Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810201618X/bk0119sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810201618X/bk0119sup2.hkl |
For both compounds, data collection: Kuma CrysAlis; cell refinement: Kuma CrysAlis; data reduction: Kuma CrysAlis; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: STACK (Birkedal et al., 1998); molecular graphics: Cerius2; software used to prepare material for publication: Cerius2, Bruker SHELXTL.
HgI2 | Melting point: 529 K |
Mr = 454.39 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/amd | Cell parameters from 618 reflections |
a = 8.7863 (5) Å | θ = 14.3–24.1° |
c = 24.667 (3) Å | µ = 45.09 mm−1 |
V = 1904.3 (4) Å3 | T = 200 K |
Z = 16 | Truncated pyramid, orange |
F(000) = 2976 | 0.10 × 0.10 × 0.02 mm |
Dx = 6.340 Mg m−3 |
Kuma CCD diffractometer | 585 independent reflections |
Radiation source: fine-focus sealed tube | 585 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.073 |
Detector resolution: 17.07 pixels mm-1 | θmax = 26.6°, θmin = 3.7° |
ω scans | h = 0→7 |
Absorption correction: analytical based on the shape of the crystal | k = 0→10 |
Tmin = 0.017, Tmax = 0.411 | l = 0→30 |
843 measured reflections |
Refinement on F | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.065 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.131 | w = 1/[σ2(Yo2) + (0.0303P)2 + 4.60896P] where P = (Yo + 2Yc)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
585 reflections | Δρmax = not computed with STACK e Å−3 |
20 parameters | Δρmin = not computed with STACK e Å−3 |
HgI2 | Z = 16 |
Mr = 454.39 | Mo Kα radiation |
Tetragonal, I41/amd | µ = 45.09 mm−1 |
a = 8.7863 (5) Å | T = 200 K |
c = 24.667 (3) Å | 0.10 × 0.10 × 0.02 mm |
V = 1904.3 (4) Å3 |
Kuma CCD diffractometer | 585 independent reflections |
Absorption correction: analytical based on the shape of the crystal | 585 reflections with I > 2σ(I) |
Tmin = 0.017, Tmax = 0.411 | Rint = 0.073 |
843 measured reflections |
R[F2 > 2σ(F2)] = 0.065 | 20 parameters |
wR(F2) = 0.131 | 0 restraints |
S = 1.07 | Δρmax = not computed with STACK e Å−3 |
585 reflections | Δρmin = not computed with STACK e Å−3 |
Refinement. STACK program allows the refinement of several structures against a single data-set. It has been used for the refinement of two structures that are end-members with maximum degree of order (MDO) of a polytypic layer structure. See the text for more details. |
x | y | z | Uiso*/Ueq | ||
Hg | 0.74792 (15) | 0.25 | 0.06232 (1) | 0.0315 (2) | |
I1 | 0.50 | 0.75 | 0.25752 (9) | 0.0249 (6) | |
I2 | 0.76416 (14) | 0.51416 (14) | 0.125 | 0.0331 (3) | |
I3 | 0.50 | 0.25 | 0.25758 (12) | 0.0333 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg | 0.0266 (4) | 0.0360 (4) | 0.0318 (2) | 0.0 | 0.0003 (3) | 0.0 |
I1 | 0.0304 (11) | 0.0261 (10) | 0.0182 (9) | 0.0 | 0.0 | 0.0 |
I2 | 0.0313 (4) | 0.0313 (4) | 0.0364 (6) | −0.0034 (4) | 0.0001 (2) | −0.0001 (2) |
I3 | 0.0335 (12) | 0.0355 (12) | 0.0308 (12) | 0.0 | 0.0 | 0.0 |
HgI2 | Melting point: 529 K |
Mr = 454.39 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P42/nmc | Cell parameters from 618 reflections |
a = 8.7863 (5) Å | θ = 14.3–24.1° |
c = 12.334 (3) Å | µ = 45.09 mm−1 |
V = 952.2 (2) Å3 | T = 200 K |
Z = 8 | Truncated pyramid, orange |
F(000) = 1488 | 0.10 × 0.10 × 0.02 mm |
Dx = 6.340 Mg m−3 |
Kuma CCD diffractometer | 570 independent reflections |
Radiation source: fine-focus sealed tube | 570 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.073 |
Detector resolution: 17.07 pixels mm-1 | θmax = 26.6°, θmin = 3.7° |
ω scans | h = 0→7 |
Absorption correction: analytical based on the shape of the crystal | k = 0→10 |
Tmin = 0.017, Tmax = 0.411 | l = 0→30 |
843 measured reflections |
Refinement on F | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.066 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.133 | w = 1/[σ2(Yo2) + (0.0303P)2 + 4.60896P] where P = (Yo + 2Yc)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
570 reflections | Δρmax = not computed with STACK e Å−3 |
20 parameters | Δρmin = not computed with STACK e Å−3 |
HgI2 | Z = 8 |
Mr = 454.39 | Mo Kα radiation |
Tetragonal, P42/nmc | µ = 45.09 mm−1 |
a = 8.7863 (5) Å | T = 200 K |
c = 12.334 (3) Å | 0.10 × 0.10 × 0.02 mm |
V = 952.2 (2) Å3 |
Kuma CCD diffractometer | 570 independent reflections |
Absorption correction: analytical based on the shape of the crystal | 570 reflections with I > 2σ(I) |
Tmin = 0.017, Tmax = 0.411 | Rint = 0.073 |
843 measured reflections |
R[F2 > 2σ(F2)] = 0.066 | 20 parameters |
wR(F2) = 0.133 | 0 restraints |
S = 1.07 | Δρmax = not computed with STACK e Å−3 |
570 reflections | Δρmin = not computed with STACK e Å−3 |
Refinement. STACK program allows the refinement of several structures against a single data-set. It has been used for the refinement of two structures that are end-members with maximum degree of order (MDO) of a polytypic layer structure. See the text for more details. |
x | y | z | Uiso*/Ueq | ||
Hg | 0.50043 (19) | 0.75 | 0.12481 (13) | 0.0399 (5) | |
I1 | 0.25 | 0.25 | 0.5165 (3) | 0.0343 (10) | |
I2 | 0.51381 (17) | 0.01381 (17) | 0.25 | 0.0292 (4) | |
I3 | 0.25 | 0.75 | 0.5136 (3) | 0.0316 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg | 0.0367 (7) | 0.0446 (7) | 0.0385 (11) | 0.0 | −0.0008 (3) | 0.0 |
I1 | 0.058 (2) | 0.0146 (13) | 0.0301 (14) | 0.0 | 0.0 | 0.0 |
I2 | 0.0302 (7) | 0.0302 (7) | 0.0272 (8) | −0.0029 (5) | 0.0008 (3) | −0.0008 (3) |
I3 | 0.0454 (18) | 0.0282 (16) | 0.0211 (14) | 0.0 | 0.0 | 0.0 |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | HgI2 | HgI2 |
Mr | 454.39 | 454.39 |
Crystal system, space group | Tetragonal, I41/amd | Tetragonal, P42/nmc |
Temperature (K) | 200 | 200 |
a, c (Å) | 8.7863 (5), 24.667 (3) | 8.7863 (5), 12.334 (3) |
V (Å3) | 1904.3 (4) | 952.2 (2) |
Z | 16 | 8 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 45.09 | 45.09 |
Crystal size (mm) | 0.10 × 0.10 × 0.02 | 0.10 × 0.10 × 0.02 |
Data collection | ||
Diffractometer | Kuma CCD diffractometer | Kuma CCD diffractometer |
Absorption correction | Analytical based on the shape of the crystal | Analytical based on the shape of the crystal |
Tmin, Tmax | 0.017, 0.411 | 0.017, 0.411 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 843, 585, 585 | 843, 570, 570 |
Rint | 0.073 | 0.073 |
(sin θ/λ)max (Å−1) | 0.630 | 0.630 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.065, 0.131, 1.07 | 0.066, 0.133, 1.07 |
No. of reflections | 585 | 570 |
No. of parameters | 20 | 20 |
Δρmax, Δρmin (e Å−3) | not computed with STACK, not computed with STACK | not computed with STACK, not computed with STACK |
Computer programs: Kuma CrysAlis, SHELXS97 (Sheldrick, 1990), STACK (Birkedal et al., 1998), Cerius2, Bruker SHELXTL.