[P,P-Di-tert-butyl-N-trimethylsilyl-P-(trimethylsilylamino)phosphine imidato-[kappa]²N,N']bis(pyridine-[kappa]N)lithium(I)

In the title compound, [Li(C₁₄H₃₆N₂PSi₂)(C₅H₅N)₂], the bulky chelating monoanionic P,P-di-tert-butyl-N-trimethylsilyl-P-(trimethylsilylamino)phosphine imidate ligand and two pyridine ligands bind to Li in a pseudo-tetrahedral arrangement with twofold symmetry. The Li-N_phosphine distance is 2.048 (5) Å, while the Li...P distance is 2.520 (6) Å.

Computing details

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.

[P,P-Di-tert-butyl-N-trimethylsilyl-P-(trimethylsilylamino)phosphine imidato-κ²N,N']bis(pyridine-κN)lithium(I)

Crystal data

[Li(C14H36N2PSi2)(C5H5N)2]	F(000) = 1056
Mr = 484.74	Dx = 1.062 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3164 reflections
a = 8.8980 (2) Å	θ = 2.1–24.1°
b = 19.3848 (5) Å	µ = 0.19 mm^−1
c = 17.5894 (3) Å	T = 200 K
β = 92.302 (1)°	Needle-like, colourless
V = 3031.48 (12) Å^3	0.83 × 0.29 × 0.12 mm
Z = 4

Data collection

Bruker SMART CCD area-detector Query diffractometer	2410 independent reflections
Radiation source: fine-focus sealed tube	1674 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.075
φ and ω scans	θmax = 24.1°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick 1996)	h = −10→10
Tmin = 0.56, Tmax = 0.97	k = −22→22
11861 measured reflections	l = −20→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.144	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0764P)^2 + 1.4419P] where P = (Fo^2 + 2Fc^2)/3
2410 reflections	(Δ/σ)max = 0.029
152 parameters	Δρmax = 0.42 e Å^−3
0 restraints	Δρmin = −0.34 e Å^−3

Special details

Experimental. Attempts to cut the long thin needle-like crystals resulted in shattering. Therefore, a crystal was used which was longer than the beam-width. Correction for this by SADABS may be the cause of the low Tmin.

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 (Ų)

	x	y	z	Uiso*/Ueq
Li1	0.5000	0.3058 (3)	0.2500	0.0360 (16)
N1	0.4007 (2)	0.38824 (11)	0.19516 (12)	0.0356 (6)
N2	0.6009 (3)	0.23292 (12)	0.17865 (14)	0.0456 (7)
Si1	0.28204 (9)	0.37396 (5)	0.12070 (5)	0.0429 (3)
P1	0.5000	0.43581 (5)	0.2500	0.0326 (3)
C1	0.6270 (4)	0.49019 (16)	0.19230 (18)	0.0486 (8)
C2	0.5443 (5)	0.5240 (2)	0.1241 (2)	0.0811 (13)
H2A	0.6170	0.5478	0.0929	0.122*
H2C	0.4711	0.5574	0.1421	0.122*
H2B	0.4918	0.4885	0.0935	0.122*
C3	0.7419 (4)	0.4403 (2)	0.1608 (2)	0.0788 (13)
H3B	0.8064	0.4650	0.1261	0.118*
H3C	0.6892	0.4029	0.1333	0.118*
H3A	0.8038	0.4209	0.2029	0.118*
C4	0.7120 (5)	0.5450 (2)	0.2390 (2)	0.0941 (15)
H4C	0.7636	0.5233	0.2831	0.141*
H4A	0.6408	0.5796	0.2565	0.141*
H4B	0.7861	0.5674	0.2074	0.141*
C5	0.1425 (4)	0.3061 (2)	0.1454 (2)	0.0752 (12)
H5A	0.0808	0.3230	0.1863	0.113*
H5C	0.1960	0.2643	0.1622	0.113*
H5B	0.0778	0.2956	0.1005	0.113*
C6	0.1668 (4)	0.44924 (19)	0.0852 (2)	0.0765 (12)
H6A	0.2338	0.4859	0.0684	0.115*
H6B	0.1059	0.4666	0.1262	0.115*
H6C	0.1007	0.4345	0.0423	0.115*
C7	0.3810 (4)	0.33967 (17)	0.03652 (16)	0.0553 (9)
H7A	0.4395	0.2987	0.0517	0.083*
H7B	0.4486	0.3751	0.0176	0.083*
H7C	0.3066	0.3272	−0.0038	0.083*
C8	0.5152 (4)	0.18181 (15)	0.15133 (19)	0.0515 (9)
H8	0.4204	0.1744	0.1729	0.062*
C9	0.5570 (4)	0.13899 (17)	0.09324 (19)	0.0578 (10)
H9	0.4924	0.1030	0.0752	0.069*
C10	0.6932 (5)	0.14945 (19)	0.06234 (19)	0.0654 (11)
H10	0.7246	0.1212	0.0218	0.078*
C11	0.7832 (4)	0.20072 (19)	0.0902 (2)	0.0653 (11)
H11	0.8791	0.2085	0.0699	0.078*
C12	0.7343 (4)	0.24129 (17)	0.14827 (19)	0.0515 (9)
H12	0.7985	0.2769	0.1676	0.062*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Li1	0.043 (4)	0.032 (4)	0.034 (4)	0.000	0.014 (3)	0.000
N1	0.0356 (14)	0.0403 (14)	0.0313 (13)	0.0027 (11)	0.0055 (11)	−0.0014 (11)
N2	0.0507 (17)	0.0414 (15)	0.0458 (15)	−0.0030 (13)	0.0149 (13)	−0.0055 (12)
Si1	0.0403 (5)	0.0575 (6)	0.0307 (5)	0.0015 (4)	0.0009 (4)	−0.0082 (4)
P1	0.0374 (6)	0.0357 (6)	0.0250 (6)	0.000	0.0051 (4)	0.000
C1	0.055 (2)	0.0488 (19)	0.0417 (18)	−0.0135 (16)	0.0026 (16)	0.0156 (15)
C2	0.096 (3)	0.088 (3)	0.059 (3)	−0.014 (2)	0.002 (2)	0.037 (2)
C3	0.068 (3)	0.094 (3)	0.077 (3)	−0.007 (2)	0.044 (2)	0.024 (2)
C4	0.113 (4)	0.092 (3)	0.077 (3)	−0.061 (3)	−0.005 (3)	0.018 (2)
C5	0.058 (2)	0.111 (3)	0.056 (2)	−0.033 (2)	0.0021 (19)	−0.019 (2)
C6	0.071 (3)	0.089 (3)	0.068 (3)	0.025 (2)	−0.023 (2)	−0.018 (2)
C7	0.075 (2)	0.065 (2)	0.0253 (16)	0.0051 (19)	0.0037 (16)	−0.0056 (15)
C8	0.054 (2)	0.0434 (19)	0.058 (2)	−0.0029 (16)	0.0087 (17)	−0.0014 (17)
C9	0.074 (3)	0.050 (2)	0.050 (2)	−0.0079 (18)	0.0046 (19)	−0.0119 (17)
C10	0.094 (3)	0.061 (2)	0.043 (2)	0.009 (2)	0.017 (2)	−0.0150 (18)
C11	0.066 (3)	0.070 (3)	0.063 (2)	−0.001 (2)	0.032 (2)	−0.012 (2)
C12	0.053 (2)	0.049 (2)	0.053 (2)	−0.0090 (16)	0.0161 (18)	−0.0043 (16)

Geometric parameters (Å, º)

Li1—N1	2.048 (5)	C4—H4A	0.9800
Li1—N2	2.114 (5)	C4—H4B	0.9800
Li1—P1	2.520 (6)	C5—H5A	0.9800
N1—P1	1.579 (2)	C5—H5C	0.9800
N1—Si1	1.672 (2)	C5—H5B	0.9800
N2—C8	1.328 (4)	C6—H6A	0.9800
N2—C12	1.332 (4)	C6—H6B	0.9800
Si1—C5	1.871 (4)	C6—H6C	0.9800
Si1—C7	1.875 (3)	C7—H7A	0.9800
Si1—C6	1.876 (4)	C7—H7B	0.9800
P1—C1	1.873 (3)	C7—H7C	0.9800
C1—C4	1.525 (5)	C8—C9	1.379 (4)
C1—C3	1.528 (5)	C8—H8	0.9500
C1—C2	1.530 (4)	C9—C10	1.363 (5)
C2—H2A	0.9800	C9—H9	0.9500
C2—H2C	0.9800	C10—C11	1.356 (5)
C2—H2B	0.9800	C10—H10	0.9500
C3—H3B	0.9800	C11—C12	1.373 (4)
C3—H3C	0.9800	C11—H11	0.9500
C3—H3A	0.9800	C12—H12	0.9500
C4—H4C	0.9800
N1^i—Li1—N1	77.5 (2)	H3C—C3—H3A	109.5
N1^i—Li1—N2	128.01 (10)	C1—C4—H4C	109.5
N1—Li1—N2	115.30 (9)	C1—C4—H4A	109.5
N2—Li1—N2^i	96.1 (3)	H4C—C4—H4A	109.5
N2—Li1—P1	131.96 (14)	C1—C4—H4B	109.5
P1—N1—Si1	153.57 (15)	H4C—C4—H4B	109.5
P1—N1—Li1	87.00 (15)	H4A—C4—H4B	109.5
Si1—N1—Li1	119.12 (16)	Si1—C5—H5A	109.5
C8—N2—C12	117.0 (3)	Si1—C5—H5C	109.5
C8—N2—Li1	117.5 (2)	H5A—C5—H5C	109.5
C12—N2—Li1	124.3 (2)	Si1—C5—H5B	109.5
N1—Si1—C5	109.80 (15)	H5A—C5—H5B	109.5
N1—Si1—C7	112.05 (14)	H5C—C5—H5B	109.5
C5—Si1—C7	105.71 (17)	Si1—C6—H6A	109.5
N1—Si1—C6	116.85 (14)	Si1—C6—H6B	109.5
C5—Si1—C6	105.38 (19)	H6A—C6—H6B	109.5
C7—Si1—C6	106.28 (17)	Si1—C6—H6C	109.5
N1—P1—N1^i	108.52 (17)	H6A—C6—H6C	109.5
N1—P1—C1^i	108.96 (13)	H6B—C6—H6C	109.5
N1—P1—C1	109.42 (13)	Si1—C7—H7A	109.5
C1^i—P1—C1	111.5 (2)	Si1—C7—H7B	109.5
N1—P1—Li1	54.26 (8)	H7A—C7—H7B	109.5
C1—P1—Li1	124.24 (11)	Si1—C7—H7C	109.5
C4—C1—C3	108.2 (3)	H7A—C7—H7C	109.5
C4—C1—C2	109.6 (3)	H7B—C7—H7C	109.5
C3—C1—C2	107.2 (3)	N2—C8—C9	123.3 (3)
C4—C1—P1	113.4 (2)	N2—C8—H8	118.3
C3—C1—P1	105.5 (2)	C9—C8—H8	118.3
C2—C1—P1	112.6 (2)	C10—C9—C8	118.4 (3)
C1—C2—H2A	109.5	C10—C9—H9	120.8
C1—C2—H2C	109.5	C8—C9—H9	120.8
H2A—C2—H2C	109.5	C11—C10—C9	119.1 (3)
C1—C2—H2B	109.5	C11—C10—H10	120.4
H2A—C2—H2B	109.5	C9—C10—H10	120.4
H2C—C2—H2B	109.5	C10—C11—C12	119.2 (3)
C1—C3—H3B	109.5	C10—C11—H11	120.4
C1—C3—H3C	109.5	C12—C11—H11	120.4
H3B—C3—H3C	109.5	N2—C12—C11	122.9 (3)
C1—C3—H3A	109.5	N2—C12—H12	118.6
H3B—C3—H3A	109.5	C11—C12—H12	118.6

Symmetry code: (i) −x+1, y, −z+1/2.