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The crystal structures of rare-earth diaryl- or di­alkyl­phosphate derivatives are poorly explored. Crystals of bis­[bis­(2,6-diiso­propyl­phen­yl)phosphato-κO]chlorido­tetra­kis­(methanol-κO)neodymium methanol disolvate, [Nd(C24H34O4P)Cl(CH4O)4]·2CH3OH, (1), and of the lutetium, [Lu(C24H34O4P)Cl(CH4O)4]·2CH3OH, (2), and yttrium, [Y(C24H34O4P)Cl(CH4O)4]·2CH3OH, (3), analogues have been obtained by reactions between lithium bis­(2,6-diiso­propyl­phen­yl)phosphate and LnCl3(H2O)6 (in a 2:1 ratio) in methanol. Compounds (1)–(3) crystallize in the C2/c space group. Their crystal structures are isomorphous. The mol­ecule possesses C2 symmetry with a twofold crystallographic axis passing through the Ln and Cl atoms. The bis­(2,6-diiso­propyl­phen­yl)phosphate ligands all display a κ1O-monodentate coordination mode. The coordination polyhedron for the metal atom [coordination number (CN) = 7] is a distorted penta­gonal bipyramid. Each [Ln{O2P(O-2,6-iPr2C6H3)2}2Cl(CH3OH)4] mol­ecular unit exhibits two intra­molecular O—H...O hydrogen bonds, forming six-membered rings, and two intra­molecular O—H...Cl inter­actions, forming four-membered rings. Inter­molecular O—H...O hydrogen bonds connect each unit via four noncoordinating methanol mol­ecules with four other units, forming a two-dimensional hydrogen-bond network. Crystals of bis­[bis­(2,6-diiso­propyl­phen­yl)phosphato-κO]tetra­kis­(methanol-κO)(nitrato-κ2O,O′)neo­dymium methanol disolvate, [Nd(C24H34O4P)(NO3)(CH4O)4]·2CH3OH, (4), have been obtained in an analogous manner from NdCl3(H2O)6. Compound (4) also crystalizes in the C2/c space group. Its crystal structure is similar to those of (1)–(3). The κ2O,O′-bidentate nitrate anion is disordered over a twofold axis, being located nearly on it. Half of the mol­ecule is crystallographically unique (CNNd = 8). Unlike (1)–(3), complex (4) exhibits disorder of all three methanol mol­ecules, one isopropyl group of the phosphate ligand and the NO3 ligand. The structure of (4) displays intra- and inter­molecular O—H...O hydrogen bonds similar to those in (1)–(3). Compounds (1)–(4) represent the first reported mononuclear bis­[bis­(diar­yl/dialk­yl)phosphate] rare-earth complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617012979/uk3140sup1.cif
Contains datablocks mol-1, mol-2, mol-3, mol-4, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617012979/uk3140mol-1sup2.hkl
Contains datablock mol-1

cdx

Chemdraw file https://doi.org/10.1107/S2053229617012979/uk3140mol-1sup6.cdx
Supplementary material

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617012979/uk3140mol-2sup3.hkl
Contains datablock mol-2

cdx

Chemdraw file https://doi.org/10.1107/S2053229617012979/uk3140mol-2sup7.cdx
Supplementary material

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617012979/uk3140mol-3sup4.hkl
Contains datablock mol-3

cdx

Chemdraw file https://doi.org/10.1107/S2053229617012979/uk3140mol-3sup8.cdx
Supplementary material

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617012979/uk3140mol-4sup5.hkl
Contains datablock mol-4

cdx

Chemdraw file https://doi.org/10.1107/S2053229617012979/uk3140mol-4sup9.cdx
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229617012979/uk3140sup10.pdf
Additional experimental information and figures

CCDC references: 1573905; 1573904; 1573903; 1573902

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: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Bis[bis(2,6-diisopropylphenyl)phosphato-κO]chloridotetrakis(methanol-κO)neodymium methanol disolvate (mol-1) top
Crystal data top
[Nd(C24H34O4P)Cl(CH4O)4]·2CH4OF(000) = 2540
Mr = 1206.90Dx = 1.296 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 16.9491 (5) ÅCell parameters from 9990 reflections
b = 12.3954 (4) Åθ = 2.3–30.5°
c = 30.5023 (9) ŵ = 0.99 mm1
β = 105.1103 (4)°T = 100 K
V = 6186.7 (3) Å3Block, pale violet
Z = 40.40 × 0.30 × 0.25 mm
Data collection top
Bruker APEXII CCD area detector
diffractometer
9305 independent reflections
Radiation source: fine-focus sealed tube8151 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 30.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 2423
Tmin = 0.640, Tmax = 0.746k = 1717
30228 measured reflectionsl = 4243
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)] = 0.034Hydrogen site location: mixed
wR(F2) = 0.088H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0423P)2 + 9.9452P]
where P = (Fo2 + 2Fc2)/3
9305 reflections(Δ/σ)max = 0.001
349 parametersΔρmax = 1.53 e Å3
0 restraintsΔρmin = 0.61 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.50000.25251 (2)0.25000.01769 (5)
Cl10.50000.03575 (7)0.25000.0539 (3)
P10.57860 (3)0.35432 (3)0.15695 (2)0.01242 (8)
O10.52336 (8)0.29324 (10)0.17960 (4)0.0156 (2)
O20.62946 (8)0.43841 (10)0.18622 (4)0.0173 (2)
O30.63932 (7)0.27636 (10)0.14037 (4)0.0140 (2)
O40.52734 (7)0.39922 (10)0.10929 (4)0.0141 (2)
O50.59173 (11)0.41245 (13)0.26379 (6)0.0315 (4)
O60.64179 (10)0.18702 (18)0.27682 (8)0.0476 (5)
H280.609 (2)0.429 (3)0.2391 (14)0.077 (12)*
H290.650 (3)0.119 (5)0.2819 (19)0.13 (2)*
C10.62135 (10)0.22221 (14)0.09829 (6)0.0141 (3)
C20.59290 (11)0.11618 (15)0.09651 (7)0.0195 (3)
C30.58130 (12)0.06236 (16)0.05503 (8)0.0245 (4)
H3A0.56260.01020.05250.029*
C40.59649 (12)0.11267 (17)0.01752 (7)0.0246 (4)
H4A0.58810.07460.01040.030*
C50.62389 (12)0.21833 (17)0.02058 (7)0.0211 (4)
H5A0.63340.25230.00550.025*
C60.63787 (11)0.27620 (14)0.06128 (6)0.0161 (3)
C70.57849 (14)0.06005 (16)0.13791 (8)0.0270 (4)
H7A0.57700.11660.16110.032*
C80.64923 (16)0.0166 (2)0.15863 (9)0.0396 (6)
H8A0.70080.02370.16600.059*
H8B0.65150.07380.13680.059*
H8C0.64070.04890.18640.059*
C90.49687 (16)0.0003 (2)0.12710 (11)0.0412 (6)
H9A0.45220.05170.11590.062*
H9B0.49000.03480.15470.062*
H9C0.49600.05440.10380.062*
C100.67121 (11)0.39038 (14)0.06411 (7)0.0186 (3)
H10A0.67430.41940.09510.022*
C110.75759 (14)0.39072 (18)0.05705 (10)0.0347 (5)
H11A0.79390.34730.08080.052*
H11B0.77800.46500.05860.052*
H11C0.75600.36010.02720.052*
C120.61552 (15)0.46435 (18)0.02901 (8)0.0295 (5)
H12A0.56050.46420.03370.044*
H12B0.61310.43820.00160.044*
H12C0.63740.53790.03250.044*
C130.45447 (10)0.45889 (14)0.10255 (6)0.0146 (3)
C140.38046 (11)0.40258 (15)0.08915 (6)0.0170 (3)
C150.30905 (11)0.46384 (17)0.08080 (7)0.0226 (4)
H15A0.25760.42860.07150.027*
C160.31161 (12)0.57512 (17)0.08586 (7)0.0241 (4)
H16A0.26220.61510.08070.029*
C170.38583 (12)0.62766 (16)0.09835 (7)0.0218 (4)
H17A0.38680.70400.10140.026*
C180.45984 (11)0.57095 (14)0.10662 (6)0.0170 (3)
C190.37889 (12)0.28087 (16)0.08265 (7)0.0213 (4)
H19A0.42760.25060.10520.026*
C200.30285 (17)0.2283 (2)0.09162 (12)0.0432 (6)
H20A0.29690.25160.12130.065*
H20B0.30850.14960.09140.065*
H20C0.25440.25000.06790.065*
C210.38773 (19)0.25298 (18)0.03553 (9)0.0373 (6)
H21A0.43820.28500.03140.056*
H21B0.34080.28150.01250.056*
H21C0.38990.17440.03240.056*
C220.54047 (12)0.63200 (15)0.11852 (7)0.0219 (4)
H22A0.58580.57830.12210.026*
C230.55230 (15)0.69284 (18)0.16359 (8)0.0313 (5)
H23A0.55520.64100.18820.047*
H23B0.50610.74180.16160.047*
H23C0.60310.73450.16970.047*
C240.54494 (14)0.70965 (17)0.08007 (8)0.0285 (4)
H24A0.53590.66950.05150.043*
H24B0.59900.74380.08710.043*
H24C0.50280.76530.07710.043*
C250.60203 (17)0.5046 (2)0.29239 (8)0.0359 (5)
H25A0.64360.55200.28560.054*
H25B0.61950.48170.32420.054*
H25C0.55010.54360.28710.054*
C260.7205 (2)0.2288 (4)0.2773 (2)0.0816 (14)
H26A0.76270.18670.29850.122*
H26B0.72400.30440.28700.122*
H26C0.72890.22390.24680.122*
H300.741 (3)0.482 (4)0.1918 (17)0.107 (17)*
O70.79430 (14)0.4856 (2)0.19751 (11)0.0757 (9)
C270.83229 (19)0.3827 (3)0.19551 (14)0.0628 (10)
H27A0.88250.39280.18580.094*
H27B0.79470.33600.17380.094*
H27C0.84560.34910.22560.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.02032 (7)0.02024 (7)0.01381 (7)0.0000.00677 (5)0.000
Cl10.0467 (5)0.0220 (4)0.0764 (7)0.0000.0137 (5)0.000
P10.01337 (18)0.01211 (18)0.01238 (19)0.00116 (14)0.00443 (15)0.00008 (14)
O10.0165 (6)0.0176 (6)0.0139 (6)0.0005 (5)0.0062 (5)0.0007 (5)
O20.0190 (6)0.0150 (6)0.0179 (6)0.0023 (5)0.0046 (5)0.0028 (5)
O30.0145 (5)0.0137 (5)0.0144 (6)0.0037 (4)0.0047 (5)0.0001 (4)
O40.0138 (5)0.0150 (5)0.0146 (6)0.0051 (4)0.0056 (4)0.0022 (4)
O50.0442 (9)0.0319 (8)0.0237 (8)0.0146 (7)0.0183 (7)0.0115 (6)
O60.0206 (8)0.0485 (12)0.0718 (14)0.0060 (8)0.0087 (8)0.0188 (10)
C10.0130 (7)0.0146 (7)0.0158 (8)0.0033 (6)0.0054 (6)0.0015 (6)
C20.0187 (8)0.0164 (8)0.0268 (9)0.0006 (6)0.0117 (7)0.0020 (7)
C30.0212 (9)0.0196 (9)0.0346 (11)0.0012 (7)0.0107 (8)0.0094 (8)
C40.0209 (9)0.0293 (10)0.0239 (10)0.0022 (7)0.0060 (7)0.0107 (8)
C50.0197 (8)0.0270 (9)0.0175 (9)0.0078 (7)0.0067 (7)0.0001 (7)
C60.0146 (7)0.0170 (7)0.0174 (8)0.0049 (6)0.0054 (6)0.0014 (6)
C70.0393 (11)0.0149 (8)0.0337 (11)0.0011 (8)0.0218 (9)0.0003 (7)
C80.0413 (13)0.0390 (13)0.0401 (14)0.0002 (11)0.0134 (11)0.0135 (11)
C90.0378 (13)0.0252 (11)0.0692 (19)0.0024 (9)0.0291 (13)0.0101 (11)
C100.0220 (8)0.0159 (8)0.0214 (9)0.0054 (6)0.0120 (7)0.0037 (6)
C110.0297 (11)0.0215 (10)0.0615 (16)0.0022 (8)0.0272 (11)0.0017 (10)
C120.0408 (12)0.0250 (10)0.0262 (10)0.0130 (9)0.0148 (9)0.0101 (8)
C130.0142 (7)0.0169 (7)0.0134 (7)0.0053 (6)0.0049 (6)0.0018 (6)
C140.0169 (8)0.0197 (8)0.0146 (8)0.0017 (6)0.0041 (6)0.0007 (6)
C150.0150 (8)0.0302 (10)0.0217 (9)0.0026 (7)0.0029 (7)0.0024 (7)
C160.0186 (8)0.0308 (10)0.0235 (10)0.0113 (7)0.0063 (7)0.0039 (8)
C170.0255 (9)0.0193 (8)0.0206 (9)0.0096 (7)0.0057 (7)0.0023 (7)
C180.0188 (8)0.0161 (8)0.0160 (8)0.0038 (6)0.0042 (6)0.0019 (6)
C190.0205 (8)0.0192 (8)0.0217 (9)0.0018 (7)0.0008 (7)0.0010 (7)
C200.0362 (13)0.0312 (12)0.0653 (19)0.0134 (10)0.0189 (13)0.0039 (12)
C210.0557 (16)0.0288 (11)0.0255 (11)0.0064 (10)0.0073 (11)0.0055 (9)
C220.0210 (9)0.0147 (8)0.0285 (10)0.0012 (6)0.0037 (7)0.0028 (7)
C230.0372 (12)0.0220 (9)0.0289 (11)0.0024 (8)0.0017 (9)0.0009 (8)
C240.0326 (11)0.0194 (9)0.0346 (12)0.0004 (8)0.0107 (9)0.0052 (8)
C250.0476 (14)0.0396 (12)0.0228 (10)0.0138 (11)0.0133 (10)0.0126 (9)
C260.0261 (14)0.082 (3)0.133 (4)0.0021 (15)0.016 (2)0.029 (3)
O70.0334 (11)0.0707 (16)0.125 (2)0.0256 (11)0.0250 (13)0.0427 (16)
C270.0403 (16)0.064 (2)0.085 (3)0.0172 (15)0.0177 (16)0.0291 (19)
Geometric parameters (Å, º) top
Nd1—O1i2.3381 (13)C12—H12A0.9800
Nd1—O12.3381 (13)C12—H12B0.9800
Nd1—O6i2.4654 (17)C12—H12C0.9800
Nd1—O62.4655 (17)C13—C181.395 (2)
Nd1—O5i2.4866 (16)C13—C141.400 (2)
Nd1—O52.4867 (16)C14—C151.395 (3)
Nd1—Cl12.6868 (9)C14—C191.521 (3)
P1—O21.4918 (13)C15—C161.387 (3)
P1—O11.5047 (13)C15—H15A0.9500
P1—O41.5872 (13)C16—C171.379 (3)
P1—O31.5875 (13)C16—H16A0.9500
O3—C11.410 (2)C17—C181.402 (2)
O4—C131.4080 (19)C17—H17A0.9500
O5—C251.420 (3)C18—C221.521 (3)
O5—H280.90 (4)C19—C211.523 (3)
O6—C261.428 (4)C19—C201.531 (3)
O6—H290.87 (6)C19—H19A1.0000
C1—C21.396 (2)C20—H20A0.9800
C1—C61.402 (3)C20—H20B0.9800
C2—C31.398 (3)C20—H20C0.9800
C2—C71.516 (3)C21—H21A0.9800
C3—C41.385 (3)C21—H21B0.9800
C3—H3A0.9500C21—H21C0.9800
C4—C51.385 (3)C22—C241.534 (3)
C4—H4A0.9500C22—C231.535 (3)
C5—C61.400 (3)C22—H22A1.0000
C5—H5A0.9500C23—H23A0.9800
C6—C101.518 (3)C23—H23B0.9800
C7—C91.528 (3)C23—H23C0.9800
C7—C81.531 (3)C24—H24A0.9800
C7—H7A1.0000C24—H24B0.9800
C8—H8A0.9800C24—H24C0.9800
C8—H8B0.9800C25—H25A0.9800
C8—H8C0.9800C25—H25B0.9800
C9—H9A0.9800C25—H25C0.9800
C9—H9B0.9800C26—H26A0.9800
C9—H9C0.9800C26—H26B0.9800
C10—C121.533 (3)C26—H26C0.9800
C10—C111.534 (3)O7—C271.437 (4)
C10—H10A1.0000O7—H300.88 (5)
C11—H11A0.9800C27—H27A0.9800
C11—H11B0.9800C27—H27B0.9800
C11—H11C0.9800C27—H27C0.9800
O1i—Nd1—O1155.06 (6)H11A—C11—H11C109.5
O1i—Nd1—O6i89.54 (6)H11B—C11—H11C109.5
O1—Nd1—O6i98.64 (6)C10—C12—H12A109.5
O1i—Nd1—O698.64 (6)C10—C12—H12B109.5
O1—Nd1—O689.54 (6)H12A—C12—H12B109.5
O6i—Nd1—O6141.55 (10)C10—C12—H12C109.5
O1i—Nd1—O5i74.64 (5)H12A—C12—H12C109.5
O1—Nd1—O5i85.45 (5)H12B—C12—H12C109.5
O6i—Nd1—O5i72.18 (7)C18—C13—C14123.71 (16)
O6—Nd1—O5i146.20 (7)C18—C13—O4118.39 (15)
O1i—Nd1—O585.45 (5)C14—C13—O4117.76 (15)
O1—Nd1—O574.63 (5)C15—C14—C13116.78 (17)
O6i—Nd1—O5146.20 (7)C15—C14—C19122.09 (17)
O6—Nd1—O572.18 (7)C13—C14—C19121.10 (16)
O5i—Nd1—O574.26 (9)C16—C15—C14121.36 (18)
O1i—Nd1—Cl1102.47 (3)C16—C15—H15A119.3
O1—Nd1—Cl1102.47 (3)C14—C15—H15A119.3
O6i—Nd1—Cl170.78 (5)C17—C16—C15120.00 (17)
O6—Nd1—Cl170.78 (5)C17—C16—H16A120.0
O5i—Nd1—Cl1142.87 (4)C15—C16—H16A120.0
O5—Nd1—Cl1142.87 (4)C16—C17—C18121.45 (18)
O2—P1—O1114.10 (8)C16—C17—H17A119.3
O2—P1—O4113.34 (7)C18—C17—H17A119.3
O1—P1—O4109.84 (7)C13—C18—C17116.64 (17)
O2—P1—O3107.13 (7)C13—C18—C22123.38 (16)
O1—P1—O3111.88 (7)C17—C18—C22119.97 (16)
O4—P1—O399.63 (7)C14—C19—C21110.21 (17)
P1—O1—Nd1143.61 (8)C14—C19—C20112.69 (18)
C1—O3—P1125.16 (11)C21—C19—C20111.5 (2)
C13—O4—P1124.59 (11)C14—C19—H19A107.4
C25—O5—Nd1135.75 (14)C21—C19—H19A107.4
C25—O5—H28108 (3)C20—C19—H19A107.4
Nd1—O5—H28111 (3)C19—C20—H20A109.5
C26—O6—Nd1135.4 (2)C19—C20—H20B109.5
C26—O6—H29104 (4)H20A—C20—H20B109.5
Nd1—O6—H29119 (4)C19—C20—H20C109.5
C2—C1—C6123.89 (17)H20A—C20—H20C109.5
C2—C1—O3118.30 (16)H20B—C20—H20C109.5
C6—C1—O3117.70 (15)C19—C21—H21A109.5
C1—C2—C3116.74 (18)C19—C21—H21B109.5
C1—C2—C7121.91 (17)H21A—C21—H21B109.5
C3—C2—C7121.30 (17)C19—C21—H21C109.5
C4—C3—C2121.34 (18)H21A—C21—H21C109.5
C4—C3—H3A119.3H21B—C21—H21C109.5
C2—C3—H3A119.3C18—C22—C24110.49 (16)
C5—C4—C3120.11 (18)C18—C22—C23110.96 (18)
C5—C4—H4A119.9C24—C22—C23110.83 (17)
C3—C4—H4A119.9C18—C22—H22A108.2
C4—C5—C6121.38 (19)C24—C22—H22A108.2
C4—C5—H5A119.3C23—C22—H22A108.2
C6—C5—H5A119.3C22—C23—H23A109.5
C5—C6—C1116.52 (17)C22—C23—H23B109.5
C5—C6—C10120.17 (17)H23A—C23—H23B109.5
C1—C6—C10123.30 (16)C22—C23—H23C109.5
C2—C7—C9112.1 (2)H23A—C23—H23C109.5
C2—C7—C8110.47 (18)H23B—C23—H23C109.5
C9—C7—C8110.83 (18)C22—C24—H24A109.5
C2—C7—H7A107.8C22—C24—H24B109.5
C9—C7—H7A107.8H24A—C24—H24B109.5
C8—C7—H7A107.8C22—C24—H24C109.5
C7—C8—H8A109.5H24A—C24—H24C109.5
C7—C8—H8B109.5H24B—C24—H24C109.5
H8A—C8—H8B109.5O5—C25—H25A109.5
C7—C8—H8C109.5O5—C25—H25B109.5
H8A—C8—H8C109.5H25A—C25—H25B109.5
H8B—C8—H8C109.5O5—C25—H25C109.5
C7—C9—H9A109.5H25A—C25—H25C109.5
C7—C9—H9B109.5H25B—C25—H25C109.5
H9A—C9—H9B109.5O6—C26—H26A109.5
C7—C9—H9C109.5O6—C26—H26B109.5
H9A—C9—H9C109.5H26A—C26—H26B109.5
H9B—C9—H9C109.5O6—C26—H26C109.5
C6—C10—C12111.45 (17)H26A—C26—H26C109.5
C6—C10—C11110.44 (15)H26B—C26—H26C109.5
C12—C10—C11109.67 (17)C27—O7—H30113 (3)
C6—C10—H10A108.4O7—C27—H27A109.5
C12—C10—H10A108.4O7—C27—H27B109.5
C11—C10—H10A108.4H27A—C27—H27B109.5
C10—C11—H11A109.5O7—C27—H27C109.5
C10—C11—H11B109.5H27A—C27—H27C109.5
H11A—C11—H11B109.5H27B—C27—H27C109.5
C10—C11—H11C109.5
O2—P1—O1—Nd117.06 (16)C5—C6—C10—C1257.9 (2)
O4—P1—O1—Nd1145.58 (12)C1—C6—C10—C12123.66 (19)
O3—P1—O1—Nd1104.76 (13)C5—C6—C10—C1164.3 (2)
O2—P1—O3—C1147.93 (13)C1—C6—C10—C11114.2 (2)
O1—P1—O3—C186.32 (15)P1—O4—C13—C1889.22 (18)
O4—P1—O3—C129.72 (15)P1—O4—C13—C1494.97 (18)
O2—P1—O4—C1378.04 (15)C18—C13—C14—C151.8 (3)
O1—P1—O4—C1350.89 (15)O4—C13—C14—C15177.36 (16)
O3—P1—O4—C13168.47 (13)C18—C13—C14—C19176.30 (17)
P1—O3—C1—C295.29 (17)O4—C13—C14—C190.7 (3)
P1—O3—C1—C688.45 (18)C13—C14—C15—C160.4 (3)
C6—C1—C2—C30.5 (3)C19—C14—C15—C16178.44 (19)
O3—C1—C2—C3175.54 (16)C14—C15—C16—C171.5 (3)
C6—C1—C2—C7178.01 (17)C15—C16—C17—C180.6 (3)
O3—C1—C2—C72.0 (3)C14—C13—C18—C172.6 (3)
C1—C2—C3—C40.7 (3)O4—C13—C18—C17178.17 (15)
C7—C2—C3—C4178.30 (19)C14—C13—C18—C22176.29 (18)
C2—C3—C4—C50.1 (3)O4—C13—C18—C220.8 (3)
C3—C4—C5—C60.8 (3)C16—C17—C18—C131.4 (3)
C4—C5—C6—C11.1 (3)C16—C17—C18—C22177.60 (19)
C4—C5—C6—C10177.50 (17)C15—C14—C19—C2194.5 (2)
C2—C1—C6—C50.4 (3)C13—C14—C19—C2183.5 (2)
O3—C1—C6—C5176.44 (15)C15—C14—C19—C2030.8 (3)
C2—C1—C6—C10178.09 (17)C13—C14—C19—C20151.2 (2)
O3—C1—C6—C102.1 (2)C13—C18—C22—C24119.0 (2)
C1—C2—C7—C9134.4 (2)C17—C18—C22—C2459.9 (2)
C3—C2—C7—C948.2 (3)C13—C18—C22—C23117.7 (2)
C1—C2—C7—C8101.5 (2)C17—C18—C22—C2363.4 (2)
C3—C2—C7—C876.0 (3)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H28···O20.90 (4)1.74 (4)2.626 (2)168 (4)
O7—H30···O20.88 (5)1.93 (5)2.787 (3)165 (5)
O6—H29···O7ii0.87 (6)1.92 (6)2.753 (3)161 (5)
O6—H29···Cl10.87 (6)2.69 (6)2.989 (2)102 (4)
Symmetry code: (ii) x+3/2, y1/2, z+1/2.
Bis[bis(2,6-diisopropylphenyl)phosphato-κO]chloridotetrakis(methanol-κO)lutetium methanol disolvate (mol-2) top
Crystal data top
[Lu(C24H34O4P)Cl(CH4O)4]·2CH4OF(000) = 2584
Mr = 1237.63Dx = 1.328 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 16.877 (2) ÅCell parameters from 9984 reflections
b = 12.4430 (17) Åθ = 2.3–31.0°
c = 30.404 (4) ŵ = 1.75 mm1
β = 104.231 (2)°T = 183 K
V = 6188.7 (14) Å3Block, colourless
Z = 40.40 × 0.30 × 0.20 mm
Data collection top
Bruker APEXII CCD area detector
diffractometer
9435 independent reflections
Radiation source: fine-focus sealed tube8726 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
ω scansθmax = 30.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 2424
Tmin = 0.598, Tmax = 0.746k = 1617
34787 measured reflectionsl = 4343
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)] = 0.025Hydrogen site location: mixed
wR(F2) = 0.060H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0306P)2 + 4.4502P]
where P = (Fo2 + 2Fc2)/3
9435 reflections(Δ/σ)max = 0.001
349 parametersΔρmax = 1.60 e Å3
0 restraintsΔρmin = 0.56 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Lu10.50000.27331 (2)0.25000.01894 (3)
Cl10.50000.06577 (6)0.25000.04011 (17)
P10.57599 (2)0.35892 (3)0.15781 (2)0.01550 (7)
O10.52081 (7)0.30155 (10)0.18227 (4)0.0196 (2)
O20.62729 (7)0.44428 (10)0.18532 (4)0.0214 (2)
O30.63575 (7)0.27857 (9)0.14152 (4)0.0178 (2)
O40.52451 (6)0.40023 (9)0.10993 (4)0.0178 (2)
O50.58606 (9)0.42266 (12)0.26209 (5)0.0328 (3)
O60.63500 (9)0.21233 (15)0.27708 (6)0.0415 (4)
H280.6041 (15)0.437 (2)0.2402 (9)0.041 (7)*
H290.639 (2)0.150 (3)0.2807 (11)0.067 (10)*
C10.61884 (9)0.22505 (13)0.09938 (5)0.0184 (3)
C20.58992 (10)0.11990 (14)0.09761 (6)0.0233 (3)
C30.57913 (11)0.06614 (16)0.05620 (7)0.0302 (4)
H3A0.55990.00590.05370.036*
C40.59593 (11)0.11583 (17)0.01892 (6)0.0313 (4)
H4A0.58810.07790.00890.038*
C50.62410 (11)0.22061 (15)0.02191 (6)0.0270 (4)
H5A0.63470.25410.00410.032*
C60.63721 (10)0.27816 (13)0.06252 (6)0.0205 (3)
C70.57380 (12)0.06466 (15)0.13896 (7)0.0310 (4)
H7A0.56860.12170.16120.037*
C80.64584 (17)0.0060 (3)0.16121 (10)0.0602 (8)
H8A0.69500.03840.17090.090*
H8B0.65460.06000.13940.090*
H8C0.63440.04210.18760.090*
C90.49465 (16)0.0001 (2)0.12809 (10)0.0518 (6)
H9A0.44850.04820.11590.078*
H9B0.48730.03430.15580.078*
H9C0.49730.05510.10550.078*
C100.67092 (10)0.39178 (14)0.06518 (6)0.0242 (3)
H10A0.67260.42120.09600.029*
C110.75824 (13)0.39148 (19)0.05874 (9)0.0450 (6)
H11A0.79350.34830.08270.067*
H11B0.77890.46530.06030.067*
H11C0.75810.36060.02910.067*
C120.61709 (14)0.46514 (18)0.02994 (7)0.0381 (5)
H12A0.56100.46340.03350.057*
H12B0.61770.44030.00060.057*
H12C0.63810.53880.03420.057*
C130.45207 (9)0.46085 (13)0.10294 (5)0.0188 (3)
C140.37799 (10)0.40483 (15)0.09039 (5)0.0227 (3)
C150.30717 (11)0.46667 (17)0.08227 (6)0.0303 (4)
H15A0.25550.43210.07350.036*
C160.31032 (11)0.57745 (17)0.08661 (7)0.0329 (4)
H16A0.26110.61770.08170.039*
C170.38444 (11)0.62933 (16)0.09806 (6)0.0283 (4)
H17A0.38570.70540.10060.034*
C180.45806 (10)0.57233 (14)0.10608 (5)0.0215 (3)
C190.37623 (12)0.28394 (15)0.08430 (6)0.0280 (4)
H19A0.42350.25370.10750.034*
C200.29859 (17)0.2315 (2)0.09182 (11)0.0539 (7)
H20A0.29070.25330.12140.081*
H20B0.30390.15310.09100.081*
H20C0.25140.25440.06780.081*
C210.38881 (18)0.2552 (2)0.03770 (8)0.0458 (6)
H21A0.44030.28650.03430.069*
H21B0.34330.28370.01410.069*
H21C0.39090.17690.03480.069*
C220.53887 (11)0.63281 (15)0.11673 (6)0.0273 (4)
H22A0.58380.57900.11950.033*
C230.55262 (14)0.69317 (18)0.16187 (7)0.0389 (5)
H23A0.55720.64140.18670.058*
H23B0.50640.74140.16110.058*
H23C0.60310.73530.16680.058*
C240.54288 (14)0.71036 (16)0.07811 (8)0.0367 (4)
H24A0.53350.67050.04950.055*
H24B0.59690.74430.08450.055*
H24C0.50080.76580.07570.055*
C250.60128 (17)0.5111 (2)0.29211 (8)0.0484 (6)
H25A0.63940.56060.28290.073*
H25B0.62510.48550.32300.073*
H25C0.54980.54850.29120.073*
C260.71452 (16)0.2524 (3)0.27804 (15)0.0772 (11)
H26A0.75580.20510.29680.116*
H26B0.72040.32500.29090.116*
H26C0.72200.25460.24710.116*
H300.749 (2)0.502 (3)0.1938 (12)0.071 (11)*
O70.79287 (13)0.5056 (2)0.19924 (10)0.0781 (8)
C270.83015 (17)0.4058 (3)0.19658 (12)0.0699 (9)
H27A0.87880.41600.18490.105*
H27B0.79160.35830.17610.105*
H27C0.84610.37340.22690.105*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Lu10.01740 (5)0.02530 (6)0.01526 (5)0.0000.00620 (3)0.000
Cl10.0283 (3)0.0263 (3)0.0599 (5)0.0000.0003 (3)0.000
P10.01604 (17)0.01654 (18)0.01452 (16)0.00219 (13)0.00488 (13)0.00021 (13)
O10.0200 (5)0.0227 (6)0.0172 (5)0.0005 (4)0.0069 (4)0.0003 (4)
O20.0226 (5)0.0216 (6)0.0201 (5)0.0024 (4)0.0054 (4)0.0027 (4)
O30.0170 (5)0.0195 (6)0.0170 (5)0.0048 (4)0.0048 (4)0.0001 (4)
O40.0174 (5)0.0207 (5)0.0162 (5)0.0066 (4)0.0054 (4)0.0024 (4)
O50.0422 (8)0.0361 (8)0.0253 (6)0.0133 (6)0.0181 (6)0.0115 (6)
O60.0183 (6)0.0433 (10)0.0590 (11)0.0006 (6)0.0022 (6)0.0116 (8)
C10.0174 (7)0.0199 (7)0.0184 (7)0.0055 (6)0.0056 (5)0.0016 (6)
C20.0216 (7)0.0218 (8)0.0283 (8)0.0030 (6)0.0097 (6)0.0017 (6)
C30.0274 (8)0.0274 (9)0.0365 (10)0.0007 (7)0.0092 (7)0.0093 (7)
C40.0281 (9)0.0386 (11)0.0259 (8)0.0035 (8)0.0042 (7)0.0117 (8)
C50.0289 (8)0.0348 (10)0.0183 (7)0.0093 (7)0.0078 (6)0.0005 (7)
C60.0193 (7)0.0230 (8)0.0204 (7)0.0077 (6)0.0070 (6)0.0023 (6)
C70.0425 (10)0.0214 (9)0.0351 (10)0.0009 (7)0.0207 (8)0.0000 (7)
C80.0534 (15)0.074 (2)0.0559 (16)0.0112 (14)0.0179 (12)0.0342 (14)
C90.0532 (14)0.0409 (13)0.0693 (17)0.0126 (11)0.0305 (13)0.0046 (12)
C100.0279 (8)0.0220 (8)0.0270 (8)0.0058 (6)0.0148 (7)0.0038 (6)
C110.0355 (11)0.0324 (11)0.0765 (17)0.0007 (9)0.0319 (11)0.0011 (11)
C120.0535 (13)0.0317 (11)0.0328 (10)0.0142 (9)0.0181 (9)0.0119 (8)
C130.0180 (7)0.0227 (8)0.0162 (6)0.0062 (6)0.0054 (5)0.0015 (6)
C140.0207 (7)0.0281 (9)0.0188 (7)0.0022 (6)0.0039 (6)0.0011 (6)
C150.0190 (8)0.0416 (11)0.0297 (9)0.0044 (7)0.0047 (6)0.0035 (8)
C160.0242 (8)0.0417 (11)0.0328 (9)0.0156 (8)0.0069 (7)0.0052 (8)
C170.0300 (9)0.0271 (9)0.0279 (8)0.0132 (7)0.0071 (7)0.0039 (7)
C180.0226 (7)0.0223 (8)0.0194 (7)0.0062 (6)0.0050 (6)0.0028 (6)
C190.0265 (8)0.0277 (10)0.0271 (8)0.0029 (7)0.0012 (7)0.0009 (7)
C200.0454 (14)0.0444 (14)0.0750 (19)0.0178 (11)0.0211 (13)0.0049 (13)
C210.0628 (16)0.0391 (12)0.0347 (11)0.0053 (11)0.0105 (11)0.0088 (9)
C220.0259 (8)0.0199 (8)0.0347 (9)0.0018 (6)0.0048 (7)0.0041 (7)
C230.0438 (11)0.0295 (10)0.0376 (11)0.0027 (9)0.0009 (9)0.0006 (8)
C240.0407 (11)0.0265 (10)0.0447 (12)0.0002 (8)0.0139 (9)0.0083 (8)
C250.0684 (16)0.0495 (14)0.0319 (11)0.0237 (12)0.0208 (11)0.0170 (10)
C260.0217 (11)0.085 (2)0.121 (3)0.0053 (12)0.0088 (15)0.033 (2)
O70.0346 (10)0.0710 (15)0.127 (2)0.0237 (10)0.0163 (12)0.0267 (14)
C270.0434 (14)0.077 (2)0.093 (2)0.0219 (14)0.0234 (15)0.0326 (18)
Geometric parameters (Å, º) top
Lu1—O1i2.2005 (11)C12—H12A0.9800
Lu1—O12.2006 (11)C12—H12B0.9800
Lu1—O5i2.3314 (14)C12—H12C0.9800
Lu1—O52.3314 (14)C13—C181.392 (2)
Lu1—O62.3499 (15)C13—C141.400 (2)
Lu1—O6i2.3499 (15)C14—C151.392 (2)
Lu1—Cl12.5824 (8)C14—C191.515 (3)
P1—O21.4903 (12)C15—C161.384 (3)
P1—O11.5069 (12)C15—H15A0.9500
P1—O31.5836 (11)C16—C171.374 (3)
P1—O41.5862 (11)C16—H16A0.9500
O3—C11.4093 (19)C17—C181.399 (2)
O4—C131.4074 (18)C17—H17A0.9500
O5—C251.412 (2)C18—C221.521 (2)
O5—H280.82 (3)C19—C211.526 (3)
O6—C261.425 (3)C19—C201.531 (3)
O6—H290.79 (3)C19—H19A1.0000
C1—C21.393 (2)C20—H20A0.9800
C1—C61.400 (2)C20—H20B0.9800
C2—C31.398 (2)C20—H20C0.9800
C2—C71.515 (3)C21—H21A0.9800
C3—C41.380 (3)C21—H21B0.9800
C3—H3A0.9500C21—H21C0.9800
C4—C51.383 (3)C22—C231.531 (3)
C4—H4A0.9500C22—C241.534 (3)
C5—C61.397 (2)C22—H22A1.0000
C5—H5A0.9500C23—H23A0.9800
C6—C101.519 (3)C23—H23B0.9800
C7—C81.518 (3)C23—H23C0.9800
C7—C91.524 (3)C24—H24A0.9800
C7—H7A1.0000C24—H24B0.9800
C8—H8A0.9800C24—H24C0.9800
C8—H8B0.9800C25—H25A0.9800
C8—H8C0.9800C25—H25B0.9800
C9—H9A0.9800C25—H25C0.9800
C9—H9B0.9800C26—H26A0.9800
C9—H9C0.9800C26—H26B0.9800
C10—C121.526 (3)C26—H26C0.9800
C10—C111.534 (3)O7—C271.403 (4)
C10—H10A1.0000O7—H300.71 (3)
C11—H11A0.9800C27—H27A0.9800
C11—H11B0.9800C27—H27B0.9800
C11—H11C0.9800C27—H27C0.9800
O1i—Lu1—O1161.62 (6)H11A—C11—H11C109.5
O1i—Lu1—O5i77.51 (5)H11B—C11—H11C109.5
O1—Lu1—O5i87.81 (4)C10—C12—H12A109.5
O1i—Lu1—O587.81 (4)C10—C12—H12B109.5
O1—Lu1—O577.51 (5)H12A—C12—H12B109.5
O5i—Lu1—O574.29 (8)C10—C12—H12C109.5
O1i—Lu1—O695.03 (6)H12A—C12—H12C109.5
O1—Lu1—O690.88 (6)H12B—C12—H12C109.5
O5i—Lu1—O6145.62 (6)C18—C13—C14124.03 (15)
O5—Lu1—O671.90 (6)C18—C13—O4118.54 (14)
O1i—Lu1—O6i90.88 (6)C14—C13—O4117.30 (14)
O1—Lu1—O6i95.03 (6)C15—C14—C13116.33 (17)
O5i—Lu1—O6i71.90 (6)C15—C14—C19122.49 (16)
O5—Lu1—O6i145.63 (6)C13—C14—C19121.13 (15)
O6—Lu1—O6i142.32 (9)C16—C15—C14121.51 (17)
O1i—Lu1—Cl199.19 (3)C16—C15—H15A119.2
O1—Lu1—Cl199.19 (3)C14—C15—H15A119.2
O5i—Lu1—Cl1142.85 (4)C17—C16—C15120.20 (16)
O5—Lu1—Cl1142.85 (4)C17—C16—H16A119.9
O6—Lu1—Cl171.16 (4)C15—C16—H16A119.9
O6i—Lu1—Cl171.16 (4)C16—C17—C18121.34 (18)
O2—P1—O1113.88 (7)C16—C17—H17A119.3
O2—P1—O3107.38 (7)C18—C17—H17A119.3
O1—P1—O3111.94 (7)C13—C18—C17116.54 (16)
O2—P1—O4113.31 (7)C13—C18—C22123.61 (14)
O1—P1—O4109.93 (6)C17—C18—C22119.84 (16)
O3—P1—O499.49 (6)C14—C19—C21110.07 (17)
P1—O1—Lu1142.91 (7)C14—C19—C20113.40 (18)
C1—O3—P1125.48 (10)C21—C19—C20111.0 (2)
C13—O4—P1124.87 (9)C14—C19—H19A107.4
C25—O5—Lu1136.90 (13)C21—C19—H19A107.4
C25—O5—H28108.5 (18)C20—C19—H19A107.4
Lu1—O5—H28112.5 (18)C19—C20—H20A109.5
C26—O6—Lu1136.16 (17)C19—C20—H20B109.5
C26—O6—H29107 (2)H20A—C20—H20B109.5
Lu1—O6—H29115 (2)C19—C20—H20C109.5
C2—C1—C6123.84 (15)H20A—C20—H20C109.5
C2—C1—O3118.01 (14)H20B—C20—H20C109.5
C6—C1—O3118.00 (14)C19—C21—H21A109.5
C1—C2—C3116.82 (16)C19—C21—H21B109.5
C1—C2—C7121.79 (15)H21A—C21—H21B109.5
C3—C2—C7121.35 (17)C19—C21—H21C109.5
C4—C3—C2121.19 (18)H21A—C21—H21C109.5
C4—C3—H3A119.4H21B—C21—H21C109.5
C2—C3—H3A119.4C18—C22—C23111.34 (16)
C3—C4—C5120.33 (17)C18—C22—C24110.75 (15)
C3—C4—H4A119.8C23—C22—C24110.60 (17)
C5—C4—H4A119.8C18—C22—H22A108.0
C4—C5—C6121.22 (17)C23—C22—H22A108.0
C4—C5—H5A119.4C24—C22—H22A108.0
C6—C5—H5A119.4C22—C23—H23A109.5
C5—C6—C1116.59 (16)C22—C23—H23B109.5
C5—C6—C10120.00 (15)H23A—C23—H23B109.5
C1—C6—C10123.41 (15)C22—C23—H23C109.5
C2—C7—C8110.18 (17)H23A—C23—H23C109.5
C2—C7—C9112.69 (18)H23B—C23—H23C109.5
C8—C7—C9110.8 (2)C22—C24—H24A109.5
C2—C7—H7A107.7C22—C24—H24B109.5
C8—C7—H7A107.7H24A—C24—H24B109.5
C9—C7—H7A107.7C22—C24—H24C109.5
C7—C8—H8A109.5H24A—C24—H24C109.5
C7—C8—H8B109.5H24B—C24—H24C109.5
H8A—C8—H8B109.5O5—C25—H25A109.5
C7—C8—H8C109.5O5—C25—H25B109.5
H8A—C8—H8C109.5H25A—C25—H25B109.5
H8B—C8—H8C109.5O5—C25—H25C109.5
C7—C9—H9A109.5H25A—C25—H25C109.5
C7—C9—H9B109.5H25B—C25—H25C109.5
H9A—C9—H9B109.5O6—C26—H26A109.5
C7—C9—H9C109.5O6—C26—H26B109.5
H9A—C9—H9C109.5H26A—C26—H26B109.5
H9B—C9—H9C109.5O6—C26—H26C109.5
C6—C10—C12111.65 (16)H26A—C26—H26C109.5
C6—C10—C11110.49 (15)H26B—C26—H26C109.5
C12—C10—C11109.68 (17)C27—O7—H30112 (3)
C6—C10—H10A108.3O7—C27—H27A109.5
C12—C10—H10A108.3O7—C27—H27B109.5
C11—C10—H10A108.3H27A—C27—H27B109.5
C10—C11—H11A109.5O7—C27—H27C109.5
C10—C11—H11B109.5H27A—C27—H27C109.5
H11A—C11—H11B109.5H27B—C27—H27C109.5
C10—C11—H11C109.5
O2—P1—O1—Lu116.05 (15)C5—C6—C10—C1257.2 (2)
O3—P1—O1—Lu1106.00 (12)C1—C6—C10—C12123.72 (17)
O4—P1—O1—Lu1144.42 (11)C5—C6—C10—C1165.2 (2)
O2—P1—O3—C1144.58 (12)C1—C6—C10—C11113.93 (19)
O1—P1—O3—C189.72 (13)P1—O4—C13—C1887.82 (16)
O4—P1—O3—C126.38 (13)P1—O4—C13—C1496.11 (16)
O2—P1—O4—C1377.73 (14)C18—C13—C14—C152.2 (2)
O1—P1—O4—C1350.96 (14)O4—C13—C14—C15178.05 (14)
O3—P1—O4—C13168.58 (12)C18—C13—C14—C19175.42 (15)
P1—O3—C1—C297.08 (16)O4—C13—C14—C190.4 (2)
P1—O3—C1—C687.07 (16)C13—C14—C15—C160.2 (3)
C6—C1—C2—C30.0 (2)C19—C14—C15—C16177.84 (17)
O3—C1—C2—C3175.62 (14)C14—C15—C16—C171.7 (3)
C6—C1—C2—C7177.78 (16)C15—C16—C17—C180.7 (3)
O3—C1—C2—C72.2 (2)C14—C13—C18—C173.1 (2)
C1—C2—C3—C40.5 (3)O4—C13—C18—C17178.87 (14)
C7—C2—C3—C4178.29 (17)C14—C13—C18—C22175.83 (16)
C2—C3—C4—C50.1 (3)O4—C13—C18—C220.1 (2)
C3—C4—C5—C60.8 (3)C16—C17—C18—C131.5 (3)
C4—C5—C6—C11.2 (3)C16—C17—C18—C22177.42 (17)
C4—C5—C6—C10177.92 (16)C15—C14—C19—C2196.5 (2)
C2—C1—C6—C50.9 (2)C13—C14—C19—C2181.0 (2)
O3—C1—C6—C5176.45 (14)C15—C14—C19—C2028.5 (3)
C2—C1—C6—C10178.26 (15)C13—C14—C19—C20154.03 (19)
O3—C1—C6—C102.7 (2)C13—C18—C22—C23116.08 (18)
C1—C2—C7—C898.0 (2)C17—C18—C22—C2365.0 (2)
C3—C2—C7—C879.8 (2)C13—C18—C22—C24120.41 (18)
C1—C2—C7—C9137.75 (19)C17—C18—C22—C2458.5 (2)
C3—C2—C7—C944.5 (2)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H28···O20.82 (3)1.81 (3)2.6082 (18)167 (3)
O7—H30···O20.71 (3)2.14 (4)2.826 (2)163 (4)
O6—H29···O7ii0.79 (3)2.13 (3)2.861 (3)153 (3)
O6—H29···Cl10.79 (3)2.53 (3)2.8761 (17)108 (3)
Symmetry code: (ii) x+3/2, y1/2, z+1/2.
Bis[bis(2,6-diisopropylphenyl)phosphato-κO]chloridotetrakis(methanol-κO)yttrium methanol disolvate (mol-3) top
Crystal data top
[Y(C24H34O4P)Cl(CH4O)4]·2CH4OF(000) = 2456
Mr = 1151.57Dx = 1.242 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 16.9203 (5) ÅCell parameters from 8624 reflections
b = 12.3877 (4) Åθ = 2.3–32.1°
c = 30.3676 (10) ŵ = 1.10 mm1
β = 104.708 (1)°T = 100 K
V = 6156.6 (3) Å3Prism, colourless
Z = 40.25 × 0.21 × 0.20 mm
Data collection top
Bruker APEXII CCD area detector
diffractometer
11155 independent reflections
Radiation source: fine-focus sealed tube8714 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ω scansθmax = 32.6°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 2525
Tmin = 0.692, Tmax = 0.889k = 1816
36276 measured reflectionsl = 4645
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)] = 0.039Hydrogen site location: mixed
wR(F2) = 0.095H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0472P)2 + 2.7232P]
where P = (Fo2 + 2Fc2)/3
11155 reflections(Δ/σ)max = 0.001
349 parametersΔρmax = 0.57 e Å3
0 restraintsΔρmin = 0.37 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Y10.50000.26657 (2)0.25000.01333 (5)
Cl10.50000.05508 (5)0.25000.02981 (13)
P10.57755 (2)0.35767 (3)0.15767 (2)0.01065 (7)
O10.52252 (6)0.29814 (8)0.18154 (3)0.01332 (18)
O20.62830 (6)0.44344 (8)0.18592 (3)0.01494 (19)
O30.63810 (6)0.27813 (8)0.14144 (3)0.01214 (18)
O40.52584 (6)0.39971 (8)0.10950 (3)0.01245 (18)
O50.58771 (7)0.41957 (10)0.26299 (4)0.0237 (2)
O60.63698 (7)0.20442 (12)0.27763 (5)0.0301 (3)
H280.6050 (14)0.435 (2)0.2416 (9)0.050 (7)*
H290.6397 (16)0.141 (2)0.2803 (9)0.052 (8)*
C10.62062 (8)0.22403 (12)0.09920 (4)0.0128 (2)
C20.59191 (8)0.11795 (12)0.09750 (5)0.0156 (3)
C30.58070 (9)0.06367 (13)0.05590 (5)0.0192 (3)
H3A0.56210.00900.05350.023*
C40.59628 (9)0.11397 (14)0.01815 (5)0.0202 (3)
H4A0.58790.07600.00980.024*
C50.62403 (9)0.21961 (13)0.02129 (5)0.0176 (3)
H5A0.63390.25350.00490.021*
C60.63790 (8)0.27757 (12)0.06209 (4)0.0135 (2)
C70.57672 (10)0.06253 (13)0.13906 (5)0.0207 (3)
H7A0.57370.11970.16180.025*
C80.64827 (12)0.01193 (17)0.16068 (7)0.0361 (4)
H8A0.69900.03010.16870.054*
H8B0.65290.06860.13900.054*
H8C0.63870.04500.18820.054*
C90.49583 (11)0.00049 (15)0.12823 (7)0.0326 (4)
H9A0.45090.04970.11460.049*
H9B0.48690.02990.15640.049*
H9C0.49790.05800.10680.049*
C100.67141 (8)0.39198 (12)0.06482 (5)0.0159 (3)
H10A0.67400.42130.09580.019*
C110.75802 (10)0.39201 (15)0.05785 (7)0.0292 (4)
H11A0.79390.34810.08160.044*
H11B0.77870.46620.05970.044*
H11C0.75680.36180.02790.044*
C120.61588 (11)0.46586 (14)0.02939 (5)0.0241 (3)
H12A0.56050.46520.03390.036*
H12B0.61430.43980.00130.036*
H12C0.63740.53970.03300.036*
C130.45330 (8)0.46036 (12)0.10258 (4)0.0128 (2)
C140.37897 (8)0.40381 (12)0.08994 (4)0.0145 (3)
C150.30775 (9)0.46539 (13)0.08159 (5)0.0190 (3)
H15A0.25620.43030.07280.023*
C160.31065 (9)0.57709 (14)0.08588 (5)0.0206 (3)
H16A0.26140.61740.08070.025*
C170.38518 (9)0.62952 (13)0.09774 (5)0.0182 (3)
H17A0.38640.70590.10040.022*
C180.45899 (8)0.57257 (12)0.10587 (4)0.0142 (2)
C190.37752 (9)0.28185 (12)0.08412 (5)0.0181 (3)
H19A0.42490.25170.10760.022*
C200.29968 (11)0.22990 (16)0.09148 (7)0.0346 (4)
H20A0.29090.25450.12050.052*
H20B0.30550.15120.09200.052*
H20C0.25290.25070.06660.052*
C210.38949 (12)0.25205 (14)0.03727 (6)0.0294 (4)
H21A0.44100.28280.03390.044*
H21B0.34400.28090.01340.044*
H21C0.39110.17330.03450.044*
C220.53968 (9)0.63343 (12)0.11692 (5)0.0179 (3)
H22A0.58470.57950.12000.022*
C230.55315 (10)0.69441 (14)0.16214 (6)0.0248 (3)
H23A0.55720.64260.18700.037*
H23B0.50700.74320.16090.037*
H23C0.60380.73640.16740.037*
C240.54354 (10)0.71121 (13)0.07811 (6)0.0229 (3)
H24A0.53280.67130.04930.034*
H24B0.59800.74400.08430.034*
H24C0.50230.76790.07590.034*
C250.59930 (12)0.51119 (15)0.29229 (6)0.0290 (4)
H25A0.63920.56000.28450.043*
H25B0.61940.48760.32400.043*
H25C0.54720.54910.28860.043*
C260.71665 (12)0.2457 (2)0.27909 (11)0.0575 (7)
H26A0.75810.19600.29640.086*
H26B0.72340.31660.29380.086*
H26C0.72300.25250.24800.086*
H300.7472 (17)0.494 (2)0.1956 (10)0.060 (8)*
O70.79371 (9)0.49959 (14)0.19830 (7)0.0537 (5)
C270.83070 (12)0.3975 (2)0.19620 (8)0.0456 (5)
H27A0.88270.40750.18810.068*
H27B0.79430.35260.17320.068*
H27C0.84070.36200.22590.068*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.01262 (8)0.01651 (10)0.01154 (8)0.0000.00433 (6)0.000
Cl10.0216 (2)0.0176 (3)0.0438 (3)0.0000.0034 (2)0.000
P10.01099 (14)0.01092 (16)0.01046 (14)0.00132 (12)0.00350 (11)0.00023 (11)
O10.0134 (4)0.0156 (5)0.0117 (4)0.0010 (4)0.0047 (3)0.0006 (4)
O20.0152 (4)0.0147 (5)0.0151 (4)0.0017 (4)0.0042 (4)0.0021 (4)
O30.0121 (4)0.0130 (5)0.0114 (4)0.0029 (4)0.0031 (3)0.0007 (3)
O40.0120 (4)0.0135 (5)0.0123 (4)0.0046 (4)0.0040 (3)0.0017 (3)
O50.0322 (6)0.0241 (6)0.0189 (5)0.0106 (5)0.0141 (5)0.0089 (4)
O60.0137 (5)0.0299 (7)0.0439 (8)0.0008 (5)0.0023 (5)0.0083 (6)
C10.0118 (5)0.0140 (6)0.0130 (5)0.0037 (5)0.0038 (4)0.0012 (5)
C20.0145 (6)0.0137 (7)0.0202 (6)0.0012 (5)0.0073 (5)0.0013 (5)
C30.0181 (6)0.0167 (7)0.0233 (7)0.0020 (6)0.0063 (5)0.0064 (6)
C40.0171 (6)0.0255 (8)0.0175 (6)0.0034 (6)0.0034 (5)0.0072 (6)
C50.0180 (6)0.0218 (8)0.0131 (6)0.0058 (6)0.0044 (5)0.0010 (5)
C60.0121 (5)0.0151 (7)0.0138 (5)0.0044 (5)0.0044 (4)0.0011 (5)
C70.0298 (8)0.0130 (7)0.0235 (7)0.0013 (6)0.0145 (6)0.0001 (5)
C80.0337 (10)0.0400 (11)0.0343 (9)0.0037 (8)0.0080 (8)0.0166 (8)
C90.0323 (9)0.0241 (9)0.0473 (11)0.0048 (7)0.0209 (8)0.0048 (8)
C100.0172 (6)0.0153 (7)0.0176 (6)0.0038 (5)0.0088 (5)0.0028 (5)
C110.0237 (8)0.0197 (8)0.0504 (11)0.0014 (7)0.0208 (7)0.0003 (8)
C120.0335 (8)0.0200 (8)0.0218 (7)0.0092 (7)0.0124 (6)0.0080 (6)
C130.0119 (5)0.0158 (7)0.0112 (5)0.0040 (5)0.0037 (4)0.0011 (5)
C140.0136 (6)0.0169 (7)0.0129 (5)0.0004 (5)0.0029 (4)0.0005 (5)
C150.0122 (6)0.0258 (8)0.0180 (6)0.0018 (6)0.0018 (5)0.0003 (6)
C160.0152 (6)0.0259 (8)0.0204 (7)0.0089 (6)0.0039 (5)0.0030 (6)
C170.0200 (7)0.0157 (7)0.0189 (6)0.0066 (5)0.0046 (5)0.0022 (5)
C180.0143 (6)0.0145 (7)0.0135 (6)0.0033 (5)0.0032 (5)0.0019 (5)
C190.0173 (6)0.0174 (7)0.0173 (6)0.0024 (5)0.0004 (5)0.0013 (5)
C200.0297 (9)0.0280 (9)0.0475 (11)0.0111 (8)0.0124 (8)0.0037 (8)
C210.0411 (10)0.0241 (9)0.0222 (7)0.0037 (7)0.0065 (7)0.0045 (6)
C220.0174 (6)0.0130 (7)0.0224 (7)0.0011 (5)0.0032 (5)0.0022 (5)
C230.0285 (8)0.0177 (7)0.0243 (7)0.0022 (6)0.0003 (6)0.0005 (6)
C240.0253 (7)0.0170 (8)0.0278 (8)0.0001 (6)0.0091 (6)0.0048 (6)
C250.0412 (10)0.0274 (9)0.0206 (7)0.0102 (8)0.0122 (7)0.0109 (6)
C260.0153 (8)0.0597 (16)0.093 (2)0.0042 (9)0.0059 (10)0.0226 (14)
O70.0234 (7)0.0484 (10)0.0892 (14)0.0156 (7)0.0139 (8)0.0216 (9)
C270.0306 (10)0.0488 (14)0.0597 (14)0.0129 (10)0.0157 (9)0.0198 (11)
Geometric parameters (Å, º) top
Y1—O1i2.2411 (9)C12—H12A0.9800
Y1—O12.2411 (9)C12—H12B0.9800
Y1—O52.3776 (12)C12—H12C0.9800
Y1—O5i2.3776 (12)C13—C181.395 (2)
Y1—O62.3835 (12)C13—C141.4052 (19)
Y1—O6i2.3835 (12)C14—C151.394 (2)
Y1—Cl12.6199 (6)C14—C191.520 (2)
P1—O21.4927 (10)C15—C161.390 (2)
P1—O11.5095 (10)C15—H15A0.9500
P1—O31.5873 (10)C16—C171.382 (2)
P1—O41.5895 (10)C16—H16A0.9500
O3—C11.4104 (16)C17—C181.4006 (19)
O4—C131.4087 (16)C17—H17A0.9500
O5—C251.4247 (19)C18—C221.521 (2)
O5—H280.80 (3)C19—C201.532 (2)
O6—C261.432 (2)C19—C211.532 (2)
O6—H290.79 (3)C19—H19A1.0000
C1—C21.397 (2)C20—H20A0.9800
C1—C61.4011 (19)C20—H20B0.9800
C2—C31.401 (2)C20—H20C0.9800
C2—C71.515 (2)C21—H21A0.9800
C3—C41.388 (2)C21—H21B0.9800
C3—H3A0.9500C21—H21C0.9800
C4—C51.385 (2)C22—C231.533 (2)
C4—H4A0.9500C22—C241.537 (2)
C5—C61.3993 (19)C22—H22A1.0000
C5—H5A0.9500C23—H23A0.9800
C6—C101.521 (2)C23—H23B0.9800
C7—C91.531 (2)C23—H23C0.9800
C7—C81.531 (2)C24—H24A0.9800
C7—H7A1.0000C24—H24B0.9800
C8—H8A0.9800C24—H24C0.9800
C8—H8B0.9800C25—H25A0.9800
C8—H8C0.9800C25—H25B0.9800
C9—H9A0.9800C25—H25C0.9800
C9—H9B0.9800C26—H26A0.9800
C9—H9C0.9800C26—H26B0.9800
C10—C111.533 (2)C26—H26C0.9800
C10—C121.538 (2)O7—C271.420 (3)
C10—H10A1.0000O7—H300.77 (3)
C11—H11A0.9800C27—H27A0.9800
C11—H11B0.9800C27—H27B0.9800
C11—H11C0.9800C27—H27C0.9800
O1i—Y1—O1159.90 (5)H11A—C11—H11C109.5
O1i—Y1—O587.30 (4)H11B—C11—H11C109.5
O1—Y1—O576.64 (4)C10—C12—H12A109.5
O1i—Y1—O5i76.64 (4)C10—C12—H12B109.5
O1—Y1—O5i87.30 (4)H12A—C12—H12B109.5
O5—Y1—O5i74.29 (6)C10—C12—H12C109.5
O1i—Y1—O696.26 (4)H12A—C12—H12C109.5
O1—Y1—O690.21 (4)H12B—C12—H12C109.5
O5—Y1—O671.87 (5)C18—C13—C14123.85 (12)
O5i—Y1—O6145.71 (5)C18—C13—O4118.62 (12)
O1i—Y1—O6i90.21 (4)C14—C13—O4117.41 (12)
O1—Y1—O6i96.26 (4)C15—C14—C13116.69 (14)
O5—Y1—O6i145.71 (5)C15—C14—C19122.34 (13)
O5i—Y1—O6i71.87 (5)C13—C14—C19120.93 (12)
O6—Y1—O6i142.30 (7)C16—C15—C14121.31 (14)
O1i—Y1—Cl1100.05 (3)C16—C15—H15A119.3
O1—Y1—Cl1100.05 (3)C14—C15—H15A119.3
O5—Y1—Cl1142.86 (3)C17—C16—C15120.02 (13)
O5i—Y1—Cl1142.86 (3)C17—C16—H16A120.0
O6—Y1—Cl171.15 (4)C15—C16—H16A120.0
O6i—Y1—Cl171.15 (4)C16—C17—C18121.53 (14)
O2—P1—O1114.01 (6)C16—C17—H17A119.2
O2—P1—O3107.32 (5)C18—C17—H17A119.2
O1—P1—O3111.79 (6)C13—C18—C17116.54 (13)
O2—P1—O4113.42 (6)C13—C18—C22123.47 (12)
O1—P1—O4109.84 (5)C17—C18—C22119.98 (13)
O3—P1—O499.53 (5)C14—C19—C20112.92 (13)
P1—O1—Y1143.28 (6)C14—C19—C21110.20 (13)
C1—O3—P1125.06 (8)C20—C19—C21110.81 (14)
C13—O4—P1124.56 (8)C14—C19—H19A107.6
C25—O5—Y1136.04 (10)C20—C19—H19A107.6
C25—O5—H28107.6 (18)C21—C19—H19A107.6
Y1—O5—H28113.1 (18)C19—C20—H20A109.5
C26—O6—Y1136.00 (13)C19—C20—H20B109.5
C26—O6—H29108.8 (19)H20A—C20—H20B109.5
Y1—O6—H29112.6 (19)C19—C20—H20C109.5
C2—C1—C6123.85 (13)H20A—C20—H20C109.5
C2—C1—O3118.10 (12)H20B—C20—H20C109.5
C6—C1—O3117.93 (12)C19—C21—H21A109.5
C1—C2—C3116.80 (13)C19—C21—H21B109.5
C1—C2—C7121.76 (13)H21A—C21—H21B109.5
C3—C2—C7121.40 (14)C19—C21—H21C109.5
C4—C3—C2121.26 (14)H21A—C21—H21C109.5
C4—C3—H3A119.4H21B—C21—H21C109.5
C2—C3—H3A119.4C18—C22—C23111.28 (13)
C5—C4—C3119.97 (13)C18—C22—C24110.62 (12)
C5—C4—H4A120.0C23—C22—C24110.64 (13)
C3—C4—H4A120.0C18—C22—H22A108.1
C4—C5—C6121.54 (13)C23—C22—H22A108.1
C4—C5—H5A119.2C24—C22—H22A108.1
C6—C5—H5A119.2C22—C23—H23A109.5
C5—C6—C1116.56 (13)C22—C23—H23B109.5
C5—C6—C10120.18 (12)H23A—C23—H23B109.5
C1—C6—C10123.25 (12)C22—C23—H23C109.5
C2—C7—C9112.34 (14)H23A—C23—H23C109.5
C2—C7—C8110.34 (13)H23B—C23—H23C109.5
C9—C7—C8110.87 (14)C22—C24—H24A109.5
C2—C7—H7A107.7C22—C24—H24B109.5
C9—C7—H7A107.7H24A—C24—H24B109.5
C8—C7—H7A107.7C22—C24—H24C109.5
C7—C8—H8A109.5H24A—C24—H24C109.5
C7—C8—H8B109.5H24B—C24—H24C109.5
H8A—C8—H8B109.5O5—C25—H25A109.5
C7—C8—H8C109.5O5—C25—H25B109.5
H8A—C8—H8C109.5H25A—C25—H25B109.5
H8B—C8—H8C109.5O5—C25—H25C109.5
C7—C9—H9A109.5H25A—C25—H25C109.5
C7—C9—H9B109.5H25B—C25—H25C109.5
H9A—C9—H9B109.5O6—C26—H26A109.5
C7—C9—H9C109.5O6—C26—H26B109.5
H9A—C9—H9C109.5H26A—C26—H26B109.5
H9B—C9—H9C109.5O6—C26—H26C109.5
C6—C10—C11110.42 (12)H26A—C26—H26C109.5
C6—C10—C12111.31 (12)H26B—C26—H26C109.5
C11—C10—C12109.81 (13)C27—O7—H30111 (2)
C6—C10—H10A108.4O7—C27—H27A109.5
C11—C10—H10A108.4O7—C27—H27B109.5
C12—C10—H10A108.4H27A—C27—H27B109.5
C10—C11—H11A109.5O7—C27—H27C109.5
C10—C11—H11B109.5H27A—C27—H27C109.5
H11A—C11—H11B109.5H27B—C27—H27C109.5
C10—C11—H11C109.5
O2—P1—O1—Y115.49 (12)C5—C6—C10—C1164.69 (17)
O3—P1—O1—Y1106.46 (10)C1—C6—C10—C11114.25 (15)
O4—P1—O1—Y1144.04 (9)C5—C6—C10—C1257.55 (16)
O2—P1—O3—C1145.88 (10)C1—C6—C10—C12123.51 (14)
O1—P1—O3—C188.41 (11)P1—O4—C13—C1888.17 (14)
O4—P1—O3—C127.55 (11)P1—O4—C13—C1495.67 (13)
O2—P1—O4—C1377.23 (11)C18—C13—C14—C151.8 (2)
O1—P1—O4—C1351.65 (12)O4—C13—C14—C15177.71 (11)
O3—P1—O4—C13169.09 (10)C18—C13—C14—C19176.04 (13)
P1—O3—C1—C296.27 (13)O4—C13—C14—C190.09 (18)
P1—O3—C1—C687.60 (14)C13—C14—C15—C160.4 (2)
C6—C1—C2—C30.3 (2)C19—C14—C15—C16178.13 (13)
O3—C1—C2—C3175.53 (12)C14—C15—C16—C171.3 (2)
C6—C1—C2—C7178.01 (13)C15—C16—C17—C180.3 (2)
O3—C1—C2—C72.13 (19)C14—C13—C18—C172.8 (2)
C1—C2—C3—C41.0 (2)O4—C13—C18—C17178.65 (11)
C7—C2—C3—C4178.65 (13)C14—C13—C18—C22176.36 (13)
C2—C3—C4—C50.5 (2)O4—C13—C18—C220.47 (19)
C3—C4—C5—C60.7 (2)C16—C17—C18—C131.7 (2)
C4—C5—C6—C11.3 (2)C16—C17—C18—C22177.48 (13)
C4—C5—C6—C10177.70 (13)C15—C14—C19—C2028.0 (2)
C2—C1—C6—C50.8 (2)C13—C14—C19—C20154.34 (14)
O3—C1—C6—C5176.65 (11)C15—C14—C19—C2196.53 (17)
C2—C1—C6—C10178.21 (12)C13—C14—C19—C2181.15 (16)
O3—C1—C6—C102.32 (18)C13—C18—C22—C23116.50 (15)
C1—C2—C7—C9135.76 (15)C17—C18—C22—C2364.41 (17)
C3—C2—C7—C946.68 (19)C13—C18—C22—C24120.08 (15)
C1—C2—C7—C899.98 (17)C17—C18—C22—C2459.01 (18)
C3—C2—C7—C877.58 (19)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H28···O20.80 (3)1.83 (3)2.6179 (15)166 (3)
O7—H30···O20.77 (3)2.06 (3)2.8150 (18)168 (3)
O6—H29···O7ii0.79 (3)2.09 (3)2.813 (2)151 (3)
O6—H29···Cl10.79 (3)2.54 (3)2.9173 (14)111 (2)
Symmetry code: (ii) x+3/2, y1/2, z+1/2.
Bis[bis(2,6-diisopropylphenyl)phosphato-κO]tetrakis(methanol-κO)(nitrato-κO)neodymium methanol disolvate (mol-4) top
Crystal data top
[Nd(C24H34O4P)(NO3)(CH4O)4]·2CH4OF(000) = 2596
Mr = 1233.46Dx = 1.308 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 16.7581 (11) ÅCell parameters from 9976 reflections
b = 12.5821 (9) Åθ = 2.3–35.0°
c = 30.732 (2) ŵ = 0.94 mm1
β = 104.876 (1)°T = 100 K
V = 6262.6 (7) Å3Block, pale violet
Z = 40.26 × 0.25 × 0.22 mm
Data collection top
Bruker APEXII CCD area detector
diffractometer
13974 independent reflections
Radiation source: fine-focus sealed tube11131 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω scansθmax = 36.2°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 2727
Tmin = 0.382, Tmax = 0.438k = 1920
36432 measured reflectionsl = 4549
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) = 0.101H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0356P)2 + 12.2862P]
where P = (Fo2 + 2Fc2)/3
13974 reflections(Δ/σ)max = 0.001
416 parametersΔρmax = 1.22 e Å3
15 restraintsΔρmin = 0.86 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Nd10.50000.25296 (2)0.25000.01606 (4)
P10.57732 (3)0.35306 (4)0.15583 (2)0.01383 (8)
O10.52166 (8)0.29444 (11)0.17930 (5)0.0170 (2)
O20.63127 (9)0.43464 (11)0.18456 (5)0.0197 (3)
O30.63628 (8)0.27391 (10)0.13832 (4)0.0147 (2)
O40.52511 (8)0.39877 (10)0.10896 (5)0.0162 (2)
O50.59215 (12)0.41062 (14)0.26257 (6)0.0329 (4)
H280.602 (3)0.428 (3)0.2384 (9)0.074 (13)*
C10.61876 (11)0.22621 (13)0.09521 (6)0.0142 (3)
C20.58787 (12)0.12267 (15)0.09075 (7)0.0178 (3)
C30.57805 (13)0.07391 (16)0.04878 (7)0.0216 (4)
H3A0.55760.00330.04440.026*
C40.59778 (13)0.12718 (18)0.01344 (7)0.0234 (4)
H4A0.59070.09280.01480.028*
C50.62766 (13)0.23015 (16)0.01910 (7)0.0208 (4)
H5A0.64040.26580.00550.025*
C60.63959 (11)0.28308 (15)0.06048 (6)0.0167 (3)
C70.56822 (14)0.06410 (16)0.12970 (7)0.0231 (4)
H7A0.55660.11870.15090.028*
C80.6421 (2)0.0004 (3)0.15528 (11)0.0479 (8)
H8A0.68990.04660.16550.072*
H8B0.65480.05530.13550.072*
H8C0.62920.03410.18140.072*
C90.49150 (19)0.0060 (2)0.11505 (9)0.0381 (6)
H9A0.44440.03740.09930.057*
H9B0.47950.03870.14160.057*
H9C0.50140.06180.09480.057*
C100.67452 (11)0.39474 (15)0.06599 (7)0.0208 (4)
H10A0.67590.42080.09690.025*
C110.76258 (18)0.3967 (2)0.05983 (16)0.0387 (9)0.836 (5)
H11A0.79980.35890.08490.058*0.836 (5)
H11B0.78100.47060.05930.058*0.836 (5)
H11C0.76320.36200.03140.058*0.836 (5)
C120.6195 (2)0.4699 (2)0.03107 (9)0.0303 (6)0.836 (5)
H12A0.56280.46750.03420.046*0.836 (5)
H12B0.62020.44720.00070.046*0.836 (5)
H12C0.64070.54270.03620.046*0.836 (5)
C11'0.7687 (3)0.3829 (13)0.0849 (7)0.0387 (9)0.164 (5)
H11D0.79110.34060.06400.058*0.164 (5)
H11E0.78030.34720.11420.058*0.164 (5)
H11F0.79440.45330.08850.058*0.164 (5)
C12'0.6605 (12)0.4708 (10)0.0256 (3)0.0303 (6)0.164 (5)
H12D0.69990.45440.00780.046*0.164 (5)
H12E0.66860.54430.03640.046*0.164 (5)
H12F0.60410.46230.00670.046*0.164 (5)
C130.45187 (11)0.45800 (14)0.10294 (6)0.0160 (3)
C140.37706 (12)0.40300 (17)0.08981 (6)0.0200 (3)
C150.30503 (13)0.4637 (2)0.08172 (8)0.0289 (5)
H15A0.25290.42930.07260.035*
C160.30828 (14)0.5733 (2)0.08671 (8)0.0313 (5)
H16A0.25860.61310.08140.038*
C170.38343 (14)0.62478 (19)0.09938 (8)0.0287 (5)
H17A0.38470.69980.10290.034*
C180.45771 (13)0.56851 (16)0.10715 (7)0.0216 (4)
C190.37475 (14)0.28304 (18)0.08306 (7)0.0251 (4)
H19A0.42500.25260.10430.030*
C200.2990 (2)0.2313 (3)0.09379 (12)0.0481 (8)
H20A0.29500.25430.12360.072*
H20B0.30460.15380.09350.072*
H20C0.24900.25270.07110.072*
C210.37944 (19)0.2568 (2)0.03513 (8)0.0373 (5)
H21A0.43080.28540.03020.056*
H21B0.33220.28880.01350.056*
H21C0.37830.17950.03100.056*
C220.53956 (15)0.62760 (17)0.11842 (9)0.0324 (5)
H22A0.58480.57400.12170.039*
C230.5534 (2)0.6881 (2)0.16291 (11)0.0527 (9)
H23A0.55580.63760.18750.079*
H23B0.50780.73800.16120.079*
H23C0.60560.72740.16860.079*
C240.54436 (18)0.7036 (2)0.08013 (11)0.0423 (7)
H24A0.53580.66360.05190.063*
H24B0.59880.73750.08710.063*
H24C0.50150.75820.07690.063*
C250.6042 (3)0.5005 (3)0.29174 (12)0.0338 (8)0.691 (6)
H25A0.55780.54980.28180.051*0.691 (6)
H25B0.65560.53650.29090.051*0.691 (6)
H25C0.60760.47710.32260.051*0.691 (6)
C25'0.6418 (6)0.4524 (8)0.2989 (3)0.0338 (8)0.309 (6)
H25D0.62590.42710.32570.051*0.309 (6)
H25E0.63740.53010.29730.051*0.309 (6)
H25F0.69880.43120.30070.051*0.309 (6)
O60.64455 (11)0.1878 (2)0.27305 (7)0.0455 (5)
H290.65370.13970.29270.055*0.782 (4)
H29'0.67190.22290.25860.055*0.218 (4)
C260.7182 (3)0.2188 (5)0.2643 (2)0.0678 (14)0.782 (4)
H26A0.76140.16720.27770.102*0.782 (4)
H26B0.73390.28910.27750.102*0.782 (4)
H26C0.71140.22190.23170.102*0.782 (4)
O70.7922 (2)0.4962 (3)0.19125 (15)0.0755 (13)0.782 (4)
H300.7428 (12)0.497 (4)0.1868 (16)0.054 (14)*0.782 (4)
C270.8310 (4)0.3959 (5)0.1910 (3)0.118 (3)0.782 (4)
H27A0.88670.40630.18720.176*0.782 (4)
H27B0.79860.35280.16610.176*0.782 (4)
H27C0.83430.35940.21960.176*0.782 (4)
C26'0.6832 (9)0.0978 (16)0.2870 (7)0.0678 (14)0.218 (4)
H26D0.73930.11320.30490.102*0.218 (4)
H26E0.68560.05440.26090.102*0.218 (4)
H26F0.65320.05910.30550.102*0.218 (4)
O7'0.7675 (6)0.3106 (8)0.2458 (4)0.048 (3)0.218 (4)
H30'0.75580.36690.23090.02 (3)*0.218 (4)
C27'0.8137 (7)0.2439 (13)0.2250 (6)0.057 (5)0.218 (4)
H27D0.86870.27440.22830.086*0.218 (4)
H27E0.78570.23720.19290.086*0.218 (4)
H27F0.81890.17360.23910.086*0.218 (4)
O80.5010 (6)0.0664 (10)0.2175 (5)0.0281 (14)0.5
O90.5199 (6)0.0791 (9)0.2894 (4)0.039 (2)0.5
O100.5273 (4)0.0759 (3)0.2582 (3)0.070 (2)0.5
N10.5157 (6)0.0204 (3)0.2554 (6)0.045 (3)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.01770 (6)0.01742 (6)0.01507 (6)0.0000.00786 (4)0.000
P10.01610 (19)0.01216 (18)0.01518 (19)0.00108 (14)0.00756 (15)0.00018 (15)
O10.0196 (6)0.0169 (6)0.0170 (6)0.0007 (5)0.0095 (5)0.0005 (5)
O20.0232 (6)0.0168 (6)0.0216 (7)0.0031 (5)0.0102 (5)0.0038 (5)
O30.0166 (5)0.0138 (5)0.0152 (6)0.0035 (4)0.0066 (4)0.0003 (4)
O40.0163 (6)0.0163 (6)0.0181 (6)0.0048 (4)0.0083 (5)0.0033 (5)
O50.0464 (10)0.0327 (8)0.0274 (8)0.0183 (8)0.0238 (8)0.0141 (7)
C10.0146 (7)0.0139 (7)0.0156 (7)0.0024 (5)0.0064 (6)0.0007 (5)
C20.0198 (8)0.0161 (7)0.0206 (8)0.0017 (6)0.0108 (7)0.0012 (6)
C30.0224 (9)0.0207 (8)0.0240 (9)0.0029 (7)0.0100 (7)0.0059 (7)
C40.0230 (9)0.0285 (10)0.0195 (9)0.0007 (7)0.0069 (7)0.0055 (7)
C50.0224 (8)0.0243 (9)0.0172 (8)0.0026 (6)0.0080 (6)0.0004 (6)
C60.0165 (7)0.0180 (7)0.0174 (8)0.0044 (6)0.0076 (6)0.0026 (6)
C70.0328 (10)0.0150 (8)0.0264 (10)0.0030 (7)0.0168 (8)0.0016 (7)
C80.0488 (16)0.0577 (18)0.0424 (16)0.0181 (14)0.0212 (13)0.0276 (14)
C90.0534 (16)0.0302 (12)0.0370 (13)0.0190 (11)0.0229 (12)0.0058 (10)
C100.0252 (9)0.0158 (7)0.0260 (9)0.0012 (6)0.0153 (7)0.0018 (7)
C110.0331 (14)0.0247 (12)0.070 (3)0.0047 (10)0.0344 (17)0.0048 (15)
C120.0454 (17)0.0227 (11)0.0270 (13)0.0059 (11)0.0167 (12)0.0083 (9)
C11'0.0331 (14)0.0247 (12)0.070 (3)0.0047 (10)0.0344 (17)0.0048 (15)
C12'0.0454 (17)0.0227 (11)0.0270 (13)0.0059 (11)0.0167 (12)0.0083 (9)
C130.0148 (7)0.0180 (7)0.0162 (8)0.0034 (6)0.0059 (6)0.0008 (6)
C140.0173 (8)0.0281 (9)0.0150 (8)0.0015 (7)0.0049 (6)0.0009 (7)
C150.0147 (8)0.0482 (14)0.0238 (10)0.0033 (8)0.0050 (7)0.0046 (9)
C160.0222 (10)0.0448 (13)0.0278 (11)0.0172 (9)0.0079 (8)0.0041 (9)
C170.0303 (11)0.0287 (10)0.0255 (10)0.0165 (8)0.0044 (8)0.0023 (8)
C180.0216 (8)0.0185 (8)0.0228 (9)0.0060 (7)0.0025 (7)0.0007 (7)
C190.0299 (10)0.0243 (9)0.0195 (9)0.0083 (8)0.0037 (8)0.0011 (7)
C200.0491 (16)0.0486 (17)0.0499 (17)0.0273 (13)0.0187 (14)0.0031 (13)
C210.0540 (15)0.0315 (12)0.0258 (10)0.0045 (12)0.0090 (10)0.0057 (10)
C220.0297 (11)0.0149 (8)0.0449 (14)0.0015 (7)0.0045 (10)0.0039 (8)
C230.067 (2)0.0263 (12)0.0465 (17)0.0025 (13)0.0194 (15)0.0032 (11)
C240.0398 (14)0.0209 (11)0.0605 (18)0.0033 (9)0.0029 (13)0.0096 (11)
C250.048 (2)0.0344 (19)0.0215 (14)0.0174 (14)0.0141 (15)0.0112 (13)
C25'0.048 (2)0.0344 (19)0.0215 (14)0.0174 (14)0.0141 (15)0.0112 (13)
O60.0247 (8)0.0697 (15)0.0411 (11)0.0160 (9)0.0064 (8)0.0012 (10)
C260.0299 (18)0.076 (3)0.097 (4)0.0099 (19)0.016 (2)0.003 (3)
O70.0376 (16)0.079 (3)0.114 (3)0.0388 (17)0.0278 (19)0.044 (2)
C270.084 (5)0.158 (8)0.131 (6)0.075 (5)0.064 (5)0.072 (6)
C26'0.0299 (18)0.076 (3)0.097 (4)0.0099 (19)0.016 (2)0.003 (3)
O7'0.064 (7)0.043 (5)0.052 (6)0.010 (5)0.041 (5)0.014 (5)
C27'0.027 (5)0.087 (12)0.059 (9)0.008 (7)0.011 (6)0.041 (9)
O80.034 (3)0.023 (3)0.031 (4)0.0028 (19)0.015 (2)0.004 (2)
O90.073 (7)0.023 (3)0.032 (4)0.015 (4)0.033 (5)0.008 (3)
O100.117 (6)0.0206 (16)0.083 (5)0.019 (2)0.044 (4)0.011 (2)
N10.072 (8)0.0217 (15)0.053 (7)0.013 (2)0.035 (6)0.011 (3)
Geometric parameters (Å, º) top
Nd1—O1i2.3516 (13)C14—C151.395 (3)
Nd1—O12.3516 (13)C14—C191.523 (3)
Nd1—O92.481 (13)C15—C161.388 (4)
Nd1—O6i2.4821 (18)C15—H15A0.9500
Nd1—O62.4821 (18)C16—C171.380 (4)
Nd1—O52.4825 (16)C16—H16A0.9500
Nd1—O5i2.4825 (16)C17—C181.398 (3)
Nd1—O82.553 (14)C17—H17A0.9500
Nd1—N12.939 (4)C18—C221.520 (3)
P1—O21.4970 (15)C19—C211.531 (3)
P1—O11.5099 (14)C19—C201.536 (4)
P1—O41.5887 (14)C19—H19A1.0000
P1—O31.5907 (13)C20—H20A0.9800
O3—C11.415 (2)C20—H20B0.9800
O4—C131.407 (2)C20—H20C0.9800
O5—C25'1.318 (8)C21—H21A0.9800
O5—C251.425 (4)C21—H21B0.9800
O5—H280.831 (18)C21—H21C0.9800
C1—C21.395 (3)C22—C231.530 (4)
C1—C61.402 (3)C22—C241.534 (4)
C2—C31.399 (3)C22—H22A1.0000
C2—C71.512 (3)C23—H23A0.9800
C3—C41.386 (3)C23—H23B0.9800
C3—H3A0.9500C23—H23C0.9800
C4—C51.384 (3)C24—H24A0.9800
C4—H4A0.9500C24—H24B0.9800
C5—C61.404 (3)C24—H24C0.9800
C5—H5A0.9500C25—H25A0.9800
C6—C101.515 (3)C25—H25B0.9800
C7—C81.520 (4)C25—H25C0.9800
C7—C91.529 (3)C25'—H25D0.9800
C7—H7A1.0000C25'—H25E0.9800
C8—H8A0.9800C25'—H25F0.9800
C8—H8B0.9800O6—C26'1.319 (19)
C8—H8C0.9800O6—C261.385 (5)
C9—H9A0.9800O6—H290.8400
C9—H9B0.9800O6—H29'0.8400
C9—H9C0.9800C26—H26A0.9800
C10—C111.536 (2)C26—H26B0.9800
C10—C12'1.538 (3)C26—H26C0.9800
C10—C11'1.542 (3)O7—C271.420 (5)
C10—C121.545 (3)O7—H300.803 (19)
C10—H10A1.0000C27—H27A0.9800
C11—H11A0.9800C27—H27B0.9800
C11—H11B0.9800C27—H27C0.9800
C11—H11C0.9800C26'—H26D0.9800
C12—H12A0.9800C26'—H26E0.9800
C12—H12B0.9800C26'—H26F0.9800
C12—H12C0.9800O7'—C27'1.403 (5)
C11'—H11D0.9800O7'—H30'0.8400
C11'—H11E0.9800C27'—H27D0.9800
C11'—H11F0.9800C27'—H27E0.9800
C12'—H12D0.9800C27'—H27F0.9800
C12'—H12E0.9800O8—N11.265 (19)
C12'—H12F0.9800O9—N11.267 (19)
C13—C181.398 (3)O10—N11.227 (6)
C13—C141.398 (3)
O1i—Nd1—O1154.36 (7)C10—C12'—H12D109.5
O1i—Nd1—O977.2 (3)C10—C12'—H12E109.5
O1—Nd1—O9127.8 (3)H12D—C12'—H12E109.5
O1i—Nd1—O6i88.07 (6)C10—C12'—H12F109.5
O1—Nd1—O6i100.39 (6)H12D—C12'—H12F109.5
O9—Nd1—O6i81.2 (2)H12E—C12'—H12F109.5
O1i—Nd1—O6100.39 (6)C18—C13—C14123.75 (17)
O1—Nd1—O688.07 (6)C18—C13—O4118.49 (16)
O9—Nd1—O664.6 (2)C14—C13—O4117.59 (16)
O6i—Nd1—O6141.41 (12)C15—C14—C13116.8 (2)
O1i—Nd1—O585.20 (5)C15—C14—C19121.8 (2)
O1—Nd1—O574.28 (5)C13—C14—C19121.31 (18)
O9—Nd1—O5128.9 (2)C16—C15—C14121.1 (2)
O6i—Nd1—O5146.20 (8)C16—C15—H15A119.4
O6—Nd1—O572.37 (8)C14—C15—H15A119.4
O1i—Nd1—O5i74.28 (5)C17—C16—C15120.3 (2)
O1—Nd1—O5i85.20 (5)C17—C16—H16A119.8
O9—Nd1—O5i141.3 (3)C15—C16—H16A119.8
O6i—Nd1—O5i72.37 (8)C16—C17—C18121.2 (2)
O6—Nd1—O5i146.20 (8)C16—C17—H17A119.4
O5—Nd1—O5i73.92 (10)C18—C17—H17A119.4
O1i—Nd1—O8125.7 (3)C13—C18—C17116.7 (2)
O1—Nd1—O879.9 (3)C13—C18—C22123.05 (17)
O9—Nd1—O850.67 (13)C17—C18—C22120.20 (19)
O6i—Nd1—O871.8 (3)C14—C19—C21109.81 (19)
O6—Nd1—O872.8 (2)C14—C19—C20112.6 (2)
O5—Nd1—O8136.8 (3)C21—C19—C20111.4 (2)
O5i—Nd1—O8137.8 (2)C14—C19—H19A107.6
O1i—Nd1—N1101.7 (4)C21—C19—H19A107.6
O1—Nd1—N1103.9 (4)C20—C19—H19A107.6
O9—Nd1—N125.3 (4)C19—C20—H20A109.5
O6i—Nd1—N175.8 (2)C19—C20—H20B109.5
O6—Nd1—N165.7 (2)H20A—C20—H20B109.5
O5—Nd1—N1138.0 (2)C19—C20—H20C109.5
O5i—Nd1—N1148.0 (2)H20A—C20—H20C109.5
O8—Nd1—N125.4 (4)H20B—C20—H20C109.5
O2—P1—O1114.00 (8)C19—C21—H21A109.5
O2—P1—O4113.28 (8)C19—C21—H21B109.5
O1—P1—O4110.24 (8)H21A—C21—H21B109.5
O2—P1—O3107.17 (8)C19—C21—H21C109.5
O1—P1—O3111.68 (7)H21A—C21—H21C109.5
O4—P1—O399.52 (7)H21B—C21—H21C109.5
P1—O1—Nd1144.15 (8)C18—C22—C23111.6 (2)
C1—O3—P1125.78 (11)C18—C22—C24110.61 (19)
C13—O4—P1124.73 (12)C23—C22—C24110.5 (2)
C25'—O5—Nd1133.0 (4)C18—C22—H22A108.0
C25—O5—Nd1135.58 (18)C23—C22—H22A108.0
C25'—O5—H28115 (3)C24—C22—H22A108.0
C25—O5—H28109 (3)C22—C23—H23A109.5
Nd1—O5—H28109 (3)C22—C23—H23B109.5
C2—C1—C6124.08 (17)H23A—C23—H23B109.5
C2—C1—O3118.08 (16)C22—C23—H23C109.5
C6—C1—O3117.65 (15)H23A—C23—H23C109.5
C1—C2—C3116.92 (17)H23B—C23—H23C109.5
C1—C2—C7121.86 (17)C22—C24—H24A109.5
C3—C2—C7121.20 (17)C22—C24—H24B109.5
C4—C3—C2120.98 (19)H24A—C24—H24B109.5
C4—C3—H3A119.5C22—C24—H24C109.5
C2—C3—H3A119.5H24A—C24—H24C109.5
C5—C4—C3120.36 (19)H24B—C24—H24C109.5
C5—C4—H4A119.8O5—C25—H25A109.5
C3—C4—H4A119.8O5—C25—H25B109.5
C4—C5—C6121.40 (19)H25A—C25—H25B109.5
C4—C5—H5A119.3O5—C25—H25C109.5
C6—C5—H5A119.3H25A—C25—H25C109.5
C1—C6—C5116.25 (17)H25B—C25—H25C109.5
C1—C6—C10123.58 (17)O5—C25'—H25D109.5
C5—C6—C10120.16 (17)O5—C25'—H25E109.5
C2—C7—C8110.84 (19)H25D—C25'—H25E109.5
C2—C7—C9112.69 (19)O5—C25'—H25F109.5
C8—C7—C9110.8 (2)H25D—C25'—H25F109.5
C2—C7—H7A107.4H25E—C25'—H25F109.5
C8—C7—H7A107.4C26'—O6—Nd1137.5 (8)
C9—C7—H7A107.4C26—O6—Nd1134.8 (3)
C7—C8—H8A109.5C26—O6—H29109.5
C7—C8—H8B109.5Nd1—O6—H29115.4
H8A—C8—H8B109.5C26'—O6—H29'109.5
C7—C8—H8C109.5Nd1—O6—H29'107.5
H8A—C8—H8C109.5O6—C26—H26A109.5
H8B—C8—H8C109.5O6—C26—H26B109.5
C7—C9—H9A109.5H26A—C26—H26B109.5
C7—C9—H9B109.5O6—C26—H26C109.5
H9A—C9—H9B109.5H26A—C26—H26C109.5
C7—C9—H9C109.5H26B—C26—H26C109.5
H9A—C9—H9C109.5C27—O7—H30117 (4)
H9B—C9—H9C109.5O7—C27—H27A109.5
C6—C10—C11110.95 (17)O7—C27—H27B109.5
C6—C10—C12'120.8 (6)H27A—C27—H27B109.5
C6—C10—C11'106.3 (6)O7—C27—H27C109.5
C12'—C10—C11'107.0 (10)H27A—C27—H27C109.5
C6—C10—C12110.22 (18)H27B—C27—H27C109.5
C11—C10—C12109.0 (2)O6—C26'—H26D109.5
C6—C10—H10A108.9O6—C26'—H26E109.5
C11—C10—H10A108.9H26D—C26'—H26E109.5
C12—C10—H10A108.9O6—C26'—H26F109.5
C10—C11—H11A109.5H26D—C26'—H26F109.5
C10—C11—H11B109.5H26E—C26'—H26F109.5
H11A—C11—H11B109.5C27'—O7'—H30'109.5
C10—C11—H11C109.5O7'—C27'—H27D109.5
H11A—C11—H11C109.5O7'—C27'—H27E109.5
H11B—C11—H11C109.5H27D—C27'—H27E109.5
C10—C12—H12A109.5O7'—C27'—H27F109.5
C10—C12—H12B109.5H27D—C27'—H27F109.5
H12A—C12—H12B109.5H27E—C27'—H27F109.5
C10—C12—H12C109.5N1—O8—Nd194.6 (9)
H12A—C12—H12C109.5N1—O9—Nd198.0 (9)
H12B—C12—H12C109.5O10—N1—O8120.4 (14)
C10—C11'—H11D109.5O10—N1—O9122.9 (14)
C10—C11'—H11E109.5O8—N1—O9116.6 (4)
H11D—C11'—H11E109.5O10—N1—Nd1176.2 (8)
C10—C11'—H11F109.5O8—N1—Nd160.0 (6)
H11D—C11'—H11F109.5O9—N1—Nd156.7 (6)
H11E—C11'—H11F109.5
O2—P1—O1—Nd117.75 (17)C1—C6—C10—C11'85.6 (9)
O4—P1—O1—Nd1146.45 (13)C5—C6—C10—C11'93.3 (9)
O3—P1—O1—Nd1103.91 (14)C1—C6—C10—C12123.3 (2)
O2—P1—O3—C1143.04 (14)C5—C6—C10—C1257.7 (2)
O1—P1—O3—C191.44 (15)P1—O4—C13—C1889.6 (2)
O4—P1—O3—C124.92 (15)P1—O4—C13—C1494.97 (19)
O2—P1—O4—C1379.58 (16)C18—C13—C14—C151.6 (3)
O1—P1—O4—C1349.51 (16)O4—C13—C14—C15176.75 (17)
O3—P1—O4—C13166.96 (14)C18—C13—C14—C19176.22 (19)
P1—O3—C1—C297.66 (18)O4—C13—C14—C191.1 (3)
P1—O3—C1—C687.16 (19)C13—C14—C15—C160.2 (3)
C6—C1—C2—C30.4 (3)C19—C14—C15—C16178.0 (2)
O3—C1—C2—C3174.44 (16)C14—C15—C16—C170.7 (4)
C6—C1—C2—C7178.59 (18)C15—C16—C17—C180.5 (4)
O3—C1—C2—C73.7 (3)C14—C13—C18—C172.7 (3)
C1—C2—C3—C40.5 (3)O4—C13—C18—C17177.82 (18)
C7—C2—C3—C4178.65 (19)C14—C13—C18—C22175.8 (2)
C2—C3—C4—C50.0 (3)O4—C13—C18—C220.7 (3)
C3—C4—C5—C60.6 (3)C16—C17—C18—C132.1 (3)
C2—C1—C6—C50.1 (3)C16—C17—C18—C22176.5 (2)
O3—C1—C6—C5174.99 (16)C15—C14—C19—C2191.7 (3)
C2—C1—C6—C10178.86 (17)C13—C14—C19—C2186.1 (2)
O3—C1—C6—C104.0 (2)C15—C14—C19—C2033.0 (3)
C4—C5—C6—C10.6 (3)C13—C14—C19—C20149.2 (2)
C4—C5—C6—C10178.38 (18)C13—C18—C22—C23118.2 (2)
C1—C2—C7—C892.0 (3)C17—C18—C22—C2363.4 (3)
C3—C2—C7—C886.1 (3)C13—C18—C22—C24118.4 (2)
C1—C2—C7—C9143.1 (2)C17—C18—C22—C2460.0 (3)
C3—C2—C7—C938.8 (3)Nd1—O8—N1—O10175.6 (9)
C1—C6—C10—C11115.9 (3)Nd1—O8—N1—O92.6 (13)
C5—C6—C10—C1163.1 (3)Nd1—O9—N1—O10175.5 (10)
C1—C6—C10—C12'152.3 (8)Nd1—O9—N1—O82.7 (14)
C5—C6—C10—C12'28.7 (8)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H28···O20.83 (2)1.84 (2)2.660 (2)167 (4)
O6—H29···O7ii0.842.022.746 (4)144
O6—H29···O70.842.062.866 (10)160
C26—H26A···O7ii0.982.613.140 (7)114
O7—H30···O20.80 (2)2.01 (3)2.762 (3)155 (5)
O7—H30···O20.842.362.998 (12)133
Symmetry code: (ii) x+3/2, y1/2, z+1/2.
Selected bond lengths (Å) for (1), (2), (3) and (4) top
(1) (Ln = Nd)(2) (Ln = Lu)(3) (Ln = Y)(4) (Ln = Nd)
Ln1—Cl12.6868 (9)2.5824 (8)2.6199 (6)-
Ln1—O12.3381 (13)2.2006 (11)2.2411 (9)2.3516 (13)
Ln1—O52.4867 (16)2.3314 (14)2.3776 (12)2.4825 (16)
Ln1—O62.4655 (17)2.3499 (15)2.3835 (12)2.4871 (19)
Ln1—O8---2.553 (14)
Ln1—O9---2.480 (13)
P1—O11.5047 (13)1.5069 (12)1.5095 (10)1.5099 (14)
P1—O21.4918 (13)1.4903 (12)1.4927 (10)1.4968 (15)
P1—O31.5875 (13)1.5836 (11)1.5873 (10)1.5907 (13)
P1—O41.5872 (13)1.5862 (11)1.5895 (10)1.5885 (14)
O3—C11.410 (2)1.4093 (19)1.4104 (16)1.415 (2)
O4—C131.4080 (19)1.4074 (18)1.4087 (16)1.407 (2)
Hydrogen-bond geometry (Å, °) for (1)–(4) top
Parameters of weak C—H···O interactions in (1)–(4) and O—H···O(NO3) interactions in (4) have been omitted.
ComplexD—H···AD—HH···AD···AD—H···A
(1)O5—H28···O20.90 (4)1.74 (4)2.626 (2)168 (4)
O6—H29···O7i0.87 (6)1.92 (6)2.753 (3)161 (5)
O7—H30···O20.88 (5)1.93 (5)2.787 (3)165 (5)
O6—H29···Cl10.87 (6)2.69 (6)2.989 (2)102 (4)
(2)O5—H28···O20.82 (3)1.81 (3)2.6082 (18)167 (3)
O6—H29···O7i0.79 (3)2.13 (3)2.861 (3)153 (3)
O7—H30···O20.71 (3)2.14 (4)2.826 (2)163 (4)
O6—H29···Cl10.79 (3)2.53 (3)2.8761 (17)108 (3)
(3)O5—H28···O20.80 (3)1.83 (3)2.6179 (15)166 (3)
O6—H29···O7i0.79 (3)2.09 (3)2.813 (2)151 (3)
O7—H30···O20.77 (3)2.06 (3)2.8150 (18)168 (3)
O6—H29···Cl10.79 (3)2.54 (3)2.9173 (14)111 (2)
(4)O5—H28···O20.831 (18)1.84 (2)2.660 (2)167 (4)
O6—H29···O7i0.842.022.746 (4)143.6
O6—H29'···O7'0.842.062.866 (10)159.5
O7—H30···O20.803 (19)2.01 (3)2.762 (3)155 (5)
O7'—H30'···O20.842.362.998 (12)132.8
Symmetry code: (i) -x+1, y, -z+1.
 

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