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The Te atom in the title complex, trans-[TeCl4(C6H4N2H2CS)2]·2CH4O or C16H20Cl4N4O2S2Te, occupies a special position at a crystallographic inversion centre and has an octahedral coordination formed by four chloro ligands and the S atoms of two benzimidazole–thione molecules. The hydrogen-bond system involving the disordered solvent methanol molecules links the tellurium complexes into the infinite two-dimensional aggregates in the crystal.
Supporting information
CCDC reference: 193766
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.008 Å
- Disorder in solvent or counterion
- R factor = 0.043
- wR factor = 0.113
- Data-to-parameter ratio = 16.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 33.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CORINC (Dräger & Gattow, 1971); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
trans-Bis(1
H-benzimidazole-1-thione-
κS)tetrachlorotellurium methanol disolvate
top
Crystal data top
C16H20Cl4N4O2S2Te | F(000) = 624 |
Mr = 633.88 | Dx = 1.727 Mg m−3 |
Monoclinic, P21/n | Cu Kα radiation, λ = 1.54178 Å |
a = 8.7211 (11) Å | Cell parameters from 25 reflections |
b = 12.4005 (7) Å | θ = 25.0–31.0° |
c = 11.6049 (11) Å | µ = 15.45 mm−1 |
β = 103.785 (5)° | T = 295 K |
V = 1218.9 (2) Å3 | Block, red brown |
Z = 2 | 0.12 × 0.07 × 0.06 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1938 reflections with I > 2σ(I)' |
Radiation source: rotating anode | Rint = 0.000 |
Graphite monochromator | θmax = 73.9°, θmin = 5.3° |
θ/2ω scans | h = −10→10 |
Absorption correction: numerical [according to de Meulenaer & Tompa (1965) in PLATON (Spek, 2001)] | k = −15→0 |
Tmin = 0.245, Tmax = 0.486 | l = −14→0 |
2465 measured reflections | 3 standard reflections every 60 min |
2465 independent reflections | intensity decay: 3% |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.113 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0617P)2] where P = (Fo2 + 2Fc2)/3 |
2465 reflections | (Δ/σ)max < 0.001 |
148 parameters | Δρmax = 0.63 e Å−3 |
0 restraints | Δρmin = −1.34 e Å−3 |
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 | Uiso*/Ueq | Occ. (<1) |
Te1 | 0.5000 | 0.5000 | 0.5000 | 0.04098 (15) | |
Cl1 | 0.50837 (19) | 0.62752 (12) | 0.33455 (12) | 0.0595 (4) | |
Cl2 | 0.3442 (2) | 0.63943 (14) | 0.58740 (14) | 0.0695 (4) | |
S1 | 0.76961 (18) | 0.59220 (12) | 0.62266 (12) | 0.0550 (3) | |
C1 | 0.7705 (6) | 0.5510 (4) | 0.7636 (5) | 0.0439 (11) | |
N2 | 0.7081 (6) | 0.6053 (4) | 0.8410 (4) | 0.0492 (10) | |
H2 | 0.6273 | 0.6622 | 0.8208 | 0.15 (4)* | |
C2A | 0.7325 (7) | 0.5453 (4) | 0.9464 (5) | 0.0452 (11) | |
C3 | 0.6906 (8) | 0.5646 (5) | 1.0522 (5) | 0.0595 (15) | |
H3 | 0.6356 | 0.6264 | 1.0638 | 0.07 (2)* | |
C4 | 0.7345 (9) | 0.4878 (5) | 1.1392 (5) | 0.0639 (17) | |
H4 | 0.7073 | 0.4977 | 1.2112 | 0.09 (3)* | |
C5 | 0.8185 (8) | 0.3956 (5) | 1.1232 (5) | 0.0595 (15) | |
H5 | 0.8473 | 0.3462 | 1.1848 | 0.062 (18)* | |
C6 | 0.8596 (7) | 0.3764 (4) | 1.0170 (5) | 0.0487 (12) | |
H6 | 0.9156 | 0.3152 | 1.0055 | 0.08 (2)* | |
C6A | 0.8135 (6) | 0.4528 (4) | 0.9290 (4) | 0.0421 (10) | |
N7 | 0.8352 (5) | 0.4600 (4) | 0.8158 (4) | 0.0429 (9) | |
H7 | 0.8800 | 0.4145 | 0.7715 | 0.09 (2)* | |
C1L | 0.4478 (8) | 0.8327 (6) | 0.8817 (7) | 0.077 (2) | |
H1LA | 0.4264 | 0.7721 | 0.9271 | 0.116* | 0.35 |
H1LB | 0.3563 | 0.8481 | 0.8194 | 0.116* | 0.35 |
H1LC | 0.4732 | 0.8944 | 0.9326 | 0.116* | 0.35 |
H1LD | 0.4326 | 0.7778 | 0.9363 | 0.116* | 0.65 |
H1LE | 0.3611 | 0.8315 | 0.8129 | 0.116* | 0.65 |
H1LF | 0.4529 | 0.9020 | 0.9193 | 0.116* | 0.65 |
O1L | 0.5165 (16) | 0.7966 (11) | 0.7926 (11) | 0.057 (3) | 0.35 |
H1L | 0.4349 | 0.7702 | 0.7308 | 0.085* | 0.35 |
O2L | 0.5906 (8) | 0.8125 (5) | 0.8477 (6) | 0.0526 (15) | 0.65 |
H2L | 0.6407 | 0.8570 | 0.8930 | 0.079* | 0.65 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Te1 | 0.0484 (2) | 0.0402 (2) | 0.0328 (2) | −0.0007 (2) | 0.00669 (16) | −0.00403 (19) |
Cl1 | 0.0704 (9) | 0.0564 (8) | 0.0495 (7) | −0.0150 (7) | 0.0098 (6) | 0.0014 (6) |
Cl2 | 0.0857 (11) | 0.0676 (9) | 0.0532 (8) | 0.0136 (8) | 0.0127 (8) | −0.0098 (7) |
S1 | 0.0633 (8) | 0.0595 (8) | 0.0404 (6) | −0.0120 (7) | 0.0087 (6) | 0.0067 (6) |
C1 | 0.047 (3) | 0.042 (3) | 0.040 (3) | −0.006 (2) | 0.005 (2) | 0.001 (2) |
N2 | 0.061 (3) | 0.044 (2) | 0.043 (2) | 0.006 (2) | 0.012 (2) | 0.0038 (19) |
C2A | 0.052 (3) | 0.040 (2) | 0.042 (3) | 0.000 (2) | 0.008 (2) | −0.002 (2) |
C3 | 0.073 (4) | 0.058 (4) | 0.051 (3) | 0.006 (3) | 0.022 (3) | −0.004 (3) |
C4 | 0.088 (5) | 0.062 (4) | 0.044 (3) | −0.021 (3) | 0.020 (3) | −0.005 (3) |
C5 | 0.083 (4) | 0.049 (3) | 0.043 (3) | −0.014 (3) | 0.008 (3) | 0.008 (2) |
C6 | 0.056 (3) | 0.038 (3) | 0.046 (3) | −0.005 (2) | 0.000 (2) | 0.003 (2) |
C6A | 0.048 (3) | 0.040 (2) | 0.035 (2) | −0.008 (2) | 0.004 (2) | −0.005 (2) |
N7 | 0.050 (2) | 0.0380 (19) | 0.038 (2) | −0.0002 (19) | 0.0064 (19) | −0.0014 (17) |
C1L | 0.072 (5) | 0.080 (5) | 0.087 (5) | 0.001 (4) | 0.033 (4) | 0.006 (4) |
O1L | 0.057 (8) | 0.055 (7) | 0.052 (7) | −0.009 (6) | −0.001 (6) | −0.002 (6) |
O2L | 0.067 (5) | 0.041 (3) | 0.052 (4) | −0.003 (3) | 0.019 (3) | 0.000 (3) |
Geometric parameters (Å, º) top
Te1—Cl1i | 2.5018 (14) | C2A—C3 | 1.382 (7) |
Te1—Cl1 | 2.5018 (14) | C2A—C6A | 1.387 (8) |
Te1—Cl2i | 2.5536 (16) | C3—C4 | 1.375 (9) |
Te1—Cl2 | 2.5536 (16) | C4—C5 | 1.394 (9) |
Te1—S1i | 2.6957 (15) | C5—C6 | 1.383 (8) |
Te1—S1 | 2.6957 (15) | C6—C6A | 1.380 (7) |
S1—C1 | 1.712 (5) | C6A—N7 | 1.374 (6) |
C1—N2 | 1.338 (7) | C1L—O1L | 1.387 (15) |
C1—N7 | 1.340 (7) | C1L—O2L | 1.416 (9) |
N2—C2A | 1.404 (6) | | |
| | | |
Cl1i—Te1—Cl1 | 180.0 | N2—C1—N7 | 108.4 (4) |
Cl1i—Te1—Cl2i | 89.57 (5) | N2—C1—S1 | 125.6 (4) |
Cl1—Te1—Cl2i | 90.43 (5) | N7—C1—S1 | 126.1 (4) |
Cl1i—Te1—Cl2 | 90.43 (5) | C1—N2—C2A | 108.5 (4) |
Cl1—Te1—Cl2 | 89.57 (5) | C3—C2A—C6A | 121.6 (5) |
Cl2i—Te1—Cl2 | 180.0 | C3—C2A—N2 | 131.6 (5) |
Cl1i—Te1—S1i | 87.47 (4) | C6A—C2A—N2 | 106.8 (4) |
Cl1—Te1—S1i | 92.53 (4) | C4—C3—C2A | 116.4 (6) |
Cl2i—Te1—S1i | 89.01 (5) | C3—C4—C5 | 122.3 (6) |
Cl2—Te1—S1i | 90.99 (5) | C6—C5—C4 | 121.0 (5) |
Cl1i—Te1—S1 | 92.53 (4) | C6A—C6—C5 | 116.7 (5) |
Cl1—Te1—S1 | 87.47 (4) | N7—C6A—C6 | 132.0 (5) |
Cl2i—Te1—S1 | 90.99 (5) | N7—C6A—C2A | 106.0 (5) |
Cl2—Te1—S1 | 89.01 (5) | C6—C6A—C2A | 121.9 (5) |
S1i—Te1—S1 | 180.0 | C1—N7—C6A | 110.4 (4) |
C1—S1—Te1 | 100.52 (18) | | |
| | | |
Cl1i—Te1—S1—C1 | −17.7 (2) | C3—C4—C5—C6 | −1.0 (10) |
Cl1—Te1—S1—C1 | 162.3 (2) | C4—C5—C6—C6A | 0.0 (9) |
Cl2i—Te1—S1—C1 | −107.3 (2) | C5—C6—C6A—N7 | 179.3 (5) |
Cl2—Te1—S1—C1 | 72.7 (2) | C5—C6—C6A—C2A | 1.2 (8) |
Te1—S1—C1—N2 | −91.4 (5) | C3—C2A—C6A—N7 | 180.0 (5) |
Te1—S1—C1—N7 | 89.6 (5) | N2—C2A—C6A—N7 | 0.1 (6) |
N7—C1—N2—C2A | −0.8 (6) | C3—C2A—C6A—C6 | −1.5 (9) |
S1—C1—N2—C2A | 180.0 (4) | N2—C2A—C6A—C6 | 178.6 (5) |
C1—N2—C2A—C3 | −179.4 (6) | N2—C1—N7—C6A | 0.9 (6) |
C1—N2—C2A—C6A | 0.4 (6) | S1—C1—N7—C6A | −179.9 (4) |
C6A—C2A—C3—C4 | 0.5 (9) | C6—C6A—N7—C1 | −178.9 (6) |
N2—C2A—C3—C4 | −179.7 (6) | C2A—C6A—N7—C1 | −0.6 (6) |
C2A—C3—C4—C5 | 0.7 (10) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O1L | 0.99 | 1.91 | 2.879 (14) | 165 |
N2—H2···O2L | 0.99 | 1.93 | 2.774 (8) | 142 |
N7—H7···O1Lii | 0.91 | 1.96 | 2.853 (14) | 167 |
N7—H7···O2Lii | 0.91 | 1.94 | 2.819 (8) | 163 |
O1L—H1L···Cl2 | 0.94 | 2.32 | 3.165 (13) | 149 |
O2L—H2L···Cl2iii | 0.81 | 2.52 | 3.171 (7) | 138 |
Symmetry codes: (ii) −x+3/2, y−1/2, −z+3/2; (iii) x+1/2, −y+3/2, z+1/2. |
Selected structural parameters of (I), (II) (von Deuten et al., 1979b) and
(III) (von Deuten et al., 1979a); atomic distances in Å, bond and torsion
angles in °; for numbering of the atoms see Fig. 1 top | (I) | (II) | (III) |
Te—Cl1 | 2.502 (1) | 2.525 (3) | 2.509 (2) |
Te—Cl2 | 2.554 (2) | 2.559 (7) | 2.502 (2) |
Te—S1 | 2.696 (2) | 2.630 (6) | 2.704 (2) |
S1—C1 | 1.712 (5) | 1.792 (12) | 1.711 (7) |
S1—Te—S1a | 180.0 | 87.3 (3) | 180.0 |
Te—S1—C1 | 100.5 (2) | 102.3 (4) | 103.1 (2) |
Σ (X—C1—Y)a | 360.1 (7) | 360.0 (10) | 359.8 (6) |
N—C—S—Te | 89.6 (5) | 87.7 | -99.2 |
Note: (a) the sum of the bond angles at C1. |
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