Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805001960/wm6049sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805001960/wm6049Isup2.hkl |
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).
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 |
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 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 |
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. |
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) |
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) |
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. |