Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802018536/ci6163sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802018536/ci6163Isup2.hkl |
CCDC reference: 190916
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.007 Å
- H-atom completeness 79%
- R factor = 0.033
- wR factor = 0.089
- Data-to-parameter ratio = 12.2
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C27 H42 N7 O18 Tb1 Atom count from the _atom_site data: C27 H33 N7 O18 Tb1 ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.375 Tmax scaled 0.357 Tmin scaled 0.298 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C27 H42 N7 O18 Tb TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 54.00 54.00 0.00 H 84.00 66.00 18.00 N 14.00 14.00 0.00 O 36.00 36.00 0.00 Tb 2.00 2.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 911.60 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 27.00 324.30 H 1.01 33.00 33.26 N 14.01 7.00 98.05 O 16.00 18.00 287.98 Tb 158.93 1.00 158.93 Calculated formula weight 902.52 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
Data collection: XSCANS (Siemens, 1991); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1997a); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL.
[Tb(C7H3NO4)3](C6H21N4)·6H2O | Z = 2 |
Mr = 911.60 | F(000) = 924 |
Triclinic, P1 | Dx = 1.761 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.538 (2) Å | Cell parameters from 38 reflections |
b = 12.068 (3) Å | θ = 4.1–15.5° |
c = 15.747 (3) Å | µ = 2.15 mm−1 |
α = 87.31 (1)° | T = 296 K |
β = 71.24 (2)° | Triclinic, colorless |
γ = 65.66 (2)° | 0.58 × 0.58 × 0.48 mm |
V = 1719.1 (6) Å3 |
Siemens P4 diffractometer | 5440 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.070 |
Graphite monochromator | θmax = 25.0°, θmin = 1.9° |
ω scans | h = 0→12 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | k = −13→14 |
Tmin = 0.795, Tmax = 0.951 | l = −17→18 |
6350 measured reflections | 3 standard reflections every 97 reflections |
6011 independent reflections | intensity decay: 6.6% |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.089 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0686P)2] where P = (Fo2 + 2Fc2)/3 |
6011 reflections | (Δ/σ)max = 0.001 |
493 parameters | Δρmax = 2.42 e Å−3 |
5 restraints | Δρmin = −1.24 e Å−3 |
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 | ||
Tb | 0.23697 (2) | 0.252096 (16) | 0.241070 (12) | 0.02105 (9) | |
O1 | 0.3033 (3) | 0.0406 (3) | 0.19483 (19) | 0.0286 (6) | |
O2 | 0.4715 (3) | −0.1427 (3) | 0.1246 (2) | 0.0345 (7) | |
O3 | 0.3671 (3) | 0.3749 (3) | 0.1762 (2) | 0.0342 (7) | |
O4 | 0.5567 (4) | 0.4034 (3) | 0.0790 (2) | 0.0427 (8) | |
O5 | 0.4179 (3) | 0.1516 (3) | 0.3176 (2) | 0.0324 (7) | |
O6 | 0.4977 (4) | 0.1474 (4) | 0.4339 (3) | 0.0535 (10) | |
O7 | 0.0456 (3) | 0.4555 (3) | 0.2733 (2) | 0.0377 (7) | |
O8 | −0.0395 (5) | 0.6494 (3) | 0.3233 (3) | 0.0667 (12) | |
O9 | 0.1790 (3) | 0.2959 (3) | 0.10251 (19) | 0.0303 (6) | |
O10 | 0.0312 (4) | 0.3252 (4) | 0.0213 (2) | 0.0452 (9) | |
O11 | 0.1075 (3) | 0.1846 (3) | 0.37600 (18) | 0.0296 (6) | |
O12 | −0.0787 (4) | 0.1421 (3) | 0.4581 (2) | 0.0445 (8) | |
N1 | 0.4800 (4) | 0.1448 (3) | 0.1205 (2) | 0.0231 (7) | |
N2 | 0.2207 (4) | 0.3801 (3) | 0.3685 (2) | 0.0259 (7) | |
N3 | 0.0038 (4) | 0.2437 (3) | 0.2414 (2) | 0.0261 (7) | |
C1 | 0.4284 (5) | −0.0310 (4) | 0.1419 (3) | 0.0248 (8) | |
C2 | 0.5331 (4) | 0.0260 (3) | 0.0957 (2) | 0.0231 (8) | |
C3 | 0.6712 (5) | −0.0378 (4) | 0.0342 (3) | 0.0326 (10) | |
H3 | 0.7040 | −0.1203 | 0.0171 | 0.039* | |
C4 | 0.7611 (5) | 0.0218 (5) | −0.0019 (3) | 0.0363 (10) | |
H4 | 0.8561 | −0.0206 | −0.0420 | 0.044* | |
C5 | 0.7072 (5) | 0.1451 (4) | 0.0226 (3) | 0.0330 (10) | |
H5 | 0.7649 | 0.1875 | −0.0011 | 0.040* | |
C6 | 0.5652 (5) | 0.2047 (4) | 0.0833 (3) | 0.0256 (8) | |
C7 | 0.4909 (5) | 0.3392 (4) | 0.1148 (3) | 0.0280 (9) | |
C8 | 0.4182 (5) | 0.1999 (4) | 0.3888 (3) | 0.0323 (10) | |
C9 | 0.3121 (5) | 0.3328 (4) | 0.4155 (3) | 0.0290 (9) | |
C10 | 0.3088 (6) | 0.4044 (5) | 0.4833 (3) | 0.0440 (12) | |
H10 | 0.3721 | 0.3709 | 0.5166 | 0.053* | |
C11 | 0.2116 (7) | 0.5246 (5) | 0.5006 (4) | 0.0512 (14) | |
H11 | 0.2080 | 0.5730 | 0.5463 | 0.061* | |
C12 | 0.1190 (6) | 0.5747 (4) | 0.4511 (3) | 0.0413 (12) | |
H12 | 0.0539 | 0.6569 | 0.4614 | 0.050* | |
C13 | 0.1260 (5) | 0.4985 (4) | 0.3853 (3) | 0.0291 (9) | |
C14 | 0.0354 (5) | 0.5392 (4) | 0.3236 (3) | 0.0344 (10) | |
C15 | 0.0629 (5) | 0.3022 (4) | 0.0912 (3) | 0.0283 (9) | |
C16 | −0.0431 (5) | 0.2742 (4) | 0.1709 (3) | 0.0275 (9) | |
C17 | −0.1751 (5) | 0.2778 (4) | 0.1699 (3) | 0.0359 (10) | |
H17 | −0.2051 | 0.2994 | 0.1198 | 0.043* | |
C18 | −0.2617 (5) | 0.2483 (4) | 0.2461 (3) | 0.0422 (12) | |
H18 | −0.3524 | 0.2514 | 0.2483 | 0.051* | |
C19 | −0.2125 (5) | 0.2142 (5) | 0.3184 (3) | 0.0399 (11) | |
H19 | −0.2686 | 0.1924 | 0.3693 | 0.048* | |
C20 | −0.0796 (4) | 0.2126 (4) | 0.3149 (3) | 0.0262 (9) | |
C21 | −0.0133 (5) | 0.1762 (4) | 0.3895 (3) | 0.0291 (9) | |
N4 | 0.4953 (4) | 0.3149 (3) | −0.2934 (2) | 0.0329 (8) | |
N5 | 0.6247 (5) | 0.3344 (4) | −0.1493 (3) | 0.0484 (11) | |
H5A | 0.5491 | 0.3981 | −0.1133 | 0.058* | |
H5B | 0.7021 | 0.3124 | −0.1304 | 0.058* | |
H5C | 0.5996 | 0.2723 | −0.1480 | 0.058* | |
N6 | 0.7286 (5) | 0.0306 (4) | −0.4569 (3) | 0.0438 (10) | |
H6A | 0.6827 | 0.0289 | −0.4951 | 0.053* | |
H6B | 0.7729 | −0.0447 | −0.4428 | 0.053* | |
H6C | 0.7957 | 0.0595 | −0.4827 | 0.053* | |
N7 | 0.2528 (4) | 0.2817 (3) | −0.1512 (2) | 0.0352 (8) | |
H7A | 0.2448 | 0.2268 | −0.1825 | 0.042* | |
H7B | 0.1841 | 0.3008 | −0.0968 | 0.042* | |
H7C | 0.3419 | 0.2505 | −0.1454 | 0.042* | |
C22 | 0.5344 (6) | 0.4124 (4) | −0.2754 (3) | 0.0401 (11) | |
H22A | 0.4497 | 0.4740 | −0.2309 | 0.048* | |
H22B | 0.5573 | 0.4508 | −0.3304 | 0.048* | |
C23 | 0.6634 (6) | 0.3683 (5) | −0.2420 (4) | 0.0431 (12) | |
H23A | 0.7436 | 0.2980 | −0.2814 | 0.052* | |
H23B | 0.6974 | 0.4322 | −0.2440 | 0.052* | |
C24 | 0.6036 (6) | 0.2387 (4) | −0.3780 (3) | 0.0395 (11) | |
H24A | 0.6986 | 0.2401 | −0.3876 | 0.047* | |
H24B | 0.5713 | 0.2725 | −0.4284 | 0.047* | |
C25 | 0.6198 (6) | 0.1104 (5) | −0.3745 (3) | 0.0481 (13) | |
H25A | 0.6500 | 0.0777 | −0.3232 | 0.058* | |
H25B | 0.5247 | 0.1096 | −0.3654 | 0.058* | |
C26 | 0.3433 (5) | 0.3634 (5) | −0.2933 (3) | 0.0398 (11) | |
H26A | 0.3322 | 0.3038 | −0.3261 | 0.048* | |
H26B | 0.3229 | 0.4368 | −0.3245 | 0.048* | |
C27 | 0.2322 (5) | 0.3933 (4) | −0.1992 (3) | 0.0374 (10) | |
H27A | 0.2434 | 0.4523 | −0.1659 | 0.045* | |
H27B | 0.1331 | 0.4298 | −0.2025 | 0.045* | |
O13 | 0.6959 (4) | −0.0604 (4) | 0.2573 (3) | 0.0533 (9) | |
O14 | 0.1129 (5) | −0.0760 (4) | 0.2469 (4) | 0.0668 (12) | |
O15 | 0.1312 (5) | 0.1096 (4) | 0.6273 (3) | 0.0652 (11) | |
O16 | 0.3028 (8) | 0.4321 (6) | −0.0215 (4) | 0.098 (2) | |
O17 | 0.1104 (6) | 0.6665 (6) | 0.1194 (4) | 0.100 (2) | |
O18 | −0.0377 (6) | −0.0752 (6) | 0.1299 (4) | 0.108 (2) | |
H13A | 0.631 (6) | 0.009 (3) | 0.274 (5) | 0.10 (3)* | |
H14A | 0.064 (5) | −0.055 (3) | 0.213 (3) | 0.032 (15)* | |
H16A | 0.265 (8) | 0.393 (6) | 0.014 (4) | 0.11 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Tb | 0.02433 (12) | 0.01976 (12) | 0.02033 (12) | −0.01165 (8) | −0.00532 (8) | −0.00153 (7) |
O1 | 0.0302 (16) | 0.0241 (15) | 0.0302 (15) | −0.0147 (13) | −0.0031 (13) | −0.0040 (12) |
O2 | 0.0402 (17) | 0.0236 (16) | 0.0420 (18) | −0.0158 (14) | −0.0130 (15) | 0.0007 (13) |
O3 | 0.0395 (18) | 0.0250 (16) | 0.0370 (17) | −0.0207 (14) | −0.0010 (14) | −0.0034 (13) |
O4 | 0.0461 (19) | 0.0365 (19) | 0.050 (2) | −0.0290 (16) | −0.0062 (16) | 0.0050 (15) |
O5 | 0.0351 (17) | 0.0264 (16) | 0.0342 (16) | −0.0104 (13) | −0.0121 (14) | −0.0042 (13) |
O6 | 0.060 (2) | 0.055 (2) | 0.048 (2) | −0.0146 (19) | −0.034 (2) | 0.0075 (18) |
O7 | 0.0365 (17) | 0.0220 (16) | 0.053 (2) | −0.0045 (13) | −0.0222 (16) | −0.0076 (14) |
O8 | 0.072 (3) | 0.027 (2) | 0.108 (4) | −0.0108 (19) | −0.051 (3) | −0.004 (2) |
O9 | 0.0274 (15) | 0.0355 (17) | 0.0282 (15) | −0.0160 (13) | −0.0057 (13) | 0.0016 (12) |
O10 | 0.0391 (19) | 0.072 (3) | 0.0265 (17) | −0.0233 (18) | −0.0141 (15) | 0.0130 (16) |
O11 | 0.0326 (16) | 0.0359 (17) | 0.0237 (14) | −0.0204 (14) | −0.0058 (13) | 0.0028 (12) |
O12 | 0.049 (2) | 0.061 (2) | 0.0311 (17) | −0.0361 (19) | −0.0067 (15) | 0.0108 (16) |
N1 | 0.0293 (18) | 0.0242 (18) | 0.0210 (16) | −0.0153 (15) | −0.0097 (14) | 0.0025 (13) |
N2 | 0.0320 (18) | 0.0233 (18) | 0.0247 (17) | −0.0158 (15) | −0.0063 (15) | −0.0004 (14) |
N3 | 0.0236 (17) | 0.0300 (19) | 0.0210 (16) | −0.0114 (15) | −0.0018 (14) | −0.0036 (14) |
C1 | 0.032 (2) | 0.026 (2) | 0.0226 (19) | −0.0161 (18) | −0.0127 (18) | 0.0053 (16) |
C2 | 0.031 (2) | 0.021 (2) | 0.0213 (19) | −0.0134 (17) | −0.0099 (17) | 0.0022 (15) |
C3 | 0.037 (2) | 0.027 (2) | 0.028 (2) | −0.0108 (19) | −0.0080 (19) | −0.0007 (17) |
C4 | 0.032 (2) | 0.041 (3) | 0.029 (2) | −0.012 (2) | −0.0039 (19) | −0.0010 (19) |
C5 | 0.033 (2) | 0.042 (3) | 0.029 (2) | −0.022 (2) | −0.0076 (19) | 0.0039 (19) |
C6 | 0.031 (2) | 0.031 (2) | 0.0213 (19) | −0.0183 (18) | −0.0094 (17) | 0.0055 (16) |
C7 | 0.035 (2) | 0.030 (2) | 0.029 (2) | −0.0219 (19) | −0.0111 (19) | 0.0057 (17) |
C8 | 0.033 (2) | 0.038 (3) | 0.032 (2) | −0.020 (2) | −0.012 (2) | 0.0060 (19) |
C9 | 0.037 (2) | 0.036 (2) | 0.0211 (19) | −0.023 (2) | −0.0084 (18) | 0.0012 (17) |
C10 | 0.056 (3) | 0.052 (3) | 0.031 (2) | −0.024 (3) | −0.020 (2) | −0.002 (2) |
C11 | 0.073 (4) | 0.048 (3) | 0.040 (3) | −0.031 (3) | −0.020 (3) | −0.011 (2) |
C12 | 0.051 (3) | 0.033 (3) | 0.037 (3) | −0.021 (2) | −0.005 (2) | −0.010 (2) |
C13 | 0.031 (2) | 0.026 (2) | 0.028 (2) | −0.0164 (19) | −0.0009 (18) | −0.0029 (17) |
C14 | 0.028 (2) | 0.024 (2) | 0.046 (3) | −0.0099 (19) | −0.005 (2) | −0.0025 (19) |
C15 | 0.029 (2) | 0.026 (2) | 0.028 (2) | −0.0103 (18) | −0.0072 (18) | 0.0005 (17) |
C16 | 0.029 (2) | 0.025 (2) | 0.025 (2) | −0.0107 (18) | −0.0042 (17) | −0.0037 (16) |
C17 | 0.033 (2) | 0.046 (3) | 0.035 (2) | −0.020 (2) | −0.015 (2) | 0.002 (2) |
C18 | 0.032 (3) | 0.056 (3) | 0.049 (3) | −0.027 (2) | −0.016 (2) | 0.007 (3) |
C19 | 0.036 (3) | 0.050 (3) | 0.039 (3) | −0.026 (2) | −0.007 (2) | 0.005 (2) |
C20 | 0.029 (2) | 0.022 (2) | 0.024 (2) | −0.0129 (17) | 0.0001 (17) | −0.0021 (16) |
C21 | 0.031 (2) | 0.029 (2) | 0.024 (2) | −0.0142 (19) | −0.0015 (18) | −0.0019 (17) |
N4 | 0.039 (2) | 0.031 (2) | 0.0270 (18) | −0.0159 (17) | −0.0053 (16) | −0.0021 (15) |
N5 | 0.053 (3) | 0.042 (3) | 0.065 (3) | −0.030 (2) | −0.027 (2) | 0.008 (2) |
N6 | 0.058 (3) | 0.038 (2) | 0.035 (2) | −0.027 (2) | −0.0043 (19) | −0.0044 (17) |
N7 | 0.036 (2) | 0.040 (2) | 0.0313 (19) | −0.0182 (18) | −0.0100 (17) | 0.0020 (16) |
C22 | 0.052 (3) | 0.025 (2) | 0.039 (3) | −0.019 (2) | −0.006 (2) | 0.0005 (19) |
C23 | 0.048 (3) | 0.031 (3) | 0.055 (3) | −0.026 (2) | −0.010 (2) | 0.003 (2) |
C24 | 0.050 (3) | 0.036 (3) | 0.026 (2) | −0.021 (2) | −0.001 (2) | −0.0004 (19) |
C25 | 0.060 (3) | 0.036 (3) | 0.036 (3) | −0.022 (3) | 0.002 (2) | 0.001 (2) |
C26 | 0.049 (3) | 0.045 (3) | 0.029 (2) | −0.021 (2) | −0.017 (2) | 0.008 (2) |
C27 | 0.035 (2) | 0.039 (3) | 0.035 (2) | −0.011 (2) | −0.013 (2) | 0.003 (2) |
O13 | 0.050 (2) | 0.048 (2) | 0.055 (2) | −0.015 (2) | −0.0135 (19) | −0.0100 (19) |
O14 | 0.054 (3) | 0.051 (3) | 0.097 (4) | −0.030 (2) | −0.016 (3) | 0.014 (2) |
O15 | 0.077 (3) | 0.051 (2) | 0.058 (2) | −0.024 (2) | −0.011 (2) | −0.0125 (19) |
O16 | 0.176 (6) | 0.129 (5) | 0.079 (3) | −0.129 (5) | −0.078 (4) | 0.060 (3) |
O17 | 0.078 (4) | 0.144 (6) | 0.104 (4) | −0.064 (4) | −0.045 (3) | 0.039 (4) |
O18 | 0.077 (4) | 0.172 (6) | 0.089 (4) | −0.070 (4) | −0.021 (3) | 0.018 (4) |
Tb—O7 | 2.393 (3) | C13—C14 | 1.504 (7) |
Tb—O3 | 2.398 (3) | C15—C16 | 1.519 (6) |
Tb—O9 | 2.428 (3) | C16—C17 | 1.379 (6) |
Tb—O1 | 2.431 (3) | C17—C18 | 1.387 (6) |
Tb—O11 | 2.435 (3) | C17—H17 | 0.93 |
Tb—O5 | 2.448 (3) | C18—C19 | 1.377 (7) |
Tb—N1 | 2.492 (3) | C18—H18 | 0.93 |
Tb—N3 | 2.499 (3) | C19—C20 | 1.376 (6) |
Tb—N2 | 2.508 (3) | C19—H19 | 0.93 |
O1—C1 | 1.265 (5) | C20—C21 | 1.513 (6) |
O2—C1 | 1.243 (5) | N4—C26 | 1.461 (6) |
O3—C7 | 1.260 (5) | N4—C22 | 1.463 (6) |
O4—C7 | 1.244 (5) | N4—C24 | 1.481 (6) |
O5—C8 | 1.290 (5) | N5—C23 | 1.472 (6) |
O6—C8 | 1.229 (6) | N5—H5A | 0.89 |
O7—C14 | 1.261 (5) | N5—H5B | 0.89 |
O8—C14 | 1.236 (6) | N5—H5C | 0.89 |
O9—C15 | 1.264 (5) | N6—C25 | 1.476 (6) |
O10—C15 | 1.239 (5) | N6—H6A | 0.89 |
O11—C21 | 1.268 (5) | N6—H6B | 0.89 |
O12—C21 | 1.235 (5) | N6—H6C | 0.89 |
N1—C2 | 1.330 (5) | N7—C27 | 1.484 (6) |
N1—C6 | 1.353 (5) | N7—H7A | 0.89 |
N2—C9 | 1.330 (6) | N7—H7B | 0.89 |
N2—C13 | 1.341 (6) | N7—H7C | 0.89 |
N3—C16 | 1.333 (6) | C22—C23 | 1.498 (7) |
N3—C20 | 1.351 (5) | C22—H22A | 0.97 |
C1—C2 | 1.511 (5) | C22—H22B | 0.97 |
C2—C3 | 1.374 (6) | C23—H23A | 0.97 |
C3—C4 | 1.383 (6) | C23—H23B | 0.97 |
C3—H3 | 0.93 | C24—C25 | 1.487 (7) |
C4—C5 | 1.379 (7) | C24—H24A | 0.97 |
C4—H4 | 0.93 | C24—H24B | 0.97 |
C5—C6 | 1.388 (6) | C25—H25A | 0.97 |
C5—H5 | 0.93 | C25—H25B | 0.97 |
C6—C7 | 1.507 (6) | C26—C27 | 1.511 (6) |
C8—C9 | 1.511 (7) | C26—H26A | 0.97 |
C9—C10 | 1.388 (6) | C26—H26B | 0.97 |
C10—C11 | 1.364 (8) | C27—H27A | 0.97 |
C10—H10 | 0.93 | C27—H27B | 0.97 |
C11—C12 | 1.373 (8) | O13—H13A | 0.82 (4) |
C11—H11 | 0.93 | O14—H14A | 0.82 (5) |
C12—C13 | 1.381 (6) | O16—H16A | 0.83 (7) |
C12—H12 | 0.93 | ||
O7—Tb—O3 | 76.76 (11) | C13—C12—H12 | 121.2 |
O7—Tb—O9 | 75.65 (11) | N2—C13—C12 | 122.0 (4) |
O3—Tb—O9 | 78.48 (10) | N2—C13—C14 | 113.5 (4) |
O7—Tb—O1 | 145.15 (10) | C12—C13—C14 | 124.4 (4) |
O3—Tb—O1 | 127.82 (10) | O8—C14—O7 | 124.6 (5) |
O9—Tb—O1 | 85.11 (10) | O8—C14—C13 | 119.5 (4) |
O7—Tb—O11 | 92.44 (11) | O7—C14—C13 | 115.9 (4) |
O3—Tb—O11 | 148.33 (10) | O10—C15—O9 | 126.1 (4) |
O9—Tb—O11 | 128.12 (10) | O10—C15—C16 | 118.2 (4) |
O1—Tb—O11 | 76.83 (10) | O9—C15—C16 | 115.7 (4) |
O7—Tb—O5 | 128.33 (10) | N3—C16—C17 | 122.9 (4) |
O3—Tb—O5 | 88.92 (11) | N3—C16—C15 | 114.1 (4) |
O9—Tb—O5 | 149.74 (10) | C17—C16—C15 | 123.0 (4) |
O1—Tb—O5 | 81.12 (10) | C16—C17—C18 | 117.8 (4) |
O11—Tb—O5 | 74.46 (10) | C16—C17—H17 | 121.1 |
O7—Tb—N1 | 135.31 (11) | C18—C17—H17 | 121.1 |
O3—Tb—N1 | 64.06 (10) | C19—C18—C17 | 119.6 (4) |
O9—Tb—N1 | 76.23 (10) | C19—C18—H18 | 120.2 |
O1—Tb—N1 | 63.99 (10) | C17—C18—H18 | 120.2 |
O11—Tb—N1 | 132.23 (10) | C20—C19—C18 | 119.5 (4) |
O5—Tb—N1 | 73.52 (10) | C20—C19—H19 | 120.3 |
O7—Tb—N3 | 71.48 (11) | C18—C19—H19 | 120.3 |
O3—Tb—N3 | 135.41 (11) | N3—C20—C19 | 121.1 (4) |
O9—Tb—N3 | 64.02 (10) | N3—C20—C21 | 114.4 (4) |
O1—Tb—N3 | 74.02 (11) | C19—C20—C21 | 124.5 (4) |
O11—Tb—N3 | 64.31 (10) | O12—C21—O11 | 124.8 (4) |
O5—Tb—N3 | 135.46 (11) | O12—C21—C20 | 119.3 (4) |
N1—Tb—N3 | 123.68 (10) | O11—C21—C20 | 115.9 (4) |
O7—Tb—N2 | 63.94 (11) | C26—N4—C22 | 111.6 (4) |
O3—Tb—N2 | 72.80 (10) | C26—N4—C24 | 112.7 (4) |
O9—Tb—N2 | 134.45 (11) | C22—N4—C24 | 110.3 (4) |
O1—Tb—N2 | 140.41 (11) | C23—N5—H5A | 109.5 |
O11—Tb—N2 | 75.70 (10) | C23—N5—H5B | 109.5 |
O5—Tb—N2 | 64.39 (10) | H5A—N5—H5B | 109.5 |
N1—Tb—N2 | 118.99 (11) | C23—N5—H5C | 109.5 |
N3—Tb—N2 | 117.31 (11) | H5A—N5—H5C | 109.5 |
C1—O1—Tb | 124.2 (2) | H5B—N5—H5C | 109.5 |
C7—O3—Tb | 126.3 (3) | C25—N6—H6A | 109.5 |
C8—O5—Tb | 124.0 (3) | C25—N6—H6B | 109.5 |
C14—O7—Tb | 125.1 (3) | H6A—N6—H6B | 109.5 |
C15—O9—Tb | 125.2 (3) | C25—N6—H6C | 109.5 |
C21—O11—Tb | 125.1 (3) | H6A—N6—H6C | 109.5 |
C2—N1—C6 | 118.5 (3) | H6B—N6—H6C | 109.5 |
C2—N1—Tb | 121.0 (2) | C27—N7—H7A | 109.5 |
C6—N1—Tb | 120.3 (3) | C27—N7—H7B | 109.5 |
C9—N2—C13 | 120.0 (4) | H7A—N7—H7B | 109.5 |
C9—N2—Tb | 120.2 (3) | C27—N7—H7C | 109.5 |
C13—N2—Tb | 119.8 (3) | H7A—N7—H7C | 109.5 |
C16—N3—C20 | 119.0 (4) | H7B—N7—H7C | 109.5 |
C16—N3—Tb | 120.7 (3) | N4—C22—C23 | 113.3 (4) |
C20—N3—Tb | 120.2 (3) | N4—C22—H22A | 108.9 |
O2—C1—O1 | 125.9 (4) | C23—C22—H22A | 108.9 |
O2—C1—C2 | 117.9 (4) | N4—C22—H22B | 108.9 |
O1—C1—C2 | 116.3 (3) | C23—C22—H22B | 108.9 |
N1—C2—C3 | 122.5 (4) | H22A—C22—H22B | 107.7 |
N1—C2—C1 | 113.8 (3) | N5—C23—C22 | 111.7 (4) |
C3—C2—C1 | 123.8 (4) | N5—C23—H23A | 109.3 |
C2—C3—C4 | 119.4 (4) | C22—C23—H23A | 109.3 |
C2—C3—H3 | 120.3 | N5—C23—H23B | 109.3 |
C4—C3—H3 | 120.3 | C22—C23—H23B | 109.3 |
C5—C4—C3 | 118.8 (4) | H23A—C23—H23B | 107.9 |
C5—C4—H4 | 120.6 | N4—C24—C25 | 111.1 (4) |
C3—C4—H4 | 120.6 | N4—C24—H24A | 109.4 |
C4—C5—C6 | 118.8 (4) | C25—C24—H24A | 109.4 |
C4—C5—H5 | 120.6 | N4—C24—H24B | 109.4 |
C6—C5—H5 | 120.6 | C25—C24—H24B | 109.4 |
N1—C6—C5 | 121.9 (4) | H24A—C24—H24B | 108.0 |
N1—C6—C7 | 113.4 (3) | N6—C25—C24 | 113.0 (4) |
C5—C6—C7 | 124.7 (4) | N6—C25—H25A | 109.0 |
O4—C7—O3 | 126.5 (4) | C24—C25—H25A | 109.0 |
O4—C7—C6 | 117.9 (4) | N6—C25—H25B | 109.0 |
O3—C7—C6 | 115.6 (3) | C24—C25—H25B | 109.0 |
O6—C8—O5 | 125.5 (5) | H25A—C25—H25B | 107.8 |
O6—C8—C9 | 119.3 (4) | N4—C26—C27 | 112.5 (4) |
O5—C8—C9 | 115.2 (4) | N4—C26—H26A | 109.1 |
N2—C9—C10 | 120.6 (4) | C27—C26—H26A | 109.1 |
N2—C9—C8 | 115.7 (4) | N4—C26—H26B | 109.1 |
C10—C9—C8 | 123.6 (4) | C27—C26—H26B | 109.1 |
C11—C10—C9 | 119.2 (5) | H26A—C26—H26B | 107.8 |
C11—C10—H10 | 120.4 | N7—C27—C26 | 110.9 (4) |
C9—C10—H10 | 120.4 | N7—C27—H27A | 109.5 |
C10—C11—C12 | 120.6 (4) | C26—C27—H27A | 109.5 |
C10—C11—H11 | 119.7 | N7—C27—H27B | 109.5 |
C12—C11—H11 | 119.7 | C26—C27—H27B | 109.5 |
C11—C12—C13 | 117.6 (5) | H27A—C27—H27B | 108.0 |
C11—C12—H12 | 121.2 | ||
O7—Tb—O1—C1 | 141.1 (3) | O11—Tb—N3—C20 | 2.9 (3) |
O3—Tb—O1—C1 | 13.6 (4) | O5—Tb—N3—C20 | 27.0 (4) |
O9—Tb—O1—C1 | 85.0 (3) | N1—Tb—N3—C20 | 128.1 (3) |
O11—Tb—O1—C1 | −144.0 (3) | N2—Tb—N3—C20 | −53.2 (3) |
O5—Tb—O1—C1 | −68.0 (3) | Tb—O1—C1—O2 | 171.6 (3) |
N1—Tb—O1—C1 | 7.9 (3) | Tb—O1—C1—C2 | −8.8 (5) |
N3—Tb—O1—C1 | 149.3 (3) | C6—N1—C2—C3 | 0.4 (6) |
N2—Tb—O1—C1 | −96.9 (3) | Tb—N1—C2—C3 | −175.1 (3) |
O7—Tb—O3—C7 | −158.0 (4) | C6—N1—C2—C1 | 179.8 (3) |
O9—Tb—O3—C7 | −80.2 (4) | Tb—N1—C2—C1 | 4.3 (4) |
O1—Tb—O3—C7 | −5.8 (4) | O2—C1—C2—N1 | −177.7 (3) |
O11—Tb—O3—C7 | 129.4 (3) | O1—C1—C2—N1 | 2.6 (5) |
O5—Tb—O3—C7 | 72.1 (4) | O2—C1—C2—C3 | 1.7 (6) |
N1—Tb—O3—C7 | 0.0 (3) | O1—C1—C2—C3 | −178.0 (4) |
N3—Tb—O3—C7 | −112.7 (3) | N1—C2—C3—C4 | 1.8 (6) |
N2—Tb—O3—C7 | 135.6 (4) | C1—C2—C3—C4 | −177.6 (4) |
O7—Tb—O5—C8 | 5.1 (4) | C2—C3—C4—C5 | −2.2 (7) |
O3—Tb—O5—C8 | 77.3 (3) | C3—C4—C5—C6 | 0.6 (7) |
O9—Tb—O5—C8 | 141.9 (3) | C2—N1—C6—C5 | −2.1 (6) |
O1—Tb—O5—C8 | −154.2 (3) | Tb—N1—C6—C5 | 173.4 (3) |
O11—Tb—O5—C8 | −75.5 (3) | C2—N1—C6—C7 | 178.3 (3) |
N1—Tb—O5—C8 | 140.5 (3) | Tb—N1—C6—C7 | −6.2 (4) |
N3—Tb—O5—C8 | −97.9 (3) | C4—C5—C6—N1 | 1.6 (6) |
N2—Tb—O5—C8 | 5.9 (3) | C4—C5—C6—C7 | −178.8 (4) |
O3—Tb—O7—C14 | −64.5 (4) | Tb—O3—C7—O4 | 177.7 (3) |
O9—Tb—O7—C14 | −145.8 (4) | Tb—O3—C7—C6 | −3.0 (5) |
O1—Tb—O7—C14 | 155.7 (3) | N1—C6—C7—O4 | −174.7 (4) |
O11—Tb—O7—C14 | 85.4 (4) | C5—C6—C7—O4 | 5.7 (6) |
O5—Tb—O7—C14 | 13.4 (4) | N1—C6—C7—O3 | 5.9 (5) |
N1—Tb—O7—C14 | −93.2 (4) | C5—C6—C7—O3 | −173.7 (4) |
N3—Tb—O7—C14 | 147.3 (4) | Tb—O5—C8—O6 | 172.1 (4) |
N2—Tb—O7—C14 | 12.6 (3) | Tb—O5—C8—C9 | −8.9 (5) |
O7—Tb—O9—C15 | −72.3 (3) | C13—N2—C9—C10 | 1.1 (6) |
O3—Tb—O9—C15 | −151.4 (3) | Tb—N2—C9—C10 | 176.9 (3) |
O1—Tb—O9—C15 | 78.4 (3) | C13—N2—C9—C8 | −177.7 (4) |
O11—Tb—O9—C15 | 9.3 (4) | Tb—N2—C9—C8 | −2.0 (5) |
O5—Tb—O9—C15 | 141.4 (3) | O6—C8—C9—N2 | −174.2 (4) |
N1—Tb—O9—C15 | 142.7 (3) | O5—C8—C9—N2 | 6.8 (5) |
N3—Tb—O9—C15 | 3.8 (3) | O6—C8—C9—C10 | 7.0 (7) |
N2—Tb—O9—C15 | −99.9 (3) | O5—C8—C9—C10 | −172.0 (4) |
O7—Tb—O11—C21 | 67.0 (3) | N2—C9—C10—C11 | −0.7 (7) |
O3—Tb—O11—C21 | 135.4 (3) | C8—C9—C10—C11 | 178.1 (5) |
O9—Tb—O11—C21 | −6.7 (4) | C9—C10—C11—C12 | −0.7 (8) |
O1—Tb—O11—C21 | −79.5 (3) | C10—C11—C12—C13 | 1.5 (8) |
O5—Tb—O11—C21 | −163.8 (3) | C9—N2—C13—C12 | −0.3 (6) |
N1—Tb—O11—C21 | −114.4 (3) | Tb—N2—C13—C12 | −176.0 (3) |
N3—Tb—O11—C21 | −1.1 (3) | C9—N2—C13—C14 | 177.3 (4) |
N2—Tb—O11—C21 | 129.3 (3) | Tb—N2—C13—C14 | 1.5 (5) |
O7—Tb—N1—C2 | −149.6 (3) | C11—C12—C13—N2 | −1.0 (7) |
O3—Tb—N1—C2 | 179.0 (3) | C11—C12—C13—C14 | −178.3 (4) |
O9—Tb—N1—C2 | −97.3 (3) | Tb—O7—C14—O8 | 161.5 (4) |
O1—Tb—N1—C2 | −6.0 (3) | Tb—O7—C14—C13 | −16.6 (6) |
O11—Tb—N1—C2 | 32.2 (3) | N2—C13—C14—O8 | −169.3 (4) |
O5—Tb—N1—C2 | 82.0 (3) | C12—C13—C14—O8 | 8.3 (7) |
N3—Tb—N1—C2 | −52.1 (3) | N2—C13—C14—O7 | 8.9 (6) |
N2—Tb—N1—C2 | 129.2 (3) | C12—C13—C14—O7 | −173.6 (4) |
O7—Tb—N1—C6 | 35.0 (3) | Tb—O9—C15—O10 | 179.5 (4) |
O3—Tb—N1—C6 | 3.6 (3) | Tb—O9—C15—C16 | −2.7 (5) |
O9—Tb—N1—C6 | 87.3 (3) | C20—N3—C16—C17 | 1.3 (6) |
O1—Tb—N1—C6 | 178.6 (3) | Tb—N3—C16—C17 | −176.1 (3) |
O11—Tb—N1—C6 | −143.2 (3) | C20—N3—C16—C15 | −177.6 (3) |
O5—Tb—N1—C6 | −93.4 (3) | Tb—N3—C16—C15 | 4.9 (5) |
N3—Tb—N1—C6 | 132.5 (3) | O10—C15—C16—N3 | 176.4 (4) |
N2—Tb—N1—C6 | −46.2 (3) | O9—C15—C16—N3 | −1.6 (5) |
O7—Tb—N2—C9 | 177.9 (3) | O10—C15—C16—C17 | −2.5 (6) |
O3—Tb—N2—C9 | −98.8 (3) | O9—C15—C16—C17 | 179.5 (4) |
O9—Tb—N2—C9 | −152.1 (3) | N3—C16—C17—C18 | 0.0 (7) |
O1—Tb—N2—C9 | 30.5 (4) | C15—C16—C17—C18 | 178.8 (4) |
O11—Tb—N2—C9 | 77.9 (3) | C16—C17—C18—C19 | −1.4 (7) |
O5—Tb—N2—C9 | −1.5 (3) | C17—C18—C19—C20 | 1.4 (7) |
N1—Tb—N2—C9 | −52.8 (3) | C16—N3—C20—C19 | −1.3 (6) |
N3—Tb—N2—C9 | 128.5 (3) | Tb—N3—C20—C19 | 176.2 (3) |
O7—Tb—N2—C13 | −6.4 (3) | C16—N3—C20—C21 | 178.3 (4) |
O3—Tb—N2—C13 | 77.0 (3) | Tb—N3—C20—C21 | −4.3 (4) |
O9—Tb—N2—C13 | 23.6 (4) | C18—C19—C20—N3 | −0.1 (7) |
O1—Tb—N2—C13 | −153.7 (3) | C18—C19—C20—C21 | −179.6 (4) |
O11—Tb—N2—C13 | −106.4 (3) | Tb—O11—C21—O12 | −179.8 (3) |
O5—Tb—N2—C13 | 174.3 (3) | Tb—O11—C21—C20 | −0.6 (5) |
N1—Tb—N2—C13 | 123.0 (3) | N3—C20—C21—O12 | −177.5 (4) |
N3—Tb—N2—C13 | −55.8 (3) | C19—C20—C21—O12 | 2.0 (7) |
O7—Tb—N3—C16 | 78.2 (3) | N3—C20—C21—O11 | 3.2 (5) |
O3—Tb—N3—C16 | 31.4 (4) | C19—C20—C21—O11 | −177.4 (4) |
O9—Tb—N3—C16 | −4.5 (3) | C26—N4—C22—C23 | 159.1 (4) |
O1—Tb—N3—C16 | −96.8 (3) | C24—N4—C22—C23 | −74.8 (5) |
O11—Tb—N3—C16 | −179.6 (3) | N4—C22—C23—N5 | −71.4 (5) |
O5—Tb—N3—C16 | −155.5 (3) | C26—N4—C24—C25 | −85.1 (5) |
N1—Tb—N3—C16 | −54.5 (3) | C22—N4—C24—C25 | 149.4 (4) |
N2—Tb—N3—C16 | 124.2 (3) | N4—C24—C25—N6 | −179.1 (4) |
O7—Tb—N3—C20 | −99.3 (3) | C22—N4—C26—C27 | −79.6 (5) |
O3—Tb—N3—C20 | −146.1 (3) | C24—N4—C26—C27 | 155.7 (4) |
O9—Tb—N3—C20 | 178.1 (3) | N4—C26—C27—N7 | −62.7 (5) |
O1—Tb—N3—C20 | 85.7 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O13—H13A···O5 | 0.82 (4) | 2.10 (3) | 2.880 (5) | 158 (8) |
O14—H14A···O18 | 0.82 (5) | 2.02 (5) | 2.789 (8) | 157 (3) |
O16—H16A···O9 | 0.83 (7) | 2.01 (7) | 2.837 (5) | 178 (8) |
N7—H7B···O10 | 0.89 | 1.97 | 2.855 (5) | 174 |
N5—H5A···O4i | 0.89 | 2.19 | 2.979 (6) | 147 |
N5—H5B···O17i | 0.89 | 2.15 | 2.971 (7) | 152 |
N5—H5C···O2ii | 0.89 | 1.97 | 2.851 (5) | 171 |
N6—H6C···O12iii | 0.89 | 1.96 | 2.840 (5) | 172 |
N6—H6B···O11ii | 0.89 | 2.12 | 2.960 (5) | 158 |
N6—H6A···O15ii | 0.89 | 2.44 | 2.838 (5) | 107 |
N7—H7C···O2ii | 0.89 | 1.98 | 2.851 (5) | 165 |
N7—H7A···O13ii | 0.89 | 2.13 | 2.977 (6) | 160 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y, −z; (iii) x+1, y, z−1. |
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