metal-organic compounds
catena-Poly[{μ-η5:η5-1-[2-(dimethylamino)ethyl-κN]cyclopentadienyl}-lithium(I)-(μ-1,1,3,3-tetra-tert-butyltriphosphane-κ3P2:P1,P3)lithium(I)]
aChemical Faculty, Gdansk University of Technology, G. Narutowicza 11/12, Gdansk PL-80233, Poland
*Correspondence e-mail: jaroslaw.chojnacki@chem.pg.gda.pl
The title compound, [Li2(C9H14N)(C16H36P3)]n, is a by-product of the reaction of [Cp(C5H4CH2CH2NMe2)ZrCl2]n with tBu2P–P(SiMe3)Li in toluene. It is a coordination polymer composed of infinite chains running along [010]. One Li(I) atom is chelated by the cyclopentadienyl ring and and the N atom of the scorpionate ligand and a P atom, whereas the other Li(I) atom is coordinated by the backside of the cyclopentadienyl ring and two P atoms. Both Li(I) atoms adopt a distorted trigonal coordination. The structure was determined from a twinned crystal, but only the data from the main twin component was used. The fraction of components in the crystal was 0.555:0.445 and the twin matrix corresponds to twofold rotation about the c axis (00/00/001).
Related literature
For the synthesis, see: Chojnacki et al. (2007); Kovacs et al. (1996b). For related structures, see: Kovacs et al. (1996a); Kunz et al. (2000).
Experimental
Crystal data
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Data collection: CrysAlis PRO (Oxford Diffraction, 2009); cell CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Supporting information
https://doi.org/10.1107/S1600536810039759/bt5361sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810039759/bt5361Isup2.hkl
The work was carried out using the standard vacuum-nitrogen line and Schlenk techniques. [Cp(C5H4CH2CH2NMe2)ZrCl2]n and tBu2P—P(SiMe3)Li . 3 THF were prepared according to the procedure described in the literature (Chojnacki et al., 2007; Kovacs et al., 1996b). Suspension of 0.105 g (0.289 mmole) [Cp(C5H4CH2CH2NMe2)ZrCl2]n in 2 ml toluene was added dropwise into solution of 0.264 g (0.559 mmole) tBu2P—P(SiMe3)Li.3THF in 2 ml of toluene at 233 K. The mixture immediately turned red. Then the volume was reduced to about 2 ml and the concentrate was stored for a few weeks at room temperature. After this time the solution yielded colourless crystals of (I).
The structure turned out to be a rotational twin, only the data from the main twin component was used. The fraction of components in crystal was 0.555 / 0.444. The twin matrix corresponds to 2-fold rotation about c axis (-1 0 0 / 0 -1 0 / 0 0 1).
The schematic structure of the linear coordination polymer of (I) is shown in Fig.1. The monomeric unit of the title compound consists of two lithium atoms and two ligands: (tBu2P)2P and C5H4CH2CH2NMe2. Both lithium atoms adopt distorted trigonal geometry. Li1 atom is bonded in a η5-fashion from the one face of C5H4 ring system and is also bonded with two terminal phosphorous atoms P2, P3 from a (tBu2P)2P ligand. Atom Li2 is coordinated by atom P1 from another triphosphane ligand and is η5-coordinated to the other face of the C5H4 ring system, assisted by κN-coordination of the attached dimethylamino substituent. Atoms Li1, P1, P2, P3 form a planar ring (maximum deviation 0.069 Å). The two lithium atoms and C5H4 ring form an "inverse sandwich". The structure of (tBu2P)2P ligand in complex (I) is similar to the one found for [Li(THF)2{η2-(tBu2P)2P}] (Kovacs et al., 1996a) with comparable P–P and P–Li distances. To the best of our knowledge only one example of lithium complex with substituted Cp ligand which exhibits κN and η5-coordination to the same lithium atom is known (Kunz et al., 2000). Li–N distance in complex [{C5H4CH(Ph)NMe2}Li]n (Kunz et al., 2000) and in the title compound are similar [2.227 (5) Å; 2.237 (12) Å].
For the synthesis, see: Chojnacki et al. (2007); Kovacs et al. (1996b). For related structures, see: Kovacs et al. (1996a); Kunz et al. (2000).
Data collection: CrysAlis PRO (Oxford Diffraction, 2009); cell
CrysAlis PRO (Oxford Diffraction, 2009); data reduction: CrysAlis PRO (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).Fig. 1. The asymmetric unit of the title compound. Ellipsoids are drawn at the 50% probability level. | |
Fig. 2. Coordination polymer of the title compound. |
[Li2(C9H14N)(C16H36P3)] | F(000) = 1032 |
Mr = 471.45 | Dx = 1.064 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9383 reflections |
a = 8.9063 (6) Å | θ = 2.4–32.4° |
b = 18.8522 (8) Å | µ = 0.21 mm−1 |
c = 19.3934 (17) Å | T = 120 K |
β = 115.314 (6)° | Block, colourless |
V = 2943.5 (3) Å3 | 0.44 × 0.23 × 0.2 mm |
Z = 4 |
Oxford Diffraction Xcalibur diffractometer with a Sapphire2 (large Be window) detector | 4818 independent reflections |
Graphite monochromator | 3492 reflections with I > 2σ(I) |
Detector resolution: 8.1883 pixels mm-1 | Rint = 0.093 |
ω scans | θmax = 25.1°, θmin = 2.5° |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009) | h = −10→10 |
Tmin = 0.734, Tmax = 1 | k = −22→21 |
14505 measured reflections | l = −23→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.095 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.258 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0825P)2 + 14.0784P] where P = (Fo2 + 2Fc2)/3 |
4818 reflections | (Δ/σ)max = 0.001 |
294 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
[Li2(C9H14N)(C16H36P3)] | V = 2943.5 (3) Å3 |
Mr = 471.45 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.9063 (6) Å | µ = 0.21 mm−1 |
b = 18.8522 (8) Å | T = 120 K |
c = 19.3934 (17) Å | 0.44 × 0.23 × 0.2 mm |
β = 115.314 (6)° |
Oxford Diffraction Xcalibur diffractometer with a Sapphire2 (large Be window) detector | 4818 independent reflections |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009) | 3492 reflections with I > 2σ(I) |
Tmin = 0.734, Tmax = 1 | Rint = 0.093 |
14505 measured reflections |
R[F2 > 2σ(F2)] = 0.095 | 0 restraints |
wR(F2) = 0.258 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0825P)2 + 14.0784P] where P = (Fo2 + 2Fc2)/3 |
4818 reflections | Δρmax = 0.72 e Å−3 |
294 parameters | Δρmin = −0.61 e Å−3 |
Experimental. Absorption correction: CrysAlisPro, Oxford Diffraction (2009). Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
P1 | 0.3565 (2) | 0.56638 (7) | 0.24090 (8) | 0.0290 (4) | |
P2 | 0.51867 (18) | 0.63068 (7) | 0.33654 (8) | 0.0269 (4) | |
P3 | 0.33668 (18) | 0.64220 (7) | 0.15340 (8) | 0.0260 (4) | |
N1 | 0.9399 (6) | 0.9125 (3) | 0.2580 (3) | 0.0349 (12) | |
Li1 | 0.5000 (13) | 0.7397 (5) | 0.2529 (6) | 0.032 (2) | |
Li2 | 0.3071 (13) | 0.4320 (5) | 0.2412 (6) | 0.036 (2) | |
C1 | 0.7050 (7) | 0.8108 (3) | 0.2625 (3) | 0.0319 (13) | |
C2 | 0.5670 (8) | 0.8291 (3) | 0.1954 (3) | 0.0369 (14) | |
H2 | 0.5578 | 0.8235 | 0.145 | 0.044* | |
C3 | 0.4453 (8) | 0.8569 (3) | 0.2148 (4) | 0.0450 (17) | |
H3 | 0.3384 | 0.8727 | 0.1799 | 0.054* | |
C4 | 0.5056 (9) | 0.8575 (3) | 0.2927 (4) | 0.0460 (17) | |
H4 | 0.4478 | 0.8738 | 0.321 | 0.055* | |
C5 | 0.6659 (9) | 0.8301 (3) | 0.3232 (3) | 0.0400 (16) | |
H5 | 0.737 | 0.8252 | 0.376 | 0.048* | |
C6 | 0.8712 (9) | 0.7859 (4) | 0.2700 (5) | 0.0536 (19) | |
H6A | 0.8619 | 0.7704 | 0.2206 | 0.064* | |
H6B | 0.9075 | 0.7458 | 0.3046 | 0.064* | |
C7 | 0.9994 (9) | 0.8457 (4) | 0.3003 (5) | 0.0528 (19) | |
H7A | 1.0261 | 0.8538 | 0.3537 | 0.063* | |
H7B | 1.1005 | 0.8312 | 0.2969 | 0.063* | |
C8 | 1.0617 (9) | 0.9682 (4) | 0.2961 (4) | 0.0498 (17) | |
H8A | 1.0249 | 1.0119 | 0.2687 | 0.075* | |
H8B | 1.167 | 0.9551 | 0.2973 | 0.075* | |
H8C | 1.0731 | 0.974 | 0.3473 | 0.075* | |
C9 | 0.9215 (10) | 0.9045 (4) | 0.1805 (4) | 0.0552 (19) | |
H9A | 1.0235 | 0.8871 | 0.1812 | 0.083* | |
H9B | 0.8952 | 0.9496 | 0.1551 | 0.083* | |
H9C | 0.8336 | 0.8715 | 0.1537 | 0.083* | |
C10 | 0.7138 (8) | 0.5767 (4) | 0.3918 (4) | 0.0415 (15) | |
C11 | 0.6889 (11) | 0.5100 (4) | 0.4292 (4) | 0.060 (2) | |
H11A | 0.6598 | 0.5226 | 0.4699 | 0.09* | |
H11B | 0.7898 | 0.4828 | 0.4493 | 0.09* | |
H11C | 0.6012 | 0.4822 | 0.3921 | 0.09* | |
C12 | 0.8439 (10) | 0.6256 (5) | 0.4510 (4) | 0.062 (2) | |
H12A | 0.859 | 0.667 | 0.426 | 0.093* | |
H12B | 0.9475 | 0.6007 | 0.4753 | 0.093* | |
H12C | 0.8064 | 0.6394 | 0.4887 | 0.093* | |
C13 | 0.7840 (9) | 0.5558 (4) | 0.3354 (4) | 0.0536 (19) | |
H13A | 0.8041 | 0.5977 | 0.3125 | 0.08* | |
H13B | 0.7057 | 0.526 | 0.2964 | 0.08* | |
H13C | 0.8864 | 0.5305 | 0.3617 | 0.08* | |
C14 | 0.4030 (9) | 0.6415 (4) | 0.3992 (3) | 0.0427 (16) | |
C15 | 0.3039 (12) | 0.5759 (5) | 0.4005 (5) | 0.067 (2) | |
H15A | 0.2249 | 0.5648 | 0.3495 | 0.1* | |
H15B | 0.2463 | 0.5851 | 0.4316 | 0.1* | |
H15C | 0.3781 | 0.5366 | 0.4213 | 0.1* | |
C16 | 0.5123 (11) | 0.6646 (5) | 0.4799 (4) | 0.063 (2) | |
H16A | 0.5816 | 0.7032 | 0.4789 | 0.094* | |
H16B | 0.5807 | 0.6255 | 0.5076 | 0.094* | |
H16C | 0.4441 | 0.6796 | 0.5043 | 0.094* | |
C17 | 0.2809 (10) | 0.7008 (4) | 0.3627 (4) | 0.055 (2) | |
H17A | 0.2075 | 0.6878 | 0.3113 | 0.082* | |
H17B | 0.34 | 0.7432 | 0.3621 | 0.082* | |
H17C | 0.2174 | 0.709 | 0.3914 | 0.082* | |
C18 | 0.4247 (8) | 0.5971 (3) | 0.0903 (3) | 0.0340 (13) | |
C19 | 0.3811 (13) | 0.5198 (4) | 0.0759 (5) | 0.062 (2) | |
H19A | 0.265 | 0.5151 | 0.0429 | 0.093* | |
H19B | 0.4051 | 0.4964 | 0.1235 | 0.093* | |
H19C | 0.4453 | 0.4985 | 0.0523 | 0.093* | |
C20 | 0.3761 (12) | 0.6371 (4) | 0.0141 (4) | 0.059 (2) | |
H20A | 0.4116 | 0.6856 | 0.0243 | 0.089* | |
H20B | 0.2578 | 0.6355 | −0.015 | 0.089* | |
H20C | 0.4289 | 0.615 | −0.0144 | 0.089* | |
C21 | 0.6111 (10) | 0.6071 (5) | 0.1337 (4) | 0.064 (2) | |
H21A | 0.6354 | 0.6565 | 0.1452 | 0.096* | |
H21B | 0.6649 | 0.5907 | 0.103 | 0.096* | |
H21C | 0.651 | 0.5804 | 0.1803 | 0.096* | |
C22 | 0.1056 (7) | 0.6575 (3) | 0.0937 (3) | 0.0343 (14) | |
C23 | 0.0350 (9) | 0.6805 (4) | 0.1482 (4) | 0.0488 (17) | |
H23A | 0.0928 | 0.722 | 0.1753 | 0.073* | |
H23B | 0.0481 | 0.643 | 0.1838 | 0.073* | |
H23C | −0.0808 | 0.6912 | 0.1201 | 0.073* | |
C24 | 0.0087 (9) | 0.5933 (4) | 0.0490 (4) | 0.055 (2) | |
H24A | 0.0451 | 0.5812 | 0.0105 | 0.082* | |
H24B | −0.1077 | 0.6043 | 0.0252 | 0.082* | |
H24C | 0.0275 | 0.5539 | 0.083 | 0.082* | |
C25 | 0.0831 (10) | 0.7205 (4) | 0.0392 (4) | 0.0540 (19) | |
H25A | 0.1163 | 0.7065 | 0.0002 | 0.081* | |
H25B | 0.1505 | 0.7596 | 0.0674 | 0.081* | |
H25C | −0.0314 | 0.7346 | 0.0161 | 0.081* |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0402 (9) | 0.0167 (7) | 0.0282 (8) | −0.0029 (6) | 0.0129 (7) | 0.0010 (5) |
P2 | 0.0360 (8) | 0.0175 (7) | 0.0253 (8) | 0.0028 (6) | 0.0113 (6) | 0.0008 (5) |
P3 | 0.0339 (8) | 0.0165 (7) | 0.0256 (8) | 0.0011 (6) | 0.0108 (6) | 0.0011 (5) |
N1 | 0.035 (3) | 0.026 (3) | 0.047 (3) | −0.002 (2) | 0.021 (2) | −0.003 (2) |
Li1 | 0.041 (5) | 0.018 (5) | 0.040 (6) | −0.001 (4) | 0.021 (4) | −0.001 (4) |
Li2 | 0.043 (6) | 0.019 (5) | 0.049 (6) | −0.004 (4) | 0.023 (5) | 0.002 (4) |
C1 | 0.036 (3) | 0.012 (3) | 0.048 (4) | 0.000 (2) | 0.017 (3) | 0.001 (2) |
C2 | 0.051 (4) | 0.027 (3) | 0.034 (3) | −0.015 (3) | 0.018 (3) | −0.001 (2) |
C3 | 0.035 (3) | 0.020 (3) | 0.072 (5) | −0.005 (3) | 0.015 (3) | 0.012 (3) |
C4 | 0.059 (4) | 0.020 (3) | 0.074 (5) | −0.008 (3) | 0.043 (4) | −0.013 (3) |
C5 | 0.060 (4) | 0.025 (3) | 0.030 (3) | −0.018 (3) | 0.015 (3) | −0.004 (2) |
C6 | 0.046 (4) | 0.027 (4) | 0.094 (6) | 0.005 (3) | 0.035 (4) | 0.004 (3) |
C7 | 0.035 (4) | 0.044 (4) | 0.076 (5) | −0.001 (3) | 0.022 (4) | 0.010 (4) |
C8 | 0.044 (4) | 0.040 (4) | 0.061 (5) | −0.007 (3) | 0.018 (3) | −0.008 (3) |
C9 | 0.062 (5) | 0.054 (5) | 0.059 (5) | −0.011 (4) | 0.035 (4) | −0.008 (3) |
C10 | 0.043 (4) | 0.041 (4) | 0.031 (3) | 0.006 (3) | 0.007 (3) | −0.003 (3) |
C11 | 0.087 (6) | 0.038 (4) | 0.042 (4) | 0.027 (4) | 0.016 (4) | 0.017 (3) |
C12 | 0.049 (4) | 0.061 (5) | 0.049 (5) | 0.001 (4) | −0.003 (4) | −0.012 (4) |
C13 | 0.044 (4) | 0.059 (5) | 0.053 (5) | 0.016 (3) | 0.016 (3) | −0.003 (3) |
C14 | 0.051 (4) | 0.053 (4) | 0.027 (3) | 0.012 (3) | 0.018 (3) | 0.005 (3) |
C15 | 0.089 (6) | 0.074 (6) | 0.061 (5) | 0.005 (5) | 0.054 (5) | 0.011 (4) |
C16 | 0.081 (6) | 0.069 (6) | 0.034 (4) | 0.026 (4) | 0.019 (4) | −0.006 (3) |
C17 | 0.064 (5) | 0.062 (5) | 0.045 (4) | 0.026 (4) | 0.029 (4) | 0.002 (3) |
C18 | 0.048 (4) | 0.024 (3) | 0.032 (3) | 0.006 (3) | 0.019 (3) | 0.000 (2) |
C19 | 0.108 (7) | 0.033 (4) | 0.068 (5) | 0.007 (4) | 0.058 (5) | −0.008 (3) |
C20 | 0.091 (6) | 0.053 (5) | 0.045 (4) | 0.004 (4) | 0.040 (4) | 0.009 (3) |
C21 | 0.057 (5) | 0.088 (7) | 0.054 (5) | 0.013 (4) | 0.031 (4) | −0.003 (4) |
C22 | 0.033 (3) | 0.031 (3) | 0.030 (3) | 0.005 (2) | 0.005 (3) | 0.001 (2) |
C23 | 0.038 (4) | 0.052 (4) | 0.048 (4) | 0.011 (3) | 0.010 (3) | −0.002 (3) |
C24 | 0.048 (4) | 0.048 (5) | 0.048 (4) | −0.008 (3) | 0.001 (3) | −0.006 (3) |
C25 | 0.058 (4) | 0.044 (4) | 0.048 (4) | 0.015 (3) | 0.010 (3) | 0.017 (3) |
P1—P3 | 2.168 (2) | C9—H9C | 0.96 |
P1—P2 | 2.169 (2) | C10—C11 | 1.515 (10) |
P1—Li2 | 2.571 (10) | C10—C13 | 1.527 (10) |
P2—C10 | 1.900 (7) | C10—C12 | 1.540 (10) |
P2—C14 | 1.910 (7) | C11—H11A | 0.96 |
P2—Li1 | 2.579 (10) | C11—H11B | 0.96 |
P3—C22 | 1.903 (6) | C11—H11C | 0.96 |
P3—C18 | 1.912 (6) | C12—H12A | 0.96 |
P3—Li1 | 2.611 (10) | C12—H12B | 0.96 |
N1—C9 | 1.448 (8) | C12—H12C | 0.96 |
N1—C8 | 1.463 (8) | C13—H13A | 0.96 |
N1—C7 | 1.472 (9) | C13—H13B | 0.96 |
N1—Li2i | 2.237 (12) | C13—H13C | 0.96 |
Li1—C1 | 2.208 (11) | C14—C17 | 1.508 (10) |
Li1—C2 | 2.238 (11) | C14—C16 | 1.511 (10) |
Li1—C5 | 2.286 (11) | C14—C15 | 1.525 (12) |
Li1—C3 | 2.314 (11) | C15—H15A | 0.96 |
Li1—C4 | 2.345 (11) | C15—H15B | 0.96 |
Li2—N1ii | 2.237 (12) | C15—H15C | 0.96 |
Li2—C1ii | 2.287 (11) | C16—H16A | 0.96 |
Li2—C2ii | 2.314 (12) | C16—H16B | 0.96 |
Li2—C5ii | 2.359 (12) | C16—H16C | 0.96 |
Li2—C3ii | 2.447 (12) | C17—H17A | 0.96 |
Li2—C4ii | 2.475 (12) | C17—H17B | 0.96 |
C1—C2 | 1.398 (9) | C17—H17C | 0.96 |
C1—C5 | 1.410 (9) | C18—C19 | 1.503 (10) |
C1—C6 | 1.500 (9) | C18—C21 | 1.518 (11) |
C1—Li2i | 2.287 (11) | C18—C20 | 1.547 (9) |
C2—C3 | 1.394 (10) | C19—H19A | 0.96 |
C2—Li2i | 2.314 (12) | C19—H19B | 0.96 |
C2—H2 | 0.95 | C19—H19C | 0.96 |
C3—C4 | 1.370 (10) | C20—H20A | 0.96 |
C3—Li2i | 2.447 (12) | C20—H20B | 0.96 |
C3—H3 | 0.95 | C20—H20C | 0.96 |
C4—C5 | 1.390 (10) | C21—H21A | 0.96 |
C4—Li2i | 2.475 (12) | C21—H21B | 0.96 |
C4—H4 | 0.95 | C21—H21C | 0.96 |
C5—Li2i | 2.359 (12) | C22—C23 | 1.506 (9) |
C5—H5 | 0.9501 | C22—C24 | 1.524 (9) |
C6—C7 | 1.533 (10) | C22—C25 | 1.546 (9) |
C6—H6A | 0.97 | C23—H23A | 0.96 |
C6—H6B | 0.97 | C23—H23B | 0.96 |
C7—H7A | 0.97 | C23—H23C | 0.96 |
C7—H7B | 0.97 | C24—H24A | 0.96 |
C8—H8A | 0.96 | C24—H24B | 0.96 |
C8—H8B | 0.96 | C24—H24C | 0.96 |
C8—H8C | 0.96 | C25—H25A | 0.96 |
C9—H9A | 0.96 | C25—H25B | 0.96 |
C9—H9B | 0.96 | C25—H25C | 0.96 |
P3—P1—P2 | 95.87 (8) | C7—C6—H6B | 109.6 |
P3—P1—Li2 | 134.0 (2) | H6A—C6—H6B | 108.1 |
P2—P1—Li2 | 126.9 (2) | N1—C7—C6 | 112.6 (6) |
C10—P2—C14 | 108.1 (3) | N1—C7—H7A | 109.1 |
C10—P2—P1 | 107.3 (2) | C6—C7—H7A | 109.1 |
C14—P2—P1 | 105.1 (2) | N1—C7—H7B | 109.1 |
C10—P2—Li1 | 125.4 (3) | C6—C7—H7B | 109.1 |
C14—P2—Li1 | 114.1 (3) | H7A—C7—H7B | 107.8 |
P1—P2—Li1 | 93.8 (2) | N1—C8—H8A | 109.5 |
C22—P3—C18 | 108.1 (3) | N1—C8—H8B | 109.5 |
C22—P3—P1 | 106.3 (2) | H8A—C8—H8B | 109.5 |
C18—P3—P1 | 106.83 (19) | N1—C8—H8C | 109.5 |
C22—P3—Li1 | 117.3 (3) | H8A—C8—H8C | 109.5 |
C18—P3—Li1 | 122.3 (3) | H8B—C8—H8C | 109.5 |
P1—P3—Li1 | 93.0 (2) | N1—C9—H9A | 109.5 |
C9—N1—C8 | 109.2 (5) | N1—C9—H9B | 109.5 |
C9—N1—C7 | 110.1 (6) | H9A—C9—H9B | 109.5 |
C8—N1—C7 | 108.6 (5) | N1—C9—H9C | 109.5 |
C9—N1—Li2i | 110.5 (5) | H9A—C9—H9C | 109.5 |
C8—N1—Li2i | 113.4 (5) | H9B—C9—H9C | 109.5 |
C7—N1—Li2i | 104.9 (5) | C11—C10—C13 | 108.5 (6) |
C1—Li1—C2 | 36.6 (3) | C11—C10—C12 | 110.9 (6) |
C1—Li1—C5 | 36.5 (3) | C13—C10—C12 | 106.3 (6) |
C2—Li1—C5 | 59.6 (3) | C11—C10—P2 | 115.4 (5) |
C1—Li1—C3 | 60.0 (3) | C13—C10—P2 | 106.9 (4) |
C2—Li1—C3 | 35.6 (3) | C12—C10—P2 | 108.4 (5) |
C5—Li1—C3 | 58.2 (3) | C10—C11—H11A | 109.5 |
C1—Li1—C4 | 59.8 (3) | C10—C11—H11B | 109.5 |
C2—Li1—C4 | 58.6 (3) | H11A—C11—H11B | 109.5 |
C5—Li1—C4 | 34.9 (3) | C10—C11—H11C | 109.5 |
C3—Li1—C4 | 34.2 (3) | H11A—C11—H11C | 109.5 |
C1—Li1—P2 | 127.0 (5) | H11B—C11—H11C | 109.5 |
C2—Li1—P2 | 162.6 (5) | C10—C12—H12A | 109.5 |
C5—Li1—P2 | 111.6 (4) | C10—C12—H12B | 109.5 |
C3—Li1—P2 | 155.4 (5) | H12A—C12—H12B | 109.5 |
C4—Li1—P2 | 124.1 (4) | C10—C12—H12C | 109.5 |
C1—Li1—P3 | 132.0 (5) | H12A—C12—H12C | 109.5 |
C2—Li1—P3 | 110.2 (4) | H12B—C12—H12C | 109.5 |
C5—Li1—P3 | 168.4 (5) | C10—C13—H13A | 109.5 |
C3—Li1—P3 | 117.5 (4) | C10—C13—H13B | 109.5 |
C4—Li1—P3 | 146.8 (5) | H13A—C13—H13B | 109.5 |
P2—Li1—P3 | 76.7 (3) | C10—C13—H13C | 109.5 |
N1ii—Li2—C1ii | 78.6 (4) | H13A—C13—H13C | 109.5 |
N1ii—Li2—C2ii | 96.4 (4) | H13B—C13—H13C | 109.5 |
C1ii—Li2—C2ii | 35.4 (3) | C17—C14—C16 | 106.8 (6) |
N1ii—Li2—C5ii | 101.1 (4) | C17—C14—C15 | 107.5 (7) |
C1ii—Li2—C5ii | 35.3 (3) | C16—C14—C15 | 109.7 (6) |
C2ii—Li2—C5ii | 57.5 (3) | C17—C14—P2 | 104.9 (4) |
N1ii—Li2—C3ii | 130.1 (5) | C16—C14—P2 | 113.9 (5) |
C1ii—Li2—C3ii | 57.0 (3) | C15—C14—P2 | 113.5 (5) |
C2ii—Li2—C3ii | 33.9 (3) | C14—C15—H15A | 109.5 |
C5ii—Li2—C3ii | 55.4 (3) | C14—C15—H15B | 109.5 |
N1ii—Li2—C4ii | 133.2 (5) | H15A—C15—H15B | 109.5 |
C1ii—Li2—C4ii | 56.8 (3) | C14—C15—H15C | 109.5 |
C2ii—Li2—C4ii | 55.7 (3) | H15A—C15—H15C | 109.5 |
C5ii—Li2—C4ii | 33.3 (3) | H15B—C15—H15C | 109.5 |
C3ii—Li2—C4ii | 32.3 (3) | C14—C16—H16A | 109.5 |
N1ii—Li2—P1 | 109.4 (4) | C14—C16—H16B | 109.5 |
C1ii—Li2—P1 | 171.8 (5) | H16A—C16—H16B | 109.5 |
C2ii—Li2—P1 | 141.5 (5) | C14—C16—H16C | 109.5 |
C5ii—Li2—P1 | 138.1 (5) | H16A—C16—H16C | 109.5 |
C3ii—Li2—P1 | 116.2 (4) | H16B—C16—H16C | 109.5 |
C4ii—Li2—P1 | 115.0 (4) | C14—C17—H17A | 109.5 |
C2—C1—C5 | 106.4 (6) | C14—C17—H17B | 109.5 |
C2—C1—C6 | 127.2 (6) | H17A—C17—H17B | 109.5 |
C5—C1—C6 | 125.9 (6) | C14—C17—H17C | 109.5 |
C2—C1—Li1 | 72.9 (4) | H17A—C17—H17C | 109.5 |
C5—C1—Li1 | 74.7 (4) | H17B—C17—H17C | 109.5 |
C6—C1—Li1 | 124.3 (5) | C19—C18—C21 | 111.0 (7) |
C2—C1—Li2i | 73.4 (4) | C19—C18—C20 | 110.5 (6) |
C5—C1—Li2i | 75.2 (4) | C21—C18—C20 | 105.2 (6) |
C6—C1—Li2i | 110.3 (5) | C19—C18—P3 | 113.9 (5) |
Li1—C1—Li2i | 125.3 (5) | C21—C18—P3 | 103.9 (4) |
C3—C2—C1 | 108.4 (6) | C20—C18—P3 | 111.8 (4) |
C3—C2—Li1 | 75.2 (4) | C18—C19—H19A | 109.5 |
C1—C2—Li1 | 70.5 (4) | C18—C19—H19B | 109.5 |
C3—C2—Li2i | 78.3 (5) | H19A—C19—H19B | 109.5 |
C1—C2—Li2i | 71.2 (4) | C18—C19—H19C | 109.5 |
Li1—C2—Li2i | 122.6 (4) | H19A—C19—H19C | 109.5 |
C3—C2—H2 | 125.8 | H19B—C19—H19C | 109.5 |
C1—C2—H2 | 125.8 | C18—C20—H20A | 109.5 |
Li1—C2—H2 | 120.3 | C18—C20—H20B | 109.5 |
Li2i—C2—H2 | 116.6 | H20A—C20—H20B | 109.5 |
C4—C3—C2 | 108.5 (6) | C18—C20—H20C | 109.5 |
C4—C3—Li1 | 74.1 (4) | H20A—C20—H20C | 109.5 |
C2—C3—Li1 | 69.2 (4) | H20B—C20—H20C | 109.5 |
C4—C3—Li2i | 75.0 (5) | C18—C21—H21A | 109.5 |
C2—C3—Li2i | 67.8 (4) | C18—C21—H21B | 109.5 |
Li1—C3—Li2i | 113.9 (4) | H21A—C21—H21B | 109.5 |
C4—C3—H3 | 125.7 | C18—C21—H21C | 109.5 |
C2—C3—H3 | 125.7 | H21A—C21—H21C | 109.5 |
Li1—C3—H3 | 122.5 | H21B—C21—H21C | 109.5 |
Li2i—C3—H3 | 123.1 | C23—C22—C24 | 108.9 (6) |
C3—C4—C5 | 108.2 (6) | C23—C22—C25 | 106.7 (6) |
C3—C4—Li1 | 71.7 (4) | C24—C22—C25 | 110.2 (5) |
C5—C4—Li1 | 70.2 (4) | C23—C22—P3 | 106.5 (4) |
C3—C4—Li2i | 72.7 (4) | C24—C22—P3 | 115.4 (5) |
C5—C4—Li2i | 68.8 (4) | C25—C22—P3 | 108.8 (5) |
Li1—C4—Li2i | 111.8 (4) | C22—C23—H23A | 109.5 |
C3—C4—H4 | 125.9 | C22—C23—H23B | 109.5 |
C5—C4—H4 | 125.9 | H23A—C23—H23B | 109.5 |
Li1—C4—H4 | 123.8 | C22—C23—H23C | 109.5 |
Li2i—C4—H4 | 124.2 | H23A—C23—H23C | 109.5 |
C4—C5—C1 | 108.4 (6) | H23B—C23—H23C | 109.5 |
C4—C5—Li1 | 74.9 (4) | C22—C24—H24A | 109.5 |
C1—C5—Li1 | 68.7 (4) | C22—C24—H24B | 109.5 |
C4—C5—Li2i | 77.9 (5) | H24A—C24—H24B | 109.5 |
C1—C5—Li2i | 69.5 (4) | C22—C24—H24C | 109.5 |
Li1—C5—Li2i | 118.5 (4) | H24A—C24—H24C | 109.5 |
C4—C5—H5 | 125.8 | H24B—C24—H24C | 109.5 |
C1—C5—H5 | 125.8 | C22—C25—H25A | 109.5 |
Li1—C5—H5 | 122.3 | C22—C25—H25B | 109.5 |
Li2i—C5—H5 | 118.5 | H25A—C25—H25B | 109.5 |
C1—C6—C7 | 110.4 (6) | C22—C25—H25C | 109.5 |
C1—C6—H6A | 109.6 | H25A—C25—H25C | 109.5 |
C7—C6—H6A | 109.6 | H25B—C25—H25C | 109.5 |
C1—C6—H6B | 109.6 | ||
P3—P1—P2—C10 | −122.7 (2) | C5—Li1—C3—C4 | −36.5 (4) |
Li2—P1—P2—C10 | 39.2 (4) | P2—Li1—C3—C4 | 35.0 (12) |
P3—P1—P2—C14 | 122.5 (2) | P3—Li1—C3—C4 | 155.9 (6) |
Li2—P1—P2—C14 | −75.6 (4) | C1—Li1—C3—C2 | 38.2 (4) |
P3—P1—P2—Li1 | 6.3 (2) | C5—Li1—C3—C2 | 81.0 (4) |
Li2—P1—P2—Li1 | 168.2 (4) | C4—Li1—C3—C2 | 117.5 (6) |
P2—P1—P3—C22 | −125.8 (2) | P2—Li1—C3—C2 | 152.5 (12) |
Li2—P1—P3—C22 | 74.4 (4) | P3—Li1—C3—C2 | −86.6 (5) |
P2—P1—P3—C18 | 118.9 (2) | C1—Li1—C3—Li2i | −14.2 (5) |
Li2—P1—P3—C18 | −40.9 (4) | C2—Li1—C3—Li2i | −52.4 (5) |
P2—P1—P3—Li1 | −6.2 (2) | C5—Li1—C3—Li2i | 28.6 (5) |
Li2—P1—P3—Li1 | −166.0 (4) | C4—Li1—C3—Li2i | 65.1 (5) |
C10—P2—Li1—C1 | −24.0 (7) | P2—Li1—C3—Li2i | 100.1 (12) |
C14—P2—Li1—C1 | 113.2 (5) | P3—Li1—C3—Li2i | −139.0 (5) |
P1—P2—Li1—C1 | −138.4 (5) | C2—C3—C4—C5 | 0.0 (7) |
C10—P2—Li1—C2 | −6.4 (17) | Li1—C3—C4—C5 | 61.0 (5) |
C14—P2—Li1—C2 | 130.8 (15) | Li2i—C3—C4—C5 | −59.9 (5) |
P1—P2—Li1—C2 | −120.8 (16) | C2—C3—C4—Li1 | −61.0 (5) |
C10—P2—Li1—C5 | −62.4 (5) | Li2i—C3—C4—Li1 | −120.9 (4) |
C14—P2—Li1—C5 | 74.8 (5) | C2—C3—C4—Li2i | 59.8 (5) |
P1—P2—Li1—C5 | −176.7 (4) | Li1—C3—C4—Li2i | 120.9 (4) |
C10—P2—Li1—C3 | −122.4 (11) | C1—Li1—C4—C3 | 80.2 (4) |
C14—P2—Li1—C3 | 14.8 (13) | C2—Li1—C4—C3 | 37.3 (4) |
P1—P2—Li1—C3 | 123.2 (12) | C5—Li1—C4—C3 | 118.0 (6) |
C10—P2—Li1—C4 | −99.5 (6) | P2—Li1—C4—C3 | −163.3 (6) |
C14—P2—Li1—C4 | 37.7 (6) | P3—Li1—C4—C3 | −41.4 (9) |
P1—P2—Li1—C4 | 146.1 (5) | C1—Li1—C4—C5 | −37.8 (4) |
C10—P2—Li1—P3 | 109.1 (3) | C2—Li1—C4—C5 | −80.7 (5) |
C14—P2—Li1—P3 | −113.7 (3) | C3—Li1—C4—C5 | −118.0 (6) |
P1—P2—Li1—P3 | −5.3 (2) | P2—Li1—C4—C5 | 78.7 (6) |
C22—P3—Li1—C1 | −116.3 (6) | P3—Li1—C4—C5 | −159.4 (9) |
C18—P3—Li1—C1 | 21.5 (7) | C1—Li1—C4—Li2i | 18.2 (4) |
P1—P3—Li1—C1 | 133.6 (6) | C2—Li1—C4—Li2i | −24.7 (4) |
C22—P3—Li1—C2 | −81.3 (5) | C5—Li1—C4—Li2i | 56.0 (5) |
C18—P3—Li1—C2 | 56.5 (5) | C3—Li1—C4—Li2i | −62.0 (5) |
P1—P3—Li1—C2 | 168.6 (4) | P2—Li1—C4—Li2i | 134.8 (5) |
C22—P3—Li1—C5 | −108 (2) | P3—Li1—C4—Li2i | −103.4 (9) |
C18—P3—Li1—C5 | 30 (3) | C3—C4—C5—C1 | −1.0 (7) |
P1—P3—Li1—C5 | 142 (2) | Li1—C4—C5—C1 | 60.9 (5) |
C22—P3—Li1—C3 | −43.1 (6) | Li2i—C4—C5—C1 | −63.4 (5) |
C18—P3—Li1—C3 | 94.7 (5) | C3—C4—C5—Li1 | −61.9 (5) |
P1—P3—Li1—C3 | −153.2 (4) | Li2i—C4—C5—Li1 | −124.3 (4) |
C22—P3—Li1—C4 | −18.3 (10) | C3—C4—C5—Li2i | 62.4 (5) |
C18—P3—Li1—C4 | 119.5 (8) | Li1—C4—C5—Li2i | 124.3 (4) |
P1—P3—Li1—C4 | −128.4 (8) | C2—C1—C5—C4 | 1.6 (7) |
C22—P3—Li1—P2 | 115.4 (3) | C6—C1—C5—C4 | 173.5 (6) |
C18—P3—Li1—P2 | −106.8 (3) | Li1—C1—C5—C4 | −64.9 (5) |
P1—P3—Li1—P2 | 5.3 (2) | Li2i—C1—C5—C4 | 68.9 (5) |
P3—P1—Li2—N1ii | −101.3 (4) | C2—C1—C5—Li1 | 66.5 (5) |
P2—P1—Li2—N1ii | 104.1 (4) | C6—C1—C5—Li1 | −121.6 (6) |
P3—P1—Li2—C2ii | 129.4 (7) | Li2i—C1—C5—Li1 | 133.8 (4) |
P2—P1—Li2—C2ii | −25.2 (9) | C2—C1—C5—Li2i | −67.3 (5) |
P3—P1—Li2—C5ii | 33.1 (9) | C6—C1—C5—Li2i | 104.6 (7) |
P2—P1—Li2—C5ii | −121.5 (6) | Li1—C1—C5—Li2i | −133.8 (4) |
P3—P1—Li2—C3ii | 99.6 (5) | C1—Li1—C5—C4 | 117.2 (6) |
P2—P1—Li2—C3ii | −55.0 (6) | C2—Li1—C5—C4 | 77.6 (5) |
P3—P1—Li2—C4ii | 63.7 (6) | C3—Li1—C5—C4 | 35.7 (4) |
P2—P1—Li2—C4ii | −91.0 (5) | P2—Li1—C5—C4 | −119.2 (5) |
C5—Li1—C1—C2 | −112.9 (6) | P3—Li1—C5—C4 | 107 (2) |
C3—Li1—C1—C2 | −37.1 (4) | C2—Li1—C5—C1 | −39.6 (4) |
C4—Li1—C1—C2 | −76.8 (4) | C3—Li1—C5—C1 | −81.4 (4) |
P2—Li1—C1—C2 | 171.2 (6) | C4—Li1—C5—C1 | −117.2 (6) |
P3—Li1—C1—C2 | 64.3 (6) | P2—Li1—C5—C1 | 123.7 (5) |
C2—Li1—C1—C5 | 112.9 (6) | P3—Li1—C5—C1 | −10 (2) |
C3—Li1—C1—C5 | 75.8 (4) | C1—Li1—C5—Li2i | 50.3 (5) |
C4—Li1—C1—C5 | 36.1 (4) | C2—Li1—C5—Li2i | 10.7 (5) |
P2—Li1—C1—C5 | −75.8 (6) | C3—Li1—C5—Li2i | −31.1 (5) |
P3—Li1—C1—C5 | 177.2 (7) | C4—Li1—C5—Li2i | −66.8 (5) |
C2—Li1—C1—C6 | −123.8 (8) | P2—Li1—C5—Li2i | 174.0 (4) |
C5—Li1—C1—C6 | 123.3 (7) | P3—Li1—C5—Li2i | 40 (3) |
C3—Li1—C1—C6 | −160.9 (7) | C2—C1—C6—C7 | 103.9 (8) |
C4—Li1—C1—C6 | 159.4 (7) | C5—C1—C6—C7 | −66.4 (9) |
P2—Li1—C1—C6 | 47.5 (9) | Li1—C1—C6—C7 | −162.1 (6) |
P3—Li1—C1—C6 | −59.5 (9) | Li2i—C1—C6—C7 | 19.7 (8) |
C2—Li1—C1—Li2i | 54.2 (5) | C9—N1—C7—C6 | −66.8 (8) |
C5—Li1—C1—Li2i | −58.8 (6) | C8—N1—C7—C6 | 173.6 (6) |
C3—Li1—C1—Li2i | 17.1 (5) | Li2i—N1—C7—C6 | 52.1 (8) |
C4—Li1—C1—Li2i | −22.7 (5) | C1—C6—C7—N1 | −49.6 (9) |
P2—Li1—C1—Li2i | −134.6 (5) | C14—P2—C10—C11 | 47.7 (6) |
P3—Li1—C1—Li2i | 118.5 (6) | P1—P2—C10—C11 | −65.1 (5) |
C5—C1—C2—C3 | −1.6 (6) | Li1—P2—C10—C11 | −173.0 (5) |
C6—C1—C2—C3 | −173.4 (6) | C14—P2—C10—C13 | 168.4 (5) |
Li1—C1—C2—C3 | 66.2 (5) | P1—P2—C10—C13 | 55.6 (5) |
Li2i—C1—C2—C3 | −70.2 (5) | Li1—P2—C10—C13 | −52.3 (6) |
C5—C1—C2—Li1 | −67.8 (5) | C14—P2—C10—C12 | −77.4 (6) |
C6—C1—C2—Li1 | 120.4 (7) | P1—P2—C10—C12 | 169.8 (5) |
Li2i—C1—C2—Li1 | −136.4 (4) | Li1—P2—C10—C12 | 61.9 (6) |
C5—C1—C2—Li2i | 68.5 (5) | C10—P2—C14—C17 | 164.2 (5) |
C6—C1—C2—Li2i | −103.2 (7) | P1—P2—C14—C17 | −81.5 (5) |
Li1—C1—C2—Li2i | 136.4 (4) | Li1—P2—C14—C17 | 19.8 (6) |
C1—Li1—C2—C3 | −116.1 (6) | C10—P2—C14—C16 | 47.7 (6) |
C5—Li1—C2—C3 | −76.7 (5) | P1—P2—C14—C16 | 162.0 (5) |
C4—Li1—C2—C3 | −35.8 (4) | Li1—P2—C14—C16 | −96.6 (6) |
P2—Li1—C2—C3 | −140.1 (16) | C10—P2—C14—C15 | −78.7 (6) |
P3—Li1—C2—C3 | 109.4 (5) | P1—P2—C14—C15 | 35.6 (6) |
C5—Li1—C2—C1 | 39.5 (4) | Li1—P2—C14—C15 | 136.9 (5) |
C3—Li1—C2—C1 | 116.1 (6) | C22—P3—C18—C19 | −75.4 (6) |
C4—Li1—C2—C1 | 80.4 (4) | P1—P3—C18—C19 | 38.6 (6) |
P2—Li1—C2—C1 | −23.9 (16) | Li1—P3—C18—C19 | 143.5 (5) |
P3—Li1—C2—C1 | −134.5 (5) | C22—P3—C18—C21 | 163.7 (5) |
C1—Li1—C2—Li2i | −50.9 (5) | P1—P3—C18—C21 | −82.2 (5) |
C5—Li1—C2—Li2i | −11.4 (5) | Li1—P3—C18—C21 | 22.6 (6) |
C3—Li1—C2—Li2i | 65.3 (6) | C22—P3—C18—C20 | 50.8 (6) |
C4—Li1—C2—Li2i | 29.5 (5) | P1—P3—C18—C20 | 164.8 (5) |
P2—Li1—C2—Li2i | −74.8 (17) | Li1—P3—C18—C20 | −90.3 (6) |
P3—Li1—C2—Li2i | 174.6 (4) | C18—P3—C22—C23 | 170.0 (4) |
C1—C2—C3—C4 | 1.0 (7) | P1—P3—C22—C23 | 55.6 (5) |
Li1—C2—C3—C4 | 64.2 (5) | Li1—P3—C22—C23 | −46.7 (6) |
Li2i—C2—C3—C4 | −64.4 (5) | C18—P3—C22—C24 | 49.0 (6) |
C1—C2—C3—Li1 | −63.1 (5) | P1—P3—C22—C24 | −65.4 (5) |
Li2i—C2—C3—Li1 | −128.6 (4) | Li1—P3—C22—C24 | −167.6 (5) |
C1—C2—C3—Li2i | 65.5 (5) | C18—P3—C22—C25 | −75.4 (5) |
Li1—C2—C3—Li2i | 128.6 (4) | P1—P3—C22—C25 | 170.2 (4) |
C1—Li1—C3—C4 | −79.3 (5) | Li1—P3—C22—C25 | 68.0 (5) |
C2—Li1—C3—C4 | −117.5 (6) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Li2(C9H14N)(C16H36P3)] |
Mr | 471.45 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 120 |
a, b, c (Å) | 8.9063 (6), 18.8522 (8), 19.3934 (17) |
β (°) | 115.314 (6) |
V (Å3) | 2943.5 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.21 |
Crystal size (mm) | 0.44 × 0.23 × 0.2 |
Data collection | |
Diffractometer | Oxford Diffraction Xcalibur diffractometer with a Sapphire2 (large Be window) detector |
Absorption correction | Multi-scan (CrysAlis PRO; Oxford Diffraction, 2009) |
Tmin, Tmax | 0.734, 1 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14505, 4818, 3492 |
Rint | 0.093 |
(sin θ/λ)max (Å−1) | 0.597 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.095, 0.258, 1.13 |
No. of reflections | 4818 |
No. of parameters | 294 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0825P)2 + 14.0784P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.72, −0.61 |
Computer programs: CrysAlis PRO (Oxford Diffraction, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).
Acknowledgements
We thank the Polish State Committee of Scientific Research (project No. NN204271535) for financial support.
References
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The schematic structure of the linear coordination polymer of (I) is shown in Fig.1. The monomeric unit of the title compound consists of two lithium atoms and two ligands: (tBu2P)2P and C5H4CH2CH2NMe2. Both lithium atoms adopt distorted trigonal geometry. Li1 atom is bonded in a η5-fashion from the one face of C5H4 ring system and is also bonded with two terminal phosphorous atoms P2, P3 from a (tBu2P)2P ligand. Atom Li2 is coordinated by atom P1 from another triphosphane ligand and is η5-coordinated to the other face of the C5H4 ring system, assisted by κN-coordination of the attached dimethylamino substituent. Atoms Li1, P1, P2, P3 form a planar ring (maximum deviation 0.069 Å). The two lithium atoms and C5H4 ring form an "inverse sandwich". The structure of (tBu2P)2P ligand in complex (I) is similar to the one found for [Li(THF)2{η2-(tBu2P)2P}] (Kovacs et al., 1996a) with comparable P–P and P–Li distances. To the best of our knowledge only one example of lithium complex with substituted Cp ligand which exhibits κN and η5-coordination to the same lithium atom is known (Kunz et al., 2000). Li–N distance in complex [{C5H4CH(Ph)NMe2}Li]n (Kunz et al., 2000) and in the title compound are similar [2.227 (5) Å; 2.237 (12) Å].