Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807022350/hg2233sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807022350/hg2233Isup2.hkl |
CCDC reference: 650676
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (C-C) = 0.016 Å
- Disorder in solvent or counterion
- R factor = 0.050
- wR factor = 0.104
- Data-to-parameter ratio = 10.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 16 PLAT480_ALERT_4_C Long H...A H-Bond Reported H6A .. O6 .. 2.63 Ang.
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 26.00 From the CIF: _reflns_number_total 9791 Count of symmetry unique reflns 7131 Completeness (_total/calc) 137.30% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2660 Fraction of Friedel pairs measured 0.373 Are heavy atom types Z>Si present yes PLAT792_ALERT_1_G Check the Absolute Configuration of C21 = ... S PLAT792_ALERT_1_G Check the Absolute Configuration of C52 = ... R PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Alexander (1995); Hu et al. (2003, 2004, 2007); Spodine et al. (2000).
To a methanolic solution (20 ml) of 2,6-diformyl-4-methylphenol(1 mmol) and Lu(NO3)3.6H2O (0.5 mmol), 1,5-diamino-3-azapentane (1 mmol) was added dropwise. After refluxing 3 h, the solvent was removed. The resultant yellow solid was recrystallized in methanol/ethyl acetate (4/1,v/v) to yield yellow crystals suitable for X-ray analysis.
The carbon-bound H atoms were generated geometrically (C—H 0.93 to 0.97 Å) and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2Ueq(C). The nitrogen H were located in a difference Fourier map, and were refined with an N—H distance restraint of 0.90 (1) Å for the sp3-N and 0.86 (1) Å for the sp2-N, their temperature factors were set to 1.2Ueq(C). The water H atoms were also located in a difference Fourier map, and was refined with an O—H distance restraint of 0.85 (1) Å.
Lanthanide macrocyclic complexes are of particular interest because they have many possible applications in biological systems, material science and chemical processes (Alexander, 1995). Our research is focused on the syntheses, crystal structures and properties of lanthanide(III) complexes with macrocyclic Schiff bases (Hu et al., 2003; Hu et al., 2004). Recently, we have reported the crystal structure of a gadolinium(III) complex with the macrocyclic ligand dervided from 2,6-diformyl-4-methylphenol and 1,5-diamino-3-azapentane ([Gd(III)(C26H34N6O2)(NO3)2]+.(NO3)-.H20), in which the central ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O atoms of two bidentae nitrates (Hu et al., 2007). As a part of a continuing study, herein we report a new lutecium analogue [Lu(III)(C26H34N6O2)(NO3)2]+. (NO3)-. 0.5H20. 0.25CH3COOC2H5 (I), but which is a different solvate, belonging to a different space group (space group Cc, compared with C2/c).
In the asymmetric unit (Fig. 1), there are two molecules of the title complex (I) which exhibit a similar coordinate geometry with the previous complex (Hu et al., 2007)(Fig. 2). Lu1 is encapsulated within the macrocyclic ligand which provided five donor atoms (the two O atoms O1,O2 from the phenolates and the three N atoms N1, N2, N3 from one end of the macrocycle). The ninefold coordination is completed around Lu1 by two bidentate nitrates which locate on the opposite sides of the bisphenoidal positions. The third nitrate is ionic. At the free end of the macrocycle, a five-membered imidazole rings is formed. The coordination polyhedron can be described as a distorted tricapped trigonal prism in which N2, O3 and O6 are located at capped sites, as shown in Fig.2. When the phenol oxygen atoms coordinate to the lanthanide ion, the phenol H atoms dissociate and are transferred to the neigbouring imidazole nitrogen to give a zwitterionic structure. This proton transfer has been conformed by NMR study of the tetraiminodiphenol analogue (Spodine et al., 2000).
For related literature, see: Alexander (1995); Hu et al. (2003, 2004, 2007); Spodine et al. (2000).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. Thermal ellipsoid plot of (I). Displacement ellipsoids are drawn at the 30% probability level. | |
Fig. 2. Coordination polyhedron in (I). |
[Lu(C26H34N6O2)(NO3)2]NO3·0.5H2O·0.25C4H8O2 | F(000) = 3432 |
Mr = 854.63 | Dx = 1.568 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 5188 reflections |
a = 24.649 (3) Å | θ = 2.7–25.6° |
b = 14.0182 (11) Å | µ = 2.80 mm−1 |
c = 21.4453 (17) Å | T = 291 K |
β = 102.307 (2)° | Block, yellow |
V = 7239.8 (11) Å3 | 0.32 × 0.26 × 0.24 mm |
Z = 8 |
Bruker SMART CCD area-detector diffractometer | 9791 independent reflections |
Radiation source: sealed tube | 8284 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
φ and ω scans | θmax = 26.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −28→30 |
Tmin = 0.42, Tmax = 0.51 | k = −17→17 |
20514 measured reflections | l = −26→18 |
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)] = 0.050 | H-atom parameters constrained |
wR(F2) = 0.104 | w = 1/[σ2(Fo2) + (0.06P)2 + 1.55P] where P = (Fo2 + 2Fc2)/3 |
S = 0.98 | (Δ/σ)max < 0.001 |
9791 reflections | Δρmax = 1.07 e Å−3 |
913 parameters | Δρmin = −1.58 e Å−3 |
2 restraints | Absolute structure: Flack (1983), with 2678 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.016 (10) |
[Lu(C26H34N6O2)(NO3)2]NO3·0.5H2O·0.25C4H8O2 | V = 7239.8 (11) Å3 |
Mr = 854.63 | Z = 8 |
Monoclinic, Cc | Mo Kα radiation |
a = 24.649 (3) Å | µ = 2.80 mm−1 |
b = 14.0182 (11) Å | T = 291 K |
c = 21.4453 (17) Å | 0.32 × 0.26 × 0.24 mm |
β = 102.307 (2)° |
Bruker SMART CCD area-detector diffractometer | 9791 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 8284 reflections with I > 2σ(I) |
Tmin = 0.42, Tmax = 0.51 | Rint = 0.046 |
20514 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | H-atom parameters constrained |
wR(F2) = 0.104 | Δρmax = 1.07 e Å−3 |
S = 0.98 | Δρmin = −1.58 e Å−3 |
9791 reflections | Absolute structure: Flack (1983), with 2678 Friedel pairs |
913 parameters | Absolute structure parameter: 0.016 (10) |
2 restraints |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.9197 (4) | 0.6393 (7) | 0.5542 (6) | 0.043 (2) | |
C2 | 0.9711 (4) | 0.6880 (7) | 0.5549 (6) | 0.040 (2) | |
C3 | 0.9722 (5) | 0.7835 (6) | 0.5339 (6) | 0.045 (3) | |
H3 | 1.0062 | 0.8125 | 0.5342 | 0.054* | |
C4 | 0.9244 (5) | 0.8340 (7) | 0.5132 (6) | 0.050 (3) | |
C5 | 0.8765 (5) | 0.7906 (8) | 0.5130 (6) | 0.055 (3) | |
H5 | 0.8442 | 0.8258 | 0.4995 | 0.066* | |
C6 | 0.8709 (4) | 0.6956 (8) | 0.5316 (6) | 0.045 (3) | |
C7 | 0.9282 (5) | 0.9340 (7) | 0.4926 (6) | 0.054 (3) | |
H7A | 0.8916 | 0.9582 | 0.4757 | 0.080* | |
H7B | 0.9497 | 0.9367 | 0.4602 | 0.080* | |
H7C | 0.9458 | 0.9720 | 0.5284 | 0.080* | |
C8 | 0.8162 (5) | 0.6599 (8) | 0.5362 (6) | 0.049 (3) | |
H8 | 0.7878 | 0.7049 | 0.5283 | 0.059* | |
C9 | 0.7438 (5) | 0.5612 (9) | 0.5532 (7) | 0.052 (3) | |
H9A | 0.7247 | 0.5244 | 0.5168 | 0.063* | |
H9B | 0.7251 | 0.6222 | 0.5528 | 0.063* | |
C10 | 0.7423 (5) | 0.5092 (8) | 0.6134 (6) | 0.049 (3) | |
H10A | 0.7599 | 0.5470 | 0.6500 | 0.059* | |
H10B | 0.7042 | 0.4971 | 0.6163 | 0.059* | |
C11 | 0.7781 (5) | 0.3693 (8) | 0.6744 (6) | 0.052 (3) | |
H11A | 0.7420 | 0.3599 | 0.6846 | 0.062* | |
H11B | 0.8007 | 0.4071 | 0.7080 | 0.062* | |
C12 | 0.8055 (5) | 0.2746 (9) | 0.6691 (6) | 0.057 (3) | |
H12A | 0.8178 | 0.2472 | 0.7112 | 0.069* | |
H12B | 0.7789 | 0.2312 | 0.6438 | 0.069* | |
C13 | 0.8871 (5) | 0.2180 (9) | 0.6469 (5) | 0.051 (3) | |
H13 | 0.8802 | 0.1712 | 0.6749 | 0.062* | |
C14 | 0.9349 (3) | 0.2014 (5) | 0.6188 (3) | 0.040 (3) | |
C15 | 0.9667 (3) | 0.1209 (4) | 0.6392 (3) | 0.054 (4) | |
H15 | 0.9573 | 0.0813 | 0.6701 | 0.065* | |
C16 | 1.0125 (3) | 0.0996 (4) | 0.6135 (4) | 0.059 (4) | |
C17 | 1.0265 (3) | 0.1588 (6) | 0.5674 (4) | 0.056 (3) | |
H17 | 1.0571 | 0.1446 | 0.5502 | 0.067* | |
C18 | 0.9947 (3) | 0.2393 (5) | 0.5470 (3) | 0.054 (3) | |
C19 | 0.9489 (3) | 0.2606 (4) | 0.5727 (3) | 0.046 (3) | |
C20 | 1.0465 (5) | 0.0076 (8) | 0.6313 (6) | 0.058 (3) | |
H20A | 1.0267 | −0.0345 | 0.6539 | 0.088* | |
H20B | 1.0818 | 0.0232 | 0.6580 | 0.088* | |
H20C | 1.0520 | −0.0231 | 0.5932 | 0.088* | |
C21 | 1.0143 (6) | 0.3040 (10) | 0.4989 (7) | 0.065 (4) | |
H21 | 1.0444 | 0.2733 | 0.4831 | 0.078* | |
C22 | 0.9861 (6) | 0.4177 (8) | 0.4176 (7) | 0.062 (3) | |
H22A | 0.9938 | 0.4066 | 0.3757 | 0.074* | |
H22B | 0.9578 | 0.4667 | 0.4142 | 0.074* | |
C23 | 1.0382 (5) | 0.4466 (8) | 0.4648 (6) | 0.049 (3) | |
H23A | 1.0713 | 0.4243 | 0.4516 | 0.059* | |
H23B | 1.0404 | 0.5153 | 0.4705 | 0.059* | |
C24 | 1.0743 (5) | 0.4001 (9) | 0.5807 (6) | 0.061 (3) | |
H24A | 1.1089 | 0.3773 | 0.5714 | 0.073* | |
H24B | 1.0640 | 0.3578 | 0.6121 | 0.073* | |
C25 | 1.0821 (5) | 0.5007 (8) | 0.6073 (7) | 0.054 (3) | |
H25A | 1.0968 | 0.4984 | 0.6530 | 0.064* | |
H25B | 1.1083 | 0.5350 | 0.5877 | 0.064* | |
C26 | 1.0234 (4) | 0.6374 (7) | 0.5722 (5) | 0.043 (2) | |
H26 | 1.0555 | 0.6687 | 0.5675 | 0.052* | |
C27 | 0.6628 (5) | −0.0607 (8) | 0.8491 (6) | 0.051 (3) | |
C28 | 0.6884 (4) | −0.1463 (7) | 0.8727 (5) | 0.043 (2) | |
C29 | 0.6701 (4) | −0.2323 (7) | 0.8434 (7) | 0.051 (3) | |
H29 | 0.6879 | −0.2880 | 0.8604 | 0.061* | |
C30 | 0.6263 (5) | −0.2399 (7) | 0.7895 (7) | 0.056 (3) | |
C31 | 0.5985 (5) | −0.1562 (7) | 0.7699 (6) | 0.050 (3) | |
H31 | 0.5670 | −0.1592 | 0.7372 | 0.060* | |
C32 | 0.6154 (5) | −0.0653 (7) | 0.7970 (5) | 0.042 (2) | |
C33 | 0.6069 (5) | −0.3341 (8) | 0.7597 (7) | 0.062 (4) | |
H33A | 0.6329 | −0.3568 | 0.7355 | 0.093* | |
H33B | 0.5711 | −0.3265 | 0.7319 | 0.093* | |
H33C | 0.6044 | −0.3793 | 0.7926 | 0.093* | |
C34 | 0.5814 (4) | 0.0168 (8) | 0.7729 (6) | 0.049 (3) | |
H34 | 0.5461 | 0.0044 | 0.7486 | 0.059* | |
C35 | 0.5516 (4) | 0.1746 (8) | 0.7561 (6) | 0.050 (3) | |
H35A | 0.5271 | 0.1493 | 0.7182 | 0.060* | |
H35B | 0.5295 | 0.1873 | 0.7876 | 0.060* | |
C36 | 0.5767 (5) | 0.2641 (8) | 0.7401 (6) | 0.049 (3) | |
H36A | 0.5938 | 0.2546 | 0.7038 | 0.059* | |
H36B | 0.5486 | 0.3133 | 0.7293 | 0.059* | |
C37 | 0.6478 (5) | 0.3853 (7) | 0.7905 (6) | 0.050 (3) | |
H37A | 0.6624 | 0.3846 | 0.7519 | 0.060* | |
H37B | 0.6213 | 0.4372 | 0.7871 | 0.060* | |
C38 | 0.6937 (4) | 0.4018 (9) | 0.8460 (6) | 0.051 (3) | |
H38A | 0.6797 | 0.4046 | 0.8850 | 0.061* | |
H38B | 0.7123 | 0.4615 | 0.8412 | 0.061* | |
C39 | 0.7845 (5) | 0.3431 (8) | 0.8509 (6) | 0.049 (3) | |
H39 | 0.7936 | 0.4075 | 0.8555 | 0.059* | |
C40 | 0.8274 (5) | 0.2798 (8) | 0.8475 (6) | 0.053 (3) | |
C41 | 0.8802 (5) | 0.3194 (8) | 0.8479 (6) | 0.051 (3) | |
H41 | 0.8848 | 0.3850 | 0.8531 | 0.061* | |
C42 | 0.9261 (5) | 0.2645 (9) | 0.8407 (7) | 0.059 (3) | |
C43 | 0.9177 (5) | 0.1680 (9) | 0.8314 (6) | 0.056 (3) | |
H43 | 0.9469 | 0.1308 | 0.8241 | 0.067* | |
C44 | 0.8659 (5) | 0.1219 (8) | 0.8326 (6) | 0.050 (3) | |
C45 | 0.8203 (4) | 0.1779 (6) | 0.8436 (5) | 0.038 (2) | |
C46 | 0.9822 (5) | 0.3050 (9) | 0.8427 (7) | 0.058 (3) | |
H46A | 1.0025 | 0.2634 | 0.8204 | 0.088* | |
H46B | 1.0018 | 0.3111 | 0.8863 | 0.088* | |
H46C | 0.9786 | 0.3666 | 0.8227 | 0.088* | |
C47 | 0.8622 (4) | 0.0231 (7) | 0.8258 (6) | 0.045 (3) | |
H47 | 0.8922 | −0.0100 | 0.8166 | 0.054* | |
C48 | 0.8125 (6) | −0.1293 (8) | 0.8313 (7) | 0.056 (3) | |
H48A | 0.8399 | −0.1581 | 0.8107 | 0.068* | |
H48B | 0.7759 | −0.1466 | 0.8071 | 0.068* | |
C49 | 0.8200 (6) | −0.1655 (8) | 0.8978 (7) | 0.057 (3) | |
H49A | 0.8088 | −0.2320 | 0.8968 | 0.068* | |
H49B | 0.8589 | −0.1619 | 0.9186 | 0.068* | |
C50 | 0.8126 (5) | −0.1082 (9) | 1.0030 (6) | 0.053 (3) | |
H50A | 0.8464 | −0.0707 | 1.0113 | 0.064* | |
H50B | 0.8206 | −0.1718 | 1.0202 | 0.064* | |
C51 | 0.7663 (5) | −0.0596 (10) | 1.0305 (6) | 0.058 (3) | |
H51A | 0.7636 | −0.0869 | 1.0713 | 0.070* | |
H51B | 0.7722 | 0.0086 | 1.0353 | 0.070* | |
C52 | 0.7310 (5) | −0.1478 (7) | 0.9330 (6) | 0.045 (3) | |
H52 | 0.7338 | −0.2126 | 0.9505 | 0.054* | |
C53 | 0.7210 (8) | 0.7880 (17) | 0.6733 (11) | 0.048 (5) | 0.50 |
H53A | 0.7306 | 0.7770 | 0.7185 | 0.072* | 0.50 |
H53B | 0.7231 | 0.7290 | 0.6512 | 0.072* | 0.50 |
H53C | 0.6839 | 0.8128 | 0.6617 | 0.072* | 0.50 |
C54 | 0.7593 (9) | 0.8558 (15) | 0.6559 (9) | 0.041 (5) | 0.50 |
H54A | 0.7586 | 0.9148 | 0.6793 | 0.049* | 0.50 |
H54B | 0.7488 | 0.8699 | 0.6106 | 0.049* | 0.50 |
C55 | 0.8599 (8) | 0.8684 (18) | 0.6700 (14) | 0.054 (7) | 0.50 |
C56 | 0.9091 (9) | 0.8130 (16) | 0.6889 (11) | 0.048 (5) | 0.50 |
H56A | 0.9384 | 0.8525 | 0.7120 | 0.072* | 0.50 |
H56B | 0.9198 | 0.7875 | 0.6518 | 0.072* | 0.50 |
H56C | 0.9023 | 0.7615 | 0.7158 | 0.072* | 0.50 |
Lu1 | 0.861690 (18) | 0.43572 (3) | 0.58012 (2) | 0.04135 (12) | |
Lu2 | 0.686348 (16) | 0.16395 (2) | 0.834229 (18) | 0.03540 (10) | |
N1 | 0.8014 (4) | 0.5761 (6) | 0.5494 (5) | 0.046 (2) | |
N2 | 0.7720 (4) | 0.4191 (6) | 0.6124 (5) | 0.046 (2) | |
H2 | 0.7502 | 0.3815 | 0.5827 | 0.055* | |
N3 | 0.8538 (4) | 0.2866 (6) | 0.6385 (4) | 0.045 (2) | |
N4 | 0.9676 (5) | 0.3261 (7) | 0.4451 (5) | 0.057 (3) | |
H4A | 0.9359 | 0.3351 | 0.4588 | 0.069* | |
H4B | 0.9625 | 0.2790 | 0.4159 | 0.069* | |
N5 | 1.0309 (4) | 0.3991 (6) | 0.5223 (5) | 0.055 (2) | |
N6 | 1.0278 (4) | 0.5506 (6) | 0.5939 (5) | 0.052 (2) | |
H6A | 0.9988 | 0.5216 | 0.6006 | 0.062* | |
N7 | 0.8102 (5) | 0.4138 (7) | 0.4465 (6) | 0.056 (3) | |
N8 | 0.9215 (4) | 0.4878 (8) | 0.7090 (5) | 0.057 (3) | |
N9 | 0.7326 (4) | 0.3201 (6) | 0.8481 (6) | 0.051 (3) | |
N10 | 0.6186 (4) | 0.2922 (6) | 0.7962 (5) | 0.048 (2) | |
H10 | 0.5997 | 0.3011 | 0.8279 | 0.058* | |
N11 | 0.5950 (3) | 0.1032 (6) | 0.7817 (4) | 0.042 (2) | |
N12 | 0.7163 (4) | −0.0818 (6) | 0.9802 (5) | 0.050 (2) | |
H12C | 0.6901 | −0.1084 | 0.9981 | 0.061* | |
H12D | 0.7024 | −0.0275 | 0.9607 | 0.061* | |
N13 | 0.7873 (3) | −0.1108 (6) | 0.9349 (4) | 0.041 (2) | |
N14 | 0.8188 (4) | −0.0240 (6) | 0.8319 (4) | 0.042 (2) | |
H14A | 0.7905 | 0.0089 | 0.8368 | 0.050* | |
N15 | 0.7020 (4) | 0.1155 (7) | 0.7101 (5) | 0.049 (2) | |
N16 | 0.6773 (5) | 0.2001 (7) | 0.9653 (6) | 0.057 (3) | |
N17 | 0.6489 (4) | 0.7472 (7) | 0.0480 (5) | 0.056 (2) | |
N18 | 0.9898 (5) | 0.1321 (8) | 0.3560 (5) | 0.059 (3) | |
O1 | 0.9185 (3) | 0.5520 (5) | 0.5724 (4) | 0.0416 (17) | |
O2 | 0.9172 (3) | 0.3362 (5) | 0.5484 (4) | 0.0427 (17) | |
O3 | 0.8551 (4) | 0.4623 (6) | 0.4596 (4) | 0.057 (2) | |
O4 | 0.7950 (4) | 0.3748 (6) | 0.4930 (4) | 0.060 (2) | |
O5 | 0.7842 (4) | 0.4060 (6) | 0.3895 (5) | 0.070 (3) | |
O6 | 0.9455 (4) | 0.4326 (6) | 0.6774 (4) | 0.059 (2) | |
O7 | 0.8713 (3) | 0.5109 (5) | 0.6807 (4) | 0.051 (2) | |
O8 | 0.9429 (4) | 0.5204 (6) | 0.7596 (4) | 0.066 (2) | |
O9 | 0.7745 (3) | 0.1369 (5) | 0.8477 (4) | 0.0429 (17) | |
O10 | 0.6809 (3) | 0.0204 (5) | 0.8760 (3) | 0.0414 (17) | |
O11 | 0.6952 (3) | 0.1997 (5) | 0.7290 (4) | 0.050 (2) | |
O12 | 0.7000 (4) | 0.0487 (6) | 0.7474 (4) | 0.054 (2) | |
O13 | 0.7098 (4) | 0.1021 (6) | 0.6571 (4) | 0.056 (2) | |
O14 | 0.7238 (4) | 0.1754 (6) | 0.9538 (4) | 0.052 (2) | |
O15 | 0.6371 (4) | 0.2078 (6) | 0.9178 (4) | 0.054 (2) | |
O16 | 0.6708 (3) | 0.2150 (6) | 1.0200 (4) | 0.056 (2) | |
O17 | 0.6216 (3) | 0.6988 (5) | 0.0788 (4) | 0.052 (2) | |
O18 | 0.6296 (3) | 0.8255 (6) | 0.0222 (4) | 0.054 (2) | |
O19 | 0.6943 (3) | 0.7219 (6) | 0.0393 (4) | 0.054 (2) | |
O20 | 1.0301 (4) | 0.1780 (6) | 0.3784 (4) | 0.060 (2) | |
O21 | 0.9908 (3) | 0.0624 (6) | 0.3228 (5) | 0.059 (2) | |
O22 | 0.9461 (3) | 0.1601 (5) | 0.3690 (4) | 0.055 (2) | |
O23 | 0.8155 (6) | 0.8141 (9) | 0.6712 (7) | 0.039 (3) | 0.50 |
O24 | 0.8546 (6) | 0.9498 (14) | 0.6541 (10) | 0.065 (5) | 0.50 |
O25 | 0.8703 (6) | 0.6513 (10) | 0.8171 (8) | 0.066 (4) | 0.60 |
H25F | 0.8771 | 0.6497 | 0.7799 | 0.079* | 0.60 |
H25C | 0.8395 | 0.6238 | 0.8167 | 0.079* | 0.60 |
O26 | 0.5948 (7) | 0.5428 (14) | 0.9459 (10) | 0.056 (5) | 0.40 |
H26A | 0.6012 | 0.5507 | 0.9861 | 0.067* | 0.40 |
H26B | 0.5846 | 0.4856 | 0.9370 | 0.067* | 0.40 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.046 (6) | 0.027 (5) | 0.053 (7) | −0.003 (4) | 0.006 (5) | −0.004 (5) |
C2 | 0.031 (5) | 0.038 (5) | 0.057 (7) | −0.012 (4) | 0.019 (4) | −0.010 (5) |
C3 | 0.057 (6) | 0.024 (5) | 0.057 (7) | −0.004 (4) | 0.018 (5) | −0.006 (5) |
C4 | 0.058 (7) | 0.032 (5) | 0.053 (7) | −0.006 (5) | −0.004 (5) | −0.009 (5) |
C5 | 0.061 (7) | 0.036 (6) | 0.065 (8) | 0.020 (5) | 0.009 (6) | 0.007 (6) |
C6 | 0.041 (6) | 0.043 (6) | 0.053 (7) | 0.014 (5) | 0.015 (5) | −0.004 (5) |
C7 | 0.063 (7) | 0.038 (6) | 0.049 (7) | 0.007 (5) | −0.010 (6) | 0.002 (5) |
C8 | 0.044 (6) | 0.051 (6) | 0.050 (7) | 0.013 (5) | 0.005 (5) | −0.014 (5) |
C9 | 0.037 (6) | 0.057 (7) | 0.061 (9) | 0.007 (5) | 0.007 (6) | 0.001 (6) |
C10 | 0.048 (6) | 0.041 (6) | 0.058 (8) | 0.004 (5) | 0.013 (5) | 0.006 (5) |
C11 | 0.067 (8) | 0.044 (6) | 0.055 (7) | −0.019 (5) | 0.037 (6) | −0.016 (5) |
C12 | 0.056 (7) | 0.062 (7) | 0.055 (8) | −0.027 (6) | 0.015 (6) | −0.002 (6) |
C13 | 0.054 (7) | 0.061 (7) | 0.033 (6) | −0.018 (6) | −0.006 (5) | 0.007 (5) |
C14 | 0.056 (7) | 0.018 (4) | 0.039 (6) | 0.002 (4) | −0.005 (5) | 0.009 (4) |
C15 | 0.066 (8) | 0.028 (5) | 0.055 (7) | −0.003 (5) | −0.020 (6) | 0.011 (5) |
C16 | 0.068 (8) | 0.053 (7) | 0.046 (7) | 0.010 (6) | −0.013 (6) | −0.025 (6) |
C17 | 0.039 (6) | 0.058 (7) | 0.062 (8) | 0.008 (5) | −0.009 (5) | −0.016 (6) |
C18 | 0.065 (8) | 0.052 (7) | 0.040 (6) | 0.007 (5) | −0.003 (6) | −0.014 (5) |
C19 | 0.049 (7) | 0.040 (6) | 0.040 (6) | −0.002 (5) | −0.010 (5) | −0.008 (5) |
C20 | 0.064 (8) | 0.046 (6) | 0.052 (8) | 0.017 (5) | −0.015 (6) | −0.011 (6) |
C21 | 0.057 (8) | 0.066 (8) | 0.068 (9) | 0.024 (6) | 0.005 (7) | −0.006 (7) |
C22 | 0.073 (9) | 0.052 (7) | 0.066 (9) | 0.015 (6) | 0.032 (7) | 0.014 (6) |
C23 | 0.048 (6) | 0.050 (6) | 0.055 (7) | 0.010 (5) | 0.027 (5) | −0.020 (5) |
C24 | 0.056 (7) | 0.065 (7) | 0.054 (8) | 0.019 (6) | −0.003 (6) | −0.015 (6) |
C25 | 0.040 (6) | 0.048 (6) | 0.070 (9) | 0.006 (5) | 0.007 (5) | 0.006 (6) |
C26 | 0.032 (5) | 0.046 (6) | 0.051 (7) | −0.002 (4) | 0.010 (5) | 0.008 (5) |
C27 | 0.047 (6) | 0.047 (6) | 0.058 (8) | −0.012 (5) | 0.015 (6) | 0.019 (6) |
C28 | 0.044 (6) | 0.042 (6) | 0.045 (6) | −0.007 (4) | 0.014 (5) | −0.012 (5) |
C29 | 0.049 (6) | 0.022 (4) | 0.078 (9) | 0.002 (4) | 0.007 (6) | 0.011 (5) |
C30 | 0.066 (7) | 0.019 (5) | 0.077 (9) | −0.010 (4) | 0.006 (6) | −0.013 (5) |
C31 | 0.037 (6) | 0.040 (6) | 0.070 (8) | −0.004 (4) | 0.007 (5) | 0.007 (6) |
C32 | 0.044 (6) | 0.041 (5) | 0.039 (6) | −0.001 (4) | 0.002 (5) | −0.003 (5) |
C33 | 0.057 (7) | 0.046 (6) | 0.070 (9) | −0.014 (5) | −0.015 (6) | −0.018 (6) |
C34 | 0.031 (5) | 0.058 (7) | 0.051 (7) | −0.011 (5) | −0.009 (5) | −0.013 (6) |
C35 | 0.038 (5) | 0.050 (6) | 0.057 (7) | 0.008 (4) | 0.003 (5) | 0.020 (6) |
C36 | 0.055 (7) | 0.043 (6) | 0.048 (7) | 0.010 (5) | 0.009 (5) | −0.003 (5) |
C37 | 0.071 (8) | 0.034 (5) | 0.050 (7) | 0.009 (5) | 0.026 (6) | 0.018 (5) |
C38 | 0.032 (6) | 0.067 (7) | 0.055 (8) | −0.002 (5) | 0.011 (5) | −0.003 (6) |
C39 | 0.060 (7) | 0.039 (6) | 0.054 (8) | −0.007 (5) | 0.022 (6) | −0.014 (5) |
C40 | 0.051 (7) | 0.049 (6) | 0.057 (8) | −0.009 (5) | 0.007 (6) | −0.004 (6) |
C41 | 0.061 (7) | 0.039 (6) | 0.049 (7) | −0.016 (5) | 0.005 (6) | 0.016 (5) |
C42 | 0.040 (6) | 0.062 (7) | 0.078 (9) | −0.013 (5) | 0.018 (6) | 0.023 (7) |
C43 | 0.055 (7) | 0.062 (7) | 0.057 (8) | 0.001 (6) | 0.026 (6) | 0.002 (6) |
C44 | 0.053 (7) | 0.042 (6) | 0.054 (7) | −0.006 (5) | 0.006 (5) | −0.002 (5) |
C45 | 0.038 (5) | 0.030 (5) | 0.048 (6) | −0.010 (4) | 0.018 (4) | −0.006 (4) |
C46 | 0.053 (7) | 0.048 (6) | 0.072 (9) | −0.020 (5) | 0.008 (6) | 0.020 (6) |
C47 | 0.034 (5) | 0.047 (6) | 0.053 (7) | 0.016 (5) | 0.008 (4) | 0.016 (6) |
C48 | 0.066 (8) | 0.037 (6) | 0.074 (9) | −0.011 (5) | 0.031 (7) | 0.003 (6) |
C49 | 0.059 (8) | 0.048 (6) | 0.069 (9) | 0.011 (5) | 0.027 (7) | 0.025 (6) |
C50 | 0.043 (6) | 0.052 (7) | 0.059 (8) | −0.005 (5) | −0.001 (5) | 0.002 (6) |
C51 | 0.056 (7) | 0.074 (9) | 0.045 (7) | −0.016 (6) | 0.010 (6) | −0.003 (6) |
C52 | 0.051 (6) | 0.039 (6) | 0.049 (7) | 0.001 (4) | 0.019 (5) | 0.014 (5) |
C53 | 0.033 (10) | 0.067 (14) | 0.044 (12) | −0.009 (9) | 0.007 (9) | −0.022 (11) |
C54 | 0.060 (14) | 0.044 (11) | 0.023 (10) | 0.030 (10) | 0.018 (9) | 0.013 (8) |
C55 | 0.026 (10) | 0.053 (13) | 0.082 (19) | 0.015 (9) | 0.011 (11) | −0.023 (13) |
C56 | 0.037 (11) | 0.060 (13) | 0.049 (13) | 0.027 (10) | 0.011 (9) | 0.001 (11) |
Lu1 | 0.0338 (2) | 0.0395 (2) | 0.0515 (3) | −0.00315 (19) | 0.01054 (18) | −0.0019 (2) |
Lu2 | 0.0344 (2) | 0.02812 (18) | 0.0447 (2) | −0.00110 (17) | 0.01064 (16) | 0.0027 (2) |
N1 | 0.035 (5) | 0.045 (5) | 0.056 (6) | 0.005 (4) | 0.004 (4) | −0.001 (4) |
N2 | 0.042 (5) | 0.035 (4) | 0.062 (6) | −0.010 (4) | 0.016 (4) | −0.006 (4) |
N3 | 0.045 (5) | 0.050 (5) | 0.038 (5) | −0.015 (4) | 0.008 (4) | 0.009 (4) |
N4 | 0.062 (6) | 0.070 (7) | 0.039 (6) | 0.004 (5) | 0.009 (5) | 0.000 (5) |
N5 | 0.062 (6) | 0.042 (5) | 0.058 (6) | 0.004 (4) | 0.007 (5) | 0.000 (5) |
N6 | 0.033 (5) | 0.044 (5) | 0.079 (7) | −0.005 (4) | 0.011 (5) | −0.002 (5) |
N7 | 0.071 (7) | 0.040 (5) | 0.051 (7) | 0.001 (5) | −0.001 (6) | 0.006 (5) |
N8 | 0.041 (5) | 0.069 (6) | 0.059 (7) | −0.018 (5) | 0.005 (5) | −0.021 (6) |
N9 | 0.046 (5) | 0.025 (4) | 0.080 (8) | −0.008 (4) | 0.008 (5) | −0.013 (5) |
N10 | 0.033 (4) | 0.042 (5) | 0.069 (7) | 0.005 (4) | 0.008 (4) | 0.015 (5) |
N11 | 0.030 (4) | 0.047 (5) | 0.043 (5) | 0.006 (4) | −0.001 (4) | 0.009 (4) |
N12 | 0.042 (5) | 0.035 (5) | 0.073 (7) | 0.003 (4) | 0.010 (5) | 0.002 (5) |
N13 | 0.040 (5) | 0.036 (4) | 0.045 (5) | −0.003 (3) | 0.002 (4) | 0.001 (4) |
N14 | 0.039 (5) | 0.031 (4) | 0.054 (6) | 0.009 (3) | 0.008 (4) | −0.002 (4) |
N15 | 0.034 (5) | 0.069 (7) | 0.045 (6) | −0.005 (4) | 0.014 (4) | 0.000 (5) |
N16 | 0.070 (7) | 0.042 (5) | 0.063 (8) | −0.024 (5) | 0.021 (6) | 0.005 (5) |
N17 | 0.058 (6) | 0.062 (6) | 0.055 (6) | 0.010 (5) | 0.026 (5) | 0.007 (5) |
N18 | 0.062 (7) | 0.062 (6) | 0.056 (7) | −0.011 (5) | 0.022 (5) | −0.012 (6) |
O1 | 0.033 (3) | 0.041 (4) | 0.052 (5) | −0.003 (3) | 0.011 (3) | 0.002 (3) |
O2 | 0.053 (4) | 0.035 (4) | 0.041 (4) | 0.012 (3) | 0.011 (3) | 0.005 (3) |
O3 | 0.055 (5) | 0.054 (5) | 0.059 (6) | −0.007 (4) | 0.007 (4) | −0.001 (4) |
O4 | 0.062 (5) | 0.058 (5) | 0.054 (5) | −0.007 (4) | 0.001 (4) | 0.002 (4) |
O5 | 0.056 (5) | 0.066 (5) | 0.072 (7) | 0.005 (4) | −0.020 (5) | 0.012 (5) |
O6 | 0.059 (5) | 0.066 (5) | 0.051 (5) | −0.005 (4) | 0.010 (4) | 0.000 (4) |
O7 | 0.035 (4) | 0.055 (5) | 0.064 (5) | −0.018 (3) | 0.011 (4) | −0.018 (4) |
O8 | 0.068 (6) | 0.063 (5) | 0.057 (6) | −0.009 (4) | −0.007 (4) | −0.031 (5) |
O9 | 0.046 (4) | 0.033 (3) | 0.053 (5) | 0.003 (3) | 0.017 (4) | 0.001 (3) |
O10 | 0.044 (4) | 0.035 (3) | 0.041 (4) | −0.012 (3) | −0.001 (3) | 0.004 (3) |
O11 | 0.052 (5) | 0.035 (4) | 0.068 (6) | 0.011 (3) | 0.021 (4) | 0.008 (4) |
O12 | 0.060 (5) | 0.051 (5) | 0.056 (5) | −0.002 (4) | 0.022 (4) | 0.004 (4) |
O13 | 0.066 (5) | 0.062 (5) | 0.054 (5) | −0.014 (4) | 0.044 (4) | −0.011 (4) |
O14 | 0.048 (5) | 0.056 (5) | 0.053 (5) | −0.023 (4) | 0.012 (4) | −0.014 (4) |
O15 | 0.058 (5) | 0.052 (5) | 0.052 (5) | 0.002 (4) | 0.014 (4) | −0.003 (4) |
O16 | 0.054 (5) | 0.056 (5) | 0.057 (6) | −0.012 (4) | 0.013 (4) | −0.012 (4) |
O17 | 0.054 (5) | 0.049 (4) | 0.057 (5) | −0.010 (4) | 0.018 (4) | 0.017 (4) |
O18 | 0.049 (5) | 0.053 (5) | 0.067 (6) | 0.015 (4) | 0.027 (4) | 0.027 (4) |
O19 | 0.046 (4) | 0.063 (5) | 0.055 (5) | 0.013 (4) | 0.012 (4) | 0.022 (4) |
O20 | 0.058 (5) | 0.065 (5) | 0.059 (6) | −0.025 (4) | 0.015 (4) | −0.023 (4) |
O21 | 0.049 (5) | 0.058 (5) | 0.070 (6) | −0.004 (4) | 0.015 (4) | −0.009 (5) |
O22 | 0.049 (5) | 0.054 (4) | 0.064 (6) | −0.015 (4) | 0.014 (4) | −0.016 (4) |
O23 | 0.035 (7) | 0.036 (7) | 0.041 (8) | 0.011 (5) | −0.006 (6) | 0.001 (6) |
O24 | 0.031 (8) | 0.081 (13) | 0.082 (14) | −0.011 (8) | 0.011 (8) | 0.008 (10) |
O25 | 0.068 (10) | 0.061 (9) | 0.075 (11) | −0.009 (7) | 0.028 (8) | 0.020 (8) |
O26 | 0.034 (9) | 0.072 (13) | 0.061 (13) | −0.028 (9) | 0.009 (9) | −0.027 (11) |
C1—O1 | 1.286 (12) | C39—C40 | 1.394 (17) |
C1—C6 | 1.434 (14) | C39—H39 | 0.9300 |
C1—C2 | 1.436 (14) | C40—C41 | 1.414 (17) |
C2—C3 | 1.416 (14) | C40—C45 | 1.439 (14) |
C2—C26 | 1.449 (14) | C41—C42 | 1.404 (18) |
C3—C4 | 1.365 (15) | C41—H41 | 0.9300 |
C3—H3 | 0.9300 | C42—C43 | 1.376 (18) |
C4—C5 | 1.328 (18) | C42—C46 | 1.488 (15) |
C4—C7 | 1.479 (15) | C43—C44 | 1.434 (17) |
C5—C6 | 1.405 (16) | C43—H43 | 0.9300 |
C5—H5 | 0.9300 | C44—C47 | 1.393 (15) |
C6—C8 | 1.460 (17) | C44—C45 | 1.432 (16) |
C7—H7A | 0.9600 | C45—O9 | 1.287 (12) |
C7—H7B | 0.9600 | C46—H46A | 0.9600 |
C7—H7C | 0.9600 | C46—H46B | 0.9600 |
C8—N1 | 1.279 (15) | C46—H46C | 0.9600 |
C8—H8 | 0.9300 | C47—N14 | 1.287 (14) |
C9—N1 | 1.456 (15) | C47—H47 | 0.9300 |
C9—C10 | 1.489 (18) | C48—N14 | 1.483 (13) |
C9—H9A | 0.9700 | C48—C49 | 1.489 (18) |
C9—H9B | 0.9700 | C48—H48A | 0.9700 |
C10—N2 | 1.462 (13) | C48—H48B | 0.9700 |
C10—H10A | 0.9700 | C49—N13 | 1.464 (15) |
C10—H10B | 0.9700 | C49—H49A | 0.9700 |
C11—N2 | 1.479 (15) | C49—H49B | 0.9700 |
C11—C12 | 1.504 (17) | C50—N13 | 1.461 (15) |
C11—H11A | 0.9700 | C50—C51 | 1.550 (19) |
C11—H11B | 0.9700 | C50—H50A | 0.9700 |
C12—N3 | 1.486 (15) | C50—H50B | 0.9700 |
C12—H12A | 0.9700 | C51—N12 | 1.486 (15) |
C12—H12B | 0.9700 | C51—H51A | 0.9700 |
C13—N3 | 1.252 (15) | C51—H51B | 0.9700 |
C13—C14 | 1.452 (14) | C52—N13 | 1.472 (13) |
C13—H13 | 0.9300 | C52—N12 | 1.474 (15) |
C14—C15 | 1.3900 | C52—H52 | 0.9800 |
C14—C19 | 1.3900 | C53—C54 | 1.44 (3) |
C15—C16 | 1.3900 | C53—H53A | 0.9600 |
C15—H15 | 0.9300 | C53—H53B | 0.9600 |
C16—C17 | 1.3900 | C53—H53C | 0.9600 |
C16—C20 | 1.541 (11) | C54—O23 | 1.47 (2) |
C17—C18 | 1.3900 | C54—H54A | 0.9700 |
C17—H17 | 0.9300 | C54—H54B | 0.9700 |
C18—C19 | 1.3900 | C55—O24 | 1.19 (3) |
C18—C21 | 1.526 (17) | C55—O23 | 1.34 (3) |
C19—O2 | 1.353 (8) | C55—C56 | 1.43 (3) |
C20—H20A | 0.9600 | C56—H56A | 0.9600 |
C20—H20B | 0.9600 | C56—H56B | 0.9600 |
C20—H20C | 0.9600 | C56—H56C | 0.9600 |
C21—N5 | 1.452 (17) | Lu1—O2 | 2.163 (7) |
C21—N4 | 1.478 (16) | Lu1—O1 | 2.178 (7) |
C21—H21 | 0.9800 | Lu1—O7 | 2.366 (8) |
C22—C23 | 1.512 (18) | Lu1—O4 | 2.368 (8) |
C22—N4 | 1.522 (15) | Lu1—N2 | 2.465 (9) |
C22—H22A | 0.9700 | Lu1—N3 | 2.466 (9) |
C22—H22B | 0.9700 | Lu1—N1 | 2.469 (9) |
C23—N5 | 1.446 (16) | Lu1—O3 | 2.582 (9) |
C23—H23A | 0.9700 | Lu1—O6 | 2.605 (8) |
C23—H23B | 0.9700 | Lu1—N7 | 2.892 (11) |
C24—N5 | 1.462 (14) | Lu2—O9 | 2.163 (7) |
C24—C25 | 1.519 (16) | Lu2—O10 | 2.218 (7) |
C24—H24A | 0.9700 | Lu2—O11 | 2.366 (9) |
C24—H24B | 0.9700 | Lu2—N11 | 2.446 (8) |
C25—N6 | 1.482 (13) | Lu2—O15 | 2.447 (9) |
C25—H25A | 0.9700 | Lu2—N9 | 2.457 (8) |
C25—H25B | 0.9700 | Lu2—N10 | 2.471 (8) |
C26—N6 | 1.299 (13) | Lu2—O14 | 2.539 (9) |
C26—H26 | 0.9300 | Lu2—O12 | 2.542 (9) |
C27—O10 | 1.310 (13) | Lu2—N15 | 2.852 (10) |
C27—C28 | 1.399 (15) | Lu2—N16 | 2.912 (12) |
C27—C32 | 1.436 (16) | N2—H2 | 0.9100 |
C28—C29 | 1.389 (14) | N4—H4A | 0.9000 |
C28—C52 | 1.482 (15) | N4—H4B | 0.9000 |
C29—C30 | 1.408 (16) | N6—H6A | 0.8600 |
C29—H29 | 0.9300 | N7—O5 | 1.258 (14) |
C30—C31 | 1.378 (15) | N7—O4 | 1.263 (14) |
C30—C33 | 1.500 (13) | N7—O3 | 1.277 (13) |
C31—C32 | 1.425 (15) | N8—O8 | 1.191 (12) |
C31—H31 | 0.9300 | N8—O6 | 1.257 (13) |
C32—C34 | 1.453 (15) | N8—O7 | 1.298 (12) |
C33—H33A | 0.9600 | N10—H10 | 0.9100 |
C33—H33B | 0.9600 | N12—H12C | 0.9000 |
C33—H33C | 0.9600 | N12—H12D | 0.9000 |
C34—N11 | 1.260 (14) | N14—H14A | 0.8600 |
C34—H34 | 0.9300 | N15—O13 | 1.209 (12) |
C35—C36 | 1.472 (16) | N15—O12 | 1.239 (12) |
C35—N11 | 1.483 (12) | N15—O11 | 1.271 (12) |
C35—H35A | 0.9700 | N16—O16 | 1.234 (14) |
C35—H35B | 0.9700 | N16—O15 | 1.265 (14) |
C36—N10 | 1.462 (14) | N16—O14 | 1.271 (14) |
C36—H36A | 0.9700 | N17—O19 | 1.224 (12) |
C36—H36B | 0.9700 | N17—O17 | 1.241 (12) |
C37—C38 | 1.476 (16) | N17—O18 | 1.275 (12) |
C37—N10 | 1.508 (14) | N18—O20 | 1.194 (12) |
C37—H37A | 0.9700 | N18—O21 | 1.211 (13) |
C37—H37B | 0.9700 | N18—O22 | 1.234 (13) |
C38—N9 | 1.489 (15) | O25—H25F | 0.8499 |
C38—H38A | 0.9700 | O25—H25C | 0.8500 |
C38—H38B | 0.9700 | O26—H26A | 0.8499 |
C39—N9 | 1.309 (15) | O26—H26B | 0.8500 |
O1—C1—C6 | 123.7 (10) | N13—C52—C28 | 120.6 (9) |
O1—C1—C2 | 121.7 (9) | N12—C52—C28 | 110.9 (9) |
C6—C1—C2 | 114.6 (9) | N13—C52—H52 | 109.1 |
C3—C2—C1 | 121.6 (10) | N12—C52—H52 | 109.1 |
C3—C2—C26 | 117.9 (9) | C28—C52—H52 | 109.1 |
C1—C2—C26 | 120.3 (9) | C54—C53—H53A | 109.5 |
C4—C3—C2 | 121.3 (10) | C54—C53—H53B | 109.5 |
C4—C3—H3 | 119.4 | H53A—C53—H53B | 109.5 |
C2—C3—H3 | 119.4 | C54—C53—H53C | 109.5 |
C5—C4—C3 | 118.0 (10) | H53A—C53—H53C | 109.5 |
C5—C4—C7 | 123.1 (11) | H53B—C53—H53C | 109.5 |
C3—C4—C7 | 118.9 (11) | C53—C54—O23 | 108.4 (16) |
C4—C5—C6 | 125.2 (11) | C53—C54—H54A | 110.0 |
C4—C5—H5 | 117.4 | O23—C54—H54A | 110.0 |
C6—C5—H5 | 117.4 | C53—C54—H54B | 110.0 |
C5—C6—C1 | 119.4 (10) | O23—C54—H54B | 110.0 |
C5—C6—C8 | 119.6 (10) | H54A—C54—H54B | 108.4 |
C1—C6—C8 | 120.5 (10) | O24—C55—O23 | 120.7 (18) |
C4—C7—H7A | 109.5 | O24—C55—C56 | 130 (2) |
C4—C7—H7B | 109.5 | O23—C55—C56 | 110 (2) |
H7A—C7—H7B | 109.5 | C55—C56—H56A | 109.5 |
C4—C7—H7C | 109.5 | C55—C56—H56B | 109.5 |
H7A—C7—H7C | 109.5 | H56A—C56—H56B | 109.5 |
H7B—C7—H7C | 109.5 | C55—C56—H56C | 109.5 |
N1—C8—C6 | 129.8 (10) | H56A—C56—H56C | 109.5 |
N1—C8—H8 | 115.1 | H56B—C56—H56C | 109.5 |
C6—C8—H8 | 115.1 | O2—Lu1—O1 | 90.0 (3) |
N1—C9—C10 | 108.9 (10) | O2—Lu1—O7 | 128.8 (3) |
N1—C9—H9A | 109.9 | O1—Lu1—O7 | 78.1 (3) |
C10—C9—H9A | 109.9 | O2—Lu1—O4 | 84.2 (3) |
N1—C9—H9B | 109.9 | O1—Lu1—O4 | 124.0 (3) |
C10—C9—H9B | 109.9 | O7—Lu1—O4 | 142.9 (3) |
H9A—C9—H9B | 108.3 | O2—Lu1—N2 | 133.9 (3) |
N2—C10—C9 | 107.8 (10) | O1—Lu1—N2 | 136.2 (3) |
N2—C10—H10A | 110.1 | O7—Lu1—N2 | 73.0 (3) |
C9—C10—H10A | 110.1 | O4—Lu1—N2 | 71.0 (3) |
N2—C10—H10B | 110.1 | O2—Lu1—N3 | 74.7 (3) |
C9—C10—H10B | 110.1 | O1—Lu1—N3 | 142.6 (3) |
H10A—C10—H10B | 108.5 | O7—Lu1—N3 | 85.3 (3) |
N2—C11—C12 | 108.1 (9) | O4—Lu1—N3 | 88.7 (3) |
N2—C11—H11A | 110.1 | N2—Lu1—N3 | 66.7 (3) |
C12—C11—H11A | 110.1 | O2—Lu1—N1 | 144.6 (3) |
N2—C11—H11B | 110.1 | O1—Lu1—N1 | 75.1 (3) |
C12—C11—H11B | 110.1 | O7—Lu1—N1 | 80.0 (3) |
H11A—C11—H11B | 108.4 | O4—Lu1—N1 | 78.5 (3) |
N3—C12—C11 | 110.3 (9) | N2—Lu1—N1 | 68.0 (3) |
N3—C12—H12A | 109.6 | N3—Lu1—N1 | 134.7 (3) |
C11—C12—H12A | 109.6 | O2—Lu1—O3 | 71.8 (3) |
N3—C12—H12B | 109.6 | O1—Lu1—O3 | 73.8 (3) |
C11—C12—H12B | 109.6 | O7—Lu1—O3 | 145.2 (3) |
H12A—C12—H12B | 108.1 | O4—Lu1—O3 | 51.5 (3) |
N3—C13—C14 | 129.0 (10) | N2—Lu1—O3 | 115.2 (3) |
N3—C13—H13 | 115.5 | N3—Lu1—O3 | 129.5 (3) |
C14—C13—H13 | 115.5 | N1—Lu1—O3 | 73.2 (3) |
C15—C14—C19 | 120.0 | O2—Lu1—O6 | 78.1 (3) |
C15—C14—C13 | 116.9 (6) | O1—Lu1—O6 | 70.2 (3) |
C19—C14—C13 | 123.1 (6) | O7—Lu1—O6 | 50.9 (3) |
C14—C15—C16 | 120.0 | O4—Lu1—O6 | 157.5 (3) |
C14—C15—H15 | 120.0 | N2—Lu1—O6 | 112.3 (3) |
C16—C15—H15 | 120.0 | N3—Lu1—O6 | 73.4 (3) |
C17—C16—C15 | 120.0 | N1—Lu1—O6 | 123.8 (3) |
C17—C16—C20 | 118.2 (8) | O3—Lu1—O6 | 132.4 (3) |
C15—C16—C20 | 121.7 (8) | O2—Lu1—N7 | 78.1 (3) |
C18—C17—C16 | 120.0 | O1—Lu1—N7 | 99.1 (3) |
C18—C17—H17 | 120.0 | O7—Lu1—N7 | 152.6 (3) |
C16—C17—H17 | 120.0 | O4—Lu1—N7 | 25.4 (3) |
C19—C18—C17 | 120.0 | N2—Lu1—N7 | 92.2 (3) |
C19—C18—C21 | 122.7 (7) | N3—Lu1—N7 | 110.4 (3) |
C17—C18—C21 | 117.2 (7) | N1—Lu1—N7 | 73.0 (3) |
O2—C19—C18 | 117.8 (6) | O3—Lu1—N7 | 26.2 (3) |
O2—C19—C14 | 122.1 (6) | O6—Lu1—N7 | 153.8 (3) |
C18—C19—C14 | 120.0 | O9—Lu2—O10 | 86.1 (3) |
C16—C20—H20A | 109.5 | O9—Lu2—O11 | 82.6 (3) |
C16—C20—H20B | 109.5 | O10—Lu2—O11 | 127.1 (3) |
H20A—C20—H20B | 109.5 | O9—Lu2—N11 | 143.1 (3) |
C16—C20—H20C | 109.5 | O10—Lu2—N11 | 75.0 (3) |
H20A—C20—H20C | 109.5 | O11—Lu2—N11 | 84.1 (3) |
H20B—C20—H20C | 109.5 | O9—Lu2—O15 | 125.9 (3) |
N5—C21—N4 | 101.2 (10) | O10—Lu2—O15 | 81.4 (3) |
N5—C21—C18 | 114.8 (11) | O11—Lu2—O15 | 143.7 (3) |
N4—C21—C18 | 110.3 (11) | N11—Lu2—O15 | 82.7 (3) |
N5—C21—H21 | 110.1 | O9—Lu2—N9 | 73.3 (3) |
N4—C21—H21 | 110.1 | O10—Lu2—N9 | 145.6 (3) |
C18—C21—H21 | 110.1 | O11—Lu2—N9 | 78.0 (3) |
C23—C22—N4 | 104.4 (10) | N11—Lu2—N9 | 136.4 (3) |
C23—C22—H22A | 110.9 | O15—Lu2—N9 | 88.7 (3) |
N4—C22—H22A | 110.9 | O9—Lu2—N10 | 139.5 (3) |
C23—C22—H22B | 110.9 | O10—Lu2—N10 | 134.3 (3) |
N4—C22—H22B | 110.9 | O11—Lu2—N10 | 74.0 (3) |
H22A—C22—H22B | 108.9 | N11—Lu2—N10 | 67.1 (3) |
N5—C23—C22 | 101.8 (10) | O15—Lu2—N10 | 69.7 (3) |
N5—C23—H23A | 111.4 | N9—Lu2—N10 | 69.9 (3) |
C22—C23—H23A | 111.4 | O9—Lu2—O14 | 74.8 (3) |
N5—C23—H23B | 111.4 | O10—Lu2—O14 | 71.9 (3) |
C22—C23—H23B | 111.4 | O11—Lu2—O14 | 149.6 (3) |
H23A—C23—H23B | 109.3 | N11—Lu2—O14 | 126.0 (3) |
N5—C24—C25 | 110.0 (10) | O15—Lu2—O14 | 51.3 (3) |
N5—C24—H24A | 109.7 | N9—Lu2—O14 | 76.2 (3) |
C25—C24—H24A | 109.7 | N10—Lu2—O14 | 111.2 (3) |
N5—C24—H24B | 109.7 | O9—Lu2—O12 | 72.6 (3) |
C25—C24—H24B | 109.7 | O10—Lu2—O12 | 75.4 (3) |
H24A—C24—H24B | 108.2 | O11—Lu2—O12 | 51.9 (3) |
N6—C25—C24 | 109.2 (9) | N11—Lu2—O12 | 72.2 (3) |
N6—C25—H25A | 109.8 | O15—Lu2—O12 | 149.3 (3) |
C24—C25—H25A | 109.8 | N9—Lu2—O12 | 121.7 (3) |
N6—C25—H25B | 109.8 | N10—Lu2—O12 | 114.0 (3) |
C24—C25—H25B | 109.8 | O14—Lu2—O12 | 134.8 (3) |
H25A—C25—H25B | 108.3 | O9—Lu2—N15 | 75.6 (3) |
N6—C26—C2 | 123.6 (9) | O10—Lu2—N15 | 101.1 (3) |
N6—C26—H26 | 118.2 | O11—Lu2—N15 | 26.1 (3) |
C2—C26—H26 | 118.2 | N11—Lu2—N15 | 77.4 (3) |
O10—C27—C28 | 120.0 (10) | O15—Lu2—N15 | 158.4 (3) |
O10—C27—C32 | 121.8 (10) | N9—Lu2—N15 | 100.0 (3) |
C28—C27—C32 | 118.2 (10) | N10—Lu2—N15 | 94.7 (3) |
C29—C28—C27 | 120.2 (10) | O14—Lu2—N15 | 150.0 (3) |
C29—C28—C52 | 118.9 (10) | O12—Lu2—N15 | 25.7 (3) |
C27—C28—C52 | 120.6 (9) | O9—Lu2—N16 | 100.5 (3) |
C28—C29—C30 | 123.7 (9) | O10—Lu2—N16 | 75.1 (3) |
C28—C29—H29 | 118.2 | O11—Lu2—N16 | 157.7 (3) |
C30—C29—H29 | 118.2 | N11—Lu2—N16 | 104.6 (3) |
C31—C30—C29 | 115.5 (9) | O15—Lu2—N16 | 25.5 (3) |
C31—C30—C33 | 121.8 (11) | N9—Lu2—N16 | 81.8 (3) |
C29—C30—C33 | 122.3 (10) | N10—Lu2—N16 | 90.4 (4) |
C30—C31—C32 | 123.6 (10) | O14—Lu2—N16 | 25.8 (3) |
C30—C31—H31 | 118.2 | O12—Lu2—N16 | 150.2 (3) |
C32—C31—H31 | 118.2 | N15—Lu2—N16 | 175.0 (3) |
C31—C32—C27 | 118.5 (10) | C8—N1—C9 | 118.1 (9) |
C31—C32—C34 | 117.8 (9) | C8—N1—Lu1 | 127.4 (7) |
C27—C32—C34 | 123.6 (9) | C9—N1—Lu1 | 114.2 (7) |
C30—C33—H33A | 109.5 | C10—N2—C11 | 110.5 (9) |
C30—C33—H33B | 109.5 | C10—N2—Lu1 | 113.8 (7) |
H33A—C33—H33B | 109.5 | C11—N2—Lu1 | 111.7 (7) |
C30—C33—H33C | 109.5 | C10—N2—H2 | 106.8 |
H33A—C33—H33C | 109.5 | C11—N2—H2 | 106.8 |
H33B—C33—H33C | 109.5 | Lu1—N2—H2 | 106.8 |
N11—C34—C32 | 126.3 (9) | C13—N3—C12 | 114.3 (10) |
N11—C34—H34 | 116.8 | C13—N3—Lu1 | 127.1 (8) |
C32—C34—H34 | 116.8 | C12—N3—Lu1 | 118.5 (7) |
C36—C35—N11 | 110.8 (9) | C21—N4—C22 | 103.4 (11) |
C36—C35—H35A | 109.5 | C21—N4—H4A | 111.1 |
N11—C35—H35A | 109.5 | C22—N4—H4A | 111.1 |
C36—C35—H35B | 109.5 | C21—N4—H4B | 111.1 |
N11—C35—H35B | 109.5 | C22—N4—H4B | 111.1 |
H35A—C35—H35B | 108.1 | H4A—N4—H4B | 109.0 |
N10—C36—C35 | 107.2 (10) | C23—N5—C21 | 101.9 (10) |
N10—C36—H36A | 110.3 | C23—N5—C24 | 121.6 (11) |
C35—C36—H36A | 110.3 | C21—N5—C24 | 113.9 (9) |
N10—C36—H36B | 110.3 | C26—N6—C25 | 121.0 (9) |
C35—C36—H36B | 110.3 | C26—N6—H6A | 119.5 |
H36A—C36—H36B | 108.5 | C25—N6—H6A | 119.5 |
C38—C37—N10 | 111.6 (9) | O5—N7—O4 | 123.6 (11) |
C38—C37—H37A | 109.3 | O5—N7—O3 | 119.9 (12) |
N10—C37—H37A | 109.3 | O4—N7—O3 | 116.4 (10) |
C38—C37—H37B | 109.3 | O5—N7—Lu1 | 175.4 (10) |
N10—C37—H37B | 109.3 | O4—N7—Lu1 | 53.4 (5) |
H37A—C37—H37B | 108.0 | O3—N7—Lu1 | 63.2 (6) |
C37—C38—N9 | 106.4 (10) | O8—N8—O6 | 124.0 (11) |
C37—C38—H38A | 110.5 | O8—N8—O7 | 121.6 (11) |
N9—C38—H38A | 110.5 | O6—N8—O7 | 114.3 (9) |
C37—C38—H38B | 110.5 | C39—N9—C38 | 115.4 (9) |
N9—C38—H38B | 110.5 | C39—N9—Lu2 | 130.5 (7) |
H38A—C38—H38B | 108.6 | C38—N9—Lu2 | 113.8 (7) |
N9—C39—C40 | 125.8 (10) | C36—N10—C37 | 115.6 (9) |
N9—C39—H39 | 117.1 | C36—N10—Lu2 | 112.6 (7) |
C40—C39—H39 | 117.1 | C37—N10—Lu2 | 110.8 (6) |
C39—C40—C41 | 117.2 (11) | C36—N10—H10 | 105.7 |
C39—C40—C45 | 123.4 (11) | C37—N10—H10 | 105.7 |
C41—C40—C45 | 119.4 (11) | Lu2—N10—H10 | 105.7 |
C42—C41—C40 | 123.1 (11) | C34—N11—C35 | 116.4 (9) |
C42—C41—H41 | 118.5 | C34—N11—Lu2 | 126.4 (7) |
C40—C41—H41 | 118.5 | C35—N11—Lu2 | 117.1 (6) |
C43—C42—C41 | 117.0 (10) | C52—N12—C51 | 110.1 (9) |
C43—C42—C46 | 119.4 (12) | C52—N12—H12C | 109.6 |
C41—C42—C46 | 123.6 (11) | C51—N12—H12C | 109.6 |
C42—C43—C44 | 123.2 (11) | C52—N12—H12D | 109.6 |
C42—C43—H43 | 118.4 | C51—N12—H12D | 109.6 |
C44—C43—H43 | 118.4 | H12C—N12—H12D | 108.2 |
C47—C44—C45 | 121.6 (10) | C50—N13—C49 | 112.9 (9) |
C47—C44—C43 | 119.1 (11) | C50—N13—C52 | 103.7 (9) |
C45—C44—C43 | 119.2 (10) | C49—N13—C52 | 115.1 (9) |
O9—C45—C44 | 119.8 (9) | C47—N14—C48 | 126.7 (9) |
O9—C45—C40 | 122.5 (9) | C47—N14—H14A | 116.6 |
C44—C45—C40 | 117.6 (9) | C48—N14—H14A | 116.6 |
C42—C46—H46A | 109.5 | O13—N15—O12 | 121.7 (11) |
C42—C46—H46B | 109.5 | O13—N15—O11 | 120.2 (10) |
H46A—C46—H46B | 109.5 | O12—N15—O11 | 118.1 (10) |
C42—C46—H46C | 109.5 | O13—N15—Lu2 | 175.0 (8) |
H46A—C46—H46C | 109.5 | O12—N15—Lu2 | 63.0 (6) |
H46B—C46—H46C | 109.5 | O11—N15—Lu2 | 55.1 (5) |
N14—C47—C44 | 122.6 (10) | O16—N16—O15 | 120.9 (12) |
N14—C47—H47 | 118.7 | O16—N16—O14 | 122.3 (11) |
C44—C47—H47 | 118.7 | O15—N16—O14 | 116.8 (11) |
N14—C48—C49 | 109.9 (11) | O16—N16—Lu2 | 177.0 (9) |
N14—C48—H48A | 109.7 | O15—N16—Lu2 | 56.3 (6) |
C49—C48—H48A | 109.7 | O14—N16—Lu2 | 60.5 (6) |
N14—C48—H48B | 109.7 | O19—N17—O17 | 122.7 (10) |
C49—C48—H48B | 109.7 | O19—N17—O18 | 116.9 (10) |
H48A—C48—H48B | 108.2 | O17—N17—O18 | 120.4 (10) |
N13—C49—C48 | 111.8 (10) | O20—N18—O21 | 123.6 (11) |
N13—C49—H49A | 109.3 | O20—N18—O22 | 115.3 (10) |
C48—C49—H49A | 109.3 | O21—N18—O22 | 121.2 (10) |
N13—C49—H49B | 109.3 | C1—O1—Lu1 | 142.3 (7) |
C48—C49—H49B | 109.3 | C19—O2—Lu1 | 137.4 (6) |
H49A—C49—H49B | 107.9 | N7—O3—Lu1 | 90.6 (7) |
N13—C50—C51 | 101.5 (9) | N7—O4—Lu1 | 101.2 (7) |
N13—C50—H50A | 111.5 | N8—O6—Lu1 | 92.2 (6) |
C51—C50—H50A | 111.5 | N8—O7—Lu1 | 102.5 (7) |
N13—C50—H50B | 111.5 | C45—O9—Lu2 | 141.6 (6) |
C51—C50—H50B | 111.5 | C27—O10—Lu2 | 130.8 (7) |
H50A—C50—H50B | 109.3 | N15—O11—Lu2 | 98.8 (6) |
N12—C51—C50 | 101.3 (10) | N15—O12—Lu2 | 91.2 (6) |
N12—C51—H51A | 111.5 | N16—O14—Lu2 | 93.7 (7) |
C50—C51—H51A | 111.5 | N16—O15—Lu2 | 98.2 (8) |
N12—C51—H51B | 111.5 | C55—O23—C54 | 120.3 (16) |
C50—C51—H51B | 111.5 | H25F—O25—H25C | 109.5 |
H51A—C51—H51B | 109.3 | H26A—O26—H26B | 109.5 |
N13—C52—N12 | 97.4 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O2 | 0.90 | 2.07 | 2.765 (13) | 133 |
N4—H4B···O22 | 0.90 | 1.94 | 2.826 (13) | 166 |
N4—H4B···O20 | 0.90 | 2.45 | 3.108 (14) | 130 |
N4—H4B···N18 | 0.90 | 2.59 | 3.435 (15) | 156 |
N6—H6A···O1 | 0.86 | 1.99 | 2.635 (11) | 131 |
N6—H6A···O6 | 0.86 | 2.63 | 3.407 (14) | 151 |
N10—H10···O15 | 0.91 | 2.35 | 2.810 (13) | 111 |
N12—H12D···O10 | 0.90 | 1.90 | 2.641 (12) | 138 |
N14—H14A···O9 | 0.86 | 1.86 | 2.560 (10) | 137 |
O25—H25F···O8 | 0.85 | 2.53 | 3.007 (19) | 116 |
O25—H25C···O5i | 0.85 | 2.32 | 2.992 (19) | 137 |
N2—H2···O19i | 0.91 | 2.08 | 2.959 (11) | 163 |
N10—H10···O20ii | 0.91 | 2.24 | 3.112 (14) | 161 |
N12—H12C···O18iii | 0.90 | 1.92 | 2.810 (13) | 170 |
N12—H12C···O19iii | 0.90 | 2.53 | 3.126 (12) | 124 |
N12—H12C···N17iii | 0.90 | 2.59 | 3.413 (14) | 152 |
Symmetry codes: (i) x, −y+1, z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) x, y−1, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Lu(C26H34N6O2)(NO3)2]NO3·0.5H2O·0.25C4H8O2 |
Mr | 854.63 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 291 |
a, b, c (Å) | 24.649 (3), 14.0182 (11), 21.4453 (17) |
β (°) | 102.307 (2) |
V (Å3) | 7239.8 (11) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 2.80 |
Crystal size (mm) | 0.32 × 0.26 × 0.24 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.42, 0.51 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20514, 9791, 8284 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.104, 0.98 |
No. of reflections | 9791 |
No. of parameters | 913 |
No. of restraints | 2 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.07, −1.58 |
Absolute structure | Flack (1983), with 2678 Friedel pairs |
Absolute structure parameter | 0.016 (10) |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXTL (Bruker, 2000), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O2 | 0.90 | 2.07 | 2.765 (13) | 133.2 |
N4—H4B···O22 | 0.90 | 1.94 | 2.826 (13) | 166.3 |
N4—H4B···O20 | 0.90 | 2.45 | 3.108 (14) | 130.4 |
N4—H4B···N18 | 0.90 | 2.59 | 3.435 (15) | 156.2 |
N6—H6A···O1 | 0.86 | 1.99 | 2.635 (11) | 131.0 |
N6—H6A···O6 | 0.86 | 2.63 | 3.407 (14) | 150.7 |
N10—H10···O15 | 0.91 | 2.35 | 2.810 (13) | 111.3 |
N12—H12D···O10 | 0.90 | 1.90 | 2.641 (12) | 138.1 |
N14—H14A···O9 | 0.86 | 1.86 | 2.560 (10) | 137.0 |
O25—H25F···O8 | 0.85 | 2.53 | 3.007 (19) | 116.3 |
O25—H25C···O5i | 0.85 | 2.32 | 2.992 (19) | 136.6 |
N2—H2···O19i | 0.91 | 2.08 | 2.959 (11) | 162.6 |
N10—H10···O20ii | 0.91 | 2.24 | 3.112 (14) | 161.2 |
N12—H12C···O18iii | 0.90 | 1.92 | 2.810 (13) | 170.3 |
N12—H12C···O19iii | 0.90 | 2.53 | 3.126 (12) | 124.0 |
N12—H12C···N17iii | 0.90 | 2.59 | 3.413 (14) | 151.5 |
Symmetry codes: (i) x, −y+1, z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) x, y−1, z+1. |
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Lanthanide macrocyclic complexes are of particular interest because they have many possible applications in biological systems, material science and chemical processes (Alexander, 1995). Our research is focused on the syntheses, crystal structures and properties of lanthanide(III) complexes with macrocyclic Schiff bases (Hu et al., 2003; Hu et al., 2004). Recently, we have reported the crystal structure of a gadolinium(III) complex with the macrocyclic ligand dervided from 2,6-diformyl-4-methylphenol and 1,5-diamino-3-azapentane ([Gd(III)(C26H34N6O2)(NO3)2]+.(NO3)-.H20), in which the central ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O atoms of two bidentae nitrates (Hu et al., 2007). As a part of a continuing study, herein we report a new lutecium analogue [Lu(III)(C26H34N6O2)(NO3)2]+. (NO3)-. 0.5H20. 0.25CH3COOC2H5 (I), but which is a different solvate, belonging to a different space group (space group Cc, compared with C2/c).
In the asymmetric unit (Fig. 1), there are two molecules of the title complex (I) which exhibit a similar coordinate geometry with the previous complex (Hu et al., 2007)(Fig. 2). Lu1 is encapsulated within the macrocyclic ligand which provided five donor atoms (the two O atoms O1,O2 from the phenolates and the three N atoms N1, N2, N3 from one end of the macrocycle). The ninefold coordination is completed around Lu1 by two bidentate nitrates which locate on the opposite sides of the bisphenoidal positions. The third nitrate is ionic. At the free end of the macrocycle, a five-membered imidazole rings is formed. The coordination polyhedron can be described as a distorted tricapped trigonal prism in which N2, O3 and O6 are located at capped sites, as shown in Fig.2. When the phenol oxygen atoms coordinate to the lanthanide ion, the phenol H atoms dissociate and are transferred to the neigbouring imidazole nitrogen to give a zwitterionic structure. This proton transfer has been conformed by NMR study of the tetraiminodiphenol analogue (Spodine et al., 2000).