Te
4[Ga
2Cl
7]
2 has been isolated from GaCl
3-benzene media and its structure determined. The structure features a centrosymmetric square-planar Te
cation and staggered [Ga
2Cl
7]
- anions, consisting of two corner-sharing GaCl
4 tetrahedra. The chlorine bridge between the Ga atoms in the anion is bent. The title compound is isotypic with Te
4[Al
2Cl
7]
2.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (e-Te) = 0.001 Å
- R factor = 0.032
- wR factor = 0.060
- Data-to-parameter ratio = 30.1
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact Te1 .. Cl2 .. 3.28 Ang.
| Author Response: This is not a particularly short Te-X contact considering
other structures containing tellurium polycations.
|
Alert level B
PLAT432_ALERT_2_B Short Inter X...Y Contact Te1 .. Cl5 .. 3.38 Ang.
| Author Response: This is not a particularly short Te-X contact considering
other structures containing tellurium polycations.
|
PLAT432_ALERT_2_B Short Inter X...Y Contact Te2 .. Cl2 .. 3.37 Ang.
| Author Response: This is not a particularly short Te-X contact considering
other structures containing tellurium polycations.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ga1
PLAT431_ALERT_2_C Short Inter HL..A Contact Cl5 .. Cl6 .. 3.44 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact Te2 .. Cl5 .. 3.51 Ang.
| Author Response: This is not a particularly short Te-X contact considering
other structures containing tellurium polycations.
|
1 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX/LSQ (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: program (reference?); software used to prepare material for publication: maXus (Mackay et al., 1999).
Tetratellurium bis[heptachlorodigallate(III)]
top
Crystal data top
Te4[Ga2Cl7]2 | F(000) = 1140 |
Mr = 1285.62 | Dx = 3.236 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 116 reflections |
a = 9.1244 (6) Å | θ = 4.3–20.7° |
b = 11.0468 (7) Å | µ = 9.78 mm−1 |
c = 13.0895 (7) Å | T = 296 K |
β = 90.152 (6)° | Block, black |
V = 1319.36 (14) Å3 | 0.25 × 0.25 × 0.20 mm |
Z = 2 | |
Data collection top
Nonius KappaCCD diffractometer | 2350 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.063 |
φ and ω scans | θmax = 27.5°, θmin = 4.6° |
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1997) | h = −11→10 |
Tmin = 0.111, Tmax = 0.159 | k = −14→14 |
16007 measured reflections | l = −16→16 |
3013 independent reflections | |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.032 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.0088P)2 + 3.3218P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max < 0.001 |
3013 reflections | Δρmax = 0.58 e Å−3 |
100 parameters | Δρmin = −0.94 e Å−3 |
Special details top
Experimental. A Raman spectrum of a single-crystal of (I), mounted in a melting point tube,
was recorded using a Renishaw System 1000 spectrometer equipped with a DMLM
Leica microscope and a 25 mW He—Ne laser (633 nm). |
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 | |
Te1 | 0.43687 (4) | 0.15697 (3) | −0.03397 (3) | 0.04632 (11) | |
Te2 | 0.68081 (4) | 0.06271 (3) | 0.04444 (3) | 0.05018 (12) | |
Ga1 | 0.73864 (6) | 0.42252 (5) | 0.15738 (4) | 0.03512 (13) | |
Ga2 | 1.12169 (6) | 0.31958 (5) | 0.20582 (4) | 0.03478 (13) | |
Cl1 | 0.63024 (16) | 0.58362 (13) | 0.20414 (15) | 0.0591 (4) | |
Cl2 | 0.68781 (19) | 0.36435 (13) | 0.00468 (12) | 0.0552 (4) | |
Cl3 | 0.72295 (17) | 0.27672 (14) | 0.26318 (12) | 0.0520 (3) | |
Cl4 | 0.97980 (14) | 0.47526 (12) | 0.14389 (11) | 0.0431 (3) | |
Cl5 | 1.09409 (16) | 0.32674 (14) | 0.36881 (10) | 0.0490 (3) | |
Cl6 | 1.04769 (16) | 0.16123 (12) | 0.12915 (11) | 0.0468 (3) | |
Cl7 | 1.33555 (16) | 0.37785 (14) | 0.16368 (15) | 0.0595 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Te1 | 0.0446 (2) | 0.03280 (17) | 0.0615 (3) | 0.00155 (15) | −0.01299 (17) | 0.00281 (17) |
Te2 | 0.03774 (19) | 0.04240 (19) | 0.0703 (3) | −0.00667 (16) | −0.01938 (18) | −0.00038 (19) |
Ga1 | 0.0356 (3) | 0.0323 (3) | 0.0375 (3) | −0.0010 (2) | −0.0041 (2) | −0.0008 (2) |
Ga2 | 0.0308 (3) | 0.0412 (3) | 0.0322 (3) | −0.0034 (2) | −0.0027 (2) | −0.0017 (2) |
Cl1 | 0.0408 (7) | 0.0438 (7) | 0.0926 (13) | 0.0053 (6) | −0.0042 (8) | −0.0152 (8) |
Cl2 | 0.0759 (10) | 0.0504 (8) | 0.0393 (8) | −0.0219 (7) | −0.0131 (7) | 0.0018 (7) |
Cl3 | 0.0534 (8) | 0.0561 (8) | 0.0465 (8) | 0.0013 (6) | 0.0085 (6) | 0.0152 (7) |
Cl4 | 0.0357 (7) | 0.0417 (6) | 0.0520 (8) | −0.0008 (5) | −0.0022 (5) | 0.0080 (6) |
Cl5 | 0.0507 (8) | 0.0662 (9) | 0.0302 (7) | −0.0034 (7) | −0.0073 (6) | −0.0033 (7) |
Cl6 | 0.0516 (8) | 0.0458 (7) | 0.0429 (8) | −0.0043 (6) | −0.0046 (6) | −0.0090 (6) |
Cl7 | 0.0338 (7) | 0.0607 (9) | 0.0841 (13) | −0.0068 (6) | 0.0058 (7) | 0.0122 (9) |
Geometric parameters (Å, º) top
Te1—Te2i | 2.6571 (5) | Ga1—Cl4 | 2.2835 (14) |
Te1—Te2 | 2.6608 (5) | Ga2—Cl4 | 2.2990 (14) |
Te2—Te1i | 2.6571 (5) | Ga2—Cl5 | 2.1504 (15) |
Ga1—Cl1 | 2.1269 (15) | Ga2—Cl6 | 2.1260 (14) |
Ga1—Cl2 | 2.1490 (16) | Ga2—Cl7 | 2.1289 (15) |
Ga1—Cl3 | 2.1293 (16) | | |
| | | |
Te2i—Te1—Te2 | 89.999 (15) | Cl6—Ga2—Cl7 | 114.62 (7) |
Te1i—Te2—Te1 | 90.003 (15) | Cl6—Ga2—Cl5 | 117.44 (6) |
Cl1—Ga1—Cl2 | 114.74 (7) | Cl7—Ga2—Cl4 | 101.43 (6) |
Cl1—Ga1—Cl3 | 114.43 (7) | Cl7—Ga2—Cl5 | 110.84 (7) |
Cl1—Ga1—Cl4 | 104.93 (6) | Cl6—Ga2—Cl4 | 105.74 (6) |
Cl3—Ga1—Cl4 | 108.05 (6) | Cl5—Ga2—Cl4 | 104.78 (6) |
Cl2—Ga1—Cl4 | 102.12 (7) | Ga1—Cl4—Ga2 | 108.89 (6) |
Symmetry code: (i) −x+1, −y, −z. |