Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101001445/av1069sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101001445/av1069Isup2.hkl |
CCDC reference: 163898
Data collection: KappaCCD Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 1999) and PARST97 (Nardelli, 1995).
[Gd(C11H14NO2)2Cl2(C5H5N)2]2[UCl4O2]·4C5H5N | Z = 1 |
Mr = 2329.99 | F(000) = 1156 |
Triclinic, P1 | Dx = 1.591 Mg m−3 |
a = 11.1331 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.8704 (6) Å | Cell parameters from 16824 reflections |
c = 18.8044 (7) Å | θ = 2.9–25.7° |
α = 92.239 (3)° | µ = 3.29 mm−1 |
β = 101.526 (3)° | T = 100 K |
γ = 91.353 (3)° | Platelet, translucent dark orange |
V = 2431.86 (19) Å3 | 0.18 × 0.15 × 0.10 mm |
Nonius KappaCCD diffractometer | 8501 independent reflections |
Radiation source: fine-focus sealed tube | 6568 reflections with I > 2σa(I) |
Graphite monochromator | Rint = 0.043 |
Detector resolution: 18 pixels mm-1 | θmax = 25.7°, θmin = 2.9° |
φ scans | h = −13→13 |
Absorption correction: empirical (using intensity measurements) (PLATON; Spek, 2000) | k = −14→14 |
Tmin = 0.545, Tmax = 0.720 | l = −22→22 |
16824 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.047P)2] where P = (Fo2 + 2Fc2)/3 |
8501 reflections | (Δ/σ)max = 0.001 |
547 parameters | Δρmax = 0.99 e Å−3 |
26 restraints | Δρmin = −0.80 e Å−3 |
Experimental. A 180° range in φ was scanned during data collection, with 2° φ steps. The crystal-to-detector distance was fixed at 28 mm. |
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. Structure solved by direct methods and expanded by subsequent Fourier-difference synthesis. All non-hydrogen atoms have been refined anisotropically. Some soft restraints have been applied on some terminal atoms of the tert-butyl groups. The protons on the nitrogen atoms have been found on the Fourier-difference map and introduced as riding atoms with a displacement parameter equal to 1.2 times that of the parent atom. The other hydrogen atoms were introduced (except in the disordered pyridine molecules) at calculated positions as riding atoms with a displacement parameter equal to 1.2 (CH) or 1.5 (CH3) times that of the parent atom. 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 | ||
U | 0.0000 | 0.0000 | 0.0000 | 0.02852 (9) | |
Gd | 0.64463 (2) | −0.42406 (2) | 0.294286 (13) | 0.02477 (9) | |
Cl1 | 0.44680 (13) | −0.52772 (13) | 0.32478 (8) | 0.0383 (3) | |
Cl2 | 0.86340 (13) | −0.31930 (13) | 0.34473 (7) | 0.0383 (3) | |
Cl3 | −0.19766 (14) | −0.12364 (13) | −0.06825 (8) | 0.0420 (4) | |
Cl4 | −0.10272 (15) | 0.03262 (14) | 0.11438 (8) | 0.0450 (4) | |
O1 | 0.5214 (3) | −0.5089 (3) | 0.1709 (2) | 0.0337 (9) | |
O2 | 0.7400 (3) | −0.5594 (3) | 0.23641 (18) | 0.0285 (8) | |
O3 | 0.7095 (3) | −0.3256 (3) | 0.18393 (19) | 0.0301 (8) | |
O4 | 0.5239 (3) | −0.2815 (3) | 0.24422 (18) | 0.0274 (8) | |
O5 | 0.0700 (4) | −0.1233 (3) | 0.0378 (2) | 0.0385 (10) | |
N1 | 0.9479 (4) | −0.6551 (4) | 0.2344 (2) | 0.0334 (11) | |
H1 | 0.8842 | −0.6163 | 0.2531 | 0.040* | |
N2 | 0.3172 (4) | −0.1837 (4) | 0.2407 (2) | 0.0362 (11) | |
H2 | 0.3744 | −0.2290 | 0.2597 | 0.043* | |
N3 | 0.7424 (4) | −0.5574 (4) | 0.3964 (2) | 0.0321 (11) | |
N4 | 0.6031 (4) | −0.3080 (4) | 0.4071 (2) | 0.0327 (10) | |
C1 | 0.3902 (5) | −0.5035 (5) | 0.1428 (3) | 0.0351 (13) | |
H1B | 0.3696 | −0.5422 | 0.0960 | 0.053* | |
H1C | 0.3680 | −0.4261 | 0.1384 | 0.053* | |
H1D | 0.3464 | −0.5386 | 0.1756 | 0.053* | |
C2 | 0.5859 (5) | −0.5718 (4) | 0.1296 (3) | 0.0278 (11) | |
C3 | 0.7063 (5) | −0.5961 (4) | 0.1686 (3) | 0.0276 (11) | |
C4 | 0.7826 (5) | −0.6583 (4) | 0.1313 (3) | 0.0286 (12) | |
C5 | 0.7395 (5) | −0.6969 (5) | 0.0578 (3) | 0.0331 (13) | |
H5A | 0.7896 | −0.7386 | 0.0334 | 0.040* | |
C6 | 0.6232 (6) | −0.6720 (5) | 0.0232 (3) | 0.0364 (14) | |
H6A | 0.5950 | −0.6967 | −0.0249 | 0.044* | |
C7 | 0.5469 (5) | −0.6103 (5) | 0.0592 (3) | 0.0368 (14) | |
H7A | 0.4681 | −0.5950 | 0.0349 | 0.044* | |
C8 | 0.9032 (5) | −0.6855 (5) | 0.1678 (3) | 0.0292 (12) | |
H8A | 0.9515 | −0.7271 | 0.1421 | 0.035* | |
C9 | 1.0698 (6) | −0.6831 (6) | 0.2766 (3) | 0.0541 (19) | |
C10 | 1.0554 (9) | −0.8063 (8) | 0.3014 (6) | 0.112 (4) | |
H10A | 1.1324 | −0.8293 | 0.3288 | 0.168* | |
H10B | 1.0302 | −0.8564 | 0.2594 | 0.168* | |
H10C | 0.9946 | −0.8088 | 0.3311 | 0.168* | |
C11 | 1.0940 (7) | −0.6139 (8) | 0.3450 (4) | 0.080 (3) | |
H11A | 1.1057 | −0.5363 | 0.3347 | 0.120* | |
H11B | 1.1665 | −0.6390 | 0.3762 | 0.120* | |
H11C | 1.0255 | −0.6212 | 0.3686 | 0.120* | |
C12 | 1.1626 (6) | −0.6882 (8) | 0.2317 (4) | 0.070 (2) | |
H12A | 1.1775 | −0.6142 | 0.2159 | 0.105* | |
H12B | 1.1340 | −0.7384 | 0.1902 | 0.105* | |
H12C | 1.2372 | −0.7154 | 0.2596 | 0.105* | |
C13 | 0.8221 (5) | −0.3392 (5) | 0.1576 (3) | 0.0373 (14) | |
H13A | 0.8173 | −0.3004 | 0.1133 | 0.056* | |
H13B | 0.8339 | −0.4180 | 0.1487 | 0.056* | |
H13C | 0.8899 | −0.3083 | 0.1934 | 0.056* | |
C14 | 0.6321 (5) | −0.2453 (4) | 0.1506 (3) | 0.0267 (11) | |
C15 | 0.5324 (5) | −0.2277 (4) | 0.1846 (3) | 0.0264 (11) | |
C16 | 0.4432 (5) | −0.1499 (5) | 0.1542 (3) | 0.0288 (12) | |
C17 | 0.4593 (5) | −0.0916 (5) | 0.0930 (3) | 0.0352 (13) | |
H17A | 0.4005 | −0.0416 | 0.0724 | 0.042* | |
C18 | 0.5601 (6) | −0.1077 (5) | 0.0635 (3) | 0.0402 (15) | |
H18A | 0.5715 | −0.0657 | 0.0245 | 0.048* | |
C19 | 0.6472 (5) | −0.1868 (5) | 0.0913 (3) | 0.0312 (12) | |
H19A | 0.7142 | −0.1993 | 0.0698 | 0.037* | |
C20 | 0.3371 (5) | −0.1317 (5) | 0.1849 (3) | 0.0346 (13) | |
H20A | 0.2803 | −0.0805 | 0.1637 | 0.042* | |
C21 | 0.2101 (6) | −0.1777 (7) | 0.2764 (3) | 0.055 (2) | |
C22 | 0.1607 (8) | −0.3053 (8) | 0.2768 (6) | 0.089 (3) | |
H22A | 0.1316 | −0.3339 | 0.2278 | 0.133* | |
H22B | 0.0948 | −0.3079 | 0.3028 | 0.133* | |
H22C | 0.2261 | −0.3507 | 0.3002 | 0.133* | |
C23 | 0.1092 (7) | −0.1167 (10) | 0.2331 (5) | 0.095 (3) | |
H23A | 0.1344 | −0.0392 | 0.2309 | 0.143* | |
H23B | 0.0389 | −0.1205 | 0.2554 | 0.143* | |
H23C | 0.0885 | −0.1505 | 0.1849 | 0.143* | |
C24 | 0.2558 (8) | −0.1392 (9) | 0.3538 (4) | 0.083 (3) | |
H24A | 0.2850 | −0.0621 | 0.3560 | 0.125* | |
H24B | 0.3216 | −0.1856 | 0.3753 | 0.125* | |
H24C | 0.1903 | −0.1450 | 0.3799 | 0.125* | |
C25 | 0.7193 (6) | −0.6686 (5) | 0.3842 (3) | 0.0423 (15) | |
H25A | 0.6643 | −0.6936 | 0.3423 | 0.051* | |
C26 | 0.7742 (6) | −0.7481 (6) | 0.4315 (3) | 0.0481 (17) | |
H26A | 0.7580 | −0.8249 | 0.4210 | 0.058* | |
C27 | 0.8545 (7) | −0.7099 (7) | 0.4954 (4) | 0.0547 (19) | |
H27A | 0.8931 | −0.7606 | 0.5283 | 0.066* | |
C28 | 0.8744 (6) | −0.5983 (6) | 0.5081 (3) | 0.0468 (17) | |
H28A | 0.9258 | −0.5709 | 0.5508 | 0.056* | |
C29 | 0.8185 (5) | −0.5232 (6) | 0.4576 (3) | 0.0387 (14) | |
H29A | 0.8350 | −0.4463 | 0.4671 | 0.046* | |
C30 | 0.5772 (5) | −0.3516 (5) | 0.4674 (3) | 0.0381 (14) | |
H30A | 0.5745 | −0.4297 | 0.4700 | 0.046* | |
C31 | 0.5541 (6) | −0.2874 (6) | 0.5259 (3) | 0.0487 (17) | |
H31A | 0.5349 | −0.3221 | 0.5658 | 0.058* | |
C32 | 0.5599 (6) | −0.1726 (6) | 0.5244 (3) | 0.0430 (15) | |
H32A | 0.5472 | −0.1275 | 0.5636 | 0.052* | |
C33 | 0.5860 (6) | −0.1243 (5) | 0.4614 (3) | 0.0402 (14) | |
H33A | 0.5879 | −0.0465 | 0.4573 | 0.048* | |
C34 | 0.6085 (5) | −0.1958 (5) | 0.4060 (3) | 0.0381 (14) | |
H34A | 0.6287 | −0.1636 | 0.3654 | 0.046* | |
N5 | 0.5552 (6) | 0.0687 (5) | 0.3194 (3) | 0.0566 (16) | |
C35 | 0.6524 (7) | 0.0423 (6) | 0.2910 (4) | 0.0524 (18) | |
H35A | 0.7114 | −0.0026 | 0.3172 | 0.063* | |
C36 | 0.6696 (7) | 0.0781 (6) | 0.2250 (4) | 0.0540 (18) | |
H36A | 0.7394 | 0.0595 | 0.2076 | 0.065* | |
C37 | 0.5795 (8) | 0.1435 (6) | 0.1844 (4) | 0.057 (2) | |
H37A | 0.5880 | 0.1687 | 0.1394 | 0.068* | |
C38 | 0.4789 (7) | 0.1693 (6) | 0.2124 (4) | 0.0526 (18) | |
H38A | 0.4169 | 0.2117 | 0.1867 | 0.063* | |
C39 | 0.4717 (7) | 0.1313 (6) | 0.2792 (4) | 0.0577 (19) | |
H39A | 0.4034 | 0.1505 | 0.2980 | 0.069* | |
C40 | 1.0575 (8) | −0.5946 (7) | 0.0229 (5) | 0.071 (2) | |
C41 | 1.0907 (7) | −0.4973 (7) | 0.0666 (5) | 0.064 (2) | |
C42 | 1.0300 (9) | −0.4021 (7) | 0.0413 (5) | 0.075 (3) | |
C43 | 0.9182 (9) | −0.0681 (8) | 0.4554 (7) | 0.084 (3) | |
C44 | 0.9980 (10) | −0.0077 (10) | 0.4252 (5) | 0.089 (3) | |
C45 | 1.0811 (9) | 0.0601 (10) | 0.4719 (7) | 0.093 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
U | 0.02998 (16) | 0.02591 (17) | 0.03069 (16) | 0.00621 (12) | 0.00760 (13) | 0.00287 (11) |
Gd | 0.02113 (14) | 0.02938 (16) | 0.02371 (15) | 0.00394 (11) | 0.00331 (11) | 0.00454 (10) |
Cl1 | 0.0301 (7) | 0.0462 (9) | 0.0379 (8) | −0.0064 (6) | 0.0038 (6) | 0.0135 (6) |
Cl2 | 0.0290 (7) | 0.0503 (9) | 0.0341 (7) | −0.0053 (6) | 0.0037 (6) | −0.0005 (6) |
Cl3 | 0.0393 (8) | 0.0371 (8) | 0.0458 (8) | −0.0004 (6) | 0.0002 (7) | −0.0006 (6) |
Cl4 | 0.0515 (9) | 0.0432 (9) | 0.0460 (9) | 0.0058 (7) | 0.0236 (7) | 0.0008 (7) |
O1 | 0.0193 (18) | 0.044 (2) | 0.037 (2) | 0.0043 (17) | 0.0025 (17) | 0.0010 (17) |
O2 | 0.0254 (19) | 0.031 (2) | 0.0277 (19) | 0.0039 (16) | 0.0021 (16) | 0.0005 (15) |
O3 | 0.0218 (18) | 0.039 (2) | 0.033 (2) | 0.0059 (16) | 0.0120 (16) | 0.0097 (16) |
O4 | 0.0276 (19) | 0.029 (2) | 0.0282 (19) | 0.0070 (16) | 0.0085 (16) | 0.0097 (15) |
O5 | 0.039 (2) | 0.035 (2) | 0.042 (2) | 0.0061 (18) | 0.0078 (19) | 0.0086 (18) |
N1 | 0.026 (2) | 0.040 (3) | 0.033 (3) | 0.012 (2) | 0.001 (2) | 0.002 (2) |
N2 | 0.028 (2) | 0.055 (3) | 0.028 (2) | 0.014 (2) | 0.009 (2) | 0.008 (2) |
N3 | 0.033 (3) | 0.036 (3) | 0.028 (2) | 0.010 (2) | 0.005 (2) | 0.005 (2) |
N4 | 0.037 (3) | 0.029 (3) | 0.036 (3) | 0.006 (2) | 0.014 (2) | 0.0066 (19) |
C1 | 0.021 (3) | 0.049 (4) | 0.034 (3) | 0.008 (3) | 0.003 (2) | 0.006 (3) |
C2 | 0.022 (3) | 0.029 (3) | 0.033 (3) | 0.001 (2) | 0.004 (2) | 0.003 (2) |
C3 | 0.029 (3) | 0.028 (3) | 0.023 (3) | −0.001 (2) | 0.001 (2) | 0.001 (2) |
C4 | 0.027 (3) | 0.028 (3) | 0.032 (3) | 0.003 (2) | 0.009 (2) | 0.005 (2) |
C5 | 0.035 (3) | 0.033 (3) | 0.033 (3) | −0.002 (2) | 0.010 (3) | 0.000 (2) |
C6 | 0.043 (3) | 0.039 (3) | 0.026 (3) | 0.000 (3) | 0.003 (3) | 0.001 (2) |
C7 | 0.034 (3) | 0.039 (3) | 0.033 (3) | −0.003 (3) | −0.003 (3) | 0.010 (2) |
C8 | 0.030 (3) | 0.030 (3) | 0.029 (3) | 0.003 (2) | 0.010 (2) | 0.001 (2) |
C9 | 0.027 (3) | 0.088 (6) | 0.045 (4) | 0.024 (3) | 0.002 (3) | −0.005 (4) |
C10 | 0.098 (6) | 0.098 (7) | 0.123 (7) | 0.026 (5) | −0.025 (6) | 0.034 (6) |
C11 | 0.052 (4) | 0.114 (6) | 0.072 (5) | 0.018 (4) | 0.008 (4) | −0.017 (5) |
C12 | 0.029 (3) | 0.130 (8) | 0.050 (4) | 0.011 (4) | 0.006 (3) | 0.002 (4) |
C13 | 0.027 (3) | 0.041 (4) | 0.049 (4) | 0.008 (3) | 0.017 (3) | 0.014 (3) |
C14 | 0.027 (3) | 0.027 (3) | 0.026 (3) | 0.005 (2) | 0.006 (2) | 0.003 (2) |
C15 | 0.024 (3) | 0.029 (3) | 0.024 (3) | −0.003 (2) | 0.001 (2) | 0.000 (2) |
C16 | 0.030 (3) | 0.031 (3) | 0.026 (3) | 0.002 (2) | 0.004 (2) | 0.008 (2) |
C17 | 0.041 (3) | 0.035 (3) | 0.030 (3) | 0.010 (3) | 0.005 (3) | 0.010 (2) |
C18 | 0.053 (4) | 0.039 (4) | 0.034 (3) | 0.007 (3) | 0.018 (3) | 0.017 (3) |
C19 | 0.031 (3) | 0.037 (3) | 0.027 (3) | 0.004 (2) | 0.010 (2) | 0.004 (2) |
C20 | 0.034 (3) | 0.040 (3) | 0.029 (3) | 0.010 (3) | 0.004 (3) | 0.008 (2) |
C21 | 0.040 (4) | 0.096 (6) | 0.037 (4) | 0.028 (4) | 0.018 (3) | 0.022 (4) |
C22 | 0.064 (5) | 0.097 (8) | 0.112 (8) | 0.005 (5) | 0.027 (5) | 0.035 (6) |
C23 | 0.050 (5) | 0.168 (11) | 0.080 (6) | 0.042 (6) | 0.033 (5) | 0.026 (6) |
C24 | 0.072 (5) | 0.138 (7) | 0.048 (4) | 0.017 (5) | 0.029 (4) | 0.003 (4) |
C25 | 0.044 (4) | 0.044 (4) | 0.037 (3) | 0.006 (3) | 0.003 (3) | 0.008 (3) |
C26 | 0.061 (4) | 0.041 (4) | 0.043 (4) | 0.019 (3) | 0.008 (3) | 0.011 (3) |
C27 | 0.057 (4) | 0.063 (5) | 0.050 (4) | 0.028 (4) | 0.016 (4) | 0.023 (4) |
C28 | 0.041 (4) | 0.075 (5) | 0.024 (3) | 0.015 (3) | 0.003 (3) | 0.009 (3) |
C29 | 0.036 (3) | 0.048 (4) | 0.033 (3) | 0.010 (3) | 0.006 (3) | 0.004 (3) |
C30 | 0.044 (3) | 0.035 (3) | 0.040 (3) | 0.009 (3) | 0.016 (3) | 0.008 (3) |
C31 | 0.055 (4) | 0.056 (4) | 0.043 (4) | 0.017 (3) | 0.027 (3) | 0.013 (3) |
C32 | 0.053 (4) | 0.044 (4) | 0.035 (3) | 0.014 (3) | 0.015 (3) | 0.003 (3) |
C33 | 0.051 (4) | 0.032 (3) | 0.039 (3) | 0.008 (3) | 0.013 (3) | 0.000 (3) |
C34 | 0.040 (3) | 0.043 (4) | 0.035 (3) | 0.000 (3) | 0.016 (3) | 0.009 (3) |
N5 | 0.063 (4) | 0.060 (4) | 0.052 (3) | 0.008 (3) | 0.021 (3) | 0.019 (3) |
C35 | 0.048 (4) | 0.051 (4) | 0.059 (4) | 0.004 (3) | 0.010 (4) | 0.014 (3) |
C36 | 0.050 (4) | 0.052 (4) | 0.065 (5) | −0.011 (3) | 0.027 (4) | −0.010 (4) |
C37 | 0.086 (6) | 0.045 (4) | 0.041 (4) | −0.027 (4) | 0.019 (4) | 0.002 (3) |
C38 | 0.063 (5) | 0.044 (4) | 0.047 (4) | 0.002 (3) | 0.002 (4) | 0.009 (3) |
C39 | 0.065 (5) | 0.058 (5) | 0.057 (4) | 0.020 (4) | 0.025 (4) | 0.011 (3) |
C40 | 0.085 (5) | 0.057 (5) | 0.097 (5) | 0.024 (4) | 0.070 (5) | 0.030 (4) |
C41 | 0.071 (5) | 0.047 (5) | 0.087 (6) | 0.007 (4) | 0.049 (5) | 0.008 (4) |
C42 | 0.103 (7) | 0.047 (5) | 0.095 (7) | −0.006 (5) | 0.072 (6) | 0.005 (4) |
C43 | 0.078 (7) | 0.049 (5) | 0.116 (9) | 0.018 (5) | −0.001 (6) | −0.017 (5) |
C44 | 0.061 (6) | 0.107 (8) | 0.091 (7) | 0.046 (6) | −0.005 (6) | −0.010 (6) |
C45 | 0.068 (6) | 0.097 (8) | 0.111 (9) | 0.003 (6) | 0.005 (6) | 0.038 (6) |
U—O5i | 1.780 (4) | C6—C7 | 1.392 (8) |
U—O5 | 1.780 (4) | C9—C12 | 1.460 (9) |
U—Cl4i | 2.6501 (15) | C9—C11 | 1.472 (7) |
U—Cl3 | 2.6861 (15) | C9—C10 | 1.567 (8) |
U—Cl4 | 2.6501 (15) | C14—C19 | 1.373 (7) |
U—Cl3i | 2.6862 (15) | C14—C15 | 1.403 (7) |
Gd—O1 | 2.601 (4) | C15—C16 | 1.422 (7) |
Gd—O2 | 2.302 (3) | C16—C17 | 1.406 (7) |
Gd—O3 | 2.635 (3) | C16—C20 | 1.431 (8) |
Gd—O4 | 2.298 (3) | C17—C18 | 1.362 (8) |
Gd—N3 | 2.620 (4) | C18—C19 | 1.405 (8) |
Gd—N4 | 2.609 (4) | C21—C23 | 1.472 (10) |
Gd—Cl1 | 2.6695 (14) | C21—C24 | 1.493 (10) |
Gd—Cl2 | 2.6869 (14) | C21—C22 | 1.600 (12) |
O1—C2 | 1.370 (6) | C25—C26 | 1.390 (8) |
O1—C1 | 1.454 (6) | C26—C27 | 1.399 (10) |
O2—C3 | 1.309 (6) | C27—C28 | 1.342 (10) |
O2—N1 | 2.609 (5) | C28—C29 | 1.392 (8) |
O3—C14 | 1.383 (6) | C30—C31 | 1.383 (8) |
O3—C13 | 1.448 (6) | C31—C32 | 1.364 (9) |
O4—C15 | 1.330 (6) | C32—C33 | 1.414 (8) |
O4—N2 | 2.592 (6) | C33—C34 | 1.384 (8) |
N1—C8 | 1.285 (7) | N5—C39 | 1.336 (9) |
N1—C9 | 1.481 (7) | N5—C35 | 1.337 (9) |
N2—C20 | 1.292 (7) | C35—C36 | 1.376 (10) |
N2—C21 | 1.483 (7) | C36—C37 | 1.403 (10) |
N3—C29 | 1.328 (7) | C37—C38 | 1.364 (10) |
N3—C25 | 1.342 (8) | C38—C39 | 1.369 (10) |
N4—C34 | 1.333 (7) | C40—C41 | 1.388 (12) |
N4—C30 | 1.344 (7) | C40—C42ii | 1.390 (13) |
C2—C7 | 1.366 (8) | C41—C42 | 1.381 (11) |
C2—C3 | 1.435 (7) | C42—C40ii | 1.390 (13) |
C3—C4 | 1.409 (7) | C43—C44 | 1.353 (15) |
C4—C5 | 1.423 (7) | C43—C45iii | 1.365 (14) |
C4—C8 | 1.431 (7) | C44—C45 | 1.363 (14) |
C5—C6 | 1.372 (8) | C45—C43iii | 1.365 (14) |
O5i—U—O5 | 180.0 | C34—N4—C30 | 116.4 (5) |
O5i—U—Cl4i | 90.45 (13) | C34—N4—Gd | 118.1 (4) |
O5—U—Cl4i | 89.55 (13) | C30—N4—Gd | 125.6 (4) |
O5i—U—Cl4 | 89.55 (13) | C7—C2—O1 | 127.0 (5) |
O5—U—Cl4 | 90.45 (13) | C7—C2—C3 | 120.5 (5) |
Cl4i—U—Cl4 | 180.0 | O1—C2—C3 | 112.5 (4) |
O5i—U—Cl3 | 89.43 (13) | O2—C3—C4 | 123.4 (5) |
O5—U—Cl3 | 90.57 (13) | O2—C3—C2 | 118.8 (5) |
Cl4i—U—Cl3 | 89.71 (5) | C4—C3—C2 | 117.8 (4) |
Cl4—U—Cl3 | 90.29 (5) | C3—C4—C5 | 120.5 (5) |
O5i—U—Cl3i | 90.57 (13) | C3—C4—C8 | 120.0 (5) |
O5—U—Cl3i | 89.43 (13) | C5—C4—C8 | 119.5 (5) |
Cl4i—U—Cl3i | 90.29 (5) | C6—C5—C4 | 119.4 (5) |
Cl4—U—Cl3i | 89.71 (5) | C5—C6—C7 | 120.9 (5) |
Cl3—U—Cl3i | 180.0 | C2—C7—C6 | 121.0 (5) |
O4—Gd—O2 | 128.51 (12) | N1—C8—C4 | 123.2 (5) |
O4—Gd—O1 | 74.65 (12) | C12—C9—C11 | 119.7 (7) |
O2—Gd—O1 | 63.54 (12) | C12—C9—N1 | 112.2 (5) |
O4—Gd—N4 | 76.39 (13) | C11—C9—N1 | 108.5 (5) |
O2—Gd—N4 | 154.59 (13) | C12—C9—C10 | 105.3 (7) |
O1—Gd—N4 | 138.34 (13) | C11—C9—C10 | 104.0 (7) |
O4—Gd—N3 | 156.17 (13) | N1—C9—C10 | 105.9 (6) |
O2—Gd—N3 | 74.90 (13) | C19—C14—O3 | 125.9 (5) |
O1—Gd—N3 | 120.13 (13) | C19—C14—C15 | 121.8 (5) |
N4—Gd—N3 | 80.88 (14) | O3—C14—C15 | 112.3 (4) |
O4—Gd—O3 | 63.23 (11) | O4—C15—C14 | 120.2 (4) |
O2—Gd—O3 | 74.10 (12) | O4—C15—C16 | 121.6 (5) |
O1—Gd—O3 | 68.65 (12) | C14—C15—C16 | 118.1 (5) |
N4—Gd—O3 | 121.78 (13) | C17—C16—C15 | 119.4 (5) |
N3—Gd—O3 | 137.57 (12) | C17—C16—C20 | 120.0 (5) |
O4—Gd—Cl1 | 89.58 (9) | C15—C16—C20 | 120.6 (5) |
O2—Gd—Cl1 | 105.62 (10) | C18—C17—C16 | 120.6 (5) |
O1—Gd—Cl1 | 74.25 (9) | C17—C18—C19 | 120.8 (5) |
N4—Gd—Cl1 | 76.25 (11) | C14—C19—C18 | 119.2 (5) |
N3—Gd—Cl1 | 78.05 (11) | N2—C20—C16 | 122.6 (5) |
O3—Gd—Cl1 | 138.38 (8) | C23—C21—N2 | 111.7 (5) |
O4—Gd—Cl2 | 103.34 (10) | C23—C21—C24 | 118.2 (7) |
O2—Gd—Cl2 | 89.47 (9) | N2—C21—C24 | 107.8 (6) |
O1—Gd—Cl2 | 137.57 (9) | C23—C21—C22 | 106.1 (7) |
N4—Gd—Cl2 | 78.19 (11) | N2—C21—C22 | 105.4 (6) |
N3—Gd—Cl2 | 78.62 (11) | C24—C21—C22 | 106.8 (7) |
O3—Gd—Cl2 | 72.88 (8) | N3—C25—C26 | 122.8 (6) |
Cl1—Gd—Cl2 | 147.64 (4) | C25—C26—C27 | 118.3 (6) |
C2—O1—C1 | 116.2 (4) | C28—C27—C26 | 118.4 (6) |
C2—O1—Gd | 116.4 (3) | C27—C28—C29 | 120.4 (6) |
C1—O1—Gd | 127.3 (3) | N3—C29—C28 | 122.4 (6) |
C3—O2—Gd | 126.1 (3) | N4—C30—C31 | 124.0 (6) |
C3—O2—N1 | 86.3 (3) | C32—C31—C30 | 119.4 (6) |
Gd—O2—N1 | 144.69 (19) | C31—C32—C33 | 117.9 (6) |
C14—O3—C13 | 115.7 (4) | C34—C33—C32 | 118.3 (6) |
C14—O3—Gd | 116.7 (3) | N4—C34—C33 | 124.0 (5) |
C13—O3—Gd | 127.3 (3) | C39—N5—C35 | 116.2 (6) |
C15—O4—Gd | 127.0 (3) | N5—C35—C36 | 123.3 (7) |
C15—O4—N2 | 87.2 (3) | C35—C36—C37 | 118.6 (7) |
Gd—O4—N2 | 144.44 (18) | C38—C37—C36 | 118.5 (6) |
C8—N1—C9 | 126.4 (5) | C37—C38—C39 | 118.3 (7) |
C8—N1—O2 | 87.1 (3) | N5—C39—C38 | 125.0 (7) |
C9—N1—O2 | 146.4 (4) | C41—C40—C42ii | 123.4 (8) |
C20—N2—C21 | 128.8 (5) | C42—C41—C40 | 114.8 (8) |
C20—N2—O4 | 87.8 (3) | C41—C42—C40ii | 121.8 (8) |
C21—N2—O4 | 143.3 (4) | C44—C43—C45iii | 122.1 (9) |
C29—N3—C25 | 117.7 (5) | C43—C44—C45 | 116.1 (10) |
C29—N3—Gd | 124.6 (4) | C44—C45—C43iii | 121.8 (10) |
C25—N3—Gd | 117.6 (4) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+2, −y−1, −z; (iii) −x+2, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O2 | 0.97 | 1.73 | 2.609 (5) | 148 |
N2—H2···O4 | 0.87 | 1.86 | 2.592 (6) | 140 |