Abstract
In the title centrosymmetric dinuclear complex, [Tm2(C10H11O4)6(C12H8N2)2], the unique TmIII ion is coordinated by five 3,4-dimethoxyphenylacetate (DMPA) ligands and and a bis-chelating 1,10-phenanthroline (phen) ligand via seven O atoms and two N atoms, forming a distorted tricapped trigonal-prismatic environment. The DMPA ligands coordinate in the bis-chelate, bridging and bridging tridentate modes.
Related literature
For background to the importance of coordination in magnetism, see: Yao et al. (2008 ▶); Fang & Zhang (2006 ▶); Li et al. 2008 ▶); Wang & Sevov (2008 ▶). For a related structure, see: Wang et al. (2008 ▶).
Experimental
Crystal data
[Tm2(C10H11O4)6(C12H8N2)2]
M r = 1869.40
Triclinic,
a = 12.3025 (1) Å
b = 12.3483 (2) Å
c = 14.5883 (2) Å
α = 91.457 (1)°
β = 103.403 (1)°
γ = 114.406 (1)°
V = 1944.71 (4) Å3
Z = 1
Mo Kα radiation
μ = 2.35 mm−1
T = 296 K
0.35 × 0.11 × 0.10 mm
Data collection
Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.747, T max = 0.798
32353 measured reflections
6861 independent reflections
5961 reflections with I > 2σ(I)
R int = 0.038
Refinement
R[F 2 > 2σ(F 2)] = 0.025
wR(F 2) = 0.058
S = 1.03
6861 reflections
514 parameters
H-atom parameters constrained
Δρmax = 0.64 e Å−3
Δρmin = −0.32 e Å−3
Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1999 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97.
Supplementary Material
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809051435/lh2956sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536809051435/lh2956Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
supplementary crystallographic information
Comment
In recently years, there has been an increasing interest in coordination chemistry due to the increased recognition of of it's importance in magnetism (Yao, et al., 2008; Fang, et al., 2006; Wang, et al., 2008) and this has attracted our interest (Li, et al., 2008). Here we report the crystal structure of a new thulium(III) complex with the ligand 3,4-dimethoxyphenylacetate. In the title dinuclear complex (I), the unique TmIII ion is coordinated by five DMPA ligands and a phen ligand via seven O atoms and two N atoms (see, Fig. 1). The TmIII ion is in a distorted tricapped trigonal prismatic environment. The DMPA ligands coordinate in the bis-chelate, bridging and bridging tridentate modes.
Experimental
All reagents and solvents were commercially available quality and without purified before using. The title compound was obtained by adding Tm2O3 (0.5 mmol), homoveratric acid (3 mmol) phen (1 mmol) dissolved in 30 ml water, sealed in a 50 ml stainless steel reactor and kept three days at temperature of 433 K. Then, the reactor was cooled to room temperature at a speed of 5 degrees per hour. Filtrate the solution, washing deposition with ethanol, then colorless histogram crystals can be attained.
Refinement
The H atoms bonded to C atoms were positioned geometrically and refined using a riding-model approximation with C—H distances of 0.96 and 0.93 Å for aliphatic and aromatic C atoms, respectively, and Uiso(H) = 1.2Ueq(C) or 1.5Ueq(Cmethyl).
Figures
Fig. 1.
The molecular structure of the title complex. Displacement ellipsoids are drawn at the 30% probability level. Unlabeled atoms are related by the symmetry operator (-x, -y, -z).
Crystal data
| [Tm2(C10H11O4)6(C12H8N2)2] | Z = 1 |
| Mr = 1869.40 | F(000) = 944 |
| Triclinic, P1 | Dx = 1.596 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
| a = 12.3025 (1) Å | Cell parameters from 8597 reflections |
| b = 12.3483 (2) Å | θ = 2.1–27.6° |
| c = 14.5883 (2) Å | µ = 2.35 mm−1 |
| α = 91.457 (1)° | T = 296 K |
| β = 103.403 (1)° | Block, colourless |
| γ = 114.406 (1)° | 0.35 × 0.11 × 0.10 mm |
| V = 1944.71 (4) Å3 |
Data collection
| Bruker SMART APEX diffractometer | 6861 independent reflections |
| Radiation source: fine-focus sealed tube | 5961 reflections with I > 2σ(I) |
| graphite | Rint = 0.038 |
| ω scans | θmax = 25.0°, θmin = 2.1° |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
| Tmin = 0.747, Tmax = 0.798 | k = −14→14 |
| 32353 measured reflections | l = −17→17 |
Refinement
| 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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.058 | H-atom parameters constrained |
| S = 1.03 | w = 1/[σ2(Fo2) + (0.0303P)2 + 0.071P] where P = (Fo2 + 2Fc2)/3 |
| 6861 reflections | (Δ/σ)max = 0.004 |
| 514 parameters | Δρmax = 0.64 e Å−3 |
| 0 restraints | Δρmin = −0.32 e Å−3 |
Special details
| 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | ||
| Tm1 | 0.175028 (11) | 0.102013 (13) | 0.030650 (9) | 0.04097 (6) | |
| N1 | 0.3561 (2) | 0.1554 (2) | 0.18114 (19) | 0.0465 (6) | |
| O1 | 0.3698 (2) | −0.4441 (2) | 0.30577 (16) | 0.0521 (6) | |
| C1 | 0.3391 (4) | −0.5686 (3) | 0.2846 (3) | 0.0632 (10) | |
| H1A | 0.3974 | −0.5884 | 0.3283 | 0.095* | |
| H1B | 0.3422 | −0.5848 | 0.2208 | 0.095* | |
| H1C | 0.2572 | −0.6161 | 0.2905 | 0.095* | |
| O2 | 0.3894 (2) | −0.2368 (2) | 0.36761 (18) | 0.0685 (7) | |
| N2 | 0.3785 (2) | 0.1373 (2) | 0.0008 (2) | 0.0496 (7) | |
| C2 | 0.2942 (3) | −0.4026 (3) | 0.2490 (2) | 0.0413 (7) | |
| O3 | 0.01233 (18) | −0.0982 (2) | 0.04225 (14) | 0.0462 (5) | |
| C3 | 0.2150 (3) | −0.4601 (3) | 0.1623 (2) | 0.0512 (8) | |
| H3A | 0.2115 | −0.5318 | 0.1373 | 0.061* | |
| O4 | 0.20449 (19) | −0.0728 (2) | 0.08331 (16) | 0.0487 (5) | |
| C4 | 0.1394 (3) | −0.4117 (3) | 0.1114 (3) | 0.0581 (9) | |
| H4A | 0.0872 | −0.4512 | 0.0519 | 0.070* | |
| O5 | 0.2337 (3) | 0.5128 (3) | −0.43218 (19) | 0.0821 (8) | |
| C5 | 0.1398 (3) | −0.3071 (3) | 0.1466 (2) | 0.0460 (8) | |
| C6 | 0.2248 (3) | −0.2465 (3) | 0.2326 (2) | 0.0451 (8) | |
| H6A | 0.2297 | −0.1737 | 0.2565 | 0.054* | |
| O6 | 0.1019 (2) | 0.5544 (3) | −0.3365 (2) | 0.0800 (8) | |
| O7 | 0.21737 (19) | 0.2421 (2) | −0.08600 (15) | 0.0469 (5) | |
| C7 | 0.3022 (3) | −0.2915 (3) | 0.2833 (2) | 0.0435 (7) | |
| O8 | 0.2591 (2) | 0.3120 (2) | 0.06308 (15) | 0.0555 (6) | |
| C8 | 0.4180 (4) | −0.1159 (4) | 0.3958 (3) | 0.0852 (14) | |
| H8A | 0.4800 | −0.0874 | 0.4556 | 0.128* | |
| H8B | 0.3447 | −0.1099 | 0.4022 | 0.128* | |
| H8C | 0.4488 | −0.0682 | 0.3486 | 0.128* | |
| C9 | 0.0460 (3) | −0.2642 (3) | 0.0961 (3) | 0.0550 (9) | |
| H9A | −0.0017 | −0.3175 | 0.0369 | 0.066* | |
| H9B | −0.0107 | −0.2735 | 0.1349 | 0.066* | |
| O9 | −0.2502 (3) | −0.0455 (3) | −0.5655 (2) | 0.0980 (10) | |
| C10 | 0.0931 (3) | −0.1378 (3) | 0.0735 (2) | 0.0416 (7) | |
| O10 | −0.1572 (3) | 0.1810 (3) | −0.5085 (2) | 0.0848 (9) | |
| O11 | 0.11190 (19) | −0.0205 (2) | −0.11245 (15) | 0.0470 (5) | |
| C11 | 0.3103 (5) | 0.5021 (5) | −0.4862 (3) | 0.1033 (16) | |
| H11C | 0.2831 | 0.5165 | −0.5499 | 0.155* | |
| H11D | 0.3060 | 0.4226 | −0.4875 | 0.155* | |
| H11A | 0.3942 | 0.5598 | −0.4581 | 0.155* | |
| C12 | 0.2587 (3) | 0.4949 (3) | −0.3385 (2) | 0.0576 (9) | |
| O12 | −0.09479 (19) | −0.1233 (2) | −0.15456 (15) | 0.0523 (6) | |
| C13 | 0.3461 (3) | 0.4592 (3) | −0.2948 (3) | 0.0625 (10) | |
| H13A | 0.3935 | 0.4427 | −0.3294 | 0.075* | |
| C14 | 0.3652 (3) | 0.4470 (3) | −0.1987 (3) | 0.0633 (10) | |
| H14A | 0.4253 | 0.4227 | −0.1693 | 0.076* | |
| C15 | 0.2951 (3) | 0.4710 (3) | −0.1466 (2) | 0.0534 (9) | |
| C16 | 0.2053 (3) | 0.5051 (3) | −0.1922 (3) | 0.0569 (9) | |
| H16A | 0.1564 | 0.5194 | −0.1580 | 0.068* | |
| C17 | 0.1865 (3) | 0.5185 (3) | −0.2867 (3) | 0.0564 (9) | |
| C18 | 0.0160 (4) | 0.5660 (4) | −0.2907 (4) | 0.0914 (14) | |
| H18A | −0.0379 | 0.5918 | −0.3334 | 0.137* | |
| H18B | 0.0602 | 0.6242 | −0.2347 | 0.137* | |
| H18C | −0.0322 | 0.4899 | −0.2733 | 0.137* | |
| C19 | 0.3135 (4) | 0.4569 (3) | −0.0425 (3) | 0.0640 (10) | |
| H19A | 0.2760 | 0.4999 | −0.0144 | 0.077* | |
| H19B | 0.4015 | 0.4944 | −0.0115 | 0.077* | |
| C20 | 0.2600 (3) | 0.3284 (3) | −0.0220 (2) | 0.0456 (8) | |
| C21 | −0.2939 (5) | −0.1633 (5) | −0.6054 (3) | 0.1053 (17) | |
| H21A | −0.3540 | −0.1780 | −0.6652 | 0.158* | |
| H21B | −0.3319 | −0.2160 | −0.5633 | 0.158* | |
| H21C | −0.2263 | −0.1776 | −0.6155 | 0.158* | |
| C22 | −0.1625 (3) | −0.0060 (4) | −0.4787 (3) | 0.0617 (10) | |
| C23 | −0.1222 (3) | −0.0781 (3) | −0.4219 (3) | 0.0585 (9) | |
| H23A | −0.1556 | −0.1601 | −0.4422 | 0.070* | |
| C24 | −0.0336 (3) | −0.0302 (3) | −0.3362 (2) | 0.0488 (8) | |
| C25 | 0.0151 (3) | 0.0914 (3) | −0.3078 (2) | 0.0594 (9) | |
| H25A | 0.0751 | 0.1250 | −0.2501 | 0.071* | |
| C26 | −0.0237 (4) | 0.1647 (4) | −0.3637 (3) | 0.0667 (10) | |
| H26A | 0.0107 | 0.2468 | −0.3437 | 0.080* | |
| C27 | −0.1136 (3) | 0.1156 (4) | −0.4491 (2) | 0.0602 (10) | |
| C28 | −0.1058 (5) | 0.3062 (5) | −0.4796 (4) | 0.1056 (17) | |
| H28A | −0.1433 | 0.3422 | −0.5267 | 0.158* | |
| H28B | −0.0181 | 0.3405 | −0.4726 | 0.158* | |
| H28C | −0.1210 | 0.3206 | −0.4199 | 0.158* | |
| C29 | 0.0109 (3) | −0.1085 (3) | −0.2735 (2) | 0.0544 (9) | |
| H29A | −0.0424 | −0.1925 | −0.2975 | 0.065* | |
| H29B | 0.0943 | −0.0927 | −0.2755 | 0.065* | |
| C30 | 0.0095 (3) | −0.0830 (3) | −0.1716 (2) | 0.0459 (8) | |
| C31 | 0.3467 (3) | 0.1640 (3) | 0.2691 (2) | 0.0534 (9) | |
| H31A | 0.2728 | 0.1600 | 0.2779 | 0.064* | |
| C32 | 0.4414 (3) | 0.1785 (3) | 0.3499 (3) | 0.0617 (10) | |
| H32A | 0.4311 | 0.1860 | 0.4105 | 0.074* | |
| C33 | 0.5489 (3) | 0.1816 (3) | 0.3375 (3) | 0.0645 (10) | |
| H33A | 0.6129 | 0.1906 | 0.3901 | 0.077* | |
| C34 | 0.5632 (3) | 0.1712 (3) | 0.2472 (3) | 0.0549 (9) | |
| C35 | 0.6728 (3) | 0.1718 (3) | 0.2281 (4) | 0.0746 (12) | |
| H35A | 0.7371 | 0.1761 | 0.2786 | 0.089* | |
| C36 | 0.6844 (3) | 0.1663 (4) | 0.1397 (4) | 0.0761 (13) | |
| H36A | 0.7570 | 0.1673 | 0.1302 | 0.091* | |
| C37 | 0.5883 (3) | 0.1588 (3) | 0.0593 (3) | 0.0592 (10) | |
| C38 | 0.5985 (3) | 0.1566 (3) | −0.0335 (3) | 0.0713 (12) | |
| H38A | 0.6712 | 0.1615 | −0.0457 | 0.086* | |
| C39 | 0.5023 (4) | 0.1473 (4) | −0.1062 (3) | 0.0726 (12) | |
| H39A | 0.5090 | 0.1484 | −0.1684 | 0.087* | |
| C40 | 0.3922 (3) | 0.1361 (3) | −0.0859 (3) | 0.0600 (10) | |
| H40A | 0.3258 | 0.1273 | −0.1363 | 0.072* | |
| C41 | 0.4763 (3) | 0.1515 (3) | 0.0748 (3) | 0.0485 (8) | |
| C42 | 0.4642 (3) | 0.1595 (3) | 0.1689 (2) | 0.0442 (8) |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Tm1 | 0.04263 (9) | 0.06291 (11) | 0.03925 (9) | 0.03882 (7) | 0.01862 (6) | 0.02181 (7) |
| N1 | 0.0437 (14) | 0.0538 (17) | 0.0553 (18) | 0.0325 (13) | 0.0142 (12) | 0.0189 (14) |
| O1 | 0.0606 (14) | 0.0536 (14) | 0.0516 (14) | 0.0386 (12) | 0.0048 (11) | 0.0131 (11) |
| C1 | 0.085 (3) | 0.066 (2) | 0.058 (2) | 0.055 (2) | 0.0112 (19) | 0.0174 (19) |
| O2 | 0.0852 (18) | 0.0539 (16) | 0.0568 (16) | 0.0380 (14) | −0.0132 (13) | 0.0011 (13) |
| N2 | 0.0496 (15) | 0.0606 (18) | 0.0589 (18) | 0.0355 (14) | 0.0275 (14) | 0.0227 (14) |
| C2 | 0.0425 (16) | 0.052 (2) | 0.0419 (18) | 0.0303 (15) | 0.0132 (14) | 0.0166 (15) |
| O3 | 0.0473 (12) | 0.0716 (15) | 0.0467 (13) | 0.0461 (11) | 0.0211 (10) | 0.0259 (11) |
| C3 | 0.062 (2) | 0.057 (2) | 0.048 (2) | 0.0425 (18) | 0.0064 (16) | 0.0029 (17) |
| O4 | 0.0422 (12) | 0.0622 (14) | 0.0601 (14) | 0.0369 (11) | 0.0178 (10) | 0.0243 (12) |
| C4 | 0.058 (2) | 0.064 (2) | 0.053 (2) | 0.0375 (19) | −0.0061 (16) | 0.0000 (18) |
| O5 | 0.093 (2) | 0.117 (2) | 0.0538 (16) | 0.0547 (18) | 0.0318 (15) | 0.0371 (16) |
| C5 | 0.0411 (17) | 0.049 (2) | 0.055 (2) | 0.0275 (15) | 0.0089 (15) | 0.0168 (16) |
| C6 | 0.0489 (18) | 0.0406 (18) | 0.054 (2) | 0.0255 (15) | 0.0155 (15) | 0.0158 (16) |
| O6 | 0.0758 (18) | 0.102 (2) | 0.086 (2) | 0.0550 (17) | 0.0296 (15) | 0.0426 (17) |
| O7 | 0.0538 (13) | 0.0596 (15) | 0.0419 (13) | 0.0341 (12) | 0.0197 (10) | 0.0159 (12) |
| C7 | 0.0472 (17) | 0.0441 (19) | 0.0422 (18) | 0.0235 (15) | 0.0095 (14) | 0.0116 (15) |
| O8 | 0.0776 (16) | 0.0684 (16) | 0.0387 (13) | 0.0454 (13) | 0.0210 (11) | 0.0209 (12) |
| C8 | 0.097 (3) | 0.060 (3) | 0.080 (3) | 0.039 (2) | −0.015 (2) | −0.010 (2) |
| C9 | 0.0455 (18) | 0.055 (2) | 0.070 (2) | 0.0310 (17) | 0.0078 (16) | 0.0166 (18) |
| O9 | 0.101 (2) | 0.092 (2) | 0.078 (2) | 0.0443 (19) | −0.0206 (18) | −0.0066 (18) |
| C10 | 0.0466 (18) | 0.063 (2) | 0.0347 (17) | 0.0405 (17) | 0.0144 (13) | 0.0146 (15) |
| O10 | 0.101 (2) | 0.086 (2) | 0.0683 (19) | 0.0523 (18) | 0.0012 (16) | 0.0217 (16) |
| O11 | 0.0476 (13) | 0.0688 (15) | 0.0452 (13) | 0.0393 (12) | 0.0220 (11) | 0.0189 (11) |
| C11 | 0.141 (4) | 0.134 (4) | 0.055 (3) | 0.067 (4) | 0.046 (3) | 0.034 (3) |
| C12 | 0.064 (2) | 0.066 (2) | 0.047 (2) | 0.0271 (19) | 0.0227 (17) | 0.0229 (18) |
| O12 | 0.0468 (12) | 0.0839 (17) | 0.0425 (13) | 0.0401 (12) | 0.0180 (10) | 0.0170 (12) |
| C13 | 0.067 (2) | 0.073 (3) | 0.063 (2) | 0.035 (2) | 0.0336 (19) | 0.019 (2) |
| C14 | 0.069 (2) | 0.074 (3) | 0.059 (2) | 0.042 (2) | 0.0185 (19) | 0.027 (2) |
| C15 | 0.066 (2) | 0.048 (2) | 0.048 (2) | 0.0207 (17) | 0.0237 (17) | 0.0157 (17) |
| C16 | 0.066 (2) | 0.055 (2) | 0.060 (2) | 0.0282 (18) | 0.0294 (18) | 0.0185 (18) |
| C17 | 0.061 (2) | 0.055 (2) | 0.060 (2) | 0.0288 (18) | 0.0206 (18) | 0.0229 (18) |
| C18 | 0.075 (3) | 0.101 (4) | 0.121 (4) | 0.053 (3) | 0.036 (3) | 0.033 (3) |
| C19 | 0.077 (3) | 0.064 (2) | 0.048 (2) | 0.025 (2) | 0.0199 (18) | 0.0160 (19) |
| C20 | 0.0430 (17) | 0.065 (2) | 0.043 (2) | 0.0352 (17) | 0.0141 (14) | 0.0178 (18) |
| C21 | 0.091 (3) | 0.126 (5) | 0.073 (3) | 0.040 (3) | −0.008 (3) | −0.024 (3) |
| C22 | 0.060 (2) | 0.076 (3) | 0.048 (2) | 0.032 (2) | 0.0076 (17) | 0.013 (2) |
| C23 | 0.058 (2) | 0.064 (2) | 0.054 (2) | 0.0277 (19) | 0.0145 (17) | 0.0062 (19) |
| C24 | 0.0536 (19) | 0.071 (3) | 0.0369 (18) | 0.0351 (18) | 0.0225 (15) | 0.0174 (17) |
| C25 | 0.070 (2) | 0.066 (3) | 0.041 (2) | 0.033 (2) | 0.0074 (17) | 0.0117 (18) |
| C26 | 0.082 (3) | 0.063 (2) | 0.052 (2) | 0.032 (2) | 0.011 (2) | 0.0130 (19) |
| C27 | 0.067 (2) | 0.073 (3) | 0.044 (2) | 0.035 (2) | 0.0110 (17) | 0.019 (2) |
| C28 | 0.132 (4) | 0.086 (4) | 0.097 (4) | 0.053 (3) | 0.013 (3) | 0.040 (3) |
| C29 | 0.066 (2) | 0.075 (2) | 0.046 (2) | 0.046 (2) | 0.0266 (16) | 0.0155 (18) |
| C30 | 0.054 (2) | 0.066 (2) | 0.0426 (18) | 0.0442 (18) | 0.0218 (16) | 0.0221 (17) |
| C31 | 0.054 (2) | 0.064 (2) | 0.054 (2) | 0.0370 (18) | 0.0136 (16) | 0.0200 (18) |
| C32 | 0.065 (2) | 0.067 (2) | 0.054 (2) | 0.035 (2) | 0.0039 (18) | 0.0174 (19) |
| C33 | 0.057 (2) | 0.057 (2) | 0.068 (3) | 0.0271 (19) | −0.0076 (19) | 0.009 (2) |
| C34 | 0.0394 (18) | 0.0397 (19) | 0.081 (3) | 0.0204 (15) | 0.0012 (17) | 0.0059 (18) |
| C35 | 0.0370 (19) | 0.060 (3) | 0.114 (4) | 0.0225 (18) | −0.004 (2) | −0.005 (3) |
| C36 | 0.0330 (19) | 0.065 (3) | 0.131 (4) | 0.0257 (18) | 0.016 (2) | −0.002 (3) |
| C37 | 0.0403 (18) | 0.047 (2) | 0.104 (3) | 0.0265 (16) | 0.0279 (19) | 0.010 (2) |
| C38 | 0.049 (2) | 0.063 (2) | 0.120 (4) | 0.0294 (19) | 0.046 (2) | 0.010 (2) |
| C39 | 0.073 (3) | 0.076 (3) | 0.097 (3) | 0.041 (2) | 0.055 (2) | 0.023 (2) |
| C40 | 0.059 (2) | 0.074 (3) | 0.071 (3) | 0.042 (2) | 0.0354 (19) | 0.024 (2) |
| C41 | 0.0388 (17) | 0.0427 (19) | 0.074 (2) | 0.0238 (15) | 0.0208 (16) | 0.0148 (17) |
| C42 | 0.0380 (16) | 0.0388 (18) | 0.065 (2) | 0.0244 (14) | 0.0142 (15) | 0.0163 (16) |
Geometric parameters (Å, °)
| Tm1—O3i | 2.2840 (18) | C12—C17 | 1.399 (5) |
| Tm1—O12i | 2.308 (2) | O12—C30 | 1.258 (4) |
| Tm1—O11 | 2.317 (2) | O12—Tm1i | 2.308 (2) |
| Tm1—O8 | 2.348 (2) | C13—C14 | 1.389 (5) |
| Tm1—O7 | 2.444 (2) | C13—H13A | 0.9300 |
| Tm1—O4 | 2.4459 (19) | C14—C15 | 1.382 (5) |
| Tm1—O3 | 2.497 (2) | C14—H14A | 0.9300 |
| Tm1—N2 | 2.502 (2) | C15—C16 | 1.378 (5) |
| Tm1—N1 | 2.581 (2) | C15—C19 | 1.508 (5) |
| Tm1—C20 | 2.750 (3) | C16—C17 | 1.371 (5) |
| Tm1—C10 | 2.846 (3) | C16—H16A | 0.9300 |
| Tm1—Tm1i | 3.8506 (3) | C18—H18A | 0.9600 |
| N1—C31 | 1.321 (4) | C18—H18B | 0.9600 |
| N1—C42 | 1.363 (4) | C18—H18C | 0.9600 |
| O1—C2 | 1.367 (3) | C19—C20 | 1.514 (5) |
| O1—C1 | 1.430 (4) | C19—H19A | 0.9700 |
| C1—H1A | 0.9600 | C19—H19B | 0.9700 |
| C1—H1B | 0.9600 | C21—H21A | 0.9600 |
| C1—H1C | 0.9600 | C21—H21B | 0.9600 |
| O2—C7 | 1.367 (4) | C21—H21C | 0.9600 |
| O2—C8 | 1.410 (4) | C22—C27 | 1.379 (5) |
| N2—C40 | 1.314 (4) | C22—C23 | 1.392 (5) |
| N2—C41 | 1.363 (4) | C23—C24 | 1.378 (5) |
| C2—C3 | 1.365 (4) | C23—H23A | 0.9300 |
| C2—C7 | 1.404 (4) | C24—C25 | 1.377 (5) |
| O3—C10 | 1.280 (3) | C24—C29 | 1.523 (4) |
| O3—Tm1i | 2.2840 (18) | C25—C26 | 1.388 (5) |
| C3—C4 | 1.390 (4) | C25—H25A | 0.9300 |
| C3—H3A | 0.9300 | C26—C27 | 1.383 (5) |
| O4—C10 | 1.240 (4) | C26—H26A | 0.9300 |
| C4—C5 | 1.375 (4) | C28—H28A | 0.9600 |
| C4—H4A | 0.9300 | C28—H28B | 0.9600 |
| O5—C12 | 1.374 (4) | C28—H28C | 0.9600 |
| O5—C11 | 1.403 (5) | C29—C30 | 1.517 (4) |
| C5—C6 | 1.387 (4) | C29—H29A | 0.9700 |
| C5—C9 | 1.511 (4) | C29—H29B | 0.9700 |
| C6—C7 | 1.376 (4) | C31—C32 | 1.398 (4) |
| C6—H6A | 0.9300 | C31—H31A | 0.9300 |
| O6—C17 | 1.362 (4) | C32—C33 | 1.361 (5) |
| O6—C18 | 1.425 (5) | C32—H32A | 0.9300 |
| O7—C20 | 1.242 (4) | C33—C34 | 1.378 (5) |
| O8—C20 | 1.264 (4) | C33—H33A | 0.9300 |
| C8—H8A | 0.9600 | C34—C42 | 1.418 (4) |
| C8—H8B | 0.9600 | C34—C35 | 1.436 (5) |
| C8—H8C | 0.9600 | C35—C36 | 1.333 (6) |
| C9—C10 | 1.500 (5) | C35—H35A | 0.9300 |
| C9—H9A | 0.9700 | C36—C37 | 1.430 (6) |
| C9—H9B | 0.9700 | C36—H36A | 0.9300 |
| O9—C22 | 1.380 (4) | C37—C38 | 1.388 (6) |
| O9—C21 | 1.381 (5) | C37—C41 | 1.414 (4) |
| O10—C27 | 1.367 (4) | C38—C39 | 1.356 (6) |
| O10—C28 | 1.415 (5) | C38—H38A | 0.9300 |
| O11—C30 | 1.259 (4) | C39—C40 | 1.404 (5) |
| C11—H11C | 0.9600 | C39—H39A | 0.9300 |
| C11—H11D | 0.9600 | C40—H40A | 0.9300 |
| C11—H11A | 0.9600 | C41—C42 | 1.419 (5) |
| C12—C13 | 1.359 (5) | ||
| O3i—Tm1—O12i | 75.69 (7) | O3—C10—Tm1 | 61.27 (16) |
| O3i—Tm1—O11 | 76.05 (7) | C9—C10—Tm1 | 178.2 (2) |
| O12i—Tm1—O11 | 138.51 (8) | C27—O10—C28 | 117.0 (3) |
| O3i—Tm1—O8 | 89.39 (8) | C30—O11—Tm1 | 135.28 (19) |
| O12i—Tm1—O8 | 79.23 (8) | O5—C11—H11C | 109.5 |
| O11—Tm1—O8 | 129.97 (7) | O5—C11—H11D | 109.5 |
| O3i—Tm1—O7 | 74.97 (7) | H11C—C11—H11D | 109.5 |
| O12i—Tm1—O7 | 124.10 (7) | O5—C11—H11A | 109.5 |
| O11—Tm1—O7 | 75.85 (8) | H11C—C11—H11A | 109.5 |
| O8—Tm1—O7 | 54.12 (8) | H11D—C11—H11A | 109.5 |
| O3i—Tm1—O4 | 124.40 (7) | C13—C12—O5 | 125.5 (3) |
| O12i—Tm1—O4 | 93.43 (7) | C13—C12—C17 | 119.9 (3) |
| O11—Tm1—O4 | 78.36 (7) | O5—C12—C17 | 114.6 (3) |
| O8—Tm1—O4 | 142.79 (8) | C30—O12—Tm1i | 137.4 (2) |
| O7—Tm1—O4 | 142.18 (7) | C12—C13—C14 | 120.4 (3) |
| O3i—Tm1—O3 | 72.78 (7) | C12—C13—H13A | 119.8 |
| O12i—Tm1—O3 | 71.47 (8) | C14—C13—H13A | 119.8 |
| O11—Tm1—O3 | 71.52 (7) | C15—C14—C13 | 120.3 (3) |
| O8—Tm1—O3 | 148.56 (7) | C15—C14—H14A | 119.9 |
| O7—Tm1—O3 | 138.45 (7) | C13—C14—H14A | 119.9 |
| O4—Tm1—O3 | 52.42 (6) | C16—C15—C14 | 118.7 (3) |
| O3i—Tm1—N2 | 141.43 (8) | C16—C15—C19 | 120.3 (3) |
| O12i—Tm1—N2 | 139.68 (8) | C14—C15—C19 | 121.0 (3) |
| O11—Tm1—N2 | 78.56 (8) | C17—C16—C15 | 121.5 (3) |
| O8—Tm1—N2 | 85.13 (8) | C17—C16—H16A | 119.2 |
| O7—Tm1—N2 | 70.97 (7) | C15—C16—H16A | 119.2 |
| O4—Tm1—N2 | 77.18 (8) | O6—C17—C16 | 125.2 (3) |
| O3—Tm1—N2 | 124.89 (7) | O6—C17—C12 | 115.6 (3) |
| O3i—Tm1—N1 | 149.64 (8) | C16—C17—C12 | 119.2 (3) |
| O12i—Tm1—N1 | 75.49 (8) | O6—C18—H18A | 109.5 |
| O11—Tm1—N1 | 133.46 (7) | O6—C18—H18B | 109.5 |
| O8—Tm1—N1 | 76.06 (8) | H18A—C18—H18B | 109.5 |
| O7—Tm1—N1 | 114.57 (8) | O6—C18—H18C | 109.5 |
| O4—Tm1—N1 | 66.81 (8) | H18A—C18—H18C | 109.5 |
| O3—Tm1—N1 | 106.50 (7) | H18B—C18—H18C | 109.5 |
| N2—Tm1—N1 | 64.71 (9) | C15—C19—C20 | 114.9 (3) |
| O3i—Tm1—C20 | 81.95 (8) | C15—C19—H19A | 108.5 |
| O12i—Tm1—C20 | 102.70 (9) | C20—C19—H19A | 108.5 |
| O11—Tm1—C20 | 102.70 (9) | C15—C19—H19B | 108.5 |
| O8—Tm1—C20 | 27.28 (9) | C20—C19—H19B | 108.5 |
| O7—Tm1—C20 | 26.86 (8) | H19A—C19—H19B | 107.5 |
| O4—Tm1—C20 | 152.20 (8) | O7—C20—O8 | 121.0 (3) |
| O3—Tm1—C20 | 154.73 (7) | O7—C20—C19 | 121.7 (3) |
| N2—Tm1—C20 | 75.87 (8) | O8—C20—C19 | 117.3 (3) |
| N1—Tm1—C20 | 95.26 (9) | O7—C20—Tm1 | 62.72 (17) |
| O3i—Tm1—C10 | 99.16 (8) | O8—C20—Tm1 | 58.36 (17) |
| O12i—Tm1—C10 | 81.72 (8) | C19—C20—Tm1 | 175.2 (3) |
| O11—Tm1—C10 | 73.53 (8) | O9—C21—H21A | 109.5 |
| O8—Tm1—C10 | 156.48 (8) | O9—C21—H21B | 109.5 |
| O7—Tm1—C10 | 149.32 (8) | H21A—C21—H21B | 109.5 |
| O4—Tm1—C10 | 25.70 (7) | O9—C21—H21C | 109.5 |
| O3—Tm1—C10 | 26.72 (7) | H21A—C21—H21C | 109.5 |
| N2—Tm1—C10 | 100.89 (8) | H21B—C21—H21C | 109.5 |
| N1—Tm1—C10 | 85.93 (8) | C27—C22—O9 | 114.8 (3) |
| C20—Tm1—C10 | 175.58 (9) | C27—C22—C23 | 119.8 (3) |
| O3i—Tm1—Tm1i | 38.27 (5) | O9—C22—C23 | 125.4 (4) |
| O12i—Tm1—Tm1i | 69.35 (5) | C24—C23—C22 | 121.2 (4) |
| O11—Tm1—Tm1i | 69.60 (5) | C24—C23—H23A | 119.4 |
| O8—Tm1—Tm1i | 123.15 (6) | C22—C23—H23A | 119.4 |
| O7—Tm1—Tm1i | 109.36 (5) | C25—C24—C23 | 118.5 (3) |
| O4—Tm1—Tm1i | 86.54 (5) | C25—C24—C29 | 120.0 (3) |
| O3—Tm1—Tm1i | 34.51 (4) | C23—C24—C29 | 121.5 (3) |
| N2—Tm1—Tm1i | 146.58 (7) | C24—C25—C26 | 121.1 (3) |
| N1—Tm1—Tm1i | 134.10 (6) | C24—C25—H25A | 119.4 |
| C20—Tm1—Tm1i | 120.22 (6) | C26—C25—H25A | 119.4 |
| C10—Tm1—Tm1i | 61.01 (6) | C27—C26—C25 | 119.9 (4) |
| C31—N1—C42 | 117.6 (3) | C27—C26—H26A | 120.0 |
| C31—N1—Tm1 | 124.5 (2) | C25—C26—H26A | 120.0 |
| C42—N1—Tm1 | 117.2 (2) | O10—C27—C22 | 116.6 (3) |
| C2—O1—C1 | 116.1 (2) | O10—C27—C26 | 123.9 (4) |
| O1—C1—H1A | 109.5 | C22—C27—C26 | 119.5 (3) |
| O1—C1—H1B | 109.5 | O10—C28—H28A | 109.5 |
| H1A—C1—H1B | 109.5 | O10—C28—H28B | 109.5 |
| O1—C1—H1C | 109.5 | H28A—C28—H28B | 109.5 |
| H1A—C1—H1C | 109.5 | O10—C28—H28C | 109.5 |
| H1B—C1—H1C | 109.5 | H28A—C28—H28C | 109.5 |
| C7—O2—C8 | 117.0 (3) | H28B—C28—H28C | 109.5 |
| C40—N2—C41 | 118.4 (3) | C30—C29—C24 | 110.6 (3) |
| C40—N2—Tm1 | 121.5 (2) | C30—C29—H29A | 109.5 |
| C41—N2—Tm1 | 120.0 (2) | C24—C29—H29A | 109.5 |
| C3—C2—O1 | 124.8 (3) | C30—C29—H29B | 109.5 |
| C3—C2—C7 | 118.9 (3) | C24—C29—H29B | 109.5 |
| O1—C2—C7 | 116.4 (3) | H29A—C29—H29B | 108.1 |
| C10—O3—Tm1i | 158.6 (2) | O12—C30—O11 | 125.8 (3) |
| C10—O3—Tm1 | 92.01 (18) | O12—C30—C29 | 116.7 (3) |
| Tm1i—O3—Tm1 | 107.22 (7) | O11—C30—C29 | 117.4 (3) |
| C2—C3—C4 | 120.2 (3) | N1—C31—C32 | 123.9 (3) |
| C2—C3—H3A | 119.9 | N1—C31—H31A | 118.0 |
| C4—C3—H3A | 119.9 | C32—C31—H31A | 118.0 |
| C10—O4—Tm1 | 95.47 (17) | C33—C32—C31 | 118.4 (4) |
| C5—C4—C3 | 121.8 (3) | C33—C32—H32A | 120.8 |
| C5—C4—H4A | 119.1 | C31—C32—H32A | 120.8 |
| C3—C4—H4A | 119.1 | C32—C33—C34 | 120.3 (3) |
| C12—O5—C11 | 117.8 (3) | C32—C33—H33A | 119.9 |
| C4—C5—C6 | 117.4 (3) | C34—C33—H33A | 119.9 |
| C4—C5—C9 | 121.0 (3) | C33—C34—C42 | 118.1 (3) |
| C6—C5—C9 | 121.5 (3) | C33—C34—C35 | 123.7 (4) |
| C7—C6—C5 | 121.7 (3) | C42—C34—C35 | 118.2 (4) |
| C7—C6—H6A | 119.2 | C36—C35—C34 | 121.5 (4) |
| C5—C6—H6A | 119.2 | C36—C35—H35A | 119.2 |
| C17—O6—C18 | 118.0 (3) | C34—C35—H35A | 119.2 |
| C20—O7—Tm1 | 90.42 (18) | C35—C36—C37 | 121.8 (3) |
| O2—C7—C6 | 125.3 (3) | C35—C36—H36A | 119.1 |
| O2—C7—C2 | 114.9 (3) | C37—C36—H36A | 119.1 |
| C6—C7—C2 | 119.8 (3) | C38—C37—C41 | 118.3 (3) |
| C20—O8—Tm1 | 94.4 (2) | C38—C37—C36 | 123.4 (3) |
| O2—C8—H8A | 109.5 | C41—C37—C36 | 118.3 (4) |
| O2—C8—H8B | 109.5 | C39—C38—C37 | 119.8 (3) |
| H8A—C8—H8B | 109.5 | C39—C38—H38A | 120.1 |
| O2—C8—H8C | 109.5 | C37—C38—H38A | 120.1 |
| H8A—C8—H8C | 109.5 | C38—C39—C40 | 118.9 (4) |
| H8B—C8—H8C | 109.5 | C38—C39—H39A | 120.6 |
| C10—C9—C5 | 118.0 (3) | C40—C39—H39A | 120.6 |
| C10—C9—H9A | 107.8 | N2—C40—C39 | 123.2 (4) |
| C5—C9—H9A | 107.8 | N2—C40—H40A | 118.4 |
| C10—C9—H9B | 107.8 | C39—C40—H40A | 118.4 |
| C5—C9—H9B | 107.8 | N2—C41—C37 | 121.3 (3) |
| H9A—C9—H9B | 107.1 | N2—C41—C42 | 118.6 (3) |
| C22—O9—C21 | 118.6 (4) | C37—C41—C42 | 120.1 (3) |
| O4—C10—O3 | 120.1 (3) | N1—C42—C34 | 121.7 (3) |
| O4—C10—C9 | 122.9 (3) | N1—C42—C41 | 118.4 (3) |
| O3—C10—C9 | 117.0 (3) | C34—C42—C41 | 119.9 (3) |
| O4—C10—Tm1 | 58.82 (15) | ||
| O3i—Tm1—N1—C31 | 25.7 (3) | N2—Tm1—C10—O4 | 23.0 (2) |
| O12i—Tm1—N1—C31 | 6.9 (2) | N1—Tm1—C10—O4 | −40.31 (18) |
| O11—Tm1—N1—C31 | −138.2 (2) | Tm1i—Tm1—C10—O4 | 172.9 (2) |
| O8—Tm1—N1—C31 | 89.2 (3) | O3i—Tm1—C10—O3 | −9.1 (2) |
| O7—Tm1—N1—C31 | 128.1 (2) | O12i—Tm1—C10—O3 | 64.85 (16) |
| O4—Tm1—N1—C31 | −93.3 (3) | O11—Tm1—C10—O3 | −81.50 (16) |
| O3—Tm1—N1—C31 | −58.3 (3) | O8—Tm1—C10—O3 | 101.0 (2) |
| N2—Tm1—N1—C31 | −179.6 (3) | O7—Tm1—C10—O3 | −85.0 (2) |
| C20—Tm1—N1—C31 | 108.7 (3) | O4—Tm1—C10—O3 | −178.9 (3) |
| C10—Tm1—N1—C31 | −75.6 (3) | N2—Tm1—C10—O3 | −155.98 (16) |
| Tm1i—Tm1—N1—C31 | −33.8 (3) | N1—Tm1—C10—O3 | 140.75 (17) |
| O3i—Tm1—N1—C42 | −163.31 (18) | Tm1i—Tm1—C10—O3 | −6.08 (13) |
| O12i—Tm1—N1—C42 | 178.0 (2) | O3i—Tm1—O11—C30 | −22.7 (3) |
| O11—Tm1—N1—C42 | 32.8 (2) | O12i—Tm1—O11—C30 | 25.6 (3) |
| O8—Tm1—N1—C42 | −99.8 (2) | O8—Tm1—O11—C30 | −99.8 (3) |
| O7—Tm1—N1—C42 | −60.8 (2) | O7—Tm1—O11—C30 | −100.4 (3) |
| O4—Tm1—N1—C42 | 77.7 (2) | O4—Tm1—O11—C30 | 107.5 (3) |
| O3—Tm1—N1—C42 | 112.7 (2) | O3—Tm1—O11—C30 | 53.5 (3) |
| N2—Tm1—N1—C42 | −8.6 (2) | N2—Tm1—O11—C30 | −173.4 (3) |
| C20—Tm1—N1—C42 | −80.3 (2) | N1—Tm1—O11—C30 | 149.0 (3) |
| C10—Tm1—N1—C42 | 95.5 (2) | C20—Tm1—O11—C30 | −100.9 (3) |
| Tm1i—Tm1—N1—C42 | 137.26 (18) | C10—Tm1—O11—C30 | 81.5 (3) |
| O3i—Tm1—N2—C40 | −16.0 (3) | Tm1i—Tm1—O11—C30 | 16.9 (3) |
| O12i—Tm1—N2—C40 | −165.9 (2) | C11—O5—C12—C13 | −5.0 (6) |
| O11—Tm1—N2—C40 | 33.5 (3) | C11—O5—C12—C17 | 174.0 (4) |
| O8—Tm1—N2—C40 | −98.9 (3) | O5—C12—C13—C14 | 178.4 (4) |
| O7—Tm1—N2—C40 | −45.3 (3) | C17—C12—C13—C14 | −0.7 (6) |
| O4—Tm1—N2—C40 | 114.0 (3) | C12—C13—C14—C15 | 0.1 (6) |
| O3—Tm1—N2—C40 | 91.2 (3) | C13—C14—C15—C16 | 1.0 (6) |
| N1—Tm1—N2—C40 | −175.8 (3) | C13—C14—C15—C19 | 179.3 (3) |
| C20—Tm1—N2—C40 | −72.9 (3) | C14—C15—C16—C17 | −1.6 (5) |
| C10—Tm1—N2—C40 | 104.1 (3) | C19—C15—C16—C17 | −179.9 (3) |
| Tm1i—Tm1—N2—C40 | 51.3 (3) | C18—O6—C17—C16 | −7.7 (6) |
| O3i—Tm1—N2—C41 | 167.8 (2) | C18—O6—C17—C12 | 172.8 (4) |
| O12i—Tm1—N2—C41 | 17.9 (3) | C15—C16—C17—O6 | −178.4 (3) |
| O11—Tm1—N2—C41 | −142.6 (2) | C15—C16—C17—C12 | 1.1 (5) |
| O8—Tm1—N2—C41 | 84.9 (2) | C13—C12—C17—O6 | 179.7 (3) |
| O7—Tm1—N2—C41 | 138.5 (2) | O5—C12—C17—O6 | 0.5 (5) |
| O4—Tm1—N2—C41 | −62.1 (2) | C13—C12—C17—C16 | 0.1 (6) |
| O3—Tm1—N2—C41 | −85.0 (2) | O5—C12—C17—C16 | −179.1 (3) |
| N1—Tm1—N2—C41 | 8.0 (2) | C16—C15—C19—C20 | 102.8 (4) |
| C20—Tm1—N2—C41 | 111.0 (2) | C14—C15—C19—C20 | −75.4 (4) |
| C10—Tm1—N2—C41 | −72.1 (2) | Tm1—O7—C20—O8 | −3.0 (3) |
| Tm1i—Tm1—N2—C41 | −124.9 (2) | Tm1—O7—C20—C19 | 177.8 (3) |
| C1—O1—C2—C3 | −17.4 (4) | Tm1—O8—C20—O7 | 3.1 (3) |
| C1—O1—C2—C7 | 163.7 (3) | Tm1—O8—C20—C19 | −177.6 (2) |
| O3i—Tm1—O3—C10 | 170.6 (2) | C15—C19—C20—O8 | −171.4 (3) |
| O12i—Tm1—O3—C10 | −109.14 (17) | O3i—Tm1—C20—O7 | −72.51 (16) |
| O11—Tm1—O3—C10 | 89.95 (17) | O12i—Tm1—C20—O7 | −145.79 (16) |
| O8—Tm1—O3—C10 | −131.31 (18) | O11—Tm1—C20—O7 | 1.14 (17) |
| O7—Tm1—O3—C10 | 129.97 (17) | O8—Tm1—C20—O7 | −177.0 (3) |
| O4—Tm1—O3—C10 | 0.58 (16) | O4—Tm1—C20—O7 | 90.2 (2) |
| N2—Tm1—O3—C10 | 29.2 (2) | O3—Tm1—C20—O7 | −72.4 (3) |
| N1—Tm1—O3—C10 | −41.16 (17) | N2—Tm1—C20—O7 | 75.68 (17) |
| C20—Tm1—O3—C10 | 170.5 (2) | N1—Tm1—C20—O7 | 137.93 (16) |
| Tm1i—Tm1—O3—C10 | 170.6 (2) | Tm1i—Tm1—C20—O7 | −72.47 (17) |
| O3i—Tm1—O3—Tm1i | 0.0 | O3i—Tm1—C20—O8 | 104.51 (17) |
| O12i—Tm1—O3—Tm1i | 80.27 (8) | O12i—Tm1—C20—O8 | 31.24 (18) |
| O11—Tm1—O3—Tm1i | −80.64 (8) | O11—Tm1—C20—O8 | 178.16 (16) |
| O8—Tm1—O3—Tm1i | 58.10 (16) | O7—Tm1—C20—O8 | 177.0 (3) |
| O7—Tm1—O3—Tm1i | −40.62 (13) | O4—Tm1—C20—O8 | −92.7 (2) |
| O4—Tm1—O3—Tm1i | −170.01 (13) | O3—Tm1—C20—O8 | 104.6 (2) |
| N2—Tm1—O3—Tm1i | −141.43 (9) | N2—Tm1—C20—O8 | −107.29 (18) |
| N1—Tm1—O3—Tm1i | 148.25 (9) | N1—Tm1—C20—O8 | −45.04 (18) |
| C20—Tm1—O3—Tm1i | −0.1 (2) | Tm1i—Tm1—C20—O8 | 104.56 (17) |
| C10—Tm1—O3—Tm1i | −170.6 (2) | C21—O9—C22—C27 | 173.0 (4) |
| O1—C2—C3—C4 | 178.1 (3) | C21—O9—C22—C23 | −7.0 (6) |
| C7—C2—C3—C4 | −3.1 (5) | C27—C22—C23—C24 | −0.2 (6) |
| O3i—Tm1—O4—C10 | −12.2 (2) | O9—C22—C23—C24 | 179.8 (4) |
| O12i—Tm1—O4—C10 | 62.79 (19) | C22—C23—C24—C25 | −0.3 (5) |
| O11—Tm1—O4—C10 | −76.13 (18) | C22—C23—C24—C29 | 179.9 (3) |
| O8—Tm1—O4—C10 | 139.46 (18) | C23—C24—C25—C26 | 0.1 (5) |
| O7—Tm1—O4—C10 | −123.88 (19) | C29—C24—C25—C26 | 179.9 (3) |
| O3—Tm1—O4—C10 | −0.60 (16) | C24—C25—C26—C27 | 0.6 (6) |
| N2—Tm1—O4—C10 | −156.9 (2) | C28—O10—C27—C22 | −178.8 (4) |
| N1—Tm1—O4—C10 | 135.4 (2) | C28—O10—C27—C26 | 0.1 (6) |
| C20—Tm1—O4—C10 | −171.3 (2) | O9—C22—C27—O10 | −0.2 (5) |
| Tm1i—Tm1—O4—C10 | −6.26 (18) | C23—C22—C27—O10 | 179.8 (3) |
| C2—C3—C4—C5 | −1.3 (5) | O9—C22—C27—C26 | −179.1 (4) |
| C3—C4—C5—C6 | 4.3 (5) | C23—C22—C27—C26 | 0.9 (6) |
| C3—C4—C5—C9 | −172.3 (3) | C25—C26—C27—O10 | −179.9 (4) |
| C4—C5—C6—C7 | −3.0 (5) | C25—C26—C27—C22 | −1.1 (6) |
| C9—C5—C6—C7 | 173.6 (3) | C25—C24—C29—C30 | 48.9 (4) |
| O3i—Tm1—O7—C20 | 102.08 (17) | C23—C24—C29—C30 | −131.3 (3) |
| O12i—Tm1—O7—C20 | 41.48 (19) | Tm1i—O12—C30—O11 | 8.3 (5) |
| O11—Tm1—O7—C20 | −178.85 (17) | Tm1i—O12—C30—C29 | −169.3 (2) |
| O8—Tm1—O7—C20 | 1.68 (16) | Tm1—O11—C30—O12 | −22.4 (5) |
| O4—Tm1—O7—C20 | −130.47 (17) | Tm1—O11—C30—C29 | 155.2 (2) |
| O3—Tm1—O7—C20 | 142.17 (16) | C24—C29—C30—O12 | 74.1 (4) |
| N2—Tm1—O7—C20 | −96.29 (18) | C24—C29—C30—O11 | −103.7 (3) |
| N1—Tm1—O7—C20 | −47.19 (18) | C42—N1—C31—C32 | 0.9 (5) |
| C10—Tm1—O7—C20 | −175.35 (16) | Tm1—N1—C31—C32 | 171.9 (3) |
| Tm1i—Tm1—O7—C20 | 119.15 (16) | N1—C31—C32—C33 | −1.5 (6) |
| C8—O2—C7—C6 | −12.4 (5) | C31—C32—C33—C34 | 0.4 (5) |
| C8—O2—C7—C2 | 168.0 (3) | C32—C33—C34—C42 | 1.0 (5) |
| C5—C6—C7—O2 | 179.1 (3) | C32—C33—C34—C35 | −179.0 (3) |
| C5—C6—C7—C2 | −1.2 (5) | C33—C34—C35—C36 | −177.3 (4) |
| C3—C2—C7—O2 | −176.0 (3) | C42—C34—C35—C36 | 2.7 (6) |
| O1—C2—C7—O2 | 2.9 (4) | C34—C35—C36—C37 | −0.4 (6) |
| C3—C2—C7—C6 | 4.3 (4) | C35—C36—C37—C38 | 178.0 (4) |
| O1—C2—C7—C6 | −176.8 (3) | C35—C36—C37—C41 | −3.0 (6) |
| O3i—Tm1—O8—C20 | −73.46 (17) | C41—C37—C38—C39 | −0.1 (5) |
| O12i—Tm1—O8—C20 | −149.01 (18) | C36—C37—C38—C39 | 178.8 (4) |
| O11—Tm1—O8—C20 | −2.3 (2) | C37—C38—C39—C40 | −2.1 (6) |
| O7—Tm1—O8—C20 | −1.66 (16) | C41—N2—C40—C39 | 0.7 (5) |
| O4—Tm1—O8—C20 | 129.61 (17) | Tm1—N2—C40—C39 | −175.5 (3) |
| O3—Tm1—O8—C20 | −127.64 (18) | C38—C39—C40—N2 | 1.9 (6) |
| N2—Tm1—O8—C20 | 68.32 (18) | C40—N2—C41—C37 | −3.0 (5) |
| N1—Tm1—O8—C20 | 133.45 (18) | Tm1—N2—C41—C37 | 173.2 (2) |
| C10—Tm1—O8—C20 | 174.55 (18) | C40—N2—C41—C42 | 176.6 (3) |
| Tm1i—Tm1—O8—C20 | −92.58 (17) | Tm1—N2—C41—C42 | −7.1 (4) |
| C4—C5—C9—C10 | −128.0 (4) | C38—C37—C41—N2 | 2.8 (5) |
| C6—C5—C9—C10 | 55.6 (5) | C36—C37—C41—N2 | −176.2 (3) |
| Tm1—O4—C10—O3 | 1.1 (3) | C38—C37—C41—C42 | −176.8 (3) |
| Tm1—O4—C10—C9 | −179.4 (3) | C36—C37—C41—C42 | 4.1 (5) |
| Tm1i—O3—C10—O4 | 153.6 (4) | C31—N1—C42—C34 | 0.6 (4) |
| Tm1—O3—C10—O4 | −1.1 (3) | Tm1—N1—C42—C34 | −171.0 (2) |
| Tm1i—O3—C10—C9 | −26.0 (7) | C31—N1—C42—C41 | −179.5 (3) |
| Tm1—O3—C10—C9 | 179.4 (3) | Tm1—N1—C42—C41 | 8.9 (4) |
| Tm1i—O3—C10—Tm1 | 154.6 (5) | C33—C34—C42—N1 | −1.6 (5) |
| C5—C9—C10—O4 | 9.4 (5) | C35—C34—C42—N1 | 178.4 (3) |
| C5—C9—C10—O3 | −171.1 (3) | C33—C34—C42—C41 | 178.5 (3) |
| O3i—Tm1—C10—O4 | 169.83 (18) | C35—C34—C42—C41 | −1.5 (5) |
| O12i—Tm1—C10—O4 | −116.22 (19) | N2—C41—C42—N1 | −1.5 (4) |
| O11—Tm1—C10—O4 | 97.43 (18) | C37—C41—C42—N1 | 178.2 (3) |
| O8—Tm1—C10—O4 | −80.1 (3) | N2—C41—C42—C34 | 178.4 (3) |
| O7—Tm1—C10—O4 | 93.9 (2) | C37—C41—C42—C34 | −1.9 (5) |
| O3—Tm1—C10—O4 | 178.9 (3) |
Symmetry codes: (i) −x, −y, −z.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH2956).
References
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809051435/lh2956sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536809051435/lh2956Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report

