A trigonal-bipyramidal coordinated ytterbium(III) alkyl: tris­(tri­methyl­silyl­methyl)­bis­(tetra­hydro­furan-O)­ytterbium(III)

The title compound, [Yb(CH₂SiMe₃)₃(thf)₂] (thf is tetra­hydro­furan, C₄H₈O), was obtained by direct synthesis from ICH₂SiMe₃ and Yb chips. The Yb atom shows a slightly distorted trigonal-bipyramidal environment formed by the C atoms of three alkyl ligands in equatorial positions (average Yb-C = 2.374 Å) and the O atoms of two tetra­hydro­furan mol­ecules (average Yb-O = 2.330 Å).

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.015 Å
• Disorder in main residue
• R factor = 0.055
• wR factor = 0.127
• Data-to-parameter ratio = 29.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           29.00
         From the CIF: _reflns_number_total               7113
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         7724
         Completeness (_total/calc)             92.09%
          Alert C: < 95% complete

PLAT_301  Alert C Main Residue Disorder ........................       7.00 Perc.

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.625
          Tmax scaled      0.511 Tmin scaled      0.292


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

Computing details

Data collection: P3 (Siemens 1989); cell refinement: P3; data reduction: XDISK (Siemens 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL (Sheldrick, 1998).

Tris(trimethylsilylmethyl)bis(tetrahydrofuran-O)ytterbium(III)

Crystal data

[Yb(CH2SiC3H9)3(C4H8O)2]	Dx = 1.324 Mg m^−3
Mr = 578.90	Melting point: <293K K
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.6627 (12) Å	Cell parameters from 36 reflections
b = 18.549 (2) Å	θ = 6.0–12.1°
c = 14.742 (2) Å	µ = 3.36 mm^−1
β = 95.293 (10)°	T = 173 K
V = 2903.3 (6) Å^3	Block, orange
Z = 4	0.40 × 0.35 × 0.20 mm
F(000) = 1188

Data collection

Rebuild Syntex P21/Siemens P3 four-circle diffractometer	5064 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.058
Graphite monochromator	θmax = 29.0°, θmin = 1.8°
Wyckoff scans	h = −9→14
Absorption correction: ψ scan North et al. (1968)	k = −21→25
Tmin = 0.467, Tmax = 0.818	l = −20→20
7465 measured reflections	2 standard reflections every 198 reflections
7113 independent reflections	intensity decay: 2%

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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.127	Only H-atom displacement parameters refined
S = 1.15	w = 1/[σ^2(Fo^2) + (0.052P)^2] where P = (Fo^2 + 2Fc^2)/3
7113 reflections	(Δ/σ)max = 0.002
245 parameters	Δρmax = 1.23 e Å^−3
7 restraints	Δρmin = −1.07 e Å^−3

Special details

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	Occ. (<1)
Yb	0.57857 (3)	0.991285 (13)	0.800031 (19)	0.02393 (9)
C1	0.5584 (7)	1.0899 (3)	0.8998 (5)	0.0320 (15)
H1A	0.4683	1.1034	0.8908	0.057 (12)*
H1B	0.5710	1.0688	0.9617	0.057 (12)*
C2	0.4093 (7)	0.9102 (3)	0.8101 (5)	0.0304 (15)
H2A	0.4263	0.8841	0.8685	0.057 (12)*
H2B	0.3333	0.9400	0.8158	0.057 (12)*
C3	0.7231 (8)	0.9619 (4)	0.6911 (6)	0.0388 (17)
H3A	0.7283	0.9086	0.6914	0.057 (12)*
H3B	0.6796	0.9753	0.6312	0.057 (12)*
O11	0.4596 (5)	1.0586 (3)	0.6887 (3)	0.0337 (11)
O21	0.7037 (5)	0.9281 (3)	0.9098 (4)	0.0383 (12)
Si11	0.6424 (2)	1.17531 (10)	0.90860 (15)	0.0331 (4)
Si21	0.3651 (2)	0.84187 (10)	0.72282 (14)	0.0321 (4)
Si31	0.8845 (2)	0.99302 (12)	0.68795 (16)	0.0426 (5)
C12	0.3306 (9)	1.0815 (6)	0.6983 (7)	0.056 (3)
H12A	0.3292	1.1200	0.7448	0.070 (9)*
H12B	0.2795	1.0404	0.7169	0.070 (9)*
C13	0.2801 (11)	1.1090 (5)	0.6066 (7)	0.060 (3)
H13A	0.2153	1.1466	0.6119	0.070 (9)*
H13B	0.2436	1.0695	0.5674	0.070 (9)*
C14	0.3966 (11)	1.1400 (5)	0.5698 (6)	0.057 (3)
H14A	0.3875	1.1416	0.5024	0.070 (9)*
H14B	0.4151	1.1890	0.5939	0.070 (9)*
C15	0.4974 (10)	1.0872 (4)	0.6047 (5)	0.045 (2)
H15A	0.5049	1.0480	0.5600	0.070 (9)*
H15B	0.5798	1.1118	0.6154	0.070 (9)*
C22	0.7624 (9)	0.9504 (5)	0.9986 (6)	0.047 (2)
H22A	0.7013	0.9756	1.0340	0.070 (9)*
H22B	0.8351	0.9825	0.9921	0.070 (9)*
C23	0.8045 (17)	0.8800 (6)	1.0438 (9)	0.050 (4)*	0.65
H23A	0.8815	0.8877	1.0855	0.070 (9)*	0.65
H23B	0.7378	0.8609	1.0795	0.070 (9)*	0.65
C24	0.8304 (14)	0.8281 (8)	0.9706 (9)	0.057 (4)*	0.65
H24A	0.8204	0.7774	0.9895	0.070 (9)*	0.65
H24B	0.9152	0.8350	0.9497	0.070 (9)*	0.65
C23A	0.851 (3)	0.8916 (11)	1.036 (2)	0.077 (11)*	0.35
H23C	0.9350	0.8953	1.0140	0.070 (9)*	0.35
H23D	0.8585	0.8902	1.1039	0.070 (9)*	0.35
C24A	0.776 (3)	0.8298 (14)	0.9953 (11)	0.057 (7)*	0.35
H24C	0.7054	0.8185	1.0318	0.070 (9)*	0.35
H24D	0.8304	0.7865	0.9936	0.070 (9)*	0.35
C25	0.7270 (11)	0.8514 (4)	0.8996 (7)	0.062 (3)
H25A	0.7523	0.8416	0.8379	0.070 (9)*
H25B	0.6491	0.8239	0.9074	0.070 (9)*
C111	0.6411 (9)	1.2181 (5)	0.7931 (5)	0.0427 (19)
H11A	0.6859	1.1870	0.7531	0.074 (7)*
H11B	0.6830	1.2652	0.7988	0.074 (7)*
H11C	0.5539	1.2246	0.7671	0.074 (7)*
C112	0.5733 (11)	1.2444 (4)	0.9832 (6)	0.054 (3)
H11D	0.5820	1.2278	1.0465	0.074 (7)*
H11E	0.4839	1.2512	0.9631	0.074 (7)*
H11F	0.6179	1.2903	0.9787	0.074 (7)*
C113	0.8099 (9)	1.1612 (5)	0.9564 (8)	0.056 (3)
H11G	0.8519	1.1284	0.9168	0.074 (7)*
H11H	0.8113	1.1402	1.0175	0.074 (7)*
H11I	0.8541	1.2076	0.9600	0.074 (7)*
C211	0.2164 (9)	0.7933 (5)	0.7404 (7)	0.055 (2)
H21A	0.2230	0.7720	0.8015	0.074 (7)*
H21B	0.2022	0.7551	0.6947	0.074 (7)*
H21C	0.1458	0.8273	0.7343	0.074 (7)*
C212	0.3441 (10)	0.8837 (5)	0.6066 (5)	0.046 (2)
H21D	0.4248	0.9031	0.5909	0.074 (7)*
H21E	0.2823	0.9228	0.6064	0.074 (7)*
H21F	0.3141	0.8471	0.5618	0.074 (7)*
C213	0.4881 (10)	0.7713 (5)	0.7193 (8)	0.059 (3)
H21G	0.5004	0.7472	0.7785	0.074 (7)*
H21H	0.5674	0.7937	0.7053	0.074 (7)*
H21I	0.4615	0.7359	0.6720	0.074 (7)*
C311	0.9790 (9)	0.9431 (5)	0.6078 (7)	0.053 (2)
H31A	0.9384	0.9476	0.5456	0.074 (7)*
H31B	0.9840	0.8921	0.6251	0.074 (7)*
H31C	1.0640	0.9635	0.6106	0.074 (7)*
C312	0.8874 (12)	1.0902 (5)	0.6561 (11)	0.088 (5)
H31D	0.8383	1.0974	0.5973	0.074 (7)*
H31E	0.9747	1.1054	0.6515	0.074 (7)*
H31F	0.8509	1.1190	0.7028	0.074 (7)*
C313	0.9775 (11)	0.9820 (8)	0.8026 (8)	0.092 (5)
H31G	0.9415	1.0131	0.8473	0.074 (7)*
H31H	1.0654	0.9957	0.7977	0.074 (7)*
H31I	0.9737	0.9316	0.8221	0.074 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb	0.02505 (14)	0.02125 (12)	0.02524 (13)	−0.00121 (13)	0.00097 (9)	−0.00065 (12)
C1	0.033 (4)	0.028 (3)	0.034 (4)	−0.003 (3)	−0.003 (3)	−0.011 (3)
C2	0.037 (4)	0.024 (3)	0.031 (4)	−0.007 (3)	0.007 (3)	0.002 (2)
C3	0.033 (4)	0.041 (4)	0.043 (4)	0.001 (3)	0.010 (3)	−0.002 (3)
O11	0.037 (3)	0.038 (2)	0.026 (3)	0.008 (2)	0.002 (2)	0.009 (2)
O21	0.040 (3)	0.036 (3)	0.037 (3)	0.004 (2)	−0.010 (2)	0.004 (2)
Si11	0.0357 (12)	0.0260 (8)	0.0368 (11)	−0.0035 (8)	−0.0008 (9)	−0.0015 (8)
Si21	0.0335 (12)	0.0261 (9)	0.0362 (11)	−0.0056 (8)	−0.0003 (9)	−0.0020 (7)
Si31	0.0333 (11)	0.0465 (12)	0.0498 (12)	−0.0082 (10)	0.0134 (9)	−0.0159 (10)
C12	0.045 (6)	0.067 (6)	0.057 (6)	0.022 (5)	0.009 (5)	0.027 (5)
C13	0.062 (7)	0.055 (5)	0.060 (6)	0.014 (5)	−0.012 (5)	0.015 (5)
C14	0.077 (8)	0.050 (5)	0.041 (5)	0.013 (5)	−0.003 (5)	0.013 (4)
C15	0.060 (6)	0.049 (4)	0.025 (4)	0.002 (4)	0.004 (4)	0.008 (3)
C22	0.044 (5)	0.054 (5)	0.041 (5)	−0.003 (4)	−0.007 (4)	−0.001 (4)
C25	0.083 (8)	0.035 (4)	0.061 (6)	0.015 (5)	−0.033 (5)	0.005 (4)
C111	0.039 (5)	0.051 (4)	0.037 (4)	−0.008 (4)	−0.001 (3)	0.006 (3)
C112	0.089 (8)	0.029 (4)	0.043 (5)	0.003 (4)	0.002 (5)	−0.010 (3)
C113	0.038 (5)	0.048 (5)	0.078 (7)	−0.009 (4)	−0.018 (5)	−0.001 (4)
C211	0.042 (6)	0.056 (5)	0.063 (6)	−0.021 (4)	−0.010 (5)	0.005 (4)
C212	0.065 (6)	0.047 (4)	0.027 (4)	−0.001 (4)	0.006 (4)	−0.002 (3)
C213	0.055 (6)	0.040 (4)	0.079 (7)	0.009 (4)	−0.007 (5)	−0.021 (4)
C311	0.043 (6)	0.060 (5)	0.060 (6)	0.007 (4)	0.021 (5)	−0.008 (4)
C312	0.067 (9)	0.037 (5)	0.166 (14)	−0.006 (5)	0.049 (9)	−0.010 (6)
C313	0.049 (6)	0.166 (14)	0.059 (7)	−0.025 (8)	0.006 (5)	−0.043 (8)

Geometric parameters (Å, º)

Yb—C1	2.369 (6)	C23—C24	1.491 (16)
Yb—C2	2.364 (7)	C23—H23A	0.9900
Yb—C3	2.389 (7)	C23—H23B	0.9900
Yb—O11	2.341 (5)	C24—C25	1.511 (10)
Yb—O21	2.319 (5)	C24—H24A	0.9900
C1—Si11	1.819 (7)	C24—H24B	0.9900
C1—H1A	0.9900	C23A—C24A	1.491 (17)
C1—H1B	0.9900	C23A—H23C	0.9900
C2—Si21	1.836 (7)	C23A—H23D	0.9900
C2—H2A	0.9900	C24A—C25	1.513 (11)
C2—H2B	0.9900	C24A—H24C	0.9900
C3—Si31	1.820 (8)	C24A—H24D	0.9900
C3—H3A	0.9900	C25—H25A	0.9900
C3—H3B	0.9900	C25—H25B	0.9900
O11—C15	1.437 (9)	C111—H11A	0.9800
O11—C12	1.459 (11)	C111—H11B	0.9800
O21—C25	1.453 (9)	C111—H11C	0.9800
O21—C22	1.458 (10)	C112—H11D	0.9800
Si11—C113	1.877 (10)	C112—H11E	0.9800
Si11—C111	1.878 (8)	C112—H11F	0.9800
Si11—C112	1.883 (9)	C113—H11G	0.9800
Si21—C213	1.857 (9)	C113—H11H	0.9800
Si21—C211	1.863 (9)	C113—H11I	0.9800
Si21—C212	1.875 (8)	C211—H21A	0.9800
Si31—C312	1.864 (10)	C211—H21B	0.9800
Si31—C311	1.867 (8)	C211—H21C	0.9800
Si31—C313	1.890 (12)	C212—H21D	0.9800
C12—C13	1.499 (13)	C212—H21E	0.9800
C12—H12A	0.9900	C212—H21F	0.9800
C12—H12B	0.9900	C213—H21G	0.9800
C13—C14	1.514 (15)	C213—H21H	0.9800
C13—H13A	0.9900	C213—H21I	0.9800
C13—H13B	0.9900	C311—H31A	0.9800
C14—C15	1.508 (12)	C311—H31B	0.9800
C14—H14A	0.9900	C311—H31C	0.9800
C14—H14B	0.9900	C312—H31D	0.9800
C15—H15A	0.9900	C312—H31E	0.9800
C15—H15B	0.9900	C312—H31F	0.9800
C22—C23A	1.512 (11)	C313—H31G	0.9800
C22—C23	1.514 (10)	C313—H31H	0.9800
C22—H22A	0.9900	C313—H31I	0.9800
C22—H22B	0.9900
O11—Yb—O21	177.49 (19)	C24—C23—H23A	110.1
C1—Yb—O11	87.1 (2)	C22—C23—H23A	110.1
C1—Yb—O21	92.1 (2)	C24—C23—H23B	110.1
C2—Yb—O11	90.9 (2)	C22—C23—H23B	110.1
C2—Yb—O21	91.6 (2)	H23A—C23—H23B	108.5
C3—Yb—O11	89.5 (2)	C23—C24—C25	98.3 (10)
C3—Yb—O21	89.3 (3)	C23—C24—H24A	112.1
C1—Yb—C2	109.8 (2)	C25—C24—H24A	112.1
C1—Yb—C3	134.0 (3)	C23—C24—H24B	112.1
C2—Yb—C3	116.1 (3)	C25—C24—H24B	112.1
Yb—C1—Si11	130.1 (4)	H24A—C24—H24B	109.8
Yb—C2—Si21	122.9 (3)	C24A—C23A—C22	96.6 (16)
Yb—C3—Si31	128.0 (4)	C24A—C23A—H23C	112.4
Si11—C1—H1A	104.7	C22—C23A—H23C	112.4
Yb—C1—H1A	104.7	C24A—C23A—H23D	112.4
Si11—C1—H1B	104.7	C22—C23A—H23D	112.4
Yb—C1—H1B	104.7	H23C—C23A—H23D	110.0
H1A—C1—H1B	105.7	C23A—C24A—C25	107.5 (18)
Si21—C2—H2A	106.6	C23A—C24A—H24C	110.2
Yb—C2—H2A	106.6	C25—C24A—H24C	110.2
Si21—C2—H2B	106.6	C23A—C24A—H24D	110.2
Yb—C2—H2B	106.6	C25—C24A—H24D	110.2
H2A—C2—H2B	106.6	H24C—C24A—H24D	108.5
Si31—C3—H3A	105.3	O21—C25—C24	109.2 (9)
Yb—C3—H3A	105.3	O21—C25—C24A	102.2 (13)
Si31—C3—H3B	105.3	C24—C25—C24A	27.2 (12)
Yb—C3—H3B	105.3	O21—C25—H25A	109.8
H3A—C3—H3B	106.0	C24—C25—H25A	109.8
C15—O11—C12	108.6 (6)	C24A—C25—H25A	135.0
C15—O11—Yb	128.6 (5)	O21—C25—H25B	109.8
C12—O11—Yb	122.8 (4)	C24—C25—H25B	109.8
C25—O21—C22	107.9 (6)	C24A—C25—H25B	88.8
C25—O21—Yb	121.0 (5)	H25A—C25—H25B	108.3
C22—O21—Yb	130.9 (4)	Si11—C111—H11A	109.5
C1—Si11—C113	110.5 (4)	Si11—C111—H11B	109.5
C1—Si11—C111	110.0 (4)	H11A—C111—H11B	109.5
C113—Si11—C111	109.1 (5)	Si11—C111—H11C	109.5
C1—Si11—C112	114.7 (4)	H11A—C111—H11C	109.5
C113—Si11—C112	106.6 (5)	H11B—C111—H11C	109.5
C111—Si11—C112	105.7 (4)	Si11—C112—H11D	109.5
C2—Si21—C213	111.7 (4)	Si11—C112—H11E	109.5
C2—Si21—C211	113.8 (4)	H11D—C112—H11E	109.5
C213—Si21—C211	106.0 (5)	Si11—C112—H11F	109.5
C2—Si21—C212	110.8 (3)	H11D—C112—H11F	109.5
C213—Si21—C212	106.9 (5)	H11E—C112—H11F	109.5
C211—Si21—C212	107.2 (4)	Si11—C113—H11G	109.5
C3—Si31—C312	110.5 (5)	Si11—C113—H11H	109.5
C3—Si31—C311	115.2 (4)	H11G—C113—H11H	109.5
C312—Si31—C311	107.3 (5)	Si11—C113—H11I	109.5
C3—Si31—C313	111.2 (5)	H11G—C113—H11I	109.5
C312—Si31—C313	108.1 (7)	H11H—C113—H11I	109.5
C311—Si31—C313	104.1 (5)	Si21—C211—H21A	109.5
O11—C12—C13	105.9 (8)	Si21—C211—H21B	109.5
O11—C12—H12A	110.6	H21A—C211—H21B	109.5
C13—C12—H12A	110.6	Si21—C211—H21C	109.5
O11—C12—H12B	110.6	H21A—C211—H21C	109.5
C13—C12—H12B	110.6	H21B—C211—H21C	109.5
H12A—C12—H12B	108.7	Si21—C212—H21D	109.5
C12—C13—C14	102.4 (9)	Si21—C212—H21E	109.5
C12—C13—H13A	111.3	H21D—C212—H21E	109.5
C14—C13—H13A	111.3	Si21—C212—H21F	109.5
C12—C13—H13B	111.3	H21D—C212—H21F	109.5
C14—C13—H13B	111.3	H21E—C212—H21F	109.5
H13A—C13—H13B	109.2	Si21—C213—H21G	109.5
C15—C14—C13	102.4 (7)	Si21—C213—H21H	109.5
C15—C14—H14A	111.3	H21G—C213—H21H	109.5
C13—C14—H14A	111.3	Si21—C213—H21I	109.5
C15—C14—H14B	111.3	H21G—C213—H21I	109.5
C13—C14—H14B	111.3	H21H—C213—H21I	109.5
H14A—C14—H14B	109.2	Si31—C311—H31A	109.5
O11—C15—C14	106.6 (7)	Si31—C311—H31B	109.5
O11—C15—H15A	110.4	H31A—C311—H31B	109.5
C14—C15—H15A	110.4	Si31—C311—H31C	109.5
O11—C15—H15B	110.4	H31A—C311—H31C	109.5
C14—C15—H15B	110.4	H31B—C311—H31C	109.5
H15A—C15—H15B	108.6	Si31—C312—H31D	109.5
O21—C22—C23A	109.1 (13)	Si31—C312—H31E	109.5
O21—C22—C23	103.6 (8)	H31D—C312—H31E	109.5
C23A—C22—C23	21.2 (15)	Si31—C312—H31F	109.5
O21—C22—H22A	111.0	H31D—C312—H31F	109.5
C23A—C22—H22A	124.3	H31E—C312—H31F	109.5
C23—C22—H22A	111.0	Si31—C313—H31G	109.5
O21—C22—H22B	111.0	Si31—C313—H31H	109.5
C23A—C22—H22B	90.2	H31G—C313—H31H	109.5
C23—C22—H22B	111.0	Si31—C313—H31I	109.5
H22A—C22—H22B	109.0	H31G—C313—H31I	109.5
C24—C23—C22	107.8 (10)	H31H—C313—H31I	109.5