Diytterbium(II) lithium indium(III) digermanide, Yb2LiInGe2

You, T.-S.; Bobev, S.

doi:10.1107/S1600536810014595

inorganic compounds

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Volume 66| Part 5| May 2010| Page i43

https://doi.org/10.1107/S1600536810014595

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Diytterbium(II) lithium indium(III) digermanide, Yb₂LiInGe₂

Tae-Soo You ^a and Svilen Bobev ^a ^*

^aDepartment of Chemistry and Biochemistry, University of Delaware, Newark, DE 19716, USA
^*Correspondence e-mail: sbobev@mail.chem.udel.edu

(Received 14 April 2010; accepted 20 April 2010; online 28 April 2010)

The title compound, Yb₂LiInGe₂, a new ordered quaternary intermetallic phase, crystallizes with the orthorhombic Ca₂LiInGe₂ type (Pearson code oP24). The crystal structure contains six crystallographically unique sites in the asymmetric unit, all in special positions with site symmetry .m.. The structure is complex and based on [InGe₄] tetrahedra, which share corners in two directions, forming layers parallel to (001). Yb atoms fill square-pyramidal (Yb1) and octahedral (Yb2) interstices between the [InGe_4/2] layers, while the small Li⁺ atoms fill tetrahedral sites.

Related literature

Isotypic Ae₂LiInGe₂ (Ae = Ca, Sr) compounds have been reported by Mao et al. (2001 ). Other related structures include Ca₂CdSb₂ and Yb₂CdSb₂ (Xia & Bobev, 2007 ), SrInGe and EuInGe (Mao et al., 2002 ), (Eu_1-xCa_x)₃In₂Ge₃ and (Eu_1-xCa_x)₄In₃Ge₄ (You et al., 2010 ), and (Sr_1-xCa_x)₅In₃Ge₆ (You & Bobev, 2010 ). STRUCTURE TIDY (Gelato & Parthé, 1987 ) was used for standardization of the atomic coordinates.

Experimental

Crystal data

Yb₂LiInGe₂
M_r = 613.02
Orthorhombic, P n m a
a = 7.182 (3) Å
b = 4.3899 (18) Å
c = 16.758 (7) Å
V = 528.3 (4) Å³
Z = 4
Mo Kα radiation
μ = 50.42 mm⁻¹
T = 200 K
0.04 × 0.02 × 0.02 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2002 ) T_min = 0.258, T_max = 0.365
6805 measured reflections
735 independent reflections
623 reflections with I > 2σ(I)
R_int = 0.090

Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.059
S = 1.11
735 reflections
35 parameters
Δρ_max = 2.10 e Å⁻³
Δρ_min = −2.86 e Å⁻³

Table 1
Selected bond lengths (Å)

In—Ge1ⁱ	2.7803 (13)
In—Ge1ⁱⁱ	2.7803 (13)
In—Ge2ⁱⁱⁱ	2.809 (2)
In—Ge2	2.8203 (19)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+1, z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y, z+{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, y, -z+{\script{3\over 2}}]$ .

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810014595/wm2327sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810014595/wm2327Isup2.hkl

checkCIF report

Comment top

During our exploratory investigations of lithium-containing germanides using molten indium as a metal flux, the quaternary compound Yb₂LiInGe₂ was obtained for the first time. It crystallizes in space group Pnma and is isostructural with Ae₂LiInGe₂ (Ae = Ca and Sr) compounds which were reported previously by Mao et al. (2001). This finding implies that this series can probably be extended towards other lanthanide metals, which likewise exhibit a stable oxidation state of +II, such as Eu for example.

The crystal structure of the title compound can be readily described as consisting of puckered polyanionic layers of corner-shared [InGe₄] tetrahedra, running parallel to the ab plane and alternately stacked along the c axis (Figure 1). Yb and Li atoms, in turn, can be viewed simply as "electron donors", which provide the electrons to fill the valence shells of In and Ge, as well as "spacers" that separate the [InGe_4/2]^5- polyanionic layers.

The In—Ge bond distances observed within the [InGe₄] tetrahedron range from 2.7803 (13) to 2.8203 (13) Å, and are comparable to those in other indium germanides such as Ca₂LiInGe₂ (2.806 (1) - 2.838 (1)Å; Mao et al., 2001), Sr₂LiInGe₂ (2.885 (1) - 2.926 (1) Å; Mao et al., 2001), EuInGe (2.751 (1) Å; Mao et al., 2002), SrInGe (2.780 Å; Mao et al., 2002), as well as the recently reported (Eu_1-_xCa_x)₃In₂Ge₃ (2.760 (2) - 2.869 (1) Å), (Eu_1-_xCa_x)₄In₃Ge₄ (2.755 (2) - 2.887 (1) Å; You et al., 2010), and (Sr_1-_xCa_x)₅In₃Ge₆ (2.672 (2) - 2.877 (3) Å; You & Bobev, 2010). In the absence of direct In—In or Ge—Ge bonding, the formula of the title compound can be rationalized as follows: [(Yb²⁺)₂(Li⁺)][(4b-In^-) (2b-Ge^2-)₂]. Here, the In atom is tetrahedrally surrounded by four Ge atoms (Ge1 × 2 and Ge2 × 2) and is therefore assigned a formal charge of "-1", while the Ge atoms are 2-bonded, carrying a formal charge of "-2" each (4-bonded and 2-bonded atoms are denoted as 4b- and 2b-, respectively).

Interestingly, the structure of the title compound closely resembles the structure of one of our previously reported antimonides, viz. Ca₂CdSb₂ (Xia & Bobev, 2007). The latter structure is also made up of corrugated layers of corner-shared [CdSb₄] tetrahedra, with Ca²⁺ cations filling the space between them. The obvious difference between these two structure types is the addition of Li atoms in Yb₂LiInGe₂, filling small tetrahedral holes between the layers (Figure 1).

Related literature top

Isotypic Ae₂LiInGe₂ (Ae = Ca, Sr) compounds have been reported by Mao et al. (2001). Other related structures include Ca₂CdSb₂ and Yb₂CdSb₂ (Xia & Bobev, 2007), SrInGe and EuInGe (Mao et al., 2002), (Eu_1-_xCa_x)₃In₂Ge₃ and (Eu_1-_xCa_x)₄In₃Ge₄ (You et al., 2010), and (Sr_1-_xCa_x)₅In₃Ge₆ (You & Bobev, 2010). STRUCTURE TIDY (Gelato & Parthé, 1987) was used for standardization of the atomic coordinates.

Experimental top

The flux reaction was carried out in a 2 cm³ alumina crucible, using a total ca 500 mg mixture of the elements (Yb and Ge from Alfa, Li from Sigma-Aldrich), which was then topped off with ca 2 grams of In (Alfa, shots) acting as a metal flux. The crucible was subsequently enclosed and flame-sealed in an evacuated fused silica ampoule, and then was heated at 120 Kh^-1 to 1223 K, kept there for 10 h, cooled to 573 K, where the excess In was removed by centrifugation.

Structure description top

Isotypic Ae₂LiInGe₂ (Ae = Ca, Sr) compounds have been reported by Mao et al. (2001). Other related structures include Ca₂CdSb₂ and Yb₂CdSb₂ (Xia & Bobev, 2007), SrInGe and EuInGe (Mao et al., 2002), (Eu_1-_xCa_x)₃In₂Ge₃ and (Eu_1-_xCa_x)₄In₃Ge₄ (You et al., 2010), and (Sr_1-_xCa_x)₅In₃Ge₆ (You & Bobev, 2010). STRUCTURE TIDY (Gelato & Parthé, 1987) was used for standardization of the atomic coordinates.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. Combined ellipsoid and polyhedral representations of the crystal structure of orthorhombic Yb₂LiInGe₂, viewed along [010]. Color code: Yb - light grey, Li - dark yellow, In - light blue, and Ge - magenta. Ellipsoids are drawn at the 90% probability level.

Diytterbium(II) lithium indium(III) digermanide top

Crystal data top

Yb₂LiInGe₂	F(000) = 1024
M_r = 613.02	D_x = 7.707 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 735 reflections
a = 7.182 (3) Å	θ = 2.4–28.2°
b = 4.3899 (18) Å	µ = 50.42 mm⁻¹
c = 16.758 (7) Å	T = 200 K
V = 528.3 (4) Å³	Needle, grey-silver
Z = 4	0.04 × 0.02 × 0.02 mm

Data collection top

Bruker SMART APEX diffractometer	735 independent reflections
Radiation source: fine-focus sealed tube	623 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.090
ω scans	θ_max = 28.2°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −9→9
T_min = 0.258, T_max = 0.365	k = −5→5
6805 measured reflections	l = −22→22

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)] = 0.029	w = 1/[σ²(F_o²) + (0.P)² + 1.4209P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.059	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 2.10 e Å⁻³
735 reflections	Δρ_min = −2.86 e Å⁻³
35 parameters	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00117 (14)

Crystal data top

Yb₂LiInGe₂	V = 528.3 (4) Å³
M_r = 613.02	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 7.182 (3) Å	µ = 50.42 mm⁻¹
b = 4.3899 (18) Å	T = 200 K
c = 16.758 (7) Å	0.04 × 0.02 × 0.02 mm

Data collection top

Bruker SMART APEX diffractometer	735 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2002)	623 reflections with I > 2σ(I)
T_min = 0.258, T_max = 0.365	R_int = 0.090
6805 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	35 parameters
wR(F²) = 0.059	0 restraints
S = 1.11	Δρ_max = 2.10 e Å⁻³
735 reflections	Δρ_min = −2.86 e Å⁻³

Special details top

Experimental. Selected in the glove box, crystals were put in a Paratone N oil and cut to the desired dimensions. The chosen crystal was mounted on a tip of a glass fiber and quickly transferred onto the goniometer. The crystal was kept under a cold nitrogen stream to protect from the ambient air and moisture.

Data collection is performed with four batch runs at φ = 0.00 ° (607 frames), at φ = 90.00 ° (607 frames), at φ = 180.00 ° (607 frames), and at φ = 270.00 (607 frames). Frame width = 0.30 ° in ω. Data are merged and treated with multi-scan absorption corrections.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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	0.01067 (8)	0.2500	0.27892 (3)	0.00935 (17)
Yb2	0.15804 (9)	0.2500	0.06161 (3)	0.01085 (17)
In	0.15783 (13)	0.2500	0.84697 (5)	0.0079 (2)
Ge1	0.22805 (19)	0.2500	0.43629 (8)	0.0078 (3)
Ge2	0.27452 (18)	0.2500	0.68627 (8)	0.0065 (3)
Li1	0.011 (4)	0.2500	0.5672 (16)	0.023 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Yb1	0.0083 (3)	0.0110 (3)	0.0088 (3)	0.000	0.0001 (2)	0.000
Yb2	0.0116 (3)	0.0121 (3)	0.0089 (3)	0.000	−0.0001 (2)	0.000
In	0.0076 (5)	0.0102 (4)	0.0060 (5)	0.000	−0.0004 (3)	0.000
Ge1	0.0094 (7)	0.0087 (6)	0.0052 (7)	0.000	0.0004 (5)	0.000
Ge2	0.0058 (7)	0.0083 (6)	0.0054 (7)	0.000	0.0002 (5)	0.000

Geometric parameters (Å, º) top

Yb1—Ge2ⁱ	3.0583 (13)	In—Yb1^viii	3.4331 (12)
Yb1—Ge2ⁱⁱ	3.0583 (13)	In—Yb1^ix	3.4331 (12)
Yb1—Ge1	3.0646 (18)	In—Yb2ⁱ	3.5087 (12)
Yb1—Ge2ⁱⁱⁱ	3.0997 (13)	In—Yb2ⁱⁱ	3.5087 (12)
Yb1—Ge2^iv	3.0997 (13)	In—Yb2^xii	3.5969 (18)
Yb1—Inⁱ	3.2760 (12)	Ge1—Li1	2.69 (3)
Yb1—Inⁱⁱ	3.2760 (12)	Ge1—In^iv	2.7803 (13)
Yb1—Li1ⁱⁱ	3.39 (2)	Ge1—Inⁱⁱⁱ	2.7803 (13)
Yb1—Li1ⁱ	3.39 (2)	Ge1—Li1ⁱ	2.786 (17)
Yb1—Inⁱⁱⁱ	3.4331 (12)	Ge1—Li1ⁱⁱ	2.786 (17)
Yb1—In^iv	3.4331 (12)	Ge1—Yb2^vi	3.0883 (19)
Yb1—Yb2^v	3.6817 (13)	Ge1—Yb2^viii	3.1460 (13)
Yb2—Ge2ⁱⁱⁱ	3.0686 (13)	Ge1—Yb2^ix	3.1460 (13)
Yb2—Ge2^iv	3.0686 (13)	Ge2—Li1	2.75 (3)
Yb2—Ge1^v	3.088 (2)	Ge2—In^xi	2.809 (2)
Yb2—Ge1^iv	3.1460 (13)	Ge2—Yb1ⁱ	3.0583 (13)
Yb2—Ge1ⁱⁱⁱ	3.1460 (13)	Ge2—Yb1ⁱⁱ	3.0583 (13)
Yb2—Li1ⁱⁱⁱ	3.24 (2)	Ge2—Yb2^ix	3.0686 (13)
Yb2—Li1^iv	3.24 (2)	Ge2—Yb2^viii	3.0686 (13)
Yb2—Li1^vi	3.33 (3)	Ge2—Yb1^viii	3.0997 (13)
Yb2—Inⁱ	3.5087 (12)	Ge2—Yb1^ix	3.0997 (13)
Yb2—Inⁱⁱ	3.5087 (12)	Li1—Ge1ⁱ	2.786 (17)
Yb2—In^vii	3.5969 (18)	Li1—Ge1ⁱⁱ	2.786 (17)
Yb2—Yb1^vi	3.6817 (13)	Li1—In^x	2.91 (3)
In—Ge1^viii	2.7803 (13)	Li1—Li1ⁱ	3.15 (4)
In—Ge1^ix	2.7803 (13)	Li1—Li1ⁱⁱ	3.15 (4)
In—Ge2^x	2.809 (2)	Li1—Yb2^viii	3.24 (2)
In—Ge2	2.8203 (19)	Li1—Yb2^ix	3.24 (2)
In—Li1^xi	2.91 (3)	Li1—Yb2^v	3.33 (3)
In—Yb1ⁱ	3.2760 (12)	Li1—Yb1ⁱⁱ	3.39 (2)
In—Yb1ⁱⁱ	3.2760 (12)	Li1—Yb1ⁱ	3.39 (2)

Ge2ⁱ—Yb1—Ge2ⁱⁱ	91.73 (5)	Ge1^viii—In—Yb2ⁱ	116.71 (5)
Ge2ⁱ—Yb1—Ge1	100.19 (4)	Ge1^ix—In—Yb2ⁱ	57.43 (4)
Ge2ⁱⁱ—Yb1—Ge1	100.19 (4)	Ge2^x—In—Yb2ⁱ	56.83 (3)
Ge2ⁱ—Yb1—Ge2ⁱⁱⁱ	159.57 (3)	Ge2—In—Yb2ⁱ	127.52 (3)
Ge2ⁱⁱ—Yb1—Ge2ⁱⁱⁱ	85.45 (3)	Li1^xi—In—Yb2ⁱ	110.3 (4)
Ge1—Yb1—Ge2ⁱⁱⁱ	100.22 (4)	Yb1ⁱ—In—Yb2ⁱ	67.86 (3)
Ge2ⁱ—Yb1—Ge2^iv	85.45 (3)	Yb1ⁱⁱ—In—Yb2ⁱ	117.48 (4)
Ge2ⁱⁱ—Yb1—Ge2^iv	159.57 (3)	Yb1^viii—In—Yb2ⁱ	173.39 (3)
Ge1—Yb1—Ge2^iv	100.22 (4)	Yb1^ix—In—Yb2ⁱ	101.15 (3)
Ge2ⁱⁱⁱ—Yb1—Ge2^iv	90.16 (5)	Ge1^viii—In—Yb2ⁱⁱ	57.43 (4)
Ge2ⁱ—Yb1—Inⁱ	52.74 (3)	Ge1^ix—In—Yb2ⁱⁱ	116.71 (4)
Ge2ⁱⁱ—Yb1—Inⁱ	110.87 (4)	Ge2^x—In—Yb2ⁱⁱ	56.83 (3)
Ge1—Yb1—Inⁱ	137.93 (2)	Ge2—In—Yb2ⁱⁱ	127.52 (3)
Ge2ⁱⁱⁱ—Yb1—Inⁱ	109.62 (4)	Li1^xi—In—Yb2ⁱⁱ	110.3 (4)
Ge2^iv—Yb1—Inⁱ	52.18 (4)	Yb1ⁱ—In—Yb2ⁱⁱ	117.48 (4)
Ge2ⁱ—Yb1—Inⁱⁱ	110.87 (4)	Yb1ⁱⁱ—In—Yb2ⁱⁱ	67.86 (3)
Ge2ⁱⁱ—Yb1—Inⁱⁱ	52.74 (3)	Yb1^viii—In—Yb2ⁱⁱ	101.15 (3)
Ge1—Yb1—Inⁱⁱ	137.93 (2)	Yb1^ix—In—Yb2ⁱⁱ	173.39 (3)
Ge2ⁱⁱⁱ—Yb1—Inⁱⁱ	52.18 (4)	Yb2ⁱ—In—Yb2ⁱⁱ	77.45 (4)
Ge2^iv—Yb1—Inⁱⁱ	109.62 (4)	Ge1^viii—In—Yb2^xii	57.42 (3)
Inⁱ—Yb1—Inⁱⁱ	84.13 (4)	Ge1^ix—In—Yb2^xii	57.42 (3)
Ge2ⁱ—Yb1—Li1ⁱⁱ	106.8 (4)	Ge2^x—In—Yb2^xii	101.46 (4)
Ge2ⁱⁱ—Yb1—Li1ⁱⁱ	50.2 (4)	Ge2—In—Yb2^xii	162.69 (4)
Ge1—Yb1—Li1ⁱⁱ	50.8 (4)	Li1^xi—In—Yb2^xii	60.4 (5)
Ge2ⁱⁱⁱ—Yb1—Li1ⁱⁱ	86.9 (3)	Yb1ⁱ—In—Yb2^xii	130.10 (2)
Ge2^iv—Yb1—Li1ⁱⁱ	149.6 (4)	Yb1ⁱⁱ—In—Yb2^xii	130.10 (2)
Inⁱ—Yb1—Li1ⁱⁱ	155.1 (4)	Yb1^viii—In—Yb2^xii	109.38 (3)
Inⁱⁱ—Yb1—Li1ⁱⁱ	92.3 (3)	Yb1^ix—In—Yb2^xii	109.38 (3)
Ge2ⁱ—Yb1—Li1ⁱ	50.2 (4)	Yb2ⁱ—In—Yb2^xii	64.13 (2)
Ge2ⁱⁱ—Yb1—Li1ⁱ	106.8 (4)	Yb2ⁱⁱ—In—Yb2^xii	64.13 (2)
Ge1—Yb1—Li1ⁱ	50.8 (4)	Li1—Ge1—In^iv	127.56 (6)
Ge2ⁱⁱⁱ—Yb1—Li1ⁱ	149.6 (4)	Li1—Ge1—Inⁱⁱⁱ	127.56 (6)
Ge2^iv—Yb1—Li1ⁱ	86.9 (3)	In^iv—Ge1—Inⁱⁱⁱ	104.27 (6)
Inⁱ—Yb1—Li1ⁱ	92.3 (3)	Li1—Ge1—Li1ⁱ	70.1 (7)
Inⁱⁱ—Yb1—Li1ⁱ	155.1 (4)	In^iv—Ge1—Li1ⁱ	63.1 (5)
Li1ⁱⁱ—Yb1—Li1ⁱ	80.7 (6)	Inⁱⁱⁱ—Ge1—Li1ⁱ	142.4 (5)
Ge2ⁱ—Yb1—Inⁱⁱⁱ	149.31 (4)	Li1—Ge1—Li1ⁱⁱ	70.1 (7)
Ge2ⁱⁱ—Yb1—Inⁱⁱⁱ	86.68 (4)	In^iv—Ge1—Li1ⁱⁱ	142.4 (5)
Ge1—Yb1—Inⁱⁱⁱ	50.28 (2)	Inⁱⁱⁱ—Ge1—Li1ⁱⁱ	63.1 (5)
Ge2ⁱⁱⁱ—Yb1—Inⁱⁱⁱ	50.84 (3)	Li1ⁱ—Ge1—Li1ⁱⁱ	104.0 (9)
Ge2^iv—Yb1—Inⁱⁱⁱ	105.90 (4)	Li1—Ge1—Yb1	113.9 (6)
Inⁱ—Yb1—Inⁱⁱⁱ	153.95 (3)	In^iv—Ge1—Yb1	71.75 (4)
Inⁱⁱ—Yb1—Inⁱⁱⁱ	92.39 (3)	Inⁱⁱⁱ—Ge1—Yb1	71.75 (4)
Li1ⁱⁱ—Yb1—Inⁱⁱⁱ	50.6 (4)	Li1ⁱ—Ge1—Yb1	70.6 (5)
Li1ⁱ—Yb1—Inⁱⁱⁱ	101.1 (4)	Li1ⁱⁱ—Ge1—Yb1	70.6 (5)
Ge2ⁱ—Yb1—In^iv	86.68 (4)	Li1—Ge1—Yb2^vi	124.8 (6)
Ge2ⁱⁱ—Yb1—In^iv	149.31 (4)	In^iv—Ge1—Yb2^vi	73.22 (3)
Ge1—Yb1—In^iv	50.28 (2)	Inⁱⁱⁱ—Ge1—Yb2^vi	73.22 (3)
Ge2ⁱⁱⁱ—Yb1—In^iv	105.90 (4)	Li1ⁱ—Ge1—Yb2^vi	128.0 (4)
Ge2^iv—Yb1—In^iv	50.84 (3)	Li1ⁱⁱ—Ge1—Yb2^vi	128.0 (4)
Inⁱ—Yb1—In^iv	92.39 (3)	Yb1—Ge1—Yb2^vi	121.28 (5)
Inⁱⁱ—Yb1—In^iv	153.95 (3)	Li1—Ge1—Yb2^viii	66.8 (4)
Li1ⁱⁱ—Yb1—In^iv	101.1 (4)	In^iv—Ge1—Yb2^viii	146.46 (6)
Li1ⁱ—Yb1—In^iv	50.6 (4)	Inⁱⁱⁱ—Ge1—Yb2^viii	74.45 (4)
Inⁱⁱⁱ—Yb1—In^iv	79.49 (4)	Li1ⁱ—Ge1—Yb2^viii	136.4 (5)
Ge2ⁱ—Yb1—Yb2^v	53.19 (3)	Li1ⁱⁱ—Ge1—Yb2^viii	67.9 (5)
Ge2ⁱⁱ—Yb1—Yb2^v	53.19 (3)	Yb1—Ge1—Yb2^viii	134.98 (3)
Ge1—Yb1—Yb2^v	74.08 (4)	Yb2^vi—Ge1—Yb2^viii	74.48 (3)
Ge2ⁱⁱⁱ—Yb1—Yb2^v	134.90 (2)	Li1—Ge1—Yb2^ix	66.8 (4)
Ge2^iv—Yb1—Yb2^v	134.90 (2)	In^iv—Ge1—Yb2^ix	74.45 (4)
Inⁱ—Yb1—Yb2^v	102.32 (3)	Inⁱⁱⁱ—Ge1—Yb2^ix	146.46 (6)
Inⁱⁱ—Yb1—Yb2^v	102.32 (3)	Li1ⁱ—Ge1—Yb2^ix	67.9 (5)
Li1ⁱⁱ—Yb1—Yb2^v	54.3 (4)	Li1ⁱⁱ—Ge1—Yb2^ix	136.4 (5)
Li1ⁱ—Yb1—Yb2^v	54.3 (4)	Yb1—Ge1—Yb2^ix	134.98 (3)
Inⁱⁱⁱ—Yb1—Yb2^v	103.64 (3)	Yb2^vi—Ge1—Yb2^ix	74.48 (3)
In^iv—Yb1—Yb2^v	103.64 (3)	Yb2^viii—Ge1—Yb2^ix	88.48 (5)
Ge2ⁱⁱⁱ—Yb2—Ge2^iv	91.33 (5)	Li1—Ge2—In^xi	122.1 (6)
Ge2ⁱⁱⁱ—Yb2—Ge1^v	98.63 (3)	Li1—Ge2—In	119.2 (6)
Ge2^iv—Yb2—Ge1^v	98.63 (3)	In^xi—Ge2—In	118.72 (5)
Ge2ⁱⁱⁱ—Yb2—Ge1^iv	155.85 (4)	Li1—Ge2—Yb1ⁱ	71.2 (4)
Ge2^iv—Yb2—Ge1^iv	85.09 (4)	In^xi—Ge2—Yb1ⁱ	133.97 (2)
Ge1^v—Yb2—Ge1^iv	105.52 (3)	In—Ge2—Yb1ⁱ	67.60 (3)
Ge2ⁱⁱⁱ—Yb2—Ge1ⁱⁱⁱ	85.09 (4)	Li1—Ge2—Yb1ⁱⁱ	71.2 (4)
Ge2^iv—Yb2—Ge1ⁱⁱⁱ	155.85 (4)	In^xi—Ge2—Yb1ⁱⁱ	133.97 (2)
Ge1^v—Yb2—Ge1ⁱⁱⁱ	105.52 (3)	In—Ge2—Yb1ⁱⁱ	67.60 (3)
Ge1^iv—Yb2—Ge1ⁱⁱⁱ	88.48 (5)	Yb1ⁱ—Ge2—Yb1ⁱⁱ	91.73 (5)
Ge2ⁱⁱⁱ—Yb2—Li1ⁱⁱⁱ	51.6 (4)	Li1—Ge2—Yb2^ix	67.4 (4)
Ge2^iv—Yb2—Li1ⁱⁱⁱ	110.4 (4)	In^xi—Ge2—Yb2^ix	73.16 (3)
Ge1^v—Yb2—Li1ⁱⁱⁱ	137.2 (3)	In—Ge2—Yb2^ix	134.18 (3)
Ge1^iv—Yb2—Li1ⁱⁱⁱ	107.5 (4)	Yb1ⁱ—Ge2—Yb2^ix	73.87 (3)
Ge1ⁱⁱⁱ—Yb2—Li1ⁱⁱⁱ	49.9 (4)	Yb1ⁱⁱ—Ge2—Yb2^ix	138.50 (5)
Ge2ⁱⁱⁱ—Yb2—Li1^iv	110.4 (4)	Li1—Ge2—Yb2^viii	67.4 (4)
Ge2^iv—Yb2—Li1^iv	51.6 (4)	In^xi—Ge2—Yb2^viii	73.16 (3)
Ge1^v—Yb2—Li1^iv	137.2 (3)	In—Ge2—Yb2^viii	134.18 (3)
Ge1^iv—Yb2—Li1^iv	49.9 (4)	Yb1ⁱ—Ge2—Yb2^viii	138.50 (5)
Ge1ⁱⁱⁱ—Yb2—Li1^iv	107.5 (4)	Yb1ⁱⁱ—Ge2—Yb2^viii	73.87 (3)
Li1ⁱⁱⁱ—Yb2—Li1^iv	85.4 (7)	Yb2^ix—Ge2—Yb2^viii	91.33 (5)
Ge2ⁱⁱⁱ—Yb2—Li1^vi	108.7 (3)	Li1—Ge2—Yb1^viii	134.90 (3)
Ge2^iv—Yb2—Li1^vi	108.7 (3)	In^xi—Ge2—Yb1^viii	67.14 (3)
Ge1^v—Yb2—Li1^vi	140.2 (5)	In—Ge2—Yb1^viii	70.71 (3)
Ge1^iv—Yb2—Li1^vi	50.9 (2)	Yb1ⁱ—Ge2—Yb1^viii	138.24 (5)
Ge1ⁱⁱⁱ—Yb2—Li1^vi	50.9 (2)	Yb1ⁱⁱ—Ge2—Yb1^viii	74.31 (3)
Li1ⁱⁱⁱ—Yb2—Li1^vi	57.3 (6)	Yb2^ix—Ge2—Yb1^viii	140.26 (5)
Li1^iv—Yb2—Li1^vi	57.3 (6)	Yb2^viii—Ge2—Yb1^viii	75.87 (3)
Ge2ⁱⁱⁱ—Yb2—Inⁱ	104.61 (4)	Li1—Ge2—Yb1^ix	134.90 (3)
Ge2^iv—Yb2—Inⁱ	50.01 (3)	In^xi—Ge2—Yb1^ix	67.14 (3)
Ge1^v—Yb2—Inⁱ	49.35 (3)	In—Ge2—Yb1^ix	70.71 (3)
Ge1^iv—Yb2—Inⁱ	91.33 (3)	Yb1ⁱ—Ge2—Yb1^ix	74.31 (3)
Ge1ⁱⁱⁱ—Yb2—Inⁱ	153.64 (4)	Yb1ⁱⁱ—Ge2—Yb1^ix	138.24 (5)
Li1ⁱⁱⁱ—Yb2—Inⁱ	152.4 (5)	Yb2^ix—Ge2—Yb1^ix	75.87 (3)
Li1^iv—Yb2—Inⁱ	92.2 (4)	Yb2^viii—Ge2—Yb1^ix	140.26 (5)
Li1^vi—Yb2—Inⁱ	140.83 (7)	Yb1^viii—Ge2—Yb1^ix	90.16 (5)
Ge2ⁱⁱⁱ—Yb2—Inⁱⁱ	50.01 (3)	Ge1—Li1—Ge2	101.1 (9)
Ge2^iv—Yb2—Inⁱⁱ	104.61 (4)	Ge1—Li1—Ge1ⁱ	109.9 (7)
Ge1^v—Yb2—Inⁱⁱ	49.35 (3)	Ge2—Li1—Ge1ⁱ	116.0 (6)
Ge1^iv—Yb2—Inⁱⁱ	153.64 (4)	Ge1—Li1—Ge1ⁱⁱ	109.9 (7)
Ge1ⁱⁱⁱ—Yb2—Inⁱⁱ	91.33 (3)	Ge2—Li1—Ge1ⁱⁱ	116.0 (6)
Li1ⁱⁱⁱ—Yb2—Inⁱⁱ	92.2 (4)	Ge1ⁱ—Li1—Ge1ⁱⁱ	104.0 (9)
Li1^iv—Yb2—Inⁱⁱ	152.4 (5)	Ge1—Li1—In^x	155.0 (11)
Li1^vi—Yb2—Inⁱⁱ	140.83 (7)	Ge2—Li1—In^x	103.9 (8)
Inⁱ—Yb2—Inⁱⁱ	77.45 (4)	Ge1ⁱ—Li1—In^x	58.3 (5)
Ge2ⁱⁱⁱ—Yb2—In^vii	132.91 (3)	Ge1ⁱⁱ—Li1—In^x	58.3 (5)
Ge2^iv—Yb2—In^vii	132.91 (3)	Ge1—Li1—Li1ⁱ	56.3 (8)
Ge1^v—Yb2—In^vii	90.63 (3)	Ge2—Li1—Li1ⁱ	123.5 (10)
Ge1^iv—Yb2—In^vii	48.13 (3)	Ge1ⁱ—Li1—Li1ⁱ	53.5 (5)
Ge1ⁱⁱⁱ—Yb2—In^vii	48.13 (3)	Ge1ⁱⁱ—Li1—Li1ⁱ	120.3 (13)
Li1ⁱⁱⁱ—Yb2—In^vii	91.7 (5)	In^x—Li1—Li1ⁱ	108.1 (11)
Li1^iv—Yb2—In^vii	91.7 (5)	Ge1—Li1—Li1ⁱⁱ	56.3 (8)
Li1^vi—Yb2—In^vii	49.6 (5)	Ge2—Li1—Li1ⁱⁱ	123.5 (10)
Inⁱ—Yb2—In^vii	115.87 (2)	Ge1ⁱ—Li1—Li1ⁱⁱ	120.3 (13)
Inⁱⁱ—Yb2—In^vii	115.87 (2)	Ge1ⁱⁱ—Li1—Li1ⁱⁱ	53.5 (5)
Ge2ⁱⁱⁱ—Yb2—Yb1^vi	52.94 (3)	In^x—Li1—Li1ⁱⁱ	108.1 (11)
Ge2^iv—Yb2—Yb1^vi	52.94 (3)	Li1ⁱ—Li1—Li1ⁱⁱ	88.4 (13)
Ge1^v—Yb2—Yb1^vi	132.81 (4)	Ge1—Li1—Yb2^viii	63.3 (5)
Ge1^iv—Yb2—Yb1^vi	107.80 (4)	Ge2—Li1—Yb2^viii	61.0 (5)
Ge1ⁱⁱⁱ—Yb2—Yb1^vi	107.80 (4)	Ge1ⁱ—Li1—Yb2^viii	170.3 (8)
Li1ⁱⁱⁱ—Yb2—Yb1^vi	58.2 (4)	Ge1ⁱⁱ—Li1—Yb2^viii	85.27 (12)
Li1^iv—Yb2—Yb1^vi	58.2 (4)	In^x—Li1—Yb2^viii	130.8 (5)
Li1^vi—Yb2—Yb1^vi	87.0 (5)	Li1ⁱ—Li1—Yb2^viii	119.2 (13)
Inⁱ—Yb2—Yb1^vi	97.34 (3)	Li1ⁱⁱ—Li1—Yb2^viii	62.8 (6)
Inⁱⁱ—Yb2—Yb1^vi	97.34 (3)	Ge1—Li1—Yb2^ix	63.3 (5)
In^vii—Yb2—Yb1^vi	136.56 (3)	Ge2—Li1—Yb2^ix	61.0 (5)
Ge1^viii—In—Ge1^ix	104.27 (6)	Ge1ⁱ—Li1—Yb2^ix	85.27 (12)
Ge1^viii—In—Ge2^x	113.31 (4)	Ge1ⁱⁱ—Li1—Yb2^ix	170.3 (8)
Ge1^ix—In—Ge2^x	113.31 (4)	In^x—Li1—Yb2^ix	130.8 (5)
Ge1^viii—In—Ge2	115.24 (4)	Li1ⁱ—Li1—Yb2^ix	62.8 (6)
Ge1^ix—In—Ge2	115.24 (4)	Li1ⁱⁱ—Li1—Yb2^ix	119.2 (13)
Ge2^x—In—Ge2	95.85 (4)	Yb2^viii—Li1—Yb2^ix	85.4 (6)
Ge1^viii—In—Li1^xi	58.5 (2)	Ge1—Li1—Yb2^v	85.0 (7)
Ge1^ix—In—Li1^xi	58.5 (2)	Ge2—Li1—Yb2^v	173.9 (10)
Ge2^x—In—Li1^xi	161.9 (5)	Ge1ⁱ—Li1—Yb2^v	61.2 (5)
Ge2—In—Li1^xi	102.3 (5)	Ge1ⁱⁱ—Li1—Yb2^v	61.2 (5)
Ge1^viii—In—Yb1ⁱ	169.90 (3)	In^x—Li1—Yb2^v	70.0 (6)
Ge1^ix—In—Yb1ⁱ	85.79 (4)	Li1ⁱ—Li1—Yb2^v	59.9 (8)
Ge2^x—In—Yb1ⁱ	60.68 (3)	Li1ⁱⁱ—Li1—Yb2^v	59.9 (9)
Ge2—In—Yb1ⁱ	59.66 (3)	Yb2^viii—Li1—Yb2^v	122.7 (6)
Li1^xi—In—Yb1ⁱ	129.7 (3)	Yb2^ix—Li1—Yb2^v	122.7 (6)
Ge1^viii—In—Yb1ⁱⁱ	85.79 (4)	Ge1—Li1—Yb1ⁱⁱ	130.3 (6)
Ge1^ix—In—Yb1ⁱⁱ	169.90 (3)	Ge2—Li1—Yb1ⁱⁱ	58.6 (4)
Ge2^x—In—Yb1ⁱⁱ	60.68 (3)	Ge1ⁱ—Li1—Yb1ⁱⁱ	119.9 (9)
Ge2—In—Yb1ⁱⁱ	59.66 (3)	Ge1ⁱⁱ—Li1—Yb1ⁱⁱ	58.5 (3)
Li1^xi—In—Yb1ⁱⁱ	129.7 (3)	In^x—Li1—Yb1ⁱⁱ	65.5 (5)
Yb1ⁱ—In—Yb1ⁱⁱ	84.13 (4)	Li1ⁱ—Li1—Yb1ⁱⁱ	173.3 (13)
Ge1^viii—In—Yb1^viii	57.97 (4)	Li1ⁱⁱ—Li1—Yb1ⁱⁱ	95.2 (4)
Ge1^ix—In—Yb1^viii	118.63 (5)	Yb2^viii—Li1—Yb1ⁱⁱ	67.4 (3)
Ge2^x—In—Yb1^viii	127.87 (3)	Yb2^ix—Li1—Yb1ⁱⁱ	119.6 (8)
Ge2—In—Yb1^viii	58.45 (3)	Yb2^v—Li1—Yb1ⁱⁱ	117.3 (6)
Li1^xi—In—Yb1^viii	64.0 (4)	Ge1—Li1—Yb1ⁱ	130.3 (6)
Yb1ⁱ—In—Yb1^viii	118.08 (3)	Ge2—Li1—Yb1ⁱ	58.6 (4)
Yb1ⁱⁱ—In—Yb1^viii	67.29 (3)	Ge1ⁱ—Li1—Yb1ⁱ	58.5 (3)
Ge1^viii—In—Yb1^ix	118.63 (5)	Ge1ⁱⁱ—Li1—Yb1ⁱ	119.9 (9)
Ge1^ix—In—Yb1^ix	57.97 (4)	In^x—Li1—Yb1ⁱ	65.5 (5)
Ge2^x—In—Yb1^ix	127.86 (3)	Li1ⁱ—Li1—Yb1ⁱ	95.2 (4)
Ge2—In—Yb1^ix	58.45 (3)	Li1ⁱⁱ—Li1—Yb1ⁱ	173.3 (13)
Li1^xi—In—Yb1^ix	64.0 (4)	Yb2^viii—Li1—Yb1ⁱ	119.6 (8)
Yb1ⁱ—In—Yb1^ix	67.29 (3)	Yb2^ix—Li1—Yb1ⁱ	67.4 (3)
Yb1ⁱⁱ—In—Yb1^ix	118.08 (3)	Yb2^v—Li1—Yb1ⁱ	117.3 (6)
Yb1^viii—In—Yb1^ix	79.49 (4)	Yb1ⁱⁱ—Li1—Yb1ⁱ	80.7 (6)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z+1; (iii) −x+1/2, −y+1, z−1/2; (iv) −x+1/2, −y, z−1/2; (v) x−1/2, y, −z+1/2; (vi) x+1/2, y, −z+1/2; (vii) x, y, z−1; (viii) −x+1/2, −y+1, z+1/2; (ix) −x+1/2, −y, z+1/2; (x) x−1/2, y, −z+3/2; (xi) x+1/2, y, −z+3/2; (xii) x, y, z+1.

Experimental details

Crystal data
Chemical formula	Yb₂LiInGe₂
M_r	613.02
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	200
a, b, c (Å)	7.182 (3), 4.3899 (18), 16.758 (7)
V (Å³)	528.3 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	50.42
Crystal size (mm)	0.04 × 0.02 × 0.02

Data collection
Diffractometer	Bruker SMART APEX
Absorption correction	Multi-scan (SADABS; Bruker, 2002)
T_min, T_max	0.258, 0.365
No. of measured, independent and observed [I > 2σ(I)] reflections	6805, 735, 623
R_int	0.090
(sin θ/λ)_max (Å⁻¹)	0.666

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.059, 1.11
No. of reflections	735
No. of parameters	35
Δρ_max, Δρ_min (e Å⁻³)	2.10, −2.86

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SHELXTL (Sheldrick, 2008), DIAMOND (Brandenburg, 1999).

Selected bond lengths (Å) top

In—Ge1ⁱ	2.7803 (13)	In—Ge2ⁱⁱⁱ	2.809 (2)
In—Ge1ⁱⁱ	2.7803 (13)	In—Ge2	2.8203 (19)

Symmetry codes: (i) −x+1/2, −y+1, z+1/2; (ii) −x+1/2, −y, z+1/2; (iii) x−1/2, y, −z+3/2.

Acknowledgements

The authors acknowledge financial support from the University of Delaware Research Foundation – Strategic Initiative Grants (UDRF).

References

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