Bis(tetra­methyl­guanidinium) hexa­chlorido­tellurate(IV)

The title compound, 2C₅H₁₄N₃⁺·TeCl₆²⁻, is an easily accessible salt with a relatively low melting point. The asymmetric unit consists of a Te_0.25Cl_1.5 fragment and half a cation. Weak hydrogen bonds of the type C—H...Cl and N—H...Cl are present in the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 123 K
• Mean [sigma](N-C) = 0.001 Å
• R factor = 0.013
• wR factor = 0.034
• Data-to-parameter ratio = 34.8

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
PLAT230_ALERT_2_B Hirshfeld Test Diff for    Te1      --Cl1      .       20.3 s.u.
PLAT230_ALERT_2_B Hirshfeld Test Diff for    Te1      --Cl2      .       36.3 s.u.

Alert level C
ABSMU01_ALERT_1_C  The ratio of given/expected absorption coefficient lies
               outside the range 0.99 <> 1.01
            Calculated value of mu =     1.941
            Value of mu given      =     1.916
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2B      ..CL2      .       2.84 Ang.

Alert level G
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       6.21 Why ?
PLAT794_ALERT_5_G Tentative Bond Valency for Te1       (IV)      .       3.81 Info
PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          1 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          4 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note
PLAT954_ALERT_1_G Reported (CIF) and Actual (FCF) Kmax Differ by .          1 Units
PLAT982_ALERT_1_G The Cl-f'=       0.151 Deviates from  IT-value =      0.148  Check
PLAT982_ALERT_1_G The Te-f'=      -0.498 Deviates from  IT-value =     -0.531  Check
PLAT983_ALERT_1_G The Te-f"=       1.702 Deviates from  IT-Value =      1.675  Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  11 ALERT level G = General information/check it is not something unexpected

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX3 (Bruker, 2017); cell refinement: SAINT (Bruker, 2017); data reduction: SAINT (Bruker, 2017); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg & Putz, 2014); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis(tetramethylguanidinium) hexachloridotellurate(IV)

Crystal data

2C5H14N3^+·Cl6Te^2^−	Dx = 1.609 Mg m^−3
Mr = 572.68	Melting point: 407 K
Orthorhombic, Fddd	Mo Kα radiation, λ = 0.71073 Å
a = 7.3899 (5) Å	Cell parameters from 9942 reflections
b = 22.447 (2) Å	θ = 2.3–32.5°
c = 28.512 (2) Å	µ = 1.92 mm^−1
V = 4729.6 (6) Å^3	T = 123 K
Z = 8	Stick, yellow
F(000) = 2272	0.45 × 0.35 × 0.12 mm

Data collection

Bruker APEXII CCD diffractometer	2057 reflections with I > 2σ(I)
Radiation source: microfocus sealed tube	Rint = 0.027
φ and ω scans	θmax = 32.6°, θmin = 2.9°
Absorption correction: multi-scan (SADABS; Bruker, 2017)	h = −11→11
	k = −34→33
47585 measured reflections	l = −42→42
2158 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.013	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.034	w = 1/[σ^2(Fo^2) + (0.0103P)^2 + 6.2116P] where P = (Fo^2 + 2Fc^2)/3
S = 1.26	(Δ/σ)max = 0.001
2158 reflections	Δρmax = 0.39 e Å^−3
62 parameters	Δρmin = −0.37 e Å^−3
0 restraints	Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.000156 (17)

Special details

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. All non-hydrogen atoms were refined anisotropically. The methyl H atoms were positioned with idealized geometry and refined isotropically with U_iso(H) = 1.5 U_eq(C) using a riding model. The positions of the hydrogen atoms of the NH₂ group of the guanidinium cation were taken from the electron density map and refined isotropically.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Te1	0.8750	0.3750	0.3750	0.01545 (4)
Cl1	0.8750	0.3750	0.46396 (2)	0.02182 (6)
Cl2	0.63226 (3)	0.45506 (2)	0.37388 (2)	0.02254 (5)
N1	0.3750	0.3750	0.45159 (4)	0.0222 (2)
H1	0.447 (2)	0.3533 (6)	0.4372 (5)	0.030 (4)*
C1	0.3750	0.3750	0.49798 (5)	0.0184 (2)
N2	0.3004 (1)	0.42051 (4)	0.52161 (3)	0.0241 (2)
C2	0.1980 (2)	0.41017 (6)	0.56481 (4)	0.0381 (3)
H2A	0.0721	0.4226	0.5602	0.057*
H2B	0.2517	0.4333	0.5904	0.057*
H2C	0.2017	0.3677	0.5727	0.057*
C3	0.2619 (2)	0.47675 (5)	0.49795 (4)	0.0307 (2)
H3A	0.3543	0.4842	0.4740	0.046*
H3B	0.2629	0.5092	0.5209	0.046*
H3C	0.1426	0.4746	0.4831	0.046*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Te1	0.01545 (5)	0.01243 (5)	0.01847 (6)	0	0.00	0.00
Cl1	0.0257 (1)	0.0190 (1)	0.0207 (1)	0.0020 (1)	0.00	0.00
Cl2	0.0214 (1)	0.01873 (9)	0.0274 (1)	0.00211 (7)	−0.00547 (8)	−0.00431 (7)
N1	0.0221 (5)	0.0269 (5)	0.0178 (5)	0.0099 (4)	0.00	0.00
C1	0.0161 (5)	0.0192 (5)	0.0200 (5)	−0.0008 (4)	0.00	0.00
N2	0.0272 (4)	0.0224 (4)	0.0226 (4)	0.0008 (3)	0.0022 (3)	−0.0052 (3)
C2	0.0439 (7)	0.0409 (6)	0.0296 (5)	−0.0080 (5)	0.0141 (5)	−0.0145 (5)
C3	0.0316 (5)	0.0213 (4)	0.0391 (6)	0.0060 (4)	−0.0049 (4)	−0.0062 (4)

Geometric parameters (Å, º)

Te1—Cl1	2.5363 (4)	C1—N2	1.342 (1)
Te1—Cl1^i	2.5364 (4)	N2—C3	1.459 (1)
Te1—Cl2^ii	2.5394 (3)	N2—C2	1.464 (2)
Te1—Cl2	2.5394 (3)	C2—H2A	0.9800
Te1—Cl2^i	2.5394 (3)	C2—H2B	0.9800
Te1—Cl2^iii	2.5394 (3)	C2—H2C	0.9800
N1—C1	1.323 (2)	C3—H3A	0.9800
N1—H1	0.83 (2)	C3—H3B	0.9800
C1—N2^iv	1.342 (1)	C3—H3C	0.9800
Cl1—Te1—Cl1^i	180.0	N1—C1—N2	120.14 (6)
Cl1—Te1—Cl2^ii	89.282 (5)	N2^iv—C1—N2	119.7 (1)
Cl1^i—Te1—Cl2^ii	90.718 (5)	C1—N2—C3	120.43 (9)
Cl1—Te1—Cl2	90.718 (5)	C1—N2—C2	120.93 (9)
Cl1^i—Te1—Cl2	89.282 (5)	C3—N2—C2	115.15 (9)
Cl2^ii—Te1—Cl2	90.12 (1)	N2—C2—H2A	109.5
Cl1—Te1—Cl2^i	89.283 (5)	N2—C2—H2B	109.5
Cl1^i—Te1—Cl2^i	90.717 (5)	H2A—C2—H2B	109.5
Cl2^ii—Te1—Cl2^i	178.57 (1)	N2—C2—H2C	109.5
Cl2—Te1—Cl2^i	89.90 (1)	H2A—C2—H2C	109.5
Cl1—Te1—Cl2^iii	90.717 (5)	H2B—C2—H2C	109.5
Cl1^i—Te1—Cl2^iii	89.283 (5)	N2—C3—H3A	109.5
Cl2^ii—Te1—Cl2^iii	89.90 (1)	N2—C3—H3B	109.5
Cl2—Te1—Cl2^iii	178.57 (1)	H3A—C3—H3B	109.5
Cl2^i—Te1—Cl2^iii	90.12 (1)	N2—C3—H3C	109.5
C1—N1—H1	120 (1)	H3A—C3—H3C	109.5
N1—C1—N2^iv	120.14 (6)	H3B—C3—H3C	109.5

Symmetry codes: (i) −x+7/4, y, −z+3/4; (ii) x, −y+3/4, −z+3/4; (iii) −x+7/4, −y+3/4, z; (iv) −x+3/4, −y+3/4, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Cl2^ii	0.83 (2)	2.57 (2)	3.3875 (8)	167 (1)
C2—H2B···Cl2^v	0.98	2.84	3.712 (1)	149
C3—H3B···Cl1^v	0.98	2.82	3.644 (1)	142

Symmetry codes: (ii) x, −y+3/4, −z+3/4; (v) −x+1, −y+1, −z+1.