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

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{Bis[N,N′-di­cyclo­hexyl-N′′,N′′-bis­­(tri­meth­yl­sil­yl)guanidinato-κ2N,N′]neo­dymium(III)}di-μ-chlorido-[bis­­(tetra­hydro­furan-κO)lithium]

aNingbo Institute of Technology, Zhejiang University, Ningbo 315100, People's Republic of China, and bDepartment of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027, People's Republic of China
*Correspondence e-mail: chj@nit.zju.edu.cn

(Received 9 January 2013; accepted 16 January 2013; online 23 January 2013)

In the title monomeric rare earth complex, [LiNd(C19H40N3Si2)2Cl2(C4H8O)2], the [(Me3Si)2NC(NCy)2]2Nd+ (Me is methyl, Cy is cyclo­hex­yl) and Li(THF)2+ units (THF is tetra­hydro­furan) are connected by two bridging Cl atoms. The Nd3+ ion is coordinated by two guanidinate ligands and two Cl atoms, forming a distorted chelating octa­hedral geometry. The Li+ ion is four-coordinated by two Cl atoms and two O atoms from THF mol­ecules in a distorted tetra­hedral geometry.

Related literature

For the synthesis of analogous bis­(guanidinato) rare earth complexes, see: Luo et al. (2003[Luo, Y. J., Yao, Y. M., Shen, Q., Yu, K. B. & Weng, L. H. (2003). Eur. J. Inorg. Chem. pp. 318-323.]). For a review of bis­(guanidinato) rare earth complexes, see: Trifonov (2010[Trifonov, A. A. (2010). Coord. Chem. Rev. 254, 1327-1347.]).

[Scheme 1]

Experimental

Crystal data
  • [LiNd(C19H40N3Si2)2Cl2(C4H8O)2]

  • Mr = 1099.73

  • Monoclinic, P 21 /c

  • a = 24.1739 (16) Å

  • b = 13.5238 (8) Å

  • c = 18.8108 (13) Å

  • β = 103.215 (2)°

  • V = 5986.8 (7) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.07 mm−1

  • T = 223 K

  • 0.40 × 0.40 × 0.30 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.464, Tmax = 0.752

  • 35442 measured reflections

  • 11104 independent reflections

  • 9767 reflections with I > 2σ(I)

  • Rint = 0.051

Refinement
  • R[F2 > 2σ(F2)] = 0.051

  • wR(F2) = 0.111

  • S = 1.17

  • 11104 reflections

  • 554 parameters

  • 3 restraints

  • H-atom parameters constrained

  • Δρmax = 0.74 e Å−3

  • Δρmin = −1.21 e Å−3

Table 1
Selected bond lengths (Å)

Li1—Cl1 2.336 (7)
Li1—Cl2 2.335 (7)
Li1—O1 1.907 (9)
Li1—O2 1.951 (8)
Nd1—Cl1 2.7621 (11)
Nd1—Cl2 2.7667 (11)
Nd1—N1 2.462 (3)
Nd1—N2 2.405 (3)
Nd1—N4 2.481 (3)
Nd1—N5 2.419 (3)

Data collection: CrystalClear (Rigaku, 2000[Rigaku (2000). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku, 2000[Rigaku (2000). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Rare earth metal chlorides are important precursors for preparing rare-earth metal derivatives such as Ln—C and Ln—N σ-bonded complexes (Trifonov, 2010). In the title complex, the Nd—N distances range from 2.405 (3) to 2.481 (3) Å, which are consistent with those in {(i-PrN)2C[N(SiMe3)2]}2Nd(µ-Cl)2Li(THF)2 (2.398 (7) to 2.477 (7) Å) and {(i-PrN)2C[N(i-Pr)2]}2Nd(µ-Cl)2Li(TMEDA) (2.406 (3) to 2.475 (3) Å; Luo et al., 2003), suggesting the delocalization of π-electrons within the NCN fragments in the guanidinato ligands. The Nd—Cl distances are 2.7621 (11) and 2.7667 (11) Å, which are comparable to those in {(i-PrN)2C[N(SiMe3)2]}2Nd(µ-Cl)2Li(THF)2 (2.746 (3) to 2.768 (3) Å) and {(i-PrN)2C[N(i-Pr)2]}2Nd(µ-Cl)2Li(TMEDA) (2.7888 (9) to 2.7747 (9) Å; Luo et al., 2003). The orientation of the N(SiMe3)2 groups relative to the NCNNd plane is approximately perpendicular, which increases the steric bulk above and below the planar guanidinato ligand.

Related literature top

For the synthesis of analogous ate bis(guanidinato) rare earth complexes, see: Luo et al. (2003). For a review of ate bis(guanidinato) rare earth complexes, see: Trifonov (2010).

Experimental top

The bis(guanidinato) neodymium chloride ate complex was prepared by the reaction of NdCl3 with 2 equiv. of guanidinato lithium in THF at room temperature. Blue crystals suitable for X-ray analysis were grown from a toluene solution at 243 K.

Refinement top

H-atoms were placed in calculated positions, with Csp—H = 0.99 Å, Csp2—H = 0.98 Å, Csp3—H = 0.97 Å and were included in the refinement in the riding model approximation, with Uiso(H) = 1.2Ueq(Csp, N) or 1.2Ueq(Csp2) or 1.5Ueq(Csp3). Four restraints and constraints (DFIX, EADP) were used to regularize some small parts of the structure.

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear (Rigaku, 2000); data reduction: CrystalStructure (Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound with displacement elliposids drawn at the 10% probability level. Atoms with suffix A are generated by the symmetry operation (1 - x, 1 - y, 1 - z).
{Bis[N,N'-dicyclohexyl-N'',N''-bis(trimethylsilyl)guanidinato-κ2N,N']neodymium(III)}di-µ-chlorido-[bis(tetrahydrofuran-κO)lithium] top
Crystal data top
[LiNd(C19H40N3Si2)2Cl2(C4H8O)2]F(000) = 2332
Mr = 1099.73Dx = 1.220 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybcCell parameters from 22051 reflections
a = 24.1739 (16) Åθ = 3.0–27.5°
b = 13.5238 (8) ŵ = 1.07 mm1
c = 18.8108 (13) ÅT = 223 K
β = 103.215 (2)°Block, blue
V = 5986.8 (7) Å30.40 × 0.40 × 0.30 mm
Z = 4
Data collection top
Rigaku Saturn
diffractometer
11104 independent reflections
Radiation source: fine-focus sealed tube9767 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
Detector resolution: 14.63 pixels mm-1θmax = 25.5°, θmin = 3.0°
ω scansh = 2629
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
k = 1316
Tmin = 0.464, Tmax = 0.752l = 2222
35442 measured reflections
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0336P)2 + 2.446P]
where P = (Fo2 + 2Fc2)/3
11104 reflections(Δ/σ)max = 0.002
554 parametersΔρmax = 0.74 e Å3
3 restraintsΔρmin = 1.21 e Å3
Crystal data top
[LiNd(C19H40N3Si2)2Cl2(C4H8O)2]V = 5986.8 (7) Å3
Mr = 1099.73Z = 4
Monoclinic, P21/cMo Kα radiation
a = 24.1739 (16) ŵ = 1.07 mm1
b = 13.5238 (8) ÅT = 223 K
c = 18.8108 (13) Å0.40 × 0.40 × 0.30 mm
β = 103.215 (2)°
Data collection top
Rigaku Saturn
diffractometer
11104 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)
9767 reflections with I > 2σ(I)
Tmin = 0.464, Tmax = 0.752Rint = 0.051
35442 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0513 restraints
wR(F2) = 0.111H-atom parameters constrained
S = 1.17Δρmax = 0.74 e Å3
11104 reflectionsΔρmin = 1.21 e Å3
554 parameters
Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Nd10.753934 (8)0.681163 (16)0.493605 (11)0.03401 (9)
Cl10.72460 (5)0.82878 (8)0.57959 (6)0.0490 (3)
Cl20.78168 (5)0.84300 (8)0.41875 (6)0.0479 (3)
Si10.92517 (5)0.44819 (10)0.64320 (7)0.0501 (3)
Si20.88678 (5)0.59797 (10)0.74807 (6)0.0492 (3)
Si30.59076 (6)0.44378 (11)0.32461 (8)0.0569 (4)
Si40.61562 (5)0.62828 (10)0.24047 (6)0.0463 (3)
O10.78568 (17)1.0620 (3)0.5248 (2)0.0724 (10)
O20.67309 (16)1.0011 (3)0.43762 (18)0.0796 (12)
N10.85395 (13)0.6531 (3)0.55572 (17)0.0368 (8)
N20.78750 (13)0.5577 (3)0.58538 (18)0.0403 (8)
N30.88311 (13)0.5457 (2)0.66146 (17)0.0383 (8)
N40.65391 (13)0.6378 (3)0.43657 (17)0.0408 (8)
N50.72343 (13)0.5678 (3)0.39276 (17)0.0398 (8)
N60.62701 (13)0.5540 (3)0.31891 (17)0.0390 (8)
C10.84171 (16)0.5852 (3)0.6009 (2)0.0348 (9)
C20.90922 (16)0.7015 (3)0.5676 (2)0.0375 (9)
H20.93710.66240.60340.045*
C30.90659 (17)0.8054 (3)0.5973 (2)0.0450 (11)
H3A0.89600.80180.64450.054*
H3B0.87710.84300.56380.054*
C40.96352 (19)0.8600 (4)0.6070 (3)0.0558 (12)
H4A0.95930.92770.62380.067*
H4B0.99220.82650.64450.067*
C50.9834 (2)0.8634 (4)0.5361 (3)0.0587 (13)
H5A1.02100.89410.54470.070*
H5B0.95700.90360.50020.070*
C60.98606 (18)0.7594 (4)0.5064 (3)0.0538 (12)
H6A1.01520.72140.54020.065*
H6B0.99710.76290.45940.065*
C70.92895 (17)0.7061 (3)0.4959 (2)0.0455 (11)
H7A0.93260.63890.47810.055*
H7B0.90040.74100.45900.055*
C80.76545 (17)0.4788 (3)0.6239 (2)0.0448 (10)
H80.79220.46710.67150.054*
C90.7578 (2)0.3830 (4)0.5796 (3)0.0598 (13)
H9A0.73400.39640.53100.072*
H9B0.79510.36090.57330.072*
C100.7309 (3)0.3000 (4)0.6148 (3)0.0836 (18)
H10A0.72500.24230.58240.100*
H10B0.75670.28070.66090.100*
C110.6750 (3)0.3323 (5)0.6294 (4)0.093 (2)
H11A0.66020.27980.65580.111*
H11B0.64760.34280.58280.111*
C120.6812 (3)0.4270 (5)0.6740 (3)0.092 (2)
H12A0.70510.41430.72270.111*
H12B0.64370.44830.67970.111*
C130.7081 (2)0.5101 (4)0.6370 (3)0.0702 (15)
H13A0.68250.52710.59020.084*
H13B0.71300.56920.66800.084*
C141.0021 (2)0.4727 (5)0.6799 (4)0.0865 (19)
H14A1.01270.53330.65880.130*
H14B1.02420.41810.66750.130*
H14C1.00960.47940.73260.130*
C150.9085 (2)0.3303 (4)0.6860 (3)0.0695 (15)
H15A0.92020.33580.73870.104*
H15B0.92880.27610.66950.104*
H15C0.86800.31780.67180.104*
C160.9122 (2)0.4321 (4)0.5427 (3)0.0664 (14)
H16A0.87160.43230.52180.100*
H16B0.92820.36960.53190.100*
H16C0.93000.48580.52200.100*
C170.8280 (2)0.6869 (4)0.7429 (3)0.0648 (15)
H17A0.82590.73010.70120.097*
H17B0.83480.72610.78720.097*
H17C0.79250.65120.73750.097*
C180.9561 (2)0.6635 (5)0.7819 (3)0.087 (2)
H18A0.98660.61540.79300.131*
H18B0.95480.70050.82570.131*
H18C0.96270.70850.74460.131*
C190.8819 (3)0.5016 (4)0.8170 (3)0.0775 (17)
H19A0.84700.46430.80080.116*
H19B0.88200.53290.86340.116*
H19C0.91420.45720.82270.116*
C200.66817 (16)0.5861 (3)0.3829 (2)0.0387 (9)
C210.59533 (16)0.6686 (4)0.4337 (2)0.0448 (11)
H210.56950.62960.39550.054*
C220.58665 (19)0.7770 (4)0.4154 (3)0.0602 (13)
H22A0.59630.79020.36840.072*
H22B0.61200.81650.45280.072*
C230.5246 (2)0.8076 (5)0.4111 (3)0.0776 (18)
H23A0.52010.87840.40040.093*
H23B0.49940.77140.37140.093*
C240.5081 (2)0.7857 (7)0.4823 (4)0.101 (3)
H24A0.46780.80100.47730.121*
H24B0.53020.82810.52080.121*
C250.5187 (2)0.6784 (6)0.5040 (4)0.100 (3)
H25A0.49310.63640.46860.119*
H25B0.51030.66780.55200.119*
C260.58040 (19)0.6480 (5)0.5071 (3)0.0718 (16)
H26A0.60610.68530.54570.086*
H26B0.58530.57750.51870.086*
C270.74792 (17)0.5121 (3)0.3410 (2)0.0422 (10)
H270.72060.51180.29290.051*
C280.7607 (2)0.4056 (4)0.3660 (3)0.0586 (13)
H28A0.72530.37270.36950.070*
H28B0.78610.40550.41480.070*
C290.7886 (2)0.3477 (4)0.3131 (3)0.0745 (16)
H29A0.79820.28090.33220.089*
H29B0.76180.34180.26560.089*
C300.8424 (2)0.3999 (5)0.3034 (3)0.0858 (19)
H30A0.87100.39850.34970.103*
H30B0.85790.36480.26680.103*
C310.8301 (2)0.5058 (5)0.2797 (3)0.0762 (17)
H31A0.80460.50700.23100.091*
H31B0.86560.53870.27660.091*
C320.80272 (19)0.5617 (4)0.3330 (3)0.0595 (13)
H32A0.79450.62960.31560.071*
H32B0.82940.56470.38080.071*
C330.6103 (2)0.3968 (4)0.4199 (3)0.0744 (16)
H33A0.65020.37920.43220.112*
H33B0.58750.33900.42430.112*
H33C0.60330.44790.45300.112*
C340.6078 (3)0.3470 (4)0.2629 (3)0.0862 (19)
H34A0.59310.36660.21250.129*
H34B0.59060.28490.27200.129*
H34C0.64870.33900.27190.129*
C350.5124 (2)0.4640 (5)0.2975 (4)0.092 (2)
H35A0.50180.51610.32730.138*
H35B0.49290.40340.30460.138*
H35C0.50180.48310.24640.138*
C360.6158 (2)0.5520 (4)0.1583 (2)0.0680 (15)
H36A0.64970.51140.16720.102*
H36B0.61520.59500.11690.102*
H36C0.58240.50980.14800.102*
C370.5443 (2)0.6893 (4)0.2223 (3)0.0716 (16)
H37A0.51500.63930.21860.107*
H37B0.53830.72590.17680.107*
H37C0.54270.73420.26190.107*
C380.6709 (2)0.7261 (4)0.2506 (3)0.0575 (12)
H38A0.67430.75930.29720.086*
H38B0.66010.77370.21130.086*
H38C0.70700.69640.24870.086*
C390.7944 (3)1.1257 (5)0.4664 (3)0.0856 (18)
H39A0.76701.18030.45920.103*
H39B0.78891.08830.42080.103*
C400.8531 (3)1.1650 (5)0.4870 (4)0.092 (2)
H40A0.85351.23290.50520.110*
H40B0.87111.16370.44530.110*
C410.8827 (3)1.0970 (6)0.5456 (4)0.102 (2)
H41A0.91371.13080.57960.122*
H41B0.89801.03930.52500.122*
C420.8360 (3)1.0672 (4)0.5831 (3)0.0775 (17)
H42A0.84431.00290.60720.093*
H42B0.83161.11660.61950.093*
C430.6595 (3)1.0083 (6)0.3598 (3)0.1053 (12)
H43A0.64310.94620.33770.126*
H43B0.69361.02330.34190.126*
C440.6189 (3)1.0875 (6)0.3424 (3)0.1053 (12)
H44A0.58991.07150.29830.126*
H44B0.63791.14890.33380.126*
C450.5926 (3)1.0989 (6)0.4057 (3)0.1053 (12)
H45A0.58581.16880.41440.126*
H45B0.55641.06320.39740.126*
C460.6339 (3)1.0565 (6)0.4675 (3)0.1053 (12)
H46A0.65361.10910.49930.126*
H46B0.61471.01350.49630.126*
Li10.7431 (3)0.9442 (6)0.4956 (4)0.0509 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.03086 (13)0.03540 (15)0.03492 (14)0.00010 (9)0.00580 (10)0.00130 (9)
Cl10.0601 (7)0.0484 (7)0.0435 (6)0.0081 (5)0.0224 (5)0.0024 (5)
Cl20.0561 (6)0.0458 (6)0.0468 (6)0.0009 (5)0.0218 (5)0.0059 (5)
Si10.0421 (7)0.0415 (8)0.0635 (8)0.0118 (6)0.0057 (6)0.0002 (6)
Si20.0571 (7)0.0538 (8)0.0343 (6)0.0063 (7)0.0052 (6)0.0010 (6)
Si30.0517 (7)0.0548 (9)0.0592 (8)0.0203 (7)0.0023 (7)0.0014 (7)
Si40.0452 (7)0.0558 (8)0.0371 (6)0.0093 (6)0.0079 (5)0.0010 (6)
O10.105 (3)0.051 (2)0.068 (2)0.012 (2)0.033 (2)0.0006 (18)
O20.097 (3)0.092 (3)0.054 (2)0.046 (2)0.027 (2)0.021 (2)
N10.0325 (17)0.041 (2)0.0369 (18)0.0020 (15)0.0077 (15)0.0048 (16)
N20.0375 (18)0.040 (2)0.0433 (19)0.0017 (16)0.0084 (16)0.0063 (16)
N30.0391 (18)0.039 (2)0.0346 (17)0.0077 (16)0.0031 (15)0.0037 (15)
N40.0328 (17)0.054 (2)0.0368 (18)0.0058 (16)0.0100 (15)0.0073 (17)
N50.0347 (17)0.049 (2)0.0364 (18)0.0014 (16)0.0092 (15)0.0051 (16)
N60.0366 (17)0.044 (2)0.0346 (17)0.0097 (16)0.0053 (15)0.0030 (16)
C10.039 (2)0.031 (2)0.034 (2)0.0019 (18)0.0081 (18)0.0041 (17)
C20.034 (2)0.035 (2)0.042 (2)0.0020 (18)0.0069 (18)0.0025 (19)
C30.042 (2)0.047 (3)0.047 (2)0.003 (2)0.011 (2)0.007 (2)
C40.053 (3)0.050 (3)0.059 (3)0.011 (2)0.000 (2)0.007 (2)
C50.049 (3)0.059 (3)0.067 (3)0.014 (2)0.010 (2)0.006 (3)
C60.042 (2)0.062 (3)0.060 (3)0.003 (2)0.017 (2)0.006 (3)
C70.035 (2)0.050 (3)0.052 (3)0.001 (2)0.011 (2)0.004 (2)
C80.046 (2)0.046 (3)0.042 (2)0.004 (2)0.011 (2)0.007 (2)
C90.062 (3)0.054 (3)0.061 (3)0.013 (3)0.009 (3)0.008 (3)
C100.107 (5)0.058 (4)0.088 (4)0.033 (4)0.026 (4)0.011 (3)
C110.100 (5)0.099 (5)0.077 (4)0.049 (4)0.016 (4)0.026 (4)
C120.076 (4)0.122 (6)0.092 (4)0.023 (4)0.045 (4)0.019 (4)
C130.056 (3)0.079 (4)0.085 (4)0.003 (3)0.035 (3)0.012 (3)
C140.047 (3)0.079 (4)0.131 (5)0.019 (3)0.014 (3)0.003 (4)
C150.072 (3)0.048 (3)0.085 (4)0.018 (3)0.008 (3)0.010 (3)
C160.089 (4)0.046 (3)0.072 (3)0.019 (3)0.034 (3)0.008 (3)
C170.084 (4)0.070 (4)0.042 (3)0.027 (3)0.018 (3)0.001 (2)
C180.083 (4)0.111 (5)0.059 (3)0.021 (4)0.003 (3)0.027 (3)
C190.104 (4)0.084 (4)0.044 (3)0.023 (4)0.017 (3)0.019 (3)
C200.036 (2)0.041 (2)0.039 (2)0.0090 (19)0.0073 (18)0.0025 (19)
C210.027 (2)0.066 (3)0.042 (2)0.003 (2)0.0076 (18)0.007 (2)
C220.045 (3)0.067 (4)0.069 (3)0.001 (3)0.014 (2)0.012 (3)
C230.049 (3)0.091 (5)0.090 (4)0.020 (3)0.011 (3)0.016 (3)
C240.043 (3)0.174 (8)0.084 (5)0.025 (4)0.012 (3)0.045 (5)
C250.055 (4)0.180 (8)0.075 (4)0.003 (4)0.040 (3)0.005 (5)
C260.044 (3)0.119 (5)0.058 (3)0.004 (3)0.024 (2)0.010 (3)
C270.043 (2)0.045 (3)0.039 (2)0.001 (2)0.0109 (19)0.007 (2)
C280.070 (3)0.050 (3)0.059 (3)0.000 (3)0.020 (3)0.006 (2)
C290.087 (4)0.060 (4)0.077 (4)0.014 (3)0.020 (3)0.014 (3)
C300.076 (4)0.105 (5)0.083 (4)0.029 (4)0.031 (3)0.014 (4)
C310.067 (3)0.089 (5)0.084 (4)0.006 (3)0.041 (3)0.012 (3)
C320.055 (3)0.061 (3)0.071 (3)0.005 (2)0.034 (3)0.008 (3)
C330.080 (4)0.067 (4)0.076 (4)0.026 (3)0.018 (3)0.017 (3)
C340.109 (5)0.065 (4)0.076 (4)0.026 (4)0.002 (4)0.015 (3)
C350.057 (3)0.097 (5)0.112 (5)0.034 (3)0.003 (3)0.010 (4)
C360.083 (4)0.078 (4)0.044 (3)0.021 (3)0.019 (3)0.007 (3)
C370.059 (3)0.087 (4)0.065 (3)0.008 (3)0.006 (3)0.020 (3)
C380.063 (3)0.059 (3)0.051 (3)0.013 (3)0.015 (2)0.002 (2)
C390.108 (5)0.059 (4)0.095 (5)0.006 (4)0.035 (4)0.014 (3)
C400.105 (5)0.070 (4)0.110 (5)0.012 (4)0.042 (4)0.005 (4)
C410.106 (5)0.099 (6)0.110 (5)0.005 (4)0.044 (4)0.017 (5)
C420.109 (5)0.061 (4)0.064 (3)0.004 (3)0.022 (4)0.015 (3)
C430.119 (3)0.127 (3)0.075 (2)0.055 (2)0.032 (2)0.016 (2)
C440.119 (3)0.127 (3)0.075 (2)0.055 (2)0.032 (2)0.016 (2)
C450.119 (3)0.127 (3)0.075 (2)0.055 (2)0.032 (2)0.016 (2)
C460.119 (3)0.127 (3)0.075 (2)0.055 (2)0.032 (2)0.016 (2)
Li10.061 (5)0.049 (5)0.046 (4)0.010 (4)0.019 (4)0.007 (3)
Geometric parameters (Å, º) top
Li1—Cl12.336 (7)C16—H16C0.9700
Li1—Cl22.335 (7)C17—H17A0.9700
Li1—O11.907 (9)C17—H17B0.9700
Li1—O21.951 (8)C17—H17C0.9700
Nd1—Cl12.7621 (11)C18—H18A0.9700
Nd1—Cl22.7667 (11)C18—H18B0.9700
Nd1—N12.462 (3)C18—H18C0.9700
Nd1—N22.405 (3)C19—H19A0.9700
Nd1—N42.481 (3)C19—H19B0.9700
Nd1—N52.419 (3)C19—H19C0.9700
Nd1—C12.881 (4)C21—C221.510 (7)
Nd1—C202.883 (4)C21—C261.530 (6)
O2—C461.421 (6)C21—H210.9900
O2—C431.428 (6)C22—C231.540 (6)
Si1—N31.747 (3)C22—H22A0.9800
Si1—C161.856 (5)C22—H22B0.9800
Si1—C141.860 (5)C23—C241.511 (8)
Si1—C151.871 (5)C23—H23A0.9800
Si2—N31.759 (3)C23—H23B0.9800
Si2—C171.847 (5)C24—C251.514 (9)
Si2—C191.861 (5)C24—H24A0.9800
Si2—C181.874 (6)C24—H24B0.9800
Si3—N61.745 (4)C25—C261.534 (7)
Si3—C341.858 (6)C25—H25A0.9800
Si3—C331.859 (5)C25—H25B0.9800
Si3—C351.865 (5)C26—H26A0.9800
Si4—N61.754 (3)C26—H26B0.9800
Si4—C381.858 (5)C27—C321.523 (6)
Si4—C361.859 (5)C27—C281.524 (6)
Si4—C371.870 (5)C27—H270.9900
O1—C421.442 (6)C28—C291.539 (6)
O1—C391.449 (6)C28—H28A0.9800
N1—C11.329 (5)C28—H28B0.9800
N1—C21.458 (5)C29—C301.527 (8)
N2—C11.329 (5)C29—H29A0.9800
N2—C81.458 (5)C29—H29B0.9800
N3—C11.437 (5)C30—C311.510 (8)
N4—C201.337 (5)C30—H30A0.9800
N4—C211.465 (5)C30—H30B0.9800
N5—C201.329 (5)C31—C321.523 (6)
N5—C271.459 (5)C31—H31A0.9800
N6—C201.442 (5)C31—H31B0.9800
C2—C31.520 (6)C32—H32A0.9800
C2—C71.531 (5)C32—H32B0.9800
C2—H20.9900C33—H33A0.9700
C3—C41.535 (6)C33—H33B0.9700
C3—H3A0.9800C33—H33C0.9700
C3—H3B0.9800C34—H34A0.9700
C4—C51.518 (6)C34—H34B0.9700
C4—H4A0.9800C34—H34C0.9700
C4—H4B0.9800C35—H35A0.9700
C5—C61.521 (7)C35—H35B0.9700
C5—H5A0.9800C35—H35C0.9700
C5—H5B0.9800C36—H36A0.9700
C6—C71.530 (6)C36—H36B0.9700
C6—H6A0.9800C36—H36C0.9700
C6—H6B0.9800C37—H37A0.9700
C7—H7A0.9800C37—H37B0.9700
C7—H7B0.9800C37—H37C0.9700
C8—C131.523 (6)C38—H38A0.9700
C8—C91.530 (6)C38—H38B0.9700
C8—H80.9900C38—H38C0.9700
C9—C101.522 (6)C39—C401.483 (8)
C9—H9A0.9800C39—H39A0.9800
C9—H9B0.9800C39—H39B0.9800
C10—C111.504 (8)C40—C411.487 (9)
C10—H10A0.9800C40—H40A0.9800
C10—H10B0.9800C40—H40B0.9800
C11—C121.520 (9)C41—C421.515 (8)
C11—H11A0.9800C41—H41A0.9800
C11—H11B0.9800C41—H41B0.9800
C12—C131.542 (7)C42—H42A0.9800
C12—H12A0.9800C42—H42B0.9800
C12—H12B0.9800C43—C441.438 (7)
C13—H13A0.9800C43—H43A0.9800
C13—H13B0.9800C43—H43B0.9800
C14—H14A0.9700C44—C451.480 (7)
C14—H14B0.9700C44—H44A0.9800
C14—H14C0.9700C44—H44B0.9800
C15—H15A0.9700C45—C461.466 (7)
C15—H15B0.9700C45—H45A0.9800
C15—H15C0.9700C45—H45B0.9800
C16—H16A0.9700C46—H46A0.9800
C16—H16B0.9700C46—H46B0.9800
N2—Nd1—N596.62 (12)H17A—C17—H17C109.5
N2—Nd1—N154.47 (11)H17B—C17—H17C109.5
N5—Nd1—N1111.38 (11)Si2—C18—H18A109.5
N2—Nd1—N4106.36 (11)Si2—C18—H18B109.5
N5—Nd1—N454.47 (10)H18A—C18—H18B109.5
N1—Nd1—N4157.35 (12)Si2—C18—H18C109.5
N2—Nd1—Cl199.85 (8)H18A—C18—H18C109.5
N5—Nd1—Cl1147.58 (8)H18B—C18—H18C109.5
N1—Nd1—Cl1100.91 (8)Si2—C19—H19A109.5
N4—Nd1—Cl193.95 (8)Si2—C19—H19B109.5
N2—Nd1—Cl2146.42 (8)H19A—C19—H19B109.5
N5—Nd1—Cl299.68 (8)Si2—C19—H19C109.5
N1—Nd1—Cl292.15 (8)H19A—C19—H19C109.5
N4—Nd1—Cl2107.02 (9)H19B—C19—H19C109.5
Cl1—Nd1—Cl281.42 (3)N5—C20—N4114.6 (4)
N2—Nd1—C127.26 (10)N5—C20—N6122.7 (4)
N5—Nd1—C1107.92 (11)N4—C20—N6122.7 (3)
N1—Nd1—C127.40 (10)N5—C20—Nd156.5 (2)
N4—Nd1—C1133.26 (12)N4—C20—Nd159.2 (2)
Cl1—Nd1—C199.31 (8)N6—C20—Nd1169.1 (3)
Cl2—Nd1—C1119.17 (8)N4—C21—C22111.6 (4)
N2—Nd1—C20106.13 (12)N4—C21—C26109.9 (4)
N5—Nd1—C2027.27 (10)C22—C21—C26109.5 (4)
N1—Nd1—C20137.72 (11)N4—C21—H21108.6
N4—Nd1—C2027.57 (10)C22—C21—H21108.6
Cl1—Nd1—C20120.45 (9)C26—C21—H21108.6
Cl2—Nd1—C20101.71 (8)C21—C22—C23110.8 (4)
C1—Nd1—C20126.73 (12)C21—C22—H22A109.5
N2—Nd1—Li1134.25 (14)C23—C22—H22A109.5
N5—Nd1—Li1129.07 (14)C21—C22—H22B109.5
N1—Nd1—Li1102.41 (15)C23—C22—H22B109.5
N4—Nd1—Li1100.02 (15)H22A—C22—H22B108.1
Cl1—Nd1—Li140.87 (11)C24—C23—C22110.7 (5)
Cl2—Nd1—Li140.85 (11)C24—C23—H23A109.5
C1—Nd1—Li1119.04 (15)C22—C23—H23A109.5
C20—Nd1—Li1114.21 (15)C24—C23—H23B109.5
Li1—Cl1—Nd188.43 (19)C22—C23—H23B109.5
Li1—Cl2—Nd188.34 (19)H23A—C23—H23B108.1
N3—Si1—C16108.57 (19)C23—C24—C25111.3 (5)
N3—Si1—C14111.7 (2)C23—C24—H24A109.4
C16—Si1—C14108.7 (3)C25—C24—H24A109.4
N3—Si1—C15111.5 (2)C23—C24—H24B109.4
C16—Si1—C15109.5 (3)C25—C24—H24B109.4
C14—Si1—C15106.7 (3)H24A—C24—H24B108.0
N3—Si2—C17109.71 (19)C24—C25—C26111.7 (5)
N3—Si2—C19111.5 (2)C24—C25—H25A109.3
C17—Si2—C19108.8 (2)C26—C25—H25A109.3
N3—Si2—C18110.9 (2)C24—C25—H25B109.3
C17—Si2—C18109.1 (3)C26—C25—H25B109.3
C19—Si2—C18106.8 (3)H25A—C25—H25B107.9
N6—Si3—C34112.1 (2)C21—C26—C25110.2 (4)
N6—Si3—C33109.3 (2)C21—C26—H26A109.6
C34—Si3—C33108.6 (3)C25—C26—H26A109.6
N6—Si3—C35110.5 (2)C21—C26—H26B109.6
C34—Si3—C35106.8 (3)C25—C26—H26B109.6
C33—Si3—C35109.4 (3)H26A—C26—H26B108.1
N6—Si4—C38110.51 (19)N5—C27—C32109.5 (3)
N6—Si4—C36110.6 (2)N5—C27—C28111.5 (3)
C38—Si4—C36110.0 (2)C32—C27—C28109.1 (4)
N6—Si4—C37111.6 (2)N5—C27—H27108.9
C38—Si4—C37108.4 (3)C32—C27—H27108.9
C36—Si4—C37105.6 (3)C28—C27—H27108.9
C42—O1—C39107.7 (4)C27—C28—C29111.7 (4)
C42—O1—Li1124.5 (4)C27—C28—H28A109.3
C39—O1—Li1116.2 (4)C29—C28—H28A109.3
C46—O2—C43110.5 (4)C27—C28—H28B109.3
C46—O2—Li1124.0 (4)C29—C28—H28B109.3
C43—O2—Li1124.6 (4)H28A—C28—H28B108.0
C1—N1—C2122.8 (3)C30—C29—C28110.7 (5)
C1—N1—Nd194.1 (2)C30—C29—H29A109.5
C2—N1—Nd1140.3 (3)C28—C29—H29A109.5
C1—N2—C8123.4 (3)C30—C29—H29B109.5
C1—N2—Nd196.7 (2)C28—C29—H29B109.5
C8—N2—Nd1139.8 (3)H29A—C29—H29B108.1
C1—N3—Si1117.2 (2)C31—C30—C29111.0 (5)
C1—N3—Si2117.6 (2)C31—C30—H30A109.4
Si1—N3—Si2125.24 (19)C29—C30—H30A109.4
C20—N4—C21122.3 (3)C31—C30—H30B109.4
C20—N4—Nd193.2 (2)C29—C30—H30B109.4
C21—N4—Nd1141.9 (3)H30A—C30—H30B108.0
C20—N5—C27123.4 (3)C30—C31—C32111.2 (5)
C20—N5—Nd196.2 (2)C30—C31—H31A109.4
C27—N5—Nd1138.8 (2)C32—C31—H31A109.4
C20—N6—Si3117.8 (3)C30—C31—H31B109.4
C20—N6—Si4118.4 (3)C32—C31—H31B109.4
Si3—N6—Si4123.82 (19)H31A—C31—H31B108.0
N2—C1—N1113.9 (3)C31—C32—C27111.4 (4)
N2—C1—N3122.9 (4)C31—C32—H32A109.3
N1—C1—N3123.2 (3)C27—C32—H32A109.3
N2—C1—Nd156.0 (2)C31—C32—H32B109.3
N1—C1—Nd158.5 (2)C27—C32—H32B109.3
N3—C1—Nd1172.3 (3)H32A—C32—H32B108.0
N1—C2—C3110.9 (3)Si3—C33—H33A109.5
N1—C2—C7110.1 (3)Si3—C33—H33B109.5
C3—C2—C7109.5 (3)H33A—C33—H33B109.5
N1—C2—H2108.8Si3—C33—H33C109.5
C3—C2—H2108.8H33A—C33—H33C109.5
C7—C2—H2108.8H33B—C33—H33C109.5
C2—C3—C4112.2 (3)Si3—C34—H34A109.5
C2—C3—H3A109.2Si3—C34—H34B109.5
C4—C3—H3A109.2H34A—C34—H34B109.5
C2—C3—H3B109.2Si3—C34—H34C109.5
C4—C3—H3B109.2H34A—C34—H34C109.5
H3A—C3—H3B107.9H34B—C34—H34C109.5
C5—C4—C3111.4 (4)Si3—C35—H35A109.5
C5—C4—H4A109.4Si3—C35—H35B109.5
C3—C4—H4A109.4H35A—C35—H35B109.5
C5—C4—H4B109.4Si3—C35—H35C109.5
C3—C4—H4B109.4H35A—C35—H35C109.5
H4A—C4—H4B108.0H35B—C35—H35C109.5
C4—C5—C6110.1 (4)Si4—C36—H36A109.5
C4—C5—H5A109.6Si4—C36—H36B109.5
C6—C5—H5A109.6H36A—C36—H36B109.5
C4—C5—H5B109.6Si4—C36—H36C109.5
C6—C5—H5B109.6H36A—C36—H36C109.5
H5A—C5—H5B108.1H36B—C36—H36C109.5
C5—C6—C7111.7 (4)Si4—C37—H37A109.5
C5—C6—H6A109.3Si4—C37—H37B109.5
C7—C6—H6A109.3H37A—C37—H37B109.5
C5—C6—H6B109.3Si4—C37—H37C109.5
C7—C6—H6B109.3H37A—C37—H37C109.5
H6A—C6—H6B107.9H37B—C37—H37C109.5
C6—C7—C2111.1 (4)Si4—C38—H38A109.5
C6—C7—H7A109.4Si4—C38—H38B109.5
C2—C7—H7A109.4H38A—C38—H38B109.5
C6—C7—H7B109.4Si4—C38—H38C109.5
C2—C7—H7B109.4H38A—C38—H38C109.5
H7A—C7—H7B108.0H38B—C38—H38C109.5
N2—C8—C13109.1 (4)O1—C39—C40108.2 (5)
N2—C8—C9111.2 (3)O1—C39—H39A110.1
C13—C8—C9108.8 (4)C40—C39—H39A110.1
N2—C8—H8109.2O1—C39—H39B110.1
C13—C8—H8109.2C40—C39—H39B110.1
C9—C8—H8109.2H39A—C39—H39B108.4
C10—C9—C8113.4 (4)C39—C40—C41104.0 (5)
C10—C9—H9A108.9C39—C40—H40A111.0
C8—C9—H9A108.9C41—C40—H40A111.0
C10—C9—H9B108.9C39—C40—H40B111.0
C8—C9—H9B108.9C41—C40—H40B111.0
H9A—C9—H9B107.7H40A—C40—H40B109.0
C11—C10—C9110.9 (5)C40—C41—C42103.1 (6)
C11—C10—H10A109.5C40—C41—H41A111.1
C9—C10—H10A109.5C42—C41—H41A111.1
C11—C10—H10B109.5C40—C41—H41B111.1
C9—C10—H10B109.5C42—C41—H41B111.1
H10A—C10—H10B108.0H41A—C41—H41B109.1
C10—C11—C12111.4 (5)O1—C42—C41104.4 (5)
C10—C11—H11A109.3O1—C42—H42A110.9
C12—C11—H11A109.3C41—C42—H42A110.9
C10—C11—H11B109.3O1—C42—H42B110.9
C12—C11—H11B109.3C41—C42—H42B110.9
H11A—C11—H11B108.0H42A—C42—H42B108.9
C11—C12—C13111.4 (5)O2—C43—C44105.7 (5)
C11—C12—H12A109.4O2—C43—H43A110.6
C13—C12—H12A109.4C44—C43—H43A110.6
C11—C12—H12B109.4O2—C43—H43B110.6
C13—C12—H12B109.4C44—C43—H43B110.6
H12A—C12—H12B108.0H43A—C43—H43B108.7
C8—C13—C12111.3 (5)C43—C44—C45106.9 (5)
C8—C13—H13A109.4C43—C44—H44A110.3
C12—C13—H13A109.4C45—C44—H44A110.3
C8—C13—H13B109.4C43—C44—H44B110.3
C12—C13—H13B109.4C45—C44—H44B110.3
H13A—C13—H13B108.0H44A—C44—H44B108.6
Si1—C14—H14A109.5C46—C45—C44104.9 (5)
Si1—C14—H14B109.5C46—C45—H45A110.8
H14A—C14—H14B109.5C44—C45—H45A110.8
Si1—C14—H14C109.5C46—C45—H45B110.8
H14A—C14—H14C109.5C44—C45—H45B110.8
H14B—C14—H14C109.5H45A—C45—H45B108.8
Si1—C15—H15A109.5O2—C46—C45106.7 (5)
Si1—C15—H15B109.5O2—C46—H46A110.4
H15A—C15—H15B109.5C45—C46—H46A110.4
Si1—C15—H15C109.5O2—C46—H46B110.4
H15A—C15—H15C109.5C45—C46—H46B110.4
H15B—C15—H15C109.5H46A—C46—H46B108.6
Si1—C16—H16A109.5O1—Li1—O2100.0 (4)
Si1—C16—H16B109.5O1—Li1—Cl2113.7 (3)
H16A—C16—H16B109.5O2—Li1—Cl2107.6 (3)
Si1—C16—H16C109.5O1—Li1—Cl1122.5 (4)
H16A—C16—H16C109.5O2—Li1—Cl1111.4 (4)
H16B—C16—H16C109.5Cl2—Li1—Cl1101.1 (3)
Si2—C17—H17A109.5O1—Li1—Nd1143.1 (3)
Si2—C17—H17B109.5O2—Li1—Nd1116.3 (4)
H17A—C17—H17B109.5Cl2—Li1—Nd150.82 (16)
Si2—C17—H17C109.5Cl1—Li1—Nd150.70 (16)
N2—Nd1—Cl1—Li1151.9 (2)Nd1—N2—C8—C1335.5 (6)
N5—Nd1—Cl1—Li188.7 (2)C1—N2—C8—C9101.0 (5)
N1—Nd1—Cl1—Li196.4 (2)Nd1—N2—C8—C984.5 (5)
N4—Nd1—Cl1—Li1100.8 (2)N2—C8—C9—C10175.9 (4)
Cl2—Nd1—Cl1—Li15.87 (19)C13—C8—C9—C1055.7 (6)
C1—Nd1—Cl1—Li1124.2 (2)C8—C9—C10—C1155.5 (7)
C20—Nd1—Cl1—Li192.7 (2)C9—C10—C11—C1254.2 (7)
N2—Nd1—Cl2—Li1100.8 (2)C10—C11—C12—C1355.4 (7)
N5—Nd1—Cl2—Li1141.3 (2)N2—C8—C13—C12176.9 (4)
N1—Nd1—Cl2—Li1106.6 (2)C9—C8—C13—C1255.5 (6)
N4—Nd1—Cl2—Li185.7 (2)C11—C12—C13—C856.7 (7)
Cl1—Nd1—Cl2—Li15.87 (19)C27—N5—C20—N4179.6 (4)
C1—Nd1—Cl2—Li1101.8 (2)Nd1—N5—C20—N412.1 (4)
C20—Nd1—Cl2—Li1113.6 (2)C27—N5—C20—N61.2 (6)
N2—Nd1—N1—C15.2 (2)Nd1—N5—C20—N6167.1 (3)
N5—Nd1—N1—C187.9 (2)C27—N5—C20—Nd1168.3 (4)
N4—Nd1—N1—C140.9 (4)C21—N4—C20—N5177.3 (4)
Cl1—Nd1—N1—C189.2 (2)Nd1—N4—C20—N511.8 (4)
Cl2—Nd1—N1—C1170.9 (2)C21—N4—C20—N61.9 (6)
C20—Nd1—N1—C179.0 (3)Nd1—N4—C20—N6167.4 (3)
Li1—Nd1—N1—C1131.0 (2)C21—N4—C20—Nd1165.5 (4)
N2—Nd1—N1—C2164.8 (4)Si3—N6—C20—N596.4 (4)
N5—Nd1—N1—C2112.5 (4)Si4—N6—C20—N584.4 (5)
N4—Nd1—N1—C2159.5 (3)Si3—N6—C20—N484.5 (5)
Cl1—Nd1—N1—C270.4 (4)Si4—N6—C20—N494.8 (4)
Cl2—Nd1—N1—C211.3 (4)Si3—N6—C20—Nd1179 (100)
C1—Nd1—N1—C2159.6 (5)Si4—N6—C20—Nd12.0 (16)
C20—Nd1—N1—C2121.3 (4)N2—Nd1—C20—N572.6 (3)
Li1—Nd1—N1—C228.7 (4)N1—Nd1—C20—N518.1 (3)
N5—Nd1—N2—C1116.8 (2)N4—Nd1—C20—N5167.2 (4)
N1—Nd1—N2—C15.2 (2)Cl1—Nd1—C20—N5175.3 (2)
N4—Nd1—N2—C1171.7 (2)Cl2—Nd1—C20—N588.4 (2)
Cl1—Nd1—N2—C191.2 (2)C1—Nd1—C20—N552.4 (3)
Cl2—Nd1—N2—C11.9 (3)Li1—Nd1—C20—N5129.5 (3)
C20—Nd1—N2—C1142.9 (2)N2—Nd1—C20—N494.6 (3)
Li1—Nd1—N2—C165.7 (3)N5—Nd1—C20—N4167.2 (4)
N5—Nd1—N2—C867.8 (4)N1—Nd1—C20—N4149.0 (2)
N1—Nd1—N2—C8179.4 (5)Cl1—Nd1—C20—N417.6 (3)
N4—Nd1—N2—C813.0 (4)Cl2—Nd1—C20—N4104.4 (2)
Cl1—Nd1—N2—C884.1 (4)C1—Nd1—C20—N4114.7 (3)
Cl2—Nd1—N2—C8173.4 (3)Li1—Nd1—C20—N463.3 (3)
C1—Nd1—N2—C8175.4 (6)N2—Nd1—C20—N6162.1 (15)
C20—Nd1—N2—C841.7 (4)N5—Nd1—C20—N689.5 (15)
Li1—Nd1—N2—C8109.7 (4)N1—Nd1—C20—N6107.6 (15)
C16—Si1—N3—C18.7 (4)N4—Nd1—C20—N6103.4 (15)
C14—Si1—N3—C1128.6 (3)Cl1—Nd1—C20—N685.8 (15)
C15—Si1—N3—C1112.1 (3)Cl2—Nd1—C20—N61.0 (15)
C16—Si1—N3—Si2172.2 (3)C1—Nd1—C20—N6141.9 (14)
C14—Si1—N3—Si252.4 (3)Li1—Nd1—C20—N640.0 (15)
C15—Si1—N3—Si267.0 (3)C20—N4—C21—C22103.6 (5)
C17—Si2—N3—C16.7 (4)Nd1—N4—C21—C2252.6 (6)
C19—Si2—N3—C1127.3 (3)C20—N4—C21—C26134.8 (4)
C18—Si2—N3—C1113.9 (4)Nd1—N4—C21—C2669.1 (6)
C17—Si2—N3—Si1172.3 (3)N4—C21—C22—C23178.9 (4)
C19—Si2—N3—Si151.7 (3)C26—C21—C22—C2359.2 (5)
C18—Si2—N3—Si167.1 (3)C21—C22—C23—C2457.8 (6)
N2—Nd1—N4—C2093.6 (3)C22—C23—C24—C2554.8 (7)
N5—Nd1—N4—C207.2 (2)C23—C24—C25—C2654.8 (7)
N1—Nd1—N4—C2064.0 (4)N4—C21—C26—C25178.9 (5)
Cl1—Nd1—N4—C20164.9 (2)C22—C21—C26—C2558.2 (6)
Cl2—Nd1—N4—C2082.7 (2)C24—C25—C26—C2156.3 (7)
C1—Nd1—N4—C2088.4 (3)C20—N5—C27—C32138.5 (4)
Li1—Nd1—N4—C20124.1 (3)Nd1—N5—C27—C3223.6 (6)
N2—Nd1—N4—C21106.4 (4)C20—N5—C27—C28100.7 (5)
N5—Nd1—N4—C21167.2 (5)Nd1—N5—C27—C2897.2 (5)
N1—Nd1—N4—C21136.0 (4)N5—C27—C28—C29177.9 (4)
Cl1—Nd1—N4—C214.9 (4)C32—C27—C28—C2956.8 (5)
Cl2—Nd1—N4—C2177.3 (4)C27—C28—C29—C3056.1 (6)
C1—Nd1—N4—C21111.6 (4)C28—C29—C30—C3154.8 (6)
C20—Nd1—N4—C21160.0 (6)C29—C30—C31—C3255.8 (7)
Li1—Nd1—N4—C2135.9 (5)C30—C31—C32—C2757.8 (6)
N2—Nd1—N5—C20112.7 (2)N5—C27—C32—C31179.7 (4)
N1—Nd1—N5—C20167.0 (2)C28—C27—C32—C3157.5 (5)
N4—Nd1—N5—C207.3 (2)C42—O1—C39—C404.4 (6)
Cl1—Nd1—N5—C207.6 (3)Li1—O1—C39—C40140.5 (5)
Cl2—Nd1—N5—C2096.8 (2)O1—C39—C40—C4118.1 (7)
C1—Nd1—N5—C20138.1 (2)C39—C40—C41—C4232.3 (7)
Li1—Nd1—N5—C2065.0 (3)C39—O1—C42—C4124.7 (6)
N2—Nd1—N5—C2782.2 (4)Li1—O1—C42—C41116.6 (5)
N1—Nd1—N5—C2727.9 (4)C40—C41—C42—O135.4 (6)
N4—Nd1—N5—C27172.4 (5)C46—O2—C43—C4412.9 (8)
Cl1—Nd1—N5—C27157.5 (3)Li1—O2—C43—C44156.6 (6)
Cl2—Nd1—N5—C2768.3 (4)O2—C43—C44—C4522.0 (9)
C1—Nd1—N5—C2756.8 (4)C43—C44—C45—C4622.8 (9)
C20—Nd1—N5—C27165.1 (6)C43—O2—C46—C451.4 (9)
Li1—Nd1—N5—C27100.1 (4)Li1—O2—C46—C45171.0 (5)
C34—Si3—N6—C20115.2 (3)C44—C45—C46—O214.7 (9)
C33—Si3—N6—C205.3 (4)C42—O1—Li1—O2164.3 (4)
C35—Si3—N6—C20125.8 (3)C39—O1—Li1—O257.3 (5)
C34—Si3—N6—Si465.7 (3)C42—O1—Li1—Cl281.2 (5)
C33—Si3—N6—Si4173.9 (3)C39—O1—Li1—Cl257.1 (5)
C35—Si3—N6—Si453.4 (3)C42—O1—Li1—Cl140.8 (6)
C38—Si4—N6—C2010.9 (4)C39—O1—Li1—Cl1179.1 (4)
C36—Si4—N6—C20133.0 (3)C42—O1—Li1—Nd125.6 (7)
C37—Si4—N6—C20109.7 (3)C39—O1—Li1—Nd1112.8 (6)
C38—Si4—N6—Si3169.9 (2)C46—O2—Li1—O169.5 (6)
C36—Si4—N6—Si347.8 (3)C43—O2—Li1—O198.6 (6)
C37—Si4—N6—Si369.4 (3)C46—O2—Li1—Cl2171.5 (5)
C8—N2—C1—N1175.0 (4)C43—O2—Li1—Cl220.4 (7)
Nd1—N2—C1—N18.6 (4)C46—O2—Li1—Cl161.5 (7)
C8—N2—C1—N35.5 (6)C43—O2—Li1—Cl1130.4 (5)
Nd1—N2—C1—N3170.9 (3)C46—O2—Li1—Nd1117.1 (5)
C8—N2—C1—Nd1176.4 (4)C43—O2—Li1—Nd174.8 (6)
C2—N1—C1—N2173.0 (3)Nd1—Cl2—Li1—O1140.2 (3)
Nd1—N1—C1—N28.4 (3)Nd1—Cl2—Li1—O2109.9 (3)
C2—N1—C1—N36.5 (6)Nd1—Cl2—Li1—Cl17.0 (2)
Nd1—N1—C1—N3171.1 (3)Nd1—Cl1—Li1—O1134.7 (4)
C2—N1—C1—Nd1164.6 (4)Nd1—Cl1—Li1—O2107.1 (4)
Si1—N3—C1—N296.6 (4)Nd1—Cl1—Li1—Cl27.0 (2)
Si2—N3—C1—N282.5 (4)N2—Nd1—Li1—O153.4 (6)
Si1—N3—C1—N183.9 (4)N5—Nd1—Li1—O1129.8 (5)
Si2—N3—C1—N197.0 (4)N1—Nd1—Li1—O11.5 (5)
N5—Nd1—C1—N268.7 (2)N4—Nd1—Li1—O1178.3 (5)
N1—Nd1—C1—N2170.8 (4)Cl1—Nd1—Li1—O193.9 (5)
N4—Nd1—C1—N211.0 (3)Cl2—Nd1—Li1—O177.2 (5)
Cl1—Nd1—C1—N293.5 (2)C1—Nd1—Li1—O124.9 (6)
Cl2—Nd1—C1—N2178.8 (2)C20—Nd1—Li1—O1156.9 (5)
C20—Nd1—C1—N246.3 (3)N2—Nd1—Li1—O2137.5 (3)
Li1—Nd1—C1—N2131.7 (2)N5—Nd1—Li1—O239.3 (4)
N2—Nd1—C1—N1170.8 (4)N1—Nd1—Li1—O2170.6 (3)
N5—Nd1—C1—N1102.1 (2)N4—Nd1—Li1—O212.6 (3)
N4—Nd1—C1—N1159.8 (2)Cl1—Nd1—Li1—O297.0 (3)
Cl1—Nd1—C1—N195.8 (2)Cl2—Nd1—Li1—O291.9 (3)
Cl2—Nd1—C1—N110.4 (3)C1—Nd1—Li1—O2166.0 (3)
C20—Nd1—C1—N1124.5 (2)C20—Nd1—Li1—O212.2 (3)
Li1—Nd1—C1—N157.5 (3)N2—Nd1—Li1—Cl2130.66 (15)
C1—N1—C2—C3102.9 (4)N5—Nd1—Li1—Cl252.6 (2)
Nd1—N1—C2—C352.7 (5)N1—Nd1—Li1—Cl278.71 (17)
C1—N1—C2—C7135.7 (4)N4—Nd1—Li1—Cl2104.48 (16)
Nd1—N1—C2—C768.7 (5)Cl1—Nd1—Li1—Cl2171.1 (3)
N1—C2—C3—C4177.4 (3)C1—Nd1—Li1—Cl2102.13 (17)
C7—C2—C3—C455.7 (5)C20—Nd1—Li1—Cl279.65 (18)
C2—C3—C4—C556.1 (5)N2—Nd1—Li1—Cl140.4 (3)
C3—C4—C5—C655.0 (5)N5—Nd1—Li1—Cl1136.34 (14)
C4—C5—C6—C756.2 (5)N1—Nd1—Li1—Cl192.40 (17)
C5—C6—C7—C257.4 (5)N4—Nd1—Li1—Cl184.41 (17)
N1—C2—C7—C6178.3 (4)Cl2—Nd1—Li1—Cl1171.1 (3)
C3—C2—C7—C656.1 (5)C1—Nd1—Li1—Cl169.0 (2)
C1—N2—C8—C13139.0 (4)C20—Nd1—Li1—Cl1109.24 (16)

Experimental details

Crystal data
Chemical formula[LiNd(C19H40N3Si2)2Cl2(C4H8O)2]
Mr1099.73
Crystal system, space groupMonoclinic, P21/c
Temperature (K)223
a, b, c (Å)24.1739 (16), 13.5238 (8), 18.8108 (13)
β (°) 103.215 (2)
V3)5986.8 (7)
Z4
Radiation typeMo Kα
µ (mm1)1.07
Crystal size (mm)0.40 × 0.40 × 0.30
Data collection
DiffractometerRigaku Saturn
diffractometer
Absorption correctionMulti-scan
(REQAB; Jacobson, 1998)
Tmin, Tmax0.464, 0.752
No. of measured, independent and
observed [I > 2σ(I)] reflections
35442, 11104, 9767
Rint0.051
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.111, 1.17
No. of reflections11104
No. of parameters554
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.74, 1.21

Computer programs: CrystalClear (Rigaku, 2000), CrystalStructure (Rigaku, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Li1—Cl12.336 (7)Nd1—Cl22.7667 (11)
Li1—Cl22.335 (7)Nd1—N12.462 (3)
Li1—O11.907 (9)Nd1—N22.405 (3)
Li1—O21.951 (8)Nd1—N42.481 (3)
Nd1—Cl12.7621 (11)Nd1—N52.419 (3)
 

Acknowledgements

The authors thank Yong Zhang of Suzhou University for the data collection.

References

First citationJacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.
First citationLuo, Y. J., Yao, Y. M., Shen, Q., Yu, K. B. & Weng, L. H. (2003). Eur. J. Inorg. Chem. pp. 318–323.  CSD CrossRef
First citationRigaku (2000). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationTrifonov, A. A. (2010). Coord. Chem. Rev. 254, 1327–1347.  Web of Science CrossRef CAS

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