Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102016191/bk0120sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768102016191/bk0120sup2.hkl |
Data collection: Stoe IPDS; cell refinement: Stoe IPDS; data reduction: Stoe IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker XP; software used to prepare material for publication: Bruker SHELXTL.
HgI_{2} | Melting point: 529 K |
M_{r} = 454.39 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I4_{1}/acd | Cell parameters from 978 reflections |
a = 12.3930 (18) Å | θ = 13.9–22.4° |
c = 24.889 (5) Å | µ = 44.92 mm^{−}^{1} |
V = 3822.6 (11) Å^{3} | T = 293 K |
Z = 32 | Block, yellow-orange |
F(000) = 5952 | 0.18 × 0.08 × 0.06 mm |
D_{x} = 6.316 Mg m^{−}^{3} |
Stoe IPDS diffractometer | 685 independent reflections |
Radiation source: fine-focus sealed tube | 455 reflections with I > 2σ(I) |
Graphite monochromator | R_{int} = 0.112 |
Detector resolution: 6.67 pixels mm^{-1} | θ_{max} = 23.2°, θ_{min} = 2.8° |
ϕ scans | h = 0→9 |
Absorption correction: analytical based on the shape of the crystal | k = 0→13 |
T_{min} = 0.012, T_{max} = 0.217 | l = 0→27 |
685 measured reflections |
Refinement on F^{2} | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F^{2} > 2σ(F^{2})] = 0.045 | Secondary atom site location: difference Fourier map |
wR(F^{2}) = 0.098 | w = 1/[σ^{2}(F_{o}^{2}) + (0.028P)^{2} + 5.8P] where P = (F_{o}^{2} + 2F_{c}^{2})/3 |
S = 1.78 | (Δ/σ)_{max} < 0.001 |
685 reflections | Δρ_{max} = 1.15 e Å^{−}^{3} |
29 parameters | Δρ_{min} = −1.33 e Å^{−}^{3} |
HgI_{2} | Z = 32 |
M_{r} = 454.39 | Mo Kα radiation |
Tetragonal, I4_{1}/acd | µ = 44.92 mm^{−}^{1} |
a = 12.3930 (18) Å | T = 293 K |
c = 24.889 (5) Å | 0.18 × 0.08 × 0.06 mm |
V = 3822.6 (11) Å^{3} |
Stoe IPDS diffractometer | 685 independent reflections |
Absorption correction: analytical based on the shape of the crystal | 455 reflections with I > 2σ(I) |
T_{min} = 0.012, T_{max} = 0.217 | R_{int} = 0.112 |
685 measured reflections | θ_{max} = 23.2° |
R[F^{2} > 2σ(F^{2})] = 0.045 | 29 parameters |
wR(F^{2}) = 0.098 | 0 restraints |
S = 1.78 | Δρ_{max} = 1.15 e Å^{−}^{3} |
685 reflections | Δρ_{min} = −1.33 e Å^{−}^{3} |
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 F^{2} against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^{2}, conventional R-factors R are based on F, with F set to zero for negative F^{2}. The threshold expression of F^{2} > σ(F^{2}) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^{2} 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 | U_{iso}*/U_{eq} | ||
I2 | 0.49952 (8) | 0.51362 (11) | 0.12489 (16) | 0.0390 (5) | |
I3 | 0.5000 | 0.2500 | −0.00709 (6) | 0.0396 (6) | |
I1 | 0.2500 | 0.51427 (15) | 0.0000 | 0.0378 (6) | |
Hg | 0.37417 (6) | 0.37379 (7) | 0.06244 (3) | 0.0490 (3) |
U^{11} | U^{22} | U^{33} | U^{12} | U^{13} | U^{23} | |
I2 | 0.0428 (10) | 0.0325 (8) | 0.0416 (7) | −0.0011 (5) | −0.0075 (5) | −0.0008 (17) |
I3 | 0.039 (2) | 0.045 (2) | 0.0349 (9) | 0.0032 (7) | 0.000 | 0.000 |
I1 | 0.0416 (16) | 0.0294 (11) | 0.0425 (10) | 0.000 | −0.0131 (6) | 0.000 |
Hg | 0.0492 (6) | 0.0490 (5) | 0.0488 (5) | 0.0031 (4) | −0.0064 (4) | 0.0053 (4) |
I2—Hg^{i} | 2.779 (3) | I1—Hg^{iii} | 2.7953 (14) |
I2—Hg | 2.799 (2) | I1—Hg | 2.7953 (14) |
I3—Hg^{ii} | 2.7893 (13) | Hg—I2^{iv} | 2.779 (3) |
I3—Hg | 2.7893 (13) | ||
Hg^{i}—I2—Hg | 103.82 (5) | I3—Hg—I1 | 107.78 (4) |
Hg^{ii}—I3—Hg | 103.31 (6) | I2^{iv}—Hg—I2 | 111.87 (3) |
Hg^{iii}—I1—Hg | 102.96 (7) | I3—Hg—I2 | 112.01 (5) |
I2^{iv}—Hg—I3 | 112.77 (5) | I1—Hg—I2 | 103.22 (5) |
I2^{iv}—Hg—I1 | 108.60 (5) |
Symmetry codes: (i) y+1/4, −x+3/4, −z+1/4; (ii) −x+1, −y+1/2, z; (iii) −x+1/2, y, −z; (iv) −y+3/4, x−1/4, −z+1/4. |
Experimental details
Crystal data | |
Chemical formula | HgI_{2} |
M_{r} | 454.39 |
Crystal system, space group | Tetragonal, I4_{1}/acd |
Temperature (K) | 293 |
a, c (Å) | 12.3930 (18), 24.889 (5) |
V (Å^{3}) | 3822.6 (11) |
Z | 32 |
Radiation type | Mo Kα |
µ (mm^{−}^{1}) | 44.92 |
Crystal size (mm) | 0.18 × 0.08 × 0.06 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Analytical based on the shape of the crystal |
T_{min}, T_{max} | 0.012, 0.217 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 685, 685, 455 |
R_{int} | 0.112 |
θ_{max} (°) | 23.2 |
(sin θ/λ)_{max} (Å^{−}^{1}) | 0.555 |
Refinement | |
R[F^{2} > 2σ(F^{2})], wR(F^{2}), S | 0.045, 0.098, 1.78 |
No. of reflections | 685 |
No. of parameters | 29 |
Δρ_{max}, Δρ_{min} (e Å^{−}^{3}) | 1.15, −1.33 |
Computer programs: Stoe IPDS, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Bruker XP, Bruker SHELXTL.