trans-Di­iodo­pentakis­(tetra­hydro­furan)­ytterbium(III) tetra­iodo-trans-bis­(tetra­hydro­furan)­ytterbium(III)

Niemeyer, M.

doi:10.1107/S1600536801011254

trans-Diiodopentakis(tetrahydrofuran)ytterbium(III) tetraiodo-trans-bis(tetrahydrofuran)ytterbium(III)

The ionic title complex, [YbI₂(thf)₅][YbI₄(thf)₂], was obtained by oxidation of the arylytterbium(II) iodide DppYbI(thf)₃ (Dpp = 2,6-Ph₂C₆H₃) with neopentyl iodide. In the pentagonal-bipyramidal coordinated cation [Yb-I = 2.9366 (9) Å and Yb-O = 2.340 (6), 2.347 (8) and 2.365 (6) Å], a twofold rotation axis passes through the Yb atom, the O atom and the midpoint of the C-C bond of one of the thf ligands. The centrosymmetric anion shows an almost regular coordination octahedron [Yb-I = 2.9641 (8) and 2.9856 (9) Å, and Yb-O 2.279 (6) Å].

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801011254/ya6041sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536801011254/ya6041Isup2.hkl Contains datablock I

CCDC reference: 170873

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.015 Å
R factor = 0.047
wR factor = 0.126
Data-to-parameter ratio = 23.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



PLAT_732  Alert B Angle   Calc    90.28(2), Rep   90.28(16) ....       8.00 s.u-Ratio
                     O11  -YB1  -I1      1.555   1.555   1.555


 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.404     1.000
          Tmin and Tmax expected:      0.117     0.356
          RR =      1.232
          Please check that your absorption correction is appropriate.

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      0.356
          Tmax scaled      0.356 Tmin scaled      0.144


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 1 Alert Level C = Please check

Comment top

In continuation of our work on σ-bonded rare earth organyls we have recently reported the synthesis and structural characterization of the m-terphenyl-substituted compound DppYbI(thf)₃ (Dpp = 2,6-Ph₂C₆H₃) (Heckmann & Niemeyer, 2000). The oxidation of this Grignard-analogous complex with neopentyl iodide did not produce the desired organylytterbium(III) diiodide (Niemeyer, 2000). Instead dichroic crystals of the title complex, (I), were isolated as orange/pale-yellow plates. Complex (I) is isomorphous with its samarium analogue [SmI₂(thf)₅][SmI₄(thf)₂] (Xie et al., 1996). In contrast, THF-solvated lanthanum(III) iodide crystallizes as the neutral coordination compound LaI₃(thf)₄ (Trifonov et al., 1997).

The crystal structure of (I) consists of well separated alternating layers of [YbI₂(thf)₅]⁺ cations and [YbI₄(thf)₂]^- anions. In the seven-coordinate ytterbium cation a crystallographic twofold rotation axis passes through Yb1, O11, and the midpoint of the C13—C13ⁱ bond. The coordinated iodo ligands and THF molecules occupy respectively the axial and equatorial positions of a rather undistorted (O—Yb1—O 72±0.5°; O—Yb1—I 90±0.8°) pentagonal bipyramid. An almost regular coordination octahedron is observed for the centrosymmetric [YbI₄(thf)₂]^- anion. The Yb1—I1 distance of 2.9366 (9) Å in the seven-coordinate cation is significantly shorter than the average Yb2—I bond of 2.9749 Å in the six-coordinate anion. This can be explained by a higher positive partial charge on the ytterbium center in the former (see Experimental). In contrast, the average Yb1—O distance of 2.351 Å is considerably longer than the Yb2—O41 bond length of 2.279 (6) Å. The latter is in the normal range for a trans-O(thf)—Yb^III—O(thf) fragment on a six-coordinate metal center.

Experimental top

The title compound was synthesized by the reaction of DppYbI(thf)₃ (1.33 g, 1.78 mmol) (Heckmann & Niemeyer, 2000) with neopentyl iodide (0.24 ml, 1.81 mmol) in 30 ml of THF solution. After cooling the solution to 263 K for 4 months, dichroic orange/pale-yellow crystals (0.35 g, 0.22 mmol, 14%) were obtained. A population analysis, based on the X-ray geometry (C—H distances set to 1.09 Å; 6–31G* basis sets for C, H, and O; quasi-relativistic pseudo-potentials of the Stuttgart/Bonn group for Yb and I), was calculated on the HF level of theory for the isolated cation and anion to give the following Mulliken charges: Yb1 + 2.014, Yb2 + 1.687.

Computing details top

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.

Figures top

Fig. 1. Displacement ellipsoid plot (40% probability) of the cation and anion in the crystal of (I). H atoms have been omitted for clarity.

Trans-diodo-pentakis(tetrahydrofuran)ytterbium(III)-tetraiodo- trans-bis(tetrahydrofuran)ytterbium(III) top

Crystal data top

[YbI₂(C₄H₈O)₅][YbI₄(C₄H₈O)₂]	F(000) = 2952
M_r = 1612.21	D_x = 2.474 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.722 (2) Å	Cell parameters from 20 reflections
b = 12.037 (3) Å	θ = 8.5–12.0°
c = 28.551 (4) Å	µ = 8.61 mm⁻¹
β = 98.05 (1)°	T = 173 K
V = 4329.1 (13) Å³	Plate, orange
Z = 4	0.32 × 0.22 × 0.12 mm

Data collection top

Rebuild Syntex P2₁/Siemens P3 four-circle diffractometer	3643 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.050
Graphite monochromator	θ_max = 27.0°, θ_min = 2.3°
Wyckoff scans	h = 0→16
Absorption correction: ψ scan (North et al., 1968)	k = 0→15
T_min = 0.404, T_max = 1.000	l = −36→36
4945 measured reflections	2 standard reflections every 198 reflections
4733 independent reflections	intensity decay: none

Refinement top

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.126	H-atom parameters constrained
S = 1.14	w = 1/[σ²(F_o²) + (0.0707P)²] where P = (F_o² + 2F_c²)/3
4733 reflections	(Δ/σ)_max = 0.001
198 parameters	Δρ_max = 3.10 e Å⁻³
0 restraints	Δρ_min = −3.10 e Å⁻³

Crystal data top

[YbI₂(C₄H₈O)₅][YbI₄(C₄H₈O)₂]	V = 4329.1 (13) Å³
M_r = 1612.21	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 12.722 (2) Å	µ = 8.61 mm⁻¹
b = 12.037 (3) Å	T = 173 K
c = 28.551 (4) Å	0.32 × 0.22 × 0.12 mm
β = 98.05 (1)°

Data collection top

Rebuild Syntex P2₁/Siemens P3 four-circle diffractometer	3643 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.050
T_min = 0.404, T_max = 1.000	2 standard reflections every 198 reflections
4945 measured reflections	intensity decay: none
4733 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	0 restraints
wR(F²) = 0.126	H-atom parameters constrained
S = 1.14	Δρ_max = 3.10 e Å⁻³
4733 reflections	Δρ_min = −3.10 e Å⁻³
198 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

	x	y	z	U_iso*/U_eq
Yb1	0.0000	−0.00167 (4)	0.2500	0.01565 (13)
Yb2	0.5000	0.0000	0.5000	0.01986 (14)
I1	0.20953 (4)	−0.00047 (5)	0.21799 (2)	0.02740 (16)
I2	0.46595 (5)	−0.22940 (5)	0.46325 (2)	0.03193 (17)
I3	0.41257 (5)	0.09411 (6)	0.40581 (2)	0.03066 (17)
O11	0.0000	−0.1966 (7)	0.2500	0.0214 (18)
O21	0.0791 (5)	−0.0636 (6)	0.3254 (2)	0.0270 (14)
O31	0.0464 (5)	0.1551 (5)	0.2968 (2)	0.0238 (13)
O41	0.6681 (5)	−0.0052 (5)	0.4810 (3)	0.0332 (17)
C12	0.0541 (7)	−0.2680 (7)	0.2186 (3)	0.0245 (19)
H12A	0.1319	−0.2676	0.2285	0.054 (7)*
H12B	0.0390	−0.2424	0.1854	0.054 (7)*
C13	0.0086 (8)	−0.3833 (7)	0.2239 (3)	0.028 (2)
H13A	0.0592	−0.4419	0.2175	0.054 (7)*
H13B	−0.0592	−0.3937	0.2027	0.054 (7)*
C22	0.1748 (8)	−0.1306 (9)	0.3344 (4)	0.038 (2)
H22A	0.2387	−0.0833	0.3353	0.054 (7)*
H22B	0.1759	−0.1872	0.3093	0.054 (7)*
C23	0.1723 (10)	−0.1846 (12)	0.3809 (4)	0.055 (4)
H23A	0.2447	−0.2028	0.3965	0.054 (7)*
H23B	0.1288	−0.2532	0.3777	0.054 (7)*
C24	0.1209 (10)	−0.0946 (12)	0.4079 (4)	0.055 (4)
H24A	0.0859	−0.1276	0.4335	0.054 (7)*
H24B	0.1744	−0.0399	0.4219	0.054 (7)*
C25	0.0409 (9)	−0.0409 (10)	0.3712 (4)	0.040 (3)
H25A	−0.0305	−0.0734	0.3717	0.054 (7)*
H25B	0.0371	0.0401	0.3769	0.054 (7)*
C32	0.1544 (8)	0.1825 (8)	0.3176 (4)	0.030 (2)
H32A	0.1957	0.2104	0.2932	0.054 (7)*
H32B	0.1907	0.1165	0.3329	0.054 (7)*
C33	0.1429 (9)	0.2717 (9)	0.3538 (4)	0.039 (3)
H33A	0.1312	0.2391	0.3845	0.054 (7)*
H33B	0.2062	0.3204	0.3588	0.054 (7)*
C34	0.0471 (9)	0.3335 (8)	0.3312 (4)	0.041 (3)
H34A	0.0654	0.3854	0.3067	0.054 (7)*
H34B	0.0137	0.3756	0.3550	0.054 (7)*
C35	−0.0241 (8)	0.2424 (8)	0.3098 (4)	0.032 (2)
H35A	−0.0689	0.2141	0.3329	0.054 (7)*
H35B	−0.0709	0.2697	0.2815	0.054 (7)*
C42	0.7123 (8)	0.0858 (8)	0.4573 (4)	0.033 (2)
H42A	0.7578	0.1333	0.4800	0.054 (7)*
H42B	0.6556	0.1320	0.4397	0.054 (7)*
C43	0.7759 (10)	0.0285 (10)	0.4244 (4)	0.046 (3)
H43A	0.8298	0.0787	0.4140	0.054 (7)*
H43B	0.7300	−0.0009	0.3963	0.054 (7)*
C44	0.8273 (9)	−0.0647 (9)	0.4553 (4)	0.041 (3)
H44A	0.8469	−0.1274	0.4358	0.054 (7)*
H44B	0.8916	−0.0381	0.4758	0.054 (7)*
C45	0.7426 (7)	−0.0985 (8)	0.4843 (4)	0.034 (2)
H45A	0.7065	−0.1670	0.4714	0.054 (7)*
H45B	0.7736	−0.1120	0.5176	0.054 (7)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Yb1	0.0154 (2)	0.0179 (3)	0.0126 (2)	0.000	−0.00183 (18)	0.000
Yb2	0.0186 (2)	0.0233 (3)	0.0163 (3)	−0.0040 (2)	−0.00253 (19)	0.0028 (2)
I1	0.0198 (3)	0.0349 (3)	0.0280 (3)	−0.0017 (2)	0.0052 (2)	−0.0040 (3)
I2	0.0341 (3)	0.0275 (3)	0.0321 (3)	−0.0088 (3)	−0.0027 (3)	−0.0040 (3)
I3	0.0333 (3)	0.0385 (4)	0.0175 (3)	−0.0002 (3)	−0.0059 (2)	0.0058 (3)
O11	0.019 (4)	0.021 (4)	0.026 (5)	0.000	0.010 (4)	0.000
O21	0.032 (3)	0.032 (4)	0.014 (3)	−0.001 (3)	−0.006 (3)	0.006 (3)
O31	0.023 (3)	0.025 (3)	0.021 (3)	−0.002 (3)	−0.005 (2)	−0.009 (3)
O41	0.030 (3)	0.032 (4)	0.042 (4)	−0.001 (3)	0.017 (3)	0.006 (3)
C12	0.024 (4)	0.020 (4)	0.028 (5)	0.001 (3)	0.001 (4)	−0.009 (4)
C13	0.030 (5)	0.020 (5)	0.034 (5)	−0.004 (4)	0.001 (4)	−0.002 (4)
C22	0.030 (5)	0.037 (6)	0.040 (6)	0.006 (4)	−0.016 (4)	0.013 (5)
C23	0.039 (6)	0.077 (9)	0.044 (7)	−0.012 (6)	−0.012 (5)	0.032 (7)
C24	0.056 (7)	0.088 (11)	0.017 (5)	−0.019 (7)	−0.004 (5)	0.017 (6)
C25	0.050 (6)	0.048 (6)	0.022 (5)	−0.010 (5)	0.007 (5)	0.008 (5)
C32	0.032 (5)	0.022 (4)	0.031 (5)	−0.002 (4)	−0.008 (4)	−0.007 (4)
C33	0.046 (6)	0.041 (6)	0.028 (5)	−0.016 (5)	−0.004 (5)	−0.016 (5)
C34	0.057 (7)	0.025 (5)	0.042 (6)	−0.002 (5)	0.013 (5)	−0.011 (5)
C35	0.031 (5)	0.031 (5)	0.034 (5)	0.004 (4)	0.007 (4)	−0.005 (4)
C42	0.024 (5)	0.037 (6)	0.038 (6)	−0.005 (4)	0.008 (4)	0.017 (5)
C43	0.056 (7)	0.048 (7)	0.035 (6)	−0.026 (6)	0.018 (6)	−0.010 (5)
C44	0.038 (6)	0.034 (6)	0.055 (7)	−0.004 (5)	0.019 (5)	−0.009 (5)
C45	0.025 (5)	0.031 (5)	0.046 (6)	0.000 (4)	0.005 (4)	0.002 (5)

Geometric parameters (Å, º) top

Yb1—I1	2.9366 (9)	C23—C24	1.53 (2)
Yb1—I1ⁱ	2.9366 (9)	C23—H23A	0.9900
Yb1—O11	2.347 (8)	C23—H23B	0.9900
Yb1—O21	2.365 (6)	C24—C25	1.501 (16)
Yb1—O21ⁱ	2.365 (6)	C24—H24A	0.9900
Yb1—O31	2.340 (6)	C24—H24B	0.9900
Yb1—O31ⁱ	2.340 (6)	C25—H25A	0.9900
Yb2—I2	2.9641 (8)	C25—H25B	0.9900
Yb2—I2ⁱⁱ	2.9641 (8)	C32—C33	1.511 (13)
Yb2—I3	2.9856 (9)	C32—H32A	0.9900
Yb2—I3ⁱⁱ	2.9856 (9)	C32—H32B	0.9900
Yb2—O41	2.279 (6)	C33—C34	1.495 (16)
Yb2—O41ⁱⁱ	2.279 (6)	C33—H33A	0.9900
O11—C12ⁱ	1.479 (9)	C33—H33B	0.9900
O11—C12	1.479 (9)	C34—C35	1.497 (15)
O21—C22	1.453 (12)	C34—H34A	0.9900
O21—C25	1.485 (12)	C34—H34B	0.9900
O31—C32	1.456 (11)	C35—H35A	0.9900
O31—C35	1.463 (11)	C35—H35B	0.9900
O41—C42	1.443 (10)	C42—C43	1.492 (14)
O41—C45	1.464 (11)	C42—H42A	0.9900
C12—C13	1.520 (12)	C42—H42B	0.9900
C12—H12A	0.9900	C43—C44	1.517 (18)
C12—H12B	0.9900	C43—H43A	0.9900
C13—C13ⁱ	1.534 (19)	C43—H43B	0.9900
C13—H13A	0.9900	C44—C45	1.503 (13)
C13—H13B	0.9900	C44—H44A	0.9900
C22—C23	1.483 (15)	C44—H44B	0.9900
C22—H22A	0.9900	C45—H45A	0.9900
C22—H22B	0.9900	C45—H45B	0.9900

I1—Yb1—I1ⁱ	179.44 (3)	C22—C23—C24	101.8 (10)
O11—Yb1—O21	71.64 (16)	C22—C23—H23A	111.4
O21—Yb1—O31	72.1 (2)	C24—C23—H23A	111.4
O31—Yb1—O31ⁱ	72.5 (3)	C22—C23—H23B	111.4
O11—Yb1—O21ⁱ	71.64 (16)	C24—C23—H23B	111.4
O31ⁱ—Yb1—O21ⁱ	72.1 (2)	H23A—C23—H23B	109.3
O31—Yb1—O11	143.74 (15)	C25—C24—C23	104.5 (9)
O31ⁱ—Yb1—O11	143.74 (16)	C25—C24—H24A	110.9
O31—Yb1—O21ⁱ	144.6 (2)	C23—C24—H24A	110.9
O31ⁱ—Yb1—O21	144.6 (2)	C25—C24—H24B	110.9
O21ⁱ—Yb1—O21	143.3 (3)	C23—C24—H24B	110.9
O11—Yb1—I1	90.28 (16)	H24A—C24—H24B	108.9
O21—Yb1—I1	89.73 (16)	O21—C25—C24	105.2 (9)
O31—Yb1—I1	90.37 (14)	O21—C25—H25A	110.7
O11—Yb1—I1ⁱ	90.280 (16)	C24—C25—H25A	110.7
O21ⁱ—Yb1—I1	90.45 (16)	O21—C25—H25B	110.7
O31ⁱ—Yb1—I1	89.17 (14)	C24—C25—H25B	110.7
O31—Yb1—I1ⁱ	89.17 (14)	H25A—C25—H25B	108.8
O31ⁱ—Yb1—I1ⁱ	90.37 (14)	O31—C32—C33	105.3 (8)
O21ⁱ—Yb1—I1ⁱ	89.73 (16)	O31—C32—H32A	110.7
O21—Yb1—I1ⁱ	90.45 (16)	C33—C32—H32A	110.7
I2—Yb2—I3	90.98 (2)	O31—C32—H32B	110.7
I2—Yb2—I3ⁱⁱ	89.02 (2)	C33—C32—H32B	110.7
I2—Yb2—I2ⁱⁱ	180.0	H32A—C32—H32B	108.8
I3ⁱⁱ—Yb2—I3	180.0	C34—C33—C32	102.0 (8)
I2ⁱⁱ—Yb2—I3ⁱⁱ	90.98 (2)	C34—C33—H33A	111.4
I2ⁱⁱ—Yb2—I3	89.02 (2)	C32—C33—H33A	111.4
O41—Yb2—I2	89.19 (17)	C34—C33—H33B	111.4
O41—Yb2—I2ⁱⁱ	90.81 (17)	C32—C33—H33B	111.4
O41—Yb2—I3	92.29 (19)	H33A—C33—H33B	109.2
O41—Yb2—I3ⁱⁱ	87.71 (19)	C33—C34—C35	102.9 (8)
O41ⁱⁱ—Yb2—I2	90.81 (17)	C33—C34—H34A	111.2
O41ⁱⁱ—Yb2—I2ⁱⁱ	89.19 (17)	C35—C34—H34A	111.2
O41ⁱⁱ—Yb2—I3ⁱⁱ	92.29 (19)	C33—C34—H34B	111.2
O41ⁱⁱ—Yb2—I3	87.71 (19)	C35—C34—H34B	111.2
O41—Yb2—O41ⁱⁱ	180.0	H34A—C34—H34B	109.1
C12ⁱ—O11—C12	109.0 (9)	O31—C35—C34	105.8 (8)
C12ⁱ—O11—Yb1	125.5 (4)	O31—C35—H35A	110.6
C12—O11—Yb1	125.5 (4)	C34—C35—H35A	110.6
C22—O21—C25	108.4 (8)	O31—C35—H35B	110.6
C22—O21—Yb1	125.2 (6)	C34—C35—H35B	110.6
C25—O21—Yb1	126.4 (6)	H35A—C35—H35B	108.7
C32—O31—C35	108.1 (7)	O41—C42—C43	103.1 (8)
C32—O31—Yb1	124.4 (5)	O41—C42—H42A	111.1
C35—O31—Yb1	127.6 (5)	C43—C42—H42A	111.1
C42—O41—C45	108.7 (7)	O41—C42—H42B	111.1
C42—O41—Yb2	122.1 (5)	C43—C42—H42B	111.1
C45—O41—Yb2	128.8 (5)	H42A—C42—H42B	109.1
O11—C12—C13	104.7 (7)	C42—C43—C44	101.7 (9)
O11—C12—H12A	110.8	C42—C43—H43A	111.4
C13—C12—H12A	110.8	C44—C43—H43A	111.4
O11—C12—H12B	110.8	C42—C43—H43B	111.4
C13—C12—H12B	110.8	C44—C43—H43B	111.4
H12A—C12—H12B	108.9	H43A—C43—H43B	109.3
C12—C13—C13ⁱ	101.8 (6)	C45—C44—C43	103.7 (9)
C12—C13—H13A	111.4	C45—C44—H44A	111.0
C13ⁱ—C13—H13A	111.4	C43—C44—H44A	111.0
C12—C13—H13B	111.4	C45—C44—H44B	111.0
C13ⁱ—C13—H13B	111.4	C43—C44—H44B	111.0
H13A—C13—H13B	109.3	H44A—C44—H44B	109.0
O21—C22—C23	106.2 (9)	O41—C45—C44	105.4 (8)
O21—C22—H22A	110.5	O41—C45—H45A	110.7
C23—C22—H22A	110.5	C44—C45—H45A	110.7
O21—C22—H22B	110.5	O41—C45—H45B	110.7
C23—C22—H22B	110.5	C44—C45—H45B	110.7
H22A—C22—H22B	108.7	H45A—C45—H45B	108.8

Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[YbI₂(C₄H₈O)₅][YbI₄(C₄H₈O)₂]
M_r	1612.21
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	173
a, b, c (Å)	12.722 (2), 12.037 (3), 28.551 (4)
β (°)	98.05 (1)
V (Å³)	4329.1 (13)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	8.61
Crystal size (mm)	0.32 × 0.22 × 0.12

Data collection
Diffractometer	Rebuild Syntex P2₁/Siemens P3 four-circle diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.404, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	4945, 4733, 3643
R_int	0.050
(sin θ/λ)_max (Å⁻¹)	0.639

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.047, 0.126, 1.14
No. of reflections	4733
No. of parameters	198
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	3.10, −3.10

Computer programs: P3 (Siemens, 1989), P3, XDISK (Siemens 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1998), SHELXTL.

Selected geometric parameters (Å, º) top

Yb1—I1	2.9366 (9)	Yb2—I2	2.9641 (8)
Yb1—O11	2.347 (8)	Yb2—I3	2.9856 (9)
Yb1—O21	2.365 (6)	Yb2—O41	2.279 (6)
Yb1—O31	2.340 (6)

I1—Yb1—I1ⁱ	179.44 (3)	O31—Yb1—I1	90.37 (14)
O11—Yb1—O21	71.64 (16)	O21ⁱ—Yb1—I1	90.45 (16)
O21—Yb1—O31	72.1 (2)	O31ⁱ—Yb1—I1	89.17 (14)
O31—Yb1—O31ⁱ	72.5 (3)	I2—Yb2—I3	90.98 (2)
O11—Yb1—I1	90.28 (16)	O41—Yb2—I2	89.19 (17)
O21—Yb1—I1	89.73 (16)	O41—Yb2—I3	92.29 (19)

Symmetry code: (i) −x, y, −z+1/2.

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trans-Di­iodo­pentakis­(tetra­hydro­furan)­ytterbium(III) tetra­iodo-trans-bis­(tetra­hydro­furan)­ytterbium(III)

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trans-Diiodopentakis(tetrahydrofuran)ytterbium(III) tetraiodo-trans-bis(tetrahydrofuran)ytterbium(III)