Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680300967X/bt6278sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680300967X/bt6278Isup2.hkl |
CCDC reference: 214775
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (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
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
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.
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.
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).
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. |
[Tb(NO3)3(C18H15OP)3]·1.5C3H6O | F(000) = 2576 |
Mr = 1266.88 | Dx = 1.440 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 41633 reflections |
a = 11.0612 (10) Å | θ = 2.9–27.5° |
b = 19.180 (2) Å | µ = 1.36 mm−1 |
c = 27.641 (4) Å | T = 120 K |
β = 94.895 (7)° | Block, colourless |
V = 5842.7 (12) Å3 | 0.16 × 0.16 × 0.10 mm |
Z = 4 |
Nonius KappaCCD area-detector diffractometer | 10247 independent reflections |
Radiation source: Nonius rotating anode | 6620 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.111 |
ϕ and ω scans | θmax = 25.0°, θmin = 3.0° |
Absorption correction: multi-scan (SORTAV; Blessing, 1997) | h = −13→12 |
Tmin = 0.847, Tmax = 0.873 | k = −22→22 |
40261 measured reflections | l = −32→31 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.054 | H-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 reflections | Δρmax = 1.24 e Å−3 |
711 parameters | Δρmin = −0.83 e Å−3 |
3 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00179 (16) |
[Tb(NO3)3(C18H15OP)3]·1.5C3H6O | V = 5842.7 (12) Å3 |
Mr = 1266.88 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.0612 (10) Å | µ = 1.36 mm−1 |
b = 19.180 (2) Å | T = 120 K |
c = 27.641 (4) Å | 0.16 × 0.16 × 0.10 mm |
β = 94.895 (7)° |
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 = 0.873 | Rint = 0.111 |
40261 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | 3 restraints |
wR(F2) = 0.135 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.24 e Å−3 |
10247 reflections | Δρmin = −0.83 e Å−3 |
711 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Tb1 | 1.10010 (2) | 0.248402 (15) | 0.134232 (10) | 0.01771 (12) | |
P1 | 0.76300 (14) | 0.25817 (8) | 0.11968 (6) | 0.0218 (4) | |
P2 | 1.08219 (14) | 0.29973 (8) | 0.26469 (6) | 0.0194 (4) | |
P3 | 1.11773 (14) | 0.29999 (8) | 0.00253 (6) | 0.0198 (4) | |
O1 | 0.8960 (4) | 0.2680 (2) | 0.11452 (17) | 0.0235 (10) | |
O2 | 1.0603 (4) | 0.2769 (2) | 0.21248 (15) | 0.0217 (10) | |
O3 | 1.1194 (4) | 0.2807 (2) | 0.05533 (15) | 0.0215 (10) | |
O4 | 1.0303 (5) | 0.1357 (2) | 0.16464 (18) | 0.0365 (12) | |
O5 | 1.0311 (4) | 0.1429 (2) | 0.08698 (19) | 0.0367 (12) | |
O6 | 0.9640 (5) | 0.0482 (2) | 0.1197 (2) | 0.0419 (14) | |
O7 | 1.2864 (4) | 0.1893 (3) | 0.11181 (19) | 0.0375 (13) | |
O8 | 1.2696 (4) | 0.1970 (2) | 0.18873 (18) | 0.0325 (11) | |
O9 | 1.4284 (5) | 0.1472 (4) | 0.1634 (2) | 0.069 (2) | |
O10 | 1.2590 (4) | 0.3379 (2) | 0.14605 (16) | 0.0223 (10) | |
O11 | 1.0774 (4) | 0.3801 (2) | 0.13611 (16) | 0.0226 (10) | |
O12 | 1.2317 (4) | 0.4500 (2) | 0.14810 (18) | 0.0312 (12) | |
O13 | 0.1107 (4) | 0.3797 (2) | 0.84533 (18) | 0.0356 (12) | |
O14 | 0.6420 (8) | 0.0782 (5) | 0.8947 (4) | 0.035 (2)* | 0.50 |
N1 | 1.0075 (5) | 0.1070 (3) | 0.1235 (2) | 0.0289 (14) | |
N2 | 1.3313 (5) | 0.1766 (3) | 0.1551 (2) | 0.0368 (15) | |
N3 | 1.1901 (5) | 0.3917 (3) | 0.14330 (19) | 0.0213 (12) | |
C1 | 0.6882 (6) | 0.2252 (3) | 0.0639 (3) | 0.0244 (15) | |
C2 | 0.7571 (6) | 0.2059 (3) | 0.0267 (3) | 0.0324 (17) | |
H2 | 0.8431 | 0.2086 | 0.0312 | 0.039* | |
C3 | 0.7011 (7) | 0.1826 (4) | −0.0173 (3) | 0.042 (2) | |
H3 | 0.7483 | 0.1702 | −0.0432 | 0.050* | |
C4 | 0.5764 (8) | 0.1777 (4) | −0.0230 (3) | 0.047 (2) | |
H4 | 0.5378 | 0.1623 | −0.0532 | 0.056* | |
C5 | 0.5067 (7) | 0.1948 (4) | 0.0143 (3) | 0.045 (2) | |
H5 | 0.4211 | 0.1894 | 0.0100 | 0.054* | |
C6 | 0.5608 (6) | 0.2199 (4) | 0.0584 (3) | 0.0383 (19) | |
H6 | 0.5130 | 0.2330 | 0.0839 | 0.046* | |
C7 | 0.6983 (5) | 0.3414 (3) | 0.1333 (2) | 0.0227 (15) | |
C8 | 0.5790 (5) | 0.3487 (3) | 0.1463 (3) | 0.0268 (16) | |
H8 | 0.5312 | 0.3086 | 0.1512 | 0.032* | |
C9 | 0.5310 (6) | 0.4153 (4) | 0.1520 (3) | 0.0334 (17) | |
H9 | 0.4501 | 0.4205 | 0.1605 | 0.040* | |
C10 | 0.6010 (6) | 0.4736 (4) | 0.1454 (3) | 0.0291 (16) | |
H10 | 0.5675 | 0.5188 | 0.1489 | 0.035* | |
C11 | 0.7199 (6) | 0.4667 (4) | 0.1336 (3) | 0.0299 (16) | |
H11 | 0.7681 | 0.5069 | 0.1296 | 0.036* | |
C12 | 0.7681 (6) | 0.4010 (3) | 0.1277 (2) | 0.0223 (15) | |
H12 | 0.8496 | 0.3964 | 0.1197 | 0.027* | |
C13 | 0.7379 (6) | 0.1971 (3) | 0.1661 (3) | 0.0252 (15) | |
C14 | 0.7545 (6) | 0.2169 (4) | 0.2150 (3) | 0.0339 (17) | |
H14 | 0.7627 | 0.2649 | 0.2231 | 0.041* | |
C15 | 0.7590 (6) | 0.1674 (4) | 0.2516 (3) | 0.0327 (17) | |
H15 | 0.7721 | 0.1817 | 0.2846 | 0.039* | |
C16 | 0.7448 (7) | 0.0986 (4) | 0.2408 (3) | 0.0366 (18) | |
H16 | 0.7493 | 0.0646 | 0.2659 | 0.044* | |
C17 | 0.7234 (8) | 0.0783 (4) | 0.1919 (3) | 0.045 (2) | |
H17 | 0.7101 | 0.0306 | 0.1841 | 0.054* | |
C18 | 0.7216 (7) | 0.1272 (3) | 0.1553 (3) | 0.0345 (18) | |
H18 | 0.7091 | 0.1127 | 0.1224 | 0.041* | |
C19 | 0.9457 (5) | 0.3351 (3) | 0.2861 (2) | 0.0206 (14) | |
C20 | 0.8751 (6) | 0.3796 (3) | 0.2546 (3) | 0.0260 (16) | |
H20 | 0.9023 | 0.3923 | 0.2241 | 0.031* | |
C21 | 0.7663 (6) | 0.4047 (3) | 0.2681 (3) | 0.0308 (17) | |
H21 | 0.7184 | 0.4344 | 0.2467 | 0.037* | |
C22 | 0.7258 (6) | 0.3873 (4) | 0.3128 (3) | 0.0327 (17) | |
H22 | 0.6507 | 0.4050 | 0.3219 | 0.039* | |
C23 | 0.7951 (6) | 0.3441 (4) | 0.3438 (3) | 0.0332 (17) | |
H23 | 0.7683 | 0.3327 | 0.3746 | 0.040* | |
C24 | 0.9040 (6) | 0.3171 (3) | 0.3305 (2) | 0.0261 (16) | |
H24 | 0.9500 | 0.2863 | 0.3517 | 0.031* | |
C25 | 1.1995 (6) | 0.3649 (3) | 0.2730 (2) | 0.0218 (14) | |
C26 | 1.1785 (7) | 0.4308 (4) | 0.2909 (3) | 0.0382 (19) | |
H26 | 1.1007 | 0.4436 | 0.3001 | 0.046* | |
C27 | 1.2756 (7) | 0.4784 (4) | 0.2952 (3) | 0.041 (2) | |
H27 | 1.2627 | 0.5237 | 0.3075 | 0.049* | |
C28 | 1.3868 (7) | 0.4612 (4) | 0.2822 (3) | 0.0389 (19) | |
H28 | 1.4509 | 0.4943 | 0.2854 | 0.047* | |
C29 | 1.4071 (6) | 0.3951 (4) | 0.2642 (3) | 0.0356 (18) | |
H29 | 1.4857 | 0.3823 | 0.2559 | 0.043* | |
C30 | 1.3128 (6) | 0.3483 (4) | 0.2586 (2) | 0.0262 (15) | |
H30 | 1.3257 | 0.3039 | 0.2446 | 0.031* | |
C31 | 1.1271 (5) | 0.2279 (3) | 0.3035 (2) | 0.0200 (14) | |
C32 | 1.1786 (5) | 0.2382 (3) | 0.3506 (2) | 0.0258 (15) | |
H32 | 1.1922 | 0.2841 | 0.3629 | 0.031* | |
C33 | 1.2102 (6) | 0.1803 (4) | 0.3797 (3) | 0.0285 (16) | |
H33 | 1.2444 | 0.1868 | 0.4120 | 0.034* | |
C34 | 1.1923 (5) | 0.1139 (3) | 0.3618 (3) | 0.0269 (16) | |
H34 | 1.2146 | 0.0751 | 0.3819 | 0.032* | |
C35 | 1.1424 (6) | 0.1029 (3) | 0.3151 (2) | 0.0250 (15) | |
H35 | 1.1303 | 0.0568 | 0.3031 | 0.030* | |
C36 | 1.1096 (5) | 0.1597 (3) | 0.2856 (3) | 0.0248 (15) | |
H36 | 1.0754 | 0.1525 | 0.2533 | 0.030* | |
C37 | 1.2653 (6) | 0.3292 (3) | −0.0123 (2) | 0.0208 (14) | |
C38 | 1.3441 (6) | 0.3573 (3) | 0.0241 (3) | 0.0297 (16) | |
H38 | 1.3222 | 0.3584 | 0.0566 | 0.036* | |
C39 | 1.4561 (6) | 0.3843 (4) | 0.0130 (3) | 0.0342 (17) | |
H39 | 1.5102 | 0.4039 | 0.0379 | 0.041* | |
C40 | 1.4875 (6) | 0.3823 (4) | −0.0340 (3) | 0.0361 (18) | |
H40 | 1.5633 | 0.4008 | −0.0415 | 0.043* | |
C41 | 1.4097 (6) | 0.3536 (4) | −0.0702 (3) | 0.0356 (18) | |
H41 | 1.4327 | 0.3521 | −0.1025 | 0.043* | |
C42 | 1.2992 (6) | 0.3271 (3) | −0.0601 (3) | 0.0281 (16) | |
H42 | 1.2460 | 0.3074 | −0.0853 | 0.034* | |
C43 | 1.0747 (5) | 0.2271 (3) | −0.0362 (2) | 0.0197 (14) | |
C44 | 1.0073 (6) | 0.2354 (3) | −0.0802 (3) | 0.0267 (16) | |
H44 | 0.9841 | 0.2808 | −0.0911 | 0.032* | |
C45 | 0.9728 (6) | 0.1779 (4) | −0.1089 (3) | 0.0320 (17) | |
H45 | 0.9284 | 0.1840 | −0.1395 | 0.038* | |
C46 | 1.0037 (6) | 0.1123 (4) | −0.0924 (3) | 0.0311 (17) | |
H46 | 0.9781 | 0.0728 | −0.1113 | 0.037* | |
C47 | 1.0717 (7) | 0.1031 (4) | −0.0485 (3) | 0.0378 (19) | |
H47 | 1.0943 | 0.0575 | −0.0378 | 0.045* | |
C48 | 1.1070 (6) | 0.1608 (3) | −0.0200 (3) | 0.0305 (17) | |
H48 | 1.1529 | 0.1547 | 0.0103 | 0.037* | |
C49 | 1.0109 (5) | 0.3693 (3) | −0.0126 (2) | 0.0208 (14) | |
C50 | 1.0277 (6) | 0.4170 (3) | −0.0496 (2) | 0.0253 (15) | |
H50 | 1.0976 | 0.4143 | −0.0672 | 0.030* | |
C51 | 0.9409 (6) | 0.4685 (3) | −0.0604 (3) | 0.0251 (15) | |
H51 | 0.9514 | 0.5007 | −0.0859 | 0.030* | |
C52 | 0.8408 (6) | 0.4733 (3) | −0.0348 (3) | 0.0262 (16) | |
H52 | 0.7820 | 0.5086 | −0.0425 | 0.031* | |
C53 | 0.8250 (6) | 0.4262 (3) | 0.0028 (3) | 0.0262 (16) | |
H53 | 0.7561 | 0.4300 | 0.0209 | 0.031* | |
C54 | 0.9095 (5) | 0.3742 (3) | 0.0138 (2) | 0.0239 (15) | |
H54 | 0.8984 | 0.3420 | 0.0391 | 0.029* | |
C55 | −0.0257 (7) | 0.4484 (4) | 0.7936 (3) | 0.049 (2) | |
H55A | 0.0216 | 0.4877 | 0.8078 | 0.074* | |
H55B | −0.1101 | 0.4526 | 0.8015 | 0.074* | |
H55C | −0.0228 | 0.4487 | 0.7582 | 0.074* | |
C56 | 0.0268 (6) | 0.3814 (4) | 0.8138 (3) | 0.0336 (17) | |
C57 | −0.0265 (7) | 0.3153 (4) | 0.7917 (3) | 0.0382 (19) | |
H57A | 0.0237 | 0.2755 | 0.8032 | 0.057* | |
H57B | −0.0288 | 0.3182 | 0.7563 | 0.057* | |
H57C | −0.1091 | 0.3091 | 0.8013 | 0.057* | |
C58 | 0.7265 (11) | −0.0157 (7) | 0.9406 (5) | 0.031 (3)* | 0.50 |
H58A | 0.7997 | 0.0132 | 0.9446 | 0.047* | 0.50 |
H58B | 0.7436 | −0.0581 | 0.9226 | 0.047* | 0.50 |
H58C | 0.7013 | −0.0284 | 0.9726 | 0.047* | 0.50 |
C59 | 0.6266 (9) | 0.0244 (6) | 0.9130 (5) | 0.031 (3)* | 0.50 |
C60 | 0.5047 (11) | −0.0091 (8) | 0.9114 (6) | 0.044 (4)* | 0.50 |
H60A | 0.4475 | 0.0171 | 0.8893 | 0.066* | 0.50 |
H60B | 0.4763 | −0.0091 | 0.9440 | 0.066* | 0.50 |
H60C | 0.5103 | −0.0572 | 0.8998 | 0.066* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tb1 | 0.01795 (17) | 0.01872 (18) | 0.01637 (19) | 0.00065 (14) | 0.00092 (11) | 0.00049 (14) |
P1 | 0.0185 (8) | 0.0247 (9) | 0.0222 (10) | −0.0004 (7) | 0.0014 (7) | 0.0013 (8) |
P2 | 0.0201 (8) | 0.0212 (8) | 0.0170 (10) | 0.0005 (7) | 0.0014 (7) | 0.0019 (7) |
P3 | 0.0216 (8) | 0.0212 (8) | 0.0164 (10) | −0.0003 (7) | 0.0007 (7) | −0.0007 (7) |
O1 | 0.020 (2) | 0.024 (2) | 0.027 (3) | 0.0006 (18) | 0.0032 (19) | 0.0025 (19) |
O2 | 0.029 (2) | 0.020 (2) | 0.016 (3) | 0.0036 (19) | 0.0065 (19) | 0.0032 (18) |
O3 | 0.026 (2) | 0.025 (2) | 0.014 (3) | −0.0019 (19) | 0.0028 (19) | 0.0015 (18) |
O4 | 0.054 (3) | 0.029 (3) | 0.025 (3) | −0.008 (2) | −0.006 (2) | 0.001 (2) |
O5 | 0.046 (3) | 0.034 (3) | 0.031 (3) | −0.010 (2) | 0.009 (2) | −0.003 (2) |
O6 | 0.055 (3) | 0.016 (2) | 0.055 (4) | −0.007 (2) | 0.003 (3) | −0.005 (2) |
O7 | 0.032 (3) | 0.055 (3) | 0.026 (3) | 0.011 (2) | 0.003 (2) | −0.009 (3) |
O8 | 0.027 (3) | 0.043 (3) | 0.028 (3) | 0.008 (2) | 0.000 (2) | 0.007 (2) |
O9 | 0.043 (3) | 0.116 (5) | 0.048 (4) | 0.051 (4) | −0.002 (3) | 0.001 (4) |
O10 | 0.020 (2) | 0.020 (2) | 0.026 (3) | −0.0021 (19) | −0.0005 (19) | −0.0030 (19) |
O11 | 0.016 (2) | 0.026 (2) | 0.025 (3) | −0.0029 (19) | 0.0008 (19) | 0.002 (2) |
O12 | 0.029 (3) | 0.019 (2) | 0.044 (3) | −0.005 (2) | −0.002 (2) | 0.003 (2) |
O13 | 0.041 (3) | 0.042 (3) | 0.024 (3) | −0.013 (2) | 0.003 (2) | −0.004 (2) |
N1 | 0.026 (3) | 0.024 (3) | 0.036 (4) | 0.004 (3) | 0.000 (3) | −0.003 (3) |
N2 | 0.028 (3) | 0.042 (4) | 0.041 (5) | 0.009 (3) | 0.006 (3) | 0.004 (3) |
N3 | 0.026 (3) | 0.022 (3) | 0.016 (3) | 0.000 (3) | 0.001 (2) | 0.000 (2) |
C1 | 0.028 (4) | 0.020 (3) | 0.024 (4) | 0.000 (3) | −0.001 (3) | 0.003 (3) |
C2 | 0.034 (4) | 0.033 (4) | 0.030 (5) | −0.008 (3) | 0.005 (3) | 0.004 (3) |
C3 | 0.050 (5) | 0.048 (5) | 0.027 (5) | −0.017 (4) | −0.002 (4) | −0.008 (4) |
C4 | 0.063 (6) | 0.039 (4) | 0.033 (5) | −0.004 (4) | −0.020 (4) | −0.007 (4) |
C5 | 0.027 (4) | 0.039 (4) | 0.066 (7) | 0.006 (4) | −0.015 (4) | −0.004 (4) |
C6 | 0.028 (4) | 0.041 (4) | 0.044 (5) | 0.000 (3) | −0.006 (4) | −0.009 (4) |
C7 | 0.020 (3) | 0.028 (3) | 0.020 (4) | −0.004 (3) | −0.001 (3) | 0.004 (3) |
C8 | 0.019 (3) | 0.030 (4) | 0.031 (4) | −0.004 (3) | 0.004 (3) | −0.006 (3) |
C9 | 0.022 (4) | 0.043 (4) | 0.035 (5) | 0.006 (3) | 0.001 (3) | 0.000 (4) |
C10 | 0.033 (4) | 0.030 (4) | 0.025 (4) | 0.006 (3) | 0.006 (3) | 0.001 (3) |
C11 | 0.031 (4) | 0.034 (4) | 0.025 (4) | −0.003 (3) | 0.004 (3) | 0.001 (3) |
C12 | 0.021 (3) | 0.031 (4) | 0.015 (4) | 0.006 (3) | 0.005 (3) | −0.001 (3) |
C13 | 0.020 (3) | 0.030 (4) | 0.026 (4) | −0.004 (3) | −0.001 (3) | 0.002 (3) |
C14 | 0.032 (4) | 0.040 (4) | 0.029 (5) | −0.018 (3) | −0.001 (3) | 0.001 (3) |
C15 | 0.038 (4) | 0.047 (4) | 0.012 (4) | −0.006 (4) | 0.000 (3) | 0.004 (3) |
C16 | 0.040 (4) | 0.036 (4) | 0.035 (5) | 0.001 (4) | 0.010 (4) | 0.014 (4) |
C17 | 0.066 (6) | 0.024 (4) | 0.046 (6) | 0.003 (4) | 0.007 (4) | 0.007 (4) |
C18 | 0.048 (5) | 0.030 (4) | 0.026 (4) | 0.000 (3) | 0.010 (4) | −0.006 (3) |
C19 | 0.016 (3) | 0.018 (3) | 0.027 (4) | 0.000 (3) | 0.001 (3) | −0.001 (3) |
C20 | 0.026 (4) | 0.023 (3) | 0.029 (4) | 0.002 (3) | 0.003 (3) | 0.000 (3) |
C21 | 0.024 (4) | 0.024 (3) | 0.044 (5) | 0.000 (3) | −0.004 (3) | −0.002 (3) |
C22 | 0.028 (4) | 0.033 (4) | 0.040 (5) | −0.003 (3) | 0.012 (3) | −0.008 (4) |
C23 | 0.027 (4) | 0.040 (4) | 0.034 (5) | 0.004 (3) | 0.011 (3) | 0.006 (3) |
C24 | 0.026 (4) | 0.034 (4) | 0.019 (4) | 0.004 (3) | 0.001 (3) | 0.011 (3) |
C25 | 0.025 (3) | 0.022 (3) | 0.018 (4) | −0.004 (3) | −0.004 (3) | 0.002 (3) |
C26 | 0.038 (4) | 0.035 (4) | 0.042 (5) | −0.002 (4) | 0.006 (4) | −0.002 (4) |
C27 | 0.047 (5) | 0.031 (4) | 0.042 (5) | −0.007 (4) | −0.007 (4) | −0.007 (4) |
C28 | 0.035 (4) | 0.042 (4) | 0.037 (5) | −0.018 (4) | −0.012 (4) | 0.009 (4) |
C29 | 0.027 (4) | 0.056 (5) | 0.022 (4) | −0.005 (4) | −0.004 (3) | 0.011 (4) |
C30 | 0.030 (4) | 0.033 (4) | 0.015 (4) | −0.006 (3) | −0.003 (3) | −0.001 (3) |
C31 | 0.018 (3) | 0.027 (3) | 0.014 (4) | 0.001 (3) | −0.002 (3) | 0.005 (3) |
C32 | 0.019 (3) | 0.033 (4) | 0.025 (4) | −0.001 (3) | 0.000 (3) | 0.003 (3) |
C33 | 0.024 (4) | 0.046 (4) | 0.016 (4) | 0.000 (3) | 0.002 (3) | 0.003 (3) |
C34 | 0.021 (3) | 0.029 (4) | 0.031 (5) | 0.005 (3) | 0.006 (3) | 0.008 (3) |
C35 | 0.034 (4) | 0.020 (3) | 0.021 (4) | 0.001 (3) | 0.004 (3) | −0.004 (3) |
C36 | 0.023 (3) | 0.029 (4) | 0.023 (4) | 0.004 (3) | 0.000 (3) | 0.000 (3) |
C37 | 0.026 (3) | 0.018 (3) | 0.019 (4) | 0.000 (3) | 0.006 (3) | 0.002 (3) |
C38 | 0.024 (4) | 0.034 (4) | 0.031 (5) | 0.001 (3) | 0.000 (3) | 0.002 (3) |
C39 | 0.026 (4) | 0.047 (4) | 0.029 (5) | −0.005 (3) | −0.002 (3) | −0.008 (4) |
C40 | 0.026 (4) | 0.049 (4) | 0.034 (5) | −0.004 (4) | 0.006 (3) | −0.002 (4) |
C41 | 0.034 (4) | 0.050 (5) | 0.024 (4) | −0.004 (4) | 0.009 (3) | 0.000 (4) |
C42 | 0.032 (4) | 0.031 (4) | 0.021 (4) | 0.004 (3) | −0.003 (3) | −0.001 (3) |
C43 | 0.020 (3) | 0.026 (3) | 0.013 (4) | 0.000 (3) | 0.000 (3) | 0.003 (3) |
C44 | 0.026 (3) | 0.023 (4) | 0.031 (4) | 0.003 (3) | −0.001 (3) | −0.007 (3) |
C45 | 0.029 (4) | 0.041 (4) | 0.025 (4) | 0.002 (3) | −0.005 (3) | −0.013 (3) |
C46 | 0.034 (4) | 0.032 (4) | 0.028 (5) | −0.006 (3) | 0.005 (3) | −0.007 (3) |
C47 | 0.049 (5) | 0.022 (4) | 0.042 (5) | 0.004 (3) | 0.000 (4) | 0.006 (3) |
C48 | 0.043 (4) | 0.019 (3) | 0.029 (5) | 0.000 (3) | 0.002 (3) | −0.005 (3) |
C49 | 0.019 (3) | 0.021 (3) | 0.021 (4) | −0.003 (3) | −0.003 (3) | −0.003 (3) |
C50 | 0.032 (4) | 0.026 (3) | 0.018 (4) | −0.008 (3) | 0.001 (3) | −0.004 (3) |
C51 | 0.029 (4) | 0.024 (3) | 0.021 (4) | −0.003 (3) | −0.004 (3) | 0.004 (3) |
C52 | 0.024 (4) | 0.021 (3) | 0.031 (5) | 0.007 (3) | −0.006 (3) | −0.003 (3) |
C53 | 0.026 (4) | 0.026 (3) | 0.026 (4) | 0.004 (3) | −0.002 (3) | −0.005 (3) |
C54 | 0.023 (3) | 0.028 (4) | 0.021 (4) | −0.002 (3) | 0.001 (3) | −0.001 (3) |
C55 | 0.039 (5) | 0.055 (5) | 0.054 (6) | 0.000 (4) | 0.003 (4) | 0.010 (4) |
C56 | 0.030 (4) | 0.041 (4) | 0.032 (5) | −0.007 (3) | 0.011 (3) | 0.000 (4) |
C57 | 0.041 (4) | 0.041 (4) | 0.033 (5) | −0.011 (4) | 0.007 (4) | 0.000 (4) |
Tb1—O1 | 2.307 (4) | C22—H22 | 0.9500 |
Tb1—O2 | 2.309 (4) | C23—C24 | 1.389 (9) |
Tb1—O3 | 2.295 (4) | C23—H23 | 0.9500 |
Tb1—O4 | 2.467 (4) | C24—H24 | 0.9500 |
Tb1—O5 | 2.492 (5) | C25—C30 | 1.384 (9) |
Tb1—O7 | 2.476 (4) | C25—C26 | 1.385 (9) |
Tb1—O8 | 2.505 (4) | C26—C27 | 1.406 (10) |
Tb1—O10 | 2.459 (4) | C26—H26 | 0.9500 |
Tb1—O11 | 2.539 (4) | C27—C28 | 1.351 (11) |
Tb1—N1 | 2.904 (6) | C27—H27 | 0.9500 |
Tb1—N2 | 2.918 (6) | C28—C29 | 1.386 (11) |
Tb1—N3 | 2.927 (5) | C28—H28 | 0.9500 |
P1—O1 | 1.502 (4) | C29—C30 | 1.376 (9) |
P1—C13 | 1.777 (7) | C29—H29 | 0.9500 |
P1—C1 | 1.801 (7) | C30—H30 | 0.9500 |
P1—C7 | 1.803 (6) | C31—C32 | 1.391 (9) |
P2—O2 | 1.508 (5) | C31—C36 | 1.405 (9) |
P2—C31 | 1.790 (6) | C32—C33 | 1.397 (9) |
P2—C19 | 1.801 (6) | C32—H32 | 0.9500 |
P2—C25 | 1.803 (6) | C33—C34 | 1.373 (9) |
P3—O3 | 1.504 (5) | C33—H33 | 0.9500 |
P3—C43 | 1.800 (6) | C34—C35 | 1.375 (9) |
P3—C49 | 1.804 (6) | C34—H34 | 0.9500 |
P3—C37 | 1.807 (6) | C35—C36 | 1.391 (9) |
O4—N1 | 1.268 (7) | C35—H35 | 0.9500 |
O5—N1 | 1.268 (7) | C36—H36 | 0.9500 |
O6—N1 | 1.228 (7) | C37—C38 | 1.384 (9) |
O7—N2 | 1.279 (8) | C37—C42 | 1.403 (9) |
O8—N2 | 1.261 (7) | C38—C39 | 1.401 (9) |
O9—N2 | 1.218 (7) | C38—H38 | 0.9500 |
O10—N3 | 1.282 (6) | C39—C40 | 1.372 (10) |
O11—N3 | 1.265 (6) | C39—H39 | 0.9500 |
O12—N3 | 1.212 (6) | C40—C41 | 1.379 (10) |
O13—C56 | 1.217 (8) | C40—H40 | 0.9500 |
O14—C59 | 1.168 (12) | C41—C42 | 1.375 (9) |
C1—C2 | 1.381 (9) | C41—H41 | 0.9500 |
C1—C6 | 1.409 (9) | C42—H42 | 0.9500 |
C2—C3 | 1.392 (10) | C43—C44 | 1.382 (9) |
C2—H2 | 0.9500 | C43—C48 | 1.383 (9) |
C3—C4 | 1.379 (11) | C44—C45 | 1.392 (9) |
C3—H3 | 0.9500 | C44—H44 | 0.9500 |
C4—C5 | 1.380 (11) | C45—C46 | 1.371 (10) |
C4—H4 | 0.9500 | C45—H45 | 0.9500 |
C5—C6 | 1.395 (11) | C46—C47 | 1.382 (10) |
C5—H5 | 0.9500 | C46—H46 | 0.9500 |
C6—H6 | 0.9500 | C47—C48 | 1.397 (10) |
C7—C12 | 1.395 (9) | C47—H47 | 0.9500 |
C7—C8 | 1.403 (8) | C48—H48 | 0.9500 |
C8—C9 | 1.397 (9) | C49—C54 | 1.391 (8) |
C8—H8 | 0.9500 | C49—C50 | 1.397 (9) |
C9—C10 | 1.381 (9) | C50—C51 | 1.392 (9) |
C9—H9 | 0.9500 | C50—H50 | 0.9500 |
C10—C11 | 1.388 (9) | C51—C52 | 1.369 (9) |
C10—H10 | 0.9500 | C51—H51 | 0.9500 |
C11—C12 | 1.383 (9) | C52—C53 | 1.399 (9) |
C11—H11 | 0.9500 | C52—H52 | 0.9500 |
C12—H12 | 0.9500 | C53—C54 | 1.383 (9) |
C13—C18 | 1.383 (9) | C53—H53 | 0.9500 |
C13—C14 | 1.400 (10) | C54—H54 | 0.9500 |
C14—C15 | 1.386 (10) | C55—C56 | 1.499 (10) |
C14—H14 | 0.9500 | C55—H55A | 0.9800 |
C15—C16 | 1.360 (10) | C55—H55B | 0.9800 |
C15—H15 | 0.9500 | C55—H55C | 0.9800 |
C16—C17 | 1.407 (11) | C56—C57 | 1.506 (10) |
C16—H16 | 0.9500 | C57—H57A | 0.9800 |
C17—C18 | 1.377 (10) | C57—H57B | 0.9800 |
C17—H17 | 0.9500 | C57—H57C | 0.9800 |
C18—H18 | 0.9500 | C58—C59 | 1.499 (9) |
C19—C24 | 1.391 (9) | C58—H58A | 0.9800 |
C19—C20 | 1.408 (9) | C58—H58B | 0.9800 |
C20—C21 | 1.377 (9) | C58—H58C | 0.9800 |
C20—H20 | 0.9500 | C59—C60 | 1.490 (9) |
C21—C22 | 1.390 (10) | C60—H60A | 0.9800 |
C21—H21 | 0.9500 | C60—H60B | 0.9800 |
C22—C23 | 1.378 (10) | C60—H60C | 0.9800 |
O1—Tb1—O2 | 85.51 (15) | C13—C14—H14 | 119.6 |
O1—Tb1—O3 | 84.27 (15) | C16—C15—C14 | 120.5 (7) |
O3—Tb1—O2 | 150.09 (14) | C16—C15—H15 | 119.7 |
O3—Tb1—O10 | 79.30 (14) | C14—C15—H15 | 119.7 |
O1—Tb1—O10 | 126.30 (13) | C15—C16—C17 | 119.1 (7) |
O2—Tb1—O10 | 84.35 (14) | C15—C16—H16 | 120.5 |
O3—Tb1—O4 | 128.15 (15) | C17—C16—H16 | 120.5 |
O1—Tb1—O4 | 83.94 (15) | C18—C17—C16 | 120.6 (7) |
O2—Tb1—O4 | 78.35 (15) | C18—C17—H17 | 119.7 |
O10—Tb1—O4 | 143.85 (15) | C16—C17—H17 | 119.7 |
O3—Tb1—O7 | 74.86 (16) | C17—C18—C13 | 120.5 (7) |
O1—Tb1—O7 | 146.47 (16) | C17—C18—H18 | 119.7 |
O2—Tb1—O7 | 124.89 (16) | C13—C18—H18 | 119.7 |
O10—Tb1—O7 | 75.63 (15) | C24—C19—C20 | 119.2 (6) |
O4—Tb1—O7 | 88.62 (17) | C24—C19—P2 | 123.2 (5) |
O3—Tb1—O5 | 76.72 (15) | C20—C19—P2 | 117.5 (5) |
O1—Tb1—O5 | 76.04 (15) | C21—C20—C19 | 119.7 (7) |
O2—Tb1—O5 | 127.50 (15) | C21—C20—H20 | 120.2 |
O10—Tb1—O5 | 145.05 (15) | C19—C20—H20 | 120.2 |
O4—Tb1—O5 | 51.43 (16) | C20—C21—C22 | 120.9 (7) |
O7—Tb1—O5 | 73.82 (16) | C20—C21—H21 | 119.6 |
O3—Tb1—O8 | 123.52 (15) | C22—C21—H21 | 119.6 |
O1—Tb1—O8 | 150.82 (15) | C23—C22—C21 | 119.5 (6) |
O2—Tb1—O8 | 73.90 (15) | C23—C22—H22 | 120.2 |
O10—Tb1—O8 | 72.81 (14) | C21—C22—H22 | 120.2 |
O4—Tb1—O8 | 71.97 (16) | C22—C23—C24 | 120.5 (7) |
O7—Tb1—O8 | 51.26 (16) | C22—C23—H23 | 119.7 |
O5—Tb1—O8 | 100.12 (16) | C24—C23—H23 | 119.7 |
O3—Tb1—O11 | 76.60 (14) | C23—C24—C19 | 120.1 (6) |
O1—Tb1—O11 | 75.33 (13) | C23—C24—H24 | 119.9 |
O2—Tb1—O11 | 73.63 (14) | C19—C24—H24 | 119.9 |
O10—Tb1—O11 | 51.23 (13) | C30—C25—C26 | 119.8 (6) |
O4—Tb1—O11 | 146.11 (15) | C30—C25—P2 | 117.6 (5) |
O7—Tb1—O11 | 123.10 (15) | C26—C25—P2 | 122.5 (5) |
O5—Tb1—O11 | 142.37 (15) | C25—C26—C27 | 118.2 (7) |
O8—Tb1—O11 | 116.69 (15) | C25—C26—H26 | 120.9 |
O3—Tb1—N1 | 102.46 (16) | C27—C26—H26 | 120.9 |
O1—Tb1—N1 | 78.37 (14) | C28—C27—C26 | 121.7 (7) |
O2—Tb1—N1 | 102.87 (16) | C28—C27—H27 | 119.1 |
O10—Tb1—N1 | 155.10 (14) | C26—C27—H27 | 119.1 |
O4—Tb1—N1 | 25.70 (16) | C27—C28—C29 | 119.8 (7) |
O7—Tb1—N1 | 80.85 (16) | C27—C28—H28 | 120.1 |
O5—Tb1—N1 | 25.74 (16) | C29—C28—H28 | 120.1 |
O8—Tb1—N1 | 86.18 (16) | C30—C29—C28 | 119.5 (7) |
O11—Tb1—N1 | 153.65 (14) | C30—C29—H29 | 120.2 |
O3—Tb1—N2 | 99.46 (17) | C28—C29—H29 | 120.2 |
O1—Tb1—N2 | 161.18 (15) | C29—C30—C25 | 120.9 (6) |
O2—Tb1—N2 | 99.24 (17) | C29—C30—H30 | 119.6 |
O10—Tb1—N2 | 72.46 (15) | C25—C30—H30 | 119.6 |
O4—Tb1—N2 | 79.26 (17) | C32—C31—C36 | 119.7 (6) |
O7—Tb1—N2 | 25.81 (17) | C32—C31—P2 | 121.5 (5) |
O5—Tb1—N2 | 86.80 (17) | C36—C31—P2 | 118.8 (5) |
O8—Tb1—N2 | 25.46 (16) | C31—C32—C33 | 119.1 (6) |
O11—Tb1—N2 | 123.50 (15) | C31—C32—H32 | 120.4 |
N1—Tb1—N2 | 82.81 (16) | C33—C32—H32 | 120.4 |
O3—Tb1—N3 | 76.66 (14) | C34—C33—C32 | 120.6 (7) |
O1—Tb1—N3 | 100.75 (14) | C34—C33—H33 | 119.7 |
O2—Tb1—N3 | 77.77 (14) | C32—C33—H33 | 119.7 |
O10—Tb1—N3 | 25.70 (13) | C33—C34—C35 | 120.9 (6) |
O4—Tb1—N3 | 155.19 (16) | C33—C34—H34 | 119.5 |
O7—Tb1—N3 | 99.60 (15) | C35—C34—H34 | 119.5 |
O5—Tb1—N3 | 153.38 (16) | C34—C35—C36 | 119.6 (6) |
O8—Tb1—N3 | 94.94 (15) | C34—C35—H35 | 120.2 |
O11—Tb1—N3 | 25.53 (13) | C36—C35—H35 | 120.2 |
N1—Tb1—N3 | 178.84 (15) | C35—C36—C31 | 120.1 (6) |
N2—Tb1—N3 | 98.07 (15) | C35—C36—H36 | 120.0 |
O1—P1—C13 | 111.4 (3) | C31—C36—H36 | 120.0 |
O1—P1—C1 | 110.1 (3) | C38—C37—C42 | 119.7 (6) |
C13—P1—C1 | 107.4 (3) | C38—C37—P3 | 118.7 (5) |
O1—P1—C7 | 108.6 (3) | C42—C37—P3 | 121.6 (5) |
C13—P1—C7 | 110.1 (3) | C37—C38—C39 | 119.8 (7) |
C1—P1—C7 | 109.1 (3) | C37—C38—H38 | 120.1 |
O2—P2—C31 | 111.3 (3) | C39—C38—H38 | 120.1 |
O2—P2—C19 | 110.7 (3) | C40—C39—C38 | 119.9 (7) |
C31—P2—C19 | 106.9 (3) | C40—C39—H39 | 120.1 |
O2—P2—C25 | 112.2 (3) | C38—C39—H39 | 120.1 |
C31—P2—C25 | 107.3 (3) | C39—C40—C41 | 120.4 (7) |
C19—P2—C25 | 108.1 (3) | C39—C40—H40 | 119.8 |
O3—P3—C43 | 111.5 (3) | C41—C40—H40 | 119.8 |
O3—P3—C49 | 111.1 (3) | C42—C41—C40 | 120.7 (7) |
C43—P3—C49 | 107.5 (3) | C42—C41—H41 | 119.6 |
O3—P3—C37 | 111.1 (3) | C40—C41—H41 | 119.6 |
C43—P3—C37 | 107.7 (3) | C41—C42—C37 | 119.6 (6) |
C49—P3—C37 | 107.8 (3) | C41—C42—H42 | 120.2 |
P1—O1—Tb1 | 154.7 (3) | C37—C42—H42 | 120.2 |
P2—O2—Tb1 | 159.6 (3) | C44—C43—C48 | 119.7 (6) |
P3—O3—Tb1 | 173.8 (3) | C44—C43—P3 | 121.9 (5) |
N1—O4—Tb1 | 96.8 (4) | C48—C43—P3 | 118.3 (5) |
N1—O5—Tb1 | 95.6 (4) | C43—C44—C45 | 120.7 (6) |
N2—O7—Tb1 | 96.8 (4) | C43—C44—H44 | 119.6 |
N2—O8—Tb1 | 95.9 (4) | C45—C44—H44 | 119.6 |
N3—O10—Tb1 | 98.0 (3) | C46—C45—C44 | 119.3 (7) |
N3—O11—Tb1 | 94.6 (3) | C46—C45—H45 | 120.4 |
O6—N1—O5 | 122.4 (6) | C44—C45—H45 | 120.4 |
O6—N1—O4 | 121.5 (6) | C45—C46—C47 | 120.7 (7) |
O5—N1—O4 | 116.1 (5) | C45—C46—H46 | 119.6 |
O6—N1—Tb1 | 177.4 (4) | C47—C46—H46 | 119.6 |
O5—N1—Tb1 | 58.7 (3) | C46—C47—C48 | 119.9 (6) |
O4—N1—Tb1 | 57.5 (3) | C46—C47—H47 | 120.0 |
O9—N2—O8 | 122.0 (7) | C48—C47—H47 | 120.0 |
O9—N2—O7 | 122.0 (6) | C43—C48—C47 | 119.6 (7) |
O8—N2—O7 | 116.1 (5) | C43—C48—H48 | 120.2 |
O9—N2—Tb1 | 179.1 (5) | C47—C48—H48 | 120.2 |
O8—N2—Tb1 | 58.6 (3) | C54—C49—C50 | 120.2 (6) |
O7—N2—Tb1 | 57.4 (3) | C54—C49—P3 | 118.0 (5) |
O12—N3—O11 | 122.6 (5) | C50—C49—P3 | 121.8 (5) |
O12—N3—O10 | 121.2 (5) | C51—C50—C49 | 119.4 (6) |
O11—N3—O10 | 116.1 (5) | C51—C50—H50 | 120.3 |
O12—N3—Tb1 | 177.3 (4) | C49—C50—H50 | 120.3 |
O11—N3—Tb1 | 59.8 (3) | C52—C51—C50 | 120.6 (6) |
O10—N3—Tb1 | 56.3 (3) | C52—C51—H51 | 119.7 |
C2—C1—C6 | 120.7 (7) | C50—C51—H51 | 119.7 |
C2—C1—P1 | 119.3 (5) | C51—C52—C53 | 120.0 (6) |
C6—C1—P1 | 120.0 (6) | C51—C52—H52 | 120.0 |
C1—C2—C3 | 120.3 (7) | C53—C52—H52 | 120.0 |
C1—C2—H2 | 119.9 | C54—C53—C52 | 120.2 (6) |
C3—C2—H2 | 119.9 | C54—C53—H53 | 119.9 |
C4—C3—C2 | 119.3 (8) | C52—C53—H53 | 119.9 |
C4—C3—H3 | 120.4 | C53—C54—C49 | 119.6 (6) |
C2—C3—H3 | 120.4 | C53—C54—H54 | 120.2 |
C3—C4—C5 | 121.0 (7) | C49—C54—H54 | 120.2 |
C3—C4—H4 | 119.5 | C56—C55—H55A | 109.5 |
C5—C4—H4 | 119.5 | C56—C55—H55B | 109.5 |
C4—C5—C6 | 120.7 (7) | H55A—C55—H55B | 109.5 |
C4—C5—H5 | 119.7 | C56—C55—H55C | 109.5 |
C6—C5—H5 | 119.7 | H55A—C55—H55C | 109.5 |
C5—C6—C1 | 118.0 (7) | H55B—C55—H55C | 109.5 |
C5—C6—H6 | 121.0 | O13—C56—C55 | 122.5 (7) |
C1—C6—H6 | 121.0 | O13—C56—C57 | 121.0 (7) |
C12—C7—C8 | 119.2 (6) | C55—C56—C57 | 116.4 (7) |
C12—C7—P1 | 117.9 (5) | C56—C57—H57A | 109.5 |
C8—C7—P1 | 122.7 (5) | C56—C57—H57B | 109.5 |
C9—C8—C7 | 119.7 (6) | H57A—C57—H57B | 109.5 |
C9—C8—H8 | 120.2 | C56—C57—H57C | 109.5 |
C7—C8—H8 | 120.2 | H57A—C57—H57C | 109.5 |
C10—C9—C8 | 120.2 (6) | H57B—C57—H57C | 109.5 |
C10—C9—H9 | 119.9 | C59—C58—H58A | 109.5 |
C8—C9—H9 | 119.9 | C59—C58—H58B | 109.5 |
C9—C10—C11 | 120.4 (6) | H58A—C58—H58B | 109.5 |
C9—C10—H10 | 119.8 | C59—C58—H58C | 109.5 |
C11—C10—H10 | 119.8 | H58A—C58—H58C | 109.5 |
C12—C11—C10 | 119.9 (6) | H58B—C58—H58C | 109.5 |
C12—C11—H11 | 120.1 | O14—C59—C60 | 122.2 (11) |
C10—C11—H11 | 120.1 | O14—C59—C58 | 123.0 (11) |
C11—C12—C7 | 120.7 (6) | C60—C59—C58 | 114.8 (11) |
C11—C12—H12 | 119.7 | C59—C60—H60A | 109.5 |
C7—C12—H12 | 119.7 | C59—C60—H60B | 109.5 |
C18—C13—C14 | 118.4 (6) | H60A—C60—H60B | 109.5 |
C18—C13—P1 | 120.6 (5) | C59—C60—H60C | 109.5 |
C14—C13—P1 | 120.2 (5) | H60A—C60—H60C | 109.5 |
C15—C14—C13 | 120.8 (7) | H60B—C60—H60C | 109.5 |
C15—C14—H14 | 119.6 |
Experimental details
Crystal data | |
Chemical formula | [Tb(NO3)3(C18H15OP)3]·1.5C3H6O |
Mr | 1266.88 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 120 |
a, b, c (Å) | 11.0612 (10), 19.180 (2), 27.641 (4) |
β (°) | 94.895 (7) |
V (Å3) | 5842.7 (12) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.36 |
Crystal size (mm) | 0.16 × 0.16 × 0.10 |
Data collection | |
Diffractometer | Nonius KappaCCD area-detector diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1997) |
Tmin, Tmax | 0.847, 0.873 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 40261, 10247, 6620 |
Rint | 0.111 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.135, 1.03 |
No. of reflections | 10247 |
No. of parameters | 711 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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).
Tb1—O1 | 2.307 (4) | Tb1—O8 | 2.505 (4) |
Tb1—O2 | 2.309 (4) | Tb1—O10 | 2.459 (4) |
Tb1—O3 | 2.295 (4) | Tb1—O11 | 2.539 (4) |
Tb1—O4 | 2.467 (4) | P1—O1 | 1.502 (4) |
Tb1—O5 | 2.492 (5) | P2—O2 | 1.508 (5) |
Tb1—O7 | 2.476 (4) | P3—O3 | 1.504 (5) |
O1—Tb1—O2 | 85.51 (15) | P1—O1—Tb1 | 154.7 (3) |
O1—Tb1—O3 | 84.27 (15) | P2—O2—Tb1 | 159.6 (3) |
O3—Tb1—O2 | 150.09 (14) | P3—O3—Tb1 | 173.8 (3) |
O4—Tb1—O5 | 51.43 (16) | O6—N1—O5 | 122.4 (6) |
O7—Tb1—O8 | 51.26 (16) | O6—N1—O4 | 121.5 (6) |
O10—Tb1—O11 | 51.23 (13) | O5—N1—O4 | 116.1 (5) |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
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)].