.2317 (4)0.4500 (2)0.14810 (18)0.0312 (12)
O130.1107 (4)0.3797 (2)0.84533 (18)0.0356 (12)
O140.6420 (8)0.0782 (5)0.8947 (4)0.035 (2)*0.50
N11.0075 (5)0.1070 (3)0.1235 (2)0.0289 (14)
N21.3313 (5)0.1766 (3)0.1551 (2)0.0368 (15)
N31.1901 (5)0.3917 (3)0.14330 (19)0.0213 (12)
C10.6882 (6)0.2252 (3)0.0639 (3)0.0244 (15)
C20.7571 (6)0.2059 (3)0.0267 (3)0.0324 (17)
H20.84310.20860.03120.039*
C30.7011 (7)0.1826 (4)0.0173 (3)0.042 (2)
H30.74830.17020.04320.050*
C40.5764 (8)0.1777 (4)0.0230 (3)0.047 (2)
H40.53780.16230.05320.056*
C50.5067 (7)0.1948 (4)0.0143 (3)0.045 (2)
H50.42110.18940.01000.054*
C60.5608 (6)0.2199 (4)0.0584 (3)0.0383 (19)
H60.51300.23300.08390.046*
C70.6983 (5)0.3414 (3)0.1333 (2)0.0227 (15)
C80.5790 (5)0.3487 (3)0.1463 (3)0.0268 (16)
H80.53120.30860.15120.032*
C90.5310 (6)0.4153 (4)0.1520 (3)0.0334 (17)
H90.45010.42050.16050.040*
C100.6010 (6)0.4736 (4)0.1454 (3)0.0291 (16)
H100.56750.51880.14890.035*
C110.7199 (6)0.4667 (4)0.1336 (3)0.0299 (16)
H110.76810.50690.12960.036*
C120.7681 (6)0.4010 (3)0.1277 (2)0.0223 (15)
H120.84960.39640.11970.027*
C130.7379 (6)0.1971 (3)0.1661 (3)0.0252 (15)
C140.7545 (6)0.2169 (4)0.2150 (3)0.0339 (17)
H140.76270.26490.22310.041*
C150.7590 (6)0.1674 (4)0.2516 (3)0.0327 (17)
H150.77210.18170.28460.039*
C160.7448 (7)0.0986 (4)0.2408 (3)0.0366 (18)
H160.74930.06460.26590.044*
C170.7234 (8)0.0783 (4)0.1919 (3)0.045 (2)
H170.71010.03060.18410.054*
C180.7216 (7)0.1272 (3)0.1553 (3)0.0345 (18)
H180.70910.11270.12240.041*
C190.9457 (5)0.3351 (3)0.2861 (2)0.0206 (14)
C200.8751 (6)0.3796 (3)0.2546 (3)0.0260 (16)
H200.90230.39230.22410.031*
C210.7663 (6)0.4047 (3)0.2681 (3)0.0308 (17)
H210.71840.43440.24670.037*
C220.7258 (6)0.3873 (4)0.3128 (3)0.0327 (17)
H220.65070.40500.32190.039*
C230.7951 (6)0.3441 (4)0.3438 (3)0.0332 (17)
H230.76830.33270.37460.040*
C240.9040 (6)0.3171 (3)0.3305 (2)0.0261 (16)
H240.95000.28630.35170.031*
C251.1995 (6)0.3649 (3)0.2730 (2)0.0218 (14)
C261.1785 (7)0.4308 (4)0.2909 (3)0.0382 (19)
H261.10070.44360.30010.046*
C271.2756 (7)0.4784 (4)0.2952 (3)0.041 (2)
H271.26270.52370.30750.049*
C281.3868 (7)0.4612 (4)0.2822 (3)0.0389 (19)
H281.45090.49430.28540.047*
C291.4071 (6)0.3951 (4)0.2642 (3)0.0356 (18)
H291.48570.38230.25590.043*
C301.3128 (6)0.3483 (4)0.2586 (2)0.0262 (15)
H301.32570.30390.24460.031*
C311.1271 (5)0.2279 (3)0.3035 (2)0.0200 (14)
C321.1786 (5)0.2382 (3)0.3506 (2)0.0258 (15)
H321.19220.28410.36290.031*
C331.2102 (6)0.1803 (4)0.3797 (3)0.0285 (16)
H331.24440.18680.41200.034*
C341.1923 (5)0.1139 (3)0.3618 (3)0.0269 (16)
H341.21460.07510.38190.032*
C351.1424 (6)0.1029 (3)0.3151 (2)0.0250 (15)
H351.13030.05680.30310.030*
C361.1096 (5)0.1597 (3)0.2856 (3)0.0248 (15)
H361.07540.15250.25330.030*
C371.2653 (6)0.3292 (3)0.0123 (2)0.0208 (14)
C381.3441 (6)0.3573 (3)0.0241 (3)0.0297 (16)
H381.32220.35840.05660.036*
C391.4561 (6)0.3843 (4)0.0130 (3)0.0342 (17)
H391.51020.40390.03790.041*
C401.4875 (6)0.3823 (4)0.0340 (3)0.0361 (18)
H401.56330.40080.04150.043*
C411.4097 (6)0.3536 (4)0.0702 (3)0.0356 (18)
H411.43270.35210.10250.043*
C421.2992 (6)0.3271 (3)0.0601 (3)0.0281 (16)
H421.24600.30740.08530.034*
C431.0747 (5)0.2271 (3)0.0362 (2)0.0197 (14)
C441.0073 (6)0.2354 (3)0.0802 (3)0.0267 (16)
H440.98410.28080.09110.032*
C450.9728 (6)0.1779 (4)0.1089 (3)0.0320 (17)
H450.92840.18400.13950.038*
C461.0037 (6)0.1123 (4)0.0924 (3)0.0311 (17)
H460.97810.07280.11130.037*
C471.0717 (7)0.1031 (4)0.0485 (3)0.0378 (19)
H471.09430.05750.03780.045*
C481.1070 (6)0.1608 (3)0.0200 (3)0.0305 (17)
H481.15290.15470.01030.037*
C491.0109 (5)0.3693 (3)0.0126 (2)0.0208 (14)
C501.0277 (6)0.4170 (3)0.0496 (2)0.0253 (15)
H501.09760.41430.06720.030*
C510.9409 (6)0.4685 (3)0.0604 (3)0.0251 (15)
H510.95140.50070.08590.030*
C520.8408 (6)0.4733 (3)0.0348 (3)0.0262 (16)
H520.78200.50860.04250.031*
C530.8250 (6)0.4262 (3)0.0028 (3)0.0262 (16)
H530.75610.43000.02090.031*
C540.9095 (5)0.3742 (3)0.0138 (2)0.0239 (15)
H540.89840.34200.03910.029*
C550.0257 (7)0.4484 (4)0.7936 (3)0.049 (2)
H55A0.02160.48770.80780.074*
H55B0.11010.45260.80150.074*
H55C0.02280.44870.75820.074*
C560.0268 (6)0.3814 (4)0.8138 (3)0.0336 (17)
C570.0265 (7)0.3153 (4)0.7917 (3)0.0382 (19)
H57A0.02370.27550.80320.057*
H57B0.02880.31820.75630.057*
H57C0.10910.30910.80130.057*
C580.7265 (11)0.0157 (7)0.9406 (5)0.031 (3)*0.50
H58A0.79970.01320.94460.047*0.50
H58B0.74360.05810.92260.047*0.50
H58C0.70130.02840.97260.047*0.50
C590.6266 (9)0.0244 (6)0.9130 (5)0.031 (3)*0.50
C600.5047 (11)0.0091 (8)0.9114 (6)0.044 (4)*0.50
H60A0.44750.01710.88930.066*0.50
H60B0.47630.00910.94400.066*0.50
H60C0.51030.05720.89980.066*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.01795 (17)0.01872 (18)0.01637 (19)0.00065 (14)0.00092 (11)0.00049 (14)
P10.0185 (8)0.0247 (9)0.0222 (10)0.0004 (7)0.0014 (7)0.0013 (8)
P20.0201 (8)0.0212 (8)0.0170 (10)0.0005 (7)0.0014 (7)0.0019 (7)
P30.0216 (8)0.0212 (8)0.0164 (10)0.0003 (7)0.0007 (7)0.0007 (7)
O10.020 (2)0.024 (2)0.027 (3)0.0006 (18)0.0032 (19)0.0025 (19)
O20.029 (2)0.020 (2)0.016 (3)0.0036 (19)0.0065 (19)0.0032 (18)
O30.026 (2)0.025 (2)0.014 (3)0.0019 (19)0.0028 (19)0.0015 (18)
O40.054 (3)0.029 (3)0.025 (3)0.008 (2)0.006 (2)0.001 (2)
O50.046 (3)0.034 (3)0.031 (3)0.010 (2)0.009 (2)0.003 (2)
O60.055 (3)0.016 (2)0.055 (4)0.007 (2)0.003 (3)0.005 (2)
O70.032 (3)0.055 (3)0.026 (3)0.011 (2)0.003 (2)0.009 (3)
O80.027 (3)0.043 (3)0.028 (3)0.008 (2)0.000 (2)0.007 (2)
O90.043 (3)0.116 (5)0.048 (4)0.051 (4)0.002 (3)0.001 (4)
O100.020 (2)0.020 (2)0.026 (3)0.0021 (19)0.0005 (19)0.0030 (19)
O110.016 (2)0.026 (2)0.025 (3)0.0029 (19)0.0008 (19)0.002 (2)
O120.029 (3)0.019 (2)0.044 (3)0.005 (2)0.002 (2)0.003 (2)
O130.041 (3)0.042 (3)0.024 (3)0.013 (2)0.003 (2)0.004 (2)
N10.026 (3)0.024 (3)0.036 (4)0.004 (3)0.000 (3)0.003 (3)
N20.028 (3)0.042 (4)0.041 (5)0.009 (3)0.006 (3)0.004 (3)
N30.026 (3)0.022 (3)0.016 (3)0.000 (3)0.001 (2)0.000 (2)
C10.028 (4)0.020 (3)0.024 (4)0.000 (3)0.001 (3)0.003 (3)
C20.034 (4)0.033 (4)0.030 (5)0.008 (3)0.005 (3)0.004 (3)
C30.050 (5)0.048 (5)0.027 (5)0.017 (4)0.002 (4)0.008 (4)
C40.063 (6)0.039 (4)0.033 (5)0.004 (4)0.020 (4)0.007 (4)
C50.027 (4)0.039 (4)0.066 (7)0.006 (4)0.015 (4)0.004 (4)
C60.028 (4)0.041 (4)0.044 (5)0.000 (3)0.006 (4)0.009 (4)
C70.020 (3)0.028 (3)0.020 (4)0.004 (3)0.001 (3)0.004 (3)
C80.019 (3)0.030 (4)0.031 (4)0.004 (3)0.004 (3)0.006 (3)
C90.022 (4)0.043 (4)0.035 (5)0.006 (3)0.001 (3)0.000 (4)
C100.033 (4)0.030 (4)0.025 (4)0.006 (3)0.006 (3)0.001 (3)
C110.031 (4)0.034 (4)0.025 (4)0.003 (3)0.004 (3)0.001 (3)
C120.021 (3)0.031 (4)0.015 (4)0.006 (3)0.005 (3)0.001 (3)
C130.020 (3)0.030 (4)0.026 (4)0.004 (3)0.001 (3)0.002 (3)
C140.032 (4)0.040 (4)0.029 (5)0.018 (3)0.001 (3)0.001 (3)
C150.038 (4)0.047 (4)0.012 (4)0.006 (4)0.000 (3)0.004 (3)
C160.040 (4)0.036 (4)0.035 (5)0.001 (4)0.010 (4)0.014 (4)
C170.066 (6)0.024 (4)0.046 (6)0.003 (4)0.007 (4)0.007 (4)
C180.048 (5)0.030 (4)0.026 (4)0.000 (3)0.010 (4)0.006 (3)
C190.016 (3)0.018 (3)0.027 (4)0.000 (3)0.001 (3)0.001 (3)
C200.026 (4)0.023 (3)0.029 (4)0.002 (3)0.003 (3)0.000 (3)
C210.024 (4)0.024 (3)0.044 (5)0.000 (3)0.004 (3)0.002 (3)
C220.028 (4)0.033 (4)0.040 (5)0.003 (3)0.012 (3)0.008 (4)
C230.027 (4)0.040 (4)0.034 (5)0.004 (3)0.011 (3)0.006 (3)
C240.026 (4)0.034 (4)0.019 (4)0.004 (3)0.001 (3)0.011 (3)
C250.025 (3)0.022 (3)0.018 (4)0.004 (3)0.004 (3)0.002 (3)
C260.038 (4)0.035 (4)0.042 (5)0.002 (4)0.006 (4)0.002 (4)
C270.047 (5)0.031 (4)0.042 (5)0.007 (4)0.007 (4)0.007 (4)
C280.035 (4)0.042 (4)0.037 (5)0.018 (4)0.012 (4)0.009 (4)
C290.027 (4)0.056 (5)0.022 (4)0.005 (4)0.004 (3)0.011 (4)
C300.030 (4)0.033 (4)0.015 (4)0.006 (3)0.003 (3)0.001 (3)
C310.018 (3)0.027 (3)0.014 (4)0.001 (3)0.002 (3)0.005 (3)
C320.019 (3)0.033 (4)0.025 (4)0.001 (3)0.000 (3)0.003 (3)
C330.024 (4)0.046 (4)0.016 (4)0.000 (3)0.002 (3)0.003 (3)
C340.021 (3)0.029 (4)0.031 (5)0.005 (3)0.006 (3)0.008 (3)
C350.034 (4)0.020 (3)0.021 (4)0.001 (3)0.004 (3)0.004 (3)
C360.023 (3)0.029 (4)0.023 (4)0.004 (3)0.000 (3)0.000 (3)
C370.026 (3)0.018 (3)0.019 (4)0.000 (3)0.006 (3)0.002 (3)
C380.024 (4)0.034 (4)0.031 (5)0.001 (3)0.000 (3)0.002 (3)
C390.026 (4)0.047 (4)0.029 (5)0.005 (3)0.002 (3)0.008 (4)
C400.026 (4)0.049 (4)0.034 (5)0.004 (4)0.006 (3)0.002 (4)
C410.034 (4)0.050 (5)0.024 (4)0.004 (4)0.009 (3)0.000 (4)
C420.032 (4)0.031 (4)0.021 (4)0.004 (3)0.003 (3)0.001 (3)
C430.020 (3)0.026 (3)0.013 (4)0.000 (3)0.000 (3)0.003 (3)
C440.026 (3)0.023 (4)0.031 (4)0.003 (3)0.001 (3)0.007 (3)
C450.029 (4)0.041 (4)0.025 (4)0.002 (3)0.005 (3)0.013 (3)
C460.034 (4)0.032 (4)0.028 (5)0.006 (3)0.005 (3)0.007 (3)
C470.049 (5)0.022 (4)0.042 (5)0.004 (3)0.000 (4)0.006 (3)
C480.043 (4)0.019 (3)0.029 (5)0.000 (3)0.002 (3)0.005 (3)
C490.019 (3)0.021 (3)0.021 (4)0.003 (3)0.003 (3)0.003 (3)
C500.032 (4)0.026 (3)0.018 (4)0.008 (3)0.001 (3)0.004 (3)
C510.029 (4)0.024 (3)0.021 (4)0.003 (3)0.004 (3)0.004 (3)
C520.024 (4)0.021 (3)0.031 (5)0.007 (3)0.006 (3)0.003 (3)
C530.026 (4)0.026 (3)0.026 (4)0.004 (3)0.002 (3)0.005 (3)
C540.023 (3)0.028 (4)0.021 (4)0.002 (3)0.001 (3)0.001 (3)
C550.039 (5)0.055 (5)0.054 (6)0.000 (4)0.003 (4)0.010 (4)
C560.030 (4)0.041 (4)0.032 (5)0.007 (3)0.011 (3)0.000 (4)
C570.041 (4)0.041 (4)0.033 (5)0.011 (4)0.007 (4)0.000 (4)
Geometric parameters (Å, º) top
Tb1—O12.307 (4)C22—H220.9500
Tb1—O22.309 (4)C23—C241.389 (9)
Tb1—O32.295 (4)C23—H230.9500
Tb1—O42.467 (4)C24—H240.9500
Tb1—O52.492 (5)C25—C301.384 (9)
Tb1—O72.476 (4)C25—C261.385 (9)
Tb1—O82.505 (4)C26—C271.406 (10)
Tb1—O102.459 (4)C26—H260.9500
Tb1—O112.539 (4)C27—C281.351 (11)
Tb1—N12.904 (6)C27—H270.9500
Tb1—N22.918 (6)C28—C291.386 (11)
Tb1—N32.927 (5)C28—H280.9500
P1—O11.502 (4)C29—C301.376 (9)
P1—C131.777 (7)C29—H290.9500
P1—C11.801 (7)C30—H300.9500
P1—C71.803 (6)C31—C321.391 (9)
P2—O21.508 (5)C31—C361.405 (9)
P2—C311.790 (6)C32—C331.397 (9)
P2—C191.801 (6)C32—H320.9500
P2—C251.803 (6)C33—C341.373 (9)
P3—O31.504 (5)C33—H330.9500
P3—C431.800 (6)C34—C351.375 (9)
P3—C491.804 (6)C34—H340.9500
P3—C371.807 (6)C35—C361.391 (9)
O4—N11.268 (7)C35—H350.9500
O5—N11.268 (7)C36—H360.9500
O6—N11.228 (7)C37—C381.384 (9)
O7—N21.279 (8)C37—C421.403 (9)
O8—N21.261 (7)C38—C391.401 (9)
O9—N21.218 (7)C38—H380.9500
O10—N31.282 (6)C39—C401.372 (10)
O11—N31.265 (6)C39—H390.9500
O12—N31.212 (6)C40—C411.379 (10)
O13—C561.217 (8)C40—H400.9500
O14—C591.168 (12)C41—C421.375 (9)
C1—C21.381 (9)C41—H410.9500
C1—C61.409 (9)C42—H420.9500
C2—C31.392 (10)C43—C441.382 (9)
C2—H20.9500C43—C481.383 (9)
C3—C41.379 (11)C44—C451.392 (9)
C3—H30.9500C44—H440.9500
C4—C51.380 (11)C45—C461.371 (10)
C4—H40.9500C45—H450.9500
C5—C61.395 (11)C46—C471.382 (10)
C5—H50.9500C46—H460.9500
C6—H60.9500C47—C481.397 (10)
C7—C121.395 (9)C47—H470.9500
C7—C81.403 (8)C48—H480.9500
C8—C91.397 (9)C49—C541.391 (8)
C8—H80.9500C49—C501.397 (9)
C9—C101.381 (9)C50—C511.392 (9)
C9—H90.9500C50—H500.9500
C10—C111.388 (9)C51—C521.369 (9)
C10—H100.9500C51—H510.9500
C11—C121.383 (9)C52—C531.399 (9)
C11—H110.9500C52—H520.9500
C12—H120.9500C53—C541.383 (9)
C13—C181.383 (9)C53—H530.9500
C13—C141.400 (10)C54—H540.9500
C14—C151.386 (10)C55—C561.499 (10)
C14—H140.9500C55—H55A0.9800
C15—C161.360 (10)C55—H55B0.9800
C15—H150.9500C55—H55C0.9800
C16—C171.407 (11)C56—C571.506 (10)
C16—H160.9500C57—H57A0.9800
C17—C181.377 (10)C57—H57B0.9800
C17—H170.9500C57—H57C0.9800
C18—H180.9500C58—C591.499 (9)
C19—C241.391 (9)C58—H58A0.9800
C19—C201.408 (9)C58—H58B0.9800
C20—C211.377 (9)C58—H58C0.9800
C20—H200.9500C59—C601.490 (9)
C21—C221.390 (10)C60—H60A0.9800
C21—H210.9500C60—H60B0.9800
C22—C231.378 (10)C60—H60C0.9800
O1—Tb1—O285.51 (15)C13—C14—H14119.6
O1—Tb1—O384.27 (15)C16—C15—C14120.5 (7)
O3—Tb1—O2150.09 (14)C16—C15—H15119.7
O3—Tb1—O1079.30 (14)C14—C15—H15119.7
O1—Tb1—O10126.30 (13)C15—C16—C17119.1 (7)
O2—Tb1—O1084.35 (14)C15—C16—H16120.5
O3—Tb1—O4128.15 (15)C17—C16—H16120.5
O1—Tb1—O483.94 (15)C18—C17—C16120.6 (7)
O2—Tb1—O478.35 (15)C18—C17—H17119.7
O10—Tb1—O4143.85 (15)C16—C17—H17119.7
O3—Tb1—O774.86 (16)C17—C18—C13120.5 (7)
O1—Tb1—O7146.47 (16)C17—C18—H18119.7
O2—Tb1—O7124.89 (16)C13—C18—H18119.7
O10—Tb1—O775.63 (15)C24—C19—C20119.2 (6)
O4—Tb1—O788.62 (17)C24—C19—P2123.2 (5)
O3—Tb1—O576.72 (15)C20—C19—P2117.5 (5)
O1—Tb1—O576.04 (15)C21—C20—C19119.7 (7)
O2—Tb1—O5127.50 (15)C21—C20—H20120.2
O10—Tb1—O5145.05 (15)C19—C20—H20120.2
O4—Tb1—O551.43 (16)C20—C21—C22120.9 (7)
O7—Tb1—O573.82 (16)C20—C21—H21119.6
O3—Tb1—O8123.52 (15)C22—C21—H21119.6
O1—Tb1—O8150.82 (15)C23—C22—C21119.5 (6)
O2—Tb1—O873.90 (15)C23—C22—H22120.2
O10—Tb1—O872.81 (14)C21—C22—H22120.2
O4—Tb1—O871.97 (16)C22—C23—C24120.5 (7)
O7—Tb1—O851.26 (16)C22—C23—H23119.7
O5—Tb1—O8100.12 (16)C24—C23—H23119.7
O3—Tb1—O1176.60 (14)C23—C24—C19120.1 (6)
O1—Tb1—O1175.33 (13)C23—C24—H24119.9
O2—Tb1—O1173.63 (14)C19—C24—H24119.9
O10—Tb1—O1151.23 (13)C30—C25—C26119.8 (6)
O4—Tb1—O11146.11 (15)C30—C25—P2117.6 (5)
O7—Tb1—O11123.10 (15)C26—C25—P2122.5 (5)
O5—Tb1—O11142.37 (15)C25—C26—C27118.2 (7)
O8—Tb1—O11116.69 (15)C25—C26—H26120.9
O3—Tb1—N1102.46 (16)C27—C26—H26120.9
O1—Tb1—N178.37 (14)C28—C27—C26121.7 (7)
O2—Tb1—N1102.87 (16)C28—C27—H27119.1
O10—Tb1—N1155.10 (14)C26—C27—H27119.1
O4—Tb1—N125.70 (16)C27—C28—C29119.8 (7)
O7—Tb1—N180.85 (16)C27—C28—H28120.1
O5—Tb1—N125.74 (16)C29—C28—H28120.1
O8—Tb1—N186.18 (16)C30—C29—C28119.5 (7)
O11—Tb1—N1153.65 (14)C30—C29—H29120.2
O3—Tb1—N299.46 (17)C28—C29—H29120.2
O1—Tb1—N2161.18 (15)C29—C30—C25120.9 (6)
O2—Tb1—N299.24 (17)C29—C30—H30119.6
O10—Tb1—N272.46 (15)C25—C30—H30119.6
O4—Tb1—N279.26 (17)C32—C31—C36119.7 (6)
O7—Tb1—N225.81 (17)C32—C31—P2121.5 (5)
O5—Tb1—N286.80 (17)C36—C31—P2118.8 (5)
O8—Tb1—N225.46 (16)C31—C32—C33119.1 (6)
O11—Tb1—N2123.50 (15)C31—C32—H32120.4
N1—Tb1—N282.81 (16)C33—C32—H32120.4
O3—Tb1—N376.66 (14)C34—C33—C32120.6 (7)
O1—Tb1—N3100.75 (14)C34—C33—H33119.7
O2—Tb1—N377.77 (14)C32—C33—H33119.7
O10—Tb1—N325.70 (13)C33—C34—C35120.9 (6)
O4—Tb1—N3155.19 (16)C33—C34—H34119.5
O7—Tb1—N399.60 (15)C35—C34—H34119.5
O5—Tb1—N3153.38 (16)C34—C35—C36119.6 (6)
O8—Tb1—N394.94 (15)C34—C35—H35120.2
O11—Tb1—N325.53 (13)C36—C35—H35120.2
N1—Tb1—N3178.84 (15)C35—C36—C31120.1 (6)
N2—Tb1—N398.07 (15)C35—C36—H36120.0
O1—P1—C13111.4 (3)C31—C36—H36120.0
O1—P1—C1110.1 (3)C38—C37—C42119.7 (6)
C13—P1—C1107.4 (3)C38—C37—P3118.7 (5)
O1—P1—C7108.6 (3)C42—C37—P3121.6 (5)
C13—P1—C7110.1 (3)C37—C38—C39119.8 (7)
C1—P1—C7109.1 (3)C37—C38—H38120.1
O2—P2—C31111.3 (3)C39—C38—H38120.1
O2—P2—C19110.7 (3)C40—C39—C38119.9 (7)
C31—P2—C19106.9 (3)C40—C39—H39120.1
O2—P2—C25112.2 (3)C38—C39—H39120.1
C31—P2—C25107.3 (3)C39—C40—C41120.4 (7)
C19—P2—C25108.1 (3)C39—C40—H40119.8
O3—P3—C43111.5 (3)C41—C40—H40119.8
O3—P3—C49111.1 (3)C42—C41—C40120.7 (7)
C43—P3—C49107.5 (3)C42—C41—H41119.6
O3—P3—C37111.1 (3)C40—C41—H41119.6
C43—P3—C37107.7 (3)C41—C42—C37119.6 (6)
C49—P3—C37107.8 (3)C41—C42—H42120.2
P1—O1—Tb1154.7 (3)C37—C42—H42120.2
P2—O2—Tb1159.6 (3)C44—C43—C48119.7 (6)
P3—O3—Tb1173.8 (3)C44—C43—P3121.9 (5)
N1—O4—Tb196.8 (4)C48—C43—P3118.3 (5)
N1—O5—Tb195.6 (4)C43—C44—C45120.7 (6)
N2—O7—Tb196.8 (4)C43—C44—H44119.6
N2—O8—Tb195.9 (4)C45—C44—H44119.6
N3—O10—Tb198.0 (3)C46—C45—C44119.3 (7)
N3—O11—Tb194.6 (3)C46—C45—H45120.4
O6—N1—O5122.4 (6)C44—C45—H45120.4
O6—N1—O4121.5 (6)C45—C46—C47120.7 (7)
O5—N1—O4116.1 (5)C45—C46—H46119.6
O6—N1—Tb1177.4 (4)C47—C46—H46119.6
O5—N1—Tb158.7 (3)C46—C47—C48119.9 (6)
O4—N1—Tb157.5 (3)C46—C47—H47120.0
O9—N2—O8122.0 (7)C48—C47—H47120.0
O9—N2—O7122.0 (6)C43—C48—C47119.6 (7)
O8—N2—O7116.1 (5)C43—C48—H48120.2
O9—N2—Tb1179.1 (5)C47—C48—H48120.2
O8—N2—Tb158.6 (3)C54—C49—C50120.2 (6)
O7—N2—Tb157.4 (3)C54—C49—P3118.0 (5)
O12—N3—O11122.6 (5)C50—C49—P3121.8 (5)
O12—N3—O10121.2 (5)C51—C50—C49119.4 (6)
O11—N3—O10116.1 (5)C51—C50—H50120.3
O12—N3—Tb1177.3 (4)C49—C50—H50120.3
O11—N3—Tb159.8 (3)C52—C51—C50120.6 (6)
O10—N3—Tb156.3 (3)C52—C51—H51119.7
C2—C1—C6120.7 (7)C50—C51—H51119.7
C2—C1—P1119.3 (5)C51—C52—C53120.0 (6)
C6—C1—P1120.0 (6)C51—C52—H52120.0
C1—C2—C3120.3 (7)C53—C52—H52120.0
C1—C2—H2119.9C54—C53—C52120.2 (6)
C3—C2—H2119.9C54—C53—H53119.9
C4—C3—C2119.3 (8)C52—C53—H53119.9
C4—C3—H3120.4C53—C54—C49119.6 (6)
C2—C3—H3120.4C53—C54—H54120.2
C3—C4—C5121.0 (7)C49—C54—H54120.2
C3—C4—H4119.5C56—C55—H55A109.5
C5—C4—H4119.5C56—C55—H55B109.5
C4—C5—C6120.7 (7)H55A—C55—H55B109.5
C4—C5—H5119.7C56—C55—H55C109.5
C6—C5—H5119.7H55A—C55—H55C109.5
C5—C6—C1118.0 (7)H55B—C55—H55C109.5
C5—C6—H6121.0O13—C56—C55122.5 (7)
C1—C6—H6121.0O13—C56—C57121.0 (7)
C12—C7—C8119.2 (6)C55—C56—C57116.4 (7)
C12—C7—P1117.9 (5)C56—C57—H57A109.5
C8—C7—P1122.7 (5)C56—C57—H57B109.5
C9—C8—C7119.7 (6)H57A—C57—H57B109.5
C9—C8—H8120.2C56—C57—H57C109.5
C7—C8—H8120.2H57A—C57—H57C109.5
C10—C9—C8120.2 (6)H57B—C57—H57C109.5
C10—C9—H9119.9C59—C58—H58A109.5
C8—C9—H9119.9C59—C58—H58B109.5
C9—C10—C11120.4 (6)H58A—C58—H58B109.5
C9—C10—H10119.8C59—C58—H58C109.5
C11—C10—H10119.8H58A—C58—H58C109.5
C12—C11—C10119.9 (6)H58B—C58—H58C109.5
C12—C11—H11120.1O14—C59—C60122.2 (11)
C10—C11—H11120.1O14—C59—C58123.0 (11)
C11—C12—C7120.7 (6)C60—C59—C58114.8 (11)
C11—C12—H12119.7C59—C60—H60A109.5
C7—C12—H12119.7C59—C60—H60B109.5
C18—C13—C14118.4 (6)H60A—C60—H60B109.5
C18—C13—P1120.6 (5)C59—C60—H60C109.5
C14—C13—P1120.2 (5)H60A—C60—H60C109.5
C15—C14—C13120.8 (7)H60B—C60—H60C109.5
C15—C14—H14119.6

Experimental details

Crystal data
Chemical formula[Tb(NO3)3(C18H15OP)3]·1.5C3H6O
Mr1266.88
Crystal system, space groupMonoclinic, P21/n
Temperature (K)120
a, b, c (Å)11.0612 (10), 19.180 (2), 27.641 (4)
β (°) 94.895 (7)
V3)5842.7 (12)
Z4
Radiation typeMo Kα
µ (mm1)1.36
Crystal size (mm)0.16 × 0.16 × 0.10
Data collection
DiffractometerNonius KappaCCD area-detector
diffractometer
Absorption correctionMulti-scan
(SORTAV; Blessing, 1997)
Tmin, Tmax0.847, 0.873
No. of measured, independent and
observed [I > 2σ(I)] reflections
40261, 10247, 6620
Rint0.111
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.135, 1.03
No. of reflections10247
No. of parameters711
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.24, 0.83

Computer programs: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997), COLLECT and DENZO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976).

Selected geometric parameters (Å, º) top
Tb1—O12.307 (4)Tb1—O82.505 (4)
Tb1—O22.309 (4)Tb1—O102.459 (4)
Tb1—O32.295 (4)Tb1—O112.539 (4)
Tb1—O42.467 (4)P1—O11.502 (4)
Tb1—O52.492 (5)P2—O21.508 (5)
Tb1—O72.476 (4)P3—O31.504 (5)
O1—Tb1—O285.51 (15)P1—O1—Tb1154.7 (3)
O1—Tb1—O384.27 (15)P2—O2—Tb1159.6 (3)
O3—Tb1—O2150.09 (14)P3—O3—Tb1173.8 (3)
O4—Tb1—O551.43 (16)O6—N1—O5122.4 (6)
O7—Tb1—O851.26 (16)O6—N1—O4121.5 (6)
O10—Tb1—O1151.23 (13)O5—N1—O4116.1 (5)
 

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