Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102020036/tr1042sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102020036/tr1042Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102020036/tr1042IIsup3.hkl |
CCDC references: 201262; 201263
The synthesis of (I) was carried out as follows. Ortho- or para-carborane (1.0 g, 6.90 mmol) was dissolved in dry diethyl ether (70 ml) and cooled to 273 K. n-BuLi (1.6M solution in hexanes, 6.90 mmol, 4.31 ml) was added dropwise and, after 45 min at 273 K, HgCl2 (99.5%, 3.45 mmol, 0.941 g) was added. The resulting heterogeneous solution was slowly warmed to room temperature over 45 min and then heated to reflux overnight. The reaction was quenched with water (50 ml) and the organic layer extracted with brine (50 ml). The aqueous layers were combined and further extracted with diethyl ether (3 × 20 ml). The organic layers were then combined, dried over MgSO4 and filtered, and the solvent was removed by rotary evaporation. The resulting powder was triturated with diethyl ether, affording a white solid (1.528 g, 91%). The remaining solution was evaporated under reduced pressure, and an additional aliquot of powder was isolated by flash chromatography (CH2Cl2-petroleum ether; from 3:7 to 1:1, 33 mg). The solids were combined and recrystallized from a 1:1 mixture of hexanes and CH2Cl2, affording colorless crystals of (I) (1.562 g, 93%). Analytical data: Rf (1:1 CH2Cl2-petroleum ether) = 0.48; m.p. >583 K. Spectroscopic data: IR (KBr, cm-1): 3066 (m, νCH), 2592, 2572, 2502 (s, νBH), 1700, 1073, 1025, 722; 1H NMR (200 MHz, CD2Cl2, δ, p.p.m.): 3.90–0.90 (m, 20H, 2 B10H10), 3.72 (br s, 2H, 2 CH); 13C NMR (50 MHz, CD2Cl2, δ, p.p.m.): 85.4 (C—Hg), 60.9 (CH); 11B 〈 1H 〉 NMR (160 MHz, acetone-d6, δ, p.p.m.): -0.7, -1.9, -7.5, -10.2, -12.0; EIMS: m/z = 487 [M+], having the expected boron isotope distribution.
To synthesize (II), the same methodology used to prepare (I) was employed except that, after the inital work-up and solvent evaporation, the resulting solid was purified by flash chromatography using petroleum ether. The product, a white solid, was crystallized from CH2Cl2:THF (Ratio?), giving (II) as colorless crystals (1.549 g, 92%). Analytical data: Rf (petroleum ether) = 0.70; m.p. = 531 K (decomposition). Spectroscopic data: IR (KBr, cm-1): 3063 (m, νCH), 2615 (s, νBH), 1261, 1144, 1090, 1009, 823, 763, 727; 1H NMR (200 MHz, CD2Cl2, δ, p.p.m.): 3.80–0.30 (m, 20H, 2 B10H10), 2.50 (br s, 2H, 2 CH); 13C NMR (50 MHz, CD2Cl2, δ, p.p.m.): 93.8 (C—Hg), 68.6 (CH); 11B 〈 1H 〉 NMR (160 MHz, acetone-d6, δ, p.p.m.): -11.6, -12.6; EIMS: m/z = 488 [M+], having the expected boron isotope distribution.
For both compounds, the H atoms were placed geometrically and refined using a riding model, with Uiso(H) = 1.2Ueq(C) or 1.2Ueq(B). C—H(carborane) and B—H(carborane) distances were constrained to 1.14 Å. Atom C4' in compound (II) was intentionally refined isotropically, due to the detrimental effect that anisotropic refinement at this position had on the least-squares analysis of that model. This is most likely to be due to the disordered nature of the THF solvent molecule in the crystal lattice of (II). The crystal used to collect the data for (II) was twinned. An initial unit-cell determination gave the orthorhombic mmm system. However, upon integration, it was apparent that this was incorrect, as no appropriate set of systematic absences was present. A search for alternative metric symmetry revealed three potential monoclinic systems, of which one contained a more favourable R(sym). Upon re-integrating the data in the monoclinic Laue class 2/m, followed by redetermination of the absorption correction, a unit cell was found but solution determination was still problematic. Introduction of the (100/0–10/00–1) twin law led to an immediate benefit upon least-squares analysis and the refinement proceeded smoothly to the final reported model.
For both compounds, data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and WinGX (Farrugia, 1999); software used to prepare material for publication: SHELXTL.
[Hg(C2B10H11)2]·CH2Cl2 | F(000) = 1072 |
Mr = 571.94 | Dx = 1.753 Mg m−3 |
Triclinic, P1 | Melting point > 583 K |
a = 12.4673 (18) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.5634 (18) Å | Cell parameters from 29083 reflections |
c = 13.5910 (18) Å | θ = 3.1–36.3° |
α = 105.642 (4)° | µ = 7.34 mm−1 |
β = 101.243 (4)° | T = 100 K |
γ = 90.381 (5)° | Plate, colorless |
V = 2166.4 (5) Å3 | 0.25 × 0.20 × 0.08 mm |
Z = 4 |
Bruker SMART 1K CCD area-detector diffractometer | 17966 independent reflections |
Radiation source: rotating anode | 15490 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ϕ and ω scans | θmax = 36.3°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | h = −16→20 |
Tmin = 0.298, Tmax = 0.556 | k = −22→19 |
44711 measured reflections | l = −21→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)] = 0.026 | H-atom parameters constrained |
wR(F2) = 0.062 | w = 1/[σ2(Fo2) + (0.0186P)2 + 0.6468P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.005 |
17966 reflections | Δρmax = 2.18 e Å−3 |
506 parameters | Δρmin = −2.03 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00133 (8) |
[Hg(C2B10H11)2]·CH2Cl2 | γ = 90.381 (5)° |
Mr = 571.94 | V = 2166.4 (5) Å3 |
Triclinic, P1 | Z = 4 |
a = 12.4673 (18) Å | Mo Kα radiation |
b = 13.5634 (18) Å | µ = 7.34 mm−1 |
c = 13.5910 (18) Å | T = 100 K |
α = 105.642 (4)° | 0.25 × 0.20 × 0.08 mm |
β = 101.243 (4)° |
Bruker SMART 1K CCD area-detector diffractometer | 17966 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | 15490 reflections with I > 2σ(I) |
Tmin = 0.298, Tmax = 0.556 | Rint = 0.031 |
44711 measured reflections |
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.05 | Δρmax = 2.18 e Å−3 |
17966 reflections | Δρmin = −2.03 e Å−3 |
506 parameters |
Experimental. X-ray crystallographic data were collected from a single-crystal sample of (I) and mounted on a glass fibre. Data were collected using a P4 Bruker diffractometer, equipped with a Bruker SMART 1 K CCD area detector, using the program SMART (Bruker, 1997), and a rotating anode, using graphite-monochromated Mo—Kα radiation. The crystal-to-detector distance was 4.987 cm, and the data collection was carried out in 512 × 512 pixel mode, utilizing 2 × 2 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular settings of the strong reflections, collected by a 12° scan in 40 frames over four different sections of reciprocal space (160 frames in total). Almost a complete sphere of data was collected, to better than 0.8 Å resolution at 100 K. Upon completion of the data collection, the first 40 frames were recollected in order to improve the decay correction analysis, which was determined to be negligible. |
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 | 0.442031 (5) | 0.692684 (6) | 0.228930 (6) | 0.01086 (2) | |
C1A | 0.56461 (15) | 0.79544 (16) | 0.22163 (18) | 0.0123 (4) | |
C2A | 0.53076 (19) | 0.8652 (2) | 0.1353 (2) | 0.0243 (5) | |
H2A | 0.4455 | 0.8571 | 0.0838 | 0.029* | |
B3A | 0.61953 (19) | 0.7667 (2) | 0.1104 (2) | 0.0160 (5) | |
H3A | 0.5974 | 0.6932 | 0.0439 | 0.019* | |
B4A | 0.69909 (18) | 0.7672 (2) | 0.2341 (2) | 0.0163 (5) | |
H4A | 0.7311 | 0.6935 | 0.2506 | 0.020* | |
B5A | 0.6550 (2) | 0.8649 (2) | 0.3316 (2) | 0.0188 (5) | |
H5A | 0.6568 | 0.8573 | 0.4134 | 0.023* | |
B6A | 0.55200 (18) | 0.9227 (2) | 0.2647 (2) | 0.0162 (5) | |
H6A | 0.4811 | 0.9547 | 0.3028 | 0.019* | |
B7A | 0.60085 (19) | 0.9851 (2) | 0.1854 (2) | 0.0181 (5) | |
H7A | 0.5667 | 1.0581 | 0.1690 | 0.022* | |
B8A | 0.6457 (2) | 0.8869 (2) | 0.0872 (2) | 0.0177 (5) | |
H8A | 0.6421 | 0.8942 | 0.0050 | 0.021* | |
B9A | 0.75374 (19) | 0.8265 (2) | 0.1510 (2) | 0.0180 (5) | |
H9A | 0.8236 | 0.7935 | 0.1118 | 0.022* | |
B10A | 0.7754 (2) | 0.8872 (2) | 0.2882 (2) | 0.0191 (5) | |
H10A | 0.8599 | 0.8947 | 0.3409 | 0.023* | |
B11A | 0.6809 (2) | 0.9851 (2) | 0.3089 (2) | 0.0207 (5) | |
H11A | 0.7009 | 1.0585 | 0.3757 | 0.025* | |
B12A | 0.74122 (18) | 0.9615 (2) | 0.1980 (2) | 0.0147 (4) | |
H12A | 0.8032 | 1.0196 | 0.1901 | 0.018* | |
C1B | 0.31721 (15) | 0.58608 (16) | 0.22409 (17) | 0.0111 (4) | |
C2B | 0.34841 (16) | 0.47187 (17) | 0.23809 (19) | 0.0135 (4) | |
H2B | 0.4380 | 0.4533 | 0.2556 | 0.016* | |
B3B | 0.29608 (19) | 0.4806 (2) | 0.1145 (2) | 0.0146 (4) | |
H3B | 0.3434 | 0.4696 | 0.0488 | 0.018* | |
B4B | 0.19668 (18) | 0.5738 (2) | 0.1338 (2) | 0.0145 (4) | |
H4B | 0.1759 | 0.6254 | 0.0798 | 0.017* | |
B5B | 0.20080 (19) | 0.6200 (2) | 0.2700 (2) | 0.0150 (4) | |
H5B | 0.1828 | 0.7025 | 0.3069 | 0.018* | |
B6B | 0.3017 (2) | 0.5555 (2) | 0.3362 (2) | 0.0154 (4) | |
H6B | 0.3526 | 0.5939 | 0.4172 | 0.018* | |
B7B | 0.2607 (2) | 0.4226 (2) | 0.2954 (2) | 0.0164 (5) | |
H7B | 0.2838 | 0.3716 | 0.3497 | 0.020* | |
B8B | 0.25714 (19) | 0.3759 (2) | 0.1588 (2) | 0.0161 (5) | |
H8B | 0.2778 | 0.2942 | 0.1221 | 0.019* | |
B9B | 0.15538 (19) | 0.4405 (2) | 0.0924 (2) | 0.0160 (5) | |
H9B | 0.1062 | 0.4022 | 0.0107 | 0.019* | |
B10B | 0.09645 (18) | 0.5266 (2) | 0.1895 (2) | 0.0157 (5) | |
H10B | 0.0070 | 0.5458 | 0.1726 | 0.019* | |
B11B | 0.16135 (19) | 0.5154 (2) | 0.3148 (2) | 0.0146 (4) | |
H11B | 0.1160 | 0.5270 | 0.3818 | 0.018* | |
B12B | 0.13368 (18) | 0.4043 (2) | 0.2050 (2) | 0.0139 (4) | |
H12B | 0.0696 | 0.3413 | 0.1984 | 0.017* | |
Hg2 | 0.943757 (5) | 0.191399 (6) | 0.245883 (6) | 0.00996 (2) | |
C1C | 1.06798 (15) | 0.08810 (16) | 0.24089 (17) | 0.0107 (4) | |
C2C | 1.04445 (17) | −0.02572 (18) | 0.2566 (2) | 0.0157 (4) | |
H2C | 0.9642 | −0.0454 | 0.2775 | 0.019* | |
B3C | 1.1370 (2) | 0.0594 (2) | 0.3521 (2) | 0.0171 (5) | |
H3C | 1.1246 | 0.0979 | 0.4344 | 0.021* | |
B4C | 1.20466 (19) | 0.1240 (2) | 0.2813 (2) | 0.0163 (5) | |
H4C | 1.2392 | 0.2068 | 0.3168 | 0.020* | |
B5C | 1.14393 (18) | 0.0775 (2) | 0.1467 (2) | 0.0146 (4) | |
H5C | 1.1379 | 0.1290 | 0.0923 | 0.018* | |
B6C | 1.03794 (19) | −0.0165 (2) | 0.1334 (2) | 0.0158 (5) | |
H6C | 0.9597 | −0.0281 | 0.0710 | 0.019* | |
B7C | 1.0985 (2) | −0.1210 (2) | 0.1749 (3) | 0.0197 (5) | |
H7C | 1.0616 | −0.2031 | 0.1399 | 0.024* | |
B8C | 1.1605 (2) | −0.0732 (2) | 0.3104 (2) | 0.0197 (5) | |
H8C | 1.1651 | −0.1236 | 0.3658 | 0.024* | |
B9C | 1.2658 (2) | 0.0208 (2) | 0.3242 (2) | 0.0188 (5) | |
H9C | 1.3425 | 0.0335 | 0.3886 | 0.023* | |
B10C | 1.27050 (19) | 0.0316 (2) | 0.1969 (2) | 0.0172 (5) | |
H10C | 1.3506 | 0.0514 | 0.1759 | 0.021* | |
B11C | 1.1666 (2) | −0.0552 (2) | 0.1047 (2) | 0.0179 (5) | |
H11C | 1.1766 | −0.0934 | 0.0216 | 0.022* | |
B12C | 1.24200 (19) | −0.0909 (2) | 0.2143 (2) | 0.0171 (5) | |
H12C | 1.3027 | −0.1536 | 0.2046 | 0.021* | |
C1D | 0.81591 (15) | 0.28938 (16) | 0.23029 (17) | 0.0112 (4) | |
C2D | 0.84531 (15) | 0.41114 (17) | 0.24228 (18) | 0.0118 (4) | |
H2D | 0.9341 | 0.4434 | 0.2664 | 0.014* | |
B3D | 0.78843 (18) | 0.38116 (19) | 0.3364 (2) | 0.0131 (4) | |
H3D | 0.8322 | 0.3907 | 0.4206 | 0.016* | |
B4D | 0.69340 (18) | 0.2757 (2) | 0.2656 (2) | 0.0138 (4) | |
H4D | 0.6724 | 0.2142 | 0.3029 | 0.017* | |
B5D | 0.70285 (17) | 0.2444 (2) | 0.1318 (2) | 0.0126 (4) | |
H5D | 0.6880 | 0.1621 | 0.0799 | 0.015* | |
B6D | 0.80493 (18) | 0.3300 (2) | 0.1189 (2) | 0.0128 (4) | |
H6D | 0.8597 | 0.3056 | 0.0596 | 0.015* | |
B7D | 0.75953 (18) | 0.4572 (2) | 0.1539 (2) | 0.0136 (4) | |
H7D | 0.7834 | 0.5183 | 0.1172 | 0.016* | |
B8D | 0.74900 (19) | 0.4882 (2) | 0.2878 (2) | 0.0137 (4) | |
H8D | 0.7657 | 0.5702 | 0.3402 | 0.016* | |
B9D | 0.64803 (19) | 0.4023 (2) | 0.3010 (2) | 0.0136 (4) | |
H9D | 0.5954 | 0.4264 | 0.3622 | 0.016* | |
B10D | 0.59436 (18) | 0.3177 (2) | 0.1745 (2) | 0.0140 (4) | |
H10D | 0.5056 | 0.2853 | 0.1508 | 0.017* | |
B11D | 0.66402 (18) | 0.3513 (2) | 0.0833 (2) | 0.0135 (4) | |
H11D | 0.6223 | 0.3412 | −0.0015 | 0.016* | |
B12D | 0.62963 (18) | 0.4493 (2) | 0.1882 (2) | 0.0140 (4) | |
H12D | 0.5644 | 0.5051 | 0.1735 | 0.017* | |
C1' | 0.5154 (2) | 0.7531 (2) | 0.5390 (2) | 0.0281 (6) | |
H1'A | 0.5674 | 0.7997 | 0.5949 | 0.034* | |
H1'B | 0.4720 | 0.7152 | 0.5702 | 0.034* | |
Cl1 | 0.42779 (5) | 0.82521 (6) | 0.46934 (6) | 0.02837 (14) | |
Cl2 | 0.58761 (5) | 0.66645 (6) | 0.45757 (6) | 0.02772 (14) | |
C2' | 1.0260 (3) | 0.2807 (2) | 0.5468 (2) | 0.0297 (6) | |
H2'B | 1.0051 | 0.3315 | 0.6041 | 0.036* | |
H2'A | 1.0839 | 0.2432 | 0.5760 | 0.036* | |
Cl3 | 0.91120 (6) | 0.19435 (6) | 0.47796 (6) | 0.02991 (14) | |
Cl4 | 1.07596 (5) | 0.34380 (6) | 0.46492 (5) | 0.02740 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg1 | 0.00886 (3) | 0.00956 (4) | 0.01435 (4) | −0.00171 (2) | 0.00235 (2) | 0.00370 (3) |
C1A | 0.0098 (7) | 0.0086 (9) | 0.0180 (11) | −0.0012 (6) | 0.0029 (7) | 0.0029 (7) |
C2A | 0.0177 (10) | 0.0192 (13) | 0.0413 (17) | 0.0028 (8) | 0.0110 (10) | 0.0136 (11) |
B3A | 0.0147 (9) | 0.0162 (12) | 0.0163 (12) | −0.0005 (8) | 0.0060 (8) | 0.0014 (9) |
B4A | 0.0086 (8) | 0.0151 (12) | 0.0267 (14) | 0.0009 (8) | 0.0023 (8) | 0.0094 (10) |
B5A | 0.0204 (11) | 0.0181 (13) | 0.0153 (13) | −0.0080 (9) | 0.0013 (9) | 0.0021 (10) |
B6A | 0.0092 (9) | 0.0085 (11) | 0.0305 (15) | −0.0013 (7) | 0.0045 (8) | 0.0046 (9) |
B7A | 0.0120 (9) | 0.0127 (12) | 0.0314 (15) | 0.0004 (8) | 0.0047 (9) | 0.0089 (10) |
B8A | 0.0160 (10) | 0.0209 (14) | 0.0172 (13) | −0.0026 (9) | 0.0019 (8) | 0.0082 (10) |
B9A | 0.0118 (9) | 0.0161 (13) | 0.0284 (15) | 0.0008 (8) | 0.0074 (9) | 0.0077 (10) |
B10A | 0.0135 (10) | 0.0204 (14) | 0.0232 (14) | −0.0043 (9) | −0.0018 (9) | 0.0099 (11) |
B11A | 0.0209 (11) | 0.0140 (13) | 0.0216 (14) | −0.0071 (9) | 0.0055 (9) | −0.0053 (10) |
B12A | 0.0099 (8) | 0.0134 (12) | 0.0223 (13) | −0.0018 (8) | 0.0039 (8) | 0.0073 (9) |
C1B | 0.0090 (7) | 0.0099 (9) | 0.0145 (10) | −0.0006 (6) | 0.0014 (6) | 0.0041 (7) |
C2B | 0.0092 (7) | 0.0120 (10) | 0.0204 (11) | 0.0004 (6) | 0.0013 (7) | 0.0079 (8) |
B3B | 0.0133 (9) | 0.0153 (12) | 0.0149 (12) | −0.0016 (8) | 0.0040 (8) | 0.0028 (9) |
B4B | 0.0105 (8) | 0.0163 (12) | 0.0184 (12) | 0.0004 (8) | 0.0007 (8) | 0.0094 (9) |
B5B | 0.0144 (9) | 0.0120 (12) | 0.0207 (13) | 0.0014 (8) | 0.0081 (8) | 0.0051 (9) |
B6B | 0.0171 (10) | 0.0156 (12) | 0.0137 (12) | −0.0035 (8) | 0.0023 (8) | 0.0049 (9) |
B7B | 0.0145 (9) | 0.0155 (13) | 0.0219 (13) | −0.0015 (8) | 0.0007 (8) | 0.0117 (10) |
B8B | 0.0137 (9) | 0.0103 (12) | 0.0229 (14) | −0.0002 (8) | 0.0042 (8) | 0.0022 (9) |
B9B | 0.0128 (9) | 0.0175 (13) | 0.0165 (12) | −0.0041 (8) | −0.0001 (8) | 0.0051 (9) |
B10B | 0.0098 (9) | 0.0163 (13) | 0.0227 (13) | 0.0008 (8) | 0.0035 (8) | 0.0084 (10) |
B11B | 0.0158 (9) | 0.0128 (12) | 0.0161 (12) | −0.0004 (8) | 0.0049 (8) | 0.0042 (9) |
B12B | 0.0101 (8) | 0.0118 (11) | 0.0206 (13) | −0.0023 (7) | 0.0026 (8) | 0.0061 (9) |
Hg2 | 0.00871 (3) | 0.01004 (4) | 0.01127 (4) | 0.00291 (2) | 0.00151 (2) | 0.00351 (3) |
C1C | 0.0084 (7) | 0.0110 (10) | 0.0129 (10) | 0.0020 (6) | 0.0021 (6) | 0.0035 (7) |
C2C | 0.0148 (8) | 0.0114 (10) | 0.0251 (12) | 0.0037 (7) | 0.0094 (8) | 0.0085 (8) |
B3C | 0.0196 (10) | 0.0184 (13) | 0.0148 (12) | 0.0087 (9) | 0.0041 (8) | 0.0065 (9) |
B4C | 0.0116 (9) | 0.0110 (12) | 0.0233 (13) | 0.0015 (8) | −0.0010 (8) | 0.0031 (9) |
B5C | 0.0124 (9) | 0.0192 (13) | 0.0153 (12) | 0.0039 (8) | 0.0050 (8) | 0.0083 (9) |
B6C | 0.0130 (9) | 0.0165 (12) | 0.0156 (12) | 0.0021 (8) | 0.0025 (8) | 0.0010 (9) |
B7C | 0.0169 (10) | 0.0098 (12) | 0.0323 (16) | 0.0020 (8) | 0.0081 (10) | 0.0032 (10) |
B8C | 0.0208 (11) | 0.0187 (14) | 0.0276 (15) | 0.0087 (10) | 0.0114 (10) | 0.0150 (11) |
B9C | 0.0153 (10) | 0.0184 (13) | 0.0228 (14) | 0.0061 (9) | 0.0010 (9) | 0.0079 (10) |
B10C | 0.0128 (9) | 0.0149 (12) | 0.0277 (14) | 0.0036 (8) | 0.0076 (9) | 0.0096 (10) |
B11C | 0.0155 (10) | 0.0175 (13) | 0.0214 (14) | 0.0061 (9) | 0.0086 (9) | 0.0028 (10) |
B12C | 0.0139 (9) | 0.0131 (12) | 0.0265 (14) | 0.0053 (8) | 0.0070 (9) | 0.0070 (10) |
C1D | 0.0084 (7) | 0.0110 (10) | 0.0152 (10) | 0.0030 (6) | 0.0020 (6) | 0.0055 (7) |
C2D | 0.0091 (7) | 0.0109 (10) | 0.0159 (10) | 0.0007 (6) | 0.0009 (6) | 0.0056 (7) |
B3D | 0.0134 (9) | 0.0134 (12) | 0.0130 (11) | 0.0038 (8) | 0.0028 (7) | 0.0042 (8) |
B4D | 0.0125 (9) | 0.0137 (12) | 0.0173 (12) | 0.0020 (8) | 0.0051 (8) | 0.0060 (9) |
B5D | 0.0093 (8) | 0.0132 (11) | 0.0150 (11) | 0.0009 (7) | 0.0018 (7) | 0.0038 (8) |
B6D | 0.0100 (8) | 0.0157 (12) | 0.0136 (11) | 0.0019 (7) | 0.0018 (7) | 0.0059 (9) |
B7D | 0.0103 (8) | 0.0135 (12) | 0.0179 (12) | 0.0023 (7) | 0.0017 (8) | 0.0069 (9) |
B8D | 0.0130 (9) | 0.0123 (12) | 0.0160 (12) | 0.0017 (8) | 0.0014 (8) | 0.0053 (9) |
B9D | 0.0126 (9) | 0.0144 (12) | 0.0149 (12) | 0.0027 (8) | 0.0055 (8) | 0.0039 (9) |
B10D | 0.0093 (8) | 0.0148 (12) | 0.0191 (12) | 0.0013 (7) | 0.0028 (8) | 0.0066 (9) |
B11D | 0.0092 (8) | 0.0165 (12) | 0.0143 (11) | 0.0015 (8) | −0.0011 (7) | 0.0055 (9) |
B12D | 0.0087 (8) | 0.0149 (12) | 0.0193 (12) | 0.0021 (7) | 0.0022 (7) | 0.0067 (9) |
C1' | 0.0329 (13) | 0.0329 (16) | 0.0148 (13) | −0.0088 (11) | 0.0008 (10) | 0.0037 (11) |
Cl1 | 0.0285 (3) | 0.0277 (4) | 0.0271 (3) | 0.0033 (2) | 0.0103 (2) | 0.0011 (3) |
Cl2 | 0.0230 (3) | 0.0340 (4) | 0.0277 (3) | 0.0042 (2) | −0.0002 (2) | 0.0149 (3) |
C2' | 0.0440 (15) | 0.0323 (16) | 0.0127 (12) | 0.0154 (12) | 0.0032 (10) | 0.0078 (10) |
Cl3 | 0.0374 (3) | 0.0334 (4) | 0.0293 (4) | 0.0084 (3) | 0.0172 (3) | 0.0186 (3) |
Cl4 | 0.0236 (3) | 0.0328 (4) | 0.0199 (3) | −0.0035 (2) | −0.0037 (2) | 0.0033 (3) |
Hg1—C1A | 2.096 (2) | C1C—B5C | 1.712 (3) |
Hg1—C1B | 2.097 (2) | C1C—B6C | 1.717 (3) |
C1A—B6A | 1.686 (3) | C1C—B3C | 1.730 (3) |
C1A—C2A | 1.691 (4) | C2C—B6C | 1.698 (4) |
C1A—B4A | 1.709 (3) | C2C—B7C | 1.699 (4) |
C1A—B5A | 1.721 (3) | C2C—B8C | 1.702 (3) |
C1A—B3A | 1.730 (3) | C2C—B3C | 1.715 (4) |
C2A—B6A | 1.688 (4) | C2C—H2C | 1.1400 |
C2A—B7A | 1.739 (4) | B3C—B9C | 1.771 (4) |
C2A—B8A | 1.741 (4) | B3C—B8C | 1.778 (4) |
C2A—B3A | 1.745 (4) | B3C—B4C | 1.780 (4) |
C2A—H2A | 1.1400 | B3C—H3C | 1.1400 |
B3A—B9A | 1.773 (4) | B4C—B5C | 1.774 (4) |
B3A—B4A | 1.776 (4) | B4C—B10C | 1.779 (4) |
B3A—B8A | 1.782 (4) | B4C—B9C | 1.779 (4) |
B3A—H3A | 1.1400 | B4C—H4C | 1.1400 |
B4A—B10A | 1.776 (4) | B5C—B11C | 1.779 (4) |
B4A—B5A | 1.777 (4) | B5C—B6C | 1.779 (4) |
B4A—B9A | 1.780 (4) | B5C—B10C | 1.779 (3) |
B4A—H4A | 1.1400 | B5C—H5C | 1.1400 |
B5A—B6A | 1.741 (4) | B6C—B11C | 1.774 (3) |
B5A—B10A | 1.768 (4) | B6C—B7C | 1.782 (4) |
B5A—B11A | 1.777 (4) | B6C—H6C | 1.1400 |
B5A—H5A | 1.1400 | B7C—B12C | 1.776 (4) |
B6A—B7A | 1.729 (4) | B7C—B11C | 1.787 (4) |
B6A—B11A | 1.729 (4) | B7C—B8C | 1.790 (5) |
B6A—H6A | 1.1400 | B7C—H7C | 1.1400 |
B7A—B12A | 1.765 (3) | B8C—B9C | 1.770 (4) |
B7A—B11A | 1.777 (4) | B8C—B12C | 1.774 (4) |
B7A—B8A | 1.792 (4) | B8C—H8C | 1.1400 |
B7A—H7A | 1.1400 | B9C—B10C | 1.788 (4) |
B8A—B12A | 1.781 (4) | B9C—B12C | 1.793 (4) |
B8A—B9A | 1.784 (4) | B9C—H9C | 1.1400 |
B8A—H8A | 1.1400 | B10C—B12C | 1.784 (4) |
B9A—B10A | 1.789 (4) | B10C—B11C | 1.785 (4) |
B9A—B12A | 1.788 (4) | B10C—H10C | 1.1400 |
B9A—H9A | 1.1400 | B11C—B12C | 1.784 (4) |
B10A—B12A | 1.780 (4) | B11C—H11C | 1.1400 |
B10A—B11A | 1.783 (4) | B12C—H12C | 1.1400 |
B10A—H10A | 1.1400 | C1D—C2D | 1.647 (3) |
B11A—B12A | 1.768 (4) | C1D—B4D | 1.711 (3) |
B11A—H11A | 1.1400 | C1D—B5D | 1.721 (3) |
B12A—H12A | 1.1400 | C1D—B3D | 1.725 (3) |
C1B—C2B | 1.651 (3) | C1D—B6D | 1.727 (3) |
C1B—B5B | 1.707 (3) | C2D—B8D | 1.696 (3) |
C1B—B4B | 1.720 (3) | C2D—B7D | 1.700 (3) |
C1B—B6B | 1.729 (4) | C2D—B3D | 1.713 (3) |
C1B—B3B | 1.740 (4) | C2D—B6D | 1.716 (3) |
C2B—B7B | 1.689 (3) | C2D—H2D | 1.1400 |
C2B—B8B | 1.702 (4) | B3D—B9D | 1.769 (3) |
C2B—B6B | 1.703 (4) | B3D—B4D | 1.779 (4) |
C2B—B3B | 1.716 (4) | B3D—B8D | 1.785 (4) |
C2B—H2B | 1.1400 | B3D—H3D | 1.1400 |
B3B—B9B | 1.777 (3) | B4D—B5D | 1.780 (4) |
B3B—B4B | 1.781 (3) | B4D—B9D | 1.781 (4) |
B3B—B8B | 1.784 (4) | B4D—B10D | 1.782 (3) |
B3B—H3B | 1.1400 | B4D—H4D | 1.1400 |
B4B—B5B | 1.777 (4) | B5D—B10D | 1.779 (3) |
B4B—B10B | 1.778 (4) | B5D—B11D | 1.781 (4) |
B4B—B9B | 1.782 (4) | B5D—B6D | 1.782 (4) |
B4B—H4B | 1.1400 | B5D—H5D | 1.1400 |
B5B—B6B | 1.776 (4) | B6D—B11D | 1.776 (3) |
B5B—B10B | 1.780 (4) | B6D—B7D | 1.789 (3) |
B5B—B11B | 1.789 (4) | B6D—H6D | 1.1400 |
B5B—H5B | 1.1400 | B7D—B12D | 1.780 (3) |
B6B—B11B | 1.773 (3) | B7D—B8D | 1.785 (4) |
B6B—B7B | 1.777 (4) | B7D—B11D | 1.787 (4) |
B6B—H6B | 1.1400 | B7D—H7D | 1.1400 |
B7B—B12B | 1.775 (3) | B8D—B12D | 1.774 (4) |
B7B—B11B | 1.777 (4) | B8D—B9D | 1.777 (4) |
B7B—B8B | 1.784 (4) | B8D—H8D | 1.1400 |
B7B—H7B | 1.1400 | B9D—B10D | 1.788 (4) |
B8B—B12B | 1.779 (3) | B9D—B12D | 1.790 (4) |
B8B—B9B | 1.786 (4) | B9D—H9D | 1.1400 |
B8B—H8B | 1.1400 | B10D—B12D | 1.787 (4) |
B9B—B10B | 1.790 (4) | B10D—B11D | 1.793 (4) |
B9B—B12B | 1.794 (4) | B10D—H10D | 1.1400 |
B9B—H9B | 1.1400 | B11D—B12D | 1.791 (4) |
B10B—B12B | 1.780 (4) | B11D—H11D | 1.1400 |
B10B—B11B | 1.784 (4) | B12D—H12D | 1.1400 |
B10B—H10B | 1.1400 | C1'—Cl2 | 1.766 (3) |
B11B—B12B | 1.787 (4) | C1'—Cl1 | 1.777 (3) |
B11B—H11B | 1.1400 | C1'—H1'A | 0.9700 |
B12B—H12B | 1.1400 | C1'—H1'B | 0.9700 |
Hg2—C1C | 2.0940 (19) | C2'—Cl4 | 1.770 (3) |
Hg2—C1D | 2.0976 (19) | C2'—Cl3 | 1.778 (3) |
C1C—C2C | 1.646 (3) | C2'—H2'B | 0.9700 |
C1C—B4C | 1.710 (3) | C2'—H2'A | 0.9700 |
C1A—Hg1—C1B | 175.74 (9) | B5C—C1C—B6C | 62.53 (15) |
B6A—C1A—C2A | 59.98 (16) | C2C—C1C—B3C | 60.99 (15) |
B6A—C1A—B4A | 111.36 (17) | B4C—C1C—B3C | 62.32 (15) |
C2A—C1A—B4A | 111.25 (17) | B5C—C1C—B3C | 113.91 (15) |
B6A—C1A—B5A | 61.48 (15) | B6C—C1C—B3C | 113.62 (17) |
C2A—C1A—B5A | 111.05 (18) | C2C—C1C—Hg2 | 119.38 (12) |
B4A—C1A—B5A | 62.43 (16) | B4C—C1C—Hg2 | 124.03 (14) |
B6A—C1A—B3A | 110.76 (19) | B5C—C1C—Hg2 | 117.90 (14) |
C2A—C1A—B3A | 61.32 (15) | B6C—C1C—Hg2 | 112.51 (13) |
B4A—C1A—B3A | 62.17 (15) | B3C—C1C—Hg2 | 121.77 (14) |
B5A—C1A—B3A | 113.38 (17) | C1C—C2C—B6C | 61.75 (15) |
B6A—C1A—Hg1 | 119.51 (14) | C1C—C2C—B7C | 112.85 (18) |
C2A—C1A—Hg1 | 116.68 (13) | B6C—C2C—B7C | 63.29 (16) |
B4A—C1A—Hg1 | 122.20 (15) | C1C—C2C—B8C | 112.25 (17) |
B5A—C1A—Hg1 | 121.93 (16) | B6C—C2C—B8C | 115.74 (17) |
B3A—C1A—Hg1 | 117.44 (15) | B7C—C2C—B8C | 63.51 (16) |
B6A—C2A—C1A | 59.85 (16) | C1C—C2C—B3C | 61.90 (14) |
B6A—C2A—B7A | 60.58 (17) | B6C—C2C—B3C | 115.38 (18) |
C1A—C2A—B7A | 109.2 (2) | B7C—C2C—B3C | 115.91 (17) |
B6A—C2A—B8A | 110.1 (2) | B8C—C2C—B3C | 62.71 (16) |
C1A—C2A—B8A | 109.17 (17) | C1C—C2C—H2C | 120.2 |
B7A—C2A—B8A | 61.97 (16) | B6C—C2C—H2C | 117.0 |
B6A—C2A—B3A | 109.93 (19) | B7C—C2C—H2C | 117.2 |
C1A—C2A—B3A | 60.44 (14) | B8C—C2C—H2C | 117.8 |
B7A—C2A—B3A | 111.97 (17) | B3C—C2C—H2C | 117.1 |
B8A—C2A—B3A | 61.49 (15) | C2C—B3C—C1C | 57.10 (14) |
B6A—C2A—H2A | 121.1 | C2C—B3C—B9C | 103.86 (18) |
C1A—C2A—H2A | 121.8 | C1C—B3C—B9C | 104.83 (18) |
B7A—C2A—H2A | 119.7 | C2C—B3C—B8C | 58.30 (15) |
B8A—C2A—H2A | 120.2 | C1C—B3C—B8C | 104.86 (19) |
B3A—C2A—H2A | 119.7 | B9C—B3C—B8C | 59.82 (16) |
C1A—B3A—C2A | 58.24 (14) | C2C—B3C—B4C | 103.61 (18) |
C1A—B3A—B9A | 105.21 (19) | C1C—B3C—B4C | 58.29 (14) |
C2A—B3A—B9A | 106.05 (19) | B9C—B3C—B4C | 60.12 (15) |
C1A—B3A—B4A | 58.31 (14) | B8C—B3C—B4C | 107.65 (18) |
C2A—B3A—B4A | 105.69 (19) | C2C—B3C—H3C | 125.3 |
B9A—B3A—B4A | 60.22 (15) | C1C—B3C—H3C | 124.3 |
C1A—B3A—B8A | 105.57 (18) | B9C—B3C—H3C | 123.1 |
C2A—B3A—B8A | 59.14 (15) | B8C—B3C—H3C | 122.2 |
B9A—B3A—B8A | 60.23 (15) | B4C—B3C—H3C | 122.6 |
B4A—B3A—B8A | 108.24 (19) | C1C—B4C—B5C | 58.83 (13) |
C1A—B3A—H3A | 124.2 | C1C—B4C—B10C | 105.25 (18) |
C2A—B3A—H3A | 123.4 | B5C—B4C—B10C | 60.10 (15) |
B9A—B3A—H3A | 122.5 | C1C—B4C—B9C | 105.35 (18) |
B4A—B3A—H3A | 122.1 | B5C—B4C—B9C | 108.45 (19) |
B8A—B3A—H3A | 121.8 | B10C—B4C—B9C | 60.33 (15) |
C1A—B4A—B10A | 105.50 (18) | C1C—B4C—B3C | 59.40 (14) |
C1A—B4A—B3A | 59.52 (14) | B5C—B4C—B3C | 108.55 (19) |
B10A—B4A—B3A | 108.25 (19) | B10C—B4C—B3C | 108.20 (19) |
C1A—B4A—B5A | 59.12 (14) | B9C—B4C—B3C | 59.69 (15) |
B10A—B4A—B5A | 59.69 (16) | C1C—B4C—H4C | 124.2 |
B3A—B4A—B5A | 108.54 (17) | B5C—B4C—H4C | 121.2 |
C1A—B4A—B9A | 105.83 (17) | B10C—B4C—H4C | 122.2 |
B10A—B4A—B9A | 60.42 (16) | B9C—B4C—H4C | 122.2 |
B3A—B4A—B9A | 59.81 (15) | B3C—B4C—H4C | 121.3 |
B5A—B4A—B9A | 108.24 (19) | C1C—B5C—B4C | 58.72 (14) |
C1A—B4A—H4A | 123.8 | C1C—B5C—B11C | 105.25 (18) |
B10A—B4A—H4A | 122.2 | B4C—B5C—B11C | 108.26 (18) |
B3A—B4A—H4A | 121.2 | C1C—B5C—B6C | 58.88 (14) |
B5A—B4A—H4A | 121.4 | B4C—B5C—B6C | 107.82 (19) |
B9A—B4A—H4A | 122.0 | B11C—B5C—B6C | 59.81 (15) |
C1A—B5A—B6A | 58.27 (14) | C1C—B5C—B10C | 105.15 (18) |
C1A—B5A—B10A | 105.3 (2) | B4C—B5C—B10C | 60.09 (15) |
B6A—B5A—B10A | 105.9 (2) | B11C—B5C—B10C | 60.22 (15) |
C1A—B5A—B4A | 58.45 (14) | B6C—B5C—B10C | 107.87 (18) |
B6A—B5A—B4A | 105.6 (2) | C1C—B5C—H5C | 124.4 |
B10A—B5A—B4A | 60.12 (16) | B4C—B5C—H5C | 121.5 |
C1A—B5A—B11A | 105.5 (2) | B11C—B5C—H5C | 122.1 |
B6A—B5A—B11A | 58.85 (16) | B6C—B5C—H5C | 121.7 |
B10A—B5A—B11A | 60.38 (16) | B10C—B5C—H5C | 122.2 |
B4A—B5A—B11A | 108.2 (2) | C2C—B6C—C1C | 57.64 (14) |
C1A—B5A—H5A | 124.0 | C2C—B6C—B11C | 104.40 (17) |
B6A—B5A—H5A | 123.6 | C1C—B6C—B11C | 105.23 (17) |
B10A—B5A—H5A | 122.5 | C2C—B6C—B5C | 104.43 (18) |
B4A—B5A—H5A | 122.1 | C1C—B6C—B5C | 58.59 (14) |
B11A—B5A—H5A | 121.9 | B11C—B6C—B5C | 60.08 (15) |
C1A—B6A—C2A | 60.17 (15) | C2C—B6C—B7C | 58.38 (15) |
C1A—B6A—B7A | 109.9 (2) | C1C—B6C—B7C | 105.59 (18) |
C2A—B6A—B7A | 61.18 (17) | B11C—B6C—B7C | 60.32 (15) |
C1A—B6A—B11A | 109.31 (17) | B5C—B6C—B7C | 108.36 (17) |
C2A—B6A—B11A | 110.5 (2) | C2C—B6C—H6C | 124.9 |
B7A—B6A—B11A | 61.86 (17) | C1C—B6C—H6C | 123.9 |
C1A—B6A—B5A | 60.25 (14) | B11C—B6C—H6C | 122.9 |
C2A—B6A—B5A | 110.20 (19) | B5C—B6C—H6C | 122.2 |
B7A—B6A—B5A | 112.21 (17) | B7C—B6C—H6C | 121.7 |
B11A—B6A—B5A | 61.61 (16) | C2C—B7C—B12C | 103.9 (2) |
C1A—B6A—H6A | 121.6 | C2C—B7C—B6C | 58.32 (14) |
C2A—B6A—H6A | 120.6 | B12C—B7C—B6C | 107.58 (19) |
B7A—B6A—H6A | 119.3 | C2C—B7C—B11C | 103.81 (19) |
B11A—B6A—H6A | 120.1 | B12C—B7C—B11C | 60.12 (15) |
B5A—B6A—H6A | 119.7 | B6C—B7C—B11C | 59.61 (15) |
B6A—B7A—C2A | 58.25 (16) | C2C—B7C—B8C | 58.33 (15) |
B6A—B7A—B12A | 105.55 (18) | B12C—B7C—B8C | 59.68 (16) |
C2A—B7A—B12A | 105.69 (18) | B6C—B7C—B8C | 107.41 (19) |
B6A—B7A—B11A | 59.06 (16) | B11C—B7C—B8C | 107.6 (2) |
C2A—B7A—B11A | 105.9 (2) | C2C—B7C—H7C | 125.4 |
B12A—B7A—B11A | 59.89 (15) | B12C—B7C—H7C | 122.6 |
B6A—B7A—B8A | 105.89 (19) | B6C—B7C—H7C | 121.8 |
C2A—B7A—B8A | 59.06 (15) | B11C—B7C—H7C | 122.7 |
B12A—B7A—B8A | 60.09 (15) | B8C—B7C—H7C | 121.8 |
B11A—B7A—B8A | 108.19 (18) | C2C—B8C—B9C | 104.44 (18) |
B6A—B7A—H7A | 123.7 | C2C—B8C—B12C | 103.80 (19) |
C2A—B7A—H7A | 123.6 | B9C—B8C—B12C | 60.80 (16) |
B12A—B7A—H7A | 122.7 | C2C—B8C—B3C | 58.99 (15) |
B11A—B7A—H7A | 121.9 | B9C—B8C—B3C | 59.88 (16) |
B8A—B7A—H7A | 121.8 | B12C—B8C—B3C | 108.5 (2) |
C2A—B8A—B12A | 104.9 (2) | C2C—B8C—B7C | 58.16 (15) |
C2A—B8A—B3A | 59.37 (15) | B9C—B8C—B7C | 108.6 (2) |
B12A—B8A—B3A | 107.40 (19) | B12C—B8C—B7C | 59.75 (16) |
C2A—B8A—B9A | 105.75 (19) | B3C—B8C—B7C | 108.39 (19) |
B12A—B8A—B9A | 60.22 (15) | C2C—B8C—H8C | 125.4 |
B3A—B8A—B9A | 59.62 (15) | B9C—B8C—H8C | 122.0 |
C2A—B8A—B7A | 58.97 (16) | B12C—B8C—H8C | 122.4 |
B12A—B8A—B7A | 59.21 (15) | B3C—B8C—H8C | 121.1 |
B3A—B8A—B7A | 107.83 (19) | B7C—B8C—H8C | 121.4 |
B9A—B8A—B7A | 107.8 (2) | B8C—B9C—B3C | 60.29 (15) |
C2A—B8A—H8A | 123.9 | B8C—B9C—B4C | 108.06 (17) |
B12A—B8A—H8A | 122.8 | B3C—B9C—B4C | 60.18 (15) |
B3A—B8A—H8A | 121.7 | B8C—B9C—B10C | 107.8 (2) |
B9A—B8A—H8A | 122.1 | B3C—B9C—B10C | 108.19 (17) |
B7A—B8A—H8A | 121.9 | B4C—B9C—B10C | 59.84 (16) |
B3A—B9A—B4A | 59.97 (15) | B8C—B9C—B12C | 59.72 (16) |
B3A—B9A—B8A | 60.14 (15) | B3C—B9C—B12C | 107.97 (19) |
B4A—B9A—B8A | 107.98 (17) | B4C—B9C—B12C | 107.50 (19) |
B3A—B9A—B10A | 107.79 (19) | B10C—B9C—B12C | 59.76 (16) |
B4A—B9A—B10A | 59.68 (16) | B8C—B9C—H9C | 121.7 |
B8A—B9A—B10A | 107.96 (19) | B3C—B9C—H9C | 121.4 |
B3A—B9A—B12A | 107.49 (17) | B4C—B9C—H9C | 121.8 |
B4A—B9A—B12A | 107.12 (19) | B10C—B9C—H9C | 121.8 |
B8A—B9A—B12A | 59.82 (15) | B12C—B9C—H9C | 122.1 |
B10A—B9A—B12A | 59.70 (16) | B4C—B10C—B5C | 59.81 (14) |
B3A—B9A—H9A | 121.8 | B4C—B10C—B12C | 107.90 (19) |
B4A—B9A—H9A | 122.0 | B5C—B10C—B12C | 107.82 (18) |
B8A—B9A—H9A | 121.6 | B4C—B10C—B11C | 107.77 (16) |
B10A—B9A—H9A | 121.9 | B5C—B10C—B11C | 59.88 (15) |
B12A—B9A—H9A | 122.3 | B12C—B10C—B11C | 60.00 (16) |
B5A—B10A—B4A | 60.19 (15) | B4C—B10C—B9C | 59.83 (15) |
B5A—B10A—B12A | 107.56 (18) | B5C—B10C—B9C | 107.81 (17) |
B4A—B10A—B12A | 107.64 (19) | B12C—B10C—B9C | 60.28 (16) |
B5A—B10A—B11A | 60.07 (16) | B11C—B10C—B9C | 108.20 (19) |
B4A—B10A—B11A | 108.04 (17) | B4C—B10C—H10C | 121.9 |
B12A—B10A—B11A | 59.51 (16) | B5C—B10C—H10C | 121.9 |
B5A—B10A—B9A | 108.24 (18) | B12C—B10C—H10C | 121.7 |
B4A—B10A—B9A | 59.90 (16) | B11C—B10C—H10C | 121.7 |
B12A—B10A—B9A | 60.13 (16) | B9C—B10C—H10C | 121.6 |
B11A—B10A—B9A | 108.03 (19) | B6C—B11C—B5C | 60.11 (14) |
B5A—B10A—H10A | 121.6 | B6C—B11C—B12C | 107.56 (19) |
B4A—B10A—H10A | 121.8 | B5C—B11C—B12C | 107.8 (2) |
B12A—B10A—H10A | 122.1 | B6C—B11C—B10C | 107.84 (18) |
B11A—B10A—H10A | 121.8 | B5C—B11C—B10C | 59.89 (14) |
B9A—B10A—H10A | 121.5 | B12C—B11C—B10C | 59.98 (16) |
B6A—B11A—B12A | 105.4 (2) | B6C—B11C—B7C | 60.07 (15) |
B6A—B11A—B7A | 59.08 (16) | B5C—B11C—B7C | 108.19 (18) |
B12A—B11A—B7A | 59.70 (15) | B12C—B11C—B7C | 59.63 (16) |
B6A—B11A—B5A | 59.54 (15) | B10C—B11C—B7C | 107.8 (2) |
B12A—B11A—B5A | 107.7 (2) | B6C—B11C—H11C | 121.8 |
B7A—B11A—B5A | 108.27 (19) | B5C—B11C—H11C | 121.6 |
B6A—B11A—B10A | 105.78 (19) | B12C—B11C—H11C | 122.0 |
B12A—B11A—B10A | 60.18 (16) | B10C—B11C—H11C | 121.8 |
B7A—B11A—B10A | 108.1 (2) | B7C—B11C—H11C | 121.7 |
B5A—B11A—B10A | 59.56 (16) | B8C—B12C—B7C | 60.57 (16) |
B6A—B11A—H11A | 123.7 | B8C—B12C—B10C | 107.75 (19) |
B12A—B11A—H11A | 122.4 | B7C—B12C—B10C | 108.38 (18) |
B7A—B11A—H11A | 121.5 | B8C—B12C—B11C | 108.39 (17) |
B5A—B11A—H11A | 121.5 | B7C—B12C—B11C | 60.26 (16) |
B10A—B11A—H11A | 122.2 | B10C—B12C—B11C | 60.02 (16) |
B7A—B12A—B11A | 60.40 (16) | B8C—B12C—B9C | 59.48 (17) |
B7A—B12A—B10A | 108.74 (18) | B7C—B12C—B9C | 108.19 (18) |
B11A—B12A—B10A | 60.32 (17) | B10C—B12C—B9C | 59.96 (16) |
B7A—B12A—B8A | 60.70 (16) | B11C—B12C—B9C | 107.97 (18) |
B11A—B12A—B8A | 109.07 (17) | B8C—B12C—H12C | 121.7 |
B10A—B12A—B8A | 108.46 (19) | B7C—B12C—H12C | 121.2 |
B7A—B12A—B9A | 108.74 (18) | B10C—B12C—H12C | 121.8 |
B11A—B12A—B9A | 108.72 (19) | B11C—B12C—H12C | 121.5 |
B10A—B12A—B9A | 60.18 (16) | B9C—B12C—H12C | 121.9 |
B8A—B12A—B9A | 59.97 (15) | C2D—C1D—B4D | 109.96 (15) |
B7A—B12A—H12A | 121.1 | C2D—C1D—B5D | 109.84 (16) |
B11A—B12A—H12A | 121.1 | B4D—C1D—B5D | 62.48 (14) |
B10A—B12A—H12A | 121.5 | C2D—C1D—B3D | 61.00 (14) |
B8A—B12A—H12A | 121.2 | B4D—C1D—B3D | 62.36 (14) |
B9A—B12A—H12A | 121.5 | B5D—C1D—B3D | 113.89 (15) |
C2B—C1B—B5B | 109.28 (17) | C2D—C1D—B6D | 61.08 (14) |
C2B—C1B—B4B | 109.12 (17) | B4D—C1D—B6D | 113.94 (15) |
B5B—C1B—B4B | 62.44 (14) | B5D—C1D—B6D | 62.23 (14) |
C2B—C1B—B6B | 60.48 (15) | B3D—C1D—B6D | 114.08 (17) |
B5B—C1B—B6B | 62.26 (14) | C2D—C1D—Hg2 | 119.33 (12) |
B4B—C1B—B6B | 113.44 (16) | B4D—C1D—Hg2 | 123.89 (14) |
C2B—C1B—B3B | 60.72 (14) | B5D—C1D—Hg2 | 118.03 (14) |
B5B—C1B—B3B | 113.43 (16) | B3D—C1D—Hg2 | 121.66 (14) |
B4B—C1B—B3B | 61.95 (14) | B6D—C1D—Hg2 | 112.33 (13) |
B6B—C1B—B3B | 113.21 (18) | C1D—C2D—B8D | 112.53 (16) |
C2B—C1B—Hg1 | 119.78 (12) | C1D—C2D—B7D | 112.74 (16) |
B5B—C1B—Hg1 | 123.32 (15) | B8D—C2D—B7D | 63.43 (14) |
B4B—C1B—Hg1 | 119.41 (14) | C1D—C2D—B3D | 61.76 (14) |
B6B—C1B—Hg1 | 120.55 (14) | B8D—C2D—B3D | 63.15 (14) |
B3B—C1B—Hg1 | 114.23 (14) | B7D—C2D—B3D | 116.03 (15) |
C1B—C2B—B7B | 113.02 (16) | C1D—C2D—B6D | 61.77 (14) |
C1B—C2B—B8B | 113.09 (16) | B8D—C2D—B6D | 115.75 (16) |
B7B—C2B—B8B | 63.48 (16) | B7D—C2D—B6D | 63.16 (14) |
C1B—C2B—B6B | 62.02 (14) | B3D—C2D—B6D | 115.31 (17) |
B7B—C2B—B6B | 63.17 (16) | C1D—C2D—H2D | 120.3 |
B8B—C2B—B6B | 116.11 (17) | B8D—C2D—H2D | 117.6 |
C1B—C2B—B3B | 62.22 (14) | B7D—C2D—H2D | 117.4 |
B7B—C2B—B3B | 115.85 (17) | B3D—C2D—H2D | 117.0 |
B8B—C2B—B3B | 62.94 (15) | B6D—C2D—H2D | 117.1 |
B6B—C2B—B3B | 115.79 (17) | C2D—B3D—C1D | 57.24 (13) |
C1B—C2B—H2B | 119.8 | C2D—B3D—B9D | 103.83 (17) |
B7B—C2B—H2B | 117.5 | C1D—B3D—B9D | 104.94 (17) |
B8B—C2B—H2B | 117.4 | C2D—B3D—B4D | 103.91 (18) |
B6B—C2B—H2B | 116.8 | C1D—B3D—B4D | 58.44 (13) |
B3B—C2B—H2B | 116.9 | B9D—B3D—B4D | 60.24 (14) |
C2B—B3B—C1B | 57.06 (13) | C2D—B3D—B8D | 57.95 (13) |
C2B—B3B—B9B | 103.92 (18) | C1D—B3D—B8D | 104.73 (17) |
C1B—B3B—B9B | 105.19 (17) | B9D—B3D—B8D | 59.98 (14) |
C2B—B3B—B4B | 103.52 (18) | B4D—B3D—B8D | 107.89 (17) |
C1B—B3B—B4B | 58.47 (13) | C2D—B3D—H3D | 125.3 |
B9B—B3B—B4B | 60.13 (14) | C1D—B3D—H3D | 124.3 |
C2B—B3B—B8B | 58.15 (15) | B9D—B3D—H3D | 123.0 |
C1B—B3B—B8B | 105.06 (18) | B4D—B3D—H3D | 122.3 |
B9B—B3B—B8B | 60.18 (14) | B8D—B3D—H3D | 122.2 |
B4B—B3B—B8B | 107.91 (17) | C1D—B4D—B3D | 59.20 (14) |
C2B—B3B—H3B | 125.5 | C1D—B4D—B5D | 59.03 (13) |
C1B—B3B—H3B | 124.2 | B3D—B4D—B5D | 108.49 (18) |
B9B—B3B—H3B | 122.9 | C1D—B4D—B9D | 105.04 (17) |
B4B—B3B—H3B | 122.5 | B3D—B4D—B9D | 59.60 (14) |
B8B—B3B—H3B | 122.0 | B5D—B4D—B9D | 108.13 (18) |
C1B—B4B—B5B | 58.41 (13) | C1D—B4D—B10D | 105.23 (18) |
C1B—B4B—B10B | 105.03 (18) | B3D—B4D—B10D | 108.10 (18) |
B5B—B4B—B10B | 60.10 (15) | B5D—B4D—B10D | 59.94 (14) |
C1B—B4B—B3B | 59.58 (13) | B9D—B4D—B10D | 60.23 (14) |
B5B—B4B—B3B | 108.20 (17) | C1D—B4D—H4D | 124.3 |
B10B—B4B—B3B | 107.98 (18) | B3D—B4D—H4D | 121.4 |
C1B—B4B—B9B | 105.81 (17) | B5D—B4D—H4D | 121.3 |
B5B—B4B—B9B | 108.57 (19) | B9D—B4D—H4D | 122.4 |
B10B—B4B—B9B | 60.34 (15) | B10D—B4D—H4D | 122.2 |
B3B—B4B—B9B | 59.82 (14) | C1D—B5D—B10D | 104.92 (17) |
C1B—B4B—H4B | 124.2 | C1D—B5D—B4D | 58.49 (13) |
B5B—B4B—H4B | 121.5 | B10D—B5D—B4D | 60.09 (14) |
B10B—B4B—H4B | 122.3 | C1D—B5D—B11D | 105.12 (17) |
B3B—B4B—H4B | 121.4 | B10D—B5D—B11D | 60.50 (14) |
B9B—B4B—H4B | 121.8 | B4D—B5D—B11D | 108.44 (18) |
C1B—B5B—B6B | 59.47 (14) | C1D—B5D—B6D | 59.05 (13) |
C1B—B5B—B4B | 59.15 (13) | B10D—B5D—B6D | 108.23 (17) |
B6B—B5B—B4B | 108.49 (17) | B4D—B5D—B6D | 108.05 (18) |
C1B—B5B—B10B | 105.52 (18) | B11D—B5D—B6D | 59.80 (13) |
B6B—B5B—B10B | 107.76 (18) | C1D—B5D—H5D | 124.6 |
B4B—B5B—B10B | 60.00 (15) | B10D—B5D—H5D | 122.1 |
C1B—B5B—B11B | 105.67 (17) | B4D—B5D—H5D | 121.5 |
B6B—B5B—B11B | 59.65 (14) | B11D—B5D—H5D | 122.0 |
B4B—B5B—B11B | 108.20 (19) | B6D—B5D—H5D | 121.4 |
B10B—B5B—B11B | 59.98 (15) | C2D—B6D—C1D | 57.15 (13) |
C1B—B5B—H5B | 123.8 | C2D—B6D—B11D | 103.90 (17) |
B6B—B5B—H5B | 121.4 | C1D—B6D—B11D | 105.06 (17) |
B4B—B5B—H5B | 121.3 | C2D—B6D—B5D | 104.00 (17) |
B10B—B5B—H5B | 122.4 | C1D—B6D—B5D | 58.72 (13) |
B11B—B5B—H5B | 122.3 | B11D—B6D—B5D | 60.06 (13) |
C2B—B6B—C1B | 57.49 (13) | C2D—B6D—B7D | 57.98 (13) |
C2B—B6B—B11B | 104.00 (18) | C1D—B6D—B7D | 104.84 (17) |
C1B—B6B—B11B | 105.42 (17) | B11D—B6D—B7D | 60.16 (14) |
C2B—B6B—B5B | 103.79 (18) | B5D—B6D—B7D | 108.00 (16) |
C1B—B6B—B5B | 58.27 (13) | C2D—B6D—H6D | 125.3 |
B11B—B6B—B5B | 60.52 (14) | C1D—B6D—H6D | 124.2 |
C2B—B6B—B7B | 58.03 (15) | B11D—B6D—H6D | 123.0 |
C1B—B6B—B7B | 105.23 (19) | B5D—B6D—H6D | 122.2 |
B11B—B6B—B7B | 60.06 (14) | B7D—B6D—H6D | 122.1 |
B5B—B6B—B7B | 108.07 (18) | C2D—B7D—B12D | 103.70 (18) |
C2B—B6B—H6B | 125.3 | C2D—B7D—B8D | 58.17 (13) |
C1B—B6B—H6B | 124.0 | B12D—B7D—B8D | 59.67 (14) |
B11B—B6B—H6B | 122.7 | C2D—B7D—B11D | 104.10 (17) |
B5B—B6B—H6B | 122.4 | B12D—B7D—B11D | 60.26 (14) |
B7B—B6B—H6B | 122.0 | B8D—B7D—B11D | 107.89 (18) |
C2B—B7B—B12B | 104.28 (18) | C2D—B7D—B6D | 58.85 (13) |
C2B—B7B—B11B | 104.45 (17) | B12D—B7D—B6D | 107.72 (18) |
B12B—B7B—B11B | 60.43 (14) | B8D—B7D—B6D | 107.88 (18) |
C2B—B7B—B6B | 58.81 (14) | B11D—B7D—B6D | 59.56 (13) |
B12B—B7B—B6B | 108.27 (18) | C2D—B7D—H7D | 125.4 |
B11B—B7B—B6B | 59.87 (15) | B12D—B7D—H7D | 122.7 |
C2B—B7B—B8B | 58.61 (15) | B8D—B7D—H7D | 121.6 |
B12B—B7B—B8B | 59.98 (15) | B11D—B7D—H7D | 122.5 |
B11B—B7B—B8B | 108.53 (18) | B6D—B7D—H7D | 121.5 |
B6B—B7B—B8B | 108.49 (19) | C2D—B8D—B12D | 104.16 (18) |
C2B—B7B—H7B | 125.2 | C2D—B8D—B9D | 104.24 (17) |
B12B—B7B—H7B | 122.3 | B12D—B8D—B9D | 60.54 (15) |
B11B—B7B—H7B | 122.2 | C2D—B8D—B3D | 58.90 (13) |
B6B—B7B—H7B | 121.2 | B12D—B8D—B3D | 108.17 (18) |
B8B—B7B—H7B | 121.2 | B9D—B8D—B3D | 59.58 (14) |
C2B—B8B—B12B | 103.57 (18) | C2D—B8D—B7D | 58.40 (13) |
C2B—B8B—B3B | 58.91 (14) | B12D—B8D—B7D | 60.04 (14) |
B12B—B8B—B3B | 108.01 (17) | B9D—B8D—B7D | 108.50 (18) |
C2B—B8B—B7B | 57.91 (15) | B3D—B8D—B7D | 108.37 (18) |
B12B—B8B—B7B | 59.76 (15) | C2D—B8D—H8D | 125.3 |
B3B—B8B—B7B | 107.92 (19) | B12D—B8D—H8D | 122.3 |
C2B—B8B—B9B | 104.12 (18) | B9D—B8D—H8D | 122.3 |
B12B—B8B—B9B | 60.43 (14) | B3D—B8D—H8D | 121.3 |
B3B—B8B—B9B | 59.71 (14) | B7D—B8D—H8D | 121.2 |
B7B—B8B—B9B | 108.09 (18) | B3D—B9D—B8D | 60.44 (14) |
C2B—B8B—H8B | 125.5 | B3D—B9D—B4D | 60.16 (14) |
B12B—B8B—H8B | 122.6 | B8D—B9D—B4D | 108.19 (16) |
B3B—B8B—H8B | 121.3 | B3D—B9D—B10D | 108.30 (17) |
B7B—B8B—H8B | 121.7 | B8D—B9D—B10D | 107.87 (18) |
B9B—B8B—H8B | 122.3 | B4D—B9D—B10D | 59.93 (14) |
B3B—B9B—B4B | 60.05 (14) | B3D—B9D—B12D | 108.16 (17) |
B3B—B9B—B8B | 60.11 (14) | B8D—B9D—B12D | 59.65 (14) |
B4B—B9B—B8B | 107.80 (17) | B4D—B9D—B12D | 107.79 (18) |
B3B—B9B—B10B | 107.67 (18) | B10D—B9D—B12D | 59.95 (15) |
B4B—B9B—B10B | 59.72 (15) | B3D—B9D—H9D | 121.3 |
B8B—B9B—B10B | 107.27 (19) | B8D—B9D—H9D | 121.7 |
B3B—B9B—B12B | 107.68 (18) | B4D—B9D—H9D | 121.7 |
B4B—B9B—B12B | 107.39 (19) | B10D—B9D—H9D | 121.7 |
B8B—B9B—B12B | 59.61 (14) | B12D—B9D—H9D | 121.9 |
B10B—B9B—B12B | 59.58 (15) | B5D—B10D—B4D | 59.97 (13) |
B3B—B9B—H9B | 121.7 | B5D—B10D—B12D | 107.77 (17) |
B4B—B9B—H9B | 121.9 | B4D—B10D—B12D | 107.82 (17) |
B8B—B9B—H9B | 122.0 | B5D—B10D—B9D | 107.85 (16) |
B10B—B9B—H9B | 122.2 | B4D—B10D—B9D | 59.84 (14) |
B12B—B9B—H9B | 122.2 | B12D—B10D—B9D | 60.08 (15) |
B4B—B10B—B5B | 59.89 (15) | B5D—B10D—B11D | 59.78 (14) |
B4B—B10B—B12B | 108.16 (17) | B4D—B10D—B11D | 107.78 (15) |
B5B—B10B—B12B | 108.21 (17) | B12D—B10D—B11D | 60.01 (15) |
B4B—B10B—B11B | 108.33 (17) | B9D—B10D—B11D | 108.02 (17) |
B5B—B10B—B11B | 60.25 (15) | B5D—B10D—H10D | 121.9 |
B12B—B10B—B11B | 60.19 (15) | B4D—B10D—H10D | 121.9 |
B4B—B10B—B9B | 59.94 (15) | B12D—B10D—H10D | 121.8 |
B5B—B10B—B9B | 108.09 (16) | B9D—B10D—H10D | 121.7 |
B12B—B10B—B9B | 60.34 (15) | B11D—B10D—H10D | 121.8 |
B11B—B10B—B9B | 108.66 (17) | B6D—B11D—B5D | 60.14 (13) |
B4B—B10B—H10B | 121.7 | B6D—B11D—B7D | 60.27 (13) |
B5B—B10B—H10B | 121.7 | B5D—B11D—B7D | 108.15 (16) |
B12B—B10B—H10B | 121.5 | B6D—B11D—B12D | 107.83 (17) |
B11B—B10B—H10B | 121.3 | B5D—B11D—B12D | 107.57 (18) |
B9B—B10B—H10B | 121.5 | B7D—B11D—B12D | 59.69 (14) |
B6B—B11B—B7B | 60.08 (14) | B6D—B11D—B10D | 107.87 (17) |
B6B—B11B—B10B | 107.73 (18) | B5D—B11D—B10D | 59.72 (14) |
B7B—B11B—B10B | 107.46 (19) | B7D—B11D—B10D | 107.72 (18) |
B6B—B11B—B12B | 107.89 (18) | B12D—B11D—B10D | 59.82 (15) |
B7B—B11B—B12B | 59.75 (14) | B6D—B11D—H11D | 121.6 |
B10B—B11B—B12B | 59.80 (15) | B5D—B11D—H11D | 121.8 |
B6B—B11B—B5B | 59.82 (14) | B7D—B11D—H11D | 121.7 |
B7B—B11B—B5B | 107.53 (17) | B12D—B11D—H11D | 122.1 |
B10B—B11B—B5B | 59.77 (15) | B10D—B11D—H11D | 122.0 |
B12B—B11B—B5B | 107.53 (19) | B8D—B12D—B7D | 60.30 (14) |
B6B—B11B—H11B | 121.7 | B8D—B12D—B10D | 108.02 (17) |
B7B—B11B—H11B | 122.0 | B7D—B12D—B10D | 108.28 (17) |
B10B—B11B—H11B | 122.0 | B8D—B12D—B9D | 59.81 (14) |
B12B—B11B—H11B | 121.9 | B7D—B12D—B9D | 108.13 (16) |
B5B—B11B—H11B | 122.1 | B10D—B12D—B9D | 59.97 (15) |
B7B—B12B—B8B | 60.26 (15) | B8D—B12D—B11D | 108.22 (16) |
B7B—B12B—B10B | 107.68 (18) | B7D—B12D—B11D | 60.05 (14) |
B8B—B12B—B10B | 107.94 (18) | B10D—B12D—B11D | 60.17 (15) |
B7B—B12B—B11B | 59.83 (15) | B9D—B12D—B11D | 108.06 (17) |
B8B—B12B—B11B | 108.26 (17) | B8D—B12D—H12D | 121.7 |
B10B—B12B—B11B | 60.01 (15) | B7D—B12D—H12D | 121.5 |
B7B—B12B—B9B | 108.10 (17) | B10D—B12D—H12D | 121.6 |
B8B—B12B—B9B | 59.96 (15) | B9D—B12D—H12D | 121.8 |
B10B—B12B—B9B | 60.08 (15) | B11D—B12D—H12D | 121.6 |
B11B—B12B—B9B | 108.31 (18) | Cl2—C1'—Cl1 | 112.02 (16) |
B7B—B12B—H12B | 121.8 | Cl2—C1'—H1'A | 109.2 |
B8B—B12B—H12B | 121.6 | Cl1—C1'—H1'A | 109.2 |
B10B—B12B—H12B | 121.9 | Cl2—C1'—H1'B | 109.2 |
B11B—B12B—H12B | 121.6 | Cl1—C1'—H1'B | 109.2 |
B9B—B12B—H12B | 121.6 | H1'A—C1'—H1'B | 107.9 |
C1C—Hg2—C1D | 172.78 (8) | Cl4—C2'—Cl3 | 111.88 (15) |
C2C—C1C—B4C | 109.84 (16) | Cl4—C2'—H2'B | 109.2 |
C2C—C1C—B5C | 109.86 (17) | Cl3—C2'—H2'B | 109.2 |
B4C—C1C—B5C | 62.45 (15) | Cl4—C2'—H2'A | 109.2 |
C2C—C1C—B6C | 60.60 (15) | Cl3—C2'—H2'A | 109.2 |
B4C—C1C—B6C | 113.84 (16) | H2'B—C2'—H2'A | 107.9 |
[Hg(C2B10H11)2]·C4H8O | Dx = 1.583 Mg m−3 |
Mr = 559.11 | Melting point: 531 K |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 12.186 (7) Å | Cell parameters from 21394 reflections |
b = 19.548 (12) Å | θ = 3.4–27.4° |
c = 19.700 (12) Å | µ = 6.56 mm−1 |
β = 90.055 (10)° | T = 173 K |
V = 4693 (5) Å3 | Plate, colorless |
Z = 8 | 0.35 × 0.30 × 0.12 mm |
F(000) = 2128 |
Bruker SMART 1K CCD area-detector diffractometer | 10466 independent reflections |
Radiation source: rotating anode | 8750 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
ϕ and ω scans | θmax = 27.5°, θmin = 1.0° |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | h = −15→15 |
Tmin = 0.175, Tmax = 0.455 | k = −25→25 |
34377 measured reflections | l = −25→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)] = 0.044 | H-atom parameters constrained |
wR(F2) = 0.107 | w = 1/[σ2(Fo2) + (0.0261P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.002 |
10466 reflections | Δρmax = 3.05 e Å−3 |
557 parameters | Δρmin = −3.38 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00029 (4) |
[Hg(C2B10H11)2]·C4H8O | V = 4693 (5) Å3 |
Mr = 559.11 | Z = 8 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.186 (7) Å | µ = 6.56 mm−1 |
b = 19.548 (12) Å | T = 173 K |
c = 19.700 (12) Å | 0.35 × 0.30 × 0.12 mm |
β = 90.055 (10)° |
Bruker SMART 1K CCD area-detector diffractometer | 10466 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | 8750 reflections with I > 2σ(I) |
Tmin = 0.175, Tmax = 0.455 | Rint = 0.050 |
34377 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.06 | Δρmax = 3.05 e Å−3 |
10466 reflections | Δρmin = −3.38 e Å−3 |
557 parameters |
Experimental. X-ray crystallographic data were collected from a single-crystal sample of (II) and mounted on a glass fibre. Data were collected using a P4 Bruker diffractometer, equipped with a Bruker SMART 1 K CCD area detector, using the program SMART (Bruker, 1997), and a rotating anode, using graphite-monochromated Mo—Kα radiation. Almost a complete sphere of data was collected, to better than 0.8 Å resolution at 173 K. Upon completion of the data collection, the first 40 frames were recollected in order to improve the decay correction analysis, which was negligible. The crystal-to-detector distance was 4.987 cm, and the data collection was carried out in 512 × 512 pixel mode, utilizing 2 × 2 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular settings of the strong reflections, collected by a 12° scan in 40 frames over four different sections of reciprocal space (160 frames in total). The crystal used to collect the data was twinned. The unit cell was originally determined to be orthorhombic and merging the data into this Laue group resulted in an acceptable Rint (0.061). However, a space-group determination was problematic and no acceptable set of systematic absences was observed. While performing a search for higher metric symmetry in XPREP (Sheldrick, 1997), three monoclinic systems were suggested with low R(symm) values. However, one suggestion had a slightly lower R(symm) (0.040) than the other two (0.057 and 0.056). Upon re-integrating and reperforming the absorption correction determination (assuming 2/m redundancy), the structure solution and refinement in P21/n was still problematic, as the ωR remained quite high (0.55) and the final agreement would not drop below 30%. Introduction of de-twinning about (100/0–10/00–1) immediately reduced ωR, and the refinement then proceeded satisfactorily to the final agreement factor of R = 0.0444 for reflections greater than the threshold. The fraction of the minor twin component obtained by numerous least-squares structure refinements was 0.475 (1). |
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 | 0.23983 (3) | 0.146666 (15) | 0.346938 (18) | 0.02603 (10) | |
C1A | 0.3672 (8) | 0.1996 (4) | 0.3931 (5) | 0.025 (2) | |
B2A | 0.3325 (12) | 0.2680 (6) | 0.4429 (7) | 0.039 (3) | |
H2A | 0.2451 | 0.2859 | 0.4533 | 0.047* | |
B3A | 0.3969 (10) | 0.2793 (5) | 0.3623 (6) | 0.031 (3) | |
H3A | 0.3518 | 0.3053 | 0.3187 | 0.04 (3)* | |
B4A | 0.4861 (9) | 0.2089 (6) | 0.3475 (7) | 0.032 (3) | |
H4A | 0.5010 | 0.1874 | 0.2945 | 0.038* | |
B5A | 0.4779 (12) | 0.1545 (6) | 0.4197 (6) | 0.037 (3) | |
H5A | 0.4871 | 0.0966 | 0.4152 | 0.03 (3)* | |
B6A | 0.3854 (12) | 0.1921 (6) | 0.4785 (6) | 0.035 (3) | |
H6A | 0.335 (9) | 0.157 (5) | 0.507 (5) | 0.03 (3)* | |
B7A | 0.4378 (15) | 0.2708 (6) | 0.5048 (8) | 0.049 (4) | |
H7A | 0.4239 | 0.2920 | 0.5580 | 0.058* | |
B8A | 0.4443 (12) | 0.3255 (7) | 0.4326 (7) | 0.043 (4) | |
H8A | 0.4338 | 0.3832 | 0.4380 | 0.052* | |
B9A | 0.5380 (12) | 0.2891 (7) | 0.3732 (7) | 0.042 (3) | |
H9A | 0.5896 | 0.3227 | 0.3384 | 0.051* | |
B10A | 0.5905 (11) | 0.2118 (7) | 0.4087 (7) | 0.039 (3) | |
H10A | 0.6776 | 0.1936 | 0.3980 | 0.047* | |
B11A | 0.5275 (14) | 0.2005 (7) | 0.4899 (8) | 0.044 (3) | |
H11A | 0.5731 | 0.1746 | 0.5334 | 0.04 (3)* | |
C12A | 0.5570 (10) | 0.2796 (5) | 0.4571 (6) | 0.038 (3) | |
H12A | 0.6285 | 0.3090 | 0.4803 | 0.05 (3)* | |
C1B | 0.1133 (8) | 0.1028 (5) | 0.2918 (5) | 0.026 (2) | |
B2B | 0.0766 (9) | 0.1468 (5) | 0.2214 (6) | 0.024 (2) | |
H2B | 0.1145 | 0.1974 | 0.2049 | 0.01 (2)* | |
B3B | −0.0115 (10) | 0.1429 (6) | 0.2923 (7) | 0.031 (3) | |
H3B | −0.0324 | 0.1906 | 0.3229 | 0.05 (3)* | |
B4B | 0.0072 (9) | 0.0616 (5) | 0.3318 (7) | 0.033 (3) | |
H4B | −0.0011 | 0.0545 | 0.3890 | 0.040* | |
B5B | 0.1087 (11) | 0.0157 (6) | 0.2825 (7) | 0.031 (3) | |
H5B | 0.1683 | −0.0221 | 0.3067 | 0.04 (3)* | |
B6B | 0.1529 (12) | 0.0695 (5) | 0.2146 (6) | 0.033 (3) | |
H6B | 0.2402 | 0.0680 | 0.1940 | 0.04 (3)* | |
B7B | 0.0366 (11) | 0.0842 (6) | 0.1624 (6) | 0.037 (3) | |
H7B | 0.0448 | 0.0915 | 0.1052 | 0.044* | |
B8B | −0.0640 (11) | 0.1290 (6) | 0.2104 (7) | 0.036 (3) | |
H8B | −0.1233 | 0.1661 | 0.1850 | 0.044* | |
B9B | −0.1061 (11) | 0.0765 (6) | 0.2792 (7) | 0.037 (3) | |
H9B | −0.1932 | 0.0787 | 0.3001 | 0.044* | |
B10B | −0.0330 (11) | −0.0021 (6) | 0.2732 (7) | 0.036 (3) | |
H10B | −0.0711 | −0.0525 | 0.2902 | 0.043* | |
B11B | 0.0540 (12) | 0.0029 (6) | 0.2016 (7) | 0.038 (3) | |
H11B | 0.0734 | −0.0447 | 0.1705 | 0.045* | |
C12B | −0.0682 (9) | 0.0425 (5) | 0.2025 (6) | 0.038 (3) | |
H12B | −0.1355 | 0.0199 | 0.1691 | 0.04 (3)* | |
Hg2 | 0.28017 (3) | 0.842004 (16) | 0.32756 (2) | 0.02878 (10) | |
C1C | 0.4153 (8) | 0.8850 (5) | 0.2771 (5) | 0.028 (2) | |
B2C | 0.5330 (10) | 0.8393 (6) | 0.2773 (7) | 0.033 (3) | |
H2C | 0.5439 | 0.7879 | 0.3038 | 0.040* | |
B3C | 0.5194 (9) | 0.9164 (6) | 0.3246 (7) | 0.033 (3) | |
H3C | 0.5213 | 0.9169 | 0.3824 | 0.040* | |
B4C | 0.4340 (11) | 0.9719 (6) | 0.2771 (7) | 0.035 (3) | |
H4C | 0.3780 | 1.0105 | 0.3032 | 0.042* | |
B5C | 0.3910 (11) | 0.9280 (6) | 0.2029 (6) | 0.034 (3) | |
H5C | 0.3068 | 0.9361 | 0.1790 | 0.08 (4)* | |
B6C | 0.4554 (10) | 0.8466 (6) | 0.2042 (7) | 0.033 (3) | |
H6C | 0.4128 | 0.8003 | 0.1808 | 0.040* | |
B7C | 0.5986 (11) | 0.8564 (7) | 0.2005 (7) | 0.041 (3) | |
H7C | 0.6549 | 0.8179 | 0.1745 | 0.06 (3)* | |
B8C | 0.6375 (11) | 0.9011 (7) | 0.2742 (7) | 0.040 (3) | |
H8C | 0.7221 | 0.8927 | 0.2976 | 0.048* | |
B9C | 0.5738 (11) | 0.9829 (7) | 0.2748 (8) | 0.041 (3) | |
H9C | 0.6149 | 1.0294 | 0.2988 | 0.049* | |
B10C | 0.4961 (12) | 0.9901 (7) | 0.2004 (9) | 0.043 (4) | |
H10C | 0.4840 | 1.0412 | 0.1736 | 0.052* | |
B11C | 0.5126 (11) | 0.9129 (7) | 0.1543 (7) | 0.042 (3) | |
H11C | 0.5125 | 0.9123 | 0.0964 | 0.051* | |
C12C | 0.6157 (10) | 0.9446 (6) | 0.2016 (6) | 0.045 (3) | |
H12C | 0.6898 | 0.9671 | 0.1742 | 0.054* | |
C1D | 0.1499 (7) | 0.7948 (4) | 0.3767 (5) | 0.023 (2) | |
B2D | 0.1824 (12) | 0.7227 (5) | 0.4231 (6) | 0.035 (3) | |
H2D | 0.2686 | 0.7007 | 0.4285 | 0.041* | |
B3D | 0.1077 (9) | 0.7179 (5) | 0.3453 (6) | 0.029 (2) | |
H3D | 0.1437 | 0.6923 | 0.2984 | 0.02 (2)* | |
B4D | 0.0265 (9) | 0.7911 (5) | 0.3392 (6) | 0.027 (2) | |
H4D | 0.0079 | 0.8152 | 0.2878 | 0.032* | |
B5D | 0.0454 (11) | 0.8419 (6) | 0.4135 (6) | 0.032 (3) | |
H5D | 0.0391 | 0.9000 | 0.4124 | 0.038* | |
B6D | 0.1428 (12) | 0.7998 (6) | 0.4633 (6) | 0.037 (3) | |
H6D | 0.2039 | 0.8299 | 0.4955 | 0.03 (3)* | |
B7D | 0.0839 (14) | 0.7204 (6) | 0.4906 (7) | 0.047 (4) | |
H7D | 0.1022 | 0.6959 | 0.5419 | 0.056* | |
B8D | 0.0626 (12) | 0.6705 (5) | 0.4179 (7) | 0.038 (3) | |
H8D | 0.0666 | 0.6123 | 0.4205 | 0.045* | |
B9D | −0.0318 (11) | 0.7125 (6) | 0.3655 (7) | 0.038 (3) | |
H9D | −0.0919 | 0.6826 | 0.3326 | 0.06 (4)* | |
B10D | −0.0706 (12) | 0.7902 (6) | 0.4074 (7) | 0.040 (3) | |
H10D | −0.1565 | 0.8127 | 0.4025 | 0.047* | |
B11D | 0.0026 (13) | 0.7943 (7) | 0.4843 (8) | 0.044 (4) | |
H11D | −0.0332 | 0.8193 | 0.5316 | 0.02 (3)* | |
C12D | −0.0380 (11) | 0.7185 (6) | 0.4511 (6) | 0.043 (3) | |
H12D | −0.1081 | 0.6906 | 0.4775 | 0.051* | |
O1 | 0.2345 (8) | 0.0375 (4) | 0.4428 (3) | 0.0468 (19) | |
C1 | 0.3086 (12) | −0.0141 (6) | 0.4571 (8) | 0.060 (4) | |
H1A | 0.3812 | −0.0033 | 0.4373 | 0.072* | |
H1B | 0.2828 | −0.0580 | 0.4377 | 0.072* | |
C2 | 0.3168 (16) | −0.0192 (7) | 0.5328 (9) | 0.094 (7) | |
H2E | 0.3107 | −0.0674 | 0.5479 | 0.113* | |
H2F | 0.3873 | −0.0002 | 0.5492 | 0.113* | |
C3 | 0.2242 (13) | 0.0214 (8) | 0.5576 (7) | 0.073 (4) | |
H3E | 0.1790 | −0.0058 | 0.5894 | 0.087* | |
H3F | 0.2507 | 0.0628 | 0.5815 | 0.087* | |
C4 | 0.1612 (10) | 0.0400 (7) | 0.4987 (7) | 0.055 (3) | |
H4E | 0.0998 | 0.0075 | 0.4919 | 0.066* | |
H4F | 0.1306 | 0.0866 | 0.5039 | 0.066* | |
O2 | 0.2737 (7) | 0.4979 (3) | 0.5850 (4) | 0.044 (2) | |
C1' | 0.2927 (15) | 0.5449 (7) | 0.5296 (8) | 0.076 (5) | |
H1'A | 0.3718 | 0.5555 | 0.5253 | 0.091* | |
H1'B | 0.2519 | 0.5881 | 0.5368 | 0.091* | |
C2' | 0.252 (2) | 0.5093 (7) | 0.4691 (6) | 0.089 (6) | |
H2'A | 0.2100 | 0.5409 | 0.4399 | 0.107* | |
H2'B | 0.3146 | 0.4908 | 0.4424 | 0.107* | |
C3' | 0.1829 (15) | 0.4542 (8) | 0.4931 (8) | 0.087 (5) | |
H3'A | 0.1057 | 0.4693 | 0.4972 | 0.104* | |
H3'B | 0.1864 | 0.4142 | 0.4623 | 0.104* | |
C4' | 0.2286 (12) | 0.4379 (6) | 0.5586 (6) | 0.052 (3)* | |
H4'B | 0.1705 | 0.4204 | 0.5892 | 0.062* | |
H4'A | 0.2859 | 0.4024 | 0.5541 | 0.062* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Hg1 | 0.02156 (19) | 0.02566 (14) | 0.03086 (18) | −0.00488 (13) | −0.00366 (18) | −0.00210 (12) |
C1A | 0.024 (5) | 0.024 (4) | 0.026 (5) | −0.010 (4) | −0.004 (4) | 0.002 (4) |
B2A | 0.048 (8) | 0.027 (5) | 0.042 (8) | −0.010 (6) | 0.002 (6) | −0.004 (5) |
B3A | 0.035 (7) | 0.028 (5) | 0.029 (7) | −0.005 (5) | −0.008 (5) | 0.008 (4) |
B4A | 0.015 (5) | 0.046 (6) | 0.034 (7) | −0.004 (5) | −0.002 (6) | 0.006 (5) |
B5A | 0.048 (8) | 0.031 (6) | 0.031 (7) | 0.001 (6) | −0.010 (6) | 0.006 (5) |
B6A | 0.040 (8) | 0.036 (6) | 0.028 (7) | −0.015 (6) | 0.000 (6) | −0.001 (5) |
B7A | 0.083 (12) | 0.030 (6) | 0.033 (7) | −0.020 (7) | −0.010 (8) | −0.001 (5) |
B8A | 0.044 (9) | 0.033 (6) | 0.053 (9) | −0.021 (6) | −0.017 (7) | 0.004 (6) |
B9A | 0.043 (8) | 0.049 (7) | 0.036 (7) | −0.018 (6) | −0.016 (6) | 0.020 (6) |
B10A | 0.026 (7) | 0.049 (7) | 0.042 (8) | −0.002 (6) | −0.014 (6) | 0.011 (6) |
B11A | 0.061 (10) | 0.033 (6) | 0.037 (8) | −0.012 (6) | −0.018 (7) | 0.010 (6) |
C12A | 0.041 (7) | 0.038 (5) | 0.037 (7) | −0.018 (5) | −0.010 (5) | 0.010 (5) |
C1B | 0.019 (5) | 0.027 (4) | 0.031 (5) | −0.003 (4) | −0.005 (4) | 0.000 (4) |
B2B | 0.025 (6) | 0.020 (5) | 0.028 (6) | 0.000 (4) | −0.006 (5) | 0.002 (4) |
B3B | 0.022 (6) | 0.031 (5) | 0.041 (7) | −0.004 (5) | −0.011 (5) | 0.004 (5) |
B4B | 0.028 (6) | 0.031 (5) | 0.041 (7) | −0.010 (4) | −0.010 (6) | 0.010 (5) |
B5B | 0.031 (7) | 0.028 (5) | 0.035 (7) | 0.002 (5) | −0.002 (6) | −0.001 (5) |
B6B | 0.050 (8) | 0.023 (5) | 0.026 (6) | −0.001 (5) | −0.008 (6) | −0.001 (4) |
B7B | 0.049 (8) | 0.040 (6) | 0.023 (7) | −0.005 (5) | −0.010 (6) | −0.002 (5) |
B8B | 0.026 (7) | 0.039 (6) | 0.044 (8) | −0.003 (5) | −0.011 (6) | 0.008 (5) |
B9B | 0.028 (7) | 0.039 (6) | 0.044 (8) | −0.013 (5) | −0.003 (6) | 0.007 (5) |
B10B | 0.034 (8) | 0.030 (6) | 0.043 (9) | −0.013 (5) | −0.013 (7) | 0.004 (5) |
B11B | 0.050 (9) | 0.030 (6) | 0.033 (8) | −0.009 (6) | −0.006 (7) | −0.009 (5) |
C12B | 0.036 (6) | 0.040 (6) | 0.037 (6) | −0.016 (5) | −0.012 (5) | 0.002 (5) |
Hg2 | 0.0238 (2) | 0.02761 (15) | 0.0349 (2) | −0.00696 (14) | −0.00134 (19) | 0.00378 (13) |
C1C | 0.012 (5) | 0.035 (5) | 0.037 (6) | −0.007 (4) | −0.002 (4) | 0.006 (4) |
B2C | 0.024 (6) | 0.033 (6) | 0.043 (7) | −0.004 (5) | −0.003 (5) | 0.008 (5) |
B3C | 0.019 (6) | 0.040 (6) | 0.040 (7) | −0.016 (5) | −0.004 (6) | 0.006 (6) |
B4C | 0.045 (8) | 0.018 (5) | 0.042 (8) | −0.009 (5) | −0.003 (6) | −0.003 (5) |
B5C | 0.039 (7) | 0.035 (6) | 0.027 (6) | −0.004 (5) | −0.009 (6) | 0.008 (5) |
B6C | 0.024 (6) | 0.038 (6) | 0.037 (7) | 0.008 (5) | 0.000 (5) | 0.000 (5) |
B7C | 0.029 (7) | 0.050 (7) | 0.044 (8) | 0.003 (6) | 0.001 (6) | −0.003 (6) |
B8C | 0.026 (7) | 0.052 (7) | 0.042 (8) | −0.006 (6) | −0.004 (6) | 0.004 (6) |
B9C | 0.019 (7) | 0.048 (7) | 0.057 (10) | −0.014 (6) | 0.006 (6) | 0.008 (7) |
B10C | 0.030 (7) | 0.045 (7) | 0.056 (10) | −0.008 (6) | 0.009 (7) | 0.015 (7) |
B11C | 0.043 (8) | 0.057 (8) | 0.027 (7) | 0.004 (6) | 0.005 (6) | 0.007 (6) |
C12C | 0.036 (7) | 0.053 (7) | 0.046 (7) | −0.006 (6) | 0.006 (6) | 0.014 (5) |
C1D | 0.013 (4) | 0.027 (4) | 0.030 (5) | −0.010 (4) | −0.005 (4) | −0.006 (4) |
B2D | 0.043 (8) | 0.028 (5) | 0.033 (7) | 0.000 (5) | −0.007 (6) | 0.004 (5) |
B3D | 0.026 (6) | 0.029 (5) | 0.033 (7) | −0.005 (4) | −0.001 (5) | −0.003 (5) |
B4D | 0.021 (5) | 0.032 (5) | 0.029 (7) | −0.005 (4) | −0.001 (5) | −0.001 (5) |
B5D | 0.034 (7) | 0.024 (5) | 0.037 (7) | −0.003 (5) | 0.000 (5) | −0.005 (5) |
B6D | 0.056 (9) | 0.030 (5) | 0.024 (6) | −0.006 (6) | −0.004 (6) | −0.003 (4) |
B7D | 0.077 (12) | 0.033 (6) | 0.031 (8) | −0.010 (7) | −0.005 (7) | 0.006 (5) |
B8D | 0.052 (9) | 0.017 (5) | 0.044 (8) | −0.006 (5) | 0.007 (6) | 0.000 (5) |
B9D | 0.034 (7) | 0.039 (6) | 0.042 (8) | −0.006 (6) | 0.003 (6) | −0.016 (5) |
B10D | 0.040 (8) | 0.031 (6) | 0.047 (8) | −0.008 (6) | 0.007 (6) | −0.008 (5) |
B11D | 0.063 (11) | 0.037 (7) | 0.031 (9) | −0.003 (7) | 0.010 (7) | −0.007 (6) |
C12D | 0.048 (8) | 0.038 (6) | 0.043 (7) | −0.016 (5) | 0.016 (6) | −0.008 (5) |
O1 | 0.055 (6) | 0.048 (4) | 0.038 (4) | 0.000 (4) | −0.009 (4) | 0.006 (3) |
C1 | 0.049 (9) | 0.040 (6) | 0.093 (12) | 0.003 (6) | 0.002 (8) | −0.006 (7) |
C2 | 0.120 (16) | 0.051 (7) | 0.112 (14) | 0.042 (9) | −0.084 (13) | −0.025 (8) |
C3 | 0.057 (10) | 0.107 (11) | 0.054 (8) | −0.010 (10) | 0.000 (8) | 0.035 (8) |
C4 | 0.034 (7) | 0.063 (8) | 0.069 (9) | 0.011 (6) | 0.002 (7) | 0.000 (7) |
O2 | 0.051 (6) | 0.044 (4) | 0.037 (4) | −0.004 (4) | −0.011 (5) | −0.003 (3) |
C1' | 0.091 (13) | 0.052 (7) | 0.085 (11) | −0.032 (8) | 0.007 (10) | 0.009 (7) |
C2' | 0.146 (18) | 0.083 (9) | 0.039 (8) | 0.028 (12) | −0.013 (12) | 0.020 (6) |
C3' | 0.105 (14) | 0.083 (10) | 0.072 (11) | −0.024 (10) | −0.038 (10) | −0.022 (9) |
Hg1—C1B | 2.071 (9) | B3C—B4C | 1.770 (18) |
Hg1—C1A | 2.074 (9) | B3C—B8C | 1.775 (19) |
C1A—B5A | 1.695 (16) | B3C—H3C | 1.1400 |
C1A—B6A | 1.704 (16) | B4C—B9C | 1.717 (19) |
C1A—B3A | 1.710 (14) | B4C—B10C | 1.73 (2) |
C1A—B2A | 1.712 (15) | B4C—B5C | 1.774 (17) |
C1A—B4A | 1.715 (15) | B4C—H4C | 1.1400 |
B2A—B6A | 1.764 (18) | B5C—B10C | 1.765 (18) |
B2A—B7A | 1.77 (2) | B5C—B6C | 1.775 (17) |
B2A—B8A | 1.778 (18) | B5C—B11C | 1.789 (19) |
B2A—B3A | 1.785 (18) | B5C—H5C | 1.1400 |
B2A—H2A | 1.1400 | B6C—B7C | 1.757 (18) |
B3A—B9A | 1.742 (18) | B6C—B11C | 1.771 (18) |
B3A—B8A | 1.751 (17) | B6C—H6C | 1.1400 |
B3A—B4A | 1.777 (17) | B7C—C12C | 1.737 (17) |
B3A—H3A | 1.1400 | B7C—B8C | 1.760 (19) |
B4A—B10A | 1.753 (17) | B7C—B11C | 1.773 (19) |
B4A—B9A | 1.764 (18) | B7C—H7C | 1.1400 |
B4A—B5A | 1.779 (17) | B8C—C12C | 1.684 (17) |
B4A—H4A | 1.1400 | B8C—B9C | 1.78 (2) |
B5A—B11A | 1.756 (19) | B8C—H8C | 1.1400 |
B5A—B6A | 1.78 (2) | B9C—C12C | 1.70 (2) |
B5A—B10A | 1.785 (19) | B9C—B10C | 1.75 (2) |
B5A—H5A | 1.1400 | B9C—H9C | 1.1400 |
B6A—B7A | 1.745 (17) | B10C—C12C | 1.708 (19) |
B6A—B11A | 1.75 (2) | B10C—B11C | 1.77 (2) |
B6A—H6A | 1.08 (10) | B10C—H10C | 1.1400 |
B7A—C12A | 1.74 (2) | B11C—C12C | 1.682 (19) |
B7A—B11A | 1.78 (2) | B11C—H11C | 1.1400 |
B7A—B8A | 1.782 (19) | C12C—H12C | 1.1400 |
B7A—H7A | 1.1400 | C1D—B4D | 1.676 (14) |
B8A—C12A | 1.711 (19) | C1D—B3D | 1.705 (13) |
B8A—B9A | 1.78 (2) | C1D—B6D | 1.710 (15) |
B8A—H8A | 1.1400 | C1D—B2D | 1.726 (14) |
B9A—C12A | 1.679 (17) | C1D—B5D | 1.730 (16) |
B9A—B10A | 1.783 (18) | B2D—B6D | 1.771 (17) |
B9A—H9A | 1.1400 | B2D—B3D | 1.783 (17) |
B10A—C12A | 1.681 (19) | B2D—B8D | 1.783 (18) |
B10A—B11A | 1.79 (2) | B2D—B7D | 1.79 (2) |
B10A—H10A | 1.1400 | B2D—H2D | 1.1400 |
B11A—C12A | 1.714 (16) | B3D—B4D | 1.744 (15) |
B11A—H11A | 1.1400 | B3D—B9D | 1.749 (18) |
C12A—H12A | 1.1400 | B3D—B8D | 1.790 (17) |
C1B—B2B | 1.691 (14) | B3D—H3D | 1.1400 |
C1B—B3B | 1.711 (15) | B4D—B9D | 1.771 (16) |
C1B—B5B | 1.714 (14) | B4D—B5D | 1.782 (16) |
C1B—B4B | 1.717 (15) | B4D—B10D | 1.791 (18) |
C1B—B6B | 1.723 (16) | B4D—H4D | 1.1400 |
B2B—B7B | 1.756 (15) | B5D—B10D | 1.741 (18) |
B2B—B8B | 1.761 (17) | B5D—B6D | 1.745 (18) |
B2B—B3B | 1.764 (18) | B5D—B11D | 1.755 (19) |
B2B—B6B | 1.779 (15) | B5D—H5D | 1.1400 |
B2B—H2B | 1.1400 | B6D—B11D | 1.76 (2) |
B3B—B9B | 1.756 (16) | B6D—B7D | 1.793 (17) |
B3B—B8B | 1.756 (18) | B6D—H6D | 1.1400 |
B3B—B4B | 1.785 (15) | B7D—C12D | 1.68 (2) |
B3B—H3B | 1.1400 | B7D—B8D | 1.752 (18) |
B4B—B9B | 1.750 (17) | B7D—B11D | 1.76 (2) |
B4B—B10B | 1.767 (17) | B7D—H7D | 1.1400 |
B4B—B5B | 1.810 (18) | B8D—C12D | 1.677 (18) |
B4B—H4B | 1.1400 | B8D—B9D | 1.75 (2) |
B5B—B11B | 1.744 (17) | B8D—H8D | 1.1400 |
B5B—B10B | 1.771 (18) | B9D—C12D | 1.692 (18) |
B5B—B6B | 1.784 (17) | B9D—B10D | 1.793 (17) |
B5B—H5B | 1.1400 | B9D—H9D | 1.1400 |
B6B—B7B | 1.774 (17) | B10D—C12D | 1.693 (18) |
B6B—B11B | 1.793 (17) | B10D—B11D | 1.76 (2) |
B6B—H6B | 1.1400 | B10D—H10D | 1.1400 |
B7B—C12B | 1.709 (17) | B11D—C12D | 1.693 (17) |
B7B—B8B | 1.779 (19) | B11D—H11D | 1.1400 |
B7B—B11B | 1.780 (17) | C12D—H12D | 1.1400 |
B7B—H7B | 1.1400 | O1—C1 | 1.383 (14) |
B8B—C12B | 1.699 (16) | O1—C4 | 1.419 (15) |
B8B—B9B | 1.776 (18) | C1—C2 | 1.50 (2) |
B8B—H8B | 1.1400 | C1—H1A | 0.9900 |
B9B—C12B | 1.715 (18) | C1—H1B | 0.9900 |
B9B—B10B | 1.780 (19) | C2—C3 | 1.46 (2) |
B9B—H9B | 1.1400 | C2—H2E | 0.9900 |
B10B—C12B | 1.697 (17) | C2—H2F | 0.9900 |
B10B—B11B | 1.77 (2) | C3—C4 | 1.438 (18) |
B10B—H10B | 1.1400 | C3—H3E | 0.9900 |
B11B—C12B | 1.677 (19) | C3—H3F | 0.9900 |
B11B—H11B | 1.1400 | C4—H4E | 0.9900 |
C12B—H12B | 1.1400 | C4—H4F | 0.9900 |
Hg2—C1D | 2.077 (9) | O2—C4' | 1.396 (13) |
Hg2—C1C | 2.099 (10) | O2—C1' | 1.445 (14) |
C1C—B2C | 1.690 (16) | C1'—C2' | 1.466 (19) |
C1C—B3C | 1.692 (15) | C1'—H1'A | 0.9900 |
C1C—B6C | 1.692 (16) | C1'—H1'B | 0.9900 |
C1C—B5C | 1.712 (15) | C2'—C3' | 1.45 (2) |
C1C—B4C | 1.715 (14) | C2'—H2'A | 0.9900 |
B2C—B6C | 1.728 (18) | C2'—H2'B | 0.9900 |
B2C—B7C | 1.744 (19) | C3'—C4' | 1.440 (19) |
B2C—B8C | 1.757 (17) | C3'—H3'A | 0.9900 |
B2C—B3C | 1.780 (18) | C3'—H3'B | 0.9900 |
B2C—H2C | 1.1400 | C4'—H4'B | 0.9900 |
B3C—B9C | 1.759 (18) | C4'—H4'A | 0.9900 |
C1B—Hg1—C1A | 173.0 (4) | B8C—B2C—B3C | 60.2 (7) |
B5A—C1A—B6A | 63.0 (7) | C1C—B2C—H2C | 124.4 |
B5A—C1A—B3A | 114.5 (8) | B6C—B2C—H2C | 121.2 |
B6A—C1A—B3A | 113.7 (7) | B7C—B2C—H2C | 120.9 |
B5A—C1A—B2A | 115.2 (8) | B8C—B2C—H2C | 122.6 |
B6A—C1A—B2A | 62.2 (7) | B3C—B2C—H2C | 121.2 |
B3A—C1A—B2A | 62.9 (7) | C1C—B3C—B9C | 104.0 (9) |
B5A—C1A—B4A | 62.9 (7) | C1C—B3C—B4C | 59.3 (6) |
B6A—C1A—B4A | 114.6 (8) | B9C—B3C—B4C | 58.2 (7) |
B3A—C1A—B4A | 62.5 (7) | C1C—B3C—B8C | 103.8 (9) |
B2A—C1A—B4A | 115.3 (8) | B9C—B3C—B8C | 60.4 (8) |
B5A—C1A—Hg1 | 118.1 (6) | B4C—B3C—B8C | 106.5 (9) |
B6A—C1A—Hg1 | 119.1 (6) | C1C—B3C—B2C | 58.2 (7) |
B3A—C1A—Hg1 | 117.3 (6) | B9C—B3C—B2C | 107.4 (10) |
B2A—C1A—Hg1 | 117.1 (7) | B4C—B3C—B2C | 107.3 (9) |
B4A—C1A—Hg1 | 117.1 (7) | B8C—B3C—B2C | 59.2 (7) |
C1A—B2A—B6A | 58.7 (6) | C1C—B3C—H3C | 124.9 |
C1A—B2A—B7A | 103.9 (10) | B9C—B3C—H3C | 122.9 |
B6A—B2A—B7A | 59.2 (7) | B4C—B3C—H3C | 122.3 |
C1A—B2A—B8A | 103.8 (10) | B8C—B3C—H3C | 123.0 |
B6A—B2A—B8A | 107.3 (10) | B2C—B3C—H3C | 122.0 |
B7A—B2A—B8A | 60.3 (8) | C1C—B4C—B9C | 104.9 (9) |
C1A—B2A—B3A | 58.5 (6) | C1C—B4C—B10C | 105.2 (9) |
B6A—B2A—B3A | 107.2 (9) | B9C—B4C—B10C | 61.0 (8) |
B7A—B2A—B3A | 106.8 (10) | C1C—B4C—B3C | 58.1 (6) |
B8A—B2A—B3A | 58.9 (7) | B9C—B4C—B3C | 60.6 (8) |
C1A—B2A—H2A | 125.1 | B10C—B4C—B3C | 109.3 (10) |
B6A—B2A—H2A | 121.9 | C1C—B4C—B5C | 58.7 (6) |
B7A—B2A—H2A | 122.9 | B9C—B4C—B5C | 109.4 (10) |
B8A—B2A—H2A | 122.8 | B10C—B4C—B5C | 60.5 (8) |
B3A—B2A—H2A | 122.3 | B3C—B4C—B5C | 108.2 (8) |
C1A—B3A—B9A | 105.4 (8) | C1C—B4C—H4C | 125.2 |
C1A—B3A—B8A | 105.1 (8) | B9C—B4C—H4C | 121.5 |
B9A—B3A—B8A | 61.5 (8) | B10C—B4C—H4C | 121.4 |
C1A—B3A—B4A | 58.9 (6) | B3C—B4C—H4C | 121.3 |
B9A—B3A—B4A | 60.1 (7) | B5C—B4C—H4C | 121.0 |
B8A—B3A—B4A | 109.2 (9) | C1C—B5C—B10C | 103.7 (9) |
C1A—B3A—B2A | 58.6 (6) | C1C—B5C—B4C | 58.9 (6) |
B9A—B3A—B2A | 109.8 (9) | B10C—B5C—B4C | 58.4 (8) |
B8A—B3A—B2A | 60.4 (7) | C1C—B5C—B6C | 58.0 (7) |
B4A—B3A—B2A | 108.7 (8) | B10C—B5C—B6C | 107.2 (10) |
C1A—B3A—H3A | 124.9 | B4C—B5C—B6C | 106.9 (9) |
B9A—B3A—H3A | 121.2 | C1C—B5C—B11C | 103.5 (9) |
B8A—B3A—H3A | 121.6 | B10C—B5C—B11C | 59.8 (8) |
B4A—B3A—H3A | 121.1 | B4C—B5C—B11C | 106.0 (9) |
B2A—B3A—H3A | 120.9 | B6C—B5C—B11C | 59.6 (7) |
C1A—B4A—B10A | 104.9 (9) | C1C—B5C—H5C | 125.2 |
C1A—B4A—B9A | 104.3 (9) | B10C—B5C—H5C | 123.1 |
B10A—B4A—B9A | 60.9 (7) | B4C—B5C—H5C | 122.6 |
C1A—B4A—B3A | 58.6 (6) | B6C—B5C—H5C | 121.9 |
B10A—B4A—B3A | 107.7 (9) | B11C—B5C—H5C | 123.2 |
B9A—B4A—B3A | 58.9 (7) | C1C—B6C—B2C | 59.2 (7) |
C1A—B4A—B5A | 58.0 (7) | C1C—B6C—B7C | 105.9 (9) |
B10A—B4A—B5A | 60.7 (7) | B2C—B6C—B7C | 60.0 (8) |
B9A—B4A—B5A | 108.8 (9) | C1C—B6C—B11C | 105.1 (9) |
B3A—B4A—B5A | 107.3 (9) | B2C—B6C—B11C | 107.9 (9) |
C1A—B4A—H4A | 125.1 | B7C—B6C—B11C | 60.3 (7) |
B10A—B4A—H4A | 121.7 | C1C—B6C—B5C | 59.1 (6) |
B9A—B4A—H4A | 122.2 | B2C—B6C—B5C | 109.1 (9) |
B3A—B4A—H4A | 122.3 | B7C—B6C—B5C | 109.9 (9) |
B5A—B4A—H4A | 121.4 | B11C—B6C—B5C | 60.6 (7) |
C1A—B5A—B11A | 104.5 (9) | C1C—B6C—H6C | 124.3 |
C1A—B5A—B6A | 58.7 (7) | B2C—B6C—H6C | 121.3 |
B11A—B5A—B6A | 59.6 (8) | B7C—B6C—H6C | 121.4 |
C1A—B5A—B4A | 59.1 (6) | B11C—B6C—H6C | 122.4 |
B11A—B5A—B4A | 107.7 (9) | B5C—B6C—H6C | 120.3 |
B6A—B5A—B4A | 108.1 (9) | C12C—B7C—B2C | 103.6 (9) |
C1A—B5A—B10A | 104.3 (8) | C12C—B7C—B6C | 103.2 (9) |
B11A—B5A—B10A | 60.7 (8) | B2C—B7C—B6C | 59.2 (7) |
B6A—B5A—B10A | 107.9 (9) | C12C—B7C—B8C | 57.6 (7) |
B4A—B5A—B10A | 58.9 (7) | B2C—B7C—B8C | 60.2 (8) |
C1A—B5A—H5A | 124.7 | B6C—B7C—B8C | 106.7 (10) |
B11A—B5A—H5A | 122.4 | C12C—B7C—B11C | 57.3 (7) |
B6A—B5A—H5A | 121.5 | B2C—B7C—B11C | 107.1 (9) |
B4A—B5A—H5A | 121.7 | B6C—B7C—B11C | 60.2 (7) |
B10A—B5A—H5A | 122.6 | B8C—B7C—B11C | 105.8 (10) |
C1A—B6A—B7A | 105.3 (8) | C12C—B7C—H7C | 126.0 |
C1A—B6A—B11A | 104.3 (10) | B2C—B7C—H7C | 122.7 |
B7A—B6A—B11A | 61.2 (9) | B6C—B7C—H7C | 123.0 |
C1A—B6A—B2A | 59.2 (7) | B8C—B7C—H7C | 122.5 |
B7A—B6A—B2A | 60.6 (8) | B11C—B7C—H7C | 122.4 |
B11A—B6A—B2A | 109.4 (9) | C12C—B8C—B2C | 105.2 (9) |
C1A—B6A—B5A | 58.3 (7) | C12C—B8C—B7C | 60.5 (8) |
B7A—B6A—B5A | 109.0 (10) | B2C—B8C—B7C | 59.4 (8) |
B11A—B6A—B5A | 59.6 (8) | C12C—B8C—B3C | 105.2 (9) |
B2A—B6A—B5A | 108.7 (9) | B2C—B8C—B3C | 60.5 (7) |
C1A—B6A—H6A | 119 (6) | B7C—B8C—B3C | 109.1 (9) |
B7A—B6A—H6A | 128 (6) | C12C—B8C—B9C | 58.9 (8) |
B11A—B6A—H6A | 124 (6) | B2C—B8C—B9C | 107.6 (9) |
B2A—B6A—H6A | 122 (6) | B7C—B8C—B9C | 109.6 (10) |
B5A—B6A—H6A | 116 (5) | B3C—B8C—B9C | 59.4 (7) |
C12A—B7A—B6A | 103.4 (10) | C12C—B8C—H8C | 123.9 |
C12A—B7A—B2A | 103.6 (10) | B2C—B8C—H8C | 122.7 |
B6A—B7A—B2A | 60.2 (7) | B7C—B8C—H8C | 120.3 |
C12A—B7A—B11A | 58.2 (8) | B3C—B8C—H8C | 122.1 |
B6A—B7A—B11A | 59.7 (8) | B9C—B8C—H8C | 121.5 |
B2A—B7A—B11A | 107.9 (10) | C12C—B9C—B4C | 105.4 (10) |
C12A—B7A—B8A | 58.1 (8) | C12C—B9C—B10C | 59.3 (9) |
B6A—B7A—B8A | 108.0 (9) | B4C—B9C—B10C | 59.7 (8) |
B2A—B7A—B8A | 60.1 (7) | C12C—B9C—B3C | 105.1 (10) |
B11A—B7A—B8A | 107.7 (12) | B4C—B9C—B3C | 61.2 (7) |
C12A—B7A—H7A | 125.9 | B10C—B9C—B3C | 108.8 (9) |
B6A—B7A—H7A | 122.6 | C12C—B9C—B8C | 57.8 (8) |
B2A—B7A—H7A | 122.4 | B4C—B9C—B8C | 108.7 (9) |
B11A—B7A—H7A | 121.6 | B10C—B9C—B8C | 107.6 (11) |
B8A—B7A—H7A | 121.5 | B3C—B9C—B8C | 60.2 (8) |
C12A—B8A—B3A | 102.4 (9) | C12C—B9C—H9C | 124.7 |
C12A—B8A—B2A | 104.5 (9) | B4C—B9C—H9C | 121.7 |
B3A—B8A—B2A | 60.8 (7) | B10C—B9C—H9C | 121.4 |
C12A—B8A—B7A | 59.7 (8) | B3C—B9C—H9C | 121.6 |
B3A—B8A—B7A | 107.8 (8) | B8C—B9C—H9C | 121.8 |
B2A—B8A—B7A | 59.6 (8) | C12C—B10C—B4C | 104.8 (10) |
C12A—B8A—B9A | 57.4 (8) | C12C—B10C—B9C | 59.0 (8) |
B3A—B8A—B9A | 59.0 (8) | B4C—B10C—B9C | 59.2 (8) |
B2A—B8A—B9A | 108.2 (9) | C12C—B10C—B5C | 105.2 (10) |
B7A—B8A—B9A | 108.2 (10) | B4C—B10C—B5C | 61.1 (7) |
C12A—B8A—H8A | 125.7 | B9C—B10C—B5C | 108.3 (10) |
B3A—B8A—H8A | 123.2 | C12C—B10C—B11C | 57.8 (8) |
B2A—B8A—H8A | 121.9 | B4C—B10C—B11C | 108.9 (9) |
B7A—B8A—H8A | 121.0 | B9C—B10C—B11C | 107.5 (11) |
B9A—B8A—H8A | 121.9 | B5C—B10C—B11C | 60.8 (8) |
C12A—B9A—B3A | 104.1 (10) | C12C—B10C—H10C | 124.9 |
C12A—B9A—B4A | 103.5 (8) | B4C—B10C—H10C | 122.0 |
B3A—B9A—B4A | 60.9 (7) | B9C—B10C—H10C | 121.9 |
C12A—B9A—B10A | 58.0 (7) | B5C—B10C—H10C | 121.5 |
B3A—B9A—B10A | 108.0 (9) | B11C—B10C—H10C | 121.5 |
B4A—B9A—B10A | 59.2 (7) | C12C—B11C—B6C | 104.9 (9) |
C12A—B9A—B8A | 59.1 (8) | C12C—B11C—B10C | 59.2 (8) |
B3A—B9A—B8A | 59.5 (8) | B6C—B11C—B10C | 107.1 (9) |
B4A—B9A—B8A | 108.3 (9) | C12C—B11C—B7C | 60.3 (8) |
B10A—B9A—B8A | 108.1 (9) | B6C—B11C—B7C | 59.4 (7) |
C12A—B9A—H9A | 125.5 | B10C—B11C—B7C | 109.5 (10) |
B3A—B9A—H9A | 122.3 | C12C—B11C—B5C | 105.2 (9) |
B4A—B9A—H9A | 122.5 | B6C—B11C—B5C | 59.8 (7) |
B10A—B9A—H9A | 121.8 | B10C—B11C—B5C | 59.4 (7) |
B8A—B9A—H9A | 121.2 | B7C—B11C—B5C | 108.5 (9) |
C12A—B10A—B4A | 103.8 (9) | C12C—B11C—H11C | 123.9 |
C12A—B10A—B9A | 57.9 (7) | B6C—B11C—H11C | 123.2 |
B4A—B10A—B9A | 59.9 (7) | B10C—B11C—H11C | 121.5 |
C12A—B10A—B5A | 103.8 (10) | B7C—B11C—H11C | 120.4 |
B4A—B10A—B5A | 60.4 (7) | B5C—B11C—H11C | 122.5 |
B9A—B10A—B5A | 107.7 (9) | B11C—C12C—B8C | 113.7 (9) |
C12A—B10A—B11A | 59.1 (7) | B11C—C12C—B9C | 114.0 (10) |
B4A—B10A—B11A | 107.4 (10) | B8C—C12C—B9C | 63.3 (8) |
B9A—B10A—B11A | 107.6 (10) | B11C—C12C—B10C | 63.0 (8) |
B5A—B10A—B11A | 58.9 (7) | B8C—C12C—B10C | 114.1 (10) |
C12A—B10A—H10A | 125.3 | B9C—C12C—B10C | 61.7 (8) |
B4A—B10A—H10A | 122.5 | B11C—C12C—B7C | 62.4 (8) |
B9A—B10A—H10A | 121.8 | B8C—C12C—B7C | 61.9 (8) |
B5A—B10A—H10A | 122.8 | B9C—C12C—B7C | 114.3 (9) |
B11A—B10A—H10A | 121.8 | B10C—C12C—B7C | 114.4 (9) |
C12A—B11A—B6A | 104.1 (10) | B11C—C12C—H12C | 118.1 |
C12A—B11A—B5A | 103.7 (10) | B8C—C12C—H12C | 118.2 |
B6A—B11A—B5A | 60.8 (8) | B9C—C12C—H12C | 118.0 |
C12A—B11A—B7A | 59.7 (8) | B10C—C12C—H12C | 118.0 |
B6A—B11A—B7A | 59.1 (8) | B7C—C12C—H12C | 118.1 |
B5A—B11A—B7A | 108.3 (11) | B4D—C1D—B3D | 62.1 (6) |
C12A—B11A—B10A | 57.3 (8) | B4D—C1D—B6D | 113.3 (8) |
B6A—B11A—B10A | 108.8 (10) | B3D—C1D—B6D | 113.4 (8) |
B5A—B11A—B10A | 60.5 (8) | B4D—C1D—B2D | 113.8 (7) |
B7A—B11A—B10A | 108.4 (10) | B3D—C1D—B2D | 62.6 (6) |
C12A—B11A—H11A | 125.6 | B6D—C1D—B2D | 62.0 (6) |
B6A—B11A—H11A | 122.3 | B4D—C1D—B5D | 63.1 (6) |
B5A—B11A—H11A | 122.2 | B3D—C1D—B5D | 113.5 (7) |
B7A—B11A—H11A | 121.1 | B6D—C1D—B5D | 61.0 (7) |
B10A—B11A—H11A | 121.3 | B2D—C1D—B5D | 112.4 (8) |
B9A—C12A—B10A | 64.1 (8) | B4D—C1D—Hg2 | 120.0 (7) |
B9A—C12A—B8A | 63.5 (8) | B3D—C1D—Hg2 | 116.9 (6) |
B10A—C12A—B8A | 116.7 (9) | B6D—C1D—Hg2 | 118.6 (6) |
B9A—C12A—B11A | 116.3 (9) | B2D—C1D—Hg2 | 115.7 (7) |
B10A—C12A—B11A | 63.5 (8) | B5D—C1D—Hg2 | 121.5 (6) |
B8A—C12A—B11A | 114.3 (10) | C1D—B2D—B6D | 58.5 (6) |
B9A—C12A—B7A | 115.4 (10) | C1D—B2D—B3D | 58.1 (6) |
B10A—C12A—B7A | 115.6 (9) | B6D—B2D—B3D | 106.9 (8) |
B8A—C12A—B7A | 62.2 (8) | C1D—B2D—B8D | 104.4 (8) |
B11A—C12A—B7A | 62.1 (8) | B6D—B2D—B8D | 106.8 (9) |
B9A—C12A—H12A | 116.3 | B3D—B2D—B8D | 60.2 (7) |
B10A—C12A—H12A | 116.1 | C1D—B2D—B7D | 105.0 (9) |
B8A—C12A—H12A | 117.5 | B6D—B2D—B7D | 60.4 (7) |
B11A—C12A—H12A | 117.7 | B3D—B2D—B7D | 107.1 (10) |
B7A—C12A—H12A | 118.1 | B8D—B2D—B7D | 58.7 (7) |
B2B—C1B—B3B | 62.4 (7) | C1D—B2D—H2D | 124.6 |
B2B—C1B—B5B | 114.1 (8) | B6D—B2D—H2D | 122.0 |
B3B—C1B—B5B | 115.2 (8) | B3D—B2D—H2D | 122.1 |
B2B—C1B—B4B | 114.6 (8) | B8D—B2D—H2D | 123.0 |
B3B—C1B—B4B | 62.8 (6) | B7D—B2D—H2D | 122.6 |
B5B—C1B—B4B | 63.7 (7) | C1D—B3D—B4D | 58.1 (6) |
B2B—C1B—B6B | 62.8 (6) | C1D—B3D—B9D | 105.3 (8) |
B3B—C1B—B6B | 115.3 (8) | B4D—B3D—B9D | 60.9 (7) |
B5B—C1B—B6B | 62.6 (7) | C1D—B3D—B2D | 59.3 (6) |
B4B—C1B—B6B | 116.0 (8) | B4D—B3D—B2D | 107.8 (8) |
B2B—C1B—Hg1 | 114.6 (6) | B9D—B3D—B2D | 107.6 (9) |
B3B—C1B—Hg1 | 118.0 (6) | C1D—B3D—B8D | 105.0 (8) |
B5B—C1B—Hg1 | 119.4 (7) | B4D—B3D—B8D | 107.8 (8) |
B4B—C1B—Hg1 | 120.9 (7) | B9D—B3D—B8D | 59.2 (8) |
B6B—C1B—Hg1 | 114.3 (7) | B2D—B3D—B8D | 59.9 (7) |
C1B—B2B—B7B | 105.2 (7) | C1D—B3D—H3D | 124.4 |
C1B—B2B—B8B | 104.9 (8) | B4D—B3D—H3D | 121.5 |
B7B—B2B—B8B | 60.8 (7) | B9D—B3D—H3D | 122.2 |
C1B—B2B—B3B | 59.3 (6) | B2D—B3D—H3D | 121.6 |
B7B—B2B—B3B | 109.0 (8) | B8D—B3D—H3D | 122.7 |
B8B—B2B—B3B | 59.8 (7) | C1D—B4D—B3D | 59.8 (6) |
C1B—B2B—B6B | 59.5 (6) | C1D—B4D—B9D | 105.6 (8) |
B7B—B2B—B6B | 60.2 (6) | B3D—B4D—B9D | 59.7 (7) |
B8B—B2B—B6B | 109.4 (8) | C1D—B4D—B5D | 59.9 (7) |
B3B—B2B—B6B | 110.0 (8) | B3D—B4D—B5D | 109.1 (8) |
C1B—B2B—H2B | 124.6 | B9D—B4D—B5D | 107.1 (9) |
B7B—B2B—H2B | 121.9 | C1D—B4D—B10D | 105.2 (9) |
B8B—B2B—H2B | 122.1 | B3D—B4D—B10D | 108.4 (8) |
B3B—B2B—H2B | 120.7 | B9D—B4D—B10D | 60.4 (7) |
B6B—B2B—H2B | 120.3 | B5D—B4D—B10D | 58.3 (7) |
C1B—B3B—B9B | 104.1 (8) | C1D—B4D—H4D | 123.5 |
C1B—B3B—B8B | 104.3 (9) | B3D—B4D—H4D | 120.8 |
B9B—B3B—B8B | 60.8 (7) | B9D—B4D—H4D | 122.6 |
C1B—B3B—B2B | 58.2 (6) | B5D—B4D—H4D | 121.8 |
B9B—B3B—B2B | 108.4 (9) | B10D—B4D—H4D | 122.7 |
B8B—B3B—B2B | 60.0 (7) | C1D—B5D—B10D | 105.1 (8) |
C1B—B3B—B4B | 58.8 (6) | C1D—B5D—B6D | 59.0 (7) |
B9B—B3B—B4B | 59.2 (7) | B10D—B5D—B6D | 108.5 (9) |
B8B—B3B—B4B | 108.0 (8) | C1D—B5D—B11D | 105.7 (9) |
B2B—B3B—B4B | 107.8 (9) | B10D—B5D—B11D | 60.4 (8) |
C1B—B3B—H3B | 125.3 | B6D—B5D—B11D | 60.4 (8) |
B9B—B3B—H3B | 122.3 | C1D—B5D—B4D | 57.0 (6) |
B8B—B3B—H3B | 122.1 | B10D—B5D—B4D | 61.1 (7) |
B2B—B3B—H3B | 121.4 | B6D—B5D—B4D | 106.7 (8) |
B4B—B3B—H3B | 121.7 | B11D—B5D—B4D | 108.6 (8) |
C1B—B4B—B9B | 104.1 (8) | C1D—B5D—H5D | 124.9 |
C1B—B4B—B10B | 103.9 (9) | B10D—B5D—H5D | 121.5 |
B9B—B4B—B10B | 60.8 (7) | B6D—B5D—H5D | 121.7 |
C1B—B4B—B3B | 58.5 (6) | B11D—B5D—H5D | 121.5 |
B9B—B4B—B3B | 59.5 (6) | B4D—B5D—H5D | 122.1 |
B10B—B4B—B3B | 107.9 (9) | C1D—B6D—B5D | 60.1 (7) |
C1B—B4B—B5B | 58.1 (6) | C1D—B6D—B11D | 106.3 (9) |
B9B—B4B—B5B | 107.7 (9) | B5D—B6D—B11D | 60.1 (8) |
B10B—B4B—B5B | 59.3 (7) | C1D—B6D—B2D | 59.4 (6) |
B3B—B4B—B5B | 107.1 (9) | B5D—B6D—B2D | 109.5 (9) |
C1B—B4B—H4B | 125.4 | B11D—B6D—B2D | 108.5 (9) |
B9B—B4B—H4B | 122.3 | C1D—B6D—B7D | 105.7 (8) |
B10B—B4B—H4B | 122.4 | B5D—B6D—B7D | 107.7 (10) |
B3B—B4B—H4B | 121.8 | B11D—B6D—B7D | 59.2 (8) |
B5B—B4B—H4B | 122.2 | B2D—B6D—B7D | 60.4 (7) |
C1B—B5B—B11B | 104.7 (8) | C1D—B6D—H6D | 123.4 |
C1B—B5B—B10B | 103.8 (8) | B5D—B6D—H6D | 120.9 |
B11B—B5B—B10B | 60.4 (8) | B11D—B6D—H6D | 122.3 |
C1B—B5B—B6B | 59.0 (6) | B2D—B6D—H6D | 120.7 |
B11B—B5B—B6B | 61.1 (7) | B7D—B6D—H6D | 122.7 |
B10B—B5B—B6B | 109.5 (9) | C12D—B7D—B8D | 58.5 (8) |
C1B—B5B—B4B | 58.2 (6) | C12D—B7D—B11D | 59.1 (8) |
B11B—B5B—B4B | 107.5 (9) | B8D—B7D—B11D | 108.5 (10) |
B10B—B5B—B4B | 59.1 (7) | C12D—B7D—B2D | 104.5 (9) |
B6B—B5B—B4B | 108.5 (8) | B8D—B7D—B2D | 60.4 (8) |
C1B—B5B—H5B | 125.3 | B11D—B7D—B2D | 107.7 (9) |
B11B—B5B—H5B | 122.1 | C12D—B7D—B6D | 103.6 (9) |
B10B—B5B—H5B | 122.4 | B8D—B7D—B6D | 107.2 (9) |
B6B—B5B—H5B | 120.2 | B11D—B7D—B6D | 59.5 (8) |
B4B—B5B—H5B | 122.1 | B2D—B7D—B6D | 59.2 (7) |
C1B—B6B—B7B | 103.1 (9) | C12D—B7D—H7D | 125.1 |
C1B—B6B—B2B | 57.7 (6) | B8D—B7D—H7D | 121.3 |
B7B—B6B—B2B | 59.3 (6) | B11D—B7D—H7D | 121.2 |
C1B—B6B—B5B | 58.5 (6) | B2D—B7D—H7D | 122.5 |
B7B—B6B—B5B | 106.8 (9) | B6D—B7D—H7D | 123.5 |
B2B—B6B—B5B | 106.6 (9) | C12D—B8D—B9D | 59.2 (8) |
C1B—B6B—B11B | 102.2 (9) | C12D—B8D—B7D | 58.5 (8) |
B7B—B6B—B11B | 59.9 (7) | B9D—B8D—B7D | 108.5 (9) |
B2B—B6B—B11B | 106.0 (9) | C12D—B8D—B2D | 104.8 (8) |
B5B—B6B—B11B | 58.4 (7) | B9D—B8D—B2D | 107.7 (8) |
C1B—B6B—H6B | 125.9 | B7D—B8D—B2D | 60.9 (8) |
B7B—B6B—H6B | 122.9 | C12D—B8D—B3D | 104.3 (8) |
B2B—B6B—H6B | 122.5 | B9D—B8D—B3D | 59.2 (7) |
B5B—B6B—H6B | 122.3 | B7D—B8D—B3D | 108.6 (8) |
B11B—B6B—H6B | 123.9 | B2D—B8D—B3D | 59.9 (6) |
C12B—B7B—B2B | 103.5 (8) | C12D—B8D—H8D | 124.9 |
C12B—B7B—B6B | 104.6 (8) | B9D—B8D—H8D | 121.6 |
B2B—B7B—B6B | 60.5 (6) | B7D—B8D—H8D | 120.8 |
C12B—B7B—B8B | 58.3 (7) | B2D—B8D—H8D | 122.2 |
B2B—B7B—B8B | 59.7 (7) | B3D—B8D—H8D | 122.7 |
B6B—B7B—B8B | 108.7 (8) | C12D—B9D—B8D | 58.3 (8) |
C12B—B7B—B11B | 57.4 (7) | C12D—B9D—B3D | 105.5 (10) |
B2B—B7B—B11B | 107.6 (8) | B8D—B9D—B3D | 61.6 (8) |
B6B—B7B—B11B | 60.6 (7) | C12D—B9D—B4D | 104.5 (8) |
B8B—B7B—B11B | 106.9 (9) | B8D—B9D—B4D | 108.4 (9) |
C12B—B7B—H7B | 125.8 | B3D—B9D—B4D | 59.4 (7) |
B2B—B7B—H7B | 122.7 | C12D—B9D—B10D | 58.0 (7) |
B6B—B7B—H7B | 121.5 | B8D—B9D—B10D | 107.5 (9) |
B8B—B7B—H7B | 121.6 | B3D—B9D—B10D | 108.1 (9) |
B11B—B7B—H7B | 122.1 | B4D—B9D—B10D | 60.3 (7) |
C12B—B8B—B3B | 104.4 (8) | C12D—B9D—H9D | 125.0 |
C12B—B8B—B2B | 103.7 (8) | B8D—B9D—H9D | 121.1 |
B3B—B8B—B2B | 60.2 (7) | B3D—B9D—H9D | 121.7 |
C12B—B8B—B9B | 59.1 (7) | B4D—B9D—H9D | 122.5 |
B3B—B8B—B9B | 59.6 (7) | B10D—B9D—H9D | 121.8 |
B2B—B8B—B9B | 107.6 (8) | C12D—B10D—B5D | 104.8 (10) |
C12B—B8B—B7B | 58.8 (7) | C12D—B10D—B11D | 58.7 (8) |
B3B—B8B—B7B | 108.3 (9) | B5D—B10D—B11D | 60.2 (8) |
B2B—B8B—B7B | 59.5 (7) | C12D—B10D—B4D | 103.6 (9) |
B9B—B8B—B7B | 108.7 (9) | B5D—B10D—B4D | 60.6 (7) |
C12B—B8B—H8B | 125.1 | B11D—B10D—B4D | 108.1 (10) |
B3B—B8B—H8B | 122.3 | C12D—B10D—B9D | 58.0 (7) |
B2B—B8B—H8B | 123.0 | B5D—B10D—B9D | 108.0 (9) |
B9B—B8B—H8B | 121.3 | B11D—B10D—B9D | 107.5 (10) |
B7B—B8B—H8B | 121.1 | B4D—B10D—B9D | 59.2 (7) |
C12B—B9B—B4B | 104.1 (9) | C12D—B10D—H10D | 125.3 |
C12B—B9B—B3B | 103.8 (9) | B5D—B10D—H10D | 121.9 |
B4B—B9B—B3B | 61.2 (7) | B11D—B10D—H10D | 121.4 |
C12B—B9B—B8B | 58.2 (7) | B4D—B10D—H10D | 122.7 |
B4B—B9B—B8B | 108.6 (9) | B9D—B10D—H10D | 122.1 |
B3B—B9B—B8B | 59.6 (7) | C12D—B11D—B5D | 104.1 (9) |
C12B—B9B—B10B | 58.1 (7) | C12D—B11D—B7D | 58.1 (8) |
B4B—B9B—B10B | 60.1 (7) | B5D—B11D—B7D | 108.9 (10) |
B3B—B9B—B10B | 108.7 (9) | C12D—B11D—B10D | 58.7 (8) |
B8B—B9B—B10B | 107.6 (10) | B5D—B11D—B10D | 59.4 (8) |
C12B—B9B—H9B | 125.8 | B7D—B11D—B10D | 108.0 (10) |
B4B—B9B—H9B | 121.8 | C12D—B11D—B6D | 104.3 (10) |
B3B—B9B—H9B | 122.1 | B5D—B11D—B6D | 59.5 (8) |
B8B—B9B—H9B | 121.6 | B7D—B11D—B6D | 61.3 (8) |
B10B—B9B—H9B | 121.5 | B10D—B11D—B6D | 107.0 (10) |
C12B—B10B—B4B | 104.1 (8) | C12D—B11D—H11D | 125.3 |
C12B—B10B—B11B | 57.9 (8) | B5D—B11D—H11D | 122.5 |
B4B—B10B—B11B | 108.4 (9) | B7D—B11D—H11D | 120.7 |
C12B—B10B—B5B | 103.2 (9) | B10D—B11D—H11D | 122.0 |
B4B—B10B—B5B | 61.6 (7) | B6D—B11D—H11D | 122.5 |
B11B—B10B—B5B | 59.1 (7) | B7D—C12D—B8D | 63.0 (8) |
C12B—B10B—B9B | 59.0 (7) | B7D—C12D—B9D | 115.1 (10) |
B4B—B10B—B9B | 59.1 (7) | B8D—C12D—B9D | 62.5 (8) |
B11B—B10B—B9B | 107.8 (9) | B7D—C12D—B10D | 115.2 (9) |
B5B—B10B—B9B | 108.1 (8) | B8D—C12D—B10D | 115.8 (9) |
C12B—B10B—H10B | 125.7 | B9D—C12D—B10D | 64.0 (8) |
B4B—B10B—H10B | 122.0 | B7D—C12D—B11D | 62.8 (8) |
B11B—B10B—H10B | 121.8 | B8D—C12D—B11D | 115.3 (10) |
B5B—B10B—H10B | 122.5 | B9D—C12D—B11D | 115.6 (9) |
B9B—B10B—H10B | 121.5 | B10D—C12D—B11D | 62.6 (8) |
C12B—B11B—B5B | 105.2 (10) | B7D—C12D—H12D | 117.6 |
C12B—B11B—B10B | 59.0 (8) | B8D—C12D—H12D | 117.3 |
B5B—B11B—B10B | 60.6 (8) | B9D—C12D—H12D | 117.1 |
C12B—B11B—B7B | 59.1 (7) | B10D—C12D—H12D | 116.9 |
B5B—B11B—B7B | 108.3 (8) | B11D—C12D—H12D | 117.5 |
B10B—B11B—B7B | 108.9 (10) | C1—O1—C4 | 106.1 (9) |
C12B—B11B—B6B | 105.1 (8) | O1—C1—C2 | 107.1 (11) |
B5B—B11B—B6B | 60.6 (7) | O1—C1—H1A | 110.3 |
B10B—B11B—B6B | 109.3 (9) | C2—C1—H1A | 110.3 |
B7B—B11B—B6B | 59.6 (7) | O1—C1—H1B | 110.3 |
C12B—B11B—H11B | 124.5 | C2—C1—H1B | 110.3 |
B5B—B11B—H11B | 122.0 | H1A—C1—H1B | 108.5 |
B10B—B11B—H11B | 120.6 | C3—C2—C1 | 104.2 (11) |
B7B—B11B—H11B | 121.3 | C3—C2—H2E | 110.9 |
B6B—B11B—H11B | 122.0 | C1—C2—H2E | 110.9 |
B11B—C12B—B10B | 63.2 (8) | C3—C2—H2F | 110.9 |
B11B—C12B—B8B | 115.7 (8) | C1—C2—H2F | 110.9 |
B10B—C12B—B8B | 115.4 (9) | H2E—C2—H2F | 108.9 |
B11B—C12B—B7B | 63.4 (7) | C4—C3—C2 | 106.2 (13) |
B10B—C12B—B7B | 115.9 (9) | C4—C3—H3E | 110.5 |
B8B—C12B—B7B | 62.9 (7) | C2—C3—H3E | 110.5 |
B11B—C12B—B9B | 115.3 (9) | C4—C3—H3F | 110.5 |
B10B—C12B—B9B | 62.9 (8) | C2—C3—H3F | 110.5 |
B8B—C12B—B9B | 62.7 (7) | H3E—C3—H3F | 108.7 |
B7B—C12B—B9B | 115.1 (8) | O1—C4—C3 | 106.4 (11) |
B11B—C12B—H12B | 117.0 | O1—C4—H4E | 110.5 |
B10B—C12B—H12B | 117.1 | C3—C4—H4E | 110.5 |
B8B—C12B—H12B | 117.4 | O1—C4—H4F | 110.5 |
B7B—C12B—H12B | 117.1 | C3—C4—H4F | 110.5 |
B9B—C12B—H12B | 117.6 | H4E—C4—H4F | 108.6 |
C1D—Hg2—C1C | 177.2 (4) | C4'—O2—C1' | 108.4 (8) |
B2C—C1C—B3C | 63.5 (7) | O2—C1'—C2' | 105.0 (10) |
B2C—C1C—B6C | 61.4 (7) | O2—C1'—H1'A | 110.7 |
B3C—C1C—B6C | 114.4 (8) | C2'—C1'—H1'A | 110.7 |
B2C—C1C—B5C | 114.1 (9) | O2—C1'—H1'B | 110.7 |
B3C—C1C—B5C | 115.0 (8) | C2'—C1'—H1'B | 110.7 |
B6C—C1C—B5C | 62.8 (7) | H1'A—C1'—H1'B | 108.8 |
B2C—C1C—B4C | 114.2 (8) | C3'—C2'—C1' | 106.4 (12) |
B3C—C1C—B4C | 62.6 (7) | C3'—C2'—H2'A | 110.5 |
B6C—C1C—B4C | 113.6 (8) | C1'—C2'—H2'A | 110.5 |
B5C—C1C—B4C | 62.4 (7) | C3'—C2'—H2'B | 110.5 |
B2C—C1C—Hg2 | 117.0 (7) | C1'—C2'—H2'B | 110.5 |
B3C—C1C—Hg2 | 118.1 (7) | H2'A—C2'—H2'B | 108.6 |
B6C—C1C—Hg2 | 116.9 (7) | C4'—C3'—C2' | 103.4 (12) |
B5C—C1C—Hg2 | 117.8 (7) | C4'—C3'—H3'A | 111.1 |
B4C—C1C—Hg2 | 120.1 (7) | C2'—C3'—H3'A | 111.1 |
C1C—B2C—B6C | 59.3 (7) | C4'—C3'—H3'B | 111.1 |
C1C—B2C—B7C | 106.6 (9) | C2'—C3'—H3'B | 111.1 |
B6C—B2C—B7C | 60.8 (8) | H3'A—C3'—H3'B | 109.0 |
C1C—B2C—B8C | 104.6 (8) | O2—C4'—C3' | 107.5 (10) |
B6C—B2C—B8C | 108.1 (9) | O2—C4'—H4'B | 110.2 |
B7C—B2C—B8C | 60.4 (7) | C3'—C4'—H4'B | 110.2 |
C1C—B2C—B3C | 58.3 (6) | O2—C4'—H4'A | 110.2 |
B6C—B2C—B3C | 108.4 (9) | C3'—C4'—H4'A | 110.2 |
B7C—B2C—B3C | 109.6 (9) | H4'B—C4'—H4'A | 108.5 |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | [Hg(C2B10H11)2]·CH2Cl2 | [Hg(C2B10H11)2]·C4H8O |
Mr | 571.94 | 559.11 |
Crystal system, space group | Triclinic, P1 | Monoclinic, P21/n |
Temperature (K) | 100 | 173 |
a, b, c (Å) | 12.4673 (18), 13.5634 (18), 13.5910 (18) | 12.186 (7), 19.548 (12), 19.700 (12) |
α, β, γ (°) | 105.642 (4), 101.243 (4), 90.381 (5) | 90, 90.055 (10), 90 |
V (Å3) | 2166.4 (5) | 4693 (5) |
Z | 4 | 8 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 7.34 | 6.56 |
Crystal size (mm) | 0.25 × 0.20 × 0.08 | 0.35 × 0.30 × 0.12 |
Data collection | ||
Diffractometer | Bruker SMART 1K CCD area-detector diffractometer | Bruker SMART 1K CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1997) | Multi-scan (SADABS; Bruker, 1997) |
Tmin, Tmax | 0.298, 0.556 | 0.175, 0.455 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 44711, 17966, 15490 | 34377, 10466, 8750 |
Rint | 0.031 | 0.050 |
(sin θ/λ)max (Å−1) | 0.833 | 0.650 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.062, 1.05 | 0.044, 0.107, 1.06 |
No. of reflections | 17966 | 10466 |
No. of parameters | 506 | 557 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.18, −2.03 | 3.05, −3.38 |
Computer programs: SMART (Bruker, 1997), SMART, SAINT, SHELXTL (Sheldrick, 1997), SHELXTL and WinGX (Farrugia, 1999).
The observation that linear mercury(II) complexes and mercuracycles interact with a variety of substrates (Beauchamp et al., 1986; Wuest & Zacharie, 1987), including CO, NO and N2 (Tevault et al., 1977), has led to the development of Hg-derived molecular recognition motifs (Wuest & Zacharie, 1987) and ion transport mediators (Zheng et al., 1993). Hawthorne and coworkers have extensively investigated the chemistry of carborane-derived tri- and tetrameric mercury macrocycles (Yang et al., 1991; Zheng et al., 1995; Hawthorne & Zheng, 1997), including studying their potential as catalysts (Yang et al., 1991) and their ability to coordinate different anions (Zinn et al., 1999).
We observed the Lewis acidic nature of simple Hg-carborane compounds during a course of experiments involving the use of RHgR complexes (R is ortho- or para-carborane) as reagents for the synthesis of arylcarborane derivatives (Tsvetkov et al., 2000). Compounds (I) and (II) were synthesized using a modification of the procedure reported by Zakharkin et al. (1965), in which HgCl2 was reacted with the corresponding mono-lithiated anions of ortho- and para-carborane in ether. \sch
Crystals of (I) decompose slowly upon removal from the mother liquor and are sensitive to prolonged exposure to light. The crystal structure of (I) has two independent molecules, (IA) and (IB), in the asymmetric unit. Both molecules exhibit near-linear geometry, with the C—Hg—C angles being 175.74 (9) and 172.78 (8)°, respectively (Fig. 1). The average Hg—C bond distances are within normal ranges, at 2.097 (2) and 2.095 (2) Å for molecules (IA) and (IB), respectively (Wu et al., 1998; Potenza & Lipscomb, 1964). All four carborane cages are slightly distorted icosahedra, with average B—B bond distances of 1.777 (4) Å in (IA) and 1.781 (4) Å in (IB), and average B—C bond distances of 1.717 (4) Å in (IA) and 1.712 (3) Å in (IB). The C atoms of each cage were identified based on the shorter C—C bond lengths of 1.671 (4) and 1.647 (3) Å for (IA) and (IB), respectively. The crystal packing of (I) shows alternating layers of solvent and Hg-carborane units (Fig. 2).
Compound (II) (Fig. 3) is organized into a lattice comprised of two crystallographically independent molecules, (IIA) and (IIB), containing channels of tetrahydrofuran (THF) solvent molecules along the b axis. Both molecules have C—Hg—C bond angles which do not deviate significantly from linearity [173.0 (4)° for (IIA) and 177.2 (4)° for (IIB)]. The average Hg—C bond lengths for molecules (IIA) and (IIB) [2.073 (9) and 2.088 (10) Å, respectively] are slightly shorter than the same bonds in the ortho-carborane derivative, (I). The four carborane cages are essentially symmetrical icosahedral polyhedra, with average B—B distances of 1.771 (18) Å for molecule (IIA) and 1.765 (18) Å for molecule (IIB), and average B—C bond lengths of 1.706 (16) and 1.700 (16) Å, respectively.
The interaction of the CH2Cl2 solvent with Hg in (I) is surprisingly pronounced. Both independent molecules of (I) show the Cl atoms of the CH2Cl2 closely approaching the Hg metal center, with Hg—Cl distances of 3.317 (1) and 3.389 (1) Å for molecule (IA), and 3.248 (1) and 3.252 (2) Å for molecule (IB). These distances are smaller than the van der Waals distance of 3.53 Å (Pauling, 1960) and similar to the intramolecular coordination of Cl to Hg in 1-methylmercury-2-chloromethyl-ortho-carborane (Bokii et al., 1978).
In compound (II), one of the two independent molecules is closely associated with the O atom of the THF solvent. The Hg—O distance of 2.850 (7) Å is again much smaller than the van der Waals sum of 3.13 Å (Pauling, 1960). Hawthorne and coworkers have reported pronounced interactions between the coordinating solvents ethanol and acetonitrile with the Hg atoms of Hg-carborane derivatives. The Hg—O(ethanol) distances in an acyclic mercury compound containing two Hg atoms and three carborane units were 2.85 (2) and 2.89 (2) Å (Zheng et al., 1995), while the Hg—N(acetonitrile) distances in [9]mercuracarborand-3 Query spelling, having the general formula (C2B10H10Hg)3, ranged between 2.74 (3) and 3.13 (2) Å (Yang et al., 1993).
This report describes the first X-ray structure determination of simple bis(carboran-1-yl)mercury(II) derivatives. The reported structures demonstrate pronounced interactions between the lattice solvent and the (Lewis) acidic HgII centers. The interaction between the Hg center and the dichloromethane Cl atoms is of particular interest, as it implies that Hg-carborane derivatives, including mercuramacrocycles, could potentially be used as recognition motifs for chlorocarbon solvents.