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A simple and effective synthetic route to homo- and heteroleptic rare-earth (Ln = Y, La and Nd) complexes with a tridentate Schiff base anion has been demonstrated using exchange reactions of rare-earth chlorides with in-situ-generated sodium (E)-2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenoxide in dif­fer­ent molar ratios in absolute methanol. Five crystal structures have been deter­mined and studied, namely tris­(2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato-κ3O1,N,O2)lanthanum, [La(C14H12NO2)3], (1), tris­(2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato-κ3O1,N,O2)neodymium tetra­hydro­furan disolvate, [La(C14H12NO2)3]·2C4H8O, (2)·2THF, tris­(2-{[(2-meth­oxy­phen­yl)imino]meth­yl}phenolato)-κ3O1,N,O23O1,N,O22N,O1-yttrium, [Y(C14H12NO2)3], (3), di­chlorido-1κCl,2κCl-μ-methano­lato-1:2κ2O:O-methanol-2κO-(μ-2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato-1κ3O1,N,O2:2κO1)bis­(2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato)-1κ3O1,N,O2;2κ3O1,N,O2-diyttrium–tetra­hydro­furan–methanol (1/1/1), [Y2(C14H12NO2)3(CH3O)Cl2(CH4O)]·CH4O·C4H8O, (4)·MeOH·THF, and bis­(μ-2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato-1κ3O1,N,O2:2κO1)bis­(2-{[(2-meth­oxy­phen­yl)imino]­meth­yl}phenolato-2κ3O1,N,O2)sodiumyttrium chloro­form disolvate, [NaY(C14H12NO2)4]·2CHCl3, (5)·2CHCl3. Structural peculiarities of homoleptic tris­(imino­phenoxide)s (1)–(3), binuclear tris­(imino­phenoxide) (4) and homoleptic ate tetra­kis(imino­phenoxide) (5) are discussed. The nonflat Schiff base ligand displays μ23O1,N,O2O1 bridging, and κ3O1,N,O2 and κ2N,O1 terminal coordination modes, depending on steric congestion, which in turn depends on the ionic radii of the rare-earth metals and the number of coordinated ligands. It has been demonstrated that inter­ligand dihedral angles of the phenoxide ligand are convenient for comparing steric hindrance in complexes. (4)·MeOH has a flat Y2O2 rhomboid core and exhibits both inter- and intra­molecular MeO—H...Cl hydrogen bonding. Catalytic systems based on complexes (1)–(3) and (5) have demonstrated medium catalytic performance in acrylo­nitrile polymerization, providing polyacrylo­nitrile samples with narrow polydispersity.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618012421/jx3019sup1.cif
Contains datablocks mol1, mol2, mol3, mol4, mol5, gloabl

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618012421/jx3019mol1sup2.hkl
Contains datablock mol1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618012421/jx3019mol2sup3.hkl
Contains datablock mol2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618012421/jx3019mol3sup4.hkl
Contains datablock mol3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618012421/jx3019mol4sup5.hkl
Contains datablock mol4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618012421/jx3019mol5sup6.hkl
Contains datablock mol5

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618012421/jx3019sup7.pdf
COSY and HSQC spectra

CCDC references: 1865684; 1865683; 1865682; 1865681; 1865680

Computing details top

For all structures, data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015a); molecular graphics: SHELXTL (Sheldrick, 2015b); software used to prepare material for publication: SHELXTL (Sheldrick, 2015b).

Tris(2-{[(2-methoxyphenyl)imino]methyl}phenolato-κ3O,N,O')lanthanum (mol1) top
Crystal data top
[La(C14H12NO2)3]Z = 2
Mr = 817.65F(000) = 828
Triclinic, P1Dx = 1.487 Mg m3
a = 8.0705 (18) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.588 (3) ÅCell parameters from 632 reflections
c = 19.096 (4) Åθ = 3–28°
α = 79.209 (5)°µ = 1.22 mm1
β = 86.351 (5)°T = 120 K
γ = 73.384 (5)°Prism, colourless
V = 1826.0 (7) Å30.21 × 0.16 × 0.12 mm
Data collection top
Bruker APEXII CCD
diffractometer
8805 independent reflections
Radiation source: fine-focus sealed tube6381 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
φ and ω scansθmax = 28.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1010
Tmin = 0.760, Tmax = 0.934k = 1616
21233 measured reflectionsl = 2525
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)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.033P)2]
where P = (Fo2 + 2Fc2)/3
8805 reflections(Δ/σ)max = 0.001
472 parametersΔρmax = 0.89 e Å3
0 restraintsΔρmin = 0.73 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
La10.21643 (3)0.10340 (2)0.27348 (2)0.02877 (8)
O10.4558 (3)0.0329 (2)0.32647 (15)0.0380 (7)
C10.5491 (5)0.1376 (3)0.3394 (2)0.0333 (9)
C20.7028 (5)0.1696 (4)0.3795 (2)0.0424 (10)
H20.7398980.1137910.3963130.051*
C30.7983 (6)0.2797 (4)0.3943 (2)0.0478 (11)
H30.9014620.2986370.4208950.057*
C40.7500 (6)0.3639 (4)0.3721 (3)0.0543 (13)
H40.8167050.4401830.3840430.065*
C50.6038 (5)0.3353 (4)0.3325 (3)0.0472 (11)
H50.5698030.3930610.3166270.057*
C60.5021 (5)0.2235 (3)0.3144 (2)0.0338 (9)
C70.3509 (5)0.2038 (3)0.2729 (2)0.0354 (9)
H70.3317640.2684270.2598090.043*
N10.2377 (4)0.1095 (3)0.25123 (17)0.0314 (7)
C80.1004 (5)0.1169 (4)0.2105 (2)0.0372 (10)
C90.1242 (7)0.1876 (4)0.1610 (3)0.0567 (13)
H90.2358460.2354220.1533300.068*
C100.0161 (8)0.1884 (6)0.1226 (3)0.0769 (18)
H100.0003470.2353110.0877250.092*
C110.1768 (8)0.1220 (6)0.1350 (3)0.0788 (18)
H110.2722010.1250670.1095260.095*
C120.2040 (6)0.0501 (5)0.1837 (3)0.0609 (14)
H120.3168890.0047310.1923820.073*
C130.0632 (5)0.0458 (4)0.2196 (2)0.0393 (10)
O20.0713 (3)0.0255 (2)0.26800 (16)0.0410 (7)
C140.2400 (5)0.0958 (4)0.2827 (3)0.0529 (13)
H14A0.3203800.0495120.2947670.079*
H14B0.2814710.1531780.2405290.079*
H14C0.2331660.1327080.3228940.079*
O30.3754 (4)0.1055 (2)0.16509 (15)0.0459 (8)
C150.4288 (5)0.1664 (4)0.1107 (2)0.0414 (10)
C160.4784 (7)0.1256 (4)0.0465 (3)0.0593 (14)
H160.4692480.0531860.0430870.071*
C170.5393 (7)0.1864 (5)0.0109 (2)0.0618 (14)
H170.5689500.1563510.0535730.074*
C180.5582 (7)0.2910 (5)0.0079 (3)0.0608 (14)
H180.6026330.3322820.0478170.073*
C190.5123 (6)0.3341 (4)0.0532 (2)0.0527 (12)
H190.5258750.4059280.0554670.063*
C200.4450 (5)0.2750 (4)0.1132 (2)0.0388 (10)
C210.4014 (5)0.3289 (3)0.1750 (2)0.0384 (10)
H210.4280540.3982880.1723660.046*
N20.3298 (4)0.2924 (3)0.23332 (18)0.0354 (8)
C220.2955 (5)0.3612 (3)0.2875 (2)0.0367 (10)
C230.2282 (6)0.4769 (4)0.2740 (3)0.0487 (12)
H230.2073990.5160380.2264000.058*
C240.1908 (7)0.5361 (4)0.3306 (3)0.0599 (14)
H240.1447910.6156620.3214560.072*
C250.2202 (7)0.4799 (5)0.3989 (3)0.0634 (15)
H250.1921300.5207280.4371290.076*
C260.2902 (6)0.3641 (4)0.4134 (3)0.0498 (12)
H260.3137400.3256980.4610090.060*
C270.3254 (5)0.3054 (4)0.3571 (2)0.0385 (10)
O40.3932 (4)0.1901 (2)0.36473 (15)0.0444 (7)
C280.4384 (7)0.1278 (4)0.4354 (2)0.0585 (14)
H28A0.5246540.1549930.4549950.088*
H28B0.4863920.0475740.4332690.088*
H28C0.3348550.1383050.4659700.088*
O50.0797 (4)0.1164 (2)0.38396 (14)0.0435 (7)
C290.0299 (5)0.1762 (4)0.4250 (2)0.0382 (10)
C300.0360 (6)0.1374 (4)0.4994 (2)0.0501 (12)
H300.0466130.0702040.5201360.060*
C310.1584 (7)0.1949 (5)0.5422 (3)0.0607 (14)
H310.1605330.1665530.5918710.073*
C320.2793 (7)0.2939 (5)0.5137 (3)0.0603 (15)
H320.3647880.3328110.5435890.072*
C330.2746 (6)0.3353 (4)0.4424 (3)0.0508 (12)
H330.3568950.4036560.4230770.061*
C340.1500 (6)0.2784 (4)0.3970 (2)0.0387 (10)
C350.1569 (5)0.3304 (3)0.3228 (2)0.0417 (10)
H350.2486220.3970590.3099710.050*
N30.0539 (4)0.2977 (3)0.27154 (18)0.0357 (8)
C360.0899 (5)0.3710 (4)0.2038 (2)0.0429 (11)
C370.1476 (6)0.4877 (4)0.1961 (3)0.0550 (13)
H370.1620280.5224760.2370130.066*
C380.1839 (7)0.5532 (5)0.1296 (3)0.0715 (17)
H380.2276330.6326710.1250400.086*
C390.1575 (8)0.5050 (5)0.0705 (3)0.0743 (18)
H390.1824960.5511870.0248910.089*
C400.0950 (7)0.3898 (4)0.0757 (3)0.0599 (14)
H400.0755560.3569240.0338880.072*
C410.0608 (6)0.3222 (4)0.1423 (2)0.0449 (11)
O60.0012 (4)0.2059 (3)0.15338 (15)0.0507 (8)
C420.0206 (7)0.1549 (4)0.0909 (3)0.0633 (14)
H42A0.0927950.1706900.0692710.095*
H42B0.0700420.0732700.1042830.095*
H42C0.0976410.1859020.0565680.095*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La10.02729 (12)0.02870 (12)0.02971 (12)0.00629 (9)0.00191 (8)0.00682 (8)
O10.0359 (15)0.0296 (16)0.0490 (18)0.0053 (12)0.0115 (13)0.0107 (13)
C10.028 (2)0.034 (2)0.035 (2)0.0057 (18)0.0040 (18)0.0077 (17)
C20.040 (2)0.042 (3)0.046 (3)0.007 (2)0.006 (2)0.014 (2)
C30.035 (2)0.051 (3)0.051 (3)0.001 (2)0.009 (2)0.006 (2)
C40.039 (3)0.038 (3)0.078 (4)0.005 (2)0.007 (3)0.011 (2)
C50.035 (2)0.037 (3)0.069 (3)0.004 (2)0.002 (2)0.017 (2)
C60.027 (2)0.033 (2)0.042 (2)0.0065 (17)0.0045 (18)0.0122 (18)
C70.035 (2)0.034 (2)0.042 (2)0.0141 (19)0.0070 (19)0.0143 (18)
N10.0269 (17)0.0363 (19)0.0329 (18)0.0109 (15)0.0030 (14)0.0088 (14)
C80.034 (2)0.047 (3)0.036 (2)0.017 (2)0.0007 (19)0.0117 (19)
C90.050 (3)0.074 (4)0.055 (3)0.023 (3)0.002 (3)0.028 (3)
C100.071 (4)0.111 (5)0.067 (4)0.032 (4)0.005 (3)0.049 (4)
C110.060 (4)0.111 (5)0.081 (4)0.033 (4)0.022 (3)0.035 (4)
C120.039 (3)0.079 (4)0.071 (4)0.018 (3)0.011 (3)0.023 (3)
C130.035 (2)0.045 (3)0.041 (2)0.014 (2)0.0033 (19)0.010 (2)
O20.0300 (15)0.0398 (17)0.0539 (19)0.0090 (13)0.0016 (14)0.0107 (14)
C140.024 (2)0.061 (3)0.078 (4)0.012 (2)0.009 (2)0.024 (3)
O30.059 (2)0.0422 (18)0.0384 (17)0.0180 (15)0.0157 (15)0.0117 (14)
C150.039 (2)0.047 (3)0.038 (2)0.012 (2)0.008 (2)0.009 (2)
C160.076 (4)0.060 (3)0.050 (3)0.025 (3)0.018 (3)0.024 (2)
C170.079 (4)0.071 (4)0.033 (3)0.020 (3)0.015 (3)0.012 (2)
C180.062 (3)0.078 (4)0.036 (3)0.023 (3)0.009 (2)0.008 (3)
C190.053 (3)0.051 (3)0.049 (3)0.015 (2)0.007 (2)0.002 (2)
C200.034 (2)0.047 (3)0.032 (2)0.010 (2)0.0023 (19)0.0034 (19)
C210.038 (2)0.035 (2)0.041 (2)0.0097 (19)0.000 (2)0.0037 (19)
N20.0363 (19)0.0339 (19)0.0366 (19)0.0101 (15)0.0008 (16)0.0073 (15)
C220.035 (2)0.036 (2)0.043 (3)0.0126 (19)0.0033 (19)0.0149 (19)
C230.043 (3)0.037 (3)0.067 (3)0.014 (2)0.010 (2)0.011 (2)
C240.054 (3)0.040 (3)0.091 (4)0.016 (2)0.019 (3)0.027 (3)
C250.062 (3)0.064 (4)0.079 (4)0.023 (3)0.019 (3)0.050 (3)
C260.051 (3)0.055 (3)0.051 (3)0.016 (2)0.006 (2)0.029 (2)
C270.034 (2)0.037 (2)0.048 (3)0.0127 (19)0.003 (2)0.015 (2)
O40.0571 (19)0.0376 (17)0.0380 (17)0.0085 (15)0.0044 (14)0.0114 (13)
C280.074 (4)0.059 (3)0.041 (3)0.011 (3)0.016 (3)0.012 (2)
O50.0428 (17)0.0463 (18)0.0339 (16)0.0019 (14)0.0013 (14)0.0058 (13)
C290.037 (2)0.048 (3)0.036 (2)0.019 (2)0.0086 (19)0.0148 (19)
C300.061 (3)0.057 (3)0.039 (3)0.024 (3)0.004 (2)0.015 (2)
C310.085 (4)0.075 (4)0.036 (3)0.039 (3)0.013 (3)0.022 (3)
C320.075 (4)0.070 (4)0.055 (3)0.038 (3)0.030 (3)0.038 (3)
C330.053 (3)0.045 (3)0.062 (3)0.020 (2)0.018 (2)0.027 (2)
C340.043 (2)0.040 (2)0.040 (2)0.019 (2)0.010 (2)0.0162 (19)
C350.036 (2)0.031 (2)0.057 (3)0.0056 (19)0.003 (2)0.012 (2)
N30.0324 (18)0.0335 (19)0.039 (2)0.0060 (15)0.0004 (16)0.0051 (15)
C360.033 (2)0.046 (3)0.044 (3)0.009 (2)0.001 (2)0.002 (2)
C370.047 (3)0.040 (3)0.068 (3)0.003 (2)0.003 (3)0.002 (2)
C380.070 (4)0.041 (3)0.087 (5)0.006 (3)0.010 (3)0.015 (3)
C390.072 (4)0.073 (4)0.060 (4)0.017 (3)0.014 (3)0.033 (3)
C400.064 (3)0.065 (4)0.043 (3)0.020 (3)0.007 (2)0.014 (2)
C410.037 (2)0.051 (3)0.041 (3)0.011 (2)0.004 (2)0.005 (2)
O60.061 (2)0.051 (2)0.0358 (17)0.0081 (16)0.0028 (15)0.0076 (14)
C420.078 (4)0.068 (4)0.042 (3)0.014 (3)0.003 (3)0.013 (3)
Geometric parameters (Å, º) top
La1—O12.324 (3)C20—C211.444 (6)
La1—O52.329 (3)C21—N21.290 (5)
La1—O32.365 (3)C21—H210.9500
La1—N12.747 (3)N2—C221.436 (5)
La1—N22.749 (3)C22—C231.381 (6)
La1—N32.769 (3)C22—C271.382 (6)
La1—O22.781 (3)C23—C241.393 (7)
La1—O62.839 (3)C23—H230.9500
La1—O42.860 (3)C24—C251.362 (7)
O1—C11.304 (4)C24—H240.9500
C1—C61.413 (5)C25—C261.384 (7)
C1—C21.416 (6)C25—H250.9500
C2—C31.366 (6)C26—C271.386 (6)
C2—H20.9500C26—H260.9500
C3—C41.370 (6)C27—O41.380 (5)
C3—H30.9500O4—C281.439 (5)
C4—C51.366 (6)C28—H28A0.9800
C4—H40.9500C28—H28B0.9800
C5—C61.402 (6)C28—H28C0.9800
C5—H50.9500O5—C291.310 (5)
C6—C71.432 (5)C29—C341.406 (6)
C7—N11.288 (5)C29—C301.416 (6)
C7—H70.9500C30—C311.370 (6)
N1—C81.427 (5)C30—H300.9500
C8—C91.385 (6)C31—C321.385 (7)
C8—C131.388 (6)C31—H310.9500
C9—C101.390 (7)C32—C331.366 (7)
C9—H90.9500C32—H320.9500
C10—C111.360 (8)C33—C341.409 (6)
C10—H100.9500C33—H330.9500
C11—C121.381 (7)C34—C351.443 (6)
C11—H110.9500C35—N31.292 (5)
C12—C131.383 (6)C35—H350.9500
C12—H120.9500N3—C361.433 (5)
C13—O21.390 (5)C36—C371.390 (6)
O2—C141.439 (5)C36—C411.402 (6)
C14—H14A0.9800C37—C381.378 (7)
C14—H14B0.9800C37—H370.9500
C14—H14C0.9800C38—C391.356 (8)
O3—C151.298 (5)C38—H380.9500
C15—C161.409 (6)C39—C401.379 (7)
C15—C201.419 (6)C39—H390.9500
C16—C171.365 (6)C40—C411.387 (6)
C16—H160.9500C40—H400.9500
C17—C181.379 (7)C41—O61.384 (5)
C17—H170.9500O6—C421.438 (5)
C18—C191.365 (7)C42—H42A0.9800
C18—H180.9500C42—H42B0.9800
C19—C201.412 (6)C42—H42C0.9800
C19—H190.9500
O1—La1—O591.10 (10)C16—C17—H17119.5
O1—La1—O387.68 (10)C18—C17—H17119.5
O5—La1—O3172.59 (11)C19—C18—C17119.0 (5)
O1—La1—N166.73 (9)C19—C18—H18120.5
O5—La1—N1105.31 (10)C17—C18—H18120.5
O3—La1—N180.91 (10)C18—C19—C20121.8 (5)
O1—La1—N2104.15 (10)C18—C19—H19119.1
O5—La1—N2106.83 (10)C20—C19—H19119.1
O3—La1—N266.47 (10)C19—C20—C15119.3 (4)
N1—La1—N2146.73 (10)C19—C20—C21116.9 (4)
O1—La1—N3152.26 (10)C15—C20—C21123.8 (4)
O5—La1—N366.91 (10)N2—C21—C20126.7 (4)
O3—La1—N3111.88 (10)N2—C21—H21116.7
N1—La1—N3133.54 (10)C20—C21—H21116.7
N2—La1—N368.88 (10)C21—N2—C22117.1 (3)
O1—La1—O2113.99 (9)C21—N2—La1131.2 (3)
O5—La1—O274.90 (10)C22—N2—La1111.8 (2)
O3—La1—O2112.24 (10)C23—C22—C27119.5 (4)
N1—La1—O256.69 (9)C23—C22—N2123.9 (4)
N2—La1—O2141.83 (9)C27—C22—N2116.5 (4)
N3—La1—O277.71 (9)C22—C23—C24119.7 (5)
O1—La1—O6150.42 (9)C22—C23—H23120.1
O5—La1—O6115.36 (9)C24—C23—H23120.1
O3—La1—O667.74 (10)C25—C24—C23120.1 (5)
N1—La1—O692.34 (9)C25—C24—H24120.0
N2—La1—O681.59 (10)C23—C24—H24120.0
N3—La1—O657.06 (9)C24—C25—C26121.0 (5)
O2—La1—O664.62 (9)C24—C25—H25119.5
O1—La1—O467.88 (9)C26—C25—H25119.5
O5—La1—O467.43 (10)C25—C26—C27118.8 (5)
O3—La1—O4105.40 (10)C25—C26—H26120.6
N1—La1—O4133.82 (9)C27—C26—H26120.6
N2—La1—O455.33 (9)O4—C27—C22114.9 (4)
N3—La1—O487.43 (9)O4—C27—C26124.2 (4)
O2—La1—O4142.34 (9)C22—C27—C26120.8 (4)
O6—La1—O4132.91 (9)C27—O4—C28117.7 (3)
C1—O1—La1149.8 (2)C27—O4—La1109.9 (2)
O1—C1—C6121.8 (4)C28—O4—La1118.9 (3)
O1—C1—C2120.9 (4)O4—C28—H28A109.5
C6—C1—C2117.3 (4)O4—C28—H28B109.5
C3—C2—C1120.8 (4)H28A—C28—H28B109.5
C3—C2—H2119.6O4—C28—H28C109.5
C1—C2—H2119.6H28A—C28—H28C109.5
C2—C3—C4122.1 (4)H28B—C28—H28C109.5
C2—C3—H3118.9C29—O5—La1149.3 (3)
C4—C3—H3118.9O5—C29—C34121.7 (4)
C5—C4—C3118.4 (4)O5—C29—C30120.8 (4)
C5—C4—H4120.8C34—C29—C30117.5 (4)
C3—C4—H4120.8C31—C30—C29121.4 (5)
C4—C5—C6122.2 (4)C31—C30—H30119.3
C4—C5—H5118.9C29—C30—H30119.3
C6—C5—H5118.9C30—C31—C32120.7 (5)
C5—C6—C1119.2 (4)C30—C31—H31119.7
C5—C6—C7117.2 (4)C32—C31—H31119.7
C1—C6—C7123.5 (4)C33—C32—C31119.6 (5)
N1—C7—C6128.2 (4)C33—C32—H32120.2
N1—C7—H7115.9C31—C32—H32120.2
C6—C7—H7115.9C32—C33—C34121.2 (5)
C7—N1—C8115.2 (3)C32—C33—H33119.4
C7—N1—La1129.9 (3)C34—C33—H33119.4
C8—N1—La1114.9 (2)C29—C34—C33119.7 (4)
C9—C8—C13119.1 (4)C29—C34—C35124.0 (4)
C9—C8—N1123.3 (4)C33—C34—C35116.3 (4)
C13—C8—N1117.6 (4)N3—C35—C34128.1 (4)
C8—C9—C10119.8 (5)N3—C35—H35115.9
C8—C9—H9120.1C34—C35—H35115.9
C10—C9—H9120.1C35—N3—C36114.8 (4)
C11—C10—C9120.1 (5)C35—N3—La1129.1 (3)
C11—C10—H10120.0C36—N3—La1116.0 (3)
C9—C10—H10120.0C37—C36—C41118.5 (4)
C10—C11—C12121.3 (5)C37—C36—N3123.4 (4)
C10—C11—H11119.3C41—C36—N3118.1 (4)
C12—C11—H11119.3C38—C37—C36120.5 (5)
C11—C12—C13118.5 (5)C38—C37—H37119.8
C11—C12—H12120.7C36—C37—H37119.8
C13—C12—H12120.7C39—C38—C37120.4 (5)
C12—C13—C8121.1 (4)C39—C38—H38119.8
C12—C13—O2124.4 (4)C37—C38—H38119.8
C8—C13—O2114.5 (3)C38—C39—C40120.9 (5)
C13—O2—C14116.6 (3)C38—C39—H39119.5
C13—O2—La1116.5 (2)C40—C39—H39119.5
C14—O2—La1119.3 (2)C39—C40—C41119.5 (5)
O2—C14—H14A109.5C39—C40—H40120.2
O2—C14—H14B109.5C41—C40—H40120.2
H14A—C14—H14B109.5O6—C41—C40124.1 (4)
O2—C14—H14C109.5O6—C41—C36115.8 (4)
H14A—C14—H14C109.5C40—C41—C36120.1 (5)
H14B—C14—H14C109.5C41—O6—C42116.1 (3)
C15—O3—La1146.6 (3)C41—O6—La1116.4 (2)
O3—C15—C16120.9 (4)C42—O6—La1121.1 (3)
O3—C15—C20122.4 (4)O6—C42—H42A109.5
C16—C15—C20116.7 (4)O6—C42—H42B109.5
C17—C16—C15122.3 (5)H42A—C42—H42B109.5
C17—C16—H16118.8O6—C42—H42C109.5
C15—C16—H16118.8H42A—C42—H42C109.5
C16—C17—C18120.9 (5)H42B—C42—H42C109.5
La1—O1—C1—C61.6 (8)La1—N2—C22—C23135.3 (4)
La1—O1—C1—C2178.5 (3)C21—N2—C22—C27140.3 (4)
O1—C1—C2—C3178.6 (4)La1—N2—C22—C2741.6 (4)
C6—C1—C2—C31.4 (6)C27—C22—C23—C240.1 (6)
C1—C2—C3—C40.7 (7)N2—C22—C23—C24176.7 (4)
C2—C3—C4—C51.6 (8)C22—C23—C24—C250.2 (7)
C3—C4—C5—C60.4 (7)C23—C24—C25—C261.3 (8)
C4—C5—C6—C11.8 (7)C24—C25—C26—C272.0 (7)
C4—C5—C6—C7179.6 (4)C23—C22—C27—O4179.8 (4)
O1—C1—C6—C5177.4 (4)N2—C22—C27—O43.2 (5)
C2—C1—C6—C52.6 (6)C23—C22—C27—C260.6 (6)
O1—C1—C6—C70.3 (6)N2—C22—C27—C26177.7 (4)
C2—C1—C6—C7179.7 (4)C25—C26—C27—O4179.2 (4)
C5—C6—C7—N1178.8 (4)C25—C26—C27—C221.7 (7)
C1—C6—C7—N11.0 (7)C22—C27—O4—C28175.8 (4)
C6—C7—N1—C8180.0 (4)C26—C27—O4—C283.3 (6)
C6—C7—N1—La11.4 (6)C22—C27—O4—La143.8 (4)
C7—N1—C8—C938.9 (6)C26—C27—O4—La1137.1 (4)
La1—N1—C8—C9142.2 (4)La1—O5—C29—C3414.4 (8)
C7—N1—C8—C13143.7 (4)La1—O5—C29—C30168.1 (4)
La1—N1—C8—C1335.1 (4)O5—C29—C30—C31175.0 (4)
C13—C8—C9—C101.5 (7)C34—C29—C30—C312.5 (7)
N1—C8—C9—C10178.9 (5)C29—C30—C31—C320.8 (8)
C8—C9—C10—C111.7 (9)C30—C31—C32—C330.8 (8)
C9—C10—C11—C122.1 (10)C31—C32—C33—C340.6 (7)
C10—C11—C12—C130.7 (9)O5—C29—C34—C33174.8 (4)
C11—C12—C13—C84.0 (8)C30—C29—C34—C332.7 (6)
C11—C12—C13—O2177.6 (5)O5—C29—C34—C354.3 (6)
C9—C8—C13—C124.4 (7)C30—C29—C34—C35178.2 (4)
N1—C8—C13—C12178.1 (4)C32—C33—C34—C291.2 (7)
C9—C8—C13—O2177.0 (4)C32—C33—C34—C35179.6 (4)
N1—C8—C13—O20.5 (6)C29—C34—C35—N33.8 (7)
C12—C13—O2—C142.3 (6)C33—C34—C35—N3177.0 (4)
C8—C13—O2—C14176.2 (4)C34—C35—N3—C36177.0 (4)
C12—C13—O2—La1147.1 (4)C34—C35—N3—La15.6 (7)
C8—C13—O2—La134.4 (4)C35—N3—C36—C3736.5 (6)
La1—O3—C15—C16158.5 (4)La1—N3—C36—C37145.7 (4)
La1—O3—C15—C2023.3 (8)C35—N3—C36—C41145.3 (4)
O3—C15—C16—C17178.3 (5)La1—N3—C36—C4132.5 (5)
C20—C15—C16—C170.1 (8)C41—C36—C37—C383.4 (7)
C15—C16—C17—C181.4 (9)N3—C36—C37—C38178.4 (4)
C16—C17—C18—C191.1 (8)C36—C37—C38—C392.5 (8)
C17—C18—C19—C200.4 (8)C37—C38—C39—C400.4 (9)
C18—C19—C20—C151.6 (7)C38—C39—C40—C410.9 (8)
C18—C19—C20—C21179.8 (4)C39—C40—C41—O6179.6 (5)
O3—C15—C20—C19176.8 (4)C39—C40—C41—C360.1 (7)
C16—C15—C20—C191.4 (6)C37—C36—C41—O6178.2 (4)
O3—C15—C20—C211.3 (7)N3—C36—C41—O60.0 (6)
C16—C15—C20—C21179.5 (4)C37—C36—C41—C402.2 (7)
C19—C20—C21—N2175.8 (4)N3—C36—C41—C40179.5 (4)
C15—C20—C21—N26.0 (7)C40—C41—O6—C423.5 (6)
C20—C21—N2—C22179.0 (4)C36—C41—O6—C42176.0 (4)
C20—C21—N2—La11.3 (6)C40—C41—O6—La1148.8 (4)
C21—N2—C22—C2342.8 (6)C36—C41—O6—La131.7 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12···O3i0.952.513.402 (6)157
C14—H14A···O1i0.982.323.295 (5)171
C28—H28B···O10.982.503.132 (6)122
Symmetry code: (i) x1, y, z.
Tris(2-{[(2-methoxyphenyl)imino]methyl}phenolato-κ3O1,N,O2)neodymium tetrahydrofuran disolvate (mol2) top
Crystal data top
[La(C14H12NO2)3]·2C4H8OZ = 2
Mr = 967.18F(000) = 994
Triclinic, P1Dx = 1.464 Mg m3
a = 11.1951 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.8767 (8) ÅCell parameters from 999 reflections
c = 15.1894 (8) Åθ = 3–30°
α = 69.758 (1)°µ = 1.24 mm1
β = 74.797 (1)°T = 120 K
γ = 69.502 (1)°Prism, brown
V = 2194.4 (2) Å30.41 × 0.29 × 0.21 mm
Data collection top
Bruker APEXII CCD
diffractometer
10582 independent reflections
Radiation source: fine-focus sealed tube9480 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
φ and ω scansθmax = 28.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1414
Tmin = 0.650, Tmax = 0.756k = 1919
34010 measured reflectionsl = 2020
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0327P)2 + 0.9562P]
where P = (Fo2 + 2Fc2)/3
10582 reflections(Δ/σ)max = 0.001
596 parametersΔρmax = 0.99 e Å3
20 restraintsΔρmin = 0.63 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/UeqOcc. (<1)
Nd10.88487 (2)0.37135 (2)0.32444 (2)0.01386 (4)
O10.80997 (14)0.54187 (11)0.25778 (10)0.0189 (3)
C10.7271 (2)0.59427 (15)0.19942 (15)0.0181 (4)
C20.7550 (2)0.67225 (17)0.11921 (16)0.0254 (5)
H20.8329950.6885380.1102870.030*
C30.6722 (3)0.72521 (19)0.05365 (17)0.0312 (5)
H30.6953980.7756940.0003150.037*
C40.5553 (2)0.7060 (2)0.06519 (17)0.0327 (6)
H40.4991270.7420590.0193630.039*
C50.5227 (2)0.63335 (18)0.14476 (17)0.0270 (5)
H50.4418680.6211090.1541750.032*
C60.6056 (2)0.57680 (16)0.21242 (15)0.0193 (4)
C70.5607 (2)0.50368 (16)0.29465 (15)0.0191 (4)
H70.4715910.5079510.3059940.023*
N10.63081 (16)0.43393 (13)0.35322 (12)0.0165 (3)
C80.5690 (2)0.37258 (17)0.43312 (14)0.0186 (4)
C90.4557 (2)0.40896 (19)0.49135 (16)0.0227 (5)
H90.4119610.4784870.4763400.027*
C100.4070 (2)0.3434 (2)0.57132 (16)0.0307 (6)
H100.3317640.3684180.6123620.037*
C110.4674 (3)0.2422 (2)0.59121 (17)0.0366 (6)
H110.4322210.1977030.6451170.044*
C120.5794 (2)0.2044 (2)0.53333 (17)0.0313 (5)
H120.6200960.1344470.5467570.038*
C130.6307 (2)0.27015 (17)0.45589 (15)0.0215 (4)
O20.74504 (15)0.24131 (11)0.39624 (11)0.0229 (3)
C140.7790 (3)0.14353 (19)0.3847 (2)0.0367 (6)
H14A0.7030250.1323510.3745990.055*
H14B0.8099870.0933790.4419110.055*
H14C0.8474120.1378510.3296160.055*
O30.83187 (14)0.37673 (12)0.47760 (10)0.0222 (3)
C150.8756 (2)0.37267 (15)0.55082 (14)0.0160 (4)
C160.7962 (2)0.36216 (17)0.64131 (15)0.0203 (4)
H160.7125890.3555840.6481400.024*
C170.8375 (2)0.36126 (17)0.71959 (15)0.0233 (5)
H170.7819150.3540570.7792130.028*
C180.9594 (2)0.37076 (18)0.71272 (15)0.0238 (5)
H180.9866850.3713660.7666530.029*
C191.0396 (2)0.37924 (16)0.62603 (15)0.0199 (4)
H191.1226190.3860130.6208330.024*
C201.0020 (2)0.37818 (15)0.54465 (14)0.0161 (4)
C211.09777 (19)0.38312 (15)0.45913 (14)0.0166 (4)
H211.1741930.3951530.4624220.020*
N21.09278 (16)0.37327 (13)0.37879 (12)0.0153 (3)
C221.20735 (19)0.37208 (15)0.30922 (14)0.0163 (4)
C231.3324 (2)0.33635 (17)0.33056 (16)0.0202 (4)
H231.3447700.3130390.3950900.024*
C241.4391 (2)0.33435 (18)0.25891 (17)0.0249 (5)
H241.5236950.3105360.2744250.030*
C251.4217 (2)0.3672 (2)0.16490 (17)0.0279 (5)
H251.4948090.3660610.1159340.033*
C261.2985 (2)0.40169 (18)0.14133 (16)0.0238 (5)
H261.2869190.4237320.0766960.029*
C271.1927 (2)0.40353 (16)0.21351 (15)0.0176 (4)
O41.06701 (14)0.43495 (12)0.19699 (10)0.0189 (3)
C281.0471 (2)0.47289 (19)0.09954 (14)0.0239 (5)
H28A1.0818890.5301520.0675460.036*
H28B0.9543740.4940720.0971660.036*
H28C1.0913820.4203130.0674660.036*
O50.82850 (14)0.36269 (12)0.19364 (10)0.0209 (3)
C290.8539 (2)0.32021 (17)0.12708 (14)0.0193 (4)
C300.7655 (2)0.35165 (19)0.06263 (15)0.0246 (5)
H300.6877570.4035290.0695640.029*
C310.7904 (3)0.3085 (2)0.00967 (16)0.0322 (6)
H310.7291040.3303250.0511710.039*
C320.9047 (3)0.2329 (2)0.02267 (17)0.0351 (6)
H320.9220350.2043000.0734000.042*
C330.9913 (3)0.20050 (19)0.03843 (16)0.0298 (5)
H331.0686870.1488330.0296610.036*
C340.9690 (2)0.24178 (17)0.11433 (15)0.0207 (4)
C351.0629 (2)0.19917 (17)0.17766 (16)0.0231 (5)
H351.1369120.1478110.1623550.028*
N31.05773 (17)0.22308 (14)0.25316 (13)0.0202 (4)
C361.1629 (2)0.16946 (16)0.30488 (17)0.0237 (5)
C371.2921 (2)0.14392 (19)0.2615 (2)0.0330 (6)
H371.3130470.1596780.1942200.040*
C381.3893 (3)0.0957 (2)0.3167 (3)0.0437 (7)
H381.4769510.0779950.2872900.052*
C391.3587 (3)0.0734 (2)0.4143 (3)0.0462 (8)
H391.4259710.0402110.4516270.055*
C401.2308 (3)0.09872 (19)0.4595 (2)0.0377 (6)
H401.2107800.0832000.5268590.045*
C411.1337 (2)0.14701 (17)0.40401 (18)0.0258 (5)
O61.00416 (16)0.17787 (12)0.43951 (11)0.0268 (4)
C420.9651 (3)0.1443 (2)0.54049 (17)0.0359 (6)
H42A0.9896460.0710110.5612890.054*
H42B0.8712200.1707210.5561710.054*
H42C1.0078460.1681280.5728880.054*
O7A0.7607 (7)0.9863 (5)0.2928 (4)0.0602 (15)0.695 (9)
C43A0.7830 (14)1.0487 (7)0.1975 (5)0.082 (2)0.695 (9)
H43A0.8597521.0714400.1883000.099*0.695 (9)
H43B0.7074011.1082590.1851600.099*0.695 (9)
C46A0.8153 (9)0.8873 (5)0.2814 (6)0.072 (2)0.695 (9)
H46A0.7827100.8382280.3371150.086*0.695 (9)
H46B0.9107590.8674790.2739790.086*0.695 (9)
C45A0.7734 (8)0.8926 (5)0.1932 (4)0.0685 (17)0.695 (9)
H45A0.6801050.8989740.2030590.082*0.695 (9)
H45B0.8244830.8346710.1683230.082*0.695 (9)
C44A0.8046 (10)0.9877 (6)0.1310 (4)0.090 (3)0.695 (9)
H44A0.8953720.9732620.0984940.107*0.695 (9)
H44B0.7470361.0234060.0824180.107*0.695 (9)
O7B0.8101 (16)0.9804 (13)0.2793 (11)0.0602 (15)0.305 (9)
C43B0.759 (3)1.0631 (16)0.2025 (14)0.082 (2)0.305 (9)
H43C0.8269951.0964370.1665410.099*0.305 (9)
H43D0.6862011.1121590.2292950.099*0.305 (9)
C46B0.785 (3)0.8965 (15)0.2697 (13)0.072 (2)0.305 (9)
H46C0.7002350.8884190.3073810.086*0.305 (9)
H46D0.8533250.8338730.2901670.086*0.305 (9)
C45B0.7829 (19)0.9238 (11)0.1651 (12)0.0685 (17)0.305 (9)
H45C0.7373960.8843090.1523420.082*0.305 (9)
H45D0.8721320.9102310.1297020.082*0.305 (9)
C44B0.713 (2)1.0335 (11)0.1350 (11)0.090 (3)0.305 (9)
H44C0.7423701.0657470.0676130.107*0.305 (9)
H44D0.6181141.0466410.1470060.107*0.305 (9)
O8A0.2528 (5)0.0035 (4)0.0896 (5)0.0777 (16)0.623 (5)
C47A0.2151 (9)0.0787 (8)0.1613 (6)0.098 (3)0.623 (5)
H47A0.2439100.1385780.1379900.118*0.623 (5)
H47B0.1201540.0612220.1808400.118*0.623 (5)
C48A0.2819 (6)0.0968 (5)0.2426 (4)0.0691 (18)0.623 (5)
H48A0.2444380.0421860.2735980.083*0.623 (5)
H48B0.2808470.1616710.2906940.083*0.623 (5)
C49A0.4149 (6)0.0973 (5)0.1875 (4)0.0665 (18)0.623 (5)
H49A0.4598570.0700670.2159040.080*0.623 (5)
H49B0.4677190.1657590.1852860.080*0.623 (5)
C50A0.3896 (6)0.0310 (4)0.0902 (5)0.079 (2)0.623 (5)
H50A0.4239430.0267830.0735150.095*0.623 (5)
H50B0.4336490.0686740.0426030.095*0.623 (5)
O8B0.3017 (10)0.0182 (9)0.0840 (9)0.0777 (16)0.377 (5)
C47B0.1917 (14)0.0562 (16)0.1141 (7)0.098 (3)0.377 (5)
H47C0.2080860.1145620.0907170.118*0.377 (5)
H47D0.1140790.0040880.0909070.118*0.377 (5)
C49B0.3158 (9)0.1269 (8)0.2319 (8)0.0665 (18)0.377 (5)
H49C0.3261810.1247120.2937750.080*0.377 (5)
H49D0.3492030.1973300.2297470.080*0.377 (5)
C48B0.1756 (10)0.0859 (7)0.2206 (7)0.0691 (18)0.377 (5)
H48C0.1291880.1375850.2505040.083*0.377 (5)
H48D0.1307620.0277920.2463170.083*0.377 (5)
C50B0.3893 (10)0.0638 (8)0.1518 (9)0.079 (2)0.377 (5)
H50C0.4050150.0131190.1722630.095*0.377 (5)
H50D0.4727970.1053110.1260050.095*0.377 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.01245 (5)0.01877 (6)0.01095 (5)0.00422 (4)0.00305 (4)0.00427 (4)
O10.0182 (7)0.0202 (8)0.0193 (7)0.0063 (6)0.0053 (6)0.0045 (6)
C10.0197 (10)0.0163 (10)0.0178 (10)0.0020 (8)0.0033 (8)0.0071 (8)
C20.0266 (12)0.0233 (12)0.0238 (11)0.0070 (9)0.0026 (9)0.0047 (9)
C30.0369 (14)0.0254 (13)0.0217 (11)0.0036 (11)0.0050 (10)0.0005 (10)
C40.0294 (13)0.0355 (14)0.0228 (11)0.0033 (11)0.0120 (10)0.0026 (10)
C50.0204 (11)0.0322 (13)0.0261 (11)0.0013 (10)0.0073 (9)0.0090 (10)
C60.0185 (10)0.0190 (10)0.0184 (10)0.0009 (8)0.0044 (8)0.0064 (8)
C70.0136 (9)0.0246 (11)0.0220 (10)0.0042 (8)0.0027 (8)0.0116 (9)
N10.0147 (8)0.0206 (9)0.0170 (8)0.0056 (7)0.0019 (7)0.0085 (7)
C80.0166 (10)0.0279 (11)0.0166 (9)0.0103 (9)0.0026 (8)0.0087 (8)
C90.0153 (10)0.0370 (13)0.0229 (11)0.0081 (9)0.0039 (8)0.0155 (10)
C100.0185 (11)0.0592 (18)0.0196 (11)0.0172 (11)0.0020 (9)0.0150 (11)
C110.0310 (13)0.0555 (18)0.0203 (11)0.0238 (13)0.0004 (10)0.0019 (11)
C120.0287 (13)0.0327 (14)0.0281 (12)0.0140 (11)0.0051 (10)0.0026 (10)
C130.0180 (10)0.0293 (12)0.0183 (10)0.0096 (9)0.0030 (8)0.0053 (9)
O20.0210 (8)0.0199 (8)0.0262 (8)0.0074 (6)0.0018 (6)0.0072 (6)
C140.0372 (14)0.0271 (13)0.0497 (16)0.0135 (11)0.0031 (12)0.0186 (12)
O30.0179 (7)0.0365 (9)0.0145 (7)0.0090 (7)0.0033 (6)0.0081 (6)
C150.0172 (10)0.0173 (10)0.0120 (9)0.0026 (8)0.0032 (7)0.0043 (8)
C160.0165 (10)0.0256 (11)0.0170 (10)0.0050 (9)0.0011 (8)0.0060 (8)
C170.0228 (11)0.0291 (12)0.0137 (9)0.0041 (9)0.0005 (8)0.0063 (9)
C180.0269 (12)0.0301 (12)0.0168 (10)0.0047 (10)0.0073 (9)0.0103 (9)
C190.0203 (10)0.0237 (11)0.0185 (10)0.0059 (9)0.0055 (8)0.0079 (8)
C200.0182 (10)0.0171 (10)0.0125 (9)0.0039 (8)0.0040 (8)0.0037 (8)
C210.0147 (9)0.0170 (10)0.0187 (10)0.0039 (8)0.0040 (8)0.0055 (8)
N20.0148 (8)0.0185 (9)0.0126 (8)0.0052 (7)0.0023 (6)0.0040 (7)
C220.0156 (9)0.0186 (10)0.0170 (9)0.0059 (8)0.0013 (8)0.0077 (8)
C230.0174 (10)0.0249 (11)0.0221 (10)0.0054 (9)0.0041 (8)0.0113 (9)
C240.0153 (10)0.0349 (13)0.0291 (12)0.0059 (9)0.0024 (9)0.0165 (10)
C250.0193 (11)0.0433 (15)0.0243 (11)0.0127 (10)0.0054 (9)0.0161 (11)
C260.0214 (11)0.0343 (13)0.0169 (10)0.0110 (10)0.0002 (8)0.0080 (9)
C270.0160 (10)0.0213 (11)0.0181 (10)0.0063 (8)0.0030 (8)0.0074 (8)
O40.0150 (7)0.0298 (8)0.0113 (6)0.0078 (6)0.0019 (5)0.0040 (6)
C280.0237 (11)0.0358 (13)0.0126 (9)0.0121 (10)0.0041 (8)0.0026 (9)
O50.0177 (7)0.0285 (8)0.0182 (7)0.0036 (6)0.0052 (6)0.0100 (6)
C290.0210 (10)0.0276 (11)0.0126 (9)0.0147 (9)0.0006 (8)0.0043 (8)
C300.0225 (11)0.0393 (14)0.0147 (10)0.0155 (10)0.0022 (8)0.0047 (9)
C310.0360 (14)0.0536 (17)0.0167 (10)0.0256 (13)0.0056 (10)0.0075 (11)
C320.0480 (16)0.0510 (17)0.0187 (11)0.0259 (14)0.0006 (11)0.0163 (11)
C330.0383 (14)0.0329 (13)0.0219 (11)0.0144 (11)0.0028 (10)0.0136 (10)
C340.0235 (11)0.0251 (11)0.0162 (10)0.0111 (9)0.0003 (8)0.0077 (8)
C350.0216 (11)0.0232 (11)0.0240 (11)0.0064 (9)0.0002 (9)0.0091 (9)
N30.0184 (9)0.0198 (9)0.0219 (9)0.0034 (7)0.0059 (7)0.0053 (7)
C360.0214 (11)0.0161 (10)0.0335 (12)0.0002 (9)0.0120 (9)0.0067 (9)
C370.0217 (12)0.0275 (13)0.0524 (16)0.0005 (10)0.0094 (11)0.0186 (12)
C380.0253 (13)0.0300 (14)0.077 (2)0.0032 (11)0.0205 (14)0.0193 (15)
C390.0389 (16)0.0248 (14)0.079 (2)0.0005 (12)0.0410 (16)0.0044 (14)
C400.0452 (16)0.0219 (13)0.0480 (16)0.0075 (11)0.0296 (13)0.0019 (11)
C410.0291 (12)0.0151 (11)0.0347 (13)0.0050 (9)0.0167 (10)0.0014 (9)
O60.0296 (9)0.0280 (9)0.0197 (8)0.0077 (7)0.0095 (7)0.0004 (7)
C420.0560 (17)0.0276 (13)0.0199 (11)0.0108 (12)0.0123 (11)0.0019 (10)
O7A0.101 (5)0.0500 (17)0.035 (2)0.040 (3)0.019 (3)0.0220 (14)
C43A0.141 (7)0.078 (4)0.045 (2)0.072 (4)0.012 (3)0.015 (2)
C46A0.095 (6)0.059 (3)0.091 (4)0.030 (4)0.042 (3)0.027 (3)
C45A0.118 (4)0.057 (4)0.054 (4)0.062 (4)0.001 (4)0.017 (3)
C44A0.157 (9)0.092 (6)0.040 (2)0.062 (6)0.004 (5)0.026 (3)
O7B0.101 (5)0.0500 (17)0.035 (2)0.040 (3)0.019 (3)0.0220 (14)
C43B0.141 (7)0.078 (4)0.045 (2)0.072 (4)0.012 (3)0.015 (2)
C46B0.095 (6)0.059 (3)0.091 (4)0.030 (4)0.042 (3)0.027 (3)
C45B0.118 (4)0.057 (4)0.054 (4)0.062 (4)0.001 (4)0.017 (3)
C44B0.157 (9)0.092 (6)0.040 (2)0.062 (6)0.004 (5)0.026 (3)
O8A0.088 (5)0.057 (3)0.071 (2)0.035 (3)0.057 (4)0.023 (2)
C47A0.070 (5)0.152 (8)0.116 (8)0.043 (5)0.020 (5)0.074 (8)
C48A0.095 (5)0.032 (3)0.067 (4)0.016 (3)0.015 (3)0.002 (3)
C49A0.091 (5)0.033 (3)0.074 (4)0.002 (3)0.045 (4)0.011 (3)
C50A0.089 (4)0.029 (3)0.085 (5)0.020 (3)0.022 (5)0.007 (3)
O8B0.088 (5)0.057 (3)0.071 (2)0.035 (3)0.057 (4)0.023 (2)
C47B0.070 (5)0.152 (8)0.116 (8)0.043 (5)0.020 (5)0.074 (8)
C49B0.091 (5)0.033 (3)0.074 (4)0.002 (3)0.045 (4)0.011 (3)
C48B0.095 (5)0.032 (3)0.067 (4)0.016 (3)0.015 (3)0.002 (3)
C50B0.089 (4)0.029 (3)0.085 (5)0.020 (3)0.022 (5)0.007 (3)
Geometric parameters (Å, º) top
Nd1—O32.2676 (14)C32—C331.367 (4)
Nd1—O52.2922 (14)C32—H320.9500
Nd1—O12.3113 (15)C33—C341.414 (3)
Nd1—O42.6104 (14)C33—H330.9500
Nd1—N12.6311 (17)C34—C351.440 (3)
Nd1—O22.6736 (15)C35—N31.295 (3)
Nd1—N22.6778 (17)C35—H350.9500
Nd1—N32.7104 (18)N3—C361.426 (3)
Nd1—O62.8590 (16)C36—C411.399 (3)
O1—C11.304 (3)C36—C371.399 (3)
C1—C21.416 (3)C37—C381.384 (4)
C1—C61.424 (3)C37—H370.9500
C2—C31.379 (3)C38—C391.378 (5)
C2—H20.9500C38—H380.9500
C3—C41.390 (4)C39—C401.395 (4)
C3—H30.9500C39—H390.9500
C4—C51.379 (3)C40—C411.387 (3)
C4—H40.9500C40—H400.9500
C5—C61.407 (3)C41—O61.378 (3)
C5—H50.9500O6—C421.437 (3)
C6—C71.452 (3)C42—H42A0.9800
C7—N11.281 (3)C42—H42B0.9800
C7—H70.9500C42—H42C0.9800
N1—C81.421 (3)O7A—C43A1.436 (4)
C8—C131.394 (3)O7A—C46A1.436 (4)
C8—C91.395 (3)C43A—C44A1.503 (3)
C9—C101.389 (3)C43A—H43A0.9900
C9—H90.9500C43A—H43B0.9900
C10—C111.376 (4)C46A—C45A1.501 (3)
C10—H100.9500C46A—H46A0.9900
C11—C121.389 (4)C46A—H46B0.9900
C11—H110.9500C45A—C44A1.504 (3)
C12—C131.383 (3)C45A—H45A0.9900
C12—H120.9500C45A—H45B0.9900
C13—O21.386 (3)C44A—H44A0.9900
O2—C141.430 (3)C44A—H44B0.9900
C14—H14A0.9800O7B—C46B1.436 (4)
C14—H14B0.9800O7B—C43B1.436 (4)
C14—H14C0.9800C43B—C44B1.503 (3)
O3—C151.303 (2)C43B—H43C0.9900
C15—C161.418 (3)C43B—H43D0.9900
C15—C201.423 (3)C46B—C45B1.502 (3)
C16—C171.379 (3)C46B—H46C0.9900
C16—H160.9500C46B—H46D0.9900
C17—C181.395 (3)C45B—C44B1.503 (4)
C17—H170.9500C45B—H45C0.9900
C18—C191.378 (3)C45B—H45D0.9900
C18—H180.9500C44B—H44C0.9900
C19—C201.413 (3)C44B—H44D0.9900
C19—H190.9500O8A—C47A1.435 (4)
C20—C211.450 (3)O8A—C50A1.437 (4)
C21—N21.296 (3)C47A—C48A1.507 (3)
C21—H210.9500C47A—H47A0.9900
N2—C221.431 (2)C47A—H47B0.9900
C22—C231.395 (3)C48A—C49A1.504 (3)
C22—C271.400 (3)C48A—H48A0.9900
C23—C241.388 (3)C48A—H48B0.9900
C23—H230.9500C49A—C50A1.501 (3)
C24—C251.383 (3)C49A—H49A0.9900
C24—H240.9500C49A—H49B0.9900
C25—C261.390 (3)C50A—H50A0.9900
C25—H250.9500C50A—H50B0.9900
C26—C271.387 (3)O8B—C47B1.434 (4)
C26—H260.9500O8B—C50B1.436 (4)
C27—O41.380 (2)C47B—C48B1.501 (3)
O4—C281.438 (2)C47B—H47C0.9900
C28—H28A0.9800C47B—H47D0.9900
C28—H28B0.9800C49B—C50B1.504 (3)
C28—H28C0.9800C49B—C48B1.505 (3)
O5—C291.291 (3)C49B—H49C0.9900
C29—C301.422 (3)C49B—H49D0.9900
C29—C341.426 (3)C48B—H48C0.9900
C30—C311.378 (3)C48B—H48D0.9900
C30—H300.9500C50B—H50C0.9900
C31—C321.398 (4)C50B—H50D0.9900
C31—H310.9500
O3—Nd1—O5149.61 (5)C29—C30—H30119.3
O3—Nd1—O195.98 (5)C30—C31—C32120.8 (2)
O5—Nd1—O183.53 (5)C30—C31—H31119.6
O3—Nd1—O4126.54 (5)C32—C31—H31119.6
O5—Nd1—O482.02 (5)C33—C32—C31119.3 (2)
O1—Nd1—O470.26 (5)C33—C32—H32120.4
O3—Nd1—N175.80 (5)C31—C32—H32120.4
O5—Nd1—N175.80 (5)C32—C33—C34121.8 (2)
O1—Nd1—N168.58 (5)C32—C33—H33119.1
O4—Nd1—N1134.87 (5)C34—C33—H33119.1
O3—Nd1—O280.34 (5)C33—C34—C29119.3 (2)
O5—Nd1—O275.98 (5)C33—C34—C35117.6 (2)
O1—Nd1—O2126.91 (5)C29—C34—C35123.02 (19)
O4—Nd1—O2149.33 (5)N3—C35—C34127.2 (2)
N1—Nd1—O259.12 (5)N3—C35—H35116.4
O3—Nd1—N271.38 (5)C34—C35—H35116.4
O5—Nd1—N2138.97 (5)C35—N3—C36116.84 (19)
O1—Nd1—N296.88 (5)C35—N3—Nd1130.13 (15)
O4—Nd1—N260.17 (5)C36—N3—Nd1112.85 (13)
N1—Nd1—N2142.39 (5)C41—C36—C37119.3 (2)
O2—Nd1—N2130.04 (5)C41—C36—N3117.1 (2)
O3—Nd1—N3128.04 (6)C37—C36—N3123.5 (2)
O5—Nd1—N367.78 (5)C38—C37—C36120.1 (3)
O1—Nd1—N3132.20 (5)C38—C37—H37120.0
O4—Nd1—N368.59 (5)C36—C37—H37120.0
N1—Nd1—N3132.91 (5)C39—C38—C37119.9 (3)
O2—Nd1—N383.30 (5)C39—C38—H38120.1
N2—Nd1—N382.99 (5)C37—C38—H38120.1
O3—Nd1—O672.47 (5)C38—C39—C40121.4 (3)
O5—Nd1—O6111.98 (5)C38—C39—H39119.3
O1—Nd1—O6164.14 (5)C40—C39—H39119.3
O4—Nd1—O6107.47 (5)C41—C40—C39118.6 (3)
N1—Nd1—O6117.17 (5)C41—C40—H40120.7
O2—Nd1—O663.04 (5)C39—C40—H40120.7
N2—Nd1—O669.45 (5)O6—C41—C40124.4 (2)
N3—Nd1—O656.20 (5)O6—C41—C36114.78 (19)
C1—O1—Nd1131.31 (13)C40—C41—C36120.8 (2)
O1—C1—C2120.7 (2)C41—O6—C42117.70 (19)
O1—C1—C6122.53 (19)C41—O6—Nd1110.41 (13)
C2—C1—C6116.8 (2)C42—O6—Nd1123.21 (15)
C3—C2—C1121.8 (2)O6—C42—H42A109.5
C3—C2—H2119.1O6—C42—H42B109.5
C1—C2—H2119.1H42A—C42—H42B109.5
C2—C3—C4121.1 (2)O6—C42—H42C109.5
C2—C3—H3119.4H42A—C42—H42C109.5
C4—C3—H3119.4H42B—C42—H42C109.5
C5—C4—C3118.4 (2)C43A—O7A—C46A102.7 (7)
C5—C4—H4120.8O7A—C43A—C44A107.6 (6)
C3—C4—H4120.8O7A—C43A—H43A110.2
C4—C5—C6122.0 (2)C44A—C43A—H43A110.2
C4—C5—H5119.0O7A—C43A—H43B110.2
C6—C5—H5119.0C44A—C43A—H43B110.2
C5—C6—C1119.7 (2)H43A—C43A—H43B108.5
C5—C6—C7117.5 (2)O7A—C46A—C45A105.4 (6)
C1—C6—C7122.74 (19)O7A—C46A—H46A110.7
N1—C7—C6125.71 (19)C45A—C46A—H46A110.7
N1—C7—H7117.1O7A—C46A—H46B110.7
C6—C7—H7117.1C45A—C46A—H46B110.7
C7—N1—C8118.07 (18)H46A—C46A—H46B108.8
C7—N1—Nd1125.63 (14)C46A—C45A—C44A97.7 (6)
C8—N1—Nd1115.33 (13)C46A—C45A—H45A112.2
C13—C8—C9119.0 (2)C44A—C45A—H45A112.2
C13—C8—N1116.70 (18)C46A—C45A—H45B112.2
C9—C8—N1124.2 (2)C44A—C45A—H45B112.2
C10—C9—C8119.9 (2)H45A—C45A—H45B109.8
C10—C9—H9120.0C43A—C44A—C45A105.0 (6)
C8—C9—H9120.0C43A—C44A—H44A110.7
C11—C10—C9120.2 (2)C45A—C44A—H44A110.7
C11—C10—H10119.9C43A—C44A—H44B110.7
C9—C10—H10119.9C45A—C44A—H44B110.7
C10—C11—C12120.7 (2)H44A—C44A—H44B108.8
C10—C11—H11119.6C46B—O7B—C43B104.7 (18)
C12—C11—H11119.6O7B—C43B—C44B113.7 (17)
C13—C12—C11119.0 (2)O7B—C43B—H43C108.8
C13—C12—H12120.5C44B—C43B—H43C108.8
C11—C12—H12120.5O7B—C43B—H43D108.8
C12—C13—O2124.0 (2)C44B—C43B—H43D108.8
C12—C13—C8121.1 (2)H43C—C43B—H43D107.7
O2—C13—C8114.98 (18)O7B—C46B—C45B102.9 (15)
C13—O2—C14116.81 (18)O7B—C46B—H46C111.2
C13—O2—Nd1115.79 (13)C45B—C46B—H46C111.2
C14—O2—Nd1127.28 (14)O7B—C46B—H46D111.2
O2—C14—H14A109.5C45B—C46B—H46D111.2
O2—C14—H14B109.5H46C—C46B—H46D109.1
H14A—C14—H14B109.5C46B—C45B—C44B106.6 (14)
O2—C14—H14C109.5C46B—C45B—H45C110.4
H14A—C14—H14C109.5C44B—C45B—H45C110.4
H14B—C14—H14C109.5C46B—C45B—H45D110.4
C15—O3—Nd1145.19 (13)C44B—C45B—H45D110.4
O3—C15—C16119.99 (19)H45C—C45B—H45D108.6
O3—C15—C20122.68 (18)C43B—C44B—C45B96.6 (15)
C16—C15—C20117.33 (18)C43B—C44B—H44C112.4
C17—C16—C15121.6 (2)C45B—C44B—H44C112.4
C17—C16—H16119.2C43B—C44B—H44D112.4
C15—C16—H16119.2C45B—C44B—H44D112.4
C16—C17—C18121.1 (2)H44C—C44B—H44D110.0
C16—C17—H17119.5C47A—O8A—C50A99.7 (6)
C18—C17—H17119.5O8A—C47A—C48A104.3 (5)
C19—C18—C17118.6 (2)O8A—C47A—H47A110.9
C19—C18—H18120.7C48A—C47A—H47A110.9
C17—C18—H18120.7O8A—C47A—H47B110.9
C18—C19—C20122.0 (2)C48A—C47A—H47B110.9
C18—C19—H19119.0H47A—C47A—H47B108.9
C20—C19—H19119.0C49A—C48A—C47A98.4 (5)
C19—C20—C15119.30 (18)C49A—C48A—H48A112.1
C19—C20—C21116.30 (18)C47A—C48A—H48A112.1
C15—C20—C21124.40 (18)C49A—C48A—H48B112.1
N2—C21—C20128.47 (19)C47A—C48A—H48B112.1
N2—C21—H21115.8H48A—C48A—H48B109.7
C20—C21—H21115.8C50A—C49A—C48A103.5 (5)
C21—N2—C22116.29 (17)C50A—C49A—H49A111.1
C21—N2—Nd1126.67 (13)C48A—C49A—H49A111.1
C22—N2—Nd1116.80 (12)C50A—C49A—H49B111.1
C23—C22—C27118.03 (19)C48A—C49A—H49B111.1
C23—C22—N2124.43 (18)H49A—C49A—H49B109.0
C27—C22—N2117.43 (18)O8A—C50A—C49A109.0 (5)
C24—C23—C22121.0 (2)O8A—C50A—H50A109.9
C24—C23—H23119.5C49A—C50A—H50A109.9
C22—C23—H23119.5O8A—C50A—H50B109.9
C25—C24—C23119.8 (2)C49A—C50A—H50B109.9
C25—C24—H24120.1H50A—C50A—H50B108.3
C23—C24—H24120.1C47B—O8B—C50B112.2 (11)
C24—C25—C26120.7 (2)O8B—C47B—C48B103.6 (10)
C24—C25—H25119.7O8B—C47B—H47C111.0
C26—C25—H25119.7C48B—C47B—H47C111.0
C27—C26—C25119.1 (2)O8B—C47B—H47D111.0
C27—C26—H26120.5C48B—C47B—H47D111.0
C25—C26—H26120.5H47C—C47B—H47D109.0
O4—C27—C26123.12 (19)C50B—C49B—C48B108.0 (9)
O4—C27—C22115.40 (17)C50B—C49B—H49C110.1
C26—C27—C22121.49 (19)C48B—C49B—H49C110.1
C27—O4—C28117.21 (16)C50B—C49B—H49D110.1
C27—O4—Nd1121.61 (12)C48B—C49B—H49D110.1
C28—O4—Nd1117.50 (12)H49C—C49B—H49D108.4
O4—C28—H28A109.5C47B—C48B—C49B98.9 (10)
O4—C28—H28B109.5C47B—C48B—H48C112.0
H28A—C28—H28B109.5C49B—C48B—H48C112.0
O4—C28—H28C109.5C47B—C48B—H48D112.0
H28A—C28—H28C109.5C49B—C48B—H48D112.0
H28B—C28—H28C109.5H48C—C48B—H48D109.7
C29—O5—Nd1148.97 (14)O8B—C50B—C49B101.4 (9)
O5—C29—C30120.0 (2)O8B—C50B—H50C111.5
O5—C29—C34122.60 (19)C49B—C50B—H50C111.5
C30—C29—C34117.4 (2)O8B—C50B—H50D111.5
C31—C30—C29121.4 (2)C49B—C50B—H50D111.5
C31—C30—H30119.3H50C—C50B—H50D109.3
Nd1—O1—C1—C2133.63 (18)C23—C22—C27—O4177.93 (18)
Nd1—O1—C1—C646.4 (3)N2—C22—C27—O41.6 (3)
O1—C1—C2—C3176.5 (2)C23—C22—C27—C261.4 (3)
C6—C1—C2—C33.6 (3)N2—C22—C27—C26177.8 (2)
C1—C2—C3—C41.9 (4)C26—C27—O4—C283.9 (3)
C2—C3—C4—C50.9 (4)C22—C27—O4—C28176.77 (19)
C3—C4—C5—C61.9 (4)C26—C27—O4—Nd1153.98 (17)
C4—C5—C6—C10.1 (3)C22—C27—O4—Nd125.4 (2)
C4—C5—C6—C7178.7 (2)Nd1—O5—C29—C30176.72 (18)
O1—C1—C6—C5177.5 (2)Nd1—O5—C29—C343.6 (4)
C2—C1—C6—C52.6 (3)O5—C29—C30—C31179.4 (2)
O1—C1—C6—C74.0 (3)C34—C29—C30—C310.3 (3)
C2—C1—C6—C7176.0 (2)C29—C30—C31—C320.9 (4)
C5—C6—C7—N1166.2 (2)C30—C31—C32—C331.2 (4)
C1—C6—C7—N115.2 (3)C31—C32—C33—C340.4 (4)
C6—C7—N1—C8176.34 (19)C32—C33—C34—C290.8 (3)
C6—C7—N1—Nd115.5 (3)C32—C33—C34—C35176.9 (2)
C7—N1—C8—C13136.6 (2)O5—C29—C34—C33178.6 (2)
Nd1—N1—C8—C1332.8 (2)C30—C29—C34—C331.1 (3)
C7—N1—C8—C946.5 (3)O5—C29—C34—C353.8 (3)
Nd1—N1—C8—C9144.17 (17)C30—C29—C34—C35176.5 (2)
C13—C8—C9—C100.8 (3)C33—C34—C35—N3176.8 (2)
N1—C8—C9—C10176.06 (19)C29—C34—C35—N30.8 (4)
C8—C9—C10—C112.5 (3)C34—C35—N3—C36179.7 (2)
C9—C10—C11—C121.6 (4)C34—C35—N3—Nd15.6 (3)
C10—C11—C12—C131.0 (4)C35—N3—C36—C41143.2 (2)
C11—C12—C13—O2176.7 (2)Nd1—N3—C36—C4141.2 (2)
C11—C12—C13—C82.7 (4)C35—N3—C36—C3740.6 (3)
C9—C8—C13—C121.8 (3)Nd1—N3—C36—C37135.0 (2)
N1—C8—C13—C12178.9 (2)C41—C36—C37—C380.9 (4)
C9—C8—C13—O2177.62 (18)N3—C36—C37—C38177.1 (2)
N1—C8—C13—O20.5 (3)C36—C37—C38—C390.4 (4)
C12—C13—O2—C1429.9 (3)C37—C38—C39—C400.1 (4)
C8—C13—O2—C14150.7 (2)C38—C39—C40—C410.2 (4)
C12—C13—O2—Nd1146.27 (19)C39—C40—C41—O6178.6 (2)
C8—C13—O2—Nd133.1 (2)C39—C40—C41—C360.4 (4)
Nd1—O3—C15—C16168.17 (17)C37—C36—C41—O6178.1 (2)
Nd1—O3—C15—C2011.7 (4)N3—C36—C41—O61.7 (3)
O3—C15—C16—C17177.6 (2)C37—C36—C41—C400.9 (3)
C20—C15—C16—C172.5 (3)N3—C36—C41—C40177.3 (2)
C15—C16—C17—C180.0 (4)C40—C41—O6—C4210.2 (3)
C16—C17—C18—C191.2 (4)C36—C41—O6—C42170.8 (2)
C17—C18—C19—C200.3 (3)C40—C41—O6—Nd1138.6 (2)
C18—C19—C20—C152.9 (3)C36—C41—O6—Nd140.4 (2)
C18—C19—C20—C21177.3 (2)C46A—O7A—C43A—C44A20.4 (11)
O3—C15—C20—C19176.26 (19)C43A—O7A—C46A—C45A42.4 (11)
C16—C15—C20—C193.9 (3)O7A—C46A—C45A—C44A46.2 (10)
O3—C15—C20—C213.6 (3)O7A—C43A—C44A—C45A8.3 (12)
C16—C15—C20—C21176.3 (2)C46A—C45A—C44A—C43A31.7 (10)
C19—C20—C21—N2172.4 (2)C46B—O7B—C43B—C44B7 (3)
C15—C20—C21—N27.8 (3)C43B—O7B—C46B—C45B28 (3)
C20—C21—N2—C22174.1 (2)O7B—C46B—C45B—C44B41 (3)
C20—C21—N2—Nd111.7 (3)O7B—C43B—C44B—C45B17 (3)
C21—N2—C22—C2330.3 (3)C46B—C45B—C44B—C43B34 (2)
Nd1—N2—C22—C23155.00 (16)C50A—O8A—C47A—C48A48.0 (8)
C21—N2—C22—C27153.67 (19)O8A—C47A—C48A—C49A48.3 (8)
Nd1—N2—C22—C2721.1 (2)C47A—C48A—C49A—C50A28.1 (7)
C27—C22—C23—C241.6 (3)C47A—O8A—C50A—C49A28.7 (8)
N2—C22—C23—C24177.6 (2)C48A—C49A—C50A—O8A0.7 (8)
C22—C23—C24—C250.7 (3)C50B—O8B—C47B—C48B28.7 (18)
C23—C24—C25—C260.3 (4)O8B—C47B—C48B—C49B38.0 (15)
C24—C25—C26—C270.5 (4)C50B—C49B—C48B—C47B36.4 (14)
C25—C26—C27—O4178.9 (2)C47B—O8B—C50B—C49B5.4 (15)
C25—C26—C27—C220.4 (3)C48B—C49B—C50B—O8B20.3 (13)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C28—H28B···O50.982.613.174 (3)117
C35—H35···O8Aai0.952.543.413 (6)153
C40—H40···O7Aaii0.952.633.545 (7)161
Symmetry codes: (i) x+1, y, z; (ii) x+2, y+1, z+1.
Tris(2-{[(2-methoxyphenyl)imino]methyl}phenolato)-κ3O1,N,O2;κ3O1,N,O2;κ2N,O1-yttrium (mol3) top
Crystal data top
[Y(C14H12NO2)3]Z = 4
Mr = 767.65F(000) = 1584
Triclinic, P1Dx = 1.435 Mg m3
a = 12.1048 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 17.5475 (14) ÅCell parameters from 7148 reflections
c = 18.7959 (15) Åθ = 2.2–26.8°
α = 114.881 (1)°µ = 1.70 mm1
β = 91.885 (2)°T = 120 K
γ = 99.171 (1)°Block, colourless
V = 3553.2 (5) Å30.40 × 0.40 × 0.30 mm
Data collection top
Bruker APEXII CCD
diffractometer
17098 independent reflections
Radiation source: fine-focus sealed tube11818 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
φ and ω scansθmax = 28.0°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1515
Tmin = 0.532, Tmax = 0.648k = 2323
40107 measured reflectionsl = 2424
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)] = 0.060Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.150H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0619P)2 + 5.3422P]
where P = (Fo2 + 2Fc2)/3
17098 reflections(Δ/σ)max = 0.001
943 parametersΔρmax = 1.48 e Å3
0 restraintsΔρmin = 1.15 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Y10.14356 (3)0.28611 (2)0.31689 (2)0.01444 (9)
Y20.74275 (3)0.72438 (2)0.19637 (2)0.01629 (10)
O10.1323 (2)0.40353 (16)0.41977 (16)0.0180 (6)
C10.1714 (3)0.4855 (2)0.4588 (2)0.0158 (8)
C20.1348 (3)0.5330 (2)0.5324 (2)0.0176 (8)
H20.0824490.5044180.5539010.021*
C30.1733 (3)0.6205 (3)0.5741 (2)0.0204 (8)
H30.1457620.6511280.6228160.025*
C40.2524 (3)0.6637 (3)0.5448 (3)0.0222 (9)
H40.2791670.7235780.5735810.027*
C50.2911 (3)0.6189 (2)0.4740 (2)0.0189 (8)
H50.3454590.6484610.4545150.023*
C60.2522 (3)0.5301 (2)0.4295 (2)0.0171 (8)
C70.2962 (3)0.4901 (3)0.3550 (3)0.0218 (9)
H70.3522290.5257210.3425330.026*
N10.2682 (3)0.4112 (2)0.3031 (2)0.0200 (7)
C80.3248 (4)0.3898 (3)0.2320 (3)0.0271 (10)
C90.2630 (5)0.3703 (3)0.1609 (3)0.0372 (12)
H90.1852650.3729260.1592640.045*
C100.3166 (5)0.3463 (3)0.0908 (3)0.0450 (13)
H100.2753270.3326230.0417140.054*
C110.4297 (5)0.3432 (3)0.0949 (3)0.0451 (14)
H110.4658140.3269590.0480390.054*
C120.4915 (4)0.3631 (3)0.1651 (3)0.0402 (13)
H120.5694340.3608190.1665630.048*
C130.4386 (4)0.3869 (3)0.2347 (3)0.0326 (11)
O20.4909 (3)0.4100 (2)0.3065 (2)0.0421 (9)
C140.6065 (4)0.4030 (4)0.3124 (4)0.0558 (16)
H14A0.6313870.4143390.3666080.084*
H14B0.6522980.4447940.2981710.084*
H14C0.6150920.3451520.2763120.084*
O30.0312 (2)0.22911 (17)0.31670 (16)0.0178 (6)
C150.0964 (3)0.1601 (2)0.3129 (2)0.0161 (8)
C160.2129 (3)0.1434 (3)0.2874 (2)0.0210 (8)
H160.2423710.1813190.2710850.025*
C170.2841 (3)0.0727 (3)0.2859 (2)0.0231 (9)
H170.3619470.0630220.2688290.028*
C180.2437 (4)0.0153 (3)0.3089 (3)0.0253 (9)
H180.2938550.0321950.3090680.030*
C190.1302 (3)0.0285 (3)0.3314 (2)0.0229 (9)
H190.1022310.0107480.3466340.027*
C200.0545 (3)0.0993 (2)0.3324 (2)0.0182 (8)
C210.0631 (3)0.1049 (2)0.3512 (2)0.0195 (8)
H210.0825630.0625040.3655820.023*
N20.1458 (3)0.1616 (2)0.35059 (19)0.0168 (7)
C220.2575 (3)0.1516 (3)0.3661 (2)0.0189 (8)
C230.2913 (4)0.0729 (3)0.3401 (3)0.0237 (9)
H230.2375460.0215340.3127160.028*
C240.4042 (4)0.0691 (3)0.3541 (3)0.0259 (9)
H240.4267210.0152790.3369440.031*
C250.4823 (3)0.1435 (3)0.3929 (3)0.0253 (9)
H250.5588000.1406900.4021130.030*
C260.4508 (3)0.2229 (3)0.4188 (2)0.0232 (9)
H260.5052040.2740770.4452740.028*
C270.3387 (3)0.2262 (3)0.4055 (2)0.0182 (8)
O40.2984 (2)0.30172 (17)0.42623 (16)0.0200 (6)
C280.3771 (4)0.3798 (3)0.4735 (3)0.0342 (11)
H28A0.4118660.3752490.5190530.051*
H28B0.3372530.4279230.4919670.051*
H28C0.4355420.3892190.4417000.051*
O50.2866 (2)0.23512 (17)0.25958 (16)0.0185 (6)
C290.3171 (3)0.1823 (2)0.1944 (2)0.0164 (8)
C300.4276 (3)0.1641 (3)0.1938 (2)0.0221 (9)
H300.4775220.1904810.2412010.026*
C310.4630 (4)0.1090 (3)0.1259 (3)0.0263 (9)
H310.5373490.0981880.1269920.032*
C320.3919 (4)0.0687 (3)0.0553 (3)0.0275 (10)
H320.4169230.0298230.0088260.033*
C330.2845 (4)0.0857 (3)0.0537 (3)0.0242 (9)
H330.2361520.0586090.0055960.029*
C340.2455 (3)0.1426 (2)0.1222 (2)0.0184 (8)
C350.1335 (3)0.1586 (2)0.1150 (2)0.0183 (8)
H350.0948910.1337780.0632260.022*
N30.0800 (3)0.2035 (2)0.17178 (19)0.0169 (7)
C360.0318 (3)0.2097 (3)0.1518 (2)0.0185 (8)
C370.1091 (3)0.1431 (3)0.0955 (2)0.0237 (9)
H370.0879760.0894570.0665620.028*
C380.2182 (4)0.1538 (3)0.0807 (3)0.0265 (9)
H380.2711400.1073930.0423140.032*
C390.2485 (4)0.2312 (3)0.1215 (3)0.0268 (9)
H390.3220240.2387950.1103730.032*
C400.1721 (3)0.2995 (3)0.1798 (3)0.0227 (9)
H400.1937640.3530030.2086050.027*
C410.0647 (3)0.2879 (2)0.1947 (2)0.0183 (8)
O60.0166 (2)0.34911 (17)0.25182 (16)0.0199 (6)
C420.0019 (4)0.4359 (2)0.2818 (3)0.0222 (9)
H42A0.0023710.4526410.2382900.033*
H42B0.0658150.4731920.3206900.033*
H42C0.0679250.4415550.3069240.033*
O70.6765 (2)0.60508 (17)0.09330 (16)0.0209 (6)
C430.6828 (3)0.5248 (3)0.0546 (2)0.0187 (8)
C440.6269 (3)0.4744 (3)0.0217 (2)0.0219 (8)
H440.5857020.5001080.0464080.026*
C450.6301 (4)0.3886 (3)0.0615 (3)0.0260 (9)
H450.5887000.3559320.1121230.031*
C460.6936 (4)0.3490 (3)0.0285 (3)0.0271 (9)
H460.6968830.2901490.0567460.032*
C470.7506 (4)0.3965 (3)0.0450 (3)0.0247 (9)
H470.7934860.3695900.0674600.030*
C480.7481 (3)0.4843 (2)0.0890 (2)0.0192 (8)
C490.8085 (3)0.5279 (3)0.1663 (3)0.0217 (9)
H490.8470970.4942140.1830690.026*
N40.8174 (3)0.6067 (2)0.2161 (2)0.0180 (7)
C500.8838 (3)0.6296 (2)0.2907 (2)0.0202 (8)
C510.8323 (4)0.6430 (3)0.3581 (3)0.0243 (9)
H510.7526510.6363860.3553510.029*
C520.8943 (4)0.6661 (3)0.4297 (3)0.0294 (10)
H520.8579390.6754440.4759180.035*
C531.0108 (4)0.6753 (3)0.4326 (3)0.0311 (10)
H531.0543440.6911040.4813750.037*
C541.0643 (4)0.6617 (3)0.3657 (3)0.0277 (10)
H541.1440460.6687610.3688920.033*
C551.0019 (3)0.6379 (3)0.2939 (3)0.0242 (9)
O81.0453 (2)0.6199 (2)0.22317 (19)0.0312 (7)
C561.1646 (4)0.6269 (4)0.2240 (3)0.0412 (13)
H56A1.1847990.6098790.1700790.062*
H56B1.1892660.5893180.2452760.062*
H56C1.2016240.6862260.2571570.062*
O90.5817 (2)0.76673 (18)0.20159 (17)0.0220 (6)
C570.5248 (3)0.8147 (2)0.1849 (2)0.0168 (8)
C580.4155 (3)0.8239 (3)0.2098 (2)0.0204 (8)
H580.3852150.7956670.2401970.024*
C590.3532 (3)0.8733 (3)0.1904 (2)0.0213 (8)
H590.2802770.8776270.2070820.026*
C600.3952 (4)0.9166 (3)0.1470 (3)0.0323 (11)
H600.3518810.9502590.1336460.039*
C610.5004 (4)0.9096 (3)0.1241 (3)0.0355 (12)
H610.5298230.9395450.0948070.043*
C620.5670 (3)0.8599 (3)0.1422 (3)0.0231 (9)
C630.6811 (3)0.8648 (3)0.1216 (3)0.0239 (9)
H630.7022870.8982280.0938100.029*
N50.7579 (3)0.8281 (2)0.1372 (2)0.0180 (7)
C640.8691 (3)0.8540 (3)0.1212 (2)0.0187 (8)
C650.9137 (4)0.9377 (3)0.1381 (3)0.0261 (9)
H650.8685120.9802270.1576380.031*
C661.0254 (4)0.9602 (3)0.1266 (3)0.0292 (10)
H661.0565091.0180460.1385580.035*
C671.0901 (4)0.8982 (3)0.0977 (3)0.0306 (11)
H671.1657450.9136320.0893040.037*
C681.0467 (3)0.8133 (3)0.0806 (3)0.0273 (10)
H681.0918920.7709270.0604550.033*
C690.9352 (3)0.7914 (3)0.0936 (2)0.0214 (8)
O100.8830 (2)0.71108 (18)0.08161 (17)0.0241 (6)
C700.9498 (5)0.6448 (3)0.0580 (4)0.0472 (14)
H70A0.9814660.6393970.0091700.071*
H70B0.9021700.5902300.0491890.071*
H70C1.0111360.6597990.0997400.071*
O110.9150 (2)0.79074 (18)0.24660 (16)0.0206 (6)
C710.9830 (3)0.8307 (2)0.3115 (2)0.0176 (8)
C721.1013 (3)0.8479 (3)0.3072 (3)0.0236 (9)
H721.1287490.8318960.2571610.028*
C731.1761 (3)0.8874 (3)0.3748 (3)0.0252 (9)
H731.2543480.8983000.3703440.030*
C741.1398 (4)0.9118 (3)0.4496 (3)0.0268 (9)
H741.1922600.9382500.4958350.032*
C751.0249 (4)0.8963 (3)0.4545 (3)0.0248 (9)
H750.9990080.9126030.5050630.030*
C760.9460 (3)0.8575 (2)0.3873 (2)0.0190 (8)
C770.8282 (3)0.8452 (3)0.3989 (2)0.0193 (8)
H770.8105800.8673880.4518500.023*
N60.7437 (3)0.8067 (2)0.3435 (2)0.0197 (7)
C780.6333 (3)0.8032 (3)0.3678 (2)0.0191 (8)
C790.5962 (3)0.8735 (3)0.4232 (3)0.0226 (9)
H790.6469110.9266990.4499560.027*
C800.4841 (3)0.8657 (3)0.4393 (3)0.0252 (9)
H800.4578490.9139560.4760840.030*
C810.4120 (4)0.7881 (3)0.4017 (3)0.0253 (9)
H810.3365280.7827710.4140840.030*
C820.4473 (3)0.7173 (3)0.3458 (2)0.0201 (8)
H820.3964870.6640960.3197350.024*
C830.5580 (3)0.7257 (3)0.3289 (2)0.0179 (8)
O120.6029 (2)0.66165 (17)0.27255 (16)0.0185 (6)
C840.5308 (4)0.5799 (3)0.2310 (3)0.0292 (10)
H84A0.5093770.5557520.2681760.044*
H84B0.5705800.5414920.1905930.044*
H84C0.4630190.5864380.2058490.044*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.01150 (18)0.01440 (18)0.01759 (19)0.00363 (14)0.00396 (14)0.00649 (15)
Y20.01145 (18)0.01870 (19)0.0213 (2)0.00393 (14)0.00270 (14)0.01062 (16)
O10.0164 (13)0.0150 (13)0.0198 (14)0.0002 (11)0.0055 (11)0.0055 (11)
C10.0097 (17)0.0157 (18)0.022 (2)0.0034 (14)0.0005 (15)0.0080 (16)
C20.0122 (17)0.0199 (19)0.019 (2)0.0021 (15)0.0030 (15)0.0067 (16)
C30.0173 (19)0.023 (2)0.019 (2)0.0094 (16)0.0030 (16)0.0049 (17)
C40.0160 (19)0.0174 (19)0.028 (2)0.0016 (16)0.0008 (16)0.0055 (17)
C50.0135 (18)0.0173 (19)0.024 (2)0.0008 (15)0.0005 (15)0.0086 (17)
C60.0147 (18)0.0152 (18)0.023 (2)0.0051 (15)0.0033 (15)0.0089 (16)
C70.0139 (19)0.021 (2)0.035 (2)0.0040 (16)0.0093 (17)0.0156 (19)
N10.0188 (17)0.0172 (17)0.0254 (19)0.0059 (14)0.0107 (14)0.0089 (15)
C80.031 (2)0.0137 (19)0.039 (3)0.0044 (17)0.019 (2)0.0125 (19)
C90.060 (3)0.028 (2)0.025 (2)0.003 (2)0.007 (2)0.015 (2)
C100.065 (4)0.042 (3)0.034 (3)0.011 (3)0.020 (3)0.021 (2)
C110.063 (4)0.032 (3)0.045 (3)0.013 (3)0.025 (3)0.018 (3)
C120.034 (3)0.023 (2)0.062 (4)0.008 (2)0.024 (3)0.014 (2)
C130.034 (3)0.022 (2)0.039 (3)0.0013 (19)0.012 (2)0.011 (2)
O20.0224 (17)0.053 (2)0.051 (2)0.0119 (16)0.0088 (16)0.0217 (19)
C140.029 (3)0.071 (4)0.073 (4)0.019 (3)0.007 (3)0.032 (4)
O30.0134 (13)0.0180 (13)0.0231 (15)0.0042 (11)0.0045 (11)0.0093 (12)
C150.0146 (18)0.0169 (18)0.0165 (19)0.0045 (15)0.0053 (15)0.0061 (15)
C160.0157 (19)0.024 (2)0.025 (2)0.0045 (16)0.0060 (16)0.0108 (18)
C170.0149 (19)0.027 (2)0.025 (2)0.0028 (17)0.0056 (16)0.0093 (18)
C180.022 (2)0.023 (2)0.031 (2)0.0007 (17)0.0064 (18)0.0129 (19)
C190.023 (2)0.022 (2)0.024 (2)0.0034 (17)0.0036 (17)0.0110 (18)
C200.0179 (19)0.0181 (19)0.019 (2)0.0040 (15)0.0042 (15)0.0076 (16)
C210.022 (2)0.0153 (19)0.024 (2)0.0043 (16)0.0024 (16)0.0104 (17)
N20.0156 (16)0.0157 (16)0.0188 (17)0.0032 (13)0.0037 (13)0.0069 (14)
C220.0158 (19)0.022 (2)0.023 (2)0.0040 (16)0.0023 (16)0.0135 (17)
C230.022 (2)0.021 (2)0.028 (2)0.0034 (17)0.0006 (17)0.0120 (18)
C240.022 (2)0.026 (2)0.031 (2)0.0121 (18)0.0029 (18)0.0112 (19)
C250.016 (2)0.032 (2)0.026 (2)0.0099 (18)0.0008 (17)0.0097 (19)
C260.0154 (19)0.029 (2)0.023 (2)0.0060 (17)0.0007 (16)0.0074 (18)
C270.0146 (18)0.024 (2)0.0167 (19)0.0068 (16)0.0025 (15)0.0085 (17)
O40.0149 (13)0.0157 (13)0.0230 (15)0.0024 (11)0.0013 (11)0.0027 (12)
C280.025 (2)0.021 (2)0.046 (3)0.0008 (19)0.007 (2)0.006 (2)
O50.0136 (13)0.0207 (14)0.0207 (14)0.0056 (11)0.0046 (11)0.0075 (12)
C290.0170 (18)0.0139 (18)0.021 (2)0.0030 (15)0.0062 (15)0.0098 (16)
C300.018 (2)0.025 (2)0.023 (2)0.0059 (17)0.0050 (16)0.0083 (18)
C310.022 (2)0.028 (2)0.035 (3)0.0120 (18)0.0094 (19)0.017 (2)
C320.027 (2)0.030 (2)0.030 (2)0.0135 (19)0.0153 (19)0.012 (2)
C330.023 (2)0.026 (2)0.022 (2)0.0083 (18)0.0071 (17)0.0082 (18)
C340.0184 (19)0.0186 (19)0.022 (2)0.0069 (16)0.0079 (16)0.0104 (17)
C350.021 (2)0.0166 (19)0.017 (2)0.0043 (16)0.0031 (16)0.0065 (16)
N30.0135 (15)0.0182 (16)0.0202 (17)0.0052 (13)0.0026 (13)0.0086 (14)
C360.0170 (19)0.021 (2)0.020 (2)0.0076 (16)0.0043 (16)0.0087 (17)
C370.020 (2)0.025 (2)0.022 (2)0.0064 (17)0.0052 (17)0.0064 (18)
C380.018 (2)0.033 (2)0.025 (2)0.0056 (18)0.0019 (17)0.0091 (19)
C390.017 (2)0.030 (2)0.034 (3)0.0041 (18)0.0018 (18)0.015 (2)
C400.021 (2)0.023 (2)0.028 (2)0.0104 (17)0.0058 (17)0.0125 (18)
C410.0168 (19)0.0192 (19)0.020 (2)0.0023 (15)0.0023 (15)0.0100 (17)
O60.0160 (13)0.0154 (13)0.0252 (15)0.0031 (11)0.0015 (11)0.0062 (12)
C420.025 (2)0.0150 (19)0.026 (2)0.0074 (16)0.0021 (17)0.0070 (17)
O70.0197 (14)0.0195 (14)0.0220 (15)0.0061 (12)0.0032 (11)0.0070 (12)
C430.0112 (18)0.026 (2)0.022 (2)0.0039 (16)0.0043 (15)0.0128 (17)
C440.019 (2)0.025 (2)0.025 (2)0.0051 (17)0.0026 (16)0.0129 (18)
C450.021 (2)0.026 (2)0.026 (2)0.0033 (18)0.0025 (18)0.0072 (19)
C460.026 (2)0.021 (2)0.031 (2)0.0067 (18)0.0048 (19)0.0075 (19)
C470.025 (2)0.025 (2)0.028 (2)0.0087 (18)0.0050 (18)0.0129 (19)
C480.0149 (19)0.019 (2)0.023 (2)0.0041 (15)0.0041 (16)0.0078 (17)
C490.0161 (19)0.023 (2)0.034 (2)0.0068 (16)0.0019 (17)0.0184 (19)
N40.0116 (15)0.0209 (17)0.0240 (18)0.0027 (13)0.0004 (13)0.0125 (15)
C500.019 (2)0.0143 (19)0.028 (2)0.0028 (16)0.0024 (17)0.0103 (17)
C510.021 (2)0.028 (2)0.028 (2)0.0058 (18)0.0008 (17)0.0161 (19)
C520.035 (3)0.031 (2)0.026 (2)0.007 (2)0.0011 (19)0.016 (2)
C530.034 (3)0.028 (2)0.031 (2)0.005 (2)0.010 (2)0.014 (2)
C540.020 (2)0.024 (2)0.040 (3)0.0036 (17)0.0075 (19)0.015 (2)
C550.021 (2)0.023 (2)0.032 (2)0.0059 (17)0.0022 (18)0.0138 (19)
O80.0150 (15)0.0434 (19)0.0369 (18)0.0070 (14)0.0039 (13)0.0183 (16)
C560.017 (2)0.051 (3)0.060 (4)0.010 (2)0.009 (2)0.027 (3)
O90.0155 (13)0.0295 (16)0.0310 (16)0.0078 (12)0.0066 (12)0.0211 (14)
C570.0144 (18)0.0180 (19)0.0151 (19)0.0021 (15)0.0010 (15)0.0046 (16)
C580.0155 (19)0.023 (2)0.022 (2)0.0049 (16)0.0049 (16)0.0089 (17)
C590.0140 (19)0.022 (2)0.028 (2)0.0030 (16)0.0048 (16)0.0104 (18)
C600.017 (2)0.042 (3)0.055 (3)0.010 (2)0.003 (2)0.037 (3)
C610.020 (2)0.052 (3)0.061 (3)0.013 (2)0.011 (2)0.047 (3)
C620.0137 (19)0.030 (2)0.030 (2)0.0039 (17)0.0016 (17)0.0177 (19)
C630.0146 (19)0.034 (2)0.034 (2)0.0042 (17)0.0055 (17)0.025 (2)
N50.0102 (15)0.0249 (18)0.0224 (18)0.0036 (13)0.0034 (13)0.0133 (15)
C640.0144 (18)0.026 (2)0.018 (2)0.0021 (16)0.0035 (15)0.0122 (17)
C650.021 (2)0.033 (2)0.029 (2)0.0057 (18)0.0042 (18)0.018 (2)
C660.023 (2)0.032 (2)0.033 (3)0.0051 (19)0.0002 (19)0.019 (2)
C670.014 (2)0.051 (3)0.034 (3)0.001 (2)0.0046 (18)0.027 (2)
C680.015 (2)0.045 (3)0.029 (2)0.0093 (19)0.0100 (17)0.020 (2)
C690.0148 (19)0.029 (2)0.022 (2)0.0041 (17)0.0025 (16)0.0127 (18)
O100.0202 (15)0.0258 (15)0.0282 (16)0.0077 (12)0.0098 (12)0.0116 (13)
C700.040 (3)0.039 (3)0.073 (4)0.020 (2)0.031 (3)0.028 (3)
O110.0144 (13)0.0274 (15)0.0211 (15)0.0015 (12)0.0012 (11)0.0125 (13)
C710.0145 (18)0.0174 (19)0.024 (2)0.0020 (15)0.0016 (16)0.0126 (17)
C720.0131 (19)0.029 (2)0.032 (2)0.0036 (17)0.0060 (17)0.0161 (19)
C730.0146 (19)0.026 (2)0.035 (3)0.0001 (17)0.0014 (17)0.015 (2)
C740.020 (2)0.025 (2)0.032 (2)0.0011 (17)0.0042 (18)0.0118 (19)
C750.022 (2)0.024 (2)0.024 (2)0.0018 (17)0.0014 (17)0.0069 (18)
C760.0158 (19)0.0186 (19)0.027 (2)0.0048 (16)0.0013 (16)0.0131 (17)
C770.0185 (19)0.021 (2)0.019 (2)0.0045 (16)0.0050 (16)0.0084 (17)
N60.0128 (16)0.0239 (18)0.0259 (19)0.0042 (14)0.0031 (14)0.0139 (15)
C780.0136 (18)0.026 (2)0.020 (2)0.0017 (16)0.0020 (15)0.0130 (17)
C790.0155 (19)0.024 (2)0.027 (2)0.0019 (16)0.0045 (17)0.0107 (18)
C800.018 (2)0.033 (2)0.028 (2)0.0094 (18)0.0086 (17)0.014 (2)
C810.018 (2)0.037 (2)0.029 (2)0.0093 (18)0.0096 (17)0.021 (2)
C820.0127 (18)0.028 (2)0.027 (2)0.0041 (16)0.0034 (16)0.0193 (18)
C830.0164 (19)0.022 (2)0.019 (2)0.0043 (16)0.0022 (15)0.0123 (17)
O120.0132 (13)0.0187 (14)0.0251 (15)0.0029 (11)0.0040 (11)0.0108 (12)
C840.025 (2)0.023 (2)0.033 (3)0.0057 (18)0.0040 (19)0.009 (2)
Geometric parameters (Å, º) top
Y1—O12.181 (3)C39—H390.9500
Y1—O52.183 (3)C40—C411.385 (5)
Y1—O32.190 (3)C40—H400.9500
Y1—N32.512 (3)C41—O61.377 (5)
Y1—N22.522 (3)O6—C421.429 (4)
Y1—N12.572 (3)C42—H42A0.9800
Y1—O62.576 (3)C42—H42B0.9800
Y1—O42.630 (3)C42—H42C0.9800
Y2—O72.174 (3)O7—C431.303 (5)
Y2—O112.183 (3)C43—C441.404 (6)
Y2—O92.185 (3)C43—C481.441 (5)
Y2—N52.489 (3)C44—C451.378 (6)
Y2—N62.524 (3)C44—H440.9500
Y2—N42.538 (3)C45—C461.400 (6)
Y2—O122.650 (3)C45—H450.9500
Y2—O102.744 (3)C46—C471.366 (6)
O1—C11.305 (4)C46—H460.9500
C1—C21.412 (5)C47—C481.416 (6)
C1—C61.424 (5)C47—H470.9500
C2—C31.386 (5)C48—C491.431 (6)
C2—H20.9500C49—N41.287 (5)
C3—C41.396 (6)C49—H490.9500
C3—H30.9500N4—C501.456 (5)
C4—C51.373 (6)C50—C511.376 (6)
C4—H40.9500C50—C551.410 (6)
C5—C61.412 (5)C51—C521.385 (6)
C5—H50.9500C51—H510.9500
C6—C71.442 (6)C52—C531.391 (6)
C7—N11.294 (5)C52—H520.9500
C7—H70.9500C53—C541.381 (7)
N1—C81.454 (5)C53—H530.9500
C8—C131.386 (7)C54—C551.387 (6)
C8—C91.389 (7)C54—H540.9500
C9—C101.419 (7)C55—O81.375 (5)
C9—H90.9500O8—C561.429 (5)
C10—C111.380 (8)C56—H56A0.9800
C10—H100.9500C56—H56B0.9800
C11—C121.373 (8)C56—H56C0.9800
C11—H110.9500O9—C571.294 (5)
C12—C131.407 (7)C57—C621.404 (6)
C12—H120.9500C57—C581.428 (5)
C13—O21.336 (6)C58—C591.380 (6)
O2—C141.428 (6)C58—H580.9500
C14—H14A0.9800C59—C601.389 (6)
C14—H14B0.9800C59—H590.9500
C14—H14C0.9800C60—C611.365 (6)
O3—C151.308 (5)C60—H600.9500
C15—C161.418 (5)C61—C621.408 (6)
C15—C201.421 (5)C61—H610.9500
C16—C171.382 (6)C62—C631.446 (5)
C16—H160.9500C63—N51.302 (5)
C17—C181.398 (6)C63—H630.9500
C17—H170.9500N5—C641.434 (5)
C18—C191.378 (6)C64—C651.376 (6)
C18—H180.9500C64—C691.395 (6)
C19—C201.415 (5)C65—C661.397 (6)
C19—H190.9500C65—H650.9500
C20—C211.433 (5)C66—C671.377 (7)
C21—N21.298 (5)C66—H660.9500
C21—H210.9500C67—C681.390 (7)
N2—C221.426 (5)C67—H670.9500
C22—C231.393 (6)C68—C691.401 (5)
C22—C271.398 (6)C68—H680.9500
C23—C241.400 (6)C69—O101.370 (5)
C23—H230.9500O10—C701.448 (5)
C24—C251.375 (6)C70—H70A0.9800
C24—H240.9500C70—H70B0.9800
C25—C261.390 (6)C70—H70C0.9800
C25—H250.9500O11—C711.299 (5)
C26—C271.386 (5)C71—C761.414 (6)
C26—H260.9500C71—C721.427 (5)
C27—O41.390 (5)C72—C731.377 (6)
O4—C281.441 (5)C72—H720.9500
C28—H28A0.9800C73—C741.396 (6)
C28—H28B0.9800C73—H730.9500
C28—H28C0.9800C74—C751.388 (6)
O5—C291.296 (5)C74—H740.9500
C29—C341.420 (6)C75—C761.401 (6)
C29—C301.423 (5)C75—H750.9500
C30—C311.369 (6)C76—C771.445 (5)
C30—H300.9500C77—N61.305 (5)
C31—C321.394 (6)C77—H770.9500
C31—H310.9500N6—C781.426 (5)
C32—C331.381 (6)C78—C791.391 (6)
C32—H320.9500C78—C831.393 (6)
C33—C341.408 (6)C79—C801.399 (6)
C33—H330.9500C79—H790.9500
C34—C351.441 (5)C80—C811.374 (6)
C35—N31.296 (5)C80—H800.9500
C35—H350.9500C81—C821.389 (6)
N3—C361.425 (5)C81—H810.9500
C36—C371.381 (6)C82—C831.387 (5)
C36—C411.399 (5)C82—H820.9500
C37—C381.399 (6)C83—O121.382 (5)
C37—H370.9500O12—C841.429 (5)
C38—C391.367 (6)C84—H84A0.9800
C38—H380.9500C84—H84B0.9800
C39—C401.402 (6)C84—H84C0.9800
O1—Y1—O5132.28 (10)C36—N3—Y1112.5 (2)
O1—Y1—O391.87 (10)C37—C36—C41119.0 (4)
O5—Y1—O3133.97 (10)C37—C36—N3124.2 (4)
O1—Y1—N3142.63 (10)C41—C36—N3116.8 (3)
O5—Y1—N372.63 (10)C36—C37—C38120.7 (4)
O3—Y1—N378.08 (10)C36—C37—H37119.7
O1—Y1—N2112.53 (10)C38—C37—H37119.7
O5—Y1—N278.06 (10)C39—C38—C37119.8 (4)
O3—Y1—N272.06 (10)C39—C38—H38120.1
N3—Y1—N298.58 (10)C37—C38—H38120.1
O1—Y1—N172.25 (10)C38—C39—C40120.6 (4)
O5—Y1—N174.47 (10)C38—C39—H39119.7
O3—Y1—N1143.52 (10)C40—C39—H39119.7
N3—Y1—N194.68 (11)C41—C40—C39119.1 (4)
N2—Y1—N1144.22 (10)C41—C40—H40120.5
O1—Y1—O680.75 (9)C39—C40—H40120.5
O5—Y1—O6119.87 (10)O6—C41—C40124.6 (4)
O3—Y1—O672.68 (9)O6—C41—C36114.6 (3)
N3—Y1—O661.88 (9)C40—C41—C36120.8 (4)
N2—Y1—O6142.55 (9)C41—O6—C42117.3 (3)
N1—Y1—O672.46 (10)C41—O6—Y1113.3 (2)
O1—Y1—O474.22 (9)C42—O6—Y1127.0 (2)
O5—Y1—O471.48 (9)O6—C42—H42A109.5
O3—Y1—O4119.60 (9)O6—C42—H42B109.5
N3—Y1—O4141.75 (9)H42A—C42—H42B109.5
N2—Y1—O461.35 (9)O6—C42—H42C109.5
N1—Y1—O488.16 (10)H42A—C42—H42C109.5
O6—Y1—O4152.12 (8)H42B—C42—H42C109.5
O7—Y2—O11131.67 (10)C43—O7—Y2145.7 (2)
O7—Y2—O992.03 (11)O7—C43—C44121.8 (4)
O11—Y2—O9133.45 (11)O7—C43—C48120.7 (4)
O7—Y2—N5100.89 (11)C44—C43—C48117.5 (4)
O11—Y2—N582.55 (10)C45—C44—C43121.8 (4)
O9—Y2—N572.56 (10)C45—C44—H44119.1
O7—Y2—N6145.37 (11)C43—C44—H44119.1
O11—Y2—N671.84 (10)C44—C45—C46120.9 (4)
O9—Y2—N679.32 (11)C44—C45—H45119.5
N5—Y2—N6108.11 (11)C46—C45—H45119.5
O7—Y2—N472.84 (10)C47—C46—C45118.7 (4)
O11—Y2—N480.30 (10)C47—C46—H46120.6
O9—Y2—N4136.46 (10)C45—C46—H46120.6
N5—Y2—N4149.26 (10)C46—C47—C48122.5 (4)
N6—Y2—N490.47 (11)C46—C47—H47118.8
O7—Y2—O1285.26 (10)C48—C47—H47118.8
O11—Y2—O12122.28 (9)C47—C48—C49118.1 (4)
O9—Y2—O1267.92 (9)C47—C48—C43118.5 (4)
N5—Y2—O12140.20 (9)C49—C48—C43123.4 (4)
N6—Y2—O1260.35 (10)N4—C49—C48128.6 (4)
N4—Y2—O1270.26 (9)N4—C49—H49115.7
O7—Y2—O1072.40 (10)C48—C49—H49115.7
O11—Y2—O1068.08 (10)C49—N4—C50114.2 (3)
O9—Y2—O10124.85 (10)C49—N4—Y2127.9 (3)
N5—Y2—O1059.97 (10)C50—N4—Y2117.9 (2)
N6—Y2—O10139.24 (10)C51—C50—C55119.7 (4)
N4—Y2—O1089.89 (10)C51—C50—N4120.6 (4)
O12—Y2—O10153.88 (8)C55—C50—N4119.7 (4)
C1—O1—Y1146.0 (2)C50—C51—C52121.4 (4)
O1—C1—C2120.6 (3)C50—C51—H51119.3
O1—C1—C6121.7 (3)C52—C51—H51119.3
C2—C1—C6117.7 (3)C51—C52—C53118.6 (4)
C3—C2—C1121.6 (4)C51—C52—H52120.7
C3—C2—H2119.2C53—C52—H52120.7
C1—C2—H2119.2C54—C53—C52121.1 (4)
C2—C3—C4120.4 (4)C54—C53—H53119.5
C2—C3—H3119.8C52—C53—H53119.5
C4—C3—H3119.8C53—C54—C55120.1 (4)
C5—C4—C3119.4 (4)C53—C54—H54119.9
C5—C4—H4120.3C55—C54—H54119.9
C3—C4—H4120.3O8—C55—C54125.3 (4)
C4—C5—C6121.7 (4)O8—C55—C50115.5 (4)
C4—C5—H5119.1C54—C55—C50119.1 (4)
C6—C5—H5119.1C55—O8—C56117.1 (4)
C5—C6—C1119.3 (4)O8—C56—H56A109.5
C5—C6—C7117.0 (3)O8—C56—H56B109.5
C1—C6—C7123.7 (3)H56A—C56—H56B109.5
N1—C7—C6127.4 (4)O8—C56—H56C109.5
N1—C7—H7116.3H56A—C56—H56C109.5
C6—C7—H7116.3H56B—C56—H56C109.5
C7—N1—C8115.0 (3)C57—O9—Y2145.4 (2)
C7—N1—Y1128.0 (3)O9—C57—C62122.0 (3)
C8—N1—Y1116.6 (2)O9—C57—C58120.9 (3)
C13—C8—C9120.3 (4)C62—C57—C58117.1 (4)
C13—C8—N1120.4 (4)C59—C58—C57121.2 (4)
C9—C8—N1119.2 (4)C59—C58—H58119.4
C8—C9—C10119.7 (5)C57—C58—H58119.4
C8—C9—H9120.2C58—C59—C60121.1 (4)
C10—C9—H9120.2C58—C59—H59119.4
C11—C10—C9118.9 (5)C60—C59—H59119.4
C11—C10—H10120.5C61—C60—C59118.3 (4)
C9—C10—H10120.5C61—C60—H60120.8
C12—C11—C10121.7 (5)C59—C60—H60120.8
C12—C11—H11119.1C60—C61—C62122.6 (4)
C10—C11—H11119.1C60—C61—H61118.7
C11—C12—C13119.5 (5)C62—C61—H61118.7
C11—C12—H12120.3C57—C62—C61119.6 (4)
C13—C12—H12120.3C57—C62—C63122.9 (4)
O2—C13—C8115.4 (4)C61—C62—C63117.2 (4)
O2—C13—C12124.7 (5)N5—C63—C62126.9 (4)
C8—C13—C12119.9 (5)N5—C63—H63116.6
C13—O2—C14117.9 (4)C62—C63—H63116.6
O2—C14—H14A109.5C63—N5—C64115.4 (3)
O2—C14—H14B109.5C63—N5—Y2129.7 (3)
H14A—C14—H14B109.5C64—N5—Y2114.8 (2)
O2—C14—H14C109.5C65—C64—C69120.4 (4)
H14A—C14—H14C109.5C65—C64—N5122.5 (4)
H14B—C14—H14C109.5C69—C64—N5116.8 (4)
C15—O3—Y1143.7 (2)C64—C65—C66120.0 (4)
O3—C15—C16119.8 (3)C64—C65—H65120.0
O3—C15—C20122.4 (3)C66—C65—H65120.0
C16—C15—C20117.8 (3)C67—C66—C65119.7 (4)
C17—C16—C15120.8 (4)C67—C66—H66120.1
C17—C16—H16119.6C65—C66—H66120.1
C15—C16—H16119.6C66—C67—C68121.1 (4)
C16—C17—C18121.3 (4)C66—C67—H67119.4
C16—C17—H17119.4C68—C67—H67119.4
C18—C17—H17119.4C67—C68—C69118.9 (4)
C19—C18—C17119.0 (4)C67—C68—H68120.5
C19—C18—H18120.5C69—C68—H68120.5
C17—C18—H18120.5O10—C69—C64115.1 (3)
C18—C19—C20121.2 (4)O10—C69—C68125.1 (4)
C18—C19—H19119.4C64—C69—C68119.8 (4)
C20—C19—H19119.4C69—O10—C70117.5 (3)
C19—C20—C15119.7 (4)C69—O10—Y2109.2 (2)
C19—C20—C21117.6 (4)C70—O10—Y2119.1 (3)
C15—C20—C21122.7 (3)O10—C70—H70A109.5
N2—C21—C20126.9 (4)O10—C70—H70B109.5
N2—C21—H21116.5H70A—C70—H70B109.5
C20—C21—H21116.5O10—C70—H70C109.5
C21—N2—C22117.6 (3)H70A—C70—H70C109.5
C21—N2—Y1130.0 (3)H70B—C70—H70C109.5
C22—N2—Y1112.2 (2)C71—O11—Y2144.7 (2)
C23—C22—C27118.5 (4)O11—C71—C76123.1 (3)
C23—C22—N2124.1 (4)O11—C71—C72119.3 (4)
C27—C22—N2117.3 (3)C76—C71—C72117.6 (4)
C22—C23—C24120.4 (4)C73—C72—C71120.8 (4)
C22—C23—H23119.8C73—C72—H72119.6
C24—C23—H23119.8C71—C72—H72119.6
C25—C24—C23119.8 (4)C72—C73—C74121.7 (4)
C25—C24—H24120.1C72—C73—H73119.1
C23—C24—H24120.1C74—C73—H73119.1
C24—C25—C26120.9 (4)C75—C74—C73118.0 (4)
C24—C25—H25119.5C75—C74—H74121.0
C26—C25—H25119.5C73—C74—H74121.0
C27—C26—C25119.0 (4)C74—C75—C76122.1 (4)
C27—C26—H26120.5C74—C75—H75118.9
C25—C26—H26120.5C76—C75—H75118.9
C26—C27—O4123.9 (4)C75—C76—C71119.8 (4)
C26—C27—C22121.4 (4)C75—C76—C77117.8 (4)
O4—C27—C22114.6 (3)C71—C76—C77122.4 (4)
C27—O4—C28116.2 (3)N6—C77—C76126.3 (4)
C27—O4—Y1110.9 (2)N6—C77—H77116.9
C28—O4—Y1124.2 (2)C76—C77—H77116.9
O4—C28—H28A109.5C77—N6—C78117.2 (3)
O4—C28—H28B109.5C77—N6—Y2130.0 (3)
H28A—C28—H28B109.5C78—N6—Y2112.6 (2)
O4—C28—H28C109.5C79—C78—C83119.4 (4)
H28A—C28—H28C109.5C79—C78—N6123.7 (4)
H28B—C28—H28C109.5C83—C78—N6116.7 (4)
C29—O5—Y1144.4 (2)C78—C79—C80119.8 (4)
O5—C29—C34122.7 (3)C78—C79—H79120.1
O5—C29—C30119.5 (4)C80—C79—H79120.1
C34—C29—C30117.8 (3)C81—C80—C79119.7 (4)
C31—C30—C29121.1 (4)C81—C80—H80120.1
C31—C30—H30119.5C79—C80—H80120.1
C29—C30—H30119.5C80—C81—C82121.3 (4)
C30—C31—C32121.1 (4)C80—C81—H81119.4
C30—C31—H31119.5C82—C81—H81119.4
C32—C31—H31119.5C83—C82—C81118.8 (4)
C33—C32—C31119.3 (4)C83—C82—H82120.6
C33—C32—H32120.4C81—C82—H82120.6
C31—C32—H32120.4O12—C83—C82124.9 (4)
C32—C33—C34121.3 (4)O12—C83—C78114.3 (3)
C32—C33—H33119.4C82—C83—C78120.9 (4)
C34—C33—H33119.4C83—O12—C84117.3 (3)
C33—C34—C29119.4 (4)C83—O12—Y2110.9 (2)
C33—C34—C35117.7 (4)C84—O12—Y2120.1 (2)
C29—C34—C35122.8 (3)O12—C84—H84A109.5
N3—C35—C34126.7 (4)O12—C84—H84B109.5
N3—C35—H35116.6H84A—C84—H84B109.5
C34—C35—H35116.6O12—C84—H84C109.5
C35—N3—C36117.7 (3)H84A—C84—H84C109.5
C35—N3—Y1129.8 (3)H84B—C84—H84C109.5
Y1—O1—C1—C2174.5 (3)Y2—O7—C43—C44169.7 (3)
Y1—O1—C1—C65.2 (7)Y2—O7—C43—C4810.4 (7)
O1—C1—C2—C3178.6 (3)O7—C43—C44—C45177.5 (4)
C6—C1—C2—C31.7 (6)C48—C43—C44—C452.4 (6)
C1—C2—C3—C41.6 (6)C43—C44—C45—C462.6 (6)
C2—C3—C4—C50.5 (6)C44—C45—C46—C471.4 (7)
C3—C4—C5—C60.6 (6)C45—C46—C47—C480.1 (7)
C4—C5—C6—C10.5 (6)C46—C47—C48—C49178.5 (4)
C4—C5—C6—C7178.3 (4)C46—C47—C48—C430.0 (6)
O1—C1—C6—C5179.7 (3)O7—C43—C48—C47178.9 (4)
C2—C1—C6—C50.6 (5)C44—C43—C48—C471.0 (5)
O1—C1—C6—C71.0 (6)O7—C43—C48—C490.4 (6)
C2—C1—C6—C7179.3 (4)C44—C43—C48—C49179.5 (4)
C5—C6—C7—N1176.1 (4)C47—C48—C49—N4179.8 (4)
C1—C6—C7—N12.6 (7)C43—C48—C49—N41.4 (7)
C6—C7—N1—C8178.2 (4)C48—C49—N4—C50178.6 (4)
C6—C7—N1—Y19.3 (6)C48—C49—N4—Y24.7 (6)
C7—N1—C8—C1370.2 (5)C49—N4—C50—C51106.5 (4)
Y1—N1—C8—C13103.2 (4)Y2—N4—C50—C5176.5 (4)
C7—N1—C8—C9111.4 (5)C49—N4—C50—C5573.5 (5)
Y1—N1—C8—C975.2 (4)Y2—N4—C50—C55103.6 (4)
C13—C8—C9—C100.6 (7)C55—C50—C51—C521.1 (6)
N1—C8—C9—C10177.7 (4)N4—C50—C51—C52179.0 (4)
C8—C9—C10—C110.2 (7)C50—C51—C52—C530.2 (7)
C9—C10—C11—C120.3 (8)C51—C52—C53—C540.1 (7)
C10—C11—C12—C130.3 (8)C52—C53—C54—C550.5 (7)
C9—C8—C13—O2177.5 (4)C53—C54—C55—O8177.7 (4)
N1—C8—C13—O24.1 (6)C53—C54—C55—C501.4 (6)
C9—C8—C13—C120.6 (7)C51—C50—C55—O8177.5 (4)
N1—C8—C13—C12177.7 (4)N4—C50—C55—O82.4 (5)
C11—C12—C13—O2177.9 (5)C51—C50—C55—C541.6 (6)
C11—C12—C13—C80.1 (7)N4—C50—C55—C54178.4 (4)
C8—C13—O2—C14176.1 (4)C54—C55—O8—C560.3 (6)
C12—C13—O2—C145.8 (7)C50—C55—O8—C56179.4 (4)
Y1—O3—C15—C16157.4 (3)Y2—O9—C57—C625.5 (7)
Y1—O3—C15—C2021.5 (6)Y2—O9—C57—C58174.3 (3)
O3—C15—C16—C17177.4 (4)O9—C57—C58—C59178.3 (4)
C20—C15—C16—C173.6 (6)C62—C57—C58—C591.9 (6)
C15—C16—C17—C180.4 (6)C57—C58—C59—C600.9 (6)
C16—C17—C18—C191.8 (6)C58—C59—C60—C610.3 (7)
C17—C18—C19—C200.7 (6)C59—C60—C61—C620.5 (8)
C18—C19—C20—C152.6 (6)O9—C57—C62—C61178.6 (4)
C18—C19—C20—C21175.7 (4)C58—C57—C62—C611.7 (6)
O3—C15—C20—C19176.4 (4)O9—C57—C62—C637.4 (6)
C16—C15—C20—C194.6 (6)C58—C57—C62—C63172.3 (4)
O3—C15—C20—C215.4 (6)C60—C61—C62—C570.5 (8)
C16—C15—C20—C21173.5 (4)C60—C61—C62—C63173.8 (5)
C19—C20—C21—N2175.7 (4)C57—C62—C63—N51.6 (7)
C15—C20—C21—N22.6 (7)C61—C62—C63—N5175.8 (5)
C20—C21—N2—C22175.7 (4)C62—C63—N5—C64170.6 (4)
C20—C21—N2—Y10.3 (6)C62—C63—N5—Y26.3 (7)
C21—N2—C22—C2337.1 (6)C63—N5—C64—C6540.6 (6)
Y1—N2—C22—C23139.1 (3)Y2—N5—C64—C65136.7 (3)
C21—N2—C22—C27147.1 (4)C63—N5—C64—C69144.8 (4)
Y1—N2—C22—C2736.7 (4)Y2—N5—C64—C6937.9 (4)
C27—C22—C23—C240.7 (6)C69—C64—C65—C660.9 (6)
N2—C22—C23—C24176.4 (4)N5—C64—C65—C66175.3 (4)
C22—C23—C24—C250.8 (7)C64—C65—C66—C670.5 (7)
C23—C24—C25—C260.3 (7)C65—C66—C67—C680.8 (7)
C24—C25—C26—C270.4 (6)C66—C67—C68—C690.3 (7)
C25—C26—C27—O4177.7 (4)C65—C64—C69—O10177.6 (4)
C25—C26—C27—C220.6 (6)N5—C64—C69—O102.9 (5)
C23—C22—C27—C260.0 (6)C65—C64—C69—C682.0 (6)
N2—C22—C27—C26176.0 (4)N5—C64—C69—C68176.7 (4)
C23—C22—C27—O4177.4 (3)C67—C68—C69—O10177.9 (4)
N2—C22—C27—O41.3 (5)C67—C68—C69—C641.7 (6)
C26—C27—O4—C288.5 (6)C64—C69—O10—C70176.0 (4)
C22—C27—O4—C28174.3 (4)C68—C69—O10—C703.7 (6)
C26—C27—O4—Y1140.7 (3)C64—C69—O10—Y236.4 (4)
C22—C27—O4—Y136.6 (4)C68—C69—O10—Y2143.2 (4)
Y1—O5—C29—C3411.6 (6)Y2—O11—C71—C7612.0 (7)
Y1—O5—C29—C30169.8 (3)Y2—O11—C71—C72167.1 (3)
O5—C29—C30—C31179.6 (4)O11—C71—C72—C73177.7 (4)
C34—C29—C30—C310.9 (6)C76—C71—C72—C731.5 (6)
C29—C30—C31—C320.4 (6)C71—C72—C73—C740.2 (6)
C30—C31—C32—C331.1 (7)C72—C73—C74—C751.0 (6)
C31—C32—C33—C340.5 (7)C73—C74—C75—C760.0 (6)
C32—C33—C34—C290.8 (6)C74—C75—C76—C711.7 (6)
C32—C33—C34—C35178.4 (4)C74—C75—C76—C77179.2 (4)
O5—C29—C34—C33179.9 (4)O11—C71—C76—C75176.7 (4)
C30—C29—C34—C331.5 (5)C72—C71—C76—C752.4 (6)
O5—C29—C34—C351.0 (6)O11—C71—C76—C772.3 (6)
C30—C29—C34—C35177.7 (4)C72—C71—C76—C77178.6 (4)
C33—C34—C35—N3174.5 (4)C75—C76—C77—N6176.4 (4)
C29—C34—C35—N36.3 (6)C71—C76—C77—N62.6 (6)
C34—C35—N3—C36178.6 (4)C76—C77—N6—C78178.7 (4)
C34—C35—N3—Y12.2 (6)C76—C77—N6—Y26.9 (6)
C35—N3—C36—C3738.4 (6)C77—N6—C78—C7947.4 (5)
Y1—N3—C36—C37142.3 (3)Y2—N6—C78—C79137.3 (3)
C35—N3—C36—C41143.9 (4)C77—N6—C78—C83137.3 (4)
Y1—N3—C36—C4135.4 (4)Y2—N6—C78—C8338.1 (4)
C41—C36—C37—C380.8 (6)C83—C78—C79—C800.1 (6)
N3—C36—C37—C38178.5 (4)N6—C78—C79—C80175.4 (4)
C36—C37—C38—C390.8 (7)C78—C79—C80—C811.5 (6)
C37—C38—C39—C401.7 (7)C79—C80—C81—C822.0 (6)
C38—C39—C40—C410.9 (6)C80—C81—C82—C830.7 (6)
C39—C40—C41—O6178.0 (4)C81—C82—C83—O12177.2 (4)
C39—C40—C41—C360.8 (6)C81—C82—C83—C780.9 (6)
C37—C36—C41—O6177.3 (3)C79—C78—C83—O12177.0 (3)
N3—C36—C41—O60.5 (5)N6—C78—C83—O121.4 (5)
C37—C36—C41—C401.7 (6)C79—C78—C83—C821.4 (6)
N3—C36—C41—C40179.5 (4)N6—C78—C83—C82176.9 (3)
C40—C41—O6—C4218.6 (5)C82—C83—O12—C842.6 (5)
C36—C41—O6—C42162.5 (3)C78—C83—O12—C84179.1 (3)
C40—C41—O6—Y1145.1 (3)C82—C83—O12—Y2140.7 (3)
C36—C41—O6—Y133.8 (4)C78—C83—O12—Y237.6 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C51—H51···O120.952.563.293 (5)134
Dichlorido-1κCl,2κCl-µ-methanolato-1:2κ2O:O-methanol-2κO-(µ-2-{[(2-methoxyphenyl)imino]methyl}phenolato-1κ3O1,N,O2:2κO1)bis(2-{[(2-methoxyphenyl)imino]methyl}phenolato)-1κ3O1,N,O2;2κ3O1,N,O2-diyttrium–tetrahydrofuran–methanol (1/1/1) (mol4) top
Crystal data top
[Y2(C14H12NO2)3(CH3O)Cl2(CH4O)]·CH4O·C4H8OF(000) = 2248
Mr = 1094.68Dx = 1.508 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 18.7839 (14) ÅCell parameters from 7434 reflections
b = 13.3371 (9) Åθ = 2.3–28.7°
c = 20.1422 (14) ŵ = 2.57 mm1
β = 107.107 (1)°T = 120 K
V = 4822.8 (6) Å3Block, colourless
Z = 40.55 × 0.40 × 0.25 mm
Data collection top
Bruker APEXII CCD
diffractometer
12827 independent reflections
Radiation source: fine-focus sealed tube8266 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
φ and ω scansθmax = 29.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 2525
Tmin = 0.372, Tmax = 0.492k = 1518
38433 measured reflectionsl = 2627
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)] = 0.044Hydrogen site location: mixed
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.0466P)2 + 2.0823P]
where P = (Fo2 + 2Fc2)/3
12827 reflections(Δ/σ)max = 0.001
609 parametersΔρmax = 1.05 e Å3
2 restraintsΔρmin = 0.71 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Y10.24912 (2)0.36119 (2)0.28482 (2)0.01915 (7)
Y20.29368 (2)0.58727 (2)0.40017 (2)0.02207 (8)
Cl10.16029 (5)0.31038 (6)0.36376 (4)0.03071 (19)
Cl20.38788 (5)0.60457 (7)0.52604 (4)0.0385 (2)
O10.29783 (12)0.21377 (15)0.31892 (11)0.0269 (5)
C10.32770 (17)0.1380 (2)0.29595 (17)0.0236 (7)
C20.38227 (18)0.0778 (2)0.34256 (19)0.0301 (8)
H20.3959960.0925480.3908230.036*
C30.41569 (19)0.0009 (2)0.3199 (2)0.0335 (8)
H30.4524660.0392860.3524930.040*
C40.39630 (18)0.0254 (2)0.2495 (2)0.0346 (8)
H40.4198740.0798750.2340600.041*
C50.34290 (18)0.0300 (2)0.2029 (2)0.0317 (8)
H50.3288580.0121070.1551580.038*
C60.30794 (17)0.1136 (2)0.22440 (18)0.0244 (7)
C70.25204 (17)0.1659 (2)0.17209 (18)0.0249 (7)
H70.2367980.1359470.1273260.030*
N10.21984 (14)0.24977 (18)0.17911 (14)0.0230 (6)
C80.16338 (16)0.2861 (2)0.11964 (16)0.0214 (6)
C90.15918 (18)0.2667 (2)0.05061 (17)0.0261 (7)
H90.1968700.2275070.0404230.031*
C100.10143 (18)0.3034 (2)0.00315 (17)0.0282 (7)
H100.0992730.2883840.0498050.034*
C110.04655 (18)0.3621 (2)0.01038 (17)0.0269 (7)
H110.0063480.3862130.0268190.032*
C120.05046 (18)0.3857 (2)0.07895 (17)0.0246 (7)
H120.0133980.4267570.0886480.029*
C130.10910 (17)0.3486 (2)0.13287 (16)0.0211 (6)
O20.11738 (11)0.36936 (15)0.20192 (10)0.0215 (4)
C140.05075 (17)0.4077 (2)0.21591 (17)0.0271 (7)
H14A0.0084230.3640520.1939520.041*
H14B0.0404380.4757030.1970170.041*
H14C0.0584810.4093520.2661830.041*
O30.21705 (11)0.52783 (15)0.29702 (10)0.0207 (4)
C150.16940 (16)0.5860 (2)0.25037 (15)0.0194 (6)
C160.11512 (17)0.6428 (2)0.26958 (17)0.0243 (7)
H160.1118880.6382690.3156730.029*
C170.06691 (18)0.7044 (2)0.22255 (17)0.0284 (7)
H170.0301320.7407260.2363910.034*
C180.07104 (19)0.7147 (2)0.15485 (18)0.0306 (8)
H180.0380830.7581100.1227050.037*
C190.12431 (18)0.6599 (2)0.13580 (17)0.0257 (7)
H190.1281710.6673150.0900780.031*
C200.17289 (16)0.5938 (2)0.18159 (15)0.0203 (6)
C210.22681 (16)0.5407 (2)0.15545 (15)0.0205 (6)
H210.2351700.5660340.1142910.025*
N20.26446 (13)0.46215 (18)0.18321 (13)0.0189 (5)
C220.31409 (16)0.4201 (2)0.14899 (16)0.0198 (6)
C230.30469 (18)0.4246 (2)0.07772 (16)0.0246 (7)
H230.2634380.4598300.0482590.030*
C240.35532 (19)0.3780 (2)0.04960 (18)0.0309 (8)
H240.3485400.3814330.0010250.037*
C250.41534 (19)0.3267 (3)0.09186 (18)0.0306 (8)
H250.4501130.2959480.0722460.037*
C260.42551 (18)0.3195 (2)0.16283 (18)0.0272 (7)
H260.4668120.2838060.1918070.033*
C270.37429 (16)0.3653 (2)0.19090 (16)0.0201 (6)
O40.37659 (11)0.36031 (15)0.26008 (10)0.0223 (4)
C280.44119 (17)0.3117 (2)0.30637 (17)0.0276 (7)
H28A0.4862840.3481290.3056950.041*
H28B0.4441400.2424980.2910510.041*
H28C0.4368640.3116060.3536810.041*
O50.22372 (12)0.70331 (16)0.42424 (11)0.0269 (5)
C290.20534 (16)0.7977 (2)0.41477 (15)0.0212 (6)
C300.16275 (18)0.8432 (2)0.45390 (17)0.0265 (7)
H300.1457780.8035260.4853570.032*
C310.14533 (17)0.9436 (2)0.44749 (17)0.0275 (7)
H310.1175970.9721420.4753430.033*
C320.16773 (18)1.0047 (2)0.40066 (18)0.0301 (8)
H320.1557181.0740210.3965650.036*
C330.20769 (18)0.9614 (2)0.36068 (17)0.0276 (7)
H330.2226411.0017710.3283000.033*
C340.22697 (16)0.8591 (2)0.36642 (15)0.0214 (6)
C350.26903 (17)0.8219 (2)0.32209 (16)0.0227 (7)
H350.2778290.8673510.2890550.027*
N30.29592 (14)0.73221 (18)0.32314 (13)0.0204 (5)
C360.33461 (17)0.7099 (2)0.27311 (16)0.0204 (6)
C370.31553 (18)0.7458 (2)0.20559 (16)0.0249 (7)
H370.2750590.7911570.1899570.030*
C380.35503 (18)0.7160 (2)0.16065 (17)0.0279 (7)
H380.3418070.7413320.1145530.033*
C390.41351 (18)0.6495 (2)0.18285 (17)0.0282 (7)
H390.4403880.6293470.1518520.034*
C400.43359 (17)0.6116 (2)0.25057 (17)0.0260 (7)
H400.4737230.5656330.2658370.031*
C410.39373 (17)0.6425 (2)0.29505 (16)0.0219 (6)
O60.40774 (12)0.61011 (15)0.36332 (11)0.0247 (5)
C420.47651 (18)0.5559 (3)0.39380 (18)0.0323 (8)
H42A0.5186710.5959060.3894510.048*
H42B0.4751170.4919070.3695330.048*
H42C0.4822350.5432220.4430240.048*
O70.32359 (12)0.42480 (15)0.38506 (10)0.0228 (5)
C430.3572 (2)0.3639 (3)0.44425 (18)0.0344 (8)
H43A0.3433150.2936680.4333160.052*
H43B0.3398140.3855930.4833250.052*
H43C0.4114670.3706770.4567610.052*
O80.21441 (17)0.49705 (19)0.44969 (14)0.0439 (7)
H80.199 (2)0.444 (2)0.4288 (19)0.049 (13)*
C440.1822 (2)0.5200 (3)0.50265 (18)0.0358 (8)
H44A0.1410790.4734490.5002380.054*
H44B0.1631020.5888100.4966660.054*
H44C0.2198070.5135840.5479560.054*
O90.47737 (18)0.8072 (3)0.52862 (17)0.0618 (9)
H9A0.452 (3)0.750 (3)0.526 (4)0.13 (3)*
C450.4213 (3)0.8751 (3)0.4938 (2)0.0580 (12)
H45A0.4043900.8585530.4441910.087*
H45B0.4412640.9434550.4998250.087*
H45C0.3792280.8704400.5131010.087*
O100.03375 (16)0.1626 (2)0.17104 (14)0.0472 (7)
C460.0800 (2)0.0928 (3)0.2186 (2)0.0414 (9)
H46A0.0560140.0726150.2542050.050*
H46B0.1287720.1237530.2423350.050*
C470.0906 (2)0.0023 (3)0.1769 (2)0.0522 (11)
H47A0.0942160.0602730.2041410.063*
H47B0.1355790.0093580.1612790.063*
C480.0199 (2)0.0044 (3)0.1159 (2)0.0522 (11)
H48A0.0274370.0287810.0744850.063*
H48B0.0221920.0280470.1277310.063*
C490.0072 (3)0.1159 (3)0.1043 (2)0.0494 (11)
H49A0.0347290.1415260.0728460.059*
H49B0.0464940.1301430.0833510.059*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.02540 (15)0.01246 (14)0.02236 (15)0.00068 (12)0.01133 (12)0.00029 (12)
Y20.03340 (17)0.01530 (14)0.01998 (15)0.00204 (12)0.01169 (13)0.00054 (13)
Cl10.0421 (5)0.0234 (4)0.0347 (4)0.0029 (3)0.0238 (4)0.0027 (4)
Cl20.0556 (6)0.0347 (5)0.0206 (4)0.0145 (4)0.0042 (4)0.0029 (4)
O10.0356 (13)0.0157 (11)0.0328 (13)0.0009 (9)0.0152 (10)0.0010 (10)
C10.0236 (15)0.0124 (14)0.0370 (18)0.0010 (12)0.0127 (14)0.0018 (14)
C20.0274 (17)0.0206 (17)0.044 (2)0.0005 (13)0.0131 (15)0.0062 (16)
C30.0287 (18)0.0199 (17)0.053 (2)0.0020 (14)0.0140 (17)0.0069 (17)
C40.0268 (18)0.0178 (16)0.063 (3)0.0013 (13)0.0185 (17)0.0043 (17)
C50.0272 (17)0.0217 (17)0.048 (2)0.0016 (14)0.0145 (16)0.0112 (16)
C60.0211 (15)0.0138 (14)0.041 (2)0.0020 (12)0.0126 (14)0.0030 (14)
C70.0237 (16)0.0185 (16)0.0365 (19)0.0062 (12)0.0153 (14)0.0082 (14)
N10.0249 (14)0.0170 (13)0.0307 (15)0.0051 (10)0.0140 (12)0.0043 (12)
C80.0226 (15)0.0167 (15)0.0278 (17)0.0053 (12)0.0122 (13)0.0036 (13)
C90.0294 (17)0.0197 (16)0.0333 (19)0.0068 (13)0.0154 (15)0.0074 (14)
C100.0368 (19)0.0243 (17)0.0279 (18)0.0108 (14)0.0161 (15)0.0087 (15)
C110.0324 (17)0.0206 (16)0.0274 (17)0.0064 (14)0.0085 (14)0.0018 (15)
C120.0267 (16)0.0180 (15)0.0311 (18)0.0037 (12)0.0116 (14)0.0025 (13)
C130.0265 (16)0.0151 (15)0.0243 (16)0.0060 (12)0.0115 (13)0.0030 (13)
O20.0230 (10)0.0202 (11)0.0242 (11)0.0003 (9)0.0116 (9)0.0047 (9)
C140.0277 (17)0.0267 (17)0.0312 (18)0.0012 (14)0.0156 (14)0.0064 (15)
O30.0272 (11)0.0146 (10)0.0226 (11)0.0012 (9)0.0110 (9)0.0007 (9)
C150.0242 (15)0.0122 (14)0.0219 (15)0.0043 (12)0.0072 (12)0.0008 (13)
C160.0286 (16)0.0191 (15)0.0275 (17)0.0009 (13)0.0119 (14)0.0052 (14)
C170.0284 (17)0.0217 (17)0.0355 (19)0.0052 (13)0.0100 (15)0.0059 (15)
C180.0341 (19)0.0230 (17)0.0314 (19)0.0074 (14)0.0046 (15)0.0018 (15)
C190.0334 (18)0.0215 (17)0.0224 (16)0.0017 (13)0.0082 (14)0.0008 (13)
C200.0241 (15)0.0125 (14)0.0232 (16)0.0022 (12)0.0050 (12)0.0007 (13)
C210.0233 (15)0.0192 (15)0.0198 (15)0.0050 (12)0.0078 (12)0.0021 (13)
N20.0216 (13)0.0141 (12)0.0230 (13)0.0028 (10)0.0096 (11)0.0038 (11)
C220.0254 (15)0.0127 (14)0.0244 (16)0.0048 (12)0.0122 (13)0.0026 (13)
C230.0286 (17)0.0199 (16)0.0277 (17)0.0045 (13)0.0120 (14)0.0010 (14)
C240.040 (2)0.0269 (18)0.0328 (19)0.0077 (15)0.0215 (16)0.0089 (15)
C250.0341 (19)0.0249 (17)0.041 (2)0.0047 (14)0.0235 (16)0.0096 (16)
C260.0274 (17)0.0184 (16)0.040 (2)0.0002 (13)0.0165 (15)0.0038 (15)
C270.0240 (15)0.0137 (14)0.0244 (16)0.0036 (12)0.0097 (12)0.0026 (13)
O40.0228 (11)0.0228 (11)0.0223 (11)0.0037 (9)0.0082 (9)0.0020 (10)
C280.0240 (16)0.0247 (17)0.0327 (18)0.0021 (13)0.0064 (14)0.0018 (15)
O50.0398 (13)0.0197 (11)0.0261 (12)0.0025 (10)0.0172 (10)0.0017 (10)
C290.0226 (15)0.0183 (15)0.0212 (16)0.0013 (12)0.0041 (12)0.0053 (13)
C300.0314 (17)0.0247 (17)0.0258 (17)0.0006 (13)0.0124 (14)0.0024 (14)
C310.0238 (16)0.0290 (18)0.0289 (18)0.0073 (13)0.0067 (14)0.0054 (15)
C320.0307 (18)0.0185 (16)0.040 (2)0.0049 (13)0.0084 (15)0.0039 (15)
C330.0339 (18)0.0188 (16)0.0312 (18)0.0014 (14)0.0114 (15)0.0024 (14)
C340.0228 (15)0.0195 (15)0.0225 (16)0.0015 (12)0.0078 (12)0.0027 (13)
C350.0251 (16)0.0180 (15)0.0268 (17)0.0031 (12)0.0104 (13)0.0009 (14)
N30.0232 (13)0.0184 (13)0.0205 (13)0.0028 (10)0.0080 (10)0.0048 (11)
C360.0252 (15)0.0157 (14)0.0221 (16)0.0066 (12)0.0098 (13)0.0055 (13)
C370.0307 (17)0.0176 (15)0.0282 (17)0.0069 (13)0.0114 (14)0.0033 (14)
C380.0370 (19)0.0236 (17)0.0254 (17)0.0109 (14)0.0128 (15)0.0018 (14)
C390.0306 (17)0.0278 (18)0.0325 (18)0.0121 (14)0.0192 (15)0.0091 (15)
C400.0239 (16)0.0223 (16)0.0328 (18)0.0044 (13)0.0098 (14)0.0073 (14)
C410.0257 (15)0.0169 (15)0.0225 (16)0.0069 (12)0.0065 (13)0.0048 (13)
O60.0285 (12)0.0214 (11)0.0240 (12)0.0046 (9)0.0071 (9)0.0021 (9)
C420.0283 (18)0.0301 (18)0.036 (2)0.0040 (14)0.0055 (15)0.0002 (16)
O70.0328 (12)0.0154 (10)0.0207 (11)0.0041 (9)0.0088 (9)0.0020 (9)
C430.050 (2)0.0214 (17)0.0306 (19)0.0087 (16)0.0103 (16)0.0020 (16)
O80.075 (2)0.0228 (13)0.0525 (17)0.0067 (13)0.0480 (16)0.0088 (13)
C440.046 (2)0.034 (2)0.0326 (19)0.0026 (17)0.0191 (17)0.0048 (17)
O90.0533 (19)0.060 (2)0.064 (2)0.0018 (17)0.0045 (16)0.0087 (18)
C450.067 (3)0.056 (3)0.051 (3)0.004 (2)0.017 (2)0.011 (2)
O100.0673 (19)0.0362 (15)0.0403 (16)0.0060 (13)0.0194 (14)0.0027 (13)
C460.044 (2)0.035 (2)0.048 (2)0.0048 (17)0.0175 (19)0.0048 (19)
C470.053 (3)0.041 (2)0.066 (3)0.009 (2)0.022 (2)0.007 (2)
C480.064 (3)0.042 (2)0.052 (3)0.019 (2)0.021 (2)0.002 (2)
C490.067 (3)0.041 (2)0.040 (2)0.019 (2)0.016 (2)0.0000 (19)
Geometric parameters (Å, º) top
Y1—O12.192 (2)C25—C261.389 (5)
Y1—O72.257 (2)C25—H250.9500
Y1—O32.335 (2)C26—C271.392 (4)
Y1—N12.521 (3)C26—H260.9500
Y1—N22.536 (2)C27—O41.383 (3)
Y1—O22.548 (2)O4—C281.448 (4)
Y1—O42.585 (2)C28—H28A0.9800
Y1—Cl12.7078 (8)C28—H28B0.9800
Y1—Y23.7479 (4)C28—H28C0.9800
Y2—O52.175 (2)O5—C291.304 (4)
Y2—O72.281 (2)C29—C301.415 (4)
Y2—O32.293 (2)C29—C341.420 (4)
Y2—O82.352 (2)C30—C311.376 (4)
Y2—O62.484 (2)C30—H300.9500
Y2—N32.487 (3)C31—C321.401 (5)
Y2—Cl22.6406 (9)C31—H310.9500
O1—C11.305 (4)C32—C331.379 (4)
C1—C61.416 (5)C32—H320.9500
C1—C21.418 (4)C33—C341.407 (4)
C2—C31.369 (5)C33—H330.9500
C2—H20.9500C34—C351.443 (4)
C3—C41.395 (5)C35—N31.296 (4)
C3—H30.9500C35—H350.9500
C4—C51.371 (5)N3—C361.436 (4)
C4—H40.9500C36—C371.386 (4)
C5—C61.425 (4)C36—C411.396 (4)
C5—H50.9500C37—C381.387 (4)
C6—C71.431 (5)C37—H370.9500
C7—N11.299 (4)C38—C391.380 (5)
C7—H70.9500C38—H380.9500
N1—C81.431 (4)C39—C401.399 (5)
C8—C91.393 (4)C39—H390.9500
C8—C131.402 (4)C40—C411.388 (4)
C9—C101.378 (5)C40—H400.9500
C9—H90.9500C41—O61.391 (4)
C10—C111.383 (5)O6—C421.450 (4)
C10—H100.9500C42—H42A0.9800
C11—C121.397 (4)C42—H42B0.9800
C11—H110.9500C42—H42C0.9800
C12—C131.391 (4)O7—C431.427 (4)
C12—H120.9500C43—H43A0.9800
C13—O21.382 (4)C43—H43B0.9800
O2—C141.455 (3)C43—H43C0.9800
C14—H14A0.9800O8—C441.407 (4)
C14—H14B0.9800O8—H80.837 (19)
C14—H14C0.9800C44—H44A0.9800
O3—C151.338 (4)C44—H44B0.9800
C15—C201.410 (4)C44—H44C0.9800
C15—C161.412 (4)O9—C451.410 (5)
C16—C171.374 (4)O9—H9A0.89 (2)
C16—H160.9500C45—H45A0.9800
C17—C181.395 (5)C45—H45B0.9800
C17—H170.9500C45—H45C0.9800
C18—C191.381 (4)O10—C491.430 (5)
C18—H180.9500O10—C461.431 (5)
C19—C201.402 (4)C46—C471.516 (6)
C19—H190.9500C46—H46A0.9900
C20—C211.455 (4)C46—H46B0.9900
C21—N21.296 (4)C47—C481.522 (6)
C21—H210.9500C47—H47A0.9900
N2—C221.427 (4)C47—H47B0.9900
C22—C231.395 (4)C48—C491.514 (6)
C22—C271.402 (4)C48—H48A0.9900
C23—C241.389 (4)C48—H48B0.9900
C23—H230.9500C49—H49A0.9900
C24—C251.378 (5)C49—H49B0.9900
C24—H240.9500
O1—Y1—O788.00 (8)C15—C20—C21123.9 (3)
O1—Y1—O3156.61 (8)N2—C21—C20125.9 (3)
O7—Y1—O370.07 (7)N2—C21—H21117.0
O1—Y1—N172.74 (8)C20—C21—H21117.0
O7—Y1—N1154.32 (8)C21—N2—C22117.4 (2)
O3—Y1—N1130.62 (8)C21—N2—Y1126.91 (19)
O1—Y1—N2126.38 (8)C22—N2—Y1115.25 (18)
O7—Y1—N2109.56 (8)C23—C22—C27118.5 (3)
O3—Y1—N270.95 (7)C23—C22—N2125.3 (3)
N1—Y1—N271.32 (8)C27—C22—N2116.1 (3)
O1—Y1—O2118.62 (7)C24—C23—C22120.4 (3)
O7—Y1—O2142.86 (7)C24—C23—H23119.8
O3—Y1—O278.31 (7)C22—C23—H23119.8
N1—Y1—O262.82 (7)C25—C24—C23120.3 (3)
N2—Y1—O276.55 (7)C25—C24—H24119.9
O1—Y1—O474.42 (7)C23—C24—H24119.9
O7—Y1—O478.97 (7)C24—C25—C26120.7 (3)
O3—Y1—O4107.87 (7)C24—C25—H25119.7
N1—Y1—O479.57 (7)C26—C25—H25119.7
N2—Y1—O461.01 (7)C25—C26—C27119.0 (3)
O2—Y1—O4130.54 (6)C25—C26—H26120.5
O1—Y1—Cl182.18 (6)C27—C26—H26120.5
O7—Y1—Cl184.00 (6)O4—C27—C26124.6 (3)
O3—Y1—Cl187.35 (5)O4—C27—C22114.4 (2)
N1—Y1—Cl1109.23 (6)C26—C27—C22121.1 (3)
N2—Y1—Cl1147.42 (6)C27—O4—C28116.2 (2)
O2—Y1—Cl175.41 (5)C27—O4—Y1115.96 (16)
O4—Y1—Cl1151.36 (5)C28—O4—Y1121.75 (17)
O1—Y1—Y2122.07 (6)O4—C28—H28A109.5
O7—Y1—Y234.53 (5)O4—C28—H28B109.5
O3—Y1—Y235.54 (5)H28A—C28—H28B109.5
N1—Y1—Y2162.04 (6)O4—C28—H28C109.5
N2—Y1—Y290.88 (5)H28A—C28—H28C109.5
O2—Y1—Y2111.62 (5)H28B—C28—H28C109.5
O4—Y1—Y294.16 (5)C29—O5—Y2143.63 (19)
Cl1—Y1—Y284.32 (2)O5—C29—C30120.1 (3)
O5—Y2—O7153.40 (8)O5—C29—C34122.7 (3)
O5—Y2—O3100.87 (8)C30—C29—C34117.2 (3)
O7—Y2—O370.39 (7)C31—C30—C29121.6 (3)
O5—Y2—O876.71 (8)C31—C30—H30119.2
O7—Y2—O877.42 (8)C29—C30—H30119.2
O3—Y2—O884.29 (9)C30—C31—C32121.2 (3)
O5—Y2—O6127.60 (7)C30—C31—H31119.4
O7—Y2—O678.97 (7)C32—C31—H31119.4
O3—Y2—O697.95 (7)C33—C32—C31118.2 (3)
O8—Y2—O6153.98 (8)C33—C32—H32120.9
O5—Y2—N373.04 (8)C31—C32—H32120.9
O7—Y2—N3127.23 (8)C32—C33—C34122.0 (3)
O3—Y2—N379.90 (8)C32—C33—H33119.0
O8—Y2—N3142.30 (9)C34—C33—H33119.0
O6—Y2—N362.86 (7)C33—C34—C29119.8 (3)
O5—Y2—Cl290.11 (6)C33—C34—C35117.2 (3)
O7—Y2—Cl295.12 (6)C29—C34—C35123.0 (3)
O3—Y2—Cl2164.78 (5)N3—C35—C34126.1 (3)
O8—Y2—Cl288.08 (8)N3—C35—H35117.0
O6—Y2—Cl283.28 (5)C34—C35—H35117.0
N3—Y2—Cl2113.68 (6)C35—N3—C36117.1 (3)
O5—Y2—Y1132.16 (6)C35—N3—Y2130.5 (2)
O7—Y2—Y134.10 (5)C36—N3—Y2112.44 (18)
O3—Y2—Y136.29 (5)C37—C36—C41119.0 (3)
O8—Y2—Y178.32 (6)C37—C36—N3125.4 (3)
O6—Y2—Y188.19 (5)C41—C36—N3115.5 (3)
N3—Y2—Y1106.28 (6)C36—C37—C38120.5 (3)
Cl2—Y2—Y1129.04 (2)C36—C37—H37119.7
C1—O1—Y1140.1 (2)C38—C37—H37119.7
O1—C1—C6121.8 (3)C39—C38—C37120.0 (3)
O1—C1—C2120.4 (3)C39—C38—H38120.0
C6—C1—C2117.8 (3)C37—C38—H38120.0
C3—C2—C1121.8 (3)C38—C39—C40120.6 (3)
C3—C2—H2119.1C38—C39—H39119.7
C1—C2—H2119.1C40—C39—H39119.7
C2—C3—C4120.7 (3)C41—C40—C39118.7 (3)
C2—C3—H3119.7C41—C40—H40120.6
C4—C3—H3119.7C39—C40—H40120.6
C5—C4—C3119.3 (3)C40—C41—O6124.4 (3)
C5—C4—H4120.3C40—C41—C36121.1 (3)
C3—C4—H4120.3O6—C41—C36114.5 (3)
C4—C5—C6121.6 (3)C41—O6—C42117.4 (2)
C4—C5—H5119.2C41—O6—Y2113.87 (17)
C6—C5—H5119.2C42—O6—Y2123.49 (19)
C1—C6—C5118.8 (3)O6—C42—H42A109.5
C1—C6—C7123.6 (3)O6—C42—H42B109.5
C5—C6—C7117.5 (3)H42A—C42—H42B109.5
N1—C7—C6127.1 (3)O6—C42—H42C109.5
N1—C7—H7116.4H42A—C42—H42C109.5
C6—C7—H7116.4H42B—C42—H42C109.5
C7—N1—C8117.0 (3)C43—O7—Y1122.61 (19)
C7—N1—Y1127.3 (2)C43—O7—Y2119.66 (18)
C8—N1—Y1115.56 (18)Y1—O7—Y2111.36 (9)
C9—C8—C13118.0 (3)O7—C43—H43A109.5
C9—C8—N1125.7 (3)O7—C43—H43B109.5
C13—C8—N1116.3 (3)H43A—C43—H43B109.5
C10—C9—C8121.3 (3)O7—C43—H43C109.5
C10—C9—H9119.4H43A—C43—H43C109.5
C8—C9—H9119.4H43B—C43—H43C109.5
C9—C10—C11120.4 (3)C44—O8—Y2132.7 (2)
C9—C10—H10119.8C44—O8—H8114 (3)
C11—C10—H10119.8Y2—O8—H8113 (3)
C10—C11—C12119.8 (3)O8—C44—H44A109.5
C10—C11—H11120.1O8—C44—H44B109.5
C12—C11—H11120.1H44A—C44—H44B109.5
C13—C12—C11119.4 (3)O8—C44—H44C109.5
C13—C12—H12120.3H44A—C44—H44C109.5
C11—C12—H12120.3H44B—C44—H44C109.5
O2—C13—C12122.9 (3)C45—O9—H9A102 (4)
O2—C13—C8116.0 (3)O9—C45—H45A109.5
C12—C13—C8121.1 (3)O9—C45—H45B109.5
C13—O2—C14114.7 (2)H45A—C45—H45B109.5
C13—O2—Y1116.82 (17)O9—C45—H45C109.5
C14—O2—Y1127.83 (17)H45A—C45—H45C109.5
O2—C14—H14A109.5H45B—C45—H45C109.5
O2—C14—H14B109.5C49—O10—C46108.8 (3)
H14A—C14—H14B109.5O10—C46—C47107.4 (3)
O2—C14—H14C109.5O10—C46—H46A110.2
H14A—C14—H14C109.5C47—C46—H46A110.2
H14B—C14—H14C109.5O10—C46—H46B110.2
C15—O3—Y2123.20 (17)C47—C46—H46B110.2
C15—O3—Y1128.17 (17)H46A—C46—H46B108.5
Y2—O3—Y1108.17 (8)C46—C47—C48102.0 (3)
O3—C15—C20121.2 (3)C46—C47—H47A111.4
O3—C15—C16120.4 (3)C48—C47—H47A111.4
C20—C15—C16118.4 (3)C46—C47—H47B111.4
C17—C16—C15121.0 (3)C48—C47—H47B111.4
C17—C16—H16119.5H47A—C47—H47B109.2
C15—C16—H16119.5C49—C48—C47101.7 (3)
C16—C17—C18121.2 (3)C49—C48—H48A111.4
C16—C17—H17119.4C47—C48—H48A111.4
C18—C17—H17119.4C49—C48—H48B111.4
C19—C18—C17118.2 (3)C47—C48—H48B111.4
C19—C18—H18120.9H48A—C48—H48B109.3
C17—C18—H18120.9O10—C49—C48106.7 (3)
C18—C19—C20122.3 (3)O10—C49—H49A110.4
C18—C19—H19118.9C48—C49—H49A110.4
C20—C19—H19118.9O10—C49—H49B110.4
C19—C20—C15118.9 (3)C48—C49—H49B110.4
C19—C20—C21117.1 (3)H49A—C49—H49B108.6
Y1—O1—C1—C628.9 (5)Y1—N2—C22—C2732.1 (3)
Y1—O1—C1—C2150.3 (2)C27—C22—C23—C241.8 (4)
O1—C1—C2—C3178.7 (3)N2—C22—C23—C24177.8 (3)
C6—C1—C2—C30.6 (5)C22—C23—C24—C250.0 (5)
C1—C2—C3—C40.7 (5)C23—C24—C25—C261.0 (5)
C2—C3—C4—C50.4 (5)C24—C25—C26—C270.3 (5)
C3—C4—C5—C61.6 (5)C25—C26—C27—O4177.4 (3)
O1—C1—C6—C5179.9 (3)C25—C26—C27—C221.5 (5)
C2—C1—C6—C50.6 (4)C23—C22—C27—O4176.5 (3)
O1—C1—C6—C72.9 (5)N2—C22—C27—O40.1 (4)
C2—C1—C6—C7177.8 (3)C23—C22—C27—C262.6 (4)
C4—C5—C6—C11.7 (5)N2—C22—C27—C26178.9 (3)
C4—C5—C6—C7179.1 (3)C26—C27—O4—C286.1 (4)
C1—C6—C7—N111.2 (5)C22—C27—O4—C28174.9 (2)
C5—C6—C7—N1171.6 (3)C26—C27—O4—Y1147.1 (2)
C6—C7—N1—C8177.9 (3)C22—C27—O4—Y131.9 (3)
C6—C7—N1—Y14.9 (4)Y2—O5—C29—C30169.0 (2)
C7—N1—C8—C927.5 (4)Y2—O5—C29—C3410.4 (5)
Y1—N1—C8—C9150.0 (2)O5—C29—C30—C31177.0 (3)
C7—N1—C8—C13154.2 (3)C34—C29—C30—C312.4 (5)
Y1—N1—C8—C1328.3 (3)C29—C30—C31—C321.4 (5)
C13—C8—C9—C103.3 (4)C30—C31—C32—C330.2 (5)
N1—C8—C9—C10178.5 (3)C31—C32—C33—C340.8 (5)
C8—C9—C10—C111.0 (5)C32—C33—C34—C290.3 (5)
C9—C10—C11—C121.1 (5)C32—C33—C34—C35179.9 (3)
C10—C11—C12—C130.9 (4)O5—C29—C34—C33177.5 (3)
C11—C12—C13—O2179.3 (3)C30—C29—C34—C331.8 (4)
C11—C12—C13—C81.4 (4)O5—C29—C34—C352.0 (5)
C9—C8—C13—O2177.2 (3)C30—C29—C34—C35178.6 (3)
N1—C8—C13—O21.2 (4)C33—C34—C35—N3175.2 (3)
C9—C8—C13—C123.5 (4)C29—C34—C35—N34.4 (5)
N1—C8—C13—C12178.1 (3)C34—C35—N3—C36178.4 (3)
C12—C13—O2—C1416.9 (4)C34—C35—N3—Y22.4 (5)
C8—C13—O2—C14162.4 (3)C35—N3—C36—C3736.3 (4)
C12—C13—O2—Y1154.3 (2)Y2—N3—C36—C37144.4 (2)
C8—C13—O2—Y126.3 (3)C35—N3—C36—C41147.0 (3)
Y2—O3—C15—C20122.4 (2)Y2—N3—C36—C4132.3 (3)
Y1—O3—C15—C2049.0 (3)C41—C36—C37—C380.7 (4)
Y2—O3—C15—C1656.4 (3)N3—C36—C37—C38177.3 (3)
Y1—O3—C15—C16132.2 (2)C36—C37—C38—C390.5 (5)
O3—C15—C16—C17178.6 (3)C37—C38—C39—C400.0 (5)
C20—C15—C16—C170.2 (4)C38—C39—C40—C410.3 (5)
C15—C16—C17—C181.4 (5)C39—C40—C41—O6179.6 (3)
C16—C17—C18—C190.9 (5)C39—C40—C41—C360.1 (4)
C17—C18—C19—C201.2 (5)C37—C36—C41—C400.4 (4)
C18—C19—C20—C152.8 (5)N3—C36—C41—C40177.3 (3)
C18—C19—C20—C21179.7 (3)C37—C36—C41—O6179.2 (3)
O3—C15—C20—C19176.6 (3)N3—C36—C41—O62.3 (4)
C16—C15—C20—C192.2 (4)C40—C41—O6—C4212.0 (4)
O3—C15—C20—C210.2 (4)C36—C41—O6—C42168.4 (3)
C16—C15—C20—C21179.0 (3)C40—C41—O6—Y2143.2 (2)
C19—C20—C21—N2163.9 (3)C36—C41—O6—Y236.4 (3)
C15—C20—C21—N219.3 (5)C49—O10—C46—C477.4 (4)
C20—C21—N2—C22179.1 (3)O10—C46—C47—C4827.4 (4)
C20—C21—N2—Y16.9 (4)C46—C47—C48—C4935.5 (4)
C21—N2—C22—C2329.2 (4)C46—O10—C49—C4816.1 (4)
Y1—N2—C22—C23143.9 (2)C47—C48—C49—O1032.6 (4)
C21—N2—C22—C27154.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8···Cl10.84 (2)2.20 (2)3.032 (3)174 (4)
O9—H9A···Cl20.89 (2)2.29 (2)3.175 (4)177 (6)
C43—H43A···O10.982.453.158 (4)129
C44—H44B···O50.982.593.132 (4)115
C14—H14C···Cl10.982.663.344 (3)128
C42—H42C···Cl20.982.893.591 (4)129
Bis(µ-2-{[(2-methoxyphenyl)imino]methyl}phenolato-1κ3O1,N,O2:2κO1)bis(2-{[(2-methoxyphenyl)imino]methyl}phenolato-2κ3O1,N,O2)sodiumyttrium chloroform disolvate (mol5) top
Crystal data top
[NaY(C14H12NO2)4]·2CHCl3Z = 2
Mr = 1255.62F(000) = 1284
Triclinic, P1Dx = 1.480 Mg m3
a = 14.542 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 15.366 (3) ÅCell parameters from 9999 reflections
c = 15.487 (3) Åθ = 2.3–30.3°
α = 108.34 (3)°µ = 1.39 mm1
β = 106.19 (3)°T = 120 K
γ = 108.77 (3)°Block, colourless
V = 2818.5 (13) Å30.27 × 0.26 × 0.12 mm
Data collection top
Bruker APEXII CCD
diffractometer
13529 independent reflections
Radiation source: fine-focus sealed tube10587 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
φ and ω scansθmax = 28.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
h = 1919
Tmin = 0.695, Tmax = 0.872k = 2015
19548 measured reflectionsl = 2020
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)] = 0.061Hydrogen site location: mixed
wR(F2) = 0.175H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0982P)2 + 3.5344P]
where P = (Fo2 + 2Fc2)/3
13529 reflections(Δ/σ)max < 0.001
743 parametersΔρmax = 1.19 e Å3
19 restraintsΔρmin = 1.79 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/UeqOcc. (<1)
Y10.13165 (2)0.27833 (2)0.41961 (2)0.01367 (9)
Na10.31568 (11)0.21868 (10)0.55695 (10)0.0172 (3)
O10.1576 (2)0.40438 (18)0.37281 (18)0.0192 (5)
C10.1175 (3)0.4165 (3)0.2934 (3)0.0175 (6)
C20.1307 (3)0.5153 (3)0.3022 (3)0.0218 (7)
H20.1710200.5727390.3665380.026*
C30.0865 (3)0.5299 (3)0.2197 (3)0.0293 (8)
H30.0953530.5965330.2284850.035*
C40.0287 (4)0.4475 (4)0.1234 (3)0.0344 (9)
H40.0030080.4574150.0669650.041*
C50.0189 (4)0.3523 (3)0.1121 (3)0.0325 (9)
H50.0189070.2967760.0465300.039*
C60.0625 (3)0.3333 (3)0.1938 (3)0.0216 (7)
C70.0576 (3)0.2335 (3)0.1723 (3)0.0216 (7)
H70.0263760.1867010.1032490.026*
N10.0903 (2)0.1995 (2)0.2351 (2)0.0168 (6)
C80.0987 (3)0.1068 (3)0.1971 (2)0.0181 (7)
C90.1229 (3)0.0761 (3)0.1151 (3)0.0228 (7)
H90.1295620.1156070.0787230.027*
C100.1374 (3)0.0123 (3)0.0862 (3)0.0284 (8)
H100.1537990.0331230.0301360.034*
C110.1280 (3)0.0694 (3)0.1392 (3)0.0296 (9)
H110.1382650.1293710.1192330.036*
C120.1039 (3)0.0410 (3)0.2211 (3)0.0240 (7)
H120.0971660.0812340.2567730.029*
C130.0896 (3)0.0476 (3)0.2503 (3)0.0183 (7)
O20.0670 (2)0.08295 (18)0.33110 (18)0.0198 (5)
C140.0408 (3)0.0158 (3)0.3771 (3)0.0234 (7)
H14A0.0169520.0515800.3256940.035*
H14B0.0174570.0451200.4278180.035*
H14C0.1042670.0082000.4090940.035*
O30.04291 (19)0.20839 (19)0.35098 (18)0.0208 (5)
C150.1200 (3)0.2352 (3)0.3474 (3)0.0169 (6)
C160.2219 (3)0.1720 (3)0.2645 (3)0.0223 (7)
H160.2320110.1121420.2121460.027*
C170.3061 (3)0.1956 (3)0.2586 (3)0.0254 (8)
H170.3734020.1518510.2022570.031*
C180.2941 (3)0.2834 (3)0.3344 (3)0.0237 (7)
H180.3530410.2988200.3300650.028*
C190.1963 (3)0.3467 (3)0.4148 (3)0.0194 (7)
H190.1876140.4066490.4658910.023*
C200.1080 (3)0.3243 (3)0.4230 (2)0.0158 (6)
C210.0103 (3)0.3937 (2)0.5129 (2)0.0158 (6)
H210.0130110.4484010.5608090.019*
N20.0807 (2)0.3900 (2)0.5358 (2)0.0141 (5)
C220.1615 (3)0.4582 (2)0.6347 (2)0.0153 (6)
C230.1416 (3)0.5002 (3)0.7175 (3)0.0196 (7)
H230.0699810.4835840.7093590.024*
C240.2261 (3)0.5661 (3)0.8119 (3)0.0238 (7)
H240.2118550.5957530.8674230.029*
C250.3307 (3)0.5887 (3)0.8253 (3)0.0231 (7)
H250.3880830.6339230.8898030.028*
C260.3517 (3)0.5451 (3)0.7443 (2)0.0184 (7)
H260.4232870.5590890.7535860.022*
C270.2677 (3)0.4810 (2)0.6499 (2)0.0155 (6)
O40.28311 (18)0.43651 (18)0.56596 (17)0.0179 (5)
C280.3829 (3)0.4915 (3)0.5656 (3)0.0212 (7)
H28A0.3961220.5627090.5823620.032*
H28B0.3803920.4591860.4988790.032*
H28C0.4408390.4903110.6154330.032*
O50.28164 (18)0.25737 (17)0.42195 (16)0.0149 (4)
C290.3271 (2)0.2513 (2)0.3593 (2)0.0150 (6)
C300.3322 (3)0.3154 (2)0.3099 (2)0.0161 (6)
H300.3025730.3622110.3232520.019*
C310.3786 (3)0.3121 (3)0.2432 (2)0.0183 (7)
H310.3797130.3557860.2112320.022*
C320.4241 (3)0.2449 (3)0.2223 (3)0.0201 (7)
H320.4573500.2431370.1773880.024*
C330.4194 (3)0.1812 (3)0.2687 (3)0.0202 (7)
H330.4493450.1347650.2540180.024*
C340.3721 (3)0.1819 (3)0.3369 (2)0.0165 (6)
C350.3703 (3)0.1056 (3)0.3743 (3)0.0199 (7)
H350.3989330.0615150.3476960.024*
N30.3358 (3)0.0902 (3)0.4374 (3)0.0293 (7)
C360.3366 (4)0.0050 (4)0.4564 (4)0.0381 (11)
C37A0.3322 (6)0.0838 (5)0.3835 (5)0.0330 (14)0.652 (6)
H37A0.3288980.0870160.3203300.040*0.652 (6)
C38A0.3329 (7)0.1650 (5)0.4055 (6)0.0374 (15)0.652 (6)
H38A0.3377290.2199470.3601880.045*0.652 (6)
C39A0.3265 (11)0.1664 (10)0.4929 (13)0.036 (3)0.652 (6)
H39A0.3297690.2204170.5090100.043*0.652 (6)
C37B0.4022 (13)0.0443 (10)0.4315 (10)0.0330 (14)0.348 (6)
H37B0.4440480.0225340.3981230.040*0.348 (6)
C38B0.4035 (13)0.1229 (10)0.4566 (12)0.0374 (15)0.348 (6)
H38B0.4363240.1631190.4317540.045*0.348 (6)
C39B0.357 (2)0.141 (2)0.517 (3)0.036 (3)0.348 (6)
H39B0.3546560.1972100.5306190.043*0.348 (6)
C400.3150 (3)0.0852 (3)0.5584 (3)0.0258 (8)
H400.2853910.0981100.6066140.031*
C410.3143 (3)0.0043 (3)0.5363 (3)0.0219 (7)
O60.2917 (3)0.0697 (2)0.5875 (2)0.0339 (7)
C420.2540 (5)0.0557 (4)0.6613 (4)0.0417 (11)
H42A0.1939490.0128910.6307330.063*
H42B0.2302650.1076310.6856800.063*
H42C0.3123160.0626990.7176340.063*
O70.16161 (19)0.23364 (18)0.54981 (17)0.0171 (5)
C430.1221 (3)0.2414 (2)0.6170 (2)0.0161 (6)
C440.0098 (3)0.2082 (3)0.5864 (3)0.0194 (7)
H440.0357910.1751910.5166840.023*
C450.0353 (3)0.2220 (3)0.6539 (3)0.0209 (7)
H450.1103860.1997990.6300940.025*
C460.0286 (3)0.2682 (3)0.7569 (3)0.0214 (7)
H460.0022220.2772620.8036530.026*
C470.1373 (3)0.3005 (3)0.7890 (3)0.0201 (7)
H470.1810990.3330130.8590760.024*
C480.1869 (3)0.2875 (3)0.7226 (3)0.0179 (6)
C490.3032 (3)0.3331 (3)0.7703 (2)0.0189 (7)
H490.3361280.3790980.8397920.023*
N40.3671 (2)0.3195 (2)0.7313 (2)0.0182 (6)
C500.4786 (3)0.3742 (3)0.7936 (3)0.0186 (7)
C510.5244 (3)0.4079 (3)0.8978 (3)0.0243 (7)
H510.4792530.3931190.9305630.029*
C520.6354 (3)0.4634 (3)0.9541 (3)0.0281 (8)
H520.6652820.4862351.0246990.034*
C530.7016 (3)0.4852 (3)0.9069 (3)0.0268 (8)
H530.7769020.5240140.9454380.032*
C540.6589 (3)0.4506 (3)0.8035 (3)0.0230 (7)
H540.7048760.4656800.7715460.028*
C550.5485 (3)0.3938 (3)0.7468 (2)0.0184 (7)
O80.5002 (2)0.3548 (2)0.64454 (18)0.0221 (5)
C560.5686 (3)0.3755 (3)0.5955 (3)0.0238 (7)
H56A0.6099370.4499010.6221340.036*
H56B0.5250010.3459120.5231670.036*
H56C0.6176900.3450390.6074120.036*
C57A0.7037 (4)0.8539 (4)0.0273 (4)0.0314 (11)0.773 (2)
H57A0.7071950.8617730.0335340.038*0.773 (2)
Cl1A0.59848 (14)0.87792 (18)0.04503 (14)0.0671 (6)0.773 (2)
Cl2A0.67662 (17)0.72574 (14)0.00496 (12)0.0538 (5)0.773 (2)
C57B0.7544 (14)0.8302 (15)0.0278 (13)0.0314 (11)0.227 (2)
H57B0.7296600.8425520.0322940.038*0.227 (2)
Cl1B0.8348 (5)0.7696 (6)0.0132 (5)0.0671 (6)0.227 (2)
Cl2B0.6420 (6)0.7546 (5)0.0361 (4)0.0538 (5)0.227 (2)
Cl30.82563 (9)0.94501 (11)0.13085 (9)0.0475 (3)
C58A0.6469 (6)0.1972 (6)0.9108 (6)0.079 (4)0.293 (3)
H58A0.6152030.2421910.9381180.094*0.293 (3)
Cl4A0.5419 (5)0.0898 (5)0.8015 (5)0.0829 (6)0.293 (3)
Cl5A0.7018 (6)0.1644 (6)1.0053 (5)0.0829 (6)0.293 (3)
Cl6A0.7473 (5)0.2704 (7)0.8851 (7)0.0829 (6)0.293 (3)
C58B0.6527 (4)0.2263 (5)0.8974 (4)0.079 (4)0.497 (3)
H58B0.6410420.2850620.9344280.094*0.497 (3)
Cl4B0.5400 (3)0.1479 (3)0.7805 (3)0.0829 (6)0.497 (3)
Cl5B0.6658 (3)0.1599 (4)0.9709 (3)0.0829 (6)0.497 (3)
Cl6B0.7701 (3)0.2780 (5)0.8806 (4)0.0829 (6)0.497 (3)
C58C0.6618 (6)0.2192 (8)0.8765 (7)0.079 (4)0.210 (3)
H58C0.6459080.2784540.9024370.094*0.210 (3)
Cl4C0.5395 (6)0.1142 (8)0.7833 (7)0.0829 (6)0.210 (3)
Cl5C0.7152 (8)0.1960 (9)0.9793 (6)0.0829 (6)0.210 (3)
Cl6C0.7556 (7)0.2563 (8)0.8276 (8)0.0829 (6)0.210 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.01529 (15)0.01361 (16)0.01239 (15)0.00798 (12)0.00561 (11)0.00480 (12)
Na10.0212 (7)0.0189 (7)0.0148 (6)0.0117 (5)0.0082 (5)0.0082 (5)
O10.0244 (12)0.0164 (12)0.0181 (11)0.0113 (10)0.0082 (10)0.0075 (10)
C10.0174 (15)0.0225 (17)0.0201 (16)0.0128 (14)0.0101 (13)0.0123 (14)
C20.0252 (17)0.0243 (18)0.0291 (18)0.0169 (15)0.0177 (15)0.0159 (15)
C30.037 (2)0.032 (2)0.041 (2)0.0253 (18)0.0243 (19)0.0254 (19)
C40.041 (2)0.043 (2)0.034 (2)0.027 (2)0.0141 (19)0.027 (2)
C50.039 (2)0.036 (2)0.0229 (19)0.0208 (19)0.0079 (17)0.0144 (17)
C60.0205 (16)0.0267 (18)0.0200 (17)0.0122 (15)0.0071 (14)0.0129 (15)
C70.0223 (17)0.0243 (18)0.0136 (15)0.0095 (14)0.0059 (13)0.0056 (14)
N10.0162 (13)0.0164 (14)0.0154 (13)0.0076 (11)0.0059 (11)0.0047 (11)
C80.0156 (15)0.0151 (16)0.0158 (15)0.0066 (13)0.0038 (13)0.0007 (13)
C90.0224 (17)0.0223 (18)0.0169 (16)0.0103 (14)0.0051 (14)0.0033 (14)
C100.0273 (19)0.0251 (19)0.0212 (18)0.0105 (16)0.0105 (15)0.0020 (15)
C110.0288 (19)0.0169 (17)0.035 (2)0.0121 (15)0.0128 (17)0.0005 (16)
C120.0229 (17)0.0146 (16)0.032 (2)0.0081 (14)0.0111 (15)0.0080 (15)
C130.0132 (14)0.0152 (16)0.0206 (16)0.0058 (12)0.0056 (13)0.0032 (13)
O20.0257 (13)0.0167 (12)0.0223 (12)0.0120 (10)0.0136 (10)0.0091 (10)
C140.0278 (18)0.0158 (16)0.0268 (18)0.0074 (14)0.0122 (15)0.0116 (15)
O30.0163 (11)0.0208 (12)0.0199 (12)0.0098 (10)0.0056 (10)0.0033 (10)
C150.0158 (15)0.0174 (16)0.0201 (16)0.0084 (13)0.0078 (13)0.0101 (13)
C160.0177 (16)0.0174 (17)0.0214 (17)0.0046 (13)0.0029 (14)0.0047 (14)
C170.0185 (17)0.0226 (18)0.0254 (18)0.0065 (14)0.0016 (14)0.0089 (15)
C180.0179 (16)0.0251 (18)0.0319 (19)0.0122 (14)0.0086 (15)0.0164 (16)
C190.0214 (16)0.0171 (16)0.0256 (17)0.0118 (14)0.0115 (14)0.0119 (14)
C200.0157 (15)0.0169 (16)0.0172 (15)0.0091 (13)0.0065 (13)0.0091 (13)
C210.0202 (16)0.0135 (15)0.0175 (15)0.0092 (13)0.0096 (13)0.0080 (13)
N20.0159 (13)0.0129 (13)0.0144 (12)0.0077 (11)0.0064 (11)0.0058 (11)
C220.0186 (15)0.0127 (15)0.0147 (15)0.0081 (12)0.0059 (12)0.0060 (12)
C230.0211 (16)0.0209 (17)0.0179 (16)0.0104 (14)0.0095 (14)0.0078 (14)
C240.0301 (19)0.0230 (18)0.0153 (16)0.0117 (15)0.0105 (15)0.0043 (14)
C250.0258 (18)0.0200 (17)0.0119 (15)0.0055 (14)0.0035 (14)0.0025 (13)
C260.0181 (16)0.0167 (16)0.0158 (15)0.0067 (13)0.0043 (13)0.0058 (13)
C270.0196 (15)0.0145 (15)0.0133 (14)0.0080 (13)0.0074 (13)0.0064 (12)
O40.0160 (11)0.0180 (12)0.0142 (11)0.0052 (9)0.0065 (9)0.0033 (9)
C280.0194 (16)0.0177 (16)0.0228 (17)0.0048 (13)0.0118 (14)0.0058 (14)
O50.0176 (11)0.0161 (11)0.0141 (11)0.0091 (9)0.0087 (9)0.0069 (9)
C290.0121 (14)0.0167 (15)0.0109 (14)0.0054 (12)0.0020 (11)0.0038 (12)
C300.0163 (15)0.0138 (15)0.0169 (15)0.0069 (12)0.0057 (13)0.0063 (13)
C310.0192 (16)0.0155 (16)0.0157 (15)0.0050 (13)0.0050 (13)0.0066 (13)
C320.0191 (16)0.0239 (18)0.0167 (15)0.0083 (14)0.0099 (13)0.0077 (14)
C330.0219 (16)0.0224 (17)0.0182 (16)0.0125 (14)0.0098 (14)0.0075 (14)
C340.0160 (15)0.0175 (16)0.0152 (15)0.0079 (13)0.0066 (12)0.0058 (13)
C350.0224 (17)0.0224 (17)0.0228 (17)0.0164 (14)0.0122 (14)0.0106 (14)
N30.053 (2)0.0297 (18)0.0313 (17)0.0306 (17)0.0293 (17)0.0208 (15)
C360.072 (3)0.038 (2)0.049 (3)0.044 (2)0.046 (3)0.034 (2)
C37A0.055 (4)0.031 (3)0.037 (4)0.029 (3)0.034 (3)0.021 (3)
C38A0.057 (4)0.028 (3)0.052 (4)0.030 (3)0.037 (3)0.023 (3)
C39A0.051 (9)0.024 (7)0.059 (10)0.025 (6)0.036 (7)0.030 (7)
C37B0.055 (4)0.031 (3)0.037 (4)0.029 (3)0.034 (3)0.021 (3)
C38B0.057 (4)0.028 (3)0.052 (4)0.030 (3)0.037 (3)0.023 (3)
C39B0.051 (9)0.024 (7)0.059 (10)0.025 (6)0.036 (7)0.030 (7)
C400.0292 (19)0.028 (2)0.031 (2)0.0161 (16)0.0152 (16)0.0207 (17)
C410.0236 (17)0.0244 (18)0.0243 (17)0.0146 (15)0.0110 (15)0.0138 (15)
O60.064 (2)0.0278 (15)0.0385 (16)0.0301 (15)0.0393 (16)0.0227 (13)
C420.069 (3)0.038 (2)0.043 (3)0.030 (2)0.041 (3)0.025 (2)
O70.0203 (11)0.0199 (12)0.0162 (11)0.0119 (10)0.0092 (9)0.0096 (10)
C430.0218 (16)0.0147 (15)0.0187 (16)0.0115 (13)0.0110 (13)0.0099 (13)
C440.0202 (16)0.0172 (16)0.0203 (16)0.0083 (13)0.0069 (14)0.0091 (14)
C450.0208 (16)0.0198 (17)0.0296 (19)0.0123 (14)0.0142 (15)0.0134 (15)
C460.0270 (18)0.0201 (17)0.0263 (18)0.0125 (15)0.0198 (15)0.0118 (15)
C470.0268 (18)0.0205 (17)0.0173 (16)0.0124 (14)0.0126 (14)0.0087 (14)
C480.0229 (16)0.0176 (16)0.0185 (16)0.0122 (14)0.0110 (14)0.0092 (13)
C490.0249 (17)0.0187 (16)0.0144 (15)0.0124 (14)0.0070 (13)0.0074 (13)
N40.0195 (14)0.0208 (14)0.0147 (13)0.0103 (12)0.0058 (11)0.0083 (11)
C500.0219 (16)0.0177 (16)0.0176 (16)0.0114 (14)0.0076 (13)0.0074 (13)
C510.0259 (18)0.029 (2)0.0177 (17)0.0139 (16)0.0089 (14)0.0088 (15)
C520.0274 (19)0.037 (2)0.0150 (16)0.0169 (17)0.0040 (15)0.0083 (16)
C530.0201 (17)0.029 (2)0.0246 (18)0.0108 (15)0.0035 (15)0.0096 (16)
C540.0214 (17)0.0244 (18)0.0204 (17)0.0101 (15)0.0075 (14)0.0080 (15)
C550.0210 (16)0.0185 (16)0.0154 (15)0.0108 (14)0.0055 (13)0.0072 (13)
O80.0206 (12)0.0276 (14)0.0155 (11)0.0081 (11)0.0074 (10)0.0097 (10)
C560.0250 (18)0.0283 (19)0.0179 (16)0.0095 (15)0.0107 (14)0.0110 (15)
C57A0.022 (2)0.042 (3)0.023 (2)0.010 (2)0.008 (2)0.011 (2)
Cl1A0.0375 (8)0.0899 (14)0.0443 (9)0.0281 (9)0.0154 (7)0.0022 (9)
Cl2A0.0792 (12)0.0444 (9)0.0322 (8)0.0213 (8)0.0168 (7)0.0231 (7)
C57B0.022 (2)0.042 (3)0.023 (2)0.010 (2)0.008 (2)0.011 (2)
Cl1B0.0375 (8)0.0899 (14)0.0443 (9)0.0281 (9)0.0154 (7)0.0022 (9)
Cl2B0.0792 (12)0.0444 (9)0.0322 (8)0.0213 (8)0.0168 (7)0.0231 (7)
Cl30.0292 (5)0.0590 (8)0.0322 (6)0.0083 (5)0.0033 (4)0.0151 (5)
C58A0.105 (7)0.081 (7)0.046 (5)0.074 (6)0.004 (5)0.015 (5)
Cl4A0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl5A0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl6A0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
C58B0.105 (7)0.081 (7)0.046 (5)0.074 (6)0.004 (5)0.015 (5)
Cl4B0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl5B0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl6B0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
C58C0.105 (7)0.081 (7)0.046 (5)0.074 (6)0.004 (5)0.015 (5)
Cl4C0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl5C0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Cl6C0.0634 (10)0.0917 (14)0.0791 (12)0.0449 (11)0.0178 (9)0.0218 (10)
Geometric parameters (Å, º) top
Y1—O32.179 (3)C31—H310.9500
Y1—O12.233 (2)C32—C331.381 (5)
Y1—O52.297 (2)C32—H320.9500
Y1—O72.303 (2)C33—C341.412 (5)
Y1—O42.490 (3)C33—H330.9500
Y1—N22.519 (3)C34—C351.458 (5)
Y1—N12.528 (3)C35—N31.268 (5)
Y1—O22.579 (3)C35—H350.9500
Y1—Na13.4867 (17)N3—C361.432 (5)
Na1—O72.301 (3)C36—C411.400 (5)
Na1—O52.316 (3)C36—C37A1.441 (8)
Na1—N42.397 (3)C36—C37B1.456 (13)
Na1—N32.405 (3)C37A—C38A1.396 (9)
Na1—O62.418 (3)C37A—H37A0.9500
Na1—O82.447 (3)C38A—C39A1.39 (2)
O1—C11.305 (4)C38A—H38A0.9500
C1—C21.423 (5)C39A—C401.431 (19)
C1—C61.437 (5)C39A—H39A0.9500
C2—C31.382 (5)C37B—C38B1.384 (17)
C2—H20.9500C37B—H37B0.9500
C3—C41.401 (6)C38B—C39B1.34 (4)
C3—H30.9500C38B—H38B0.9500
C4—C51.372 (6)C39B—C401.31 (4)
C4—H40.9500C39B—H39B0.9500
C5—C61.411 (5)C40—C411.391 (5)
C5—H50.9500C40—H401.0000
C6—C71.436 (5)C41—O61.361 (4)
C7—N11.291 (5)O6—C421.442 (5)
C7—H70.9500C42—H42A0.9800
N1—C81.420 (4)C42—H42B0.9800
C8—C91.392 (5)C42—H42C0.9800
C8—C131.408 (5)O7—C431.314 (4)
C9—C101.395 (5)C43—C441.425 (5)
C9—H90.9500C43—C481.431 (5)
C10—C111.379 (6)C44—C451.378 (5)
C10—H100.9500C44—H440.9500
C11—C121.385 (6)C45—C461.395 (5)
C11—H110.9500C45—H450.9500
C12—C131.395 (5)C46—C471.377 (5)
C12—H120.9500C46—H460.9500
C13—O21.373 (4)C47—C481.410 (5)
O2—C141.442 (4)C47—H470.9500
C14—H14A0.9800C48—C491.454 (5)
C14—H14B0.9800C49—N41.277 (4)
C14—H14C0.9800C49—H490.9500
O3—C151.306 (4)N4—C501.417 (5)
C15—C201.414 (5)C50—C511.403 (5)
C15—C161.420 (5)C50—C551.415 (5)
C16—C171.372 (5)C51—C521.398 (5)
C16—H160.9500C51—H510.9503
C17—C181.403 (6)C52—C531.384 (6)
C17—H170.9500C52—H520.9500
C18—C191.371 (5)C53—C541.389 (5)
C18—H180.9500C53—H530.9500
C19—C201.416 (5)C54—C551.393 (5)
C19—H190.9500C54—H540.9500
C20—C211.443 (5)C55—O81.368 (4)
C21—N21.297 (4)O8—C561.428 (4)
C21—H210.9500C56—H56A0.9800
N2—C221.421 (4)C56—H56B0.9800
C22—C231.397 (5)C56—H56C0.9800
C22—C271.399 (5)C57A—Cl31.755 (5)
C23—C241.392 (5)C57A—Cl1A1.756 (6)
C23—H230.9500C57A—Cl2A1.775 (6)
C24—C251.385 (5)C57A—H57A1.0000
C24—H240.9500C57B—Cl31.692 (19)
C25—C261.390 (5)C57B—Cl1B1.73 (2)
C25—H250.9500C57B—Cl2B1.74 (2)
C26—C271.387 (5)C57B—H57B1.0000
C26—H260.9500C58A—Cl4A1.761 (4)
C27—O41.382 (4)C58A—Cl6A1.762 (4)
O4—C281.428 (4)C58A—Cl5A1.762 (4)
C28—H28A0.9800C58A—H58A1.0000
C28—H28B0.9800C58B—Cl5B1.763 (4)
C28—H28C0.9800C58B—Cl6B1.765 (4)
O5—C291.314 (4)C58B—Cl4B1.765 (4)
C29—C301.421 (5)C58B—H58B1.0000
C29—C341.424 (5)C58C—Cl4C1.762 (4)
C30—C311.379 (5)C58C—Cl6C1.763 (4)
C30—H300.9500C58C—Cl5C1.763 (4)
C31—C321.399 (5)C58C—H58C1.0000
O3—Y1—O196.57 (10)O4—C28—H28B109.5
O3—Y1—O5146.22 (9)H28A—C28—H28B109.5
O1—Y1—O599.02 (9)O4—C28—H28C109.5
O3—Y1—O7100.48 (10)H28A—C28—H28C109.5
O1—Y1—O7147.28 (9)H28B—C28—H28C109.5
O5—Y1—O781.82 (8)C29—O5—Y1132.9 (2)
O3—Y1—O4137.94 (9)C29—O5—Na1128.1 (2)
O1—Y1—O473.18 (9)Y1—O5—Na198.18 (9)
O5—Y1—O475.56 (8)O5—C29—C30120.0 (3)
O7—Y1—O475.44 (9)O5—C29—C34123.0 (3)
O3—Y1—N274.09 (10)C30—C29—C34117.1 (3)
O1—Y1—N280.31 (9)C31—C30—C29122.5 (3)
O5—Y1—N2138.09 (9)C31—C30—H30118.8
O7—Y1—N277.83 (9)C29—C30—H30118.8
O4—Y1—N264.06 (9)C30—C31—C32120.4 (3)
O3—Y1—N178.51 (10)C30—C31—H31119.8
O1—Y1—N172.84 (9)C32—C31—H31119.8
O5—Y1—N177.78 (9)C33—C32—C31118.3 (3)
O7—Y1—N1137.92 (9)C33—C32—H32120.9
O4—Y1—N1132.26 (9)C31—C32—H32120.9
N2—Y1—N1138.79 (9)C32—C33—C34122.9 (3)
O3—Y1—O273.71 (10)C32—C33—H33118.5
O1—Y1—O2135.70 (8)C34—C33—H33118.5
O5—Y1—O274.19 (9)C33—C34—C29118.8 (3)
O7—Y1—O276.31 (9)C33—C34—C35114.8 (3)
O4—Y1—O2140.94 (8)C29—C34—C35126.3 (3)
N2—Y1—O2133.69 (9)N3—C35—C34128.8 (3)
N1—Y1—O262.90 (9)N3—C35—H35115.6
O3—Y1—Na1132.98 (8)C34—C35—H35115.6
O1—Y1—Na1130.45 (7)C35—N3—C36117.8 (3)
O5—Y1—Na141.11 (6)C35—N3—Na1122.8 (3)
O7—Y1—Na140.75 (6)C36—N3—Na1117.2 (2)
O4—Y1—Na169.27 (7)C41—C36—N3118.5 (3)
N2—Y1—Na1109.65 (7)C41—C36—C37A117.4 (4)
N1—Y1—Na1111.56 (7)N3—C36—C37A122.2 (4)
O2—Y1—Na171.71 (7)C41—C36—C37B113.1 (6)
O7—Na1—O581.45 (9)N3—C36—C37B122.7 (6)
O7—Na1—N479.41 (10)C38A—C37A—C36120.1 (6)
O5—Na1—N4131.33 (11)C38A—C37A—H37A120.0
O7—Na1—N3128.34 (13)C36—C37A—H37A120.0
O5—Na1—N378.16 (10)C39A—C38A—C37A120.7 (9)
N4—Na1—N3145.73 (12)C39A—C38A—H38A119.7
O7—Na1—O6102.97 (11)C37A—C38A—H38A119.7
O5—Na1—O6138.72 (11)C38A—C39A—C40119.0 (13)
N4—Na1—O689.28 (11)C38A—C39A—H39A120.5
N3—Na1—O666.95 (11)C40—C39A—H39A120.5
O7—Na1—O8128.00 (11)C38B—C37B—C36119.8 (11)
O5—Na1—O892.30 (10)C38B—C37B—H37B120.1
N4—Na1—O866.62 (11)C36—C37B—H37B120.1
N3—Na1—O899.90 (13)C39B—C38B—C37B118 (2)
O6—Na1—O8114.23 (12)C39B—C38B—H38B120.9
O7—Na1—Y140.78 (6)C37B—C38B—H38B120.9
O5—Na1—Y140.70 (6)C40—C39B—C38B124 (3)
N4—Na1—Y1107.34 (8)C40—C39B—H39B117.8
N3—Na1—Y1106.91 (10)C38B—C39B—H39B117.8
O6—Na1—Y1131.27 (10)C39B—C40—C41118.6 (18)
O8—Na1—Y1114.42 (8)C41—C40—C39A120.2 (8)
C1—O1—Y1138.4 (2)C39B—C40—H40122.1
O1—C1—C2120.5 (3)C41—C40—H40119.3
O1—C1—C6122.3 (3)C39A—C40—H40117.9
C2—C1—C6117.1 (3)O6—C41—C40124.1 (3)
C3—C2—C1121.7 (4)O6—C41—C36115.1 (3)
C3—C2—H2119.1C40—C41—C36120.8 (3)
C1—C2—H2119.1C41—O6—C42117.0 (3)
C2—C3—C4120.8 (4)C41—O6—Na1121.2 (2)
C2—C3—H3119.6C42—O6—Na1121.8 (2)
C4—C3—H3119.6O6—C42—H42A109.5
C5—C4—C3118.6 (4)O6—C42—H42B109.5
C5—C4—H4120.7H42A—C42—H42B109.5
C3—C4—H4120.7O6—C42—H42C109.5
C4—C5—C6122.8 (4)H42A—C42—H42C109.5
C4—C5—H5118.6H42B—C42—H42C109.5
C6—C5—H5118.6C43—O7—Na1128.7 (2)
C5—C6—C7118.0 (3)C43—O7—Y1130.6 (2)
C5—C6—C1118.8 (3)Na1—O7—Y198.47 (10)
C7—C6—C1123.0 (3)O7—C43—C44120.0 (3)
N1—C7—C6128.1 (3)O7—C43—C48123.4 (3)
N1—C7—H7115.9C44—C43—C48116.5 (3)
C6—C7—H7115.9C45—C44—C43122.6 (3)
C7—N1—C8117.7 (3)C45—C44—H44118.7
C7—N1—Y1125.7 (2)C43—C44—H44118.7
C8—N1—Y1116.4 (2)C44—C45—C46120.5 (3)
C9—C8—C13119.0 (3)C44—C45—H45119.7
C9—C8—N1123.3 (3)C46—C45—H45119.7
C13—C8—N1117.5 (3)C47—C46—C45118.3 (3)
C8—C9—C10120.2 (4)C47—C46—H46120.8
C8—C9—H9119.9C45—C46—H46120.8
C10—C9—H9119.9C46—C47—C48123.1 (3)
C11—C10—C9119.8 (4)C46—C47—H47118.4
C11—C10—H10120.1C48—C47—H47118.4
C9—C10—H10120.1C47—C48—C43118.9 (3)
C10—C11—C12121.3 (3)C47—C48—C49115.3 (3)
C10—C11—H11119.3C43—C48—C49125.5 (3)
C12—C11—H11119.3N4—C49—C48128.6 (3)
C11—C12—C13118.9 (4)N4—C49—H49115.7
C11—C12—H12120.5C48—C49—H49115.7
C13—C12—H12120.5C49—N4—C50118.1 (3)
O2—C13—C12123.4 (3)C49—N4—Na1125.5 (2)
O2—C13—C8116.0 (3)C50—N4—Na1116.3 (2)
C12—C13—C8120.6 (3)C51—C50—C55117.9 (3)
C13—O2—C14116.9 (3)C51—C50—N4124.7 (3)
C13—O2—Y1116.4 (2)C55—C50—N4117.4 (3)
C14—O2—Y1123.8 (2)C52—C51—C50121.0 (4)
O2—C14—H14A109.5C52—C51—H51119.6
O2—C14—H14B109.5C50—C51—H51119.5
H14A—C14—H14B109.5C53—C52—C51119.8 (3)
O2—C14—H14C109.5C53—C52—H52120.1
H14A—C14—H14C109.5C51—C52—H52120.1
H14B—C14—H14C109.5C52—C53—C54120.6 (4)
C15—O3—Y1139.3 (2)C52—C53—H53119.7
O3—C15—C20123.3 (3)C54—C53—H53119.7
O3—C15—C16119.2 (3)C53—C54—C55119.9 (3)
C20—C15—C16117.5 (3)C53—C54—H54120.1
C17—C16—C15121.3 (3)C55—C54—H54120.1
C17—C16—H16119.3O8—C55—C54123.6 (3)
C15—C16—H16119.3O8—C55—C50115.7 (3)
C16—C17—C18121.0 (3)C54—C55—C50120.8 (3)
C16—C17—H17119.5C55—O8—C56116.9 (3)
C18—C17—H17119.5C55—O8—Na1117.6 (2)
C19—C18—C17119.1 (3)C56—O8—Na1123.3 (2)
C19—C18—H18120.5O8—C56—H56A109.5
C17—C18—H18120.5O8—C56—H56B109.5
C18—C19—C20121.2 (3)H56A—C56—H56B109.5
C18—C19—H19119.4O8—C56—H56C109.5
C20—C19—H19119.4H56A—C56—H56C109.5
C15—C20—C19119.9 (3)H56B—C56—H56C109.5
C15—C20—C21123.6 (3)Cl3—C57A—Cl1A109.7 (3)
C19—C20—C21116.4 (3)Cl3—C57A—Cl2A113.0 (3)
N2—C21—C20127.4 (3)Cl1A—C57A—Cl2A109.7 (3)
N2—C21—H21116.3Cl3—C57A—H57A108.1
C20—C21—H21116.3Cl1A—C57A—H57A108.1
C21—N2—C22117.2 (3)Cl2A—C57A—H57A108.1
C21—N2—Y1126.3 (2)Cl3—C57B—Cl1B110.1 (10)
C22—N2—Y1116.4 (2)Cl3—C57B—Cl2B110.3 (10)
C23—C22—C27118.4 (3)Cl1B—C57B—Cl2B111.5 (12)
C23—C22—N2124.5 (3)Cl3—C57B—H57B108.3
C27—C22—N2117.1 (3)Cl1B—C57B—H57B108.3
C24—C23—C22120.5 (3)Cl2B—C57B—H57B108.3
C24—C23—H23119.8Cl4A—C58A—Cl6A112.2 (4)
C22—C23—H23119.8Cl4A—C58A—Cl5A112.7 (4)
C25—C24—C23120.3 (3)Cl6A—C58A—Cl5A111.2 (4)
C25—C24—H24119.9Cl4A—C58A—H58A106.8
C23—C24—H24119.9Cl6A—C58A—H58A106.8
C24—C25—C26120.0 (3)Cl5A—C58A—H58A106.8
C24—C25—H25120.0Cl5B—C58B—Cl6B112.0 (3)
C26—C25—H25120.0Cl5B—C58B—Cl4B111.5 (3)
C27—C26—C25119.6 (3)Cl6B—C58B—Cl4B110.8 (3)
C27—C26—H26120.2Cl5B—C58B—H58B107.4
C25—C26—H26120.2Cl6B—C58B—H58B107.4
O4—C27—C26122.6 (3)Cl4B—C58B—H58B107.4
O4—C27—C22116.2 (3)Cl4C—C58C—Cl6C112.1 (4)
C26—C27—C22121.2 (3)Cl4C—C58C—Cl5C111.9 (4)
C27—O4—C28116.6 (3)Cl6C—C58C—Cl5C111.6 (4)
C27—O4—Y1118.97 (19)Cl4C—C58C—H58C107.0
C28—O4—Y1124.08 (19)Cl6C—C58C—H58C107.0
O4—C28—H28A109.5Cl5C—C58C—H58C107.0
Y1—O1—C1—C2158.2 (3)C31—C32—C33—C340.8 (5)
Y1—O1—C1—C624.3 (5)C32—C33—C34—C290.1 (5)
O1—C1—C2—C3178.1 (3)C32—C33—C34—C35177.2 (3)
C6—C1—C2—C34.3 (5)O5—C29—C34—C33179.9 (3)
C1—C2—C3—C41.5 (6)C30—C29—C34—C330.6 (5)
C2—C3—C4—C51.4 (6)O5—C29—C34—C353.2 (5)
C3—C4—C5—C61.4 (7)C30—C29—C34—C35176.3 (3)
C4—C5—C6—C7173.3 (4)C33—C34—C35—N3178.1 (4)
C4—C5—C6—C11.5 (6)C29—C34—C35—N34.9 (6)
O1—C1—C6—C5178.2 (3)C34—C35—N3—C36175.8 (4)
C2—C1—C6—C54.2 (5)C34—C35—N3—Na121.4 (6)
O1—C1—C6—C77.2 (5)C35—N3—C36—C41170.5 (4)
C2—C1—C6—C7170.3 (3)Na1—N3—C36—C416.7 (6)
C5—C6—C7—N1178.4 (4)C35—N3—C36—C37A25.5 (8)
C1—C6—C7—N17.0 (6)Na1—N3—C36—C37A170.7 (5)
C6—C7—N1—C8166.4 (3)C35—N3—C36—C37B18.9 (10)
C6—C7—N1—Y117.1 (5)Na1—N3—C36—C37B144.9 (8)
C7—N1—C8—C930.8 (5)C41—C36—C37A—C38A15.7 (10)
Y1—N1—C8—C9152.4 (3)N3—C36—C37A—C38A179.9 (6)
C7—N1—C8—C13154.0 (3)C36—C37A—C38A—C39A6.7 (13)
Y1—N1—C8—C1322.8 (4)C37A—C38A—C39A—C402.4 (15)
C13—C8—C9—C100.3 (5)C41—C36—C37B—C38B23.6 (16)
N1—C8—C9—C10175.4 (3)N3—C36—C37B—C38B176.6 (11)
C8—C9—C10—C110.2 (6)C36—C37B—C38B—C39B10 (3)
C9—C10—C11—C120.2 (6)C37B—C38B—C39B—C404 (4)
C10—C11—C12—C130.4 (6)C38B—C39B—C40—C412 (3)
C11—C12—C13—O2179.1 (3)C38A—C39A—C40—C412.4 (13)
C11—C12—C13—C80.5 (5)C39B—C40—C41—O6167.4 (14)
C9—C8—C13—O2179.2 (3)C39A—C40—C41—O6172.2 (7)
N1—C8—C13—O23.8 (4)C39B—C40—C41—C3613.4 (15)
C9—C8—C13—C120.5 (5)C39A—C40—C41—C367.1 (8)
N1—C8—C13—C12175.9 (3)N3—C36—C41—O61.3 (6)
C12—C13—O2—C149.8 (5)C37A—C36—C41—O6163.5 (5)
C8—C13—O2—C14170.6 (3)C37B—C36—C41—O6155.5 (7)
C12—C13—O2—Y1151.6 (3)N3—C36—C41—C40179.4 (4)
C8—C13—O2—Y128.1 (4)C37A—C36—C41—C4015.8 (7)
Y1—O3—C15—C2024.3 (5)C37B—C36—C41—C4025.2 (9)
Y1—O3—C15—C16156.4 (3)C40—C41—O6—C427.5 (6)
O3—C15—C16—C17178.5 (3)C36—C41—O6—C42171.7 (4)
C20—C15—C16—C170.9 (5)C40—C41—O6—Na1171.8 (3)
C15—C16—C17—C180.1 (6)C36—C41—O6—Na19.0 (5)
C16—C17—C18—C190.7 (6)Na1—O7—C43—C44154.0 (2)
C17—C18—C19—C200.7 (5)Y1—O7—C43—C4446.9 (4)
O3—C15—C20—C19178.5 (3)Na1—O7—C43—C4829.7 (4)
C16—C15—C20—C190.9 (5)Y1—O7—C43—C48129.4 (3)
O3—C15—C20—C211.4 (5)O7—C43—C44—C45174.5 (3)
C16—C15—C20—C21177.9 (3)C48—C43—C44—C452.0 (5)
C18—C19—C20—C150.1 (5)C43—C44—C45—C461.2 (5)
C18—C19—C20—C21177.3 (3)C44—C45—C46—C470.7 (5)
C15—C20—C21—N24.4 (5)C45—C46—C47—C481.0 (5)
C19—C20—C21—N2178.4 (3)C46—C47—C48—C431.9 (5)
C20—C21—N2—C22171.4 (3)C46—C47—C48—C49175.6 (3)
C20—C21—N2—Y111.4 (5)O7—C43—C48—C47174.2 (3)
C21—N2—C22—C2324.5 (5)C44—C43—C48—C472.3 (5)
Y1—N2—C22—C23158.0 (3)O7—C43—C48—C491.1 (5)
C21—N2—C22—C27158.2 (3)C44—C43—C48—C49175.3 (3)
Y1—N2—C22—C2719.3 (4)C47—C48—C49—N4167.4 (3)
C27—C22—C23—C242.4 (5)C43—C48—C49—N419.3 (6)
N2—C22—C23—C24179.7 (3)C48—C49—N4—C50179.3 (3)
C22—C23—C24—C251.7 (6)C48—C49—N4—Na14.3 (5)
C23—C24—C25—C260.3 (6)C49—N4—C50—C5127.2 (5)
C24—C25—C26—C271.5 (5)Na1—N4—C50—C51157.4 (3)
C25—C26—C27—O4178.9 (3)C49—N4—C50—C55154.4 (3)
C25—C26—C27—C220.8 (5)Na1—N4—C50—C5521.1 (4)
C23—C22—C27—O4179.1 (3)C55—C50—C51—C523.0 (5)
N2—C22—C27—O41.7 (4)N4—C50—C51—C52178.6 (3)
C23—C22—C27—C261.2 (5)C50—C51—C52—C530.4 (6)
N2—C22—C27—C26178.6 (3)C51—C52—C53—C541.2 (6)
C26—C27—O4—C2828.7 (4)C52—C53—C54—C550.1 (6)
C22—C27—O4—C28151.0 (3)C53—C54—C55—O8178.3 (3)
C26—C27—O4—Y1157.6 (3)C53—C54—C55—C502.5 (5)
C22—C27—O4—Y122.7 (4)C51—C50—C55—O8176.8 (3)
Y1—O5—C29—C3039.4 (4)N4—C50—C55—O81.8 (4)
Na1—O5—C29—C30153.4 (2)C51—C50—C55—C544.0 (5)
Y1—O5—C29—C34140.1 (3)N4—C50—C55—C54177.4 (3)
Na1—O5—C29—C3427.1 (4)C54—C55—O8—C560.7 (5)
O5—C29—C30—C31179.8 (3)C50—C55—O8—C56178.5 (3)
C34—C29—C30—C310.2 (5)C54—C55—O8—Na1162.7 (3)
C29—C30—C31—C320.6 (5)C50—C55—O8—Na118.1 (4)
C30—C31—C32—C331.2 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C28—H28B···O50.982.643.129 (4)111
C28—H28C···O80.982.613.402 (5)138
C30—H30···O10.952.633.470 (4)148
C42—H42C···Cl4Bb0.982.873.604 (7)132
C42—H42C···Cl4Cc0.982.923.711 (10)139
C9—H9···Cl1Bbi0.952.613.557 (10)175
C16—H16···Cl3ii0.952.973.838 (4)153
C37Bb—H37Bb···Cl4Bbiii0.952.953.624 (13)129
C51—H51···Cl2Bbiv0.952.683.498 (8)144
Symmetry codes: (i) x+1, y+1, z; (ii) x1, y1, z; (iii) x+1, y, z+1; (iv) x+1, y+1, z+1.
The dihedral angles (°) between two planes within the same ligand top
Each plane is formed by eight atoms, i.e. six C atoms of a phenyl rings and two atoms in ortho positions. These atoms are O1/C1–C7 and N1/C8–C13/O2 (ligand 1), O3/C15–C21 and N2/C22–C27/O4 (ligand 2), O5/C29–C35 and N3/C36–C41/O6 (ligand 3), as well as O7/C43–C49 and N4/C50–C55/O8 [either ligand 1, molecule 2 in (3) or ligand 4 in (5)], O9/C57–C63 and N5/C64–C69/O10 [ligand 2, molecule 2 in (3)], and O11/C71–C77 and N6/C78–C83/O12 [ligand 3, molecule 2 in (3)].
ComplexLigand 1Ligand 2Ligand 3Ligand 4
(1)37.32 (13)36.42 (8)32.07 (9)-
(2)60.76 (5)22.69 (4)41.10 (6)-
(3), molecule 171.48 (9)32.59 (8)31.87 (12)-
(3), molecule 272.13 (9)41.23 (11)47.86 (9)-
(4)16.69 (10)9.12 (11)39.61 (8)-
(5)42.20 (8)31.03 (9)20.6 (2) a12.64 (7)
Note: (a) the value was calculated by using atoms (C37A, C38A and C39A) belonging to the major component of the phenyl-ring disorder in (5).
Acrylonitrile polymerization tests top
Polymerization conditions: [Ln]/[Bu2Mg]/[TMEDA] = 1:6:6; [AN]/[Ln] = 835:1. T = 273 K. Conversion is a monomer-to-polymer conversion value. Mn and Mw are the number and weight average molecular masses, respectively. ĐM is a polydispersity index determined as ĐM = Mw/Mn. L is the Schiff base ligand.
RunPrecatalystConversion ( %)Mn(calc)a (× 10-3)Mn(found)b (× 10-3)Mw(found)b (× 10-3)ĐMb
1c-9.6-11.546.94.06
2(1), LaL33113.724.653.22.16
3d(1), LaL3229.742.593.32.19
4(2), NdL333.314.827.668.72.49
5(3), YL332.814.530.793.63.04
6(5), Na[YL4]34.515.320.941.41.98
7Lu–phosph e5423.933.084.52.56
8Nd–phosph e26.011.513.338.32.88
9NdP f42.418.816.381.75.01
Notes: (a) Mn(calc) = MAN × [AN]/[Ln] × Conversion, where MAN is the molecular mass of acrylonitrile. (b) Found values of Mn, Mw and ĐM were determined by size-exclusion chromatography (SEC) measurements. (c) The control experiment without a precatalyst. (d) T = 293 K for for run 3. (e) Literature data; precatalysts are {Ln2[(2,6-tBu2-4-MeC6H2-O)(EtO)PO2]6} Ln = Lu, Nd (see Minyaev et al., 2018b). (f) NdP is neodymium tris(2-ethylhexyl phosphonate).
 

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