Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010100436X/gd1146sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010100436X/gd1146IIIsup2.hkl |
CCDC reference: 166970
MeCN containing a trace of water was added to a toluene solution of tantalum-tris(N,N-dimethylamide)-1,2-dicarbaundecaborate and brought to reflux, and heating was continued for 24 h. This solution was cooled and layered with pentane. Interdiffusion of the two solvents over a period of 2 weeks afforded bright yellow crystals of (III).
H atoms were included as riding atoms, with B—H = 1.12 Å and C—H = 0.98–1.00 Å. The Flack parameter (Flack, 1983) indicates racemic twinning.
Data collection: SMART-NT (Bruker, 1998); cell refinement: SMART-NT; data reduction: SAINT-NT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Bruker, 1998).
Fig. 1. The molecular structure of (III), with displacement ellipsoids drawn at the 40% probability level and H atoms shown as small spheres of arbitrary radii. |
[Ta2O(C2B9H11)2(C4H9N2)4]·0.5CH2Cl2 | F(000) = 998 |
Mr = 1025.69 | Dx = 1.554 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.414 (3) Å | Cell parameters from 616 reflections |
b = 10.769 (3) Å | θ = 13.7–19.1° |
c = 17.863 (5) Å | µ = 5.08 mm−1 |
β = 93.303 (6)° | T = 150 K |
V = 2192.1 (11) Å3 | Rectangular prism, colourless |
Z = 2 | 0.22 × 0.12 × 0.08 mm |
Bruker SMART CCD area-detector diffractometer | 10933 independent reflections |
Radiation source: fine-focus sealed tube | 9396 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
ω scans | θmax = 30.4°, θmin = 1.1° |
Absorption correction: integration (XPREP in SHELXTL-NT; Bruker, 1998) | h = −15→15 |
Tmin = 0.381, Tmax = 0.690 | k = −15→14 |
26944 measured reflections | l = −25→24 |
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)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.095 | w = 1/[σ2(Fo2) + (0.0485P)2 + 0.8328P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
10933 reflections | Δρmax = 1.34 e Å−3 |
470 parameters | Δρmin = −0.76 e Å−3 |
3 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.41 (1) |
[Ta2O(C2B9H11)2(C4H9N2)4]·0.5CH2Cl2 | V = 2192.1 (11) Å3 |
Mr = 1025.69 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 11.414 (3) Å | µ = 5.08 mm−1 |
b = 10.769 (3) Å | T = 150 K |
c = 17.863 (5) Å | 0.22 × 0.12 × 0.08 mm |
β = 93.303 (6)° |
Bruker SMART CCD area-detector diffractometer | 10933 independent reflections |
Absorption correction: integration (XPREP in SHELXTL-NT; Bruker, 1998) | 9396 reflections with I > 2σ(I) |
Tmin = 0.381, Tmax = 0.690 | Rint = 0.042 |
26944 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.095 | Δρmax = 1.34 e Å−3 |
S = 1.10 | Δρmin = −0.76 e Å−3 |
10933 reflections | Absolute structure: Flack (1983) |
470 parameters | Absolute structure parameter: 0.41 (1) |
3 restraints |
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 | Occ. (<1) | |
C1A | −0.0730 (8) | 0.3083 (8) | 0.1802 (5) | 0.0332 (17) | |
H1A | 0.0137 | 0.3076 | 0.1920 | 0.040* | |
C2A | −0.1586 (7) | 0.2868 (7) | 0.2444 (5) | 0.0336 (17) | |
H2A | −0.1277 | 0.2729 | 0.2973 | 0.040* | |
TaA | −0.12318 (2) | 0.51696 (3) | 0.235286 (16) | 0.02870 (8) | |
B4A | −0.1295 (8) | 0.4024 (9) | 0.1140 (6) | 0.038 (2) | |
H4A | −0.0767 | 0.4653 | 0.0790 | 0.046* | |
B5A | −0.1197 (10) | 0.2407 (10) | 0.0969 (6) | 0.042 (2) | |
H5A | −0.0629 | 0.2010 | 0.0538 | 0.051* | |
B6A | −0.1345 (10) | 0.1637 (10) | 0.1843 (6) | 0.046 (2) | |
H6A | −0.0879 | 0.0749 | 0.1994 | 0.055* | |
B7A | −0.2769 (10) | 0.1989 (11) | 0.2129 (7) | 0.052 (3) | |
H7A | −0.3254 | 0.1309 | 0.2470 | 0.063* | |
B8A | −0.2822 (8) | 0.3601 (10) | 0.2291 (6) | 0.043 (2) | |
H8A | −0.3375 | 0.3924 | 0.2752 | 0.051* | |
B9A | −0.2704 (8) | 0.4365 (10) | 0.1411 (6) | 0.039 (2) | |
H9A | −0.3199 | 0.5227 | 0.1240 | 0.047* | |
B10A | −0.2505 (10) | 0.3215 (10) | 0.0734 (6) | 0.044 (3) | |
H10A | −0.2813 | 0.3353 | 0.0134 | 0.053* | |
B11A | −0.2575 (11) | 0.1754 (11) | 0.1168 (6) | 0.052 (3) | |
H11A | −0.2944 | 0.0919 | 0.0865 | 0.063* | |
B12A | −0.3490 (9) | 0.2961 (10) | 0.1431 (7) | 0.048 (3) | |
H12A | −0.4462 | 0.2934 | 0.1303 | 0.058* | |
N1A | −0.2063 (5) | 0.5866 (6) | 0.3110 (4) | 0.0355 (15) | |
C3A | −0.2782 (6) | 0.6204 (8) | 0.3613 (5) | 0.0366 (18) | |
C4A | −0.3103 (7) | 0.5348 (9) | 0.4230 (5) | 0.049 (2) | |
H4A1 | −0.2826 | 0.4507 | 0.4125 | 0.074* | |
H4A2 | −0.3957 | 0.5339 | 0.4260 | 0.074* | |
H4A3 | −0.2734 | 0.5637 | 0.4707 | 0.074* | |
N2A | −0.3222 (6) | 0.7322 (7) | 0.3610 (5) | 0.0476 (19) | |
C5A | −0.4113 (8) | 0.7723 (9) | 0.4141 (6) | 0.052 (3) | |
H5A1 | −0.4795 | 0.7170 | 0.4091 | 0.079* | |
H5A2 | −0.4360 | 0.8576 | 0.4024 | 0.079* | |
H5A3 | −0.3769 | 0.7685 | 0.4656 | 0.079* | |
C6A | −0.2883 (9) | 0.8237 (9) | 0.3042 (6) | 0.054 (2) | |
H6A1 | −0.2257 | 0.7889 | 0.2753 | 0.080* | |
H6A2 | −0.2602 | 0.8998 | 0.3294 | 0.080* | |
H6A3 | −0.3565 | 0.8430 | 0.2704 | 0.080* | |
N3A | −0.0867 (6) | 0.6596 (7) | 0.1824 (5) | 0.0410 (17) | |
C7A | −0.0746 (8) | 0.7447 (9) | 0.1302 (5) | 0.044 (2) | |
C8A | −0.1663 (10) | 0.7564 (13) | 0.0671 (7) | 0.071 (3) | |
H8A1 | −0.2243 | 0.6898 | 0.0708 | 0.106* | |
H8A2 | −0.1292 | 0.7499 | 0.0191 | 0.106* | |
H8A3 | −0.2054 | 0.8371 | 0.0701 | 0.106* | |
N4A | 0.0170 (7) | 0.8239 (7) | 0.1370 (4) | 0.0478 (19) | |
C9A | 0.0369 (10) | 0.9218 (11) | 0.0832 (6) | 0.067 (3) | |
H9A1 | −0.0378 | 0.9450 | 0.0573 | 0.101* | |
H9A2 | 0.0911 | 0.8920 | 0.0465 | 0.101* | |
H9A3 | 0.0709 | 0.9943 | 0.1095 | 0.101* | |
C10A | 0.1015 (9) | 0.8145 (10) | 0.1998 (6) | 0.054 (3) | |
H1A1 | 0.1148 | 0.7268 | 0.2123 | 0.082* | |
H1A2 | 0.0716 | 0.8576 | 0.2430 | 0.082* | |
H1A3 | 0.1756 | 0.8526 | 0.1867 | 0.082* | |
O1 | 0.0213 (4) | 0.4767 (6) | 0.2862 (3) | 0.0365 (14) | |
C1B | 0.0807 (6) | 0.6582 (7) | 0.3969 (5) | 0.0325 (17) | |
H1B | 0.0192 | 0.6801 | 0.3569 | 0.039* | |
C2B | 0.0695 (6) | 0.5361 (8) | 0.4452 (4) | 0.0317 (16) | |
H2B | 0.0010 | 0.4790 | 0.4364 | 0.038* | |
TaB | 0.17936 (2) | 0.48489 (3) | 0.331441 (15) | 0.02563 (7) | |
B4B | 0.2228 (7) | 0.6943 (8) | 0.3848 (5) | 0.0271 (17) | |
H4B | 0.2557 | 0.7457 | 0.3357 | 0.033* | |
B5B | 0.1388 (8) | 0.7777 (8) | 0.4510 (5) | 0.0328 (19) | |
H5B | 0.1178 | 0.8788 | 0.4438 | 0.039* | |
B6B | 0.0377 (8) | 0.6775 (9) | 0.4857 (6) | 0.040 (2) | |
H6B | −0.0512 | 0.7103 | 0.5006 | 0.048* | |
B7B | 0.1146 (8) | 0.5579 (10) | 0.5361 (5) | 0.038 (2) | |
H7B | 0.0773 | 0.5113 | 0.5855 | 0.045* | |
B8B | 0.1987 (7) | 0.4748 (9) | 0.4723 (4) | 0.0319 (17) | |
H8B | 0.2156 | 0.3740 | 0.4840 | 0.038* | |
B9B | 0.3036 (7) | 0.5770 (8) | 0.4350 (5) | 0.0285 (18) | |
H9B | 0.3942 | 0.5471 | 0.4219 | 0.034* | |
B10B | 0.2825 (7) | 0.7262 (8) | 0.4759 (5) | 0.0304 (18) | |
H10B | 0.3576 | 0.7923 | 0.4859 | 0.036* | |
B11B | 0.1636 (8) | 0.7138 (9) | 0.5390 (6) | 0.040 (2) | |
H11B | 0.1604 | 0.7708 | 0.5913 | 0.047* | |
B12B | 0.2668 (8) | 0.5888 (9) | 0.5297 (6) | 0.038 (2) | |
H12B | 0.3326 | 0.5639 | 0.5763 | 0.045* | |
N1B | 0.2222 (6) | 0.3181 (6) | 0.3383 (4) | 0.0373 (15) | |
C3B | 0.2489 (7) | 0.1997 (8) | 0.3463 (5) | 0.0386 (19) | |
C4B | 0.1524 (8) | 0.1068 (9) | 0.3386 (6) | 0.052 (2) | |
H4B1 | 0.1538 | 0.0545 | 0.3835 | 0.079* | |
H4B2 | 0.1630 | 0.0547 | 0.2945 | 0.079* | |
H4B3 | 0.0768 | 0.1499 | 0.3327 | 0.079* | |
N2B | 0.3569 (6) | 0.1652 (7) | 0.3604 (5) | 0.0450 (18) | |
C5B | 0.3932 (9) | 0.0381 (9) | 0.3676 (7) | 0.067 (3) | |
H5B1 | 0.3243 | −0.0147 | 0.3728 | 0.100* | |
H5B2 | 0.4469 | 0.0290 | 0.4121 | 0.100* | |
H5B3 | 0.4333 | 0.0134 | 0.3229 | 0.100* | |
C6B | 0.4538 (7) | 0.2565 (9) | 0.3611 (7) | 0.055 (3) | |
H6B1 | 0.4453 | 0.3159 | 0.4019 | 0.083* | |
H6B2 | 0.4512 | 0.3009 | 0.3131 | 0.083* | |
H6B3 | 0.5290 | 0.2131 | 0.3685 | 0.083* | |
N3B | 0.2642 (5) | 0.5332 (6) | 0.2491 (3) | 0.0338 (14) | |
C7B | 0.3439 (6) | 0.5639 (8) | 0.2044 (5) | 0.0353 (17) | |
C8B | 0.4616 (7) | 0.6033 (12) | 0.2364 (6) | 0.058 (3) | |
H8B1 | 0.4611 | 0.6053 | 0.2912 | 0.087* | |
H8B2 | 0.4799 | 0.6862 | 0.2177 | 0.087* | |
H8B3 | 0.5212 | 0.5442 | 0.2213 | 0.087* | |
N4B | 0.3213 (6) | 0.5667 (8) | 0.1314 (4) | 0.0451 (18) | |
C9B | 0.4117 (9) | 0.5870 (15) | 0.0789 (5) | 0.077 (4) | |
H9B1 | 0.4593 | 0.6589 | 0.0949 | 0.115* | |
H9B2 | 0.3750 | 0.6023 | 0.0288 | 0.115* | |
H9B3 | 0.4619 | 0.5132 | 0.0775 | 0.115* | |
C10B | 0.2081 (7) | 0.5310 (11) | 0.0991 (5) | 0.056 (2) | |
H1B1 | 0.1516 | 0.5289 | 0.1383 | 0.083* | |
H1B2 | 0.2134 | 0.4485 | 0.0764 | 0.083* | |
H1B3 | 0.1822 | 0.5913 | 0.0605 | 0.083* | |
Cl1 | 0.4259 (6) | 0.9397 (6) | 0.1466 (4) | 0.087 (2) | 0.50 |
C11 | 0.3818 (11) | 1.0709 (10) | 0.0995 (7) | 0.053 (5) | 0.50 |
H111 | 0.3402 | 1.0458 | 0.0518 | 0.063* | 0.50 |
H112 | 0.4527 | 1.1176 | 0.0868 | 0.063* | 0.50 |
Cl2 | 0.2922 (4) | 1.1695 (6) | 0.1456 (3) | 0.0652 (15) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1A | 0.039 (4) | 0.034 (4) | 0.027 (4) | 0.005 (3) | 0.001 (3) | −0.008 (3) |
C2A | 0.041 (4) | 0.030 (4) | 0.030 (4) | −0.008 (3) | −0.002 (3) | 0.004 (3) |
TaA | 0.02339 (13) | 0.03408 (17) | 0.02845 (15) | −0.00003 (10) | −0.00009 (10) | −0.00364 (12) |
B4A | 0.042 (5) | 0.038 (5) | 0.033 (5) | 0.000 (4) | −0.002 (4) | −0.002 (4) |
B5A | 0.048 (6) | 0.044 (6) | 0.034 (6) | −0.009 (4) | −0.003 (4) | −0.007 (4) |
B6A | 0.061 (6) | 0.036 (5) | 0.039 (6) | −0.007 (5) | −0.003 (5) | −0.005 (4) |
B7A | 0.052 (6) | 0.052 (7) | 0.054 (7) | −0.019 (5) | 0.011 (5) | −0.008 (5) |
B8A | 0.028 (4) | 0.047 (6) | 0.054 (7) | −0.009 (4) | 0.010 (4) | −0.005 (5) |
B9A | 0.028 (4) | 0.051 (6) | 0.037 (5) | −0.009 (4) | −0.007 (4) | 0.006 (4) |
B10A | 0.057 (6) | 0.046 (6) | 0.028 (5) | −0.016 (5) | −0.013 (5) | 0.001 (4) |
B11A | 0.067 (7) | 0.055 (7) | 0.034 (6) | −0.020 (6) | −0.008 (5) | −0.010 (5) |
B12A | 0.038 (5) | 0.049 (6) | 0.056 (7) | −0.013 (4) | −0.010 (5) | −0.003 (5) |
N1A | 0.027 (3) | 0.041 (4) | 0.039 (4) | 0.005 (3) | 0.003 (3) | −0.009 (3) |
C3A | 0.027 (4) | 0.039 (4) | 0.043 (5) | 0.003 (3) | −0.010 (3) | 0.001 (4) |
C4A | 0.047 (5) | 0.043 (5) | 0.058 (6) | 0.008 (4) | 0.010 (4) | 0.014 (4) |
N2A | 0.042 (4) | 0.049 (5) | 0.051 (5) | −0.002 (3) | −0.004 (3) | −0.012 (4) |
C5A | 0.047 (5) | 0.034 (5) | 0.079 (8) | −0.003 (4) | 0.027 (5) | −0.022 (5) |
C6A | 0.061 (6) | 0.036 (5) | 0.065 (7) | −0.004 (4) | 0.016 (5) | 0.009 (5) |
N3A | 0.041 (4) | 0.042 (4) | 0.039 (5) | −0.005 (3) | −0.001 (3) | −0.004 (3) |
C7A | 0.047 (5) | 0.047 (5) | 0.037 (5) | 0.001 (4) | 0.004 (4) | 0.001 (4) |
C8A | 0.057 (7) | 0.092 (9) | 0.062 (8) | −0.001 (6) | −0.006 (6) | 0.016 (7) |
N4A | 0.067 (5) | 0.035 (4) | 0.042 (5) | 0.002 (3) | 0.009 (4) | 0.007 (3) |
C9A | 0.082 (7) | 0.065 (7) | 0.057 (7) | −0.004 (6) | 0.022 (6) | 0.034 (6) |
C10A | 0.057 (6) | 0.045 (6) | 0.059 (7) | −0.018 (5) | −0.013 (5) | 0.008 (5) |
O1 | 0.023 (2) | 0.050 (4) | 0.035 (3) | 0.002 (2) | −0.0056 (19) | −0.013 (3) |
C1B | 0.030 (4) | 0.029 (4) | 0.038 (5) | 0.008 (3) | −0.001 (3) | −0.007 (3) |
C2B | 0.024 (3) | 0.039 (4) | 0.032 (4) | −0.004 (3) | 0.001 (3) | −0.004 (3) |
TaB | 0.02190 (12) | 0.02607 (14) | 0.02867 (15) | 0.00134 (10) | −0.00085 (10) | −0.00454 (11) |
B4B | 0.032 (4) | 0.028 (4) | 0.021 (4) | −0.006 (3) | 0.002 (3) | −0.001 (3) |
B5B | 0.040 (5) | 0.028 (4) | 0.030 (5) | 0.005 (3) | 0.005 (4) | −0.005 (4) |
B6B | 0.033 (5) | 0.043 (5) | 0.045 (6) | 0.005 (4) | 0.010 (4) | −0.004 (4) |
B7B | 0.035 (4) | 0.053 (6) | 0.025 (4) | −0.011 (4) | 0.002 (3) | 0.001 (4) |
B8B | 0.035 (4) | 0.032 (4) | 0.028 (4) | −0.010 (4) | −0.002 (3) | 0.001 (4) |
B9B | 0.022 (4) | 0.028 (4) | 0.035 (5) | −0.001 (3) | −0.009 (3) | −0.003 (3) |
B10B | 0.031 (4) | 0.029 (4) | 0.032 (5) | −0.001 (3) | 0.005 (4) | −0.003 (4) |
B11B | 0.038 (5) | 0.041 (5) | 0.040 (6) | −0.007 (4) | 0.010 (4) | 0.001 (4) |
B12B | 0.037 (5) | 0.036 (5) | 0.039 (5) | −0.007 (4) | −0.003 (4) | 0.004 (4) |
N1B | 0.040 (4) | 0.032 (4) | 0.040 (4) | −0.003 (3) | 0.001 (3) | −0.006 (3) |
C3B | 0.043 (5) | 0.035 (4) | 0.038 (5) | −0.005 (3) | 0.007 (4) | −0.006 (4) |
C4B | 0.046 (5) | 0.039 (5) | 0.073 (7) | −0.016 (4) | 0.004 (5) | −0.001 (5) |
N2B | 0.040 (4) | 0.033 (4) | 0.062 (5) | 0.006 (3) | 0.001 (4) | 0.001 (3) |
C5B | 0.068 (6) | 0.038 (5) | 0.095 (9) | 0.021 (5) | 0.010 (6) | 0.017 (6) |
C6B | 0.031 (4) | 0.043 (5) | 0.092 (8) | 0.002 (4) | −0.004 (5) | 0.005 (5) |
N3B | 0.031 (3) | 0.040 (4) | 0.030 (3) | −0.001 (3) | 0.004 (2) | −0.006 (3) |
C7B | 0.031 (4) | 0.041 (4) | 0.035 (4) | 0.012 (3) | 0.007 (3) | 0.001 (3) |
C8B | 0.035 (5) | 0.092 (8) | 0.048 (6) | −0.005 (5) | 0.000 (4) | 0.011 (6) |
N4B | 0.035 (3) | 0.073 (5) | 0.027 (4) | 0.012 (3) | 0.000 (3) | 0.000 (3) |
C9B | 0.050 (6) | 0.155 (13) | 0.027 (5) | 0.029 (7) | 0.013 (4) | 0.017 (6) |
C10B | 0.048 (5) | 0.075 (7) | 0.042 (5) | 0.002 (5) | −0.007 (4) | −0.003 (5) |
Cl1 | 0.103 (5) | 0.074 (4) | 0.078 (4) | −0.004 (4) | −0.035 (4) | 0.002 (3) |
C11 | 0.055 (10) | 0.070 (12) | 0.033 (9) | −0.053 (10) | 0.005 (8) | −0.009 (8) |
Cl2 | 0.047 (3) | 0.090 (4) | 0.060 (3) | −0.013 (3) | 0.013 (2) | 0.002 (3) |
C1A—C2A | 1.565 (12) | C1B—B4B | 1.694 (11) |
C1A—B4A | 1.660 (13) | C1B—B6B | 1.701 (13) |
C1A—B6A | 1.712 (13) | C1B—B5B | 1.720 (12) |
C1A—B5A | 1.714 (13) | C1B—TaB | 2.504 (7) |
C1A—TaA | 2.531 (8) | C1B—H1B | 1.0001 |
C1A—H1A | 1.0001 | C2B—B8B | 1.663 (11) |
C2A—B8A | 1.626 (13) | C2B—B7B | 1.691 (11) |
C2A—B7A | 1.717 (13) | C2B—B6B | 1.733 (12) |
C2A—B6A | 1.737 (13) | C2B—TaB | 2.510 (7) |
C2A—TaA | 2.518 (8) | C2B—H2B | 1.0001 |
C2A—H2A | 1.0001 | TaB—N1B | 1.863 (7) |
TaA—N1A | 1.855 (6) | TaB—N3B | 1.881 (6) |
TaA—N3A | 1.862 (8) | TaB—B9B | 2.473 (8) |
TaA—O1 | 1.887 (5) | TaB—B4B | 2.487 (8) |
TaA—B9A | 2.466 (9) | TaB—B8B | 2.515 (8) |
TaA—B8A | 2.477 (9) | B4B—B10B | 1.761 (12) |
TaA—B4A | 2.491 (10) | B4B—B9B | 1.777 (12) |
B4A—B9A | 1.746 (14) | B4B—B5B | 1.805 (12) |
B4A—B10A | 1.754 (13) | B4B—H4B | 1.1200 |
B4A—B5A | 1.772 (14) | B5B—B6B | 1.722 (14) |
B4A—H4A | 1.1200 | B5B—B11B | 1.724 (14) |
B5A—B10A | 1.758 (16) | B5B—B10B | 1.764 (12) |
B5A—B11A | 1.778 (16) | B5B—H5B | 1.1200 |
B5A—B6A | 1.785 (16) | B6B—B11B | 1.722 (14) |
B5A—H5A | 1.1200 | B6B—B7B | 1.774 (14) |
B6A—B7A | 1.772 (17) | B6B—H6B | 1.1200 |
B6A—B11A | 1.801 (15) | B7B—B11B | 1.770 (14) |
B6A—H6A | 1.1200 | B7B—B8B | 1.774 (13) |
B7A—B11A | 1.761 (17) | B7B—B12B | 1.779 (12) |
B7A—B8A | 1.762 (16) | B7B—H7B | 1.1200 |
B7A—B12A | 1.792 (17) | B8B—B12B | 1.752 (12) |
B7A—H7A | 1.1200 | B8B—B9B | 1.783 (12) |
B8A—B9A | 1.787 (15) | B8B—H8B | 1.1200 |
B8A—B12A | 1.812 (15) | B9B—B12B | 1.771 (14) |
B8A—H8A | 1.1200 | B9B—B10B | 1.788 (12) |
B9A—B10A | 1.753 (15) | B9B—H9B | 1.1200 |
B9A—B12A | 1.760 (14) | B10B—B12B | 1.780 (13) |
B9A—H9A | 1.1200 | B10B—B11B | 1.819 (13) |
B10A—B12A | 1.746 (16) | B10B—H10B | 1.1200 |
B10A—B11A | 1.758 (16) | B11B—B12B | 1.803 (14) |
B10A—H10A | 1.1200 | B11B—H11B | 1.1200 |
B11A—B12A | 1.748 (18) | B12B—H12B | 1.1200 |
B11A—H11A | 1.1200 | N1B—C3B | 1.318 (11) |
B12A—H12A | 1.1200 | C3B—N2B | 1.298 (11) |
N1A—C3A | 1.303 (10) | C3B—C4B | 1.489 (11) |
C3A—N2A | 1.305 (11) | C4B—H4B1 | 0.9800 |
C3A—C4A | 1.499 (12) | C4B—H4B2 | 0.9800 |
C4A—H4A1 | 0.9800 | C4B—H4B3 | 0.9800 |
C4A—H4A2 | 0.9800 | N2B—C5B | 1.433 (11) |
C4A—H4A3 | 0.9800 | N2B—C6B | 1.480 (11) |
N2A—C6A | 1.481 (13) | C5B—H5B1 | 0.9800 |
N2A—C5A | 1.494 (11) | C5B—H5B2 | 0.9800 |
C5A—H5A1 | 0.9800 | C5B—H5B3 | 0.9800 |
C5A—H5A2 | 0.9800 | C6B—H6B1 | 0.9800 |
C5A—H5A3 | 0.9800 | C6B—H6B2 | 0.9800 |
C6A—H6A1 | 0.9800 | C6B—H6B3 | 0.9800 |
C6A—H6A2 | 0.9800 | N3B—C7B | 1.288 (9) |
C6A—H6A3 | 0.9800 | C7B—N4B | 1.315 (10) |
N3A—C7A | 1.320 (12) | C7B—C8B | 1.491 (12) |
C7A—N4A | 1.349 (12) | C8B—H8B1 | 0.9800 |
C7A—C8A | 1.499 (14) | C8B—H8B2 | 0.9800 |
C8A—H8A1 | 0.9800 | C8B—H8B3 | 0.9800 |
C8A—H8A2 | 0.9800 | N4B—C10B | 1.436 (11) |
C8A—H8A3 | 0.9800 | N4B—C9B | 1.450 (11) |
N4A—C10A | 1.440 (12) | C9B—H9B1 | 0.9800 |
N4A—C9A | 1.453 (12) | C9B—H9B2 | 0.9800 |
C9A—H9A1 | 0.9800 | C9B—H9B3 | 0.9800 |
C9A—H9A2 | 0.9800 | C10B—H1B1 | 0.9800 |
C9A—H9A3 | 0.9800 | C10B—H1B2 | 0.9800 |
C10A—H1A1 | 0.9800 | C10B—H1B3 | 0.9800 |
C10A—H1A2 | 0.9800 | Cl1—C11 | 1.705 (9) |
C10A—H1A3 | 0.9800 | C11—Cl2 | 1.718 (9) |
O1—TaB | 1.936 (4) | C11—H111 | 0.9900 |
C1B—C2B | 1.582 (11) | C11—H112 | 0.9900 |
C2A—C1A—B4A | 112.3 (7) | C2B—C1B—B5B | 110.9 (6) |
C2A—C1A—B6A | 63.8 (6) | B4B—C1B—B5B | 63.8 (5) |
B4A—C1A—B6A | 116.3 (7) | B6B—C1B—B5B | 60.5 (5) |
C2A—C1A—B5A | 113.4 (7) | C2B—C1B—TaB | 71.8 (4) |
B4A—C1A—B5A | 63.4 (6) | B4B—C1B—TaB | 69.6 (4) |
B6A—C1A—B5A | 62.8 (6) | B6B—C1B—TaB | 133.5 (5) |
C2A—C1A—TaA | 71.5 (4) | B5B—C1B—TaB | 130.7 (5) |
B4A—C1A—TaA | 69.4 (4) | C2B—C1B—H1B | 120.6 |
B6A—C1A—TaA | 133.5 (6) | B4B—C1B—H1B | 119.5 |
B5A—C1A—TaA | 130.4 (6) | B6B—C1B—H1B | 114.1 |
C2A—C1A—H1A | 119.7 | B5B—C1B—H1B | 117.2 |
B4A—C1A—H1A | 119.6 | TaB—C1B—H1B | 99.1 |
B6A—C1A—H1A | 112.8 | C1B—C2B—B8B | 113.0 (6) |
B5A—C1A—H1A | 115.7 | C1B—C2B—B7B | 112.3 (6) |
TaA—C1A—H1A | 99.7 | B8B—C2B—B7B | 63.9 (5) |
C1A—C2A—B8A | 112.2 (7) | C1B—C2B—B6B | 61.5 (5) |
C1A—C2A—B7A | 110.7 (7) | B8B—C2B—B6B | 115.5 (6) |
B8A—C2A—B7A | 63.5 (6) | B7B—C2B—B6B | 62.4 (6) |
C1A—C2A—B6A | 62.2 (6) | C1B—C2B—TaB | 71.4 (4) |
B8A—C2A—B6A | 115.7 (7) | B8B—C2B—TaB | 70.8 (4) |
B7A—C2A—B6A | 61.7 (6) | B7B—C2B—TaB | 132.0 (5) |
C1A—C2A—TaA | 72.4 (4) | B6B—C2B—TaB | 131.1 (5) |
B8A—C2A—TaA | 69.7 (4) | C1B—C2B—H2B | 120.9 |
B7A—C2A—TaA | 130.4 (6) | B8B—C2B—H2B | 118.3 |
B6A—C2A—TaA | 132.8 (6) | B7B—C2B—H2B | 115.3 |
C1A—C2A—H2A | 120.9 | B6B—C2B—H2B | 115.2 |
B8A—C2A—H2A | 119.1 | TaB—C2B—H2B | 99.2 |
B7A—C2A—H2A | 117.0 | N1B—TaB—N3B | 100.0 (3) |
B6A—C2A—H2A | 114.2 | N1B—TaB—O1 | 102.6 (3) |
TaA—C2A—H2A | 99.2 | N3B—TaB—O1 | 101.3 (2) |
N1A—TaA—N3A | 100.1 (3) | N1B—TaB—B9B | 101.5 (3) |
N1A—TaA—O1 | 102.2 (3) | N3B—TaB—B9B | 100.1 (3) |
N3A—TaA—O1 | 102.7 (3) | O1—TaB—B9B | 144.2 (3) |
N1A—TaA—B9A | 106.4 (3) | N1B—TaB—B4B | 143.4 (3) |
N3A—TaA—B9A | 96.1 (3) | N3B—TaB—B4B | 87.1 (3) |
O1—TaA—B9A | 142.2 (3) | O1—TaB—B4B | 111.2 (3) |
N1A—TaA—B8A | 84.5 (3) | B9B—TaB—B4B | 42.0 (3) |
N3A—TaA—B8A | 136.4 (3) | N1B—TaB—C1B | 144.2 (3) |
O1—TaA—B8A | 118.9 (3) | N3B—TaB—C1B | 115.1 (3) |
B9A—TaA—B8A | 42.4 (3) | O1—TaB—C1B | 78.2 (2) |
N1A—TaA—B4A | 147.6 (3) | B9B—TaB—C1B | 66.8 (3) |
N3A—TaA—B4A | 87.9 (3) | B4B—TaB—C1B | 39.7 (3) |
O1—TaA—B4A | 106.6 (3) | N1B—TaB—C2B | 107.4 (3) |
B9A—TaA—B4A | 41.2 (3) | N3B—TaB—C2B | 151.2 (3) |
B8A—TaA—B4A | 68.9 (3) | O1—TaB—C2B | 81.4 (2) |
N1A—TaA—C2A | 105.1 (3) | B9B—TaB—C2B | 66.3 (3) |
N3A—TaA—C2A | 152.3 (3) | B4B—TaB—C2B | 65.7 (3) |
O1—TaA—C2A | 83.2 (3) | C1B—TaB—C2B | 36.8 (3) |
B9A—TaA—C2A | 66.0 (3) | N1B—TaB—B8B | 83.4 (3) |
B8A—TaA—C2A | 38.0 (3) | N3B—TaB—B8B | 140.8 (3) |
B4A—TaA—C2A | 64.7 (3) | O1—TaB—B8B | 116.2 (2) |
N1A—TaA—C1A | 141.2 (3) | B9B—TaB—B8B | 41.9 (3) |
N3A—TaA—C1A | 118.2 (3) | B4B—TaB—B8B | 69.6 (3) |
O1—TaA—C1A | 76.8 (3) | C1B—TaB—B8B | 65.2 (3) |
B9A—TaA—C1A | 65.4 (3) | C2B—TaB—B8B | 38.6 (3) |
B8A—TaA—C1A | 63.9 (3) | C1B—B4B—B10B | 104.4 (6) |
B4A—TaA—C1A | 38.6 (3) | C1B—B4B—B9B | 104.2 (6) |
C2A—TaA—C1A | 36.1 (3) | B10B—B4B—B9B | 60.7 (5) |
C1A—B4A—B9A | 104.9 (7) | C1B—B4B—B5B | 58.8 (5) |
C1A—B4A—B10A | 104.8 (7) | B10B—B4B—B5B | 59.3 (5) |
B9A—B4A—B10A | 60.1 (6) | B9B—B4B—B5B | 107.6 (6) |
C1A—B4A—B5A | 59.8 (5) | C1B—B4B—TaB | 70.7 (4) |
B9A—B4A—B5A | 108.8 (7) | B10B—B4B—TaB | 126.1 (5) |
B10A—B4A—B5A | 59.8 (6) | B9B—B4B—TaB | 68.6 (4) |
C1A—B4A—TaA | 72.0 (4) | B5B—B4B—TaB | 126.9 (5) |
B9A—B4A—TaA | 68.6 (5) | C1B—B4B—H4B | 125.5 |
B10A—B4A—TaA | 126.0 (6) | B10B—B4B—H4B | 119.9 |
B5A—B4A—TaA | 129.6 (6) | B9B—B4B—H4B | 124.0 |
C1A—B4A—H4A | 124.6 | B5B—B4B—H4B | 118.8 |
B9A—B4A—H4A | 124.1 | TaB—B4B—H4B | 102.5 |
B10A—B4A—H4A | 120.4 | C1B—B5B—B6B | 59.2 (5) |
B5A—B4A—H4A | 117.2 | C1B—B5B—B11B | 104.5 (7) |
TaA—B4A—H4A | 101.3 | B6B—B5B—B11B | 60.0 (6) |
C1A—B5A—B10A | 102.4 (7) | C1B—B5B—B10B | 103.2 (6) |
C1A—B5A—B4A | 56.8 (5) | B6B—B5B—B10B | 110.2 (7) |
B10A—B5A—B4A | 59.6 (6) | B11B—B5B—B10B | 62.9 (5) |
C1A—B5A—B11A | 103.2 (8) | C1B—B5B—B4B | 57.4 (5) |
B10A—B5A—B11A | 59.6 (6) | B6B—B5B—B4B | 108.5 (6) |
B4A—B5A—B11A | 106.8 (8) | B11B—B5B—B4B | 109.5 (6) |
C1A—B5A—B6A | 58.5 (5) | B10B—B5B—B4B | 59.1 (5) |
B10A—B5A—B6A | 108.4 (8) | C1B—B5B—H5B | 126.1 |
B4A—B5A—B6A | 107.2 (7) | B6B—B5B—H5B | 120.5 |
B11A—B5A—B6A | 60.7 (6) | B11B—B5B—H5B | 121.0 |
C1A—B5A—H5A | 126.6 | B10B—B5B—H5B | 121.6 |
B10A—B5A—H5A | 122.9 | B4B—B5B—H5B | 121.8 |
B4A—B5A—H5A | 122.5 | C1B—B6B—B11B | 105.4 (7) |
B11A—B5A—H5A | 122.7 | C1B—B6B—B5B | 60.3 (5) |
B6A—B5A—H5A | 120.8 | B11B—B6B—B5B | 60.1 (5) |
C1A—B6A—C2A | 54.0 (5) | C1B—B6B—C2B | 54.9 (5) |
C1A—B6A—B7A | 101.7 (7) | B11B—B6B—C2B | 104.0 (6) |
C2A—B6A—B7A | 58.6 (6) | B5B—B6B—C2B | 103.8 (6) |
C1A—B6A—B5A | 58.7 (6) | C1B—B6B—B7B | 102.9 (6) |
C2A—B6A—B5A | 102.2 (7) | B11B—B6B—B7B | 60.8 (5) |
B7A—B6A—B5A | 106.7 (8) | B5B—B6B—B7B | 108.4 (6) |
C1A—B6A—B11A | 102.3 (7) | C2B—B6B—B7B | 57.6 (5) |
C2A—B6A—B11A | 102.4 (8) | C1B—B6B—H6B | 125.0 |
B7A—B6A—B11A | 59.1 (7) | B11B—B6B—H6B | 122.4 |
B5A—B6A—B11A | 59.4 (6) | B5B—B6B—H6B | 121.5 |
C1A—B6A—H6A | 126.6 | C2B—B6B—H6B | 126.2 |
C2A—B6A—H6A | 126.4 | B7B—B6B—H6B | 122.5 |
B7A—B6A—H6A | 123.0 | C2B—B7B—B11B | 103.7 (7) |
B5A—B6A—H6A | 122.6 | C2B—B7B—B6B | 60.0 (5) |
B11A—B6A—H6A | 124.2 | B11B—B7B—B6B | 58.1 (6) |
C2A—B7A—B11A | 104.9 (8) | C2B—B7B—B8B | 57.3 (5) |
C2A—B7A—B8A | 55.7 (5) | B11B—B7B—B8B | 108.4 (6) |
B11A—B7A—B8A | 108.0 (9) | B6B—B7B—B8B | 108.1 (7) |
C2A—B7A—B6A | 59.7 (6) | C2B—B7B—B12B | 102.0 (6) |
B11A—B7A—B6A | 61.3 (7) | B11B—B7B—B12B | 61.1 (5) |
B8A—B7A—B6A | 107.4 (7) | B6B—B7B—B12B | 106.8 (7) |
C2A—B7A—B12A | 103.1 (7) | B8B—B7B—B12B | 59.1 (5) |
B11A—B7A—B12A | 58.9 (7) | C2B—B7B—H7B | 125.9 |
B8A—B7A—B12A | 61.3 (7) | B11B—B7B—H7B | 122.4 |
B6A—B7A—B12A | 108.5 (8) | B6B—B7B—H7B | 121.7 |
C2A—B7A—H7A | 126.0 | B8B—B7B—H7B | 121.6 |
B11A—B7A—H7A | 122.0 | B12B—B7B—H7B | 123.4 |
B8A—B7A—H7A | 122.2 | C2B—B8B—B12B | 104.4 (7) |
B6A—B7A—H7A | 120.5 | C2B—B8B—B7B | 58.8 (5) |
B12A—B7A—H7A | 122.6 | B12B—B8B—B7B | 60.6 (5) |
C2A—B8A—B7A | 60.7 (6) | C2B—B8B—B9B | 104.5 (6) |
C2A—B8A—B9A | 105.2 (7) | B12B—B8B—B9B | 60.1 (5) |
B7A—B8A—B9A | 107.7 (8) | B7B—B8B—B9B | 109.2 (6) |
C2A—B8A—B12A | 106.0 (7) | C2B—B8B—TaB | 70.5 (4) |
B7A—B8A—B12A | 60.1 (7) | B12B—B8B—TaB | 124.4 (5) |
B9A—B8A—B12A | 58.5 (6) | B7B—B8B—TaB | 127.0 (5) |
C2A—B8A—TaA | 72.4 (4) | B9B—B8B—TaB | 67.8 (4) |
B7A—B8A—TaA | 130.3 (6) | C2B—B8B—H8B | 125.4 |
B9A—B8A—TaA | 68.5 (4) | B12B—B8B—H8B | 120.2 |
B12A—B8A—TaA | 124.7 (6) | B7B—B8B—H8B | 117.5 |
C2A—B8A—H8A | 123.2 | B9B—B8B—H8B | 123.8 |
B7A—B8A—H8A | 116.9 | TaB—B8B—H8B | 103.5 |
B9A—B8A—H8A | 125.3 | B12B—B9B—B4B | 106.6 (6) |
B12A—B8A—H8A | 120.9 | B12B—B9B—B8B | 59.1 (5) |
TaA—B8A—H8A | 101.4 | B4B—B9B—B8B | 106.7 (5) |
B4A—B9A—B10A | 60.2 (6) | B12B—B9B—B10B | 60.0 (5) |
B4A—B9A—B12A | 107.7 (8) | B4B—B9B—B10B | 59.2 (5) |
B10A—B9A—B12A | 59.6 (6) | B8B—B9B—B10B | 107.0 (6) |
B4A—B9A—B8A | 105.4 (7) | B12B—B9B—TaB | 125.9 (5) |
B10A—B9A—B8A | 107.5 (8) | B4B—B9B—TaB | 69.4 (4) |
B12A—B9A—B8A | 61.5 (6) | B8B—B9B—TaB | 70.3 (4) |
B4A—B9A—TaA | 70.2 (4) | B10B—B9B—TaB | 125.5 (5) |
B10A—B9A—TaA | 127.4 (6) | B12B—B9B—H9B | 119.5 |
B12A—B9A—TaA | 128.0 (6) | B4B—B9B—H9B | 123.8 |
B8A—B9A—TaA | 69.1 (4) | B8B—B9B—H9B | 123.3 |
B4A—B9A—H9A | 123.9 | B10B—B9B—H9B | 119.4 |
B10A—B9A—H9A | 118.8 | TaB—B9B—H9B | 103.0 |
B12A—B9A—H9A | 117.9 | B4B—B10B—B5B | 61.6 (5) |
B8A—B9A—H9A | 123.9 | B4B—B10B—B12B | 106.9 (6) |
TaA—B9A—H9A | 102.0 | B5B—B10B—B12B | 106.0 (6) |
B12A—B10A—B9A | 60.4 (6) | B4B—B10B—B9B | 60.1 (5) |
B12A—B10A—B4A | 108.0 (7) | B5B—B10B—B9B | 109.0 (6) |
B9A—B10A—B4A | 59.7 (5) | B12B—B10B—B9B | 59.5 (5) |
B12A—B10A—B5A | 109.0 (8) | B4B—B10B—B11B | 107.2 (6) |
B9A—B10A—B5A | 109.1 (7) | B5B—B10B—B11B | 57.5 (5) |
B4A—B10A—B5A | 60.6 (6) | B12B—B10B—B11B | 60.1 (5) |
B12A—B10A—B11A | 59.8 (7) | B9B—B10B—B11B | 108.1 (6) |
B9A—B10A—B11A | 108.5 (8) | B4B—B10B—H10B | 121.5 |
B4A—B10A—B11A | 108.5 (7) | B5B—B10B—H10B | 122.1 |
B5A—B10A—B11A | 60.8 (7) | B12B—B10B—H10B | 122.8 |
B12A—B10A—H10A | 121.6 | B9B—B10B—H10B | 121.1 |
B9A—B10A—H10A | 121.4 | B11B—B10B—H10B | 122.6 |
B4A—B10A—H10A | 121.8 | B6B—B11B—B5B | 60.0 (6) |
B5A—B10A—H10A | 120.6 | B6B—B11B—B7B | 61.1 (5) |
B11A—B10A—H10A | 121.4 | B5B—B11B—B7B | 108.5 (7) |
B12A—B11A—B10A | 59.7 (7) | B6B—B11B—B12B | 108.0 (7) |
B12A—B11A—B7A | 61.4 (7) | B5B—B11B—B12B | 106.8 (7) |
B10A—B11A—B7A | 108.2 (8) | B7B—B11B—B12B | 59.7 (5) |
B12A—B11A—B5A | 108.0 (8) | B6B—B11B—B10B | 107.7 (7) |
B10A—B11A—B5A | 59.6 (6) | B5B—B11B—B10B | 59.7 (5) |
B7A—B11A—B5A | 107.5 (7) | B7B—B11B—B10B | 107.3 (7) |
B12A—B11A—B6A | 109.1 (7) | B12B—B11B—B10B | 58.9 (5) |
B10A—B11A—B6A | 107.7 (7) | B6B—B11B—H11B | 121.3 |
B7A—B11A—B6A | 59.6 (6) | B5B—B11B—H11B | 122.0 |
B5A—B11A—B6A | 59.8 (6) | B7B—B11B—H11B | 121.3 |
B12A—B11A—H11A | 120.9 | B12B—B11B—H11B | 122.6 |
B10A—B11A—H11A | 122.1 | B10B—B11B—H11B | 122.5 |
B7A—B11A—H11A | 121.5 | B8B—B12B—B9B | 60.8 (5) |
B5A—B11A—H11A | 122.2 | B8B—B12B—B7B | 60.3 (5) |
B6A—B11A—H11A | 121.7 | B9B—B12B—B7B | 109.5 (6) |
B10A—B12A—B11A | 60.4 (7) | B8B—B12B—B10B | 108.7 (7) |
B10A—B12A—B9A | 60.0 (6) | B9B—B12B—B10B | 60.4 (5) |
B11A—B12A—B9A | 108.6 (8) | B7B—B12B—B10B | 108.6 (7) |
B10A—B12A—B7A | 107.4 (8) | B8B—B12B—B11B | 107.9 (6) |
B11A—B12A—B7A | 59.7 (7) | B9B—B12B—B11B | 109.5 (7) |
B9A—B12A—B7A | 107.6 (7) | B7B—B12B—B11B | 59.2 (5) |
B10A—B12A—B8A | 106.7 (7) | B10B—B12B—B11B | 61.0 (5) |
B11A—B12A—B8A | 106.4 (7) | B8B—B12B—H12B | 121.5 |
B9A—B12A—B8A | 60.0 (6) | B9B—B12B—H12B | 120.5 |
B7A—B12A—B8A | 58.5 (6) | B7B—B12B—H12B | 121.5 |
B10A—B12A—H12A | 122.0 | B10B—B12B—H12B | 121.1 |
B11A—B12A—H12A | 121.7 | B11B—B12B—H12B | 121.6 |
B9A—B12A—H12A | 121.2 | C3B—N1B—TaB | 177.0 (7) |
B7A—B12A—H12A | 122.5 | N2B—C3B—N1B | 120.6 (8) |
B8A—B12A—H12A | 123.1 | N2B—C3B—C4B | 121.0 (8) |
C3A—N1A—TaA | 170.0 (6) | N1B—C3B—C4B | 118.4 (8) |
N1A—C3A—N2A | 120.9 (8) | C3B—C4B—H4B1 | 109.5 |
N1A—C3A—C4A | 121.7 (8) | C3B—C4B—H4B2 | 109.5 |
N2A—C3A—C4A | 117.4 (8) | H4B1—C4B—H4B2 | 109.5 |
C3A—C4A—H4A1 | 109.5 | C3B—C4B—H4B3 | 109.5 |
C3A—C4A—H4A2 | 109.5 | H4B1—C4B—H4B3 | 109.5 |
H4A1—C4A—H4A2 | 109.5 | H4B2—C4B—H4B3 | 109.5 |
C3A—C4A—H4A3 | 109.5 | C3B—N2B—C5B | 123.9 (8) |
H4A1—C4A—H4A3 | 109.5 | C3B—N2B—C6B | 120.8 (7) |
H4A2—C4A—H4A3 | 109.5 | C5B—N2B—C6B | 114.9 (7) |
C3A—N2A—C6A | 120.1 (8) | N2B—C5B—H5B1 | 109.5 |
C3A—N2A—C5A | 122.7 (8) | N2B—C5B—H5B2 | 109.5 |
C6A—N2A—C5A | 117.2 (8) | H5B1—C5B—H5B2 | 109.5 |
N2A—C5A—H5A1 | 109.5 | N2B—C5B—H5B3 | 109.5 |
N2A—C5A—H5A2 | 109.5 | H5B1—C5B—H5B3 | 109.5 |
H5A1—C5A—H5A2 | 109.5 | H5B2—C5B—H5B3 | 109.5 |
N2A—C5A—H5A3 | 109.5 | N2B—C6B—H6B1 | 109.5 |
H5A1—C5A—H5A3 | 109.5 | N2B—C6B—H6B2 | 109.5 |
H5A2—C5A—H5A3 | 109.5 | H6B1—C6B—H6B2 | 109.5 |
N2A—C6A—H6A1 | 109.5 | N2B—C6B—H6B3 | 109.5 |
N2A—C6A—H6A2 | 109.5 | H6B1—C6B—H6B3 | 109.5 |
H6A1—C6A—H6A2 | 109.5 | H6B2—C6B—H6B3 | 109.5 |
N2A—C6A—H6A3 | 109.5 | C7B—N3B—TaB | 166.0 (6) |
H6A1—C6A—H6A3 | 109.5 | N3B—C7B—N4B | 121.0 (7) |
H6A2—C6A—H6A3 | 109.5 | N3B—C7B—C8B | 119.2 (8) |
C7A—N3A—TaA | 165.0 (7) | N4B—C7B—C8B | 119.7 (7) |
N3A—C7A—N4A | 119.2 (8) | C7B—C8B—H8B1 | 109.5 |
N3A—C7A—C8A | 119.5 (9) | C7B—C8B—H8B2 | 109.5 |
N4A—C7A—C8A | 121.2 (9) | H8B1—C8B—H8B2 | 109.5 |
C7A—C8A—H8A1 | 109.5 | C7B—C8B—H8B3 | 109.5 |
C7A—C8A—H8A2 | 109.5 | H8B1—C8B—H8B3 | 109.5 |
H8A1—C8A—H8A2 | 109.5 | H8B2—C8B—H8B3 | 109.5 |
C7A—C8A—H8A3 | 109.5 | C7B—N4B—C10B | 120.8 (7) |
H8A1—C8A—H8A3 | 109.5 | C7B—N4B—C9B | 122.6 (7) |
H8A2—C8A—H8A3 | 109.5 | C10B—N4B—C9B | 116.0 (8) |
C7A—N4A—C10A | 120.4 (8) | N4B—C9B—H9B1 | 109.5 |
C7A—N4A—C9A | 123.3 (9) | N4B—C9B—H9B2 | 109.5 |
C10A—N4A—C9A | 116.3 (9) | H9B1—C9B—H9B2 | 109.5 |
N4A—C9A—H9A1 | 109.5 | N4B—C9B—H9B3 | 109.5 |
N4A—C9A—H9A2 | 109.5 | H9B1—C9B—H9B3 | 109.5 |
H9A1—C9A—H9A2 | 109.5 | H9B2—C9B—H9B3 | 109.5 |
N4A—C9A—H9A3 | 109.5 | N4B—C10B—H1B1 | 109.5 |
H9A1—C9A—H9A3 | 109.5 | N4B—C10B—H1B2 | 109.5 |
H9A2—C9A—H9A3 | 109.5 | H1B1—C10B—H1B2 | 109.5 |
N4A—C10A—H1A1 | 109.5 | N4B—C10B—H1B3 | 109.5 |
N4A—C10A—H1A2 | 109.5 | H1B1—C10B—H1B3 | 109.5 |
H1A1—C10A—H1A2 | 109.5 | H1B2—C10B—H1B3 | 109.5 |
N4A—C10A—H1A3 | 109.5 | Cl1—C11—Cl2 | 116.3 (8) |
H1A1—C10A—H1A3 | 109.5 | Cl1—C11—H111 | 108.2 |
H1A2—C10A—H1A3 | 109.5 | Cl2—C11—H111 | 108.2 |
TaA—O1—TaB | 163.4 (4) | Cl1—C11—H112 | 108.2 |
C2B—C1B—B4B | 111.7 (6) | Cl2—C11—H112 | 108.2 |
C2B—C1B—B6B | 63.6 (5) | H111—C11—H112 | 107.4 |
B4B—C1B—B6B | 114.9 (6) |
Experimental details
Crystal data | |
Chemical formula | [Ta2O(C2B9H11)2(C4H9N2)4]·0.5CH2Cl2 |
Mr | 1025.69 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 150 |
a, b, c (Å) | 11.414 (3), 10.769 (3), 17.863 (5) |
β (°) | 93.303 (6) |
V (Å3) | 2192.1 (11) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 5.08 |
Crystal size (mm) | 0.22 × 0.12 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Integration (XPREP in SHELXTL-NT; Bruker, 1998) |
Tmin, Tmax | 0.381, 0.690 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26944, 10933, 9396 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.712 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.095, 1.10 |
No. of reflections | 10933 |
No. of parameters | 470 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.34, −0.76 |
Absolute structure | Flack (1983) |
Absolute structure parameter | 0.41 (1) |
Computer programs: SMART-NT (Bruker, 1998), SMART-NT, SAINT-NT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-NT (Bruker, 1998).
Treating tantalum-tris(N,N-dimethylamide)-1,2-dicarbaundecaborate, (C2B9H11)Ta(NMe2)3, (I), with MeCN results in insertion of the nitrile into the metal-amide bond to give mainly tantalum-tris(N,N-dimethylacetamidinate)-1,2-dicarbaundecaborate, (C2B9H11)Ta[NC(Me)NMe2]3, (II), whose structure has been described by Broder et al. (2000). The title complex, (III), was identified as a minor product and results from hydrolysis of (II) by adventitious water. Following recrystallization, the poor solubility of (III), {(C2B9H11)Ta[NC(Me)NMe2]2}2(µ-O), in all common laboratory solvents hampered attempts to obtain supporting spectroscopic data, but the crystals proved suitable for a diffraction study. \sch
The asymmetric unit of (III) comprises two Ta atoms, each ligated by two monodentate N,N-dimethylacetamidinate ligands, [NC(Me)NMe2], and tethered by a µ-oxo bridge, plus a half-occupancy dichloromethane solvent molecule. The two Ta units are oriented mutually trans to each other to minimize the considerable steric interactions between the amidinate ligands. These factors are reflected in the almost linear [163.4 (4)°] Ta—O—Ta bond. The N,N-dimethylacetamidinate ligands are close to planar, with the mean deviations from planarity of the N—C-(C)NC2 units varying from 0.011 to 0.038 Å (s.u.s?), and the Me2N—C(Me)N bonds in the amidinate are shorter than typical N—C single bonds. The Ta—N bonds [1.855 (6) to 1.881 (6) Å] are intermediate between tantalum amido, Ta—NR2 [CSD (Allen & Kennard, 1993) mean 1.99 Å], and tantalum imido, Ta—NR (CSD mean 1.79 Å), distances.
These structural features reflect a delocalized π-bonding framework over the entire amidinate ligand and a balance between tantalum amide and tantalum imide canonical forms. The strong π-donation to the metal atom from the amidinate ligands results in a competitive weakening of the carborane to metal π-donation, and the C2B3 ring-centroid-metal distances of 2.050 (8) Å to TaA and 2.037 (7) Å to TaB are intermediate between those of the parent amide complex, (I) [2.019 (6) and 2.003 (6) Å; Batsanov et al., 1999], with moderate π-donor amide ligands, and the tris(acetamidinate), (II) [2.097 (5) Å]. There is often an orientational preference displayed by C2B9H11 ligands with respect to other ligands, as previously noted in amido (Batsanov et al., 1999, 2000), indenyl (Grädler et al., 1996; Smith & Welch, 1986), pyrollyl (Teixidor et al., 1997; Gómez et al., 1997) and carbonyl (Cowie et al., 1990) complexes. This can be described as a strong trans influence of the C2 unit of the dicarbollide, and arises from the non-equivalence of the two π-donor orbitals of the ligand. In the case of (III), the mid-point of the C—C bond of the dicarbollide is preferentially located approximately over the Ta—O vector, as quantified by the (C2 midpoint)-(C2B3 centroid)-Ta—O torsion angles, which are 11.4° to TaA and 4.6° to TaB (s.u.s?).