Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101001822/na1502sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101001822/na1502Isup2.hkl |
CCDC references: 142803; 163905
Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON98 (Spek, 1990); software used to prepare material for publication: SHELXL97.
[Hg(C4H8N2S)I2] | Z = 4 |
Mr = 570.57 | F(000) = 992 |
Orthorhombic, Pnma | Dx = 3.492 Mg m−3 |
Hall symbol: -P 2ac 2n | Mo Kα radiation, λ = 0.71073 Å |
a = 12.826 (2) Å | µ = 20.01 mm−1 |
b = 7.392 (1) Å | T = 200 K |
c = 11.447 (2) Å | Prism, yellow |
V = 1085.3 (4) Å3 | 0.2 × 0.1 × 0.1 mm |
Nonius Kappa CCD diffractometer | 1428 independent reflections |
Radiation source: fine-focus sealed tube | 1286 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
ω scans | θmax = 28.3°, θmin = 3.2° |
Absorption correction: semiempirical (using intensity measurements) (XEMP; Sheldrick, 1988) | h = −15→17 |
Tmin = 0.059, Tmax = 0.135 | k = −9→8 |
10676 measured reflections | l = −15→13 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.025 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0169P)2 + 1.6028P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max < 0.001 |
1428 reflections | Δρmax = 0.66 e Å−3 |
59 parameters | Δρmin = −0.84 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00466 (19) |
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. Diffraction data were collected on a Nonius Kappa CCD diffractometer (capillary optics) at 200 K. 188 frames were collected at the crystal-detector distance of 35 mm, 20 s/°, 1 set of φ scans, 4 sets of ω scans, 2° per frame. Program DENZO-SMN was used for data reduction (Otwinowski and Minor, 1997). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Hg | 0.09785 (2) | 0.2235 (4) | 0.06137 (3) | 0.0556 (5) | 0.50 |
I1 | 0.13565 (4) | 0.2500 | 0.29164 (4) | 0.04968 (15) | |
I2 | −0.09545 (3) | 0.2500 | −0.03145 (4) | 0.04647 (14) | |
S | 0.25088 (12) | 0.2500 | −0.06643 (14) | 0.0439 (3) | |
C1 | 0.1848 (4) | 0.2500 | −0.1991 (5) | 0.0348 (11) | |
N | 0.1606 (3) | 0.0979 (5) | −0.2489 (3) | 0.0542 (10) | |
H | 0.1769 | −0.0010 | −0.2137 | 0.065* | |
C2 | 0.1068 (4) | 0.0850 (9) | −0.3627 (5) | 0.0671 (15) | |
H2A | 0.0634 | −0.0223 | −0.3649 | 0.080* | |
H2B | 0.1575 | 0.0769 | −0.4254 | 0.080* | |
C3 | 0.0415 (5) | 0.2500 | −0.3776 (6) | 0.070 (2) | |
H3A | 0.0102 | 0.2500 | −0.4547 | 0.084* | |
H3B | −0.0142 | 0.2500 | −0.3202 | 0.084* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg | 0.04130 (18) | 0.0915 (15) | 0.03403 (17) | −0.0034 (3) | −0.00217 (10) | −0.0013 (2) |
I1 | 0.0572 (3) | 0.0607 (3) | 0.0311 (2) | 0.000 | 0.00020 (17) | 0.000 |
I2 | 0.0346 (2) | 0.0473 (2) | 0.0575 (3) | 0.000 | −0.00502 (16) | 0.000 |
S | 0.0327 (7) | 0.0602 (9) | 0.0387 (7) | 0.000 | −0.0036 (6) | 0.000 |
C1 | 0.028 (2) | 0.039 (3) | 0.037 (3) | 0.000 | 0.006 (2) | 0.000 |
N | 0.073 (3) | 0.0420 (19) | 0.048 (2) | −0.0043 (19) | −0.011 (2) | −0.0030 (17) |
C2 | 0.075 (4) | 0.077 (4) | 0.049 (3) | −0.026 (3) | −0.006 (3) | −0.011 (3) |
C3 | 0.033 (3) | 0.140 (8) | 0.036 (3) | 0.000 | 0.000 (3) | 0.000 |
Hg—Hgi | 0.391 (5) | S—Hgi | 2.456 (2) |
Hg—S | 2.456 (2) | C1—N | 1.298 (5) |
Hg—I1 | 2.6872 (7) | C1—Ni | 1.298 (5) |
Hg—I2 | 2.7044 (6) | N—C2 | 1.477 (7) |
I1—Hgi | 2.6872 (7) | C2—C3 | 1.490 (7) |
I2—Hgi | 2.7044 (6) | C3—C2i | 1.490 (7) |
S—C1 | 1.740 (6) | ||
Hgi—Hg—S | 85.43 (6) | C1—S—Hg | 97.5 (2) |
Hgi—Hg—I1 | 85.82 (6) | Hgi—S—Hg | 9.14 (12) |
S—Hg—I1 | 115.74 (4) | N—C1—Ni | 120.1 (6) |
Hgi—Hg—I2 | 85.85 (6) | N—C1—S | 120.0 (3) |
S—Hg—I2 | 119.53 (4) | Ni—C1—S | 120.0 (3) |
I1—Hg—I2 | 123.06 (2) | C1—N—C2 | 123.6 (4) |
Hg—I1—Hgi | 8.35 (11) | N—C2—C3 | 108.1 (5) |
Hg—I2—Hgi | 8.30 (11) | C2i—C3—C2 | 109.9 (6) |
C1—S—Hgi | 97.50 (18) |
Symmetry code: (i) x, −y+1/2, z. |