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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1511-m1512
https://doi.org/10.1107/S1600536810044454

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

Jia-Lu Liu,a Jian-Feng Liua and Guo-Liang Zhaoa*

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

(Received 12 October 2010; accepted 31 October 2010; online 6 November 2010)

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 asymmetric unit 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[Arias, J. C., Cabrera, A., Sharma, P., Rosas, N. & Hernandez, S. (2000). Inorg. Chim. Acta, 310, 261-264.]); Liu et al. (2010[Liu, J.-L., Li, H.-Q. & Zhao, G.-L. (2010). Acta Cryst. E66, m9.]). For applications of carb­oxy­lic metal-organic complexes, see: Wang & Sevov (2008[Wang, X.-X. & Sevov, S. (2008). Inorg. Chem. 47, 1037-1043.]); Wang et al. (2010[Wang, G.-H., Lei, Y.-Q. & Wang, N. (2010). Cryst. Growth Des. 10, 4060-4067.]); Fang & Zhang (2006[Fang, R.-Q. & Zhang, X.-M. (2006). Inorg. Chem. 45, 4801-4810.]).

[Scheme 1]

Experimental

Crystal data

  • [Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2O

  • Mr = 1573.96

  • Triclinic, [P \overline 1]

  • a = 11.7589 (3) Å

  • b = 16.3141 (4) Å

  • c = 18.4618 (5) Å

  • α = 83.619 (1)°

  • β = 72.025 (1)°

  • γ = 70.941 (1)°

  • V = 3183.90 (14) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.91 mm−1

  • T = 296 K

  • 0.34 × 0.14 × 0.03 mm
Data collection

  • Bruker APEXII area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.733, Tmax = 0.941

  • 49293 measured reflections

  • 14715 independent reflections

  • 11851 reflections with I > 2σ(I)

  • Rint = 0.047
Refinement

  • R[F2 > 2σ(F2)] = 0.029

  • wR(F2) = 0.070

  • S = 1.02

  • 14715 reflections

  • 875 parameters

  • 9 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.66 e Å−3

  • Δρmin = −0.72 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

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.

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810044454/kj2162sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810044454/kj2162Isup2.hkl

checkCIF report


Comment top

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).

Related literature top

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 top

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.

Refinement top

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 refinement 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 refinement they were treated as riding on their parent O atom.

Structure description top

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).

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).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: 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).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title complex, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.
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 top
Crystal data top
[Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2OZ = 2
Mr = 1573.96F(000) = 1584
Triclinic, P1Dx = 1.642 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.7589 (3) ÅCell parameters from 9956 reflections
b = 16.3141 (4) Åθ = 1.7–27.7°
c = 18.4618 (5) ŵ = 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
Data collection top
Bruker APEXII area-detector
diffractometer		14715 independent reflections
Radiation source: fine-focus sealed tube11851 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
phi and ω scansθmax = 27.7°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −15→15
Tmin = 0.733, Tmax = 0.941k = −21→21
49293 measured reflectionsl = −24→24
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H 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 parametersΔρmax = 0.66 e Å−3
9 restraintsΔρmin = −0.72 e Å−3
Crystal data top
[Sm2(C8H7O3)6(C10H8N2)2(H2O)2]·H2Oγ = 70.941 (1)°
Mr = 1573.96V = 3183.90 (14) Å3
Triclinic, P1Z = 2
a = 11.7589 (3) ÅMo Kα radiation
b = 16.3141 (4) ŵ = 1.91 mm−1
c = 18.4618 (5) ÅT = 296 K
α = 83.619 (1)°0.34 × 0.14 × 0.03 mm
β = 72.025 (1)°
Data collection top
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 = 0.941Rint = 0.047
49293 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0299 restraints
wR(F2) = 0.070H atoms treated by a mixture of independent and constrained refinement
S = 1.02Δρmax = 0.66 e Å−3
14715 reflectionsΔρmin = −0.72 e Å−3
875 parameters
Special details top

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) top
xyzUiso*/Ueq
Sm10.271174 (13)0.364512 (8)0.283786 (7)0.02579 (4)
Sm20.131899 (13)0.206492 (8)0.195381 (7)0.02577 (4)
N10.3136 (2)0.51130 (14)0.28289 (14)0.0359 (6)
N20.3976 (3)0.92617 (19)0.2162 (2)0.0667 (10)
N30.0840 (2)0.06204 (14)0.18856 (13)0.0337 (5)
N40.0282 (4)−0.36185 (19)0.2326 (2)0.0683 (10)
C10.2248 (3)0.51101 (19)0.51768 (16)0.0363 (7)
C20.3403 (3)0.5160 (2)0.47296 (17)0.0458 (8)
H2A0.39620.46890.44330.055*
C30.3750 (3)0.5896 (2)0.47116 (19)0.0505 (8)
H3A0.45330.59180.44040.061*
C40.2940 (3)0.6592 (2)0.51481 (19)0.0449 (8)
C50.1799 (3)0.6549 (2)0.56137 (19)0.0482 (8)
H5A0.12610.70130.59260.058*
C60.1449 (3)0.5823 (2)0.56210 (18)0.0445 (8)
H6A0.06640.58080.59290.053*
C70.1855 (3)0.4307 (2)0.52126 (16)0.0429 (8)
H7A0.23160.38550.54970.052*
H7B0.09670.44400.54810.052*
C80.2096 (3)0.39816 (19)0.44318 (16)0.0355 (7)
C90.6232 (3)0.08807 (18)0.30336 (18)0.0378 (7)
C100.6052 (3)0.0570 (2)0.37691 (18)0.0492 (8)
H10A0.59380.09370.41540.059*
C110.6033 (3)−0.0276 (2)0.39568 (18)0.0494 (8)
H11A0.5911−0.04720.44590.059*
C120.6199 (3)−0.08171 (18)0.33913 (17)0.0394 (7)
C130.6364 (3)−0.0518 (2)0.26524 (17)0.0438 (8)
H13A0.6459−0.08820.22700.053*
C140.6389 (3)0.03153 (19)0.24766 (17)0.0432 (7)
H14A0.65150.05060.19730.052*
C150.6269 (3)0.17940 (19)0.2834 (2)0.0478 (8)
H15A0.69390.17830.23670.057*
H15B0.64750.20050.32330.057*
C160.5063 (3)0.24269 (17)0.27316 (16)0.0331 (6)
C170.2720 (3)0.4547 (2)0.01289 (16)0.0424 (8)
C180.1461 (4)0.5016 (2)0.02779 (17)0.0497 (9)
H18A0.08610.47470.05370.060*
C190.1070 (3)0.5873 (2)0.00524 (17)0.0453 (8)
H19A0.02180.61770.01580.054*
C200.1963 (3)0.62750 (19)−0.03339 (17)0.0405 (7)
C210.3219 (3)0.58206 (19)−0.04820 (17)0.0415 (7)
H21A0.38200.6090−0.07370.050*
C220.3589 (3)0.4964 (2)−0.02525 (17)0.0434 (7)
H22A0.44420.4662−0.03570.052*
C230.3132 (4)0.3613 (2)0.03920 (17)0.0587 (10)
H23A0.25870.33160.03150.070*
H23B0.39810.33280.00850.070*
C240.3094 (3)0.35389 (17)0.12169 (15)0.0330 (6)
C250.1416 (3)0.11314 (19)0.47589 (16)0.0392 (7)
C260.0393 (3)0.1063 (2)0.53593 (17)0.0434 (7)
H26A−0.02930.15540.55210.052*
C270.0378 (3)0.0273 (2)0.57213 (17)0.0421 (7)
H27A−0.03120.02380.61250.051*
C280.1382 (3)−0.04551 (19)0.54821 (16)0.0359 (7)
C290.2418 (3)−0.0397 (2)0.48932 (17)0.0437 (7)
H29A0.3106−0.08880.47350.052*
C300.2428 (3)0.0393 (2)0.45411 (17)0.0436 (8)
H30A0.31310.04290.41480.052*
C310.1430 (4)0.1978 (2)0.43418 (17)0.0461 (8)
H31A0.22380.20580.42740.055*
H31B0.07910.24460.46570.055*
C320.1204 (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−0.17670.48450.13130.048*
C35−0.2258 (3)0.60528 (19)0.16781 (17)0.0412 (7)
H35A−0.19630.62900.12030.049*
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−0.36220.65600.34450.052*
C38−0.3109 (3)0.53371 (19)0.30752 (17)0.0396 (7)
H38A−0.33940.50990.35520.048*
C39−0.2442 (3)0.38587 (17)0.25117 (18)0.0385 (7)
H39A−0.28960.37380.30260.046*
H39B−0.28480.37360.21710.046*
C40−0.1118 (3)0.32472 (17)0.23337 (15)0.0309 (6)
C410.2359 (3)0.05195 (19)−0.04822 (16)0.0395 (7)
C420.3536 (3)0.0011 (2)−0.04455 (16)0.0430 (7)
H42A0.41010.0278−0.04050.052*
C430.3896 (3)−0.0878 (2)−0.04677 (17)0.0458 (8)
H43A0.4701−0.1206−0.04520.055*
C440.3057 (3)−0.1283 (2)−0.05126 (18)0.0483 (8)
C450.1879 (3)−0.0793 (2)−0.05580 (19)0.0506 (8)
H45A0.1316−0.1062−0.05980.061*
C460.1538 (3)0.0102 (2)−0.05431 (17)0.0466 (8)
H46A0.07420.0431−0.05750.056*
C470.1936 (3)0.1500 (2)−0.04211 (17)0.0464 (8)
H47A0.25640.1724−0.07810.056*
H47B0.11560.1742−0.05560.056*
C480.1739 (3)0.17845 (18)0.03700 (16)0.0358 (7)
C490.2317 (3)0.58065 (18)0.32245 (17)0.0385 (7)
H49A0.15900.57450.35780.046*
C500.2495 (3)0.66107 (18)0.31352 (17)0.0404 (7)
H50A0.18970.70750.34260.048*
C510.3563 (3)0.67260 (18)0.26136 (17)0.0377 (7)
C520.4429 (3)0.60032 (19)0.22209 (19)0.0455 (8)
H52A0.51750.60440.18740.055*
C530.4187 (3)0.52211 (19)0.23437 (19)0.0435 (8)
H53A0.47870.47420.20740.052*
C540.4496 (4)0.8649 (2)0.1638 (3)0.0724 (13)
H54A0.49490.87870.11580.087*
C550.4407 (3)0.7819 (2)0.1761 (2)0.0588 (10)
H55A0.47880.74170.13710.071*
C560.3751 (3)0.75940 (19)0.24675 (19)0.0427 (8)
C570.3238 (4)0.8221 (2)0.3018 (2)0.0613 (10)
H57A0.28100.80960.35110.074*
C580.3363 (5)0.9036 (2)0.2835 (3)0.0726 (12)
H58A0.29880.94520.32140.087*
C590.1697 (3)−0.00447 (18)0.14641 (17)0.0406 (7)
H59A0.24280.00420.11360.049*
C600.1549 (3)−0.08558 (18)0.14936 (17)0.0420 (7)
H60A0.2165−0.12940.11800.050*
C610.0493 (3)−0.10176 (18)0.19860 (17)0.0376 (7)
C62−0.0413 (3)−0.03205 (19)0.24020 (18)0.0417 (7)
H62A−0.1156−0.03900.27290.050*
C63−0.0217 (3)0.04762 (18)0.23331 (17)0.0390 (7)
H63A−0.08500.09360.26110.047*
C640.1071 (5)−0.3394 (2)0.1717 (2)0.0729 (13)
H64A0.1613−0.38240.13700.088*
C650.1141 (4)−0.2559 (2)0.1565 (2)0.0635 (11)
H65A0.1694−0.24360.11160.076*
C660.0382 (3)−0.19087 (19)0.20833 (19)0.0445 (8)
C67−0.0452 (3)−0.2136 (2)0.2724 (2)0.0622 (11)
H67A−0.0988−0.17250.30900.075*
C68−0.0474 (4)−0.2986 (2)0.2811 (3)0.0751 (14)
H68A−0.1056−0.31240.32360.090*
O1W0.0812 (2)0.45996 (13)0.25489 (13)0.0402 (5)
O10.3063 (2)0.33572 (14)0.41483 (12)0.0464 (5)
O2W0.3290 (2)0.11013 (13)0.21451 (13)0.0413 (5)
O20.13551 (19)0.43506 (13)0.40444 (11)0.0393 (5)
O30.3309 (2)0.73187 (16)0.51131 (16)0.0669 (7)
H3B0.27290.77030.53720.057 (12)*
O3W0.5581 (3)0.76686 (17)0.49096 (15)0.0579 (6)
O40.49742 (19)0.32158 (12)0.26433 (13)0.0470 (6)
O50.41478 (19)0.21718 (12)0.27608 (12)0.0400 (5)
O60.6210 (3)−0.16638 (13)0.35286 (12)0.0596 (7)
H6B0.5940−0.17420.39880.089*
O70.3524 (2)0.40008 (14)0.14780 (11)0.0460 (6)
O80.25816 (18)0.30140 (11)0.16494 (10)0.0319 (4)
O90.1635 (2)0.71240 (14)−0.05719 (14)0.0560 (6)
H9A0.09280.7265−0.06240.084*
O100.14230 (18)0.26764 (11)0.31403 (10)0.0308 (4)
O110.0819 (2)0.15184 (12)0.33561 (10)0.0379 (5)
O120.1417 (2)−0.12554 (13)0.58163 (12)0.0468 (5)
H12A0.0699−0.12590.60430.070*
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−0.31830.76710.26260.084*
O160.2617 (2)0.15313 (13)0.06689 (11)0.0410 (5)
O170.0674 (2)0.22729 (14)0.07417 (12)0.0479 (5)
O180.3448 (3)−0.21694 (15)−0.05145 (16)0.0742 (8)
H18B0.2885−0.2341−0.05490.111*
H2WA0.377 (4)0.125 (3)0.231 (3)0.111*
H2WB0.362 (4)0.0568 (13)0.208 (3)0.111*
H3WB0.497 (3)0.748 (3)0.495 (3)0.111*
H1WA0.043 (4)0.436 (2)0.239 (3)0.111*
H1WB0.048 (4)0.5124 (12)0.249 (3)0.111*
H3WA0.594 (4)0.734 (3)0.521 (2)0.111*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm10.02854 (8)0.01798 (7)0.03435 (8)−0.00970 (6)−0.01220 (6)0.00222 (5)
Sm20.02720 (8)0.01720 (7)0.03501 (8)−0.00788 (6)−0.01100 (6)0.00011 (5)
N10.0358 (15)0.0245 (12)0.0504 (15)−0.0115 (11)−0.0146 (12)−0.0006 (10)
N20.065 (2)0.0320 (16)0.121 (3)−0.0237 (16)−0.049 (2)0.0175 (18)
N30.0388 (15)0.0216 (11)0.0433 (14)−0.0100 (10)−0.0154 (11)0.0014 (10)
N40.084 (3)0.0323 (17)0.119 (3)−0.0256 (17)−0.070 (2)0.0171 (18)
C10.0403 (18)0.0384 (16)0.0334 (15)−0.0138 (14)−0.0124 (13)−0.0034 (12)
C20.0385 (19)0.0460 (19)0.0467 (18)−0.0089 (15)−0.0036 (15)−0.0133 (14)
C30.0343 (18)0.053 (2)0.060 (2)−0.0180 (16)0.0001 (16)−0.0114 (16)
C40.0403 (19)0.0419 (18)0.055 (2)−0.0162 (15)−0.0129 (16)−0.0037 (14)
C50.0385 (19)0.0425 (18)0.059 (2)−0.0096 (15)−0.0063 (16)−0.0140 (15)
C60.0358 (18)0.0426 (18)0.0514 (19)−0.0124 (15)−0.0034 (15)−0.0115 (14)
C70.056 (2)0.0414 (18)0.0351 (16)−0.0220 (16)−0.0108 (15)0.0002 (13)
C80.0425 (19)0.0340 (16)0.0354 (15)−0.0216 (14)−0.0093 (14)0.0027 (12)
C90.0284 (16)0.0280 (15)0.060 (2)−0.0047 (12)−0.0215 (14)−0.0002 (13)
C100.067 (2)0.0310 (17)0.0507 (19)−0.0045 (16)−0.0273 (18)−0.0096 (14)
C110.069 (2)0.0375 (18)0.0395 (17)−0.0109 (16)−0.0179 (17)−0.0032 (13)
C120.0428 (19)0.0300 (15)0.0434 (17)−0.0105 (13)−0.0105 (14)−0.0006 (12)
C130.056 (2)0.0346 (17)0.0419 (17)−0.0125 (15)−0.0155 (15)−0.0059 (13)
C140.051 (2)0.0368 (17)0.0403 (17)−0.0120 (15)−0.0145 (15)0.0047 (13)
C150.0329 (18)0.0280 (16)0.088 (2)−0.0069 (13)−0.0296 (17)0.0056 (15)
C160.0306 (16)0.0269 (14)0.0416 (16)−0.0067 (12)−0.0124 (13)−0.0004 (11)
C170.066 (2)0.0394 (17)0.0331 (16)−0.0272 (17)−0.0205 (15)0.0043 (12)
C180.067 (3)0.063 (2)0.0339 (16)−0.045 (2)−0.0108 (16)0.0033 (15)
C190.0409 (19)0.056 (2)0.0424 (18)−0.0187 (16)−0.0106 (15)−0.0078 (15)
C200.053 (2)0.0359 (16)0.0438 (17)−0.0191 (15)−0.0251 (15)0.0029 (13)
C210.046 (2)0.0366 (17)0.0500 (18)−0.0219 (15)−0.0177 (15)0.0086 (13)
C220.051 (2)0.0382 (17)0.0470 (18)−0.0170 (15)−0.0214 (16)0.0045 (13)
C230.112 (3)0.0389 (18)0.0380 (18)−0.037 (2)−0.0281 (19)0.0078 (14)
C240.0423 (18)0.0254 (14)0.0322 (14)−0.0139 (13)−0.0086 (13)0.0006 (11)
C250.058 (2)0.0380 (17)0.0354 (16)−0.0256 (16)−0.0236 (15)0.0076 (12)
C260.052 (2)0.0332 (16)0.0448 (18)−0.0104 (15)−0.0177 (16)−0.0001 (13)
C270.0437 (19)0.0457 (18)0.0366 (16)−0.0181 (15)−0.0084 (14)0.0049 (13)
C280.0446 (19)0.0354 (16)0.0358 (15)−0.0204 (14)−0.0179 (14)0.0096 (12)
C290.043 (2)0.0442 (18)0.0441 (18)−0.0155 (15)−0.0135 (15)0.0063 (14)
C300.047 (2)0.051 (2)0.0387 (17)−0.0268 (17)−0.0119 (15)0.0109 (14)
C310.072 (2)0.0375 (17)0.0451 (18)−0.0312 (17)−0.0274 (17)0.0092 (13)
C320.0301 (16)0.0266 (14)0.0387 (15)−0.0133 (12)−0.0089 (12)0.0021 (11)
C330.0274 (15)0.0256 (14)0.0424 (16)−0.0039 (11)−0.0123 (13)−0.0026 (11)
C340.0435 (19)0.0350 (16)0.0377 (16)−0.0063 (14)−0.0088 (14)−0.0122 (12)
C350.047 (2)0.0363 (17)0.0385 (16)−0.0137 (14)−0.0100 (14)0.0015 (13)
C360.0421 (19)0.0273 (15)0.0491 (18)−0.0069 (13)−0.0192 (15)−0.0014 (12)
C370.052 (2)0.0341 (16)0.0404 (17)−0.0069 (15)−0.0140 (15)−0.0077 (13)
C380.0403 (18)0.0344 (16)0.0390 (16)−0.0077 (13)−0.0087 (14)0.0001 (12)
C390.0309 (17)0.0268 (15)0.0569 (19)−0.0050 (12)−0.0144 (14)−0.0035 (13)
C400.0306 (16)0.0234 (13)0.0403 (15)−0.0060 (12)−0.0138 (13)−0.0036 (11)
C410.050 (2)0.0382 (17)0.0303 (15)−0.0157 (15)−0.0087 (14)−0.0027 (12)
C420.048 (2)0.0441 (18)0.0407 (17)−0.0219 (16)−0.0106 (15)−0.0005 (13)
C430.048 (2)0.0385 (18)0.0484 (19)−0.0121 (15)−0.0103 (15)−0.0027 (14)
C440.059 (2)0.0353 (17)0.0499 (19)−0.0194 (16)−0.0095 (17)−0.0024 (14)
C450.053 (2)0.049 (2)0.057 (2)−0.0267 (18)−0.0118 (17)−0.0055 (16)
C460.043 (2)0.049 (2)0.0451 (18)−0.0098 (16)−0.0112 (15)−0.0086 (14)
C470.062 (2)0.0369 (17)0.0376 (17)−0.0106 (16)−0.0155 (16)0.0003 (13)
C480.050 (2)0.0246 (14)0.0339 (15)−0.0152 (14)−0.0098 (14)0.0010 (11)
C490.0425 (19)0.0296 (15)0.0442 (17)−0.0142 (14)−0.0111 (14)0.0019 (12)
C500.0465 (19)0.0244 (15)0.0516 (18)−0.0103 (13)−0.0165 (15)−0.0014 (12)
C510.0402 (18)0.0245 (14)0.0552 (18)−0.0129 (13)−0.0222 (15)0.0044 (12)
C520.0345 (18)0.0329 (16)0.070 (2)−0.0153 (14)−0.0117 (16)0.0025 (15)
C530.0365 (18)0.0257 (15)0.067 (2)−0.0103 (13)−0.0112 (16)−0.0048 (14)
C540.054 (3)0.041 (2)0.114 (3)−0.0220 (19)−0.013 (2)0.023 (2)
C550.049 (2)0.0320 (18)0.085 (3)−0.0160 (16)−0.0029 (19)0.0024 (17)
C560.0408 (19)0.0270 (15)0.069 (2)−0.0149 (14)−0.0258 (16)0.0054 (14)
C570.094 (3)0.0378 (19)0.065 (2)−0.031 (2)−0.033 (2)0.0052 (16)
C580.112 (4)0.039 (2)0.089 (3)−0.034 (2)−0.049 (3)0.0000 (19)
C590.0458 (19)0.0291 (15)0.0432 (17)−0.0120 (14)−0.0086 (15)0.0028 (12)
C600.051 (2)0.0242 (15)0.0479 (18)−0.0088 (14)−0.0123 (15)−0.0038 (12)
C610.0477 (19)0.0276 (15)0.0493 (17)−0.0142 (14)−0.0303 (15)0.0072 (12)
C620.0391 (18)0.0327 (16)0.0574 (19)−0.0172 (14)−0.0145 (15)0.0034 (14)
C630.0381 (18)0.0269 (15)0.0547 (18)−0.0122 (13)−0.0145 (15)−0.0014 (13)
C640.133 (4)0.035 (2)0.076 (3)−0.028 (2)−0.063 (3)−0.0010 (18)
C650.118 (4)0.0349 (19)0.055 (2)−0.032 (2)−0.043 (2)0.0041 (15)
C660.056 (2)0.0276 (15)0.066 (2)−0.0162 (15)−0.0398 (18)0.0080 (14)
C670.045 (2)0.0343 (18)0.109 (3)−0.0162 (16)−0.026 (2)0.0130 (19)
C680.054 (3)0.039 (2)0.145 (4)−0.0274 (19)−0.044 (3)0.030 (2)
O1W0.0430 (13)0.0232 (10)0.0624 (14)−0.0089 (9)−0.0288 (11)0.0028 (9)
O10.0521 (15)0.0388 (12)0.0462 (12)−0.0040 (11)−0.0207 (11)−0.0047 (10)
O2W0.0404 (13)0.0237 (10)0.0655 (14)−0.0073 (9)−0.0257 (11)−0.0013 (10)
O20.0383 (12)0.0408 (12)0.0412 (11)−0.0132 (10)−0.0135 (10)−0.0021 (9)
O30.0475 (15)0.0463 (14)0.105 (2)−0.0237 (13)−0.0038 (15)−0.0185 (14)
O3W0.0609 (18)0.0564 (16)0.0613 (16)−0.0235 (14)−0.0260 (13)0.0190 (12)
O40.0360 (12)0.0236 (10)0.0820 (16)−0.0104 (9)−0.0201 (11)0.0091 (10)
O50.0338 (12)0.0249 (10)0.0686 (14)−0.0079 (9)−0.0251 (10)−0.0035 (9)
O60.096 (2)0.0339 (12)0.0485 (13)−0.0285 (13)−0.0118 (13)−0.0006 (10)
O70.0632 (15)0.0504 (13)0.0399 (12)−0.0408 (12)−0.0145 (11)0.0078 (9)
O80.0365 (11)0.0243 (10)0.0378 (10)−0.0148 (8)−0.0106 (9)0.0039 (8)
O90.0606 (16)0.0360 (12)0.0839 (17)−0.0159 (11)−0.0408 (14)0.0096 (11)
O100.0356 (11)0.0241 (9)0.0349 (10)−0.0144 (8)−0.0096 (8)0.0049 (7)
O110.0527 (14)0.0350 (11)0.0373 (11)−0.0272 (10)−0.0170 (10)0.0073 (8)
O120.0511 (14)0.0344 (11)0.0541 (13)−0.0201 (10)−0.0117 (11)0.0130 (9)
O130.0279 (11)0.0236 (10)0.0687 (14)−0.0064 (8)−0.0167 (10)−0.0029 (9)
O140.0330 (12)0.0220 (10)0.0713 (15)−0.0078 (9)−0.0105 (10)0.0022 (9)
O150.0844 (19)0.0294 (12)0.0591 (14)−0.0195 (12)−0.0253 (13)0.0020 (10)
O160.0394 (13)0.0397 (12)0.0450 (12)−0.0109 (10)−0.0131 (10)−0.0062 (9)
O170.0487 (14)0.0455 (13)0.0436 (12)0.0021 (11)−0.0204 (11)−0.0075 (10)
O180.077 (2)0.0375 (14)0.112 (2)−0.0190 (14)−0.0312 (17)−0.0027 (14)
Geometric parameters (Å, º) top
Sm1—O52.4344 (19)C28—O121.374 (3)
Sm1—O42.439 (2)C28—C291.382 (4)
Sm1—O1W2.445 (2)C29—C301.379 (4)
Sm1—O102.4396 (16)C29—H29A0.9300
Sm1—O22.451 (2)C30—H30A0.9300
Sm1—O72.4718 (19)C31—C321.502 (4)
Sm1—O12.546 (2)C31—H31A0.9700
Sm1—O82.5904 (18)C31—H31B0.9700
Sm1—N12.598 (2)C32—O111.251 (3)
Sm1—C162.792 (3)C32—O101.274 (3)
Sm1—C82.876 (3)C33—C381.381 (4)
Sm1—C242.902 (3)C33—C341.393 (4)
Sm2—O82.3896 (16)C33—C391.499 (4)
Sm2—O142.424 (2)C34—C351.370 (4)
Sm2—O132.4379 (19)C34—H34A0.9300
Sm2—O2W2.444 (2)C35—C361.385 (4)
Sm2—O162.464 (2)C35—H35A0.9300
Sm2—O172.532 (2)C36—O151.361 (3)
Sm2—O102.5572 (18)C36—C371.380 (4)
Sm2—O112.5947 (18)C37—C381.385 (4)
Sm2—N32.620 (2)C37—H37A0.9300
Sm2—C402.806 (3)C38—H38A0.9300
Sm2—C482.874 (3)C39—C401.506 (4)
Sm2—C322.954 (3)C39—H39A0.9700
N1—C531.336 (4)C39—H39B0.9700
N1—C491.334 (4)C40—O141.257 (3)
N2—C581.312 (5)C40—O131.265 (3)
N2—C541.326 (5)C41—C421.380 (4)
N3—C631.341 (4)C41—C461.386 (4)
N3—C591.337 (4)C41—C471.517 (4)
N4—C641.320 (5)C42—C431.373 (4)
N4—C681.331 (6)C42—H42A0.9300
C1—C21.378 (4)C43—C441.380 (4)
C1—C61.389 (4)C43—H43A0.9300
C1—C71.514 (4)C44—O181.368 (4)
C2—C31.383 (4)C44—C451.378 (5)
C2—H2A0.9300C45—C461.383 (4)
C3—C41.367 (4)C45—H45A0.9300
C3—H3A0.9300C46—H46A0.9300
C4—C51.372 (4)C47—C481.508 (4)
C4—O31.378 (4)C47—H47A0.9700
C5—C61.372 (4)C47—H47B0.9700
C5—H5A0.9300C48—O161.250 (4)
C6—H6A0.9300C48—O171.271 (4)
C7—C81.503 (4)C49—C501.379 (4)
C7—H7A0.9700C49—H49A0.9300
C7—H7B0.9700C50—C511.381 (4)
C8—O11.264 (4)C50—H50A0.9300
C8—O21.257 (4)C51—C521.380 (4)
C9—C101.373 (4)C51—C561.486 (4)
C9—C141.387 (4)C52—C531.376 (4)
C9—C151.506 (4)C52—H52A0.9300
C10—C111.392 (4)C53—H53A0.9300
C10—H10A0.9300C54—C551.380 (4)
C11—C121.369 (4)C54—H54A0.9300
C11—H11A0.9300C55—C561.374 (5)
C12—C131.374 (4)C55—H55A0.9300
C12—O61.373 (3)C56—C571.376 (5)
C13—C141.369 (4)C57—C581.378 (5)
C13—H13A0.9300C57—H57A0.9300
C14—H14A0.9300C58—H58A0.9300
C15—C161.509 (4)C59—C601.383 (4)
C15—H15A0.9700C59—H59A0.9300
C15—H15B0.9700C60—C611.380 (4)
C16—O41.253 (3)C60—H60A0.9300
C16—O51.260 (3)C61—C621.384 (4)
C17—C221.381 (4)C61—C661.488 (4)
C17—C181.381 (5)C62—C631.378 (4)
C17—C231.514 (4)C62—H62A0.9300
C18—C191.382 (5)C63—H63A0.9300
C18—H18A0.9300C64—C651.384 (5)
C19—C201.387 (4)C64—H64A0.9300
C19—H19A0.9300C65—C661.385 (5)
C20—O91.372 (3)C65—H65A0.9300
C20—C211.373 (4)C66—C671.388 (5)
C21—C221.381 (4)C67—C681.385 (5)
C21—H21A0.9300C67—H67A0.9300
C22—H22A0.9300C68—H68A0.9300
C23—C241.502 (4)O1W—H1WA0.81 (5)
C23—H23A0.9700O1W—H1WB0.826 (18)
C23—H23B0.9700O2W—H2WA0.83 (5)
C24—O71.239 (3)O2W—H2WB0.834 (18)
C24—O81.274 (3)O3—H3B0.8200
C25—C301.380 (4)O3W—H3WB0.85 (4)
C25—C261.388 (4)O3W—H3WA0.84 (4)
C25—C311.507 (4)O6—H6B0.8200
C26—C271.386 (4)O9—H9A0.8200
C26—H26A0.9300O12—H12A0.8200
C27—C281.371 (4)O15—H15C0.8200
C27—H27A0.9300O18—H18B0.8200
O5—Sm1—O453.20 (6)C17—C18—H18A119.2
O5—Sm1—O1W145.23 (6)C18—C19—C20119.3 (3)
O4—Sm1—O1W150.49 (7)C18—C19—H19A120.3
O5—Sm1—O1073.25 (6)C20—C19—H19A120.3
O4—Sm1—O10126.11 (6)O9—C20—C21118.2 (3)
O1W—Sm1—O1079.74 (6)O9—C20—C19122.0 (3)
O5—Sm1—O2123.26 (7)C21—C20—C19119.8 (3)
O4—Sm1—O2116.84 (7)C20—C21—C22119.9 (3)
O1W—Sm1—O274.90 (7)C20—C21—H21A120.0
O10—Sm1—O285.59 (6)C22—C21—H21A120.0
O5—Sm1—O795.18 (7)C17—C22—C21121.4 (3)
O4—Sm1—O777.29 (7)C17—C22—H22A119.3
O1W—Sm1—O777.80 (8)C21—C22—H22A119.3
O10—Sm1—O7116.92 (6)C24—C23—C17112.3 (3)
O2—Sm1—O7140.51 (7)C24—C23—H23A109.2
O5—Sm1—O175.97 (7)C17—C23—H23A109.2
O4—Sm1—O172.89 (8)C24—C23—H23B109.2
O1W—Sm1—O1126.25 (8)C17—C23—H23B109.2
O10—Sm1—O190.25 (6)H23A—C23—H23B107.9
O2—Sm1—O151.61 (7)O7—C24—O8120.4 (2)
O7—Sm1—O1148.06 (7)O7—C24—C23120.4 (2)
O5—Sm1—O875.80 (6)O8—C24—C23119.2 (3)
O4—Sm1—O8102.16 (7)O7—C24—Sm157.66 (14)
O1W—Sm1—O873.48 (7)O8—C24—Sm163.20 (14)
O10—Sm1—O866.26 (6)C23—C24—Sm1171.2 (2)
O2—Sm1—O8140.65 (6)C30—C25—C26118.0 (3)
O7—Sm1—O850.96 (6)C30—C25—C31120.3 (3)
O1—Sm1—O8147.46 (6)C26—C25—C31121.7 (3)
O5—Sm1—N1129.77 (7)C27—C26—C25121.0 (3)
O4—Sm1—N176.68 (7)C27—C26—H26A119.5
O1W—Sm1—N181.72 (7)C25—C26—H26A119.5
O10—Sm1—N1155.06 (7)C28—C27—C26119.8 (3)
O2—Sm1—N173.54 (7)C28—C27—H27A120.1
O7—Sm1—N174.76 (7)C26—C27—H27A120.1
O1—Sm1—N187.38 (7)C27—C28—O12122.4 (3)
O8—Sm1—N1123.48 (6)C27—C28—C29120.0 (3)
O5—Sm1—C1626.79 (7)O12—C28—C29117.6 (3)
O4—Sm1—C1626.63 (7)C30—C29—C28119.7 (3)
O1W—Sm1—C16163.53 (8)C30—C29—H29A120.1
O10—Sm1—C1699.49 (7)C28—C29—H29A120.1
O2—Sm1—C16121.54 (8)C29—C30—C25121.4 (3)
O7—Sm1—C1688.13 (8)C29—C30—H30A119.3
O1—Sm1—C1670.06 (8)C25—C30—H30A119.3
O8—Sm1—C1691.05 (7)C25—C31—C32114.9 (2)
N1—Sm1—C16102.98 (8)C25—C31—H31A108.5
O5—Sm1—C8100.86 (8)C32—C31—H31A108.5
O4—Sm1—C893.91 (8)C25—C31—H31B108.5
O1W—Sm1—C8100.65 (9)C32—C31—H31B108.5
O10—Sm1—C890.08 (7)H31A—C31—H31B107.5
O2—Sm1—C825.75 (8)O11—C32—O10119.6 (2)
O7—Sm1—C8151.75 (7)O11—C32—C31122.7 (2)
O1—Sm1—C826.07 (8)O10—C32—C31117.7 (2)
O8—Sm1—C8156.18 (6)O11—C32—Sm261.23 (14)
N1—Sm1—C877.11 (7)O10—C32—Sm259.60 (13)
C16—Sm1—C895.79 (9)C31—C32—Sm2168.4 (2)
O5—Sm1—C2486.95 (8)C38—C33—C34117.3 (2)
O4—Sm1—C2491.04 (8)C38—C33—C39121.8 (3)
O1W—Sm1—C2472.29 (8)C34—C33—C39120.9 (3)
O10—Sm1—C2491.89 (7)C35—C34—C33121.4 (3)
O2—Sm1—C24147.01 (8)C35—C34—H34A119.3
O7—Sm1—C2425.05 (7)C33—C34—H34A119.3
O1—Sm1—C24161.38 (8)C34—C35—C36120.5 (3)
O8—Sm1—C2426.03 (6)C34—C35—H35A119.7
N1—Sm1—C2498.21 (7)C36—C35—H35A119.7
C16—Sm1—C2491.34 (8)O15—C36—C37123.0 (3)
C8—Sm1—C24172.18 (8)O15—C36—C35117.9 (3)
O8—Sm2—O14127.89 (6)C37—C36—C35119.0 (3)
O8—Sm2—O1375.13 (6)C36—C37—C38119.9 (3)
O14—Sm2—O1353.27 (6)C36—C37—H37A120.1
O8—Sm2—O2W78.76 (7)C38—C37—H37A120.1
O14—Sm2—O2W143.94 (7)C33—C38—C37121.8 (3)
O13—Sm2—O2W147.65 (7)C33—C38—H38A119.1
O8—Sm2—O1681.26 (6)C37—C38—H38A119.1
O14—Sm2—O16126.48 (7)C40—C39—C33115.7 (2)
O13—Sm2—O16117.96 (7)C40—C39—H39A108.4
O2W—Sm2—O1675.82 (8)C33—C39—H39A108.4
O8—Sm2—O1798.20 (7)C40—C39—H39B108.4
O14—Sm2—O1777.89 (7)C33—C39—H39B108.4
O13—Sm2—O1776.05 (7)H39A—C39—H39B107.4
O2W—Sm2—O17126.91 (7)O14—C40—O13119.7 (3)
O16—Sm2—O1751.67 (7)O14—C40—C39119.0 (2)
O8—Sm2—O1067.51 (6)O13—C40—C39121.4 (2)
O14—Sm2—O1090.92 (7)O14—C40—Sm259.52 (14)
O13—Sm2—O1075.70 (6)O13—C40—Sm260.16 (14)
O2W—Sm2—O1076.88 (7)C39—C40—Sm2177.20 (19)
O16—Sm2—O10141.76 (6)C42—C41—C46117.7 (3)
O17—Sm2—O10150.83 (6)C42—C41—C47122.1 (3)
O8—Sm2—O11115.29 (6)C46—C41—C47120.2 (3)
O14—Sm2—O1173.46 (7)C43—C42—C41121.9 (3)
O13—Sm2—O11101.66 (7)C43—C42—H42A119.0
O2W—Sm2—O1172.75 (7)C41—C42—H42A119.0
O16—Sm2—O11140.11 (7)C44—C43—C42119.6 (3)
O17—Sm2—O11144.90 (7)C44—C43—H43A120.2
O10—Sm2—O1150.14 (5)C42—C43—H43A120.2
O8—Sm2—N3155.05 (7)O18—C44—C43117.5 (3)
O14—Sm2—N375.76 (7)O18—C44—C45122.6 (3)
O13—Sm2—N3126.14 (7)C43—C44—C45119.9 (3)
O2W—Sm2—N384.29 (7)C46—C45—C44119.6 (3)
O16—Sm2—N376.90 (7)C46—C45—H45A120.2
O17—Sm2—N377.54 (7)C44—C45—H45A120.2
O10—Sm2—N3126.09 (6)C45—C46—C41121.3 (3)
O11—Sm2—N376.13 (6)C45—C46—H46A119.4
O8—Sm2—C40101.68 (7)C41—C46—H46A119.4
O14—Sm2—C4026.53 (7)C48—C47—C41112.1 (2)
O13—Sm2—C4026.75 (7)C48—C47—H47A109.2
O2W—Sm2—C40157.91 (8)C41—C47—H47A109.2
O16—Sm2—C40126.24 (8)C48—C47—H47B109.2
O17—Sm2—C4075.11 (7)C41—C47—H47B109.2
O10—Sm2—C4082.88 (7)H47A—C47—H47B107.9
O11—Sm2—C4087.53 (7)O16—C48—O17119.5 (3)
N3—Sm2—C40100.89 (7)O16—C48—C47120.3 (3)
O8—Sm2—C4891.70 (7)O17—C48—C47120.2 (3)
O14—Sm2—C48101.89 (9)O16—C48—Sm258.51 (15)
O13—Sm2—C4898.78 (8)O17—C48—Sm261.67 (15)
O2W—Sm2—C48100.77 (9)C47—C48—Sm2171.01 (19)
O16—Sm2—C4825.63 (8)N1—C49—C50123.3 (3)
O17—Sm2—C4826.22 (8)N1—C49—H49A118.4
O10—Sm2—C48159.18 (7)C50—C49—H49A118.4
O11—Sm2—C48149.49 (7)C49—C50—C51119.9 (3)
N3—Sm2—C4873.54 (7)C49—C50—H50A120.1
C40—Sm2—C48101.29 (9)C51—C50—H50A120.1
O8—Sm2—C3290.76 (6)C50—C51—C52116.9 (2)
O14—Sm2—C3284.15 (8)C50—C51—C56121.4 (3)
O13—Sm2—C3291.20 (7)C52—C51—C56121.7 (3)
O2W—Sm2—C3270.24 (8)C53—C52—C51119.8 (3)
O16—Sm2—C32146.03 (8)C53—C52—H52A120.1
O17—Sm2—C32161.85 (8)C51—C52—H52A120.1
O10—Sm2—C3225.46 (6)N1—C53—C52123.5 (3)
O11—Sm2—C3225.00 (6)N1—C53—H53A118.2
N3—Sm2—C32100.64 (7)C52—C53—H53A118.2
C40—Sm2—C3287.67 (8)N2—C54—C55124.2 (4)
C48—Sm2—C32170.02 (8)N2—C54—H54A117.9
C53—N1—C49116.6 (2)C55—C54—H54A117.9
C53—N1—Sm1118.68 (18)C54—C55—C56119.2 (4)
C49—N1—Sm1124.39 (18)C54—C55—H55A120.4
C58—N2—C54115.9 (3)C56—C55—H55A120.4
C63—N3—C59116.5 (2)C57—C56—C55116.8 (3)
C63—N3—Sm2121.64 (18)C57—C56—C51122.0 (3)
C59—N3—Sm2121.42 (18)C55—C56—C51121.1 (3)
C64—N4—C68116.2 (3)C56—C57—C58119.6 (4)
C2—C1—C6117.5 (3)C56—C57—H57A120.2
C2—C1—C7122.4 (3)C58—C57—H57A120.2
C6—C1—C7120.1 (3)N2—C58—C57124.2 (4)
C1—C2—C3121.5 (3)N2—C58—H58A117.9
C1—C2—H2A119.3C57—C58—H58A117.9
C3—C2—H2A119.3N3—C59—C60123.1 (3)
C4—C3—C2119.8 (3)N3—C59—H59A118.4
C4—C3—H3A120.1C60—C59—H59A118.4
C2—C3—H3A120.1C59—C60—C61120.3 (3)
C3—C4—C5119.7 (3)C59—C60—H60A119.9
C3—C4—O3118.5 (3)C61—C60—H60A119.9
C5—C4—O3121.8 (3)C60—C61—C62116.4 (2)
C4—C5—C6120.3 (3)C60—C61—C66120.8 (3)
C4—C5—H5A119.9C62—C61—C66122.7 (3)
C6—C5—H5A119.9C63—C62—C61120.2 (3)
C5—C6—C1121.2 (3)C63—C62—H62A119.9
C5—C6—H6A119.4C61—C62—H62A119.9
C1—C6—H6A119.4N3—C63—C62123.2 (3)
C8—C7—C1111.8 (2)N3—C63—H63A118.4
C8—C7—H7A109.3C62—C63—H63A118.4
C1—C7—H7A109.3N4—C64—C65124.0 (4)
C8—C7—H7B109.3N4—C64—H64A118.0
C1—C7—H7B109.3C65—C64—H64A118.0
H7A—C7—H7B107.9C64—C65—C66119.7 (4)
O1—C8—O2119.4 (3)C64—C65—H65A120.2
O1—C8—C7120.7 (3)C66—C65—H65A120.2
O2—C8—C7119.9 (3)C65—C66—C67116.8 (3)
O1—C8—Sm162.24 (15)C65—C66—C61122.2 (3)
O2—C8—Sm157.91 (15)C67—C66—C61120.9 (3)
C7—C8—Sm1169.06 (18)C68—C67—C66118.9 (4)
C10—C9—C14117.2 (3)C68—C67—H67A120.5
C10—C9—C15121.7 (3)C66—C67—H67A120.5
C14—C9—C15121.1 (3)N4—C68—C67124.4 (4)
C9—C10—C11122.1 (3)N4—C68—H68A117.8
C9—C10—H10A119.0C67—C68—H68A117.8
C11—C10—H10A119.0Sm1—O1W—H1WA116 (3)
C12—C11—C10119.1 (3)Sm1—O1W—H1WB138 (3)
C12—C11—H11A120.5H1WA—O1W—H1WB105 (3)
C10—C11—H11A120.5C8—O1—Sm191.69 (17)
C13—C12—C11119.9 (3)Sm2—O2W—H2WA125 (3)
C13—C12—O6117.5 (3)Sm2—O2W—H2WB130 (3)
C11—C12—O6122.6 (3)H2WA—O2W—H2WB105 (3)
C12—C13—C14120.2 (3)C8—O2—Sm196.34 (18)
C12—C13—H13A119.9C4—O3—H3B109.5
C14—C13—H13A119.9H3WB—O3W—H3WA102 (3)
C13—C14—C9121.5 (3)C16—O4—Sm192.64 (17)
C13—C14—H14A119.3C16—O5—Sm192.66 (16)
C9—C14—H14A119.3C12—O6—H6B109.5
C9—C15—C16114.9 (2)C24—O7—Sm197.28 (16)
C9—C15—H15A108.5C24—O8—Sm2153.69 (18)
C16—C15—H15A108.5C24—O8—Sm190.77 (15)
C9—C15—H15B108.5Sm2—O8—Sm1113.39 (7)
C16—C15—H15B108.5C20—O9—H9A109.5
H15A—C15—H15B107.5C32—O10—Sm1142.67 (17)
O4—C16—O5120.5 (3)C32—O10—Sm294.93 (15)
O4—C16—C15118.7 (3)Sm1—O10—Sm2112.84 (6)
O5—C16—C15120.7 (2)C32—O11—Sm293.77 (15)
O4—C16—Sm160.73 (15)C28—O12—H12A109.5
O5—C16—Sm160.56 (14)C40—O13—Sm293.09 (15)
C15—C16—Sm1169.1 (2)C40—O14—Sm293.95 (16)
C22—C17—C18117.9 (3)C36—O15—H15C109.5
C22—C17—C23121.1 (3)C48—O16—Sm295.86 (18)
C18—C17—C23121.0 (3)C48—O17—Sm292.11 (18)
C19—C18—C17121.7 (3)C44—O18—H18B109.5
C19—C18—H18A119.2
O5—Sm1—N1—C5341.9 (3)O13—Sm2—C48—O17−30.02 (17)
O4—Sm1—N1—C5338.2 (2)O2W—Sm2—C48—O17175.88 (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—C53161.8 (2)O11—Sm2—C48—O17101.6 (2)
O7—Sm1—N1—C53−42.0 (2)N3—Sm2—C48—O1795.19 (17)
O1—Sm1—N1—C53111.2 (2)C40—Sm2—C48—O17−2.97 (18)
O8—Sm1—N1—C53−57.7 (2)C53—N1—C49—C502.0 (5)
C16—Sm1—N1—C5342.4 (2)Sm1—N1—C49—C50−171.2 (2)
C8—Sm1—N1—C53135.4 (2)N1—C49—C50—C510.1 (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—C56176.2 (3)
O4—Sm1—N1—C49−148.7 (2)C50—C51—C52—C531.9 (5)
O1W—Sm1—N1—C4951.5 (2)C56—C51—C52—C53−176.5 (3)
O10—Sm1—N1—C499.2 (3)C49—N1—C53—C52−2.3 (5)
O2—Sm1—N1—C49−25.1 (2)Sm1—N1—C53—C52171.4 (3)
O7—Sm1—N1—C49131.0 (2)C51—C52—C53—N10.3 (5)
O1—Sm1—N1—C49−75.7 (2)C58—N2—C54—C551.1 (6)
O8—Sm1—N1—C49115.4 (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—C51176.2 (3)
C24—Sm1—N1—C49122.1 (2)C50—C51—C56—C5729.0 (5)
O8—Sm2—N3—C63173.16 (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—C5530.0 (5)
O2W—Sm2—N3—C63125.9 (2)C55—C56—C57—C582.2 (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—C570.0 (6)
O10—Sm2—N3—C6356.8 (2)C56—C57—C58—N2−1.7 (7)
O11—Sm2—N3—C6352.3 (2)C63—N3—C59—C60−2.1 (4)
C40—Sm2—N3—C63−32.3 (2)Sm2—N3—C59—C60170.8 (2)
C48—Sm2—N3—C63−131.0 (2)N3—C59—C60—C61−1.5 (5)
C32—Sm2—N3—C6357.3 (2)C59—C60—C61—C623.5 (4)
O8—Sm2—N3—C590.6 (3)C59—C60—C61—C66−173.5 (3)
O14—Sm2—N3—C59163.7 (2)C60—C61—C62—C63−2.2 (4)
O13—Sm2—N3—C59145.3 (2)C66—C61—C62—C63174.8 (3)
O2W—Sm2—N3—C59−46.6 (2)C59—N3—C63—C623.6 (4)
O16—Sm2—N3—C5930.1 (2)Sm2—N3—C63—C62−169.3 (2)
O17—Sm2—N3—C5983.2 (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—C662.5 (6)
C40—Sm2—N3—C59155.1 (2)C64—C65—C66—C67−2.4 (5)
C48—Sm2—N3—C5956.4 (2)C64—C65—C66—C61174.5 (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—C65166.1 (3)
C7—C1—C2—C3−179.2 (3)C60—C61—C66—C67159.7 (3)
C1—C2—C3—C40.4 (5)C62—C61—C66—C67−17.1 (5)
C2—C3—C4—C51.4 (5)C65—C66—C67—C680.4 (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—C6178.4 (3)C66—C67—C68—N41.9 (6)
C4—C5—C6—C11.8 (5)O2—C8—O1—Sm19.7 (3)
C2—C1—C6—C50.0 (5)C7—C8—O1—Sm1−167.9 (2)
C7—C1—C6—C5178.2 (3)O5—Sm1—O1—C8−162.32 (17)
C2—C1—C7—C8−48.6 (4)O4—Sm1—O1—C8142.36 (17)
C6—C1—C7—C8133.4 (3)O1W—Sm1—O1—C8−12.25 (19)
C1—C7—C8—O199.3 (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—C8120.68 (18)
O5—Sm1—C8—O117.46 (17)O8—Sm1—O1—C8−131.82 (16)
O4—Sm1—C8—O1−35.80 (16)N1—Sm1—O1—C865.50 (16)
O1W—Sm1—C8—O1169.98 (16)C16—Sm1—O1—C8170.32 (18)
O10—Sm1—C8—O190.41 (16)C24—Sm1—O1—C8173.7 (2)
O2—Sm1—C8—O1170.0 (3)O1—C8—O2—Sm1−10.1 (3)
O7—Sm1—C8—O1−106.0 (2)C7—C8—O2—Sm1167.5 (2)
O8—Sm1—C8—O196.9 (2)O5—Sm1—O2—C832.73 (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—C8179.93 (17)
O5—Sm1—C8—O2−152.59 (15)O10—Sm1—O2—C899.38 (16)
O4—Sm1—C8—O2154.15 (15)O7—Sm1—O2—C8−132.26 (16)
O1W—Sm1—C8—O2−0.07 (16)O1—Sm1—O2—C85.56 (15)
O10—Sm1—C8—O2−79.64 (16)O8—Sm1—O2—C8142.44 (15)
O7—Sm1—C8—O283.9 (2)N1—Sm1—O2—C8−94.42 (16)
O1—Sm1—C8—O2−170.0 (3)C16—Sm1—O2—C80.94 (18)
O8—Sm1—C8—O2−73.2 (2)C24—Sm1—O2—C8−173.95 (15)
N1—Sm1—C8—O278.78 (16)O5—C16—O4—Sm19.9 (3)
C16—Sm1—C8—O2−179.19 (16)C15—C16—O4—Sm1−167.6 (3)
O5—Sm1—C8—C7125.7 (12)O5—Sm1—O4—C16−5.52 (16)
O4—Sm1—C8—C772.5 (12)O1W—Sm1—O4—C16−145.07 (18)
O1W—Sm1—C8—C7−81.8 (12)O10—Sm1—O4—C162.2 (2)
O10—Sm1—C8—C7−161.3 (12)O2—Sm1—O4—C16107.38 (18)
O2—Sm1—C8—C7−81.7 (12)O7—Sm1—O4—C16−112.04 (18)
O7—Sm1—C8—C72.3 (13)O1—Sm1—O4—C1679.52 (18)
O1—Sm1—C8—C7108.3 (13)O8—Sm1—O4—C16−67.19 (18)
O8—Sm1—C8—C7−154.9 (11)N1—Sm1—O4—C16170.88 (19)
N1—Sm1—C8—C7−2.9 (12)C8—Sm1—O4—C1695.12 (18)
C16—Sm1—C8—C799.1 (12)C24—Sm1—O4—C16−90.93 (18)
C14—C9—C10—C110.4 (5)O4—C16—O5—Sm1−10.0 (3)
C15—C9—C10—C11−179.1 (3)C15—C16—O5—Sm1167.5 (3)
C9—C10—C11—C12−0.1 (5)O4—Sm1—O5—C165.49 (16)
C10—C11—C12—C13−0.8 (5)O1W—Sm1—O5—C16151.41 (17)
C10—C11—C12—O6179.1 (3)O10—Sm1—O5—C16−168.04 (18)
C11—C12—C13—C141.3 (5)O2—Sm1—O5—C16−95.10 (17)
O6—C12—C13—C14−178.6 (3)O7—Sm1—O5—C1675.38 (17)
C12—C13—C14—C9−1.0 (5)O1—Sm1—O5—C16−73.45 (17)
C10—C9—C14—C130.1 (5)O8—Sm1—O5—C16122.91 (17)
C15—C9—C14—C13179.6 (3)N1—Sm1—O5—C160.9 (2)
C10—C9—C15—C16−99.8 (4)C8—Sm1—O5—C16−81.26 (17)
C14—C9—C15—C1680.6 (4)C24—Sm1—O5—C1699.07 (17)
C9—C15—C16—O4172.7 (3)O8—C24—O7—Sm1−7.9 (3)
C9—C15—C16—O5−4.9 (4)C23—C24—O7—Sm1170.0 (3)
C9—C15—C16—Sm188.5 (10)O5—Sm1—O7—C2471.33 (19)
O5—Sm1—C16—O4170.2 (3)O4—Sm1—O7—C24121.8 (2)
O1W—Sm1—C16—O495.9 (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—O464.78 (18)O1—Sm1—O7—C24142.98 (18)
O1—Sm1—C16—O4−91.43 (18)O8—Sm1—O7—C244.32 (17)
O8—Sm1—C16—O4115.67 (18)N1—Sm1—O7—C24−158.8 (2)
N1—Sm1—C16—O4−9.11 (19)C16—Sm1—O7—C2497.2 (2)
C8—Sm1—C16—O4−87.17 (18)C8—Sm1—O7—C24−164.0 (2)
C24—Sm1—C16—O489.63 (18)O7—C24—O8—Sm2164.8 (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—Sm2157.3 (4)
O10—Sm1—C16—O511.61 (17)O7—C24—O8—Sm17.5 (3)
O2—Sm1—C16—O5102.25 (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—O598.40 (17)O13—Sm2—O8—C24−74.7 (4)
O8—Sm1—C16—O5−54.49 (17)O2W—Sm2—O8—C24124.6 (4)
N1—Sm1—C16—O5−179.27 (16)O16—Sm2—O8—C2447.4 (4)
C8—Sm1—C16—O5102.66 (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—C1590.2 (10)N3—Sm2—O8—C2476.5 (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—C2423.9 (4)
O2—Sm1—C16—C152.7 (10)C32—Sm2—O8—C24−165.7 (4)
O7—Sm1—C16—C15155.0 (10)O14—Sm2—O8—Sm172.61 (11)
O1—Sm1—C16—C15−1.2 (10)O13—Sm2—O8—Sm180.48 (8)
O8—Sm1—C16—C15−154.1 (10)O2W—Sm2—O8—Sm1−80.24 (9)
N1—Sm1—C16—C1581.1 (10)O16—Sm2—O8—Sm1−157.40 (9)
C8—Sm1—C16—C153.1 (10)O17—Sm2—O8—Sm1153.60 (8)
C24—Sm1—C16—C15179.7 (12)O10—Sm2—O8—Sm10.08 (6)
C22—C17—C18—C190.3 (4)O11—Sm2—O8—Sm1−15.60 (10)
C23—C17—C18—C19178.9 (3)N3—Sm2—O8—Sm1−128.35 (14)
C17—C18—C19—C200.0 (5)C40—Sm2—O8—Sm177.21 (9)
C18—C19—C20—O9−180.0 (3)C48—Sm2—O8—Sm1179.11 (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—C220.6 (5)O4—Sm1—O8—C24−66.49 (17)
C18—C17—C22—C21−0.2 (5)O1W—Sm1—O8—C2483.36 (17)
C23—C17—C22—C21−178.8 (3)O10—Sm1—O8—C24169.19 (18)
C20—C21—C22—C17−0.2 (5)O2—Sm1—O8—C24121.15 (17)
C22—C17—C23—C2498.0 (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—C2415.45 (19)
C17—C23—C24—O8132.7 (3)C16—Sm1—O8—C24−90.90 (17)
O5—Sm1—C24—O7−109.12 (19)C8—Sm1—O8—C24162.1 (2)
O4—Sm1—C24—O7−56.05 (19)O5—Sm1—O8—Sm277.59 (8)
O1W—Sm1—C24—O799.17 (19)O4—Sm1—O8—Sm2124.24 (8)
O10—Sm1—C24—O7177.77 (19)O1W—Sm1—O8—Sm2−85.92 (9)
O2—Sm1—C24—O793.0 (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—O720.6 (2)O1—Sm1—O8—Sm247.06 (16)
C16—Sm1—C24—O7−82.69 (19)N1—Sm1—O8—Sm2−153.82 (8)
O5—Sm1—C24—O863.22 (16)C16—Sm1—O8—Sm299.83 (9)
O4—Sm1—C24—O8116.29 (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—Sm128.0 (4)
O7—Sm1—C24—O8172.3 (3)Sm2—C32—O10—Sm1−139.1 (3)
O1—Sm1—C24—O886.5 (3)O11—C32—O10—Sm2−12.7 (3)
N1—Sm1—C24—O8−167.03 (16)C31—C32—O10—Sm2167.1 (2)
C16—Sm1—C24—O889.66 (17)O5—Sm1—O10—C3253.5 (3)
C30—C25—C26—C27−1.0 (4)O4—Sm1—O10—C3247.1 (3)
C31—C25—C26—C27177.9 (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—C32140.8 (3)
C26—C27—C28—C291.5 (5)O1—Sm1—O10—C32−21.8 (3)
C27—C28—C29—C30−1.0 (5)O8—Sm1—O10—C32135.0 (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—C3248.1 (3)
C26—C25—C30—C291.6 (5)C8—Sm1—O10—C32−47.8 (3)
C31—C25—C30—C29−177.3 (3)C24—Sm1—O10—C32139.7 (3)
C30—C25—C31—C3275.7 (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—O1112.0 (5)O1W—Sm1—O10—Sm276.42 (8)
C25—C31—C32—O10−167.8 (3)O2—Sm1—O10—Sm2151.85 (8)
C25—C31—C32—Sm2−94.3 (9)O7—Sm1—O10—Sm25.86 (11)
O8—Sm2—C32—O11−169.19 (17)O1—Sm1—O10—Sm2−156.70 (8)
O14—Sm2—C32—O1162.78 (17)O8—Sm1—O10—Sm20.07 (6)
O13—Sm2—C32—O11115.67 (17)N1—Sm1—O10—Sm2118.99 (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—Sm2177.23 (9)
O17—Sm2—C32—O1170.9 (3)C24—Sm1—O10—Sm24.80 (9)
O10—Sm2—C32—O11167.4 (3)O8—Sm2—O10—C32−154.56 (18)
N3—Sm2—C32—O11−11.50 (18)O14—Sm2—O10—C3274.28 (16)
C40—Sm2—C32—O1189.15 (17)O13—Sm2—O10—C32125.87 (17)
O8—Sm2—C32—O1023.39 (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—C32140.59 (18)
O2W—Sm2—C32—O10101.15 (16)O11—Sm2—O10—C326.88 (16)
O16—Sm2—C32—O1098.78 (18)N3—Sm2—O10—C321.30 (19)
O17—Sm2—C32—O10−96.5 (3)C40—Sm2—O10—C3299.62 (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—C31175.6 (9)O2W—Sm2—O10—Sm183.02 (8)
O13—Sm2—C32—C31−131.5 (9)O16—Sm2—O10—Sm137.63 (13)
O2W—Sm2—C32—C3121.4 (9)O17—Sm2—O10—Sm1−64.93 (16)
O16—Sm2—C32—C3119.0 (10)O11—Sm2—O10—Sm1161.36 (12)
O17—Sm2—C32—C31−176.3 (8)N3—Sm2—O10—Sm1155.78 (8)
O10—Sm2—C32—C31−79.8 (9)C40—Sm2—O10—Sm1−105.90 (8)
O11—Sm2—C32—C31112.8 (10)C48—Sm2—O10—Sm1−2.8 (3)
N3—Sm2—C32—C31101.3 (9)C32—Sm2—O10—Sm1154.5 (2)
C40—Sm2—C32—C31−158.0 (9)O10—C32—O11—Sm212.5 (3)
C38—C33—C34—C35−0.1 (5)C31—C32—O11—Sm2−167.3 (3)
C39—C33—C34—C35179.2 (3)O8—Sm2—O11—C3211.97 (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—C370.3 (5)O2W—Sm2—O11—C3280.11 (18)
O15—C36—C37—C38179.9 (3)O16—Sm2—O11—C32119.63 (18)
C35—C36—C37—C380.2 (5)O17—Sm2—O11—C32−149.20 (17)
C34—C33—C38—C370.6 (5)O10—Sm2—O11—C32−7.00 (16)
C39—C33—C38—C37−178.7 (3)N3—Sm2—O11—C32168.36 (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—C32161.98 (19)
C34—C33—C39—C4066.3 (4)O14—C40—O13—Sm21.1 (3)
C33—C39—C40—O14173.8 (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—C40115.71 (17)
O16—Sm2—C40—O14100.50 (17)O17—Sm2—O13—C4084.53 (17)
O17—Sm2—C40—O1492.67 (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—C4021.7 (2)
N3—Sm2—C40—O1418.84 (18)C48—Sm2—O13—C4097.69 (17)
C48—Sm2—C40—O1494.02 (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—O137.03 (17)C39—C40—O14—Sm2177.3 (2)
O14—Sm2—C40—O13178.9 (3)O8—Sm2—O14—C4010.1 (2)
O2W—Sm2—C40—O1395.9 (2)O13—Sm2—O14—C400.64 (16)
O16—Sm2—C40—O13−80.64 (18)O2W—Sm2—O14—C40140.64 (16)
O17—Sm2—C40—O13−88.47 (17)O16—Sm2—O14—C40−99.49 (17)
O10—Sm2—C40—O1372.22 (16)O17—Sm2—O14—C40−80.88 (17)
O11—Sm2—C40—O13122.35 (17)O10—Sm2—O14—C4071.96 (17)
N3—Sm2—C40—O13−162.29 (16)O11—Sm2—O14—C40119.62 (17)
C48—Sm2—C40—O13−87.11 (17)N3—Sm2—O14—C40−160.90 (18)
C32—Sm2—C40—O1397.32 (17)C48—Sm2—O14—C40−91.52 (17)
C46—C41—C42—C430.0 (4)C32—Sm2—O14—C4096.54 (17)
C47—C41—C42—C43177.1 (3)O17—C48—O16—Sm29.3 (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—C451.9 (5)O14—Sm2—O16—C4818.30 (19)
O18—C44—C45—C46179.2 (3)O13—Sm2—O16—C48−44.99 (17)
C43—C44—C45—C46−1.3 (5)O2W—Sm2—O16—C48166.54 (17)
C44—C45—C46—C41−0.1 (5)O17—Sm2—O16—C48−5.15 (15)
C42—C41—C46—C450.7 (4)O10—Sm2—O16—C48−147.80 (15)
C47—C41—C46—C45−176.5 (3)O11—Sm2—O16—C48127.73 (16)
C42—C41—C47—C48−69.6 (4)N3—Sm2—O16—C4879.21 (16)
C46—C41—C47—C48107.4 (3)C40—Sm2—O16—C48−14.81 (19)
C41—C47—C48—O1657.3 (4)C32—Sm2—O16—C48168.84 (15)
C41—C47—C48—O17−121.6 (3)O16—C48—O17—Sm2−9.0 (3)
O8—Sm2—C48—O1665.60 (16)C47—C48—O17—Sm2169.9 (2)
O14—Sm2—C48—O16−165.05 (15)O8—Sm2—O17—C4877.00 (17)
O13—Sm2—C48—O16140.81 (15)O14—Sm2—O17—C48−155.86 (17)
O2W—Sm2—C48—O16−13.28 (17)O13—Sm2—O17—C48149.37 (18)
O17—Sm2—C48—O16170.8 (3)O2W—Sm2—O17—C48−5.1 (2)
O10—Sm2—C48—O1668.1 (3)O16—Sm2—O17—C485.04 (15)
O11—Sm2—C48—O16−87.5 (2)O10—Sm2—O17—C48134.67 (16)
N3—Sm2—C48—O16−93.97 (16)O11—Sm2—O17—C48−120.14 (17)
C40—Sm2—C48—O16167.87 (16)N3—Sm2—O17—C48−78.00 (17)
O8—Sm2—C48—O17−105.24 (17)C40—Sm2—O17—C48176.99 (18)
O14—Sm2—C48—O1724.12 (17)C32—Sm2—O17—C48−164.1 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O12i0.821.942.749 (3)169
O6—H6B···O3Wii0.821.862.642 (3)159
O9—H9A···O17iii0.821.862.673 (3)173
O12—H12A···O11iv0.821.942.746 (3)168
O15—H15C···O6v0.821.912.722 (3)174
O18—H18B···O9ii0.821.952.768 (3)173
O2W—H2WA···O50.83 (5)2.02 (5)2.767 (3)150 (4)
O2W—H2WB···N2ii0.83 (2)2.03 (2)2.841 (3)164 (5)
O3W—H3WB···O30.85 (4)1.99 (2)2.816 (3)167 (5)
O1W—H1WA···O130.81 (5)1.96 (4)2.755 (3)165 (4)
O1W—H1WB···N4i0.83 (2)1.99 (2)2.778 (3)160 (4)
O3W—H3WA···O1vi0.84 (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
Mr1573.96
Crystal system, space groupTriclinic, 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)
Z2
Radiation typeMo Kα
µ (mm−1)1.91
Crystal size (mm)0.34 × 0.14 × 0.03
Data collection
DiffractometerBruker APEXII area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.733, 0.941
No. of measured, independent and
observed [I > 2σ(I)] reflections		49293, 14715, 11851
Rint0.047
(sin θ/λ)max (Å−1)0.654
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.070, 1.02
No. of reflections14715
No. of parameters875
No. of restraints9
H-atom treatmentH 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).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O12i0.821.942.749 (3)169.4
O6—H6B···O3Wii0.821.862.642 (3)159.2
O9—H9A···O17iii0.821.862.673 (3)172.8
O12—H12A···O11iv0.821.942.746 (3)167.7
O15—H15C···O6v0.821.912.722 (3)173.5
O18—H18B···O9ii0.821.952.768 (3)173.2
O2W—H2WA···O50.83 (5)2.02 (5)2.767 (3)150 (4)
O2W—H2WB···N2ii0.834 (18)2.03 (2)2.841 (3)164 (5)
O3W—H3WB···O30.85 (4)1.99 (2)2.816 (3)167 (5)
O1W—H1WA···O130.81 (5)1.96 (4)2.755 (3)165 (4)
O1W—H1WB···N4i0.826 (18)1.99 (2)2.778 (3)160 (4)
O3W—H3WA···O1vi0.84 (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

First citationArias, J. C., Cabrera, A., Sharma, P., Rosas, N. & Hernandez, S. (2000). Inorg. Chim. Acta, 310, 261–264.  CAS Google Scholar
 First citationBruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
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ISSN: 2056-9890
Volume 66| Part 12| December 2010| Pages m1511-m1512
https://doi.org/10.1107/S1600536810044454
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