metal-organic compounds
Bis[μ-2-(4-hydroxyphenyl)acetato]-κ3O,O′:O;κ3O:O,O′-bis{aqua(4,4′-bipyridine-κN)[2-(4-hydroxyphenyl)acetato-κ2O,O′]samarium(III)} monohydrate
aCollege of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004, People's Republic of China, and Zhejiang Normal University Xingzhi College, Jinhua 321004, People's Republic of China
*Correspondence e-mail: sky53@zjnu.cn
The dinuclear title complex, [Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O, contains two SmIII atoms, six deprotonated p-hydroxyphenylacetic acid (PAA) molecules, two 4,4′-bipyridine (bipy) molecules, two coordinated water molecules and one solvent water molecule. Each SmIIIion is nine-coordinated by seven O atoms from four PAA ligands, one water O atom and one N atom from a bipy ligand in a distorted geometry. The PAA ligands are coordinated to the SmIII ion in bridging and bridging tridentate modes. The also contains one uncoordinated water molecule. The occurrence of numerous O—H⋯O and O—H⋯N hydrogen bonds involving coordinated and non-coordinated water molecules builds up an intricate three-dimensional network.
Related literature
For related structures, see: Arias et al. (2000); Liu et al. (2010). For applications of carboxylic metal-organic complexes, see: Wang & Sevov (2008); Wang et al. (2010); Fang & Zhang (2006).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2006); cell SAINT (Bruker, 2006); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.
Supporting information
https://doi.org/10.1107/S1600536810044454/kj2162sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810044454/kj2162Isup2.hkl
All reagents and solvents used were of commercially available quality and were used without prior purification. p-hydroxyphenylacetic acid(HPAA) (0.456 g, 3 mmol) and sodium hydroxide (0.12 g, 3 mmol) were mixed together in water (10 ml). Sm(NO3)3 (0.336 g, 1 mmol), dissolved in water (10 ml), was added into the first solution. After stirring for an hour, an ethanol (5 ml) solution of 4,4'-bipyridine (0.156 g, 1 mmol) was slowly dripped into the mixture, followed by three hours stirring. After filtration, the filtrate was allowed to stand at room temperature and single crystals suitable for X–ray diffraction were obtained after a week.
All H atoms attached to C atoms and O(hydroxyl) atom were fixed geometrically and treated as riding with C—H = 0.97 Å (methylene) or 0.93 Å (aromatic) and O—H = 0.82 Å with Uiso(H) = 1.2Ueq(C) or Uiso(H) = 1.5Ueq(O). H atoms of water molecule were located in a difference Fourier map and included in the subsequent
using restraints (O—H= 0.82 (1)Å and H···H= 1.39 (2) Å) with Uiso(H) = 1.5Ueq(O). In the last cycles of they were treated as riding on their parent O atom.The design and synthesis of carboxylic metal-organic complexes have been an increasing interest for decades owing to their potential practical applications, such as fluorescence and magnetism (Wang, et al., 2010; Fang et al., 2006; Wang, et al., 2008). We have published on this subject before (Liu, et al., 2010). In the current paper we report the
of a new SmIII complex with the ligand p- hydroxyphenylacetic acid. The title compound consist of six L ligands, two bipy molecules and two coordinated water molecules. In the dinuclear compound, each Sm ion is coordinated with seven O atoms from four L ligands, one N atom from 4,4'-bipyridine ligand and one O atom from a water molecule. The central Sm atom is nine coordinated. The PAA ligands are coordinating in two modes, bridging and bridging tridentate. (Fig.1). The SmIII ion is in a distorted ball coordination geometry. The further contains one solvent water molecule. Bond lengths and bond angles involving the metals and O atoms skeleton compare well with related structure as bis((µ2-Acetato-O,O,O')-diaqua-bis(acetato-O,O') -samarium(iii))pentahydrate (Arias, et al., 2000), In addition, numerous O—H···O bonds involving both hydroxyl groups as well as coordinated and non-coordinated water molecules build up an intricate threedimensional network (Table 1).For related structures, see: Arias et al. (2000); Liu et al. (2010). For applications of carboxylic metal-organic complexes, see: Wang & Sevov (2008); Wang et al. (2010); Fang & Zhang (2006).
Data collection: APEX2 (Bruker, 2006); cell
SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. The molecular structure of the title complex, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. |
[Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O | Z = 2 |
Mr = 1573.96 | F(000) = 1584 |
Triclinic, P1 | Dx = 1.642 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.7589 (3) Å | Cell parameters from 9956 reflections |
b = 16.3141 (4) Å | θ = 1.7–27.7° |
c = 18.4618 (5) Å | µ = 1.91 mm−1 |
α = 83.619 (1)° | T = 296 K |
β = 72.025 (1)° | Block, colourless |
γ = 70.941 (1)° | 0.34 × 0.14 × 0.03 mm |
V = 3183.90 (14) Å3 |
Bruker APEXII area-detector diffractometer | 14715 independent reflections |
Radiation source: fine-focus sealed tube | 11851 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
phi and ω scans | θmax = 27.7°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.733, Tmax = 0.941 | k = −21→21 |
49293 measured reflections | l = −24→24 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.070 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0236P)2 + 0.993P] where P = (Fo2 + 2Fc2)/3 |
14715 reflections | (Δ/σ)max = 0.002 |
875 parameters | Δρmax = 0.66 e Å−3 |
9 restraints | Δρmin = −0.72 e Å−3 |
[Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O | γ = 70.941 (1)° |
Mr = 1573.96 | V = 3183.90 (14) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.7589 (3) Å | Mo Kα radiation |
b = 16.3141 (4) Å | µ = 1.91 mm−1 |
c = 18.4618 (5) Å | T = 296 K |
α = 83.619 (1)° | 0.34 × 0.14 × 0.03 mm |
β = 72.025 (1)° |
Bruker APEXII area-detector diffractometer | 14715 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 11851 reflections with I > 2σ(I) |
Tmin = 0.733, Tmax = 0.941 | Rint = 0.047 |
49293 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 9 restraints |
wR(F2) = 0.070 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 0.66 e Å−3 |
14715 reflections | Δρmin = −0.72 e Å−3 |
875 parameters |
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 | ||
Sm1 | 0.271174 (13) | 0.364512 (8) | 0.283786 (7) | 0.02579 (4) | |
Sm2 | 0.131899 (13) | 0.206492 (8) | 0.195381 (7) | 0.02577 (4) | |
N1 | 0.3136 (2) | 0.51130 (14) | 0.28289 (14) | 0.0359 (6) | |
N2 | 0.3976 (3) | 0.92617 (19) | 0.2162 (2) | 0.0667 (10) | |
N3 | 0.0840 (2) | 0.06204 (14) | 0.18856 (13) | 0.0337 (5) | |
N4 | 0.0282 (4) | −0.36185 (19) | 0.2326 (2) | 0.0683 (10) | |
C1 | 0.2248 (3) | 0.51101 (19) | 0.51768 (16) | 0.0363 (7) | |
C2 | 0.3403 (3) | 0.5160 (2) | 0.47296 (17) | 0.0458 (8) | |
H2A | 0.3962 | 0.4689 | 0.4433 | 0.055* | |
C3 | 0.3750 (3) | 0.5896 (2) | 0.47116 (19) | 0.0505 (8) | |
H3A | 0.4533 | 0.5918 | 0.4404 | 0.061* | |
C4 | 0.2940 (3) | 0.6592 (2) | 0.51481 (19) | 0.0449 (8) | |
C5 | 0.1799 (3) | 0.6549 (2) | 0.56137 (19) | 0.0482 (8) | |
H5A | 0.1261 | 0.7013 | 0.5926 | 0.058* | |
C6 | 0.1449 (3) | 0.5823 (2) | 0.56210 (18) | 0.0445 (8) | |
H6A | 0.0664 | 0.5808 | 0.5929 | 0.053* | |
C7 | 0.1855 (3) | 0.4307 (2) | 0.52126 (16) | 0.0429 (8) | |
H7A | 0.2316 | 0.3855 | 0.5497 | 0.052* | |
H7B | 0.0967 | 0.4440 | 0.5481 | 0.052* | |
C8 | 0.2096 (3) | 0.39816 (19) | 0.44318 (16) | 0.0355 (7) | |
C9 | 0.6232 (3) | 0.08807 (18) | 0.30336 (18) | 0.0378 (7) | |
C10 | 0.6052 (3) | 0.0570 (2) | 0.37691 (18) | 0.0492 (8) | |
H10A | 0.5938 | 0.0937 | 0.4154 | 0.059* | |
C11 | 0.6033 (3) | −0.0276 (2) | 0.39568 (18) | 0.0494 (8) | |
H11A | 0.5911 | −0.0472 | 0.4459 | 0.059* | |
C12 | 0.6199 (3) | −0.08171 (18) | 0.33913 (17) | 0.0394 (7) | |
C13 | 0.6364 (3) | −0.0518 (2) | 0.26524 (17) | 0.0438 (8) | |
H13A | 0.6459 | −0.0882 | 0.2270 | 0.053* | |
C14 | 0.6389 (3) | 0.03153 (19) | 0.24766 (17) | 0.0432 (7) | |
H14A | 0.6515 | 0.0506 | 0.1973 | 0.052* | |
C15 | 0.6269 (3) | 0.17940 (19) | 0.2834 (2) | 0.0478 (8) | |
H15A | 0.6939 | 0.1783 | 0.2367 | 0.057* | |
H15B | 0.6475 | 0.2005 | 0.3233 | 0.057* | |
C16 | 0.5063 (3) | 0.24269 (17) | 0.27316 (16) | 0.0331 (6) | |
C17 | 0.2720 (3) | 0.4547 (2) | 0.01289 (16) | 0.0424 (8) | |
C18 | 0.1461 (4) | 0.5016 (2) | 0.02779 (17) | 0.0497 (9) | |
H18A | 0.0861 | 0.4747 | 0.0537 | 0.060* | |
C19 | 0.1070 (3) | 0.5873 (2) | 0.00524 (17) | 0.0453 (8) | |
H19A | 0.0218 | 0.6177 | 0.0158 | 0.054* | |
C20 | 0.1963 (3) | 0.62750 (19) | −0.03339 (17) | 0.0405 (7) | |
C21 | 0.3219 (3) | 0.58206 (19) | −0.04820 (17) | 0.0415 (7) | |
H21A | 0.3820 | 0.6090 | −0.0737 | 0.050* | |
C22 | 0.3589 (3) | 0.4964 (2) | −0.02525 (17) | 0.0434 (7) | |
H22A | 0.4442 | 0.4662 | −0.0357 | 0.052* | |
C23 | 0.3132 (4) | 0.3613 (2) | 0.03920 (17) | 0.0587 (10) | |
H23A | 0.2587 | 0.3316 | 0.0315 | 0.070* | |
H23B | 0.3981 | 0.3328 | 0.0085 | 0.070* | |
C24 | 0.3094 (3) | 0.35389 (17) | 0.12169 (15) | 0.0330 (6) | |
C25 | 0.1416 (3) | 0.11314 (19) | 0.47589 (16) | 0.0392 (7) | |
C26 | 0.0393 (3) | 0.1063 (2) | 0.53593 (17) | 0.0434 (7) | |
H26A | −0.0293 | 0.1554 | 0.5521 | 0.052* | |
C27 | 0.0378 (3) | 0.0273 (2) | 0.57213 (17) | 0.0421 (7) | |
H27A | −0.0312 | 0.0238 | 0.6125 | 0.051* | |
C28 | 0.1382 (3) | −0.04551 (19) | 0.54821 (16) | 0.0359 (7) | |
C29 | 0.2418 (3) | −0.0397 (2) | 0.48932 (17) | 0.0437 (7) | |
H29A | 0.3106 | −0.0888 | 0.4735 | 0.052* | |
C30 | 0.2428 (3) | 0.0393 (2) | 0.45411 (17) | 0.0436 (8) | |
H30A | 0.3131 | 0.0429 | 0.4148 | 0.052* | |
C31 | 0.1430 (4) | 0.1978 (2) | 0.43418 (17) | 0.0461 (8) | |
H31A | 0.2238 | 0.2058 | 0.4274 | 0.055* | |
H31B | 0.0791 | 0.2446 | 0.4657 | 0.055* | |
C32 | 0.1204 (3) | 0.20483 (17) | 0.35761 (15) | 0.0311 (6) | |
C33 | −0.2564 (3) | 0.48057 (17) | 0.24478 (16) | 0.0322 (6) | |
C34 | −0.2139 (3) | 0.51863 (19) | 0.17454 (17) | 0.0400 (7) | |
H34A | −0.1767 | 0.4845 | 0.1313 | 0.048* | |
C35 | −0.2258 (3) | 0.60528 (19) | 0.16781 (17) | 0.0412 (7) | |
H35A | −0.1963 | 0.6290 | 0.1203 | 0.049* | |
C36 | −0.2815 (3) | 0.65783 (18) | 0.23124 (17) | 0.0390 (7) | |
C37 | −0.3244 (3) | 0.62157 (19) | 0.30141 (17) | 0.0431 (7) | |
H37A | −0.3622 | 0.6560 | 0.3445 | 0.052* | |
C38 | −0.3109 (3) | 0.53371 (19) | 0.30752 (17) | 0.0396 (7) | |
H38A | −0.3394 | 0.5099 | 0.3552 | 0.048* | |
C39 | −0.2442 (3) | 0.38587 (17) | 0.25117 (18) | 0.0385 (7) | |
H39A | −0.2896 | 0.3738 | 0.3026 | 0.046* | |
H39B | −0.2848 | 0.3736 | 0.2171 | 0.046* | |
C40 | −0.1118 (3) | 0.32472 (17) | 0.23337 (15) | 0.0309 (6) | |
C41 | 0.2359 (3) | 0.05195 (19) | −0.04822 (16) | 0.0395 (7) | |
C42 | 0.3536 (3) | 0.0011 (2) | −0.04455 (16) | 0.0430 (7) | |
H42A | 0.4101 | 0.0278 | −0.0405 | 0.052* | |
C43 | 0.3896 (3) | −0.0878 (2) | −0.04677 (17) | 0.0458 (8) | |
H43A | 0.4701 | −0.1206 | −0.0452 | 0.055* | |
C44 | 0.3057 (3) | −0.1283 (2) | −0.05126 (18) | 0.0483 (8) | |
C45 | 0.1879 (3) | −0.0793 (2) | −0.05580 (19) | 0.0506 (8) | |
H45A | 0.1316 | −0.1062 | −0.0598 | 0.061* | |
C46 | 0.1538 (3) | 0.0102 (2) | −0.05431 (17) | 0.0466 (8) | |
H46A | 0.0742 | 0.0431 | −0.0575 | 0.056* | |
C47 | 0.1936 (3) | 0.1500 (2) | −0.04211 (17) | 0.0464 (8) | |
H47A | 0.2564 | 0.1724 | −0.0781 | 0.056* | |
H47B | 0.1156 | 0.1742 | −0.0556 | 0.056* | |
C48 | 0.1739 (3) | 0.17845 (18) | 0.03700 (16) | 0.0358 (7) | |
C49 | 0.2317 (3) | 0.58065 (18) | 0.32245 (17) | 0.0385 (7) | |
H49A | 0.1590 | 0.5745 | 0.3578 | 0.046* | |
C50 | 0.2495 (3) | 0.66107 (18) | 0.31352 (17) | 0.0404 (7) | |
H50A | 0.1897 | 0.7075 | 0.3426 | 0.048* | |
C51 | 0.3563 (3) | 0.67260 (18) | 0.26136 (17) | 0.0377 (7) | |
C52 | 0.4429 (3) | 0.60032 (19) | 0.22209 (19) | 0.0455 (8) | |
H52A | 0.5175 | 0.6044 | 0.1874 | 0.055* | |
C53 | 0.4187 (3) | 0.52211 (19) | 0.23437 (19) | 0.0435 (8) | |
H53A | 0.4787 | 0.4742 | 0.2074 | 0.052* | |
C54 | 0.4496 (4) | 0.8649 (2) | 0.1638 (3) | 0.0724 (13) | |
H54A | 0.4949 | 0.8787 | 0.1158 | 0.087* | |
C55 | 0.4407 (3) | 0.7819 (2) | 0.1761 (2) | 0.0588 (10) | |
H55A | 0.4788 | 0.7417 | 0.1371 | 0.071* | |
C56 | 0.3751 (3) | 0.75940 (19) | 0.24675 (19) | 0.0427 (8) | |
C57 | 0.3238 (4) | 0.8221 (2) | 0.3018 (2) | 0.0613 (10) | |
H57A | 0.2810 | 0.8096 | 0.3511 | 0.074* | |
C58 | 0.3363 (5) | 0.9036 (2) | 0.2835 (3) | 0.0726 (12) | |
H58A | 0.2988 | 0.9452 | 0.3214 | 0.087* | |
C59 | 0.1697 (3) | −0.00447 (18) | 0.14641 (17) | 0.0406 (7) | |
H59A | 0.2428 | 0.0042 | 0.1136 | 0.049* | |
C60 | 0.1549 (3) | −0.08558 (18) | 0.14936 (17) | 0.0420 (7) | |
H60A | 0.2165 | −0.1294 | 0.1180 | 0.050* | |
C61 | 0.0493 (3) | −0.10176 (18) | 0.19860 (17) | 0.0376 (7) | |
C62 | −0.0413 (3) | −0.03205 (19) | 0.24020 (18) | 0.0417 (7) | |
H62A | −0.1156 | −0.0390 | 0.2729 | 0.050* | |
C63 | −0.0217 (3) | 0.04762 (18) | 0.23331 (17) | 0.0390 (7) | |
H63A | −0.0850 | 0.0936 | 0.2611 | 0.047* | |
C64 | 0.1071 (5) | −0.3394 (2) | 0.1717 (2) | 0.0729 (13) | |
H64A | 0.1613 | −0.3824 | 0.1370 | 0.088* | |
C65 | 0.1141 (4) | −0.2559 (2) | 0.1565 (2) | 0.0635 (11) | |
H65A | 0.1694 | −0.2436 | 0.1116 | 0.076* | |
C66 | 0.0382 (3) | −0.19087 (19) | 0.20833 (19) | 0.0445 (8) | |
C67 | −0.0452 (3) | −0.2136 (2) | 0.2724 (2) | 0.0622 (11) | |
H67A | −0.0988 | −0.1725 | 0.3090 | 0.075* | |
C68 | −0.0474 (4) | −0.2986 (2) | 0.2811 (3) | 0.0751 (14) | |
H68A | −0.1056 | −0.3124 | 0.3236 | 0.090* | |
O1W | 0.0812 (2) | 0.45996 (13) | 0.25489 (13) | 0.0402 (5) | |
O1 | 0.3063 (2) | 0.33572 (14) | 0.41483 (12) | 0.0464 (5) | |
O2W | 0.3290 (2) | 0.11013 (13) | 0.21451 (13) | 0.0413 (5) | |
O2 | 0.13551 (19) | 0.43506 (13) | 0.40444 (11) | 0.0393 (5) | |
O3 | 0.3309 (2) | 0.73187 (16) | 0.51131 (16) | 0.0669 (7) | |
H3B | 0.2729 | 0.7703 | 0.5372 | 0.057 (12)* | |
O3W | 0.5581 (3) | 0.76686 (17) | 0.49096 (15) | 0.0579 (6) | |
O4 | 0.49742 (19) | 0.32158 (12) | 0.26433 (13) | 0.0470 (6) | |
O5 | 0.41478 (19) | 0.21718 (12) | 0.27608 (12) | 0.0400 (5) | |
O6 | 0.6210 (3) | −0.16638 (13) | 0.35286 (12) | 0.0596 (7) | |
H6B | 0.5940 | −0.1742 | 0.3988 | 0.089* | |
O7 | 0.3524 (2) | 0.40008 (14) | 0.14780 (11) | 0.0460 (6) | |
O8 | 0.25816 (18) | 0.30140 (11) | 0.16494 (10) | 0.0319 (4) | |
O9 | 0.1635 (2) | 0.71240 (14) | −0.05719 (14) | 0.0560 (6) | |
H9A | 0.0928 | 0.7265 | −0.0624 | 0.084* | |
O10 | 0.14230 (18) | 0.26764 (11) | 0.31403 (10) | 0.0308 (4) | |
O11 | 0.0819 (2) | 0.15184 (12) | 0.33561 (10) | 0.0379 (5) | |
O12 | 0.1417 (2) | −0.12554 (13) | 0.58163 (12) | 0.0468 (5) | |
H12A | 0.0699 | −0.1259 | 0.6043 | 0.070* | |
O13 | −0.01795 (18) | 0.35213 (12) | 0.20644 (12) | 0.0396 (5) | |
O14 | −0.09509 (19) | 0.24475 (12) | 0.24404 (12) | 0.0436 (5) | |
O15 | −0.2918 (2) | 0.74357 (13) | 0.22099 (13) | 0.0563 (6) | |
H15C | −0.3183 | 0.7671 | 0.2626 | 0.084* | |
O16 | 0.2617 (2) | 0.15313 (13) | 0.06689 (11) | 0.0410 (5) | |
O17 | 0.0674 (2) | 0.22729 (14) | 0.07417 (12) | 0.0479 (5) | |
O18 | 0.3448 (3) | −0.21694 (15) | −0.05145 (16) | 0.0742 (8) | |
H18B | 0.2885 | −0.2341 | −0.0549 | 0.111* | |
H2WA | 0.377 (4) | 0.125 (3) | 0.231 (3) | 0.111* | |
H2WB | 0.362 (4) | 0.0568 (13) | 0.208 (3) | 0.111* | |
H3WB | 0.497 (3) | 0.748 (3) | 0.495 (3) | 0.111* | |
H1WA | 0.043 (4) | 0.436 (2) | 0.239 (3) | 0.111* | |
H1WB | 0.048 (4) | 0.5124 (12) | 0.249 (3) | 0.111* | |
H3WA | 0.594 (4) | 0.734 (3) | 0.521 (2) | 0.111* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.02854 (8) | 0.01798 (7) | 0.03435 (8) | −0.00970 (6) | −0.01220 (6) | 0.00222 (5) |
Sm2 | 0.02720 (8) | 0.01720 (7) | 0.03501 (8) | −0.00788 (6) | −0.01100 (6) | 0.00011 (5) |
N1 | 0.0358 (15) | 0.0245 (12) | 0.0504 (15) | −0.0115 (11) | −0.0146 (12) | −0.0006 (10) |
N2 | 0.065 (2) | 0.0320 (16) | 0.121 (3) | −0.0237 (16) | −0.049 (2) | 0.0175 (18) |
N3 | 0.0388 (15) | 0.0216 (11) | 0.0433 (14) | −0.0100 (10) | −0.0154 (11) | 0.0014 (10) |
N4 | 0.084 (3) | 0.0323 (17) | 0.119 (3) | −0.0256 (17) | −0.070 (2) | 0.0171 (18) |
C1 | 0.0403 (18) | 0.0384 (16) | 0.0334 (15) | −0.0138 (14) | −0.0124 (13) | −0.0034 (12) |
C2 | 0.0385 (19) | 0.0460 (19) | 0.0467 (18) | −0.0089 (15) | −0.0036 (15) | −0.0133 (14) |
C3 | 0.0343 (18) | 0.053 (2) | 0.060 (2) | −0.0180 (16) | 0.0001 (16) | −0.0114 (16) |
C4 | 0.0403 (19) | 0.0419 (18) | 0.055 (2) | −0.0162 (15) | −0.0129 (16) | −0.0037 (14) |
C5 | 0.0385 (19) | 0.0425 (18) | 0.059 (2) | −0.0096 (15) | −0.0063 (16) | −0.0140 (15) |
C6 | 0.0358 (18) | 0.0426 (18) | 0.0514 (19) | −0.0124 (15) | −0.0034 (15) | −0.0115 (14) |
C7 | 0.056 (2) | 0.0414 (18) | 0.0351 (16) | −0.0220 (16) | −0.0108 (15) | 0.0002 (13) |
C8 | 0.0425 (19) | 0.0340 (16) | 0.0354 (15) | −0.0216 (14) | −0.0093 (14) | 0.0027 (12) |
C9 | 0.0284 (16) | 0.0280 (15) | 0.060 (2) | −0.0047 (12) | −0.0215 (14) | −0.0002 (13) |
C10 | 0.067 (2) | 0.0310 (17) | 0.0507 (19) | −0.0045 (16) | −0.0273 (18) | −0.0096 (14) |
C11 | 0.069 (2) | 0.0375 (18) | 0.0395 (17) | −0.0109 (16) | −0.0179 (17) | −0.0032 (13) |
C12 | 0.0428 (19) | 0.0300 (15) | 0.0434 (17) | −0.0105 (13) | −0.0105 (14) | −0.0006 (12) |
C13 | 0.056 (2) | 0.0346 (17) | 0.0419 (17) | −0.0125 (15) | −0.0155 (15) | −0.0059 (13) |
C14 | 0.051 (2) | 0.0368 (17) | 0.0403 (17) | −0.0120 (15) | −0.0145 (15) | 0.0047 (13) |
C15 | 0.0329 (18) | 0.0280 (16) | 0.088 (2) | −0.0069 (13) | −0.0296 (17) | 0.0056 (15) |
C16 | 0.0306 (16) | 0.0269 (14) | 0.0416 (16) | −0.0067 (12) | −0.0124 (13) | −0.0004 (11) |
C17 | 0.066 (2) | 0.0394 (17) | 0.0331 (16) | −0.0272 (17) | −0.0205 (15) | 0.0043 (12) |
C18 | 0.067 (3) | 0.063 (2) | 0.0339 (16) | −0.045 (2) | −0.0108 (16) | 0.0033 (15) |
C19 | 0.0409 (19) | 0.056 (2) | 0.0424 (18) | −0.0187 (16) | −0.0106 (15) | −0.0078 (15) |
C20 | 0.053 (2) | 0.0359 (16) | 0.0438 (17) | −0.0191 (15) | −0.0251 (15) | 0.0029 (13) |
C21 | 0.046 (2) | 0.0366 (17) | 0.0500 (18) | −0.0219 (15) | −0.0177 (15) | 0.0086 (13) |
C22 | 0.051 (2) | 0.0382 (17) | 0.0470 (18) | −0.0170 (15) | −0.0214 (16) | 0.0045 (13) |
C23 | 0.112 (3) | 0.0389 (18) | 0.0380 (18) | −0.037 (2) | −0.0281 (19) | 0.0078 (14) |
C24 | 0.0423 (18) | 0.0254 (14) | 0.0322 (14) | −0.0139 (13) | −0.0086 (13) | 0.0006 (11) |
C25 | 0.058 (2) | 0.0380 (17) | 0.0354 (16) | −0.0256 (16) | −0.0236 (15) | 0.0076 (12) |
C26 | 0.052 (2) | 0.0332 (16) | 0.0448 (18) | −0.0104 (15) | −0.0177 (16) | −0.0001 (13) |
C27 | 0.0437 (19) | 0.0457 (18) | 0.0366 (16) | −0.0181 (15) | −0.0084 (14) | 0.0049 (13) |
C28 | 0.0446 (19) | 0.0354 (16) | 0.0358 (15) | −0.0204 (14) | −0.0179 (14) | 0.0096 (12) |
C29 | 0.043 (2) | 0.0442 (18) | 0.0441 (18) | −0.0155 (15) | −0.0135 (15) | 0.0063 (14) |
C30 | 0.047 (2) | 0.051 (2) | 0.0387 (17) | −0.0268 (17) | −0.0119 (15) | 0.0109 (14) |
C31 | 0.072 (2) | 0.0375 (17) | 0.0451 (18) | −0.0312 (17) | −0.0274 (17) | 0.0092 (13) |
C32 | 0.0301 (16) | 0.0266 (14) | 0.0387 (15) | −0.0133 (12) | −0.0089 (12) | 0.0021 (11) |
C33 | 0.0274 (15) | 0.0256 (14) | 0.0424 (16) | −0.0039 (11) | −0.0123 (13) | −0.0026 (11) |
C34 | 0.0435 (19) | 0.0350 (16) | 0.0377 (16) | −0.0063 (14) | −0.0088 (14) | −0.0122 (12) |
C35 | 0.047 (2) | 0.0363 (17) | 0.0385 (16) | −0.0137 (14) | −0.0100 (14) | 0.0015 (13) |
C36 | 0.0421 (19) | 0.0273 (15) | 0.0491 (18) | −0.0069 (13) | −0.0192 (15) | −0.0014 (12) |
C37 | 0.052 (2) | 0.0341 (16) | 0.0404 (17) | −0.0069 (15) | −0.0140 (15) | −0.0077 (13) |
C38 | 0.0403 (18) | 0.0344 (16) | 0.0390 (16) | −0.0077 (13) | −0.0087 (14) | 0.0001 (12) |
C39 | 0.0309 (17) | 0.0268 (15) | 0.0569 (19) | −0.0050 (12) | −0.0144 (14) | −0.0035 (13) |
C40 | 0.0306 (16) | 0.0234 (13) | 0.0403 (15) | −0.0060 (12) | −0.0138 (13) | −0.0036 (11) |
C41 | 0.050 (2) | 0.0382 (17) | 0.0303 (15) | −0.0157 (15) | −0.0087 (14) | −0.0027 (12) |
C42 | 0.048 (2) | 0.0441 (18) | 0.0407 (17) | −0.0219 (16) | −0.0106 (15) | −0.0005 (13) |
C43 | 0.048 (2) | 0.0385 (18) | 0.0484 (19) | −0.0121 (15) | −0.0103 (15) | −0.0027 (14) |
C44 | 0.059 (2) | 0.0353 (17) | 0.0499 (19) | −0.0194 (16) | −0.0095 (17) | −0.0024 (14) |
C45 | 0.053 (2) | 0.049 (2) | 0.057 (2) | −0.0267 (18) | −0.0118 (17) | −0.0055 (16) |
C46 | 0.043 (2) | 0.049 (2) | 0.0451 (18) | −0.0098 (16) | −0.0112 (15) | −0.0086 (14) |
C47 | 0.062 (2) | 0.0369 (17) | 0.0376 (17) | −0.0106 (16) | −0.0155 (16) | 0.0003 (13) |
C48 | 0.050 (2) | 0.0246 (14) | 0.0339 (15) | −0.0152 (14) | −0.0098 (14) | 0.0010 (11) |
C49 | 0.0425 (19) | 0.0296 (15) | 0.0442 (17) | −0.0142 (14) | −0.0111 (14) | 0.0019 (12) |
C50 | 0.0465 (19) | 0.0244 (15) | 0.0516 (18) | −0.0103 (13) | −0.0165 (15) | −0.0014 (12) |
C51 | 0.0402 (18) | 0.0245 (14) | 0.0552 (18) | −0.0129 (13) | −0.0222 (15) | 0.0044 (12) |
C52 | 0.0345 (18) | 0.0329 (16) | 0.070 (2) | −0.0153 (14) | −0.0117 (16) | 0.0025 (15) |
C53 | 0.0365 (18) | 0.0257 (15) | 0.067 (2) | −0.0103 (13) | −0.0112 (16) | −0.0048 (14) |
C54 | 0.054 (3) | 0.041 (2) | 0.114 (3) | −0.0220 (19) | −0.013 (2) | 0.023 (2) |
C55 | 0.049 (2) | 0.0320 (18) | 0.085 (3) | −0.0160 (16) | −0.0029 (19) | 0.0024 (17) |
C56 | 0.0408 (19) | 0.0270 (15) | 0.069 (2) | −0.0149 (14) | −0.0258 (16) | 0.0054 (14) |
C57 | 0.094 (3) | 0.0378 (19) | 0.065 (2) | −0.031 (2) | −0.033 (2) | 0.0052 (16) |
C58 | 0.112 (4) | 0.039 (2) | 0.089 (3) | −0.034 (2) | −0.049 (3) | 0.0000 (19) |
C59 | 0.0458 (19) | 0.0291 (15) | 0.0432 (17) | −0.0120 (14) | −0.0086 (15) | 0.0028 (12) |
C60 | 0.051 (2) | 0.0242 (15) | 0.0479 (18) | −0.0088 (14) | −0.0123 (15) | −0.0038 (12) |
C61 | 0.0477 (19) | 0.0276 (15) | 0.0493 (17) | −0.0142 (14) | −0.0303 (15) | 0.0072 (12) |
C62 | 0.0391 (18) | 0.0327 (16) | 0.0574 (19) | −0.0172 (14) | −0.0145 (15) | 0.0034 (14) |
C63 | 0.0381 (18) | 0.0269 (15) | 0.0547 (18) | −0.0122 (13) | −0.0145 (15) | −0.0014 (13) |
C64 | 0.133 (4) | 0.035 (2) | 0.076 (3) | −0.028 (2) | −0.063 (3) | −0.0010 (18) |
C65 | 0.118 (4) | 0.0349 (19) | 0.055 (2) | −0.032 (2) | −0.043 (2) | 0.0041 (15) |
C66 | 0.056 (2) | 0.0276 (15) | 0.066 (2) | −0.0162 (15) | −0.0398 (18) | 0.0080 (14) |
C67 | 0.045 (2) | 0.0343 (18) | 0.109 (3) | −0.0162 (16) | −0.026 (2) | 0.0130 (19) |
C68 | 0.054 (3) | 0.039 (2) | 0.145 (4) | −0.0274 (19) | −0.044 (3) | 0.030 (2) |
O1W | 0.0430 (13) | 0.0232 (10) | 0.0624 (14) | −0.0089 (9) | −0.0288 (11) | 0.0028 (9) |
O1 | 0.0521 (15) | 0.0388 (12) | 0.0462 (12) | −0.0040 (11) | −0.0207 (11) | −0.0047 (10) |
O2W | 0.0404 (13) | 0.0237 (10) | 0.0655 (14) | −0.0073 (9) | −0.0257 (11) | −0.0013 (10) |
O2 | 0.0383 (12) | 0.0408 (12) | 0.0412 (11) | −0.0132 (10) | −0.0135 (10) | −0.0021 (9) |
O3 | 0.0475 (15) | 0.0463 (14) | 0.105 (2) | −0.0237 (13) | −0.0038 (15) | −0.0185 (14) |
O3W | 0.0609 (18) | 0.0564 (16) | 0.0613 (16) | −0.0235 (14) | −0.0260 (13) | 0.0190 (12) |
O4 | 0.0360 (12) | 0.0236 (10) | 0.0820 (16) | −0.0104 (9) | −0.0201 (11) | 0.0091 (10) |
O5 | 0.0338 (12) | 0.0249 (10) | 0.0686 (14) | −0.0079 (9) | −0.0251 (10) | −0.0035 (9) |
O6 | 0.096 (2) | 0.0339 (12) | 0.0485 (13) | −0.0285 (13) | −0.0118 (13) | −0.0006 (10) |
O7 | 0.0632 (15) | 0.0504 (13) | 0.0399 (12) | −0.0408 (12) | −0.0145 (11) | 0.0078 (9) |
O8 | 0.0365 (11) | 0.0243 (10) | 0.0378 (10) | −0.0148 (8) | −0.0106 (9) | 0.0039 (8) |
O9 | 0.0606 (16) | 0.0360 (12) | 0.0839 (17) | −0.0159 (11) | −0.0408 (14) | 0.0096 (11) |
O10 | 0.0356 (11) | 0.0241 (9) | 0.0349 (10) | −0.0144 (8) | −0.0096 (8) | 0.0049 (7) |
O11 | 0.0527 (14) | 0.0350 (11) | 0.0373 (11) | −0.0272 (10) | −0.0170 (10) | 0.0073 (8) |
O12 | 0.0511 (14) | 0.0344 (11) | 0.0541 (13) | −0.0201 (10) | −0.0117 (11) | 0.0130 (9) |
O13 | 0.0279 (11) | 0.0236 (10) | 0.0687 (14) | −0.0064 (8) | −0.0167 (10) | −0.0029 (9) |
O14 | 0.0330 (12) | 0.0220 (10) | 0.0713 (15) | −0.0078 (9) | −0.0105 (10) | 0.0022 (9) |
O15 | 0.0844 (19) | 0.0294 (12) | 0.0591 (14) | −0.0195 (12) | −0.0253 (13) | 0.0020 (10) |
O16 | 0.0394 (13) | 0.0397 (12) | 0.0450 (12) | −0.0109 (10) | −0.0131 (10) | −0.0062 (9) |
O17 | 0.0487 (14) | 0.0455 (13) | 0.0436 (12) | 0.0021 (11) | −0.0204 (11) | −0.0075 (10) |
O18 | 0.077 (2) | 0.0375 (14) | 0.112 (2) | −0.0190 (14) | −0.0312 (17) | −0.0027 (14) |
Sm1—O5 | 2.4344 (19) | C28—O12 | 1.374 (3) |
Sm1—O4 | 2.439 (2) | C28—C29 | 1.382 (4) |
Sm1—O1W | 2.445 (2) | C29—C30 | 1.379 (4) |
Sm1—O10 | 2.4396 (16) | C29—H29A | 0.9300 |
Sm1—O2 | 2.451 (2) | C30—H30A | 0.9300 |
Sm1—O7 | 2.4718 (19) | C31—C32 | 1.502 (4) |
Sm1—O1 | 2.546 (2) | C31—H31A | 0.9700 |
Sm1—O8 | 2.5904 (18) | C31—H31B | 0.9700 |
Sm1—N1 | 2.598 (2) | C32—O11 | 1.251 (3) |
Sm1—C16 | 2.792 (3) | C32—O10 | 1.274 (3) |
Sm1—C8 | 2.876 (3) | C33—C38 | 1.381 (4) |
Sm1—C24 | 2.902 (3) | C33—C34 | 1.393 (4) |
Sm2—O8 | 2.3896 (16) | C33—C39 | 1.499 (4) |
Sm2—O14 | 2.424 (2) | C34—C35 | 1.370 (4) |
Sm2—O13 | 2.4379 (19) | C34—H34A | 0.9300 |
Sm2—O2W | 2.444 (2) | C35—C36 | 1.385 (4) |
Sm2—O16 | 2.464 (2) | C35—H35A | 0.9300 |
Sm2—O17 | 2.532 (2) | C36—O15 | 1.361 (3) |
Sm2—O10 | 2.5572 (18) | C36—C37 | 1.380 (4) |
Sm2—O11 | 2.5947 (18) | C37—C38 | 1.385 (4) |
Sm2—N3 | 2.620 (2) | C37—H37A | 0.9300 |
Sm2—C40 | 2.806 (3) | C38—H38A | 0.9300 |
Sm2—C48 | 2.874 (3) | C39—C40 | 1.506 (4) |
Sm2—C32 | 2.954 (3) | C39—H39A | 0.9700 |
N1—C53 | 1.336 (4) | C39—H39B | 0.9700 |
N1—C49 | 1.334 (4) | C40—O14 | 1.257 (3) |
N2—C58 | 1.312 (5) | C40—O13 | 1.265 (3) |
N2—C54 | 1.326 (5) | C41—C42 | 1.380 (4) |
N3—C63 | 1.341 (4) | C41—C46 | 1.386 (4) |
N3—C59 | 1.337 (4) | C41—C47 | 1.517 (4) |
N4—C64 | 1.320 (5) | C42—C43 | 1.373 (4) |
N4—C68 | 1.331 (6) | C42—H42A | 0.9300 |
C1—C2 | 1.378 (4) | C43—C44 | 1.380 (4) |
C1—C6 | 1.389 (4) | C43—H43A | 0.9300 |
C1—C7 | 1.514 (4) | C44—O18 | 1.368 (4) |
C2—C3 | 1.383 (4) | C44—C45 | 1.378 (5) |
C2—H2A | 0.9300 | C45—C46 | 1.383 (4) |
C3—C4 | 1.367 (4) | C45—H45A | 0.9300 |
C3—H3A | 0.9300 | C46—H46A | 0.9300 |
C4—C5 | 1.372 (4) | C47—C48 | 1.508 (4) |
C4—O3 | 1.378 (4) | C47—H47A | 0.9700 |
C5—C6 | 1.372 (4) | C47—H47B | 0.9700 |
C5—H5A | 0.9300 | C48—O16 | 1.250 (4) |
C6—H6A | 0.9300 | C48—O17 | 1.271 (4) |
C7—C8 | 1.503 (4) | C49—C50 | 1.379 (4) |
C7—H7A | 0.9700 | C49—H49A | 0.9300 |
C7—H7B | 0.9700 | C50—C51 | 1.381 (4) |
C8—O1 | 1.264 (4) | C50—H50A | 0.9300 |
C8—O2 | 1.257 (4) | C51—C52 | 1.380 (4) |
C9—C10 | 1.373 (4) | C51—C56 | 1.486 (4) |
C9—C14 | 1.387 (4) | C52—C53 | 1.376 (4) |
C9—C15 | 1.506 (4) | C52—H52A | 0.9300 |
C10—C11 | 1.392 (4) | C53—H53A | 0.9300 |
C10—H10A | 0.9300 | C54—C55 | 1.380 (4) |
C11—C12 | 1.369 (4) | C54—H54A | 0.9300 |
C11—H11A | 0.9300 | C55—C56 | 1.374 (5) |
C12—C13 | 1.374 (4) | C55—H55A | 0.9300 |
C12—O6 | 1.373 (3) | C56—C57 | 1.376 (5) |
C13—C14 | 1.369 (4) | C57—C58 | 1.378 (5) |
C13—H13A | 0.9300 | C57—H57A | 0.9300 |
C14—H14A | 0.9300 | C58—H58A | 0.9300 |
C15—C16 | 1.509 (4) | C59—C60 | 1.383 (4) |
C15—H15A | 0.9700 | C59—H59A | 0.9300 |
C15—H15B | 0.9700 | C60—C61 | 1.380 (4) |
C16—O4 | 1.253 (3) | C60—H60A | 0.9300 |
C16—O5 | 1.260 (3) | C61—C62 | 1.384 (4) |
C17—C22 | 1.381 (4) | C61—C66 | 1.488 (4) |
C17—C18 | 1.381 (5) | C62—C63 | 1.378 (4) |
C17—C23 | 1.514 (4) | C62—H62A | 0.9300 |
C18—C19 | 1.382 (5) | C63—H63A | 0.9300 |
C18—H18A | 0.9300 | C64—C65 | 1.384 (5) |
C19—C20 | 1.387 (4) | C64—H64A | 0.9300 |
C19—H19A | 0.9300 | C65—C66 | 1.385 (5) |
C20—O9 | 1.372 (3) | C65—H65A | 0.9300 |
C20—C21 | 1.373 (4) | C66—C67 | 1.388 (5) |
C21—C22 | 1.381 (4) | C67—C68 | 1.385 (5) |
C21—H21A | 0.9300 | C67—H67A | 0.9300 |
C22—H22A | 0.9300 | C68—H68A | 0.9300 |
C23—C24 | 1.502 (4) | O1W—H1WA | 0.81 (5) |
C23—H23A | 0.9700 | O1W—H1WB | 0.826 (18) |
C23—H23B | 0.9700 | O2W—H2WA | 0.83 (5) |
C24—O7 | 1.239 (3) | O2W—H2WB | 0.834 (18) |
C24—O8 | 1.274 (3) | O3—H3B | 0.8200 |
C25—C30 | 1.380 (4) | O3W—H3WB | 0.85 (4) |
C25—C26 | 1.388 (4) | O3W—H3WA | 0.84 (4) |
C25—C31 | 1.507 (4) | O6—H6B | 0.8200 |
C26—C27 | 1.386 (4) | O9—H9A | 0.8200 |
C26—H26A | 0.9300 | O12—H12A | 0.8200 |
C27—C28 | 1.371 (4) | O15—H15C | 0.8200 |
C27—H27A | 0.9300 | O18—H18B | 0.8200 |
O5—Sm1—O4 | 53.20 (6) | C17—C18—H18A | 119.2 |
O5—Sm1—O1W | 145.23 (6) | C18—C19—C20 | 119.3 (3) |
O4—Sm1—O1W | 150.49 (7) | C18—C19—H19A | 120.3 |
O5—Sm1—O10 | 73.25 (6) | C20—C19—H19A | 120.3 |
O4—Sm1—O10 | 126.11 (6) | O9—C20—C21 | 118.2 (3) |
O1W—Sm1—O10 | 79.74 (6) | O9—C20—C19 | 122.0 (3) |
O5—Sm1—O2 | 123.26 (7) | C21—C20—C19 | 119.8 (3) |
O4—Sm1—O2 | 116.84 (7) | C20—C21—C22 | 119.9 (3) |
O1W—Sm1—O2 | 74.90 (7) | C20—C21—H21A | 120.0 |
O10—Sm1—O2 | 85.59 (6) | C22—C21—H21A | 120.0 |
O5—Sm1—O7 | 95.18 (7) | C17—C22—C21 | 121.4 (3) |
O4—Sm1—O7 | 77.29 (7) | C17—C22—H22A | 119.3 |
O1W—Sm1—O7 | 77.80 (8) | C21—C22—H22A | 119.3 |
O10—Sm1—O7 | 116.92 (6) | C24—C23—C17 | 112.3 (3) |
O2—Sm1—O7 | 140.51 (7) | C24—C23—H23A | 109.2 |
O5—Sm1—O1 | 75.97 (7) | C17—C23—H23A | 109.2 |
O4—Sm1—O1 | 72.89 (8) | C24—C23—H23B | 109.2 |
O1W—Sm1—O1 | 126.25 (8) | C17—C23—H23B | 109.2 |
O10—Sm1—O1 | 90.25 (6) | H23A—C23—H23B | 107.9 |
O2—Sm1—O1 | 51.61 (7) | O7—C24—O8 | 120.4 (2) |
O7—Sm1—O1 | 148.06 (7) | O7—C24—C23 | 120.4 (2) |
O5—Sm1—O8 | 75.80 (6) | O8—C24—C23 | 119.2 (3) |
O4—Sm1—O8 | 102.16 (7) | O7—C24—Sm1 | 57.66 (14) |
O1W—Sm1—O8 | 73.48 (7) | O8—C24—Sm1 | 63.20 (14) |
O10—Sm1—O8 | 66.26 (6) | C23—C24—Sm1 | 171.2 (2) |
O2—Sm1—O8 | 140.65 (6) | C30—C25—C26 | 118.0 (3) |
O7—Sm1—O8 | 50.96 (6) | C30—C25—C31 | 120.3 (3) |
O1—Sm1—O8 | 147.46 (6) | C26—C25—C31 | 121.7 (3) |
O5—Sm1—N1 | 129.77 (7) | C27—C26—C25 | 121.0 (3) |
O4—Sm1—N1 | 76.68 (7) | C27—C26—H26A | 119.5 |
O1W—Sm1—N1 | 81.72 (7) | C25—C26—H26A | 119.5 |
O10—Sm1—N1 | 155.06 (7) | C28—C27—C26 | 119.8 (3) |
O2—Sm1—N1 | 73.54 (7) | C28—C27—H27A | 120.1 |
O7—Sm1—N1 | 74.76 (7) | C26—C27—H27A | 120.1 |
O1—Sm1—N1 | 87.38 (7) | C27—C28—O12 | 122.4 (3) |
O8—Sm1—N1 | 123.48 (6) | C27—C28—C29 | 120.0 (3) |
O5—Sm1—C16 | 26.79 (7) | O12—C28—C29 | 117.6 (3) |
O4—Sm1—C16 | 26.63 (7) | C30—C29—C28 | 119.7 (3) |
O1W—Sm1—C16 | 163.53 (8) | C30—C29—H29A | 120.1 |
O10—Sm1—C16 | 99.49 (7) | C28—C29—H29A | 120.1 |
O2—Sm1—C16 | 121.54 (8) | C29—C30—C25 | 121.4 (3) |
O7—Sm1—C16 | 88.13 (8) | C29—C30—H30A | 119.3 |
O1—Sm1—C16 | 70.06 (8) | C25—C30—H30A | 119.3 |
O8—Sm1—C16 | 91.05 (7) | C25—C31—C32 | 114.9 (2) |
N1—Sm1—C16 | 102.98 (8) | C25—C31—H31A | 108.5 |
O5—Sm1—C8 | 100.86 (8) | C32—C31—H31A | 108.5 |
O4—Sm1—C8 | 93.91 (8) | C25—C31—H31B | 108.5 |
O1W—Sm1—C8 | 100.65 (9) | C32—C31—H31B | 108.5 |
O10—Sm1—C8 | 90.08 (7) | H31A—C31—H31B | 107.5 |
O2—Sm1—C8 | 25.75 (8) | O11—C32—O10 | 119.6 (2) |
O7—Sm1—C8 | 151.75 (7) | O11—C32—C31 | 122.7 (2) |
O1—Sm1—C8 | 26.07 (8) | O10—C32—C31 | 117.7 (2) |
O8—Sm1—C8 | 156.18 (6) | O11—C32—Sm2 | 61.23 (14) |
N1—Sm1—C8 | 77.11 (7) | O10—C32—Sm2 | 59.60 (13) |
C16—Sm1—C8 | 95.79 (9) | C31—C32—Sm2 | 168.4 (2) |
O5—Sm1—C24 | 86.95 (8) | C38—C33—C34 | 117.3 (2) |
O4—Sm1—C24 | 91.04 (8) | C38—C33—C39 | 121.8 (3) |
O1W—Sm1—C24 | 72.29 (8) | C34—C33—C39 | 120.9 (3) |
O10—Sm1—C24 | 91.89 (7) | C35—C34—C33 | 121.4 (3) |
O2—Sm1—C24 | 147.01 (8) | C35—C34—H34A | 119.3 |
O7—Sm1—C24 | 25.05 (7) | C33—C34—H34A | 119.3 |
O1—Sm1—C24 | 161.38 (8) | C34—C35—C36 | 120.5 (3) |
O8—Sm1—C24 | 26.03 (6) | C34—C35—H35A | 119.7 |
N1—Sm1—C24 | 98.21 (7) | C36—C35—H35A | 119.7 |
C16—Sm1—C24 | 91.34 (8) | O15—C36—C37 | 123.0 (3) |
C8—Sm1—C24 | 172.18 (8) | O15—C36—C35 | 117.9 (3) |
O8—Sm2—O14 | 127.89 (6) | C37—C36—C35 | 119.0 (3) |
O8—Sm2—O13 | 75.13 (6) | C36—C37—C38 | 119.9 (3) |
O14—Sm2—O13 | 53.27 (6) | C36—C37—H37A | 120.1 |
O8—Sm2—O2W | 78.76 (7) | C38—C37—H37A | 120.1 |
O14—Sm2—O2W | 143.94 (7) | C33—C38—C37 | 121.8 (3) |
O13—Sm2—O2W | 147.65 (7) | C33—C38—H38A | 119.1 |
O8—Sm2—O16 | 81.26 (6) | C37—C38—H38A | 119.1 |
O14—Sm2—O16 | 126.48 (7) | C40—C39—C33 | 115.7 (2) |
O13—Sm2—O16 | 117.96 (7) | C40—C39—H39A | 108.4 |
O2W—Sm2—O16 | 75.82 (8) | C33—C39—H39A | 108.4 |
O8—Sm2—O17 | 98.20 (7) | C40—C39—H39B | 108.4 |
O14—Sm2—O17 | 77.89 (7) | C33—C39—H39B | 108.4 |
O13—Sm2—O17 | 76.05 (7) | H39A—C39—H39B | 107.4 |
O2W—Sm2—O17 | 126.91 (7) | O14—C40—O13 | 119.7 (3) |
O16—Sm2—O17 | 51.67 (7) | O14—C40—C39 | 119.0 (2) |
O8—Sm2—O10 | 67.51 (6) | O13—C40—C39 | 121.4 (2) |
O14—Sm2—O10 | 90.92 (7) | O14—C40—Sm2 | 59.52 (14) |
O13—Sm2—O10 | 75.70 (6) | O13—C40—Sm2 | 60.16 (14) |
O2W—Sm2—O10 | 76.88 (7) | C39—C40—Sm2 | 177.20 (19) |
O16—Sm2—O10 | 141.76 (6) | C42—C41—C46 | 117.7 (3) |
O17—Sm2—O10 | 150.83 (6) | C42—C41—C47 | 122.1 (3) |
O8—Sm2—O11 | 115.29 (6) | C46—C41—C47 | 120.2 (3) |
O14—Sm2—O11 | 73.46 (7) | C43—C42—C41 | 121.9 (3) |
O13—Sm2—O11 | 101.66 (7) | C43—C42—H42A | 119.0 |
O2W—Sm2—O11 | 72.75 (7) | C41—C42—H42A | 119.0 |
O16—Sm2—O11 | 140.11 (7) | C44—C43—C42 | 119.6 (3) |
O17—Sm2—O11 | 144.90 (7) | C44—C43—H43A | 120.2 |
O10—Sm2—O11 | 50.14 (5) | C42—C43—H43A | 120.2 |
O8—Sm2—N3 | 155.05 (7) | O18—C44—C43 | 117.5 (3) |
O14—Sm2—N3 | 75.76 (7) | O18—C44—C45 | 122.6 (3) |
O13—Sm2—N3 | 126.14 (7) | C43—C44—C45 | 119.9 (3) |
O2W—Sm2—N3 | 84.29 (7) | C46—C45—C44 | 119.6 (3) |
O16—Sm2—N3 | 76.90 (7) | C46—C45—H45A | 120.2 |
O17—Sm2—N3 | 77.54 (7) | C44—C45—H45A | 120.2 |
O10—Sm2—N3 | 126.09 (6) | C45—C46—C41 | 121.3 (3) |
O11—Sm2—N3 | 76.13 (6) | C45—C46—H46A | 119.4 |
O8—Sm2—C40 | 101.68 (7) | C41—C46—H46A | 119.4 |
O14—Sm2—C40 | 26.53 (7) | C48—C47—C41 | 112.1 (2) |
O13—Sm2—C40 | 26.75 (7) | C48—C47—H47A | 109.2 |
O2W—Sm2—C40 | 157.91 (8) | C41—C47—H47A | 109.2 |
O16—Sm2—C40 | 126.24 (8) | C48—C47—H47B | 109.2 |
O17—Sm2—C40 | 75.11 (7) | C41—C47—H47B | 109.2 |
O10—Sm2—C40 | 82.88 (7) | H47A—C47—H47B | 107.9 |
O11—Sm2—C40 | 87.53 (7) | O16—C48—O17 | 119.5 (3) |
N3—Sm2—C40 | 100.89 (7) | O16—C48—C47 | 120.3 (3) |
O8—Sm2—C48 | 91.70 (7) | O17—C48—C47 | 120.2 (3) |
O14—Sm2—C48 | 101.89 (9) | O16—C48—Sm2 | 58.51 (15) |
O13—Sm2—C48 | 98.78 (8) | O17—C48—Sm2 | 61.67 (15) |
O2W—Sm2—C48 | 100.77 (9) | C47—C48—Sm2 | 171.01 (19) |
O16—Sm2—C48 | 25.63 (8) | N1—C49—C50 | 123.3 (3) |
O17—Sm2—C48 | 26.22 (8) | N1—C49—H49A | 118.4 |
O10—Sm2—C48 | 159.18 (7) | C50—C49—H49A | 118.4 |
O11—Sm2—C48 | 149.49 (7) | C49—C50—C51 | 119.9 (3) |
N3—Sm2—C48 | 73.54 (7) | C49—C50—H50A | 120.1 |
C40—Sm2—C48 | 101.29 (9) | C51—C50—H50A | 120.1 |
O8—Sm2—C32 | 90.76 (6) | C50—C51—C52 | 116.9 (2) |
O14—Sm2—C32 | 84.15 (8) | C50—C51—C56 | 121.4 (3) |
O13—Sm2—C32 | 91.20 (7) | C52—C51—C56 | 121.7 (3) |
O2W—Sm2—C32 | 70.24 (8) | C53—C52—C51 | 119.8 (3) |
O16—Sm2—C32 | 146.03 (8) | C53—C52—H52A | 120.1 |
O17—Sm2—C32 | 161.85 (8) | C51—C52—H52A | 120.1 |
O10—Sm2—C32 | 25.46 (6) | N1—C53—C52 | 123.5 (3) |
O11—Sm2—C32 | 25.00 (6) | N1—C53—H53A | 118.2 |
N3—Sm2—C32 | 100.64 (7) | C52—C53—H53A | 118.2 |
C40—Sm2—C32 | 87.67 (8) | N2—C54—C55 | 124.2 (4) |
C48—Sm2—C32 | 170.02 (8) | N2—C54—H54A | 117.9 |
C53—N1—C49 | 116.6 (2) | C55—C54—H54A | 117.9 |
C53—N1—Sm1 | 118.68 (18) | C54—C55—C56 | 119.2 (4) |
C49—N1—Sm1 | 124.39 (18) | C54—C55—H55A | 120.4 |
C58—N2—C54 | 115.9 (3) | C56—C55—H55A | 120.4 |
C63—N3—C59 | 116.5 (2) | C57—C56—C55 | 116.8 (3) |
C63—N3—Sm2 | 121.64 (18) | C57—C56—C51 | 122.0 (3) |
C59—N3—Sm2 | 121.42 (18) | C55—C56—C51 | 121.1 (3) |
C64—N4—C68 | 116.2 (3) | C56—C57—C58 | 119.6 (4) |
C2—C1—C6 | 117.5 (3) | C56—C57—H57A | 120.2 |
C2—C1—C7 | 122.4 (3) | C58—C57—H57A | 120.2 |
C6—C1—C7 | 120.1 (3) | N2—C58—C57 | 124.2 (4) |
C1—C2—C3 | 121.5 (3) | N2—C58—H58A | 117.9 |
C1—C2—H2A | 119.3 | C57—C58—H58A | 117.9 |
C3—C2—H2A | 119.3 | N3—C59—C60 | 123.1 (3) |
C4—C3—C2 | 119.8 (3) | N3—C59—H59A | 118.4 |
C4—C3—H3A | 120.1 | C60—C59—H59A | 118.4 |
C2—C3—H3A | 120.1 | C59—C60—C61 | 120.3 (3) |
C3—C4—C5 | 119.7 (3) | C59—C60—H60A | 119.9 |
C3—C4—O3 | 118.5 (3) | C61—C60—H60A | 119.9 |
C5—C4—O3 | 121.8 (3) | C60—C61—C62 | 116.4 (2) |
C4—C5—C6 | 120.3 (3) | C60—C61—C66 | 120.8 (3) |
C4—C5—H5A | 119.9 | C62—C61—C66 | 122.7 (3) |
C6—C5—H5A | 119.9 | C63—C62—C61 | 120.2 (3) |
C5—C6—C1 | 121.2 (3) | C63—C62—H62A | 119.9 |
C5—C6—H6A | 119.4 | C61—C62—H62A | 119.9 |
C1—C6—H6A | 119.4 | N3—C63—C62 | 123.2 (3) |
C8—C7—C1 | 111.8 (2) | N3—C63—H63A | 118.4 |
C8—C7—H7A | 109.3 | C62—C63—H63A | 118.4 |
C1—C7—H7A | 109.3 | N4—C64—C65 | 124.0 (4) |
C8—C7—H7B | 109.3 | N4—C64—H64A | 118.0 |
C1—C7—H7B | 109.3 | C65—C64—H64A | 118.0 |
H7A—C7—H7B | 107.9 | C64—C65—C66 | 119.7 (4) |
O1—C8—O2 | 119.4 (3) | C64—C65—H65A | 120.2 |
O1—C8—C7 | 120.7 (3) | C66—C65—H65A | 120.2 |
O2—C8—C7 | 119.9 (3) | C65—C66—C67 | 116.8 (3) |
O1—C8—Sm1 | 62.24 (15) | C65—C66—C61 | 122.2 (3) |
O2—C8—Sm1 | 57.91 (15) | C67—C66—C61 | 120.9 (3) |
C7—C8—Sm1 | 169.06 (18) | C68—C67—C66 | 118.9 (4) |
C10—C9—C14 | 117.2 (3) | C68—C67—H67A | 120.5 |
C10—C9—C15 | 121.7 (3) | C66—C67—H67A | 120.5 |
C14—C9—C15 | 121.1 (3) | N4—C68—C67 | 124.4 (4) |
C9—C10—C11 | 122.1 (3) | N4—C68—H68A | 117.8 |
C9—C10—H10A | 119.0 | C67—C68—H68A | 117.8 |
C11—C10—H10A | 119.0 | Sm1—O1W—H1WA | 116 (3) |
C12—C11—C10 | 119.1 (3) | Sm1—O1W—H1WB | 138 (3) |
C12—C11—H11A | 120.5 | H1WA—O1W—H1WB | 105 (3) |
C10—C11—H11A | 120.5 | C8—O1—Sm1 | 91.69 (17) |
C13—C12—C11 | 119.9 (3) | Sm2—O2W—H2WA | 125 (3) |
C13—C12—O6 | 117.5 (3) | Sm2—O2W—H2WB | 130 (3) |
C11—C12—O6 | 122.6 (3) | H2WA—O2W—H2WB | 105 (3) |
C12—C13—C14 | 120.2 (3) | C8—O2—Sm1 | 96.34 (18) |
C12—C13—H13A | 119.9 | C4—O3—H3B | 109.5 |
C14—C13—H13A | 119.9 | H3WB—O3W—H3WA | 102 (3) |
C13—C14—C9 | 121.5 (3) | C16—O4—Sm1 | 92.64 (17) |
C13—C14—H14A | 119.3 | C16—O5—Sm1 | 92.66 (16) |
C9—C14—H14A | 119.3 | C12—O6—H6B | 109.5 |
C9—C15—C16 | 114.9 (2) | C24—O7—Sm1 | 97.28 (16) |
C9—C15—H15A | 108.5 | C24—O8—Sm2 | 153.69 (18) |
C16—C15—H15A | 108.5 | C24—O8—Sm1 | 90.77 (15) |
C9—C15—H15B | 108.5 | Sm2—O8—Sm1 | 113.39 (7) |
C16—C15—H15B | 108.5 | C20—O9—H9A | 109.5 |
H15A—C15—H15B | 107.5 | C32—O10—Sm1 | 142.67 (17) |
O4—C16—O5 | 120.5 (3) | C32—O10—Sm2 | 94.93 (15) |
O4—C16—C15 | 118.7 (3) | Sm1—O10—Sm2 | 112.84 (6) |
O5—C16—C15 | 120.7 (2) | C32—O11—Sm2 | 93.77 (15) |
O4—C16—Sm1 | 60.73 (15) | C28—O12—H12A | 109.5 |
O5—C16—Sm1 | 60.56 (14) | C40—O13—Sm2 | 93.09 (15) |
C15—C16—Sm1 | 169.1 (2) | C40—O14—Sm2 | 93.95 (16) |
C22—C17—C18 | 117.9 (3) | C36—O15—H15C | 109.5 |
C22—C17—C23 | 121.1 (3) | C48—O16—Sm2 | 95.86 (18) |
C18—C17—C23 | 121.0 (3) | C48—O17—Sm2 | 92.11 (18) |
C19—C18—C17 | 121.7 (3) | C44—O18—H18B | 109.5 |
C19—C18—H18A | 119.2 | ||
O5—Sm1—N1—C53 | 41.9 (3) | O13—Sm2—C48—O17 | −30.02 (17) |
O4—Sm1—N1—C53 | 38.2 (2) | O2W—Sm2—C48—O17 | 175.88 (16) |
O1W—Sm1—N1—C53 | −121.6 (2) | O16—Sm2—C48—O17 | −170.8 (3) |
O10—Sm1—N1—C53 | −163.8 (2) | O10—Sm2—C48—O17 | −102.7 (3) |
O2—Sm1—N1—C53 | 161.8 (2) | O11—Sm2—C48—O17 | 101.6 (2) |
O7—Sm1—N1—C53 | −42.0 (2) | N3—Sm2—C48—O17 | 95.19 (17) |
O1—Sm1—N1—C53 | 111.2 (2) | C40—Sm2—C48—O17 | −2.97 (18) |
O8—Sm1—N1—C53 | −57.7 (2) | C53—N1—C49—C50 | 2.0 (5) |
C16—Sm1—N1—C53 | 42.4 (2) | Sm1—N1—C49—C50 | −171.2 (2) |
C8—Sm1—N1—C53 | 135.4 (2) | N1—C49—C50—C51 | 0.1 (5) |
C24—Sm1—N1—C53 | −50.9 (2) | C49—C50—C51—C52 | −2.1 (5) |
O5—Sm1—N1—C49 | −145.0 (2) | C49—C50—C51—C56 | 176.2 (3) |
O4—Sm1—N1—C49 | −148.7 (2) | C50—C51—C52—C53 | 1.9 (5) |
O1W—Sm1—N1—C49 | 51.5 (2) | C56—C51—C52—C53 | −176.5 (3) |
O10—Sm1—N1—C49 | 9.2 (3) | C49—N1—C53—C52 | −2.3 (5) |
O2—Sm1—N1—C49 | −25.1 (2) | Sm1—N1—C53—C52 | 171.4 (3) |
O7—Sm1—N1—C49 | 131.0 (2) | C51—C52—C53—N1 | 0.3 (5) |
O1—Sm1—N1—C49 | −75.7 (2) | C58—N2—C54—C55 | 1.1 (6) |
O8—Sm1—N1—C49 | 115.4 (2) | N2—C54—C55—C56 | −0.5 (6) |
C16—Sm1—N1—C49 | −144.6 (2) | C54—C55—C56—C57 | −1.2 (5) |
C8—Sm1—N1—C49 | −51.5 (2) | C54—C55—C56—C51 | 176.2 (3) |
C24—Sm1—N1—C49 | 122.1 (2) | C50—C51—C56—C57 | 29.0 (5) |
O8—Sm2—N3—C63 | 173.16 (19) | C52—C51—C56—C57 | −152.8 (3) |
O14—Sm2—N3—C63 | −23.8 (2) | C50—C51—C56—C55 | −148.3 (3) |
O13—Sm2—N3—C63 | −42.1 (2) | C52—C51—C56—C55 | 30.0 (5) |
O2W—Sm2—N3—C63 | 125.9 (2) | C55—C56—C57—C58 | 2.2 (6) |
O16—Sm2—N3—C63 | −157.3 (2) | C51—C56—C57—C58 | −175.1 (3) |
O17—Sm2—N3—C63 | −104.2 (2) | C54—N2—C58—C57 | 0.0 (6) |
O10—Sm2—N3—C63 | 56.8 (2) | C56—C57—C58—N2 | −1.7 (7) |
O11—Sm2—N3—C63 | 52.3 (2) | C63—N3—C59—C60 | −2.1 (4) |
C40—Sm2—N3—C63 | −32.3 (2) | Sm2—N3—C59—C60 | 170.8 (2) |
C48—Sm2—N3—C63 | −131.0 (2) | N3—C59—C60—C61 | −1.5 (5) |
C32—Sm2—N3—C63 | 57.3 (2) | C59—C60—C61—C62 | 3.5 (4) |
O8—Sm2—N3—C59 | 0.6 (3) | C59—C60—C61—C66 | −173.5 (3) |
O14—Sm2—N3—C59 | 163.7 (2) | C60—C61—C62—C63 | −2.2 (4) |
O13—Sm2—N3—C59 | 145.3 (2) | C66—C61—C62—C63 | 174.8 (3) |
O2W—Sm2—N3—C59 | −46.6 (2) | C59—N3—C63—C62 | 3.6 (4) |
O16—Sm2—N3—C59 | 30.1 (2) | Sm2—N3—C63—C62 | −169.3 (2) |
O17—Sm2—N3—C59 | 83.2 (2) | C61—C62—C63—N3 | −1.5 (5) |
O10—Sm2—N3—C59 | −115.8 (2) | C68—N4—C64—C65 | −0.3 (6) |
O11—Sm2—N3—C59 | −120.2 (2) | N4—C64—C65—C66 | 2.5 (6) |
C40—Sm2—N3—C59 | 155.1 (2) | C64—C65—C66—C67 | −2.4 (5) |
C48—Sm2—N3—C59 | 56.4 (2) | C64—C65—C66—C61 | 174.5 (3) |
C32—Sm2—N3—C59 | −115.2 (2) | C60—C61—C66—C65 | −17.0 (5) |
C6—C1—C2—C3 | −1.1 (5) | C62—C61—C66—C65 | 166.1 (3) |
C7—C1—C2—C3 | −179.2 (3) | C60—C61—C66—C67 | 159.7 (3) |
C1—C2—C3—C4 | 0.4 (5) | C62—C61—C66—C67 | −17.1 (5) |
C2—C3—C4—C5 | 1.4 (5) | C65—C66—C67—C68 | 0.4 (5) |
C2—C3—C4—O3 | −179.5 (3) | C61—C66—C67—C68 | −176.5 (3) |
C3—C4—C5—C6 | −2.5 (5) | C64—N4—C68—C67 | −1.9 (6) |
O3—C4—C5—C6 | 178.4 (3) | C66—C67—C68—N4 | 1.9 (6) |
C4—C5—C6—C1 | 1.8 (5) | O2—C8—O1—Sm1 | 9.7 (3) |
C2—C1—C6—C5 | 0.0 (5) | C7—C8—O1—Sm1 | −167.9 (2) |
C7—C1—C6—C5 | 178.2 (3) | O5—Sm1—O1—C8 | −162.32 (17) |
C2—C1—C7—C8 | −48.6 (4) | O4—Sm1—O1—C8 | 142.36 (17) |
C6—C1—C7—C8 | 133.4 (3) | O1W—Sm1—O1—C8 | −12.25 (19) |
C1—C7—C8—O1 | 99.3 (3) | O10—Sm1—O1—C8 | −89.67 (16) |
C1—C7—C8—O2 | −78.3 (3) | O2—Sm1—O1—C8 | −5.50 (15) |
C1—C7—C8—Sm1 | −3.1 (14) | O7—Sm1—O1—C8 | 120.68 (18) |
O5—Sm1—C8—O1 | 17.46 (17) | O8—Sm1—O1—C8 | −131.82 (16) |
O4—Sm1—C8—O1 | −35.80 (16) | N1—Sm1—O1—C8 | 65.50 (16) |
O1W—Sm1—C8—O1 | 169.98 (16) | C16—Sm1—O1—C8 | 170.32 (18) |
O10—Sm1—C8—O1 | 90.41 (16) | C24—Sm1—O1—C8 | 173.7 (2) |
O2—Sm1—C8—O1 | 170.0 (3) | O1—C8—O2—Sm1 | −10.1 (3) |
O7—Sm1—C8—O1 | −106.0 (2) | C7—C8—O2—Sm1 | 167.5 (2) |
O8—Sm1—C8—O1 | 96.9 (2) | O5—Sm1—O2—C8 | 32.73 (18) |
N1—Sm1—C8—O1 | −111.17 (17) | O4—Sm1—O2—C8 | −29.18 (17) |
C16—Sm1—C8—O1 | −9.14 (17) | O1W—Sm1—O2—C8 | 179.93 (17) |
O5—Sm1—C8—O2 | −152.59 (15) | O10—Sm1—O2—C8 | 99.38 (16) |
O4—Sm1—C8—O2 | 154.15 (15) | O7—Sm1—O2—C8 | −132.26 (16) |
O1W—Sm1—C8—O2 | −0.07 (16) | O1—Sm1—O2—C8 | 5.56 (15) |
O10—Sm1—C8—O2 | −79.64 (16) | O8—Sm1—O2—C8 | 142.44 (15) |
O7—Sm1—C8—O2 | 83.9 (2) | N1—Sm1—O2—C8 | −94.42 (16) |
O1—Sm1—C8—O2 | −170.0 (3) | C16—Sm1—O2—C8 | 0.94 (18) |
O8—Sm1—C8—O2 | −73.2 (2) | C24—Sm1—O2—C8 | −173.95 (15) |
N1—Sm1—C8—O2 | 78.78 (16) | O5—C16—O4—Sm1 | 9.9 (3) |
C16—Sm1—C8—O2 | −179.19 (16) | C15—C16—O4—Sm1 | −167.6 (3) |
O5—Sm1—C8—C7 | 125.7 (12) | O5—Sm1—O4—C16 | −5.52 (16) |
O4—Sm1—C8—C7 | 72.5 (12) | O1W—Sm1—O4—C16 | −145.07 (18) |
O1W—Sm1—C8—C7 | −81.8 (12) | O10—Sm1—O4—C16 | 2.2 (2) |
O10—Sm1—C8—C7 | −161.3 (12) | O2—Sm1—O4—C16 | 107.38 (18) |
O2—Sm1—C8—C7 | −81.7 (12) | O7—Sm1—O4—C16 | −112.04 (18) |
O7—Sm1—C8—C7 | 2.3 (13) | O1—Sm1—O4—C16 | 79.52 (18) |
O1—Sm1—C8—C7 | 108.3 (13) | O8—Sm1—O4—C16 | −67.19 (18) |
O8—Sm1—C8—C7 | −154.9 (11) | N1—Sm1—O4—C16 | 170.88 (19) |
N1—Sm1—C8—C7 | −2.9 (12) | C8—Sm1—O4—C16 | 95.12 (18) |
C16—Sm1—C8—C7 | 99.1 (12) | C24—Sm1—O4—C16 | −90.93 (18) |
C14—C9—C10—C11 | 0.4 (5) | O4—C16—O5—Sm1 | −10.0 (3) |
C15—C9—C10—C11 | −179.1 (3) | C15—C16—O5—Sm1 | 167.5 (3) |
C9—C10—C11—C12 | −0.1 (5) | O4—Sm1—O5—C16 | 5.49 (16) |
C10—C11—C12—C13 | −0.8 (5) | O1W—Sm1—O5—C16 | 151.41 (17) |
C10—C11—C12—O6 | 179.1 (3) | O10—Sm1—O5—C16 | −168.04 (18) |
C11—C12—C13—C14 | 1.3 (5) | O2—Sm1—O5—C16 | −95.10 (17) |
O6—C12—C13—C14 | −178.6 (3) | O7—Sm1—O5—C16 | 75.38 (17) |
C12—C13—C14—C9 | −1.0 (5) | O1—Sm1—O5—C16 | −73.45 (17) |
C10—C9—C14—C13 | 0.1 (5) | O8—Sm1—O5—C16 | 122.91 (17) |
C15—C9—C14—C13 | 179.6 (3) | N1—Sm1—O5—C16 | 0.9 (2) |
C10—C9—C15—C16 | −99.8 (4) | C8—Sm1—O5—C16 | −81.26 (17) |
C14—C9—C15—C16 | 80.6 (4) | C24—Sm1—O5—C16 | 99.07 (17) |
C9—C15—C16—O4 | 172.7 (3) | O8—C24—O7—Sm1 | −7.9 (3) |
C9—C15—C16—O5 | −4.9 (4) | C23—C24—O7—Sm1 | 170.0 (3) |
C9—C15—C16—Sm1 | 88.5 (10) | O5—Sm1—O7—C24 | 71.33 (19) |
O5—Sm1—C16—O4 | 170.2 (3) | O4—Sm1—O7—C24 | 121.8 (2) |
O1W—Sm1—C16—O4 | 95.9 (3) | O1W—Sm1—O7—C24 | −74.19 (19) |
O10—Sm1—C16—O4 | −178.23 (17) | O10—Sm1—O7—C24 | −2.5 (2) |
O2—Sm1—C16—O4 | −87.59 (18) | O2—Sm1—O7—C24 | −121.23 (19) |
O7—Sm1—C16—O4 | 64.78 (18) | O1—Sm1—O7—C24 | 142.98 (18) |
O1—Sm1—C16—O4 | −91.43 (18) | O8—Sm1—O7—C24 | 4.32 (17) |
O8—Sm1—C16—O4 | 115.67 (18) | N1—Sm1—O7—C24 | −158.8 (2) |
N1—Sm1—C16—O4 | −9.11 (19) | C16—Sm1—O7—C24 | 97.2 (2) |
C8—Sm1—C16—O4 | −87.17 (18) | C8—Sm1—O7—C24 | −164.0 (2) |
C24—Sm1—C16—O4 | 89.63 (18) | O7—C24—O8—Sm2 | 164.8 (3) |
O4—Sm1—C16—O5 | −170.2 (3) | C23—C24—O8—Sm2 | −13.1 (6) |
O1W—Sm1—C16—O5 | −74.3 (3) | Sm1—C24—O8—Sm2 | 157.3 (4) |
O10—Sm1—C16—O5 | 11.61 (17) | O7—C24—O8—Sm1 | 7.5 (3) |
O2—Sm1—C16—O5 | 102.25 (17) | C23—C24—O8—Sm1 | −170.4 (3) |
O7—Sm1—C16—O5 | −105.38 (17) | O14—Sm2—O8—C24 | −82.6 (4) |
O1—Sm1—C16—O5 | 98.40 (17) | O13—Sm2—O8—C24 | −74.7 (4) |
O8—Sm1—C16—O5 | −54.49 (17) | O2W—Sm2—O8—C24 | 124.6 (4) |
N1—Sm1—C16—O5 | −179.27 (16) | O16—Sm2—O8—C24 | 47.4 (4) |
C8—Sm1—C16—O5 | 102.66 (17) | O17—Sm2—O8—C24 | −1.6 (4) |
C24—Sm1—C16—O5 | −80.53 (17) | O10—Sm2—O8—C24 | −155.1 (4) |
O5—Sm1—C16—C15 | −99.6 (10) | O11—Sm2—O8—C24 | −170.8 (4) |
O4—Sm1—C16—C15 | 90.2 (10) | N3—Sm2—O8—C24 | 76.5 (5) |
O1W—Sm1—C16—C15 | −173.9 (9) | C40—Sm2—O8—C24 | −78.0 (4) |
O10—Sm1—C16—C15 | −88.0 (10) | C48—Sm2—O8—C24 | 23.9 (4) |
O2—Sm1—C16—C15 | 2.7 (10) | C32—Sm2—O8—C24 | −165.7 (4) |
O7—Sm1—C16—C15 | 155.0 (10) | O14—Sm2—O8—Sm1 | 72.61 (11) |
O1—Sm1—C16—C15 | −1.2 (10) | O13—Sm2—O8—Sm1 | 80.48 (8) |
O8—Sm1—C16—C15 | −154.1 (10) | O2W—Sm2—O8—Sm1 | −80.24 (9) |
N1—Sm1—C16—C15 | 81.1 (10) | O16—Sm2—O8—Sm1 | −157.40 (9) |
C8—Sm1—C16—C15 | 3.1 (10) | O17—Sm2—O8—Sm1 | 153.60 (8) |
C24—Sm1—C16—C15 | 179.7 (12) | O10—Sm2—O8—Sm1 | 0.08 (6) |
C22—C17—C18—C19 | 0.3 (4) | O11—Sm2—O8—Sm1 | −15.60 (10) |
C23—C17—C18—C19 | 178.9 (3) | N3—Sm2—O8—Sm1 | −128.35 (14) |
C17—C18—C19—C20 | 0.0 (5) | C40—Sm2—O8—Sm1 | 77.21 (9) |
C18—C19—C20—O9 | −180.0 (3) | C48—Sm2—O8—Sm1 | 179.11 (9) |
C18—C19—C20—C21 | −0.5 (5) | C32—Sm2—O8—Sm1 | −10.57 (9) |
O9—C20—C21—C22 | −179.9 (3) | O5—Sm1—O8—C24 | −113.14 (17) |
C19—C20—C21—C22 | 0.6 (5) | O4—Sm1—O8—C24 | −66.49 (17) |
C18—C17—C22—C21 | −0.2 (5) | O1W—Sm1—O8—C24 | 83.36 (17) |
C23—C17—C22—C21 | −178.8 (3) | O10—Sm1—O8—C24 | 169.19 (18) |
C20—C21—C22—C17 | −0.2 (5) | O2—Sm1—O8—C24 | 121.15 (17) |
C22—C17—C23—C24 | 98.0 (4) | O7—Sm1—O8—C24 | −4.17 (17) |
C18—C17—C23—C24 | −80.5 (4) | O1—Sm1—O8—C24 | −143.66 (18) |
C17—C23—C24—O7 | −45.2 (5) | N1—Sm1—O8—C24 | 15.45 (19) |
C17—C23—C24—O8 | 132.7 (3) | C16—Sm1—O8—C24 | −90.90 (17) |
O5—Sm1—C24—O7 | −109.12 (19) | C8—Sm1—O8—C24 | 162.1 (2) |
O4—Sm1—C24—O7 | −56.05 (19) | O5—Sm1—O8—Sm2 | 77.59 (8) |
O1W—Sm1—C24—O7 | 99.17 (19) | O4—Sm1—O8—Sm2 | 124.24 (8) |
O10—Sm1—C24—O7 | 177.77 (19) | O1W—Sm1—O8—Sm2 | −85.92 (9) |
O2—Sm1—C24—O7 | 93.0 (2) | O10—Sm1—O8—Sm2 | −0.08 (7) |
O1—Sm1—C24—O7 | −85.8 (3) | O2—Sm1—O8—Sm2 | −48.12 (13) |
O8—Sm1—C24—O7 | −172.3 (3) | O7—Sm1—O8—Sm2 | −173.44 (12) |
N1—Sm1—C24—O7 | 20.6 (2) | O1—Sm1—O8—Sm2 | 47.06 (16) |
C16—Sm1—C24—O7 | −82.69 (19) | N1—Sm1—O8—Sm2 | −153.82 (8) |
O5—Sm1—C24—O8 | 63.22 (16) | C16—Sm1—O8—Sm2 | 99.83 (9) |
O4—Sm1—C24—O8 | 116.29 (16) | C8—Sm1—O8—Sm2 | −7.1 (2) |
O1W—Sm1—C24—O8 | −88.49 (17) | C24—Sm1—O8—Sm2 | −169.3 (2) |
O10—Sm1—C24—O8 | −9.89 (17) | O11—C32—O10—Sm1 | −151.8 (2) |
O2—Sm1—C24—O8 | −94.70 (19) | C31—C32—O10—Sm1 | 28.0 (4) |
O7—Sm1—C24—O8 | 172.3 (3) | Sm2—C32—O10—Sm1 | −139.1 (3) |
O1—Sm1—C24—O8 | 86.5 (3) | O11—C32—O10—Sm2 | −12.7 (3) |
N1—Sm1—C24—O8 | −167.03 (16) | C31—C32—O10—Sm2 | 167.1 (2) |
C16—Sm1—C24—O8 | 89.66 (17) | O5—Sm1—O10—C32 | 53.5 (3) |
C30—C25—C26—C27 | −1.0 (4) | O4—Sm1—O10—C32 | 47.1 (3) |
C31—C25—C26—C27 | 177.9 (3) | O1W—Sm1—O10—C32 | −148.6 (3) |
C25—C26—C27—C28 | −0.5 (5) | O2—Sm1—O10—C32 | −73.2 (3) |
C26—C27—C28—O12 | −179.6 (3) | O7—Sm1—O10—C32 | 140.8 (3) |
C26—C27—C28—C29 | 1.5 (5) | O1—Sm1—O10—C32 | −21.8 (3) |
C27—C28—C29—C30 | −1.0 (5) | O8—Sm1—O10—C32 | 135.0 (3) |
O12—C28—C29—C30 | −179.9 (3) | N1—Sm1—O10—C32 | −106.1 (3) |
C28—C29—C30—C25 | −0.6 (5) | C16—Sm1—O10—C32 | 48.1 (3) |
C26—C25—C30—C29 | 1.6 (5) | C8—Sm1—O10—C32 | −47.8 (3) |
C31—C25—C30—C29 | −177.3 (3) | C24—Sm1—O10—C32 | 139.7 (3) |
C30—C25—C31—C32 | 75.7 (4) | O5—Sm1—O10—Sm2 | −81.44 (8) |
C26—C25—C31—C32 | −103.2 (3) | O4—Sm1—O10—Sm2 | −87.86 (10) |
C25—C31—C32—O11 | 12.0 (5) | O1W—Sm1—O10—Sm2 | 76.42 (8) |
C25—C31—C32—O10 | −167.8 (3) | O2—Sm1—O10—Sm2 | 151.85 (8) |
C25—C31—C32—Sm2 | −94.3 (9) | O7—Sm1—O10—Sm2 | 5.86 (11) |
O8—Sm2—C32—O11 | −169.19 (17) | O1—Sm1—O10—Sm2 | −156.70 (8) |
O14—Sm2—C32—O11 | 62.78 (17) | O8—Sm1—O10—Sm2 | 0.07 (6) |
O13—Sm2—C32—O11 | 115.67 (17) | N1—Sm1—O10—Sm2 | 118.99 (15) |
O2W—Sm2—C32—O11 | −91.42 (18) | C16—Sm1—O10—Sm2 | −86.88 (9) |
O16—Sm2—C32—O11 | −93.80 (19) | C8—Sm1—O10—Sm2 | 177.23 (9) |
O17—Sm2—C32—O11 | 70.9 (3) | C24—Sm1—O10—Sm2 | 4.80 (9) |
O10—Sm2—C32—O11 | 167.4 (3) | O8—Sm2—O10—C32 | −154.56 (18) |
N3—Sm2—C32—O11 | −11.50 (18) | O14—Sm2—O10—C32 | 74.28 (16) |
C40—Sm2—C32—O11 | 89.15 (17) | O13—Sm2—O10—C32 | 125.87 (17) |
O8—Sm2—C32—O10 | 23.39 (16) | O2W—Sm2—O10—C32 | −71.46 (16) |
O14—Sm2—C32—O10 | −104.64 (16) | O16—Sm2—O10—C32 | −116.85 (17) |
O13—Sm2—C32—O10 | −51.76 (16) | O17—Sm2—O10—C32 | 140.59 (18) |
O2W—Sm2—C32—O10 | 101.15 (16) | O11—Sm2—O10—C32 | 6.88 (16) |
O16—Sm2—C32—O10 | 98.78 (18) | N3—Sm2—O10—C32 | 1.30 (19) |
O17—Sm2—C32—O10 | −96.5 (3) | C40—Sm2—O10—C32 | 99.62 (17) |
O11—Sm2—C32—O10 | −167.4 (3) | C48—Sm2—O10—C32 | −157.3 (2) |
N3—Sm2—C32—O10 | −178.93 (15) | O8—Sm2—O10—Sm1 | −0.08 (7) |
C40—Sm2—C32—O10 | −78.28 (16) | O14—Sm2—O10—Sm1 | −131.24 (8) |
O8—Sm2—C32—C31 | −56.4 (9) | O13—Sm2—O10—Sm1 | −79.65 (8) |
O14—Sm2—C32—C31 | 175.6 (9) | O2W—Sm2—O10—Sm1 | 83.02 (8) |
O13—Sm2—C32—C31 | −131.5 (9) | O16—Sm2—O10—Sm1 | 37.63 (13) |
O2W—Sm2—C32—C31 | 21.4 (9) | O17—Sm2—O10—Sm1 | −64.93 (16) |
O16—Sm2—C32—C31 | 19.0 (10) | O11—Sm2—O10—Sm1 | 161.36 (12) |
O17—Sm2—C32—C31 | −176.3 (8) | N3—Sm2—O10—Sm1 | 155.78 (8) |
O10—Sm2—C32—C31 | −79.8 (9) | C40—Sm2—O10—Sm1 | −105.90 (8) |
O11—Sm2—C32—C31 | 112.8 (10) | C48—Sm2—O10—Sm1 | −2.8 (3) |
N3—Sm2—C32—C31 | 101.3 (9) | C32—Sm2—O10—Sm1 | 154.5 (2) |
C40—Sm2—C32—C31 | −158.0 (9) | O10—C32—O11—Sm2 | 12.5 (3) |
C38—C33—C34—C35 | −0.1 (5) | C31—C32—O11—Sm2 | −167.3 (3) |
C39—C33—C34—C35 | 179.2 (3) | O8—Sm2—O11—C32 | 11.97 (19) |
C33—C34—C35—C36 | −0.4 (5) | O14—Sm2—O11—C32 | −112.65 (18) |
C34—C35—C36—O15 | −179.4 (3) | O13—Sm2—O11—C32 | −66.94 (18) |
C34—C35—C36—C37 | 0.3 (5) | O2W—Sm2—O11—C32 | 80.11 (18) |
O15—C36—C37—C38 | 179.9 (3) | O16—Sm2—O11—C32 | 119.63 (18) |
C35—C36—C37—C38 | 0.2 (5) | O17—Sm2—O11—C32 | −149.20 (17) |
C34—C33—C38—C37 | 0.6 (5) | O10—Sm2—O11—C32 | −7.00 (16) |
C39—C33—C38—C37 | −178.7 (3) | N3—Sm2—O11—C32 | 168.36 (18) |
C36—C37—C38—C33 | −0.6 (5) | C40—Sm2—O11—C32 | −89.78 (18) |
C38—C33—C39—C40 | −114.4 (3) | C48—Sm2—O11—C32 | 161.98 (19) |
C34—C33—C39—C40 | 66.3 (4) | O14—C40—O13—Sm2 | 1.1 (3) |
C33—C39—C40—O14 | 173.8 (3) | C39—C40—O13—Sm2 | −177.3 (2) |
C33—C39—C40—O13 | −7.8 (4) | O8—Sm2—O13—C40 | −172.88 (18) |
O8—Sm2—C40—O14 | −171.84 (16) | O14—Sm2—O13—C40 | −0.63 (16) |
O13—Sm2—C40—O14 | −178.9 (3) | O2W—Sm2—O13—C40 | −135.63 (18) |
O2W—Sm2—C40—O14 | −83.0 (2) | O16—Sm2—O13—C40 | 115.71 (17) |
O16—Sm2—C40—O14 | 100.50 (17) | O17—Sm2—O13—C40 | 84.53 (17) |
O17—Sm2—C40—O14 | 92.67 (17) | O10—Sm2—O13—C40 | −102.81 (17) |
O10—Sm2—C40—O14 | −106.64 (17) | O11—Sm2—O13—C40 | −59.52 (17) |
O11—Sm2—C40—O14 | −56.52 (17) | N3—Sm2—O13—C40 | 21.7 (2) |
N3—Sm2—C40—O14 | 18.84 (18) | C48—Sm2—O13—C40 | 97.69 (17) |
C48—Sm2—C40—O14 | 94.02 (17) | C32—Sm2—O13—C40 | −82.41 (17) |
C32—Sm2—C40—O14 | −81.54 (17) | O13—C40—O14—Sm2 | −1.1 (3) |
O8—Sm2—C40—O13 | 7.03 (17) | C39—C40—O14—Sm2 | 177.3 (2) |
O14—Sm2—C40—O13 | 178.9 (3) | O8—Sm2—O14—C40 | 10.1 (2) |
O2W—Sm2—C40—O13 | 95.9 (2) | O13—Sm2—O14—C40 | 0.64 (16) |
O16—Sm2—C40—O13 | −80.64 (18) | O2W—Sm2—O14—C40 | 140.64 (16) |
O17—Sm2—C40—O13 | −88.47 (17) | O16—Sm2—O14—C40 | −99.49 (17) |
O10—Sm2—C40—O13 | 72.22 (16) | O17—Sm2—O14—C40 | −80.88 (17) |
O11—Sm2—C40—O13 | 122.35 (17) | O10—Sm2—O14—C40 | 71.96 (17) |
N3—Sm2—C40—O13 | −162.29 (16) | O11—Sm2—O14—C40 | 119.62 (17) |
C48—Sm2—C40—O13 | −87.11 (17) | N3—Sm2—O14—C40 | −160.90 (18) |
C32—Sm2—C40—O13 | 97.32 (17) | C48—Sm2—O14—C40 | −91.52 (17) |
C46—C41—C42—C43 | 0.0 (4) | C32—Sm2—O14—C40 | 96.54 (17) |
C47—C41—C42—C43 | 177.1 (3) | O17—C48—O16—Sm2 | 9.3 (3) |
C41—C42—C43—C44 | −1.3 (5) | C47—C48—O16—Sm2 | −169.6 (2) |
C42—C43—C44—O18 | −178.4 (3) | O8—Sm2—O16—C48 | −112.93 (16) |
C42—C43—C44—C45 | 1.9 (5) | O14—Sm2—O16—C48 | 18.30 (19) |
O18—C44—C45—C46 | 179.2 (3) | O13—Sm2—O16—C48 | −44.99 (17) |
C43—C44—C45—C46 | −1.3 (5) | O2W—Sm2—O16—C48 | 166.54 (17) |
C44—C45—C46—C41 | −0.1 (5) | O17—Sm2—O16—C48 | −5.15 (15) |
C42—C41—C46—C45 | 0.7 (4) | O10—Sm2—O16—C48 | −147.80 (15) |
C47—C41—C46—C45 | −176.5 (3) | O11—Sm2—O16—C48 | 127.73 (16) |
C42—C41—C47—C48 | −69.6 (4) | N3—Sm2—O16—C48 | 79.21 (16) |
C46—C41—C47—C48 | 107.4 (3) | C40—Sm2—O16—C48 | −14.81 (19) |
C41—C47—C48—O16 | 57.3 (4) | C32—Sm2—O16—C48 | 168.84 (15) |
C41—C47—C48—O17 | −121.6 (3) | O16—C48—O17—Sm2 | −9.0 (3) |
O8—Sm2—C48—O16 | 65.60 (16) | C47—C48—O17—Sm2 | 169.9 (2) |
O14—Sm2—C48—O16 | −165.05 (15) | O8—Sm2—O17—C48 | 77.00 (17) |
O13—Sm2—C48—O16 | 140.81 (15) | O14—Sm2—O17—C48 | −155.86 (17) |
O2W—Sm2—C48—O16 | −13.28 (17) | O13—Sm2—O17—C48 | 149.37 (18) |
O17—Sm2—C48—O16 | 170.8 (3) | O2W—Sm2—O17—C48 | −5.1 (2) |
O10—Sm2—C48—O16 | 68.1 (3) | O16—Sm2—O17—C48 | 5.04 (15) |
O11—Sm2—C48—O16 | −87.5 (2) | O10—Sm2—O17—C48 | 134.67 (16) |
N3—Sm2—C48—O16 | −93.97 (16) | O11—Sm2—O17—C48 | −120.14 (17) |
C40—Sm2—C48—O16 | 167.87 (16) | N3—Sm2—O17—C48 | −78.00 (17) |
O8—Sm2—C48—O17 | −105.24 (17) | C40—Sm2—O17—C48 | 176.99 (18) |
O14—Sm2—C48—O17 | 24.12 (17) | C32—Sm2—O17—C48 | −164.1 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3B···O12i | 0.82 | 1.94 | 2.749 (3) | 169 |
O6—H6B···O3Wii | 0.82 | 1.86 | 2.642 (3) | 159 |
O9—H9A···O17iii | 0.82 | 1.86 | 2.673 (3) | 173 |
O12—H12A···O11iv | 0.82 | 1.94 | 2.746 (3) | 168 |
O15—H15C···O6v | 0.82 | 1.91 | 2.722 (3) | 174 |
O18—H18B···O9ii | 0.82 | 1.95 | 2.768 (3) | 173 |
O2W—H2WA···O5 | 0.83 (5) | 2.02 (5) | 2.767 (3) | 150 (4) |
O2W—H2WB···N2ii | 0.83 (2) | 2.03 (2) | 2.841 (3) | 164 (5) |
O3W—H3WB···O3 | 0.85 (4) | 1.99 (2) | 2.816 (3) | 167 (5) |
O1W—H1WA···O13 | 0.81 (5) | 1.96 (4) | 2.755 (3) | 165 (4) |
O1W—H1WB···N4i | 0.83 (2) | 1.99 (2) | 2.778 (3) | 160 (4) |
O3W—H3WA···O1vi | 0.84 (4) | 1.94 (4) | 2.773 (3) | 172 (4) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, −y+1, −z; (iv) −x, −y, −z+1; (v) x−1, y+1, z; (vi) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O |
Mr | 1573.96 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 11.7589 (3), 16.3141 (4), 18.4618 (5) |
α, β, γ (°) | 83.619 (1), 72.025 (1), 70.941 (1) |
V (Å3) | 3183.90 (14) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.91 |
Crystal size (mm) | 0.34 × 0.14 × 0.03 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.733, 0.941 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 49293, 14715, 11851 |
Rint | 0.047 |
(sin θ/λ)max (Å−1) | 0.654 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.070, 1.02 |
No. of reflections | 14715 |
No. of parameters | 875 |
No. of restraints | 9 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.66, −0.72 |
Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3B···O12i | 0.82 | 1.94 | 2.749 (3) | 169.4 |
O6—H6B···O3Wii | 0.82 | 1.86 | 2.642 (3) | 159.2 |
O9—H9A···O17iii | 0.82 | 1.86 | 2.673 (3) | 172.8 |
O12—H12A···O11iv | 0.82 | 1.94 | 2.746 (3) | 167.7 |
O15—H15C···O6v | 0.82 | 1.91 | 2.722 (3) | 173.5 |
O18—H18B···O9ii | 0.82 | 1.95 | 2.768 (3) | 173.2 |
O2W—H2WA···O5 | 0.83 (5) | 2.02 (5) | 2.767 (3) | 150 (4) |
O2W—H2WB···N2ii | 0.834 (18) | 2.03 (2) | 2.841 (3) | 164 (5) |
O3W—H3WB···O3 | 0.85 (4) | 1.99 (2) | 2.816 (3) | 167 (5) |
O1W—H1WA···O13 | 0.81 (5) | 1.96 (4) | 2.755 (3) | 165 (4) |
O1W—H1WB···N4i | 0.826 (18) | 1.99 (2) | 2.778 (3) | 160 (4) |
O3W—H3WA···O1vi | 0.84 (4) | 1.94 (4) | 2.773 (3) | 172 (4) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, −y+1, −z; (iv) −x, −y, −z+1; (v) x−1, y+1, z; (vi) −x+1, −y+1, −z+1. |
References
Arias, J. C., Cabrera, A., Sharma, P., Rosas, N. & Hernandez, S. (2000). Inorg. Chim. Acta, 310, 261–264. CAS Google Scholar
Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Fang, R.-Q. & Zhang, X.-M. (2006). Inorg. Chem. 45, 4801–4810. Web of Science CSD CrossRef PubMed CAS Google Scholar
Liu, J.-L., Li, H.-Q. & Zhao, G.-L. (2010). Acta Cryst. E66, m9. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, G.-H., Lei, Y.-Q. & Wang, N. (2010). Cryst. Growth Des. 10, 4060–4067. Google Scholar
Wang, X.-X. & Sevov, S. (2008). Inorg. Chem. 47, 1037–1043. Web of Science CSD CrossRef PubMed CAS Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
The design and synthesis of carboxylic metal-organic complexes have been an increasing interest for decades owing to their potential practical applications, such as fluorescence and magnetism (Wang, et al., 2010; Fang et al., 2006; Wang, et al., 2008). We have published on this subject before (Liu, et al., 2010). In the current paper we report the crystal structure of a new SmIII complex with the ligand p- hydroxyphenylacetic acid. The title compound consist of six L ligands, two bipy molecules and two coordinated water molecules. In the dinuclear compound, each Sm ion is coordinated with seven O atoms from four L ligands, one N atom from 4,4'-bipyridine ligand and one O atom from a water molecule. The central Sm atom is nine coordinated. The PAA ligands are coordinating in two modes, bridging and bridging tridentate. (Fig.1). The SmIII ion is in a distorted ball coordination geometry. The asymmetric unit further contains one solvent water molecule. Bond lengths and bond angles involving the metals and O atoms skeleton compare well with related structure as bis((µ2-Acetato-O,O,O')-diaqua-bis(acetato-O,O') -samarium(iii))pentahydrate (Arias, et al., 2000), In addition, numerous O—H···O bonds involving both hydroxyl groups as well as coordinated and non-coordinated water molecules build up an intricate threedimensional network (Table 1).