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The structure of the title compound, [GeCl4(C6H7N)2], (I), is the first example of an addition compound of GeCl4 with two aromatic nitro­gen bases. The mol­ecule, with essential D2h symmetry, has crystallographic C2h symmetry. The environment around the Ge atom can be described as a slightly distorted octahedron with the 4-methyl­pyridine ligands occupying axial positions and the four chloro ligands in the equatorial plane. The structure of (I) is isomorphous with the corresponding silicon halides.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100013482/qa0414sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100013482/qa0414Isup2.hkl
Contains datablock I

CCDC reference: 153931

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.

; top
Crystal data top
[GeCl4(C6H7N)2]Dx = 1.707 Mg m3
Mr = 400.64Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmnaCell parameters from 2407 reflections
a = 7.154 (2) Åθ = 1–25°
b = 7.933 (2) ŵ = 2.64 mm1
c = 13.731 (3) ÅT = 173 K
V = 779.3 (3) Å3Block, colourless
Z = 20.60 × 0.20 × 0.20 mm
F(000) = 400
Data collection top
Siemens CCD three-circle
diffractometer
1036 independent reflections
Radiation source: fine-focus sealed tube895 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω scansθmax = 28.3°, θmin = 2.6°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 95
Tmin = 0.301, Tmax = 0.621k = 108
3722 measured reflectionsl = 1716
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.062 w = 1/[σ2(Fo2) + (0.0334P)2 + 0.1042P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max < 0.001
1036 reflectionsΔρmax = 0.41 e Å3
57 parametersΔρmin = 0.51 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0063 (14)
Special details top

Experimental. ;

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
xyzUiso*/UeqOcc. (<1)
Cl10.72510 (7)0.16635 (6)0.43468 (3)0.02974 (16)
Ge10.50000.00000.50000.01699 (14)
N10.50000.1450 (3)0.62414 (15)0.0186 (4)
C20.50000.3149 (3)0.6175 (2)0.0230 (6)
H20.50000.36590.55490.028*
C30.50000.4162 (3)0.6989 (2)0.0240 (6)
H30.50000.53540.69190.029*
C40.50000.3445 (3)0.79128 (19)0.0205 (5)
C410.50000.4504 (4)0.8814 (2)0.0285 (6)
H41A0.50000.56230.86280.043*0.50
H41B0.39750.41800.92150.043*0.50
H41C0.50000.38360.93990.043*0.50
H41D0.39290.51790.87890.043*0.50
C50.50000.1696 (3)0.79704 (19)0.0230 (5)
H50.50000.11560.85880.028*
C60.50000.0748 (3)0.71332 (19)0.0220 (5)
H60.50000.04460.71860.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0322 (3)0.0279 (3)0.0291 (3)0.01187 (19)0.0090 (2)0.00667 (19)
Ge10.0192 (2)0.01502 (19)0.0167 (2)0.0000.0000.00263 (14)
N10.0210 (11)0.0165 (9)0.0183 (11)0.0000.0000.0028 (8)
C20.0272 (14)0.0195 (12)0.0224 (14)0.0000.0000.0010 (10)
C30.0272 (14)0.0158 (12)0.0288 (14)0.0000.0000.0032 (10)
C40.0155 (12)0.0234 (12)0.0226 (13)0.0000.0000.0064 (11)
C410.0313 (15)0.0290 (13)0.0251 (15)0.0000.0000.0112 (11)
C50.0252 (14)0.0258 (13)0.0181 (13)0.0000.0000.0006 (11)
C60.0261 (13)0.0178 (12)0.0221 (13)0.0000.0000.0018 (10)
Geometric parameters (Å, º) top
Cl1—Ge12.2670 (6)C3—H30.9500
Ge1—N12.057 (2)C4—C51.390 (4)
Ge1—N1i2.057 (2)C4—C411.495 (4)
Ge1—Cl1ii2.2670 (6)C41—H41A0.9240
Ge1—Cl1i2.2670 (6)C41—H41B0.9530
Ge1—Cl1iii2.2670 (6)C41—H41C0.9620
N1—C61.345 (3)C41—H41D0.9355
N1—C21.350 (3)C5—C61.373 (4)
C2—C31.377 (4)C5—H50.9500
C2—H20.9500C6—H60.9500
C3—C41.390 (4)
N1—Ge1—N1i180.0C2—C3—H3119.9
N1—Ge1—Cl190.13 (4)C4—C3—H3119.9
N1i—Ge1—Cl189.87 (4)C3—C4—C5117.4 (2)
N1—Ge1—Cl1ii90.13 (4)C3—C4—C41121.7 (2)
N1i—Ge1—Cl1ii89.87 (4)C5—C4—C41120.9 (2)
Cl1—Ge1—Cl1ii90.53 (3)C4—C41—H41A108.2
N1—Ge1—Cl1i89.87 (4)C4—C41—H41B109.1
N1i—Ge1—Cl1i90.13 (4)H41A—C41—H41B114.8
Cl1—Ge1—Cl1i180.0C4—C41—H41C112.4
Cl1ii—Ge1—Cl1i89.47 (3)H41A—C41—H41C139.4
N1—Ge1—Cl1iii89.87 (4)H41B—C41—H41C50.8
N1i—Ge1—Cl1iii90.13 (4)C4—C41—H41D107.0
Cl1—Ge1—Cl1iii89.47 (3)H41A—C41—H41D55.9
Cl1ii—Ge1—Cl1iii180.0H41B—C41—H41D62.9
Cl1i—Ge1—Cl1iii90.53 (3)H41C—C41—H41D110.2
C6—N1—C2118.3 (2)C6—C5—C4119.9 (2)
C6—N1—Ge1121.53 (17)C6—C5—H5120.0
C2—N1—Ge1120.14 (17)C4—C5—H5120.0
N1—C2—C3121.9 (2)N1—C6—C5122.4 (2)
N1—C2—H2119.1N1—C6—H6118.8
C3—C2—H2119.1C5—C6—H6118.8
C2—C3—C4120.1 (2)
N1i—Ge1—N1—C60.0 (3)C6—N1—C2—C30.0
Cl1—Ge1—N1—C6134.736 (16)Ge1—N1—C2—C3180.0
Cl1ii—Ge1—N1—C6134.736 (16)N1—C2—C3—C40.0
Cl1i—Ge1—N1—C645.264 (17)C2—C3—C4—C50.0
Cl1iii—Ge1—N1—C645.264 (16)C2—C3—C4—C41180.0
N1i—Ge1—N1—C2180.0 (3)C3—C4—C5—C60.0
Cl1—Ge1—N1—C245.264 (17)C41—C4—C5—C6180.0
Cl1ii—Ge1—N1—C245.264 (16)C2—N1—C6—C50.0
Cl1i—Ge1—N1—C2134.736 (17)Ge1—N1—C6—C5180.0
Cl1iii—Ge1—N1—C2134.736 (17)C4—C5—C6—N10.0
Symmetry codes: (i) x+1, y, z+1; (ii) x+1, y, z; (iii) x, y, z+1.
 

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