Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803007335/bt6259sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803007335/bt6259Isup2.hkl |
CCDC reference: 214560
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.019 Å
- R factor = 0.038
- wR factor = 0.060
- Data-to-parameter ratio = 26.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
GOODF_01 Alert C The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 0.746 RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.107 PLAT_360 Alert C Short C(sp3)-C(sp3) Bond C(11) - C(15) = 1.42 Ang.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check
1 mmol (0.369 g) of tetrabutylammonium iodide, (Bu4)NI, and 2 mmol (0.454 g) of mercuric iodide HgI2, were dissolved by stirring in 50 ml me thanol at 323 K until a clear solution was obtained. Yellow single crystals were obtained when the solution was allowed to sit at room temperature for 2 d.
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-STEP32 (Stoe & Cie, 2000); data reduction: X-RED (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, Bonn, 1999); software used to prepare material for publication: SHELXL97.
(C16H36N)2[Hg4I10] | Z = 2 |
Mr = 2556.28 | F(000) = 2256 |
Triclinic, P1 | Dx = 2.873 Mg m−3 |
Hall symbol: -P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.681 Å | Cell parameters from 37776 reflections |
b = 15.770 Å | θ = 3.6–59.3° |
c = 18.288 Å | µ = 15.60 mm−1 |
α = 114.33° | T = 293 K |
β = 104.18° | Prismatic needles, yellow |
γ = 90.18° | 0.3 × 0.15 × 0.1 mm |
V = 2955.3 Å3 |
Stoe Imaging Plate Diffraction System, IPDS-I diffractometer | 11615 independent reflections |
Radiation source: fine-focus sealed tube | 5987 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.107 |
ϕ scans | θmax = 26.0°, θmin = 1.8° |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1998) | h = −12→14 |
Tmin = 0.075, Tmax = 0.210 | k = −19→19 |
37776 measured reflections | l = −22→22 |
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)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.060 | w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3 |
S = 0.75 | (Δ/σ)max = 0.001 |
11615 reflections | Δρmax = 1.23 e Å−3 |
434 parameters | Δρmin = −1.22 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.001058 (11) |
(C16H36N)2[Hg4I10] | γ = 90.18° |
Mr = 2556.28 | V = 2955.3 Å3 |
Triclinic, P1 | Z = 2 |
a = 11.681 Å | Mo Kα radiation |
b = 15.770 Å | µ = 15.60 mm−1 |
c = 18.288 Å | T = 293 K |
α = 114.33° | 0.3 × 0.15 × 0.1 mm |
β = 104.18° |
Stoe Imaging Plate Diffraction System, IPDS-I diffractometer | 11615 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1998) | 5987 reflections with I > 2σ(I) |
Tmin = 0.075, Tmax = 0.210 | Rint = 0.107 |
37776 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 0.75 | Δρmax = 1.23 e Å−3 |
11615 reflections | Δρmin = −1.22 e Å−3 |
434 parameters |
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 | ||
Hg1 | 0.38130 (5) | 0.22200 (4) | 0.90692 (3) | 0.04672 (14) | |
Hg2 | 0.24241 (5) | 0.26466 (4) | 0.48016 (3) | 0.05259 (15) | |
Hg3 | 0.17054 (5) | 0.26822 (4) | 0.25961 (3) | 0.04796 (14) | |
Hg4 | 0.32403 (5) | 0.23488 (4) | 0.69056 (3) | 0.05249 (15) | |
I1 | 0.21389 (6) | 0.11121 (5) | 0.73107 (4) | 0.03533 (18) | |
I2 | 0.55075 (7) | 0.11387 (6) | 0.92013 (5) | 0.0418 (2) | |
I3 | 0.37342 (7) | 0.37437 (6) | 0.44126 (5) | 0.0456 (2) | |
I4 | 0.27812 (8) | 0.14200 (6) | 0.16275 (6) | 0.0498 (2) | |
I5 | 0.04493 (7) | 0.40968 (7) | 0.28468 (6) | 0.0537 (2) | |
I6 | 0.24863 (8) | 0.33706 (7) | 0.99093 (6) | 0.0580 (3) | |
I7 | 0.40076 (7) | 0.15357 (5) | 0.54342 (5) | 0.03795 (19) | |
I8 | 0.49995 (7) | 0.34043 (6) | 0.83231 (5) | 0.0405 (2) | |
I9 | 0.05955 (7) | 0.16003 (6) | 0.34222 (5) | 0.0404 (2) | |
I10 | 0.16514 (7) | 0.34376 (5) | 0.62856 (5) | 0.03698 (19) | |
N1 | 0.6372 (8) | 0.3455 (6) | 0.2355 (6) | 0.033 (2) | |
C1 | 0.6908 (9) | 0.3962 (7) | 0.1937 (6) | 0.032 (3) | |
H1B | 0.7112 | 0.4619 | 0.2322 | 0.039* | |
H1A | 0.7642 | 0.3709 | 0.1843 | 0.039* | |
C3 | 0.7231 (9) | 0.3759 (8) | 0.3206 (6) | 0.033 (3) | |
H3B | 0.8025 | 0.3667 | 0.3136 | 0.040* | |
H3A | 0.7221 | 0.4426 | 0.3520 | 0.040* | |
C2 | 0.6193 (10) | 0.2403 (7) | 0.1847 (7) | 0.033 (3) | |
H2B | 0.5823 | 0.2122 | 0.2128 | 0.040* | |
H2A | 0.5634 | 0.2264 | 0.1312 | 0.040* | |
C6 | 0.7271 (11) | 0.1935 (8) | 0.1690 (8) | 0.048 (3) | |
H6B | 0.7912 | 0.2175 | 0.2201 | 0.057* | |
H6A | 0.7527 | 0.2066 | 0.1278 | 0.057* | |
C5 | 0.6128 (10) | 0.3898 (8) | 0.1117 (6) | 0.035 (3) | |
H5B | 0.5402 | 0.4171 | 0.1202 | 0.042* | |
H5A | 0.5914 | 0.3245 | 0.0722 | 0.042* | |
C9 | 0.6784 (11) | 0.4418 (8) | 0.0762 (7) | 0.041 (3) | |
H9B | 0.6214 | 0.4513 | 0.0326 | 0.049* | |
H9A | 0.7137 | 0.5029 | 0.1200 | 0.049* | |
C13 | 0.7760 (11) | 0.3889 (9) | 0.0405 (8) | 0.047 (3) | |
H13C | 0.8149 | 0.4247 | 0.0200 | 0.056* | |
H13B | 0.7412 | 0.3292 | −0.0044 | 0.056* | |
H13A | 0.8330 | 0.3795 | 0.0833 | 0.056* | |
C4 | 0.5129 (10) | 0.3763 (8) | 0.2415 (7) | 0.036 (3) | |
H4B | 0.4624 | 0.3586 | 0.1856 | 0.043* | |
H4A | 0.4783 | 0.3421 | 0.2660 | 0.043* | |
C8 | 0.5121 (10) | 0.4802 (8) | 0.2922 (7) | 0.041 (3) | |
H8B | 0.5518 | 0.5164 | 0.2717 | 0.049* | |
H8A | 0.5530 | 0.4982 | 0.3503 | 0.049* | |
C12 | 0.3780 (11) | 0.4986 (8) | 0.2825 (8) | 0.043 (3) | |
H12B | 0.3399 | 0.4851 | 0.2248 | 0.052* | |
H12A | 0.3373 | 0.4568 | 0.2973 | 0.052* | |
C7 | 0.7001 (11) | 0.3270 (10) | 0.3713 (8) | 0.053 (3) | |
H7B | 0.7018 | 0.2601 | 0.3415 | 0.064* | |
H7A | 0.6221 | 0.3371 | 0.3808 | 0.064* | |
C11 | 0.799 (2) | 0.3666 (12) | 0.4578 (10) | 0.109 (8) | |
H11B | 0.8769 | 0.3628 | 0.4477 | 0.131* | |
H11A | 0.7916 | 0.4321 | 0.4893 | 0.131* | |
C16 | 0.3674 (12) | 0.5986 (9) | 0.3374 (9) | 0.055 (4) | |
H16C | 0.2849 | 0.6078 | 0.3306 | 0.066* | |
H16B | 0.4061 | 0.6400 | 0.3220 | 0.066* | |
H16A | 0.4044 | 0.6119 | 0.3946 | 0.066* | |
C10 | 0.6987 (12) | 0.0892 (8) | 0.1382 (9) | 0.051 (3) | |
H10B | 0.6284 | 0.0679 | 0.0911 | 0.061* | |
H10A | 0.6793 | 0.0773 | 0.1820 | 0.061* | |
C14 | 0.7961 (13) | 0.0320 (10) | 0.1119 (10) | 0.066 (4) | |
H14C | 0.7709 | −0.0330 | 0.0944 | 0.079* | |
H14B | 0.8661 | 0.0519 | 0.1581 | 0.079* | |
H14A | 0.8135 | 0.0405 | 0.0666 | 0.079* | |
N2 | 0.1871 (7) | 0.8544 (6) | 0.2661 (5) | 0.025 (2) | |
C25 | 0.1782 (11) | 0.9389 (10) | 0.4984 (7) | 0.053 (4) | |
H25B | 0.2333 | 0.9385 | 0.5475 | 0.064* | |
H25A | 0.1729 | 1.0037 | 0.5076 | 0.064* | |
C21 | 0.2272 (11) | 0.8888 (9) | 0.4227 (7) | 0.044 (3) | |
H21B | 0.3102 | 0.9122 | 0.4367 | 0.053* | |
H21A | 0.2222 | 0.8221 | 0.4083 | 0.053* | |
C17 | 0.1578 (10) | 0.9046 (7) | 0.3490 (6) | 0.032 (3) | |
H17B | 0.1677 | 0.9713 | 0.3642 | 0.039* | |
H17A | 0.0742 | 0.8868 | 0.3402 | 0.039* | |
C19 | 0.1084 (9) | 0.8829 (7) | 0.2042 (6) | 0.029 (2) | |
H19B | 0.1254 | 0.9501 | 0.2238 | 0.035* | |
H19A | 0.0265 | 0.8704 | 0.2032 | 0.035* | |
C23 | 0.1188 (11) | 0.8357 (8) | 0.1153 (7) | 0.041 (3) | |
H23B | 0.2011 | 0.8448 | 0.1155 | 0.049* | |
H23A | 0.0954 | 0.7689 | 0.0930 | 0.049* | |
C27 | 0.0417 (10) | 0.8747 (10) | 0.0600 (7) | 0.047 (3) | |
H27B | 0.0689 | 0.9406 | 0.0805 | 0.056* | |
H27A | −0.0394 | 0.8698 | 0.0634 | 0.056* | |
C31 | 0.0431 (13) | 0.8249 (12) | −0.0300 (8) | 0.065 (4) | |
H31C | −0.0072 | 0.8525 | −0.0621 | 0.078* | |
H31B | 0.0146 | 0.7598 | −0.0512 | 0.078* | |
H31A | 0.1229 | 0.8306 | −0.0341 | 0.078* | |
C20 | 0.3188 (9) | 0.8807 (7) | 0.2771 (6) | 0.028 (2) | |
H20B | 0.3382 | 0.8428 | 0.2255 | 0.034* | |
H20A | 0.3661 | 0.8644 | 0.3200 | 0.034* | |
C24 | 0.3562 (9) | 0.9847 (8) | 0.3008 (7) | 0.034 (3) | |
H24B | 0.3246 | 0.9993 | 0.2536 | 0.041* | |
H24A | 0.3258 | 1.0250 | 0.3466 | 0.041* | |
C28 | 0.4894 (9) | 0.9998 (8) | 0.3257 (7) | 0.035 (3) | |
H28B | 0.5193 | 0.9524 | 0.2832 | 0.042* | |
H28A | 0.5199 | 0.9938 | 0.3775 | 0.042* | |
C18 | 0.1714 (9) | 0.7474 (6) | 0.2367 (7) | 0.029 (2) | |
H18B | 0.1962 | 0.7178 | 0.1859 | 0.035* | |
H18A | 0.2232 | 0.7321 | 0.2787 | 0.035* | |
C22 | 0.0441 (10) | 0.7069 (8) | 0.2204 (8) | 0.044 (3) | |
H22B | 0.0166 | 0.7391 | 0.2698 | 0.053* | |
H22A | −0.0073 | 0.7172 | 0.1751 | 0.053* | |
C29 | 0.0592 (15) | 0.8946 (12) | 0.4877 (10) | 0.079 (5) | |
H29C | 0.0325 | 0.9285 | 0.5365 | 0.095* | |
H29B | 0.0643 | 0.8308 | 0.4799 | 0.095* | |
H29A | 0.0038 | 0.8959 | 0.4399 | 0.095* | |
C26 | 0.0357 (11) | 0.6017 (8) | 0.1980 (7) | 0.040 (3) | |
H26B | 0.0816 | 0.5925 | 0.2456 | 0.048* | |
H26A | −0.0466 | 0.5784 | 0.1870 | 0.048* | |
C30 | 0.0794 (13) | 0.5455 (9) | 0.1241 (9) | 0.065 (4) | |
H30C | 0.0738 | 0.4808 | 0.1145 | 0.078* | |
H30B | 0.1608 | 0.5681 | 0.1343 | 0.078* | |
H30A | 0.0318 | 0.5514 | 0.0759 | 0.078* | |
C32 | 0.5330 (11) | 1.0989 (9) | 0.3371 (8) | 0.052 (4) | |
H32C | 0.6183 | 1.1080 | 0.3535 | 0.063* | |
H32B | 0.5036 | 1.1456 | 0.3795 | 0.063* | |
H32A | 0.5039 | 1.1042 | 0.2855 | 0.063* | |
C15 | 0.789 (2) | 0.316 (2) | 0.5052 (16) | 0.167 (12) | |
H15C | 0.8509 | 0.3418 | 0.5566 | 0.200* | |
H15B | 0.7965 | 0.2516 | 0.4742 | 0.200* | |
H15A | 0.7129 | 0.3218 | 0.5170 | 0.200* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg1 | 0.0433 (3) | 0.0550 (3) | 0.0383 (3) | 0.0149 (3) | 0.0130 (2) | 0.0152 (2) |
Hg2 | 0.0576 (3) | 0.0578 (4) | 0.0441 (3) | −0.0034 (3) | 0.0078 (3) | 0.0267 (3) |
Hg3 | 0.0431 (3) | 0.0532 (3) | 0.0524 (3) | 0.0132 (3) | 0.0159 (3) | 0.0253 (3) |
Hg4 | 0.0562 (3) | 0.0607 (4) | 0.0398 (3) | −0.0009 (3) | 0.0082 (3) | 0.0234 (3) |
I1 | 0.0272 (4) | 0.0453 (5) | 0.0307 (4) | 0.0036 (3) | 0.0080 (3) | 0.0134 (3) |
I2 | 0.0395 (4) | 0.0408 (5) | 0.0414 (4) | 0.0058 (4) | 0.0083 (4) | 0.0154 (4) |
I3 | 0.0438 (5) | 0.0546 (5) | 0.0454 (5) | 0.0025 (4) | 0.0118 (4) | 0.0281 (4) |
I4 | 0.0427 (5) | 0.0526 (5) | 0.0523 (5) | 0.0076 (4) | 0.0147 (4) | 0.0195 (4) |
I5 | 0.0343 (5) | 0.0531 (5) | 0.0883 (7) | 0.0099 (4) | 0.0172 (5) | 0.0437 (5) |
I6 | 0.0442 (5) | 0.0711 (6) | 0.0472 (5) | 0.0179 (5) | 0.0187 (4) | 0.0104 (5) |
I7 | 0.0405 (4) | 0.0391 (5) | 0.0356 (4) | 0.0105 (4) | 0.0124 (3) | 0.0160 (4) |
I8 | 0.0414 (5) | 0.0396 (5) | 0.0367 (4) | 0.0062 (4) | 0.0090 (4) | 0.0133 (4) |
I9 | 0.0476 (5) | 0.0369 (4) | 0.0372 (4) | −0.0004 (4) | 0.0096 (4) | 0.0172 (4) |
I10 | 0.0357 (4) | 0.0334 (4) | 0.0378 (4) | 0.0063 (4) | 0.0109 (4) | 0.0107 (4) |
N1 | 0.025 (5) | 0.033 (5) | 0.037 (5) | 0.003 (4) | 0.007 (4) | 0.012 (4) |
C1 | 0.027 (6) | 0.033 (6) | 0.038 (6) | −0.010 (5) | 0.014 (5) | 0.014 (5) |
C3 | 0.028 (6) | 0.034 (6) | 0.031 (6) | 0.002 (5) | 0.003 (5) | 0.012 (5) |
C2 | 0.033 (6) | 0.028 (6) | 0.034 (6) | 0.006 (5) | 0.005 (5) | 0.012 (5) |
C6 | 0.042 (7) | 0.043 (7) | 0.044 (7) | −0.002 (6) | 0.014 (6) | 0.003 (6) |
C5 | 0.041 (7) | 0.044 (7) | 0.024 (6) | 0.000 (6) | 0.015 (5) | 0.016 (5) |
C9 | 0.048 (7) | 0.029 (6) | 0.041 (7) | 0.009 (6) | 0.014 (6) | 0.010 (5) |
C13 | 0.055 (8) | 0.050 (8) | 0.047 (7) | 0.025 (7) | 0.033 (7) | 0.020 (6) |
C4 | 0.030 (6) | 0.045 (7) | 0.042 (7) | 0.004 (5) | 0.016 (5) | 0.023 (6) |
C8 | 0.038 (7) | 0.045 (7) | 0.040 (7) | 0.010 (6) | 0.017 (6) | 0.015 (6) |
C12 | 0.041 (7) | 0.043 (7) | 0.057 (8) | 0.014 (6) | 0.027 (6) | 0.024 (6) |
C7 | 0.047 (8) | 0.078 (10) | 0.044 (8) | 0.022 (7) | 0.014 (6) | 0.035 (7) |
C11 | 0.23 (3) | 0.068 (11) | 0.049 (10) | 0.010 (14) | 0.052 (13) | 0.033 (9) |
C16 | 0.065 (10) | 0.047 (8) | 0.062 (9) | 0.034 (7) | 0.039 (8) | 0.020 (7) |
C10 | 0.050 (8) | 0.038 (7) | 0.069 (9) | 0.014 (6) | 0.020 (7) | 0.025 (7) |
C14 | 0.068 (10) | 0.051 (9) | 0.085 (11) | 0.021 (8) | 0.032 (9) | 0.029 (8) |
N2 | 0.025 (5) | 0.021 (5) | 0.030 (5) | 0.012 (4) | 0.011 (4) | 0.010 (4) |
C25 | 0.048 (8) | 0.074 (9) | 0.029 (6) | −0.020 (7) | 0.011 (6) | 0.013 (6) |
C21 | 0.046 (7) | 0.059 (8) | 0.035 (7) | 0.015 (7) | 0.020 (6) | 0.023 (6) |
C17 | 0.033 (6) | 0.030 (6) | 0.038 (6) | 0.005 (5) | 0.019 (5) | 0.013 (5) |
C19 | 0.025 (6) | 0.024 (6) | 0.036 (6) | 0.004 (5) | 0.002 (5) | 0.013 (5) |
C23 | 0.051 (8) | 0.043 (7) | 0.027 (6) | 0.016 (6) | 0.016 (6) | 0.011 (5) |
C27 | 0.028 (6) | 0.079 (10) | 0.042 (7) | 0.008 (7) | 0.000 (6) | 0.038 (7) |
C31 | 0.056 (9) | 0.104 (13) | 0.047 (8) | 0.029 (9) | 0.015 (7) | 0.043 (9) |
C20 | 0.033 (6) | 0.036 (6) | 0.027 (5) | 0.019 (5) | 0.020 (5) | 0.016 (5) |
C24 | 0.026 (6) | 0.043 (7) | 0.039 (6) | −0.001 (5) | 0.003 (5) | 0.026 (6) |
C28 | 0.030 (6) | 0.036 (6) | 0.044 (7) | 0.010 (5) | 0.017 (5) | 0.019 (6) |
C18 | 0.027 (6) | 0.016 (5) | 0.042 (6) | 0.006 (5) | 0.001 (5) | 0.014 (5) |
C22 | 0.036 (7) | 0.039 (7) | 0.055 (8) | −0.001 (6) | 0.006 (6) | 0.021 (6) |
C29 | 0.091 (12) | 0.089 (12) | 0.057 (10) | −0.018 (10) | 0.030 (9) | 0.026 (9) |
C26 | 0.038 (7) | 0.036 (7) | 0.047 (7) | 0.007 (6) | 0.012 (6) | 0.018 (6) |
C30 | 0.074 (10) | 0.044 (8) | 0.064 (9) | 0.000 (8) | 0.039 (8) | 0.001 (7) |
C32 | 0.037 (7) | 0.055 (8) | 0.052 (8) | −0.023 (7) | −0.009 (6) | 0.022 (7) |
C15 | 0.14 (2) | 0.25 (3) | 0.12 (2) | −0.01 (2) | 0.031 (17) | 0.09 (2) |
Hg1—I6 | 2.6347 (11) | C5—C9 | 1.536 (14) |
Hg1—I2 | 2.6476 (10) | C9—C13 | 1.530 (15) |
Hg1—I1 | 3.0800 (9) | C4—C8 | 1.516 (16) |
Hg1—I8 | 3.2065 (10) | C8—C12 | 1.574 (16) |
Hg2—I3 | 2.7152 (9) | C12—C16 | 1.507 (16) |
Hg2—I9 | 2.7489 (10) | C7—C11 | 1.58 (2) |
Hg2—I10 | 2.8554 (9) | C11—C15 | 1.42 (3) |
Hg2—I7 | 2.9103 (10) | C10—C14 | 1.503 (18) |
Hg3—I5 | 2.6167 (11) | N2—C19 | 1.497 (13) |
Hg3—I4 | 2.6231 (11) | N2—C17 | 1.519 (12) |
Hg3—I9 | 3.1534 (9) | N2—C20 | 1.535 (12) |
Hg3—I3 | 3.3150 (10) | N2—C18 | 1.541 (12) |
Hg4—I8 | 2.7435 (10) | C25—C29 | 1.486 (17) |
Hg4—I1 | 2.7659 (9) | C25—C21 | 1.535 (16) |
Hg4—I7 | 2.8346 (9) | C21—C17 | 1.510 (16) |
Hg4—I10 | 2.8759 (11) | C19—C23 | 1.520 (14) |
N1—C3 | 1.508 (13) | C23—C27 | 1.510 (16) |
N1—C2 | 1.514 (13) | C27—C31 | 1.509 (17) |
N1—C1 | 1.534 (12) | C20—C24 | 1.545 (14) |
N1—C4 | 1.548 (14) | C24—C28 | 1.499 (15) |
C1—C5 | 1.515 (15) | C28—C32 | 1.556 (15) |
C3—C7 | 1.497 (15) | C18—C22 | 1.526 (14) |
C2—C6 | 1.490 (16) | C22—C26 | 1.532 (15) |
C6—C10 | 1.507 (16) | C26—C30 | 1.492 (16) |
I6—Hg1—I2 | 142.91 (4) | C3—N1—C4 | 111.6 (8) |
I6—Hg1—I1 | 104.66 (3) | C2—N1—C4 | 106.7 (8) |
I2—Hg1—I1 | 104.76 (3) | C1—N1—C4 | 109.1 (8) |
I6—Hg1—I8 | 104.08 (3) | C5—C1—N1 | 116.0 (8) |
I2—Hg1—I8 | 99.08 (3) | C7—C3—N1 | 116.1 (9) |
I1—Hg1—I8 | 87.89 (2) | C6—C2—N1 | 117.1 (9) |
I3—Hg2—I9 | 108.93 (3) | C2—C6—C10 | 109.5 (9) |
I3—Hg2—I10 | 120.18 (3) | C1—C5—C9 | 110.4 (9) |
I9—Hg2—I10 | 112.23 (3) | C13—C9—C5 | 112.9 (10) |
I3—Hg2—I7 | 108.25 (3) | C8—C4—N1 | 114.9 (9) |
I9—Hg2—I7 | 114.09 (3) | C4—C8—C12 | 107.0 (9) |
I10—Hg2—I7 | 92.33 (3) | C16—C12—C8 | 111.2 (10) |
I5—Hg3—I4 | 149.08 (4) | C3—C7—C11 | 109.3 (11) |
I5—Hg3—I9 | 101.10 (3) | C15—C11—C7 | 111.9 (18) |
I4—Hg3—I9 | 103.60 (3) | C6—C10—C14 | 115.3 (11) |
I5—Hg3—I3 | 94.43 (3) | C19—N2—C17 | 108.2 (8) |
I4—Hg3—I3 | 105.20 (3) | C19—N2—C20 | 111.1 (7) |
I9—Hg3—I3 | 86.82 (2) | C17—N2—C20 | 109.4 (7) |
I8—Hg4—I1 | 104.75 (3) | C19—N2—C18 | 111.5 (8) |
I8—Hg4—I7 | 114.82 (3) | C17—N2—C18 | 110.9 (8) |
I1—Hg4—I7 | 115.92 (3) | C20—N2—C18 | 105.7 (7) |
I8—Hg4—I10 | 113.95 (3) | C29—C25—C21 | 112.7 (11) |
I1—Hg4—I10 | 114.20 (3) | C17—C21—C25 | 110.7 (10) |
I7—Hg4—I10 | 93.49 (3) | C21—C17—N2 | 118.5 (9) |
Hg4—I1—Hg1 | 84.53 (2) | N2—C19—C23 | 116.4 (9) |
Hg2—I3—Hg3 | 80.86 (3) | C27—C23—C19 | 111.6 (10) |
Hg4—I7—Hg2 | 86.95 (3) | C23—C27—C31 | 113.2 (11) |
Hg4—I8—Hg1 | 82.50 (3) | N2—C20—C24 | 115.9 (8) |
Hg2—I9—Hg3 | 83.38 (2) | C28—C24—C20 | 107.4 (9) |
Hg2—I10—Hg4 | 87.22 (3) | C24—C28—C32 | 110.0 (10) |
C3—N1—C2 | 113.0 (9) | C22—C18—N2 | 113.7 (9) |
C3—N1—C1 | 104.9 (8) | C26—C22—C18 | 111.4 (10) |
C2—N1—C1 | 111.6 (8) | C30—C26—C22 | 113.8 (10) |
Experimental details
Crystal data | |
Chemical formula | (C16H36N)2[Hg4I10] |
Mr | 2556.28 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 11.681, 15.770, 18.288 |
α, β, γ (°) | 114.33, 104.18, 90.18 |
V (Å3) | 2955.3 |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 15.60 |
Crystal size (mm) | 0.3 × 0.15 × 0.1 |
Data collection | |
Diffractometer | Stoe Imaging Plate Diffraction System, IPDS-I diffractometer |
Absorption correction | Numerical X-SHAPE (Stoe & Cie, 1998) |
Tmin, Tmax | 0.075, 0.210 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 37776, 11615, 5987 |
Rint | 0.107 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.060, 0.75 |
No. of reflections | 11615 |
No. of parameters | 434 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.23, −1.22 |
Computer programs: X-AREA (Stoe & Cie, 2001), X-STEP32 (Stoe & Cie, 2000), X-RED (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, Bonn, 1999), SHELXL97.
Hg1—I6 | 2.6347 (11) | Hg4—I8 | 2.7435 (10) |
Hg1—I2 | 2.6476 (10) | Hg4—I1 | 2.7659 (9) |
Hg1—I1 | 3.0800 (9) | Hg4—I7 | 2.8346 (9) |
Hg1—I8 | 3.2065 (10) | Hg4—I10 | 2.8759 (11) |
Hg2—I3 | 2.7152 (9) | N1—C3 | 1.508 (13) |
Hg2—I9 | 2.7489 (10) | N1—C2 | 1.514 (13) |
Hg2—I10 | 2.8554 (9) | N1—C1 | 1.534 (12) |
Hg2—I7 | 2.9103 (10) | N1—C4 | 1.548 (14) |
Hg3—I5 | 2.6167 (11) | N2—C19 | 1.497 (13) |
Hg3—I4 | 2.6231 (11) | N2—C17 | 1.519 (12) |
Hg3—I9 | 3.1534 (9) | N2—C20 | 1.535 (12) |
Hg3—I3 | 3.3150 (10) | N2—C18 | 1.541 (12) |
I6—Hg1—I2 | 142.91 (4) | I8—Hg4—I10 | 113.95 (3) |
I6—Hg1—I1 | 104.66 (3) | I1—Hg4—I10 | 114.20 (3) |
I2—Hg1—I1 | 104.76 (3) | I7—Hg4—I10 | 93.49 (3) |
I6—Hg1—I8 | 104.08 (3) | Hg4—I1—Hg1 | 84.53 (2) |
I2—Hg1—I8 | 99.08 (3) | Hg2—I3—Hg3 | 80.86 (3) |
I1—Hg1—I8 | 87.89 (2) | Hg4—I7—Hg2 | 86.95 (3) |
I3—Hg2—I9 | 108.93 (3) | Hg4—I8—Hg1 | 82.50 (3) |
I3—Hg2—I10 | 120.18 (3) | Hg2—I9—Hg3 | 83.38 (2) |
I9—Hg2—I10 | 112.23 (3) | Hg2—I10—Hg4 | 87.22 (3) |
I3—Hg2—I7 | 108.25 (3) | C3—N1—C2 | 113.0 (9) |
I9—Hg2—I7 | 114.09 (3) | C3—N1—C1 | 104.9 (8) |
I10—Hg2—I7 | 92.33 (3) | C2—N1—C1 | 111.6 (8) |
I5—Hg3—I4 | 149.08 (4) | C3—N1—C4 | 111.6 (8) |
I5—Hg3—I9 | 101.10 (3) | C2—N1—C4 | 106.7 (8) |
I4—Hg3—I9 | 103.60 (3) | C1—N1—C4 | 109.1 (8) |
I5—Hg3—I3 | 94.43 (3) | C19—N2—C17 | 108.2 (8) |
I4—Hg3—I3 | 105.20 (3) | C19—N2—C20 | 111.1 (7) |
I9—Hg3—I3 | 86.82 (2) | C17—N2—C20 | 109.4 (7) |
I8—Hg4—I1 | 104.75 (3) | C19—N2—C18 | 111.5 (8) |
I8—Hg4—I7 | 114.82 (3) | C17—N2—C18 | 110.9 (8) |
I1—Hg4—I7 | 115.92 (3) | C20—N2—C18 | 105.7 (7) |
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Halogenomercurate(II) anions show a wide variety of steric arrangements, dependent upon charge and size of the counter-cation(s) and the stoichiometry (Dean et al., 1994; Grdenic et al. 1965; House et al., 1994; Serezhkin et al., 2001). Up to now, only one compound has been reported for the Bu4NI/HgI2 system. (Bu4N)[HgI3] contains trigonal planar [HgI3]− units (Goggin et al., 1982).
Other discrete iodomercurate(II) anions with different cations that have been reported are the tetrahedral [HgI4]− and the octahedral [HgI6]4−, as well as the dimeric [Hg2I6]2− and the trimeric [Hg3I8]2− units.
Recently, we have reported on the structure of (Et4N)2[Hg4Cl10] (Nockemann & Meyer, 2002). Bitetrahedral [Hg2Cl6]2− anions built from two tetrahedra sharing one common edge have two slightly bent HgCl2 molecules, with Cl—Hg—Cl angles of about 170°, attached to either side so that, in summa, it may be considered as the tetrameric [Hg4Cl10]2− anion. The two terminal mercuric ions exhibit coordination number 2 + 1 in a T-shaped arrangement.
The tetrameric anion [Hg4I10]2− in the crystal structure of (Bu4N)2[Hg4I10] may also be derived from bitetrahedral [Hg2I6]2− units to which two HgI2 molecules are again attached on either side. The two central tetrahedra are only slightly distorted with Hg—I distances ranging from 2.715 (1) to 2.910 (1) Å. The outer HgI2 molecules show considerably shorter distances ranging between 2.617 (1) and 2.647 (1) Å, with I—Hg—I angles of 149.09 (5) and 142.93 (4)°, but the distances to the iodide ions of the edges shared with the central [Hg2I6]2− are, in turn, much longer, 3.080 (1)–3.316 (1) Å. In summary, in the tetrameric anion [Hg4I10]2−, all mercuric ions may be considered as having coordination number 4, and all tetrahedra share common edges, in contrast to the situation in the tetrameric [Hg4Cl10]2− where coordination numbers are 4 and 3 (twice each), respectively.
In (Bu4N)2[Hg4I10], charge balance is achieved by two crystallographically independent, perfectly ordered tetrahedral [Bu4N]+ cations which are arranged in the crystal structure, together with the anions in a 2:1 ratio, as Fig. 1 illustrates.