Tris(pyrazolyl)borate (scorpionate) ligands can be considered as the most prolific ligands in contemporary coordination chemistry due to the availability of various steric and electronic substituents at the pyrazolyl rings that allow fine-tuning of the open-coordination site for metal centres. The thallium(I) complexes of anionic tridentate-chelating scorpionate ligands, namely [tris(3-mesityl-5-methyl-1
H-pyrazol-1-yl-
N2)hydroborato]thallium(I) monohydrate, [Tl(C
39H
46BN
6)]·H
2O, (I), and [bis(3-mesityl-5-methyl-1
H-pyrazol-1-yl-
N2)(5-mesityl-3-methyl-1
H-pyrazol-1-yl-
N2)hydroborato]thallium(I), [Tl(C
39H
46BN
6)], (II), show a {Tl
IN
3} coordination, with average Tl
I-N bond lengths of 2.53 and 2.55 Å in (I) and (II), respectively. The overall Tl
I coordination geometry is distorted trigonal pyramidal, with the average N-Tl
I-N angle being approximately 73° for both. The dihedral angle between the planes of the pyrazolyl and benzene rings of the mesityl group is 82° in (I), while the corresponding angles in (II) are in the range 64-104°. The structural differences between the two ligands are expected to contribute to the different reactivities of the transition metal coordination complexes towards activation of small molecules such as dioxygen and ethylene.
Supporting information
CCDC references: 1441807; 1441806
For both compounds, data collection: CrystalClear-SM Expert (Rigaku, 2013); cell refinement: CrystalClear-SM Expert (Rigaku, 2013); data reduction: CrystalClear-SM Expert (Rigaku, 2013); program(s) used to solve structure: Il Milione (Burla et al., 2007); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: CrystalStructure (Rigaku, 2014); software used to prepare material for publication: CrystalStructure (Rigaku, 2014).
(20140719_l65tl_73) [Tris(3-mesityl-5-methyl-1
H-pyrazol-1-yl-
κN2)hydroborato]thallium(I) monohydrate
top
Crystal data top
[Tl(C39H46BN6)] | Dx = 1.444 Mg m−3 |
Mr = 832.03 | Mo Kα radiation, λ = 0.71075 Å |
Trigonal, R3:H | Cell parameters from 8683 reflections |
a = 11.7826 (11) Å | θ = 3.0–27.5° |
c = 47.7550 (4) Å | µ = 4.25 mm−1 |
V = 5741.6 (8) Å3 | T = 182 K |
Z = 6 | Block, colourless |
F(000) = 2508 | 0.21 × 0.19 × 0.16 mm |
Data collection top
Rigaku XtaLAB P200 diffractometer | 2759 reflections with F2 > 2.0σ(F2) |
Detector resolution: 5.814 pixels mm-1 | Rint = 0.020 |
ω scans | θmax = 27.5°, θmin = 3.5° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −15→15 |
Tmin = 0.428, Tmax = 0.507 | k = −14→14 |
20998 measured reflections | l = −61→61 |
2922 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0396P)2 + 2.9797P] where P = (Fo2 + 2Fc2)/3 |
2922 reflections | (Δ/σ)max = 0.001 |
146 parameters | Δρmax = 0.99 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
Primary atom site location: structure-invariant direct methods | |
Special details top
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 was performed using all reflections. The weighted R-factor (wR) and
goodness of fit (S) are based on F2. R-factor (gt) are based on F. The
threshold expression of F2 > 2.0 sigma(F2) is used only for calculating
R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Tl1 | 0.666667 | 0.333333 | 0.09482 (2) | 0.03570 (7) | |
N1 | 0.50567 (19) | 0.20237 (19) | 0.05638 (4) | 0.0360 (4) | |
N2 | 0.53507 (18) | 0.21796 (19) | 0.02817 (4) | 0.0321 (4) | |
C1 | 0.3303 (2) | 0.0537 (2) | 0.08736 (5) | 0.0397 (5) | |
C2 | 0.3406 (3) | −0.0450 (3) | 0.10139 (6) | 0.0468 (6) | |
C3 | 0.2913 (3) | −0.0785 (3) | 0.12860 (6) | 0.0546 (7) | |
C4 | 0.2334 (3) | −0.0174 (3) | 0.14203 (6) | 0.0560 (7) | |
C5 | 0.2203 (4) | 0.0767 (3) | 0.12758 (7) | 0.0636 (8) | |
C6 | 0.2667 (3) | 0.1130 (3) | 0.10028 (7) | 0.0553 (7) | |
C7 | 0.4022 (4) | −0.1174 (4) | 0.08737 (9) | 0.0714 (9) | |
C8 | 0.1850 (4) | −0.0524 (5) | 0.17226 (8) | 0.0778 (11) | |
C9 | 0.2482 (6) | 0.2153 (4) | 0.08513 (10) | 0.0971 (17) | |
C10 | 0.3879 (2) | 0.0964 (2) | 0.05895 (5) | 0.0364 (5) | |
C11 | 0.3392 (3) | 0.0430 (3) | 0.03254 (6) | 0.0444 (5) | |
C12 | 0.4342 (2) | 0.1211 (2) | 0.01368 (5) | 0.0358 (5) | |
C13 | 0.4367 (3) | 0.1051 (3) | −0.01756 (6) | 0.0484 (6) | |
B1 | 0.666667 | 0.333333 | 0.01764 (8) | 0.0323 (8) | |
H1 | 0.66666 | 0.33333 | −0.0033 | 0.0387* | |
H3 | 0.1785 | 0.11815 | 0.13649 | 0.0764* | |
H5 | 0.29797 | −0.14578 | 0.13811 | 0.0655* | |
H7A | 0.34299 | −0.17589 | 0.07287 | 0.0857* | |
H7B | 0.4174 | −0.16904 | 0.1014 | 0.0857* | |
H7C | 0.48581 | −0.05381 | 0.07883 | 0.0857* | |
H8A | 0.24143 | −0.07722 | 0.18249 | 0.0934* | |
H8B | 0.09476 | −0.12587 | 0.1723 | 0.0934* | |
H8C | 0.18796 | 0.02365 | 0.18134 | 0.0934* | |
H9A | 0.17933 | 0.17265 | 0.07097 | 0.1165* | |
H9B | 0.33047 | 0.2782 | 0.076 | 0.1165* | |
H9C | 0.22285 | 0.26141 | 0.0986 | 0.1165* | |
H11 | 0.25693 | −0.03214 | 0.02848 | 0.0532* | |
H13A | 0.50585 | 0.08543 | −0.02239 | 0.0581* | |
H13B | 0.45406 | 0.18647 | −0.02683 | 0.0581* | |
H13C | 0.35177 | 0.03312 | −0.02378 | 0.0581* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tl1 | 0.04501 (8) | 0.04501 (8) | 0.01706 (8) | 0.02250 (4) | 0.0000 | 0.0000 |
N1 | 0.0374 (9) | 0.0404 (10) | 0.0205 (8) | 0.0121 (8) | 0.0030 (7) | −0.0013 (7) |
N2 | 0.0368 (9) | 0.0382 (9) | 0.0194 (8) | 0.0173 (8) | −0.0015 (7) | −0.0038 (7) |
C1 | 0.0342 (11) | 0.0351 (11) | 0.0368 (12) | 0.0075 (9) | 0.0052 (9) | 0.0007 (9) |
C2 | 0.0381 (12) | 0.0506 (14) | 0.0440 (14) | 0.0164 (11) | 0.0012 (10) | 0.0051 (11) |
C3 | 0.0460 (14) | 0.0566 (16) | 0.0465 (15) | 0.0147 (12) | 0.0011 (12) | 0.0125 (13) |
C4 | 0.0486 (14) | 0.0563 (16) | 0.0399 (14) | 0.0089 (13) | 0.0109 (12) | 0.0069 (12) |
C5 | 0.073 (2) | 0.0558 (17) | 0.0542 (18) | 0.0267 (15) | 0.0300 (16) | 0.0072 (14) |
C6 | 0.0663 (18) | 0.0444 (14) | 0.0500 (16) | 0.0239 (13) | 0.0242 (14) | 0.0097 (12) |
C7 | 0.085 (2) | 0.087 (2) | 0.065 (2) | 0.060 (2) | 0.0115 (19) | 0.0156 (19) |
C8 | 0.077 (2) | 0.088 (3) | 0.0459 (18) | 0.024 (2) | 0.0194 (17) | 0.0164 (18) |
C9 | 0.159 (5) | 0.082 (3) | 0.086 (3) | 0.087 (3) | 0.069 (3) | 0.040 (2) |
C10 | 0.0362 (11) | 0.0347 (11) | 0.0335 (11) | 0.0142 (9) | 0.0023 (9) | −0.0029 (9) |
C11 | 0.0405 (12) | 0.0386 (12) | 0.0431 (13) | 0.0116 (10) | −0.0058 (10) | −0.0096 (10) |
C12 | 0.0440 (12) | 0.0376 (11) | 0.0292 (11) | 0.0229 (10) | −0.0079 (9) | −0.0101 (9) |
C13 | 0.0631 (17) | 0.0539 (15) | 0.0289 (12) | 0.0298 (13) | −0.0118 (11) | −0.0131 (11) |
B1 | 0.0402 (13) | 0.0402 (13) | 0.0165 (16) | 0.0201 (6) | 0.0000 | 0.0000 |
Geometric parameters (Å, º) top
Tl1—N1 | 2.5342 (19) | C11—C12 | 1.372 (3) |
Tl1—N1i | 2.5342 (19) | C12—C13 | 1.506 (4) |
Tl1—N1ii | 2.5342 (19) | C3—H5 | 0.950 |
N1—N2 | 1.380 (3) | C5—H3 | 0.950 |
N1—C10 | 1.329 (2) | C7—H7A | 0.980 |
N2—C12 | 1.356 (3) | C7—H7B | 0.980 |
N2—B1 | 1.548 (2) | C7—H7C | 0.980 |
C1—C2 | 1.399 (5) | C8—H8A | 0.980 |
C1—C6 | 1.398 (5) | C8—H8B | 0.980 |
C1—C10 | 1.487 (3) | C8—H8C | 0.980 |
C2—C3 | 1.397 (4) | C9—H9A | 0.980 |
C2—C7 | 1.524 (7) | C9—H9B | 0.980 |
C3—C4 | 1.373 (6) | C9—H9C | 0.980 |
C4—C5 | 1.379 (6) | C11—H11 | 0.950 |
C4—C8 | 1.531 (5) | C13—H13A | 0.980 |
C5—C6 | 1.395 (5) | C13—H13B | 0.980 |
C6—C9 | 1.512 (7) | C13—H13C | 0.980 |
C10—C11 | 1.398 (4) | B1—H1 | 1.000 |
| | | |
Tl1···N2i | 3.504 (2) | C7···H7Bx | 3.2536 |
Tl1···N2ii | 3.504 (2) | C7···H13Avi | 3.2461 |
Tl1···C10i | 3.514 (2) | C8···H3vii | 3.0314 |
Tl1···C10ii | 3.514 (2) | C8···H3iii | 3.5795 |
N1···N2i | 3.138 (3) | C8···H5xi | 3.5484 |
N1···N2ii | 3.047 (3) | C9···H13Cxii | 3.2439 |
N1···C2 | 3.351 (3) | C10···H13Avi | 3.4486 |
N1···C6 | 3.235 (4) | C11···H13Avi | 2.9364 |
N1···C9 | 3.402 (7) | C11···H13Bxiii | 3.1811 |
N2···C1 | 3.590 (3) | C12···H11xii | 3.5040 |
C1···C4 | 2.804 (4) | C12···H13Avi | 2.8827 |
C2···C5 | 2.768 (6) | C13···H7Avi | 3.4995 |
C2···C11 | 3.450 (4) | C13···H7Cvi | 3.2114 |
C3···C6 | 2.767 (5) | C13···H9Bxiii | 3.3544 |
C6···C11 | 3.547 (5) | C13···H11xii | 3.0996 |
C7···C10 | 2.940 (6) | C13···H13Avi | 3.2649 |
C7···C11 | 3.519 (6) | H3···C4viii | 3.0141 |
C9···C10 | 2.922 (8) | H3···C5viii | 3.1963 |
C13···B1 | 3.180 (3) | H3···C8viii | 3.0314 |
N1···H1 | 3.3429 | H3···C8iii | 3.5795 |
N1···H7C | 3.0998 | H3···H3viii | 3.2094 |
N1···H9B | 2.7896 | H3···H3vii | 3.2094 |
N1···H11 | 3.1467 | H3···H8Aiii | 3.2826 |
N2···H11 | 3.1252 | H3···H8Bviii | 2.3486 |
N2···H13A | 2.8016 | H3···H8Cviii | 3.4427 |
N2···H13B | 2.7556 | H3···H8Ciii | 3.1891 |
N2···H13C | 3.2953 | H5···C8iv | 3.5484 |
C1···H3 | 3.2616 | H5···H7Bx | 3.2470 |
C1···H5 | 3.2634 | H5···H8Aiv | 3.0407 |
C1···H7A | 2.8680 | H5···H8Axi | 3.5571 |
C1···H7B | 3.3295 | H5···H8Biv | 3.1538 |
C1···H7C | 2.7295 | H5···H9Cvii | 3.3093 |
C1···H9A | 2.8694 | H7A···C7x | 3.2987 |
C1···H9B | 2.6989 | H7A···C13vi | 3.4995 |
C1···H9C | 3.3132 | H7A···H7Ax | 3.1192 |
C1···H11 | 2.9670 | H7A···H7Aix | 3.1192 |
C3···H3 | 3.2184 | H7A···H7Bx | 2.8565 |
C3···H7A | 3.0772 | H7A···H7Cx | 3.3920 |
C3···H7B | 2.5725 | H7A···H9Cvii | 3.5634 |
C3···H7C | 3.2125 | H7A···H13Avi | 2.8673 |
C3···H8A | 2.6414 | H7A···H13Bvi | 3.2963 |
C3···H8B | 2.9556 | H7A···H13Bxiii | 2.7221 |
C3···H8C | 3.2773 | H7B···C7ix | 3.2536 |
C5···H5 | 3.2188 | H7B···H5ix | 3.2470 |
C5···H8A | 3.2678 | H7B···H7Aix | 2.8565 |
C5···H8B | 2.9860 | H7B···H7Bx | 2.9040 |
C5···H8C | 2.6247 | H7B···H7Bix | 2.9040 |
C5···H9A | 3.0603 | H7B···H8Aiv | 3.1595 |
C5···H9B | 3.2104 | H7C···C13vi | 3.2114 |
C5···H9C | 2.5665 | H7C···H7Aix | 3.3920 |
C7···H5 | 2.6609 | H7C···H13Avi | 2.7294 |
C7···H9Bi | 3.3082 | H7C···H13Bvi | 3.1967 |
C8···H3 | 2.6674 | H7C···H13Cvi | 3.1885 |
C8···H5 | 2.6658 | H8A···C2xi | 3.5509 |
C9···H3 | 2.6572 | H8A···C3xi | 3.2893 |
C9···H7Cii | 3.1525 | H8A···H3iii | 3.2826 |
C10···H7A | 3.0531 | H8A···H5iv | 3.5571 |
C10···H7C | 2.7222 | H8A···H5xi | 3.0407 |
C10···H9A | 3.0626 | H8A···H7Bxi | 3.1595 |
C10···H9B | 2.6748 | H8A···H8Biv | 3.2567 |
C11···H7A | 3.2372 | H8A···H9Ciii | 3.2876 |
C11···H7C | 3.3383 | H8B···C2xi | 3.5705 |
C11···H9A | 3.4822 | H8B···C3xi | 3.0816 |
C11···H9B | 3.5046 | H8B···C4xi | 3.2767 |
C11···H13A | 3.1633 | H8B···C5vii | 3.2499 |
C11···H13B | 3.2311 | H8B···H3vii | 2.3486 |
C11···H13C | 2.6994 | H8B···H5xi | 3.1538 |
C12···H1 | 2.7503 | H8B···H8Axi | 3.2567 |
C13···H1 | 2.7839 | H8B···H8Cvii | 2.7940 |
C13···H11 | 2.9173 | H8C···Tl1iii | 3.4380 |
B1···H13A | 3.2003 | H8C···C4iii | 3.5065 |
B1···H13Ai | 3.2003 | H8C···C5iii | 3.1314 |
B1···H13Aii | 3.2003 | H8C···C6iii | 3.4527 |
B1···H13B | 3.0732 | H8C···H3vii | 3.4427 |
B1···H13Bi | 3.0732 | H8C···H3iii | 3.1891 |
B1···H13Bii | 3.0732 | H8C···H8Bviii | 2.7940 |
H1···H13A | 2.7237 | H9A···H9Aviii | 3.5936 |
H1···H13Ai | 2.7238 | H9A···H9Avii | 3.5936 |
H1···H13Aii | 2.7237 | H9A···H11viii | 3.3743 |
H1···H13B | 2.4894 | H9A···H13Cxii | 2.9602 |
H1···H13Bi | 2.4895 | H9B···C13xii | 3.3544 |
H1···H13Bii | 2.4895 | H9B···H13Axii | 3.4684 |
H3···H8A | 3.5187 | H9B···H13Bxii | 3.4484 |
H3···H8B | 3.0541 | H9B···H13Cxii | 2.6665 |
H3···H8C | 2.4421 | H9C···C1viii | 3.3946 |
H3···H9A | 3.1932 | H9C···C2viii | 3.1006 |
H3···H9B | 3.4250 | H9C···C3viii | 2.9574 |
H3···H9C | 2.3483 | H9C···C4viii | 3.1423 |
H5···H7A | 3.2097 | H9C···C5viii | 3.3766 |
H5···H7B | 2.3483 | H9C···C6viii | 3.5003 |
H5···H7C | 3.4188 | H9C···H5viii | 3.3093 |
H5···H8A | 2.4751 | H9C···H7Aviii | 3.5634 |
H5···H8B | 3.0026 | H9C···H8Aiii | 3.2876 |
H5···H8C | 3.5377 | H11···C12xiii | 3.5040 |
H7A···H11 | 3.1793 | H11···C13xiii | 3.0996 |
H7B···H9Bi | 3.4325 | H11···H9Avii | 3.3743 |
H7B···H9Ci | 3.2993 | H11···H13Avi | 3.1696 |
H7C···H9Bi | 2.4159 | H11···H13Bxiii | 2.4675 |
H7C···H9Ci | 3.0429 | H11···H13Cxiii | 3.0820 |
H11···H13A | 3.5156 | H13A···N2vi | 3.3710 |
H11···H13C | 2.6850 | H13A···C7vi | 3.2461 |
H13A···H13Bi | 3.1644 | H13A···C10vi | 3.4486 |
Tl1···H8Ciii | 3.4380 | H13A···C11vi | 2.9364 |
Tl1···H8Civ | 3.4380 | H13A···C12vi | 2.8827 |
Tl1···H8Cv | 3.4380 | H13A···C13vi | 3.2649 |
N2···H13Avi | 3.3710 | H13A···H7Avi | 2.8673 |
C1···H9Cvii | 3.3946 | H13A···H7Cvi | 2.7294 |
C2···H8Aiv | 3.5509 | H13A···H9Bxiii | 3.4684 |
C2···H8Biv | 3.5705 | H13A···H11vi | 3.1696 |
C2···H9Cvii | 3.1006 | H13A···H13Avi | 2.8926 |
C3···H8Aiv | 3.2893 | H13A···H13Cvi | 3.4598 |
C3···H8Biv | 3.0816 | H13B···C11xii | 3.1811 |
C3···H9Cvii | 2.9574 | H13B···H7Avi | 3.2963 |
C4···H3vii | 3.0141 | H13B···H7Axii | 2.7221 |
C4···H8Biv | 3.2767 | H13B···H7Cvi | 3.1967 |
C4···H8Ciii | 3.5065 | H13B···H9Bxiii | 3.4484 |
C4···H9Cvii | 3.1423 | H13B···H11xii | 2.4675 |
C5···H3vii | 3.1963 | H13C···C9xiii | 3.2439 |
C5···H8Bviii | 3.2499 | H13C···H7Cvi | 3.1885 |
C5···H8Ciii | 3.1314 | H13C···H9Axiii | 2.9602 |
C5···H9Cvii | 3.3766 | H13C···H9Bxiii | 2.6665 |
C6···H8Ciii | 3.4527 | H13C···H11xii | 3.0820 |
C6···H9Cvii | 3.5003 | H13C···H13Avi | 3.4598 |
C7···H7Aix | 3.2987 | | |
| | | |
N1—Tl1—N1i | 73.32 (7) | C2—C3—H5 | 118.951 |
N1—Tl1—N1ii | 73.32 (7) | C4—C3—H5 | 118.948 |
N1i—Tl1—N1ii | 73.32 (7) | C4—C5—H3 | 118.992 |
Tl1—N1—N2 | 124.36 (12) | C6—C5—H3 | 119.035 |
Tl1—N1—C10 | 128.11 (15) | C2—C7—H7A | 109.465 |
N2—N1—C10 | 106.85 (17) | C2—C7—H7B | 109.470 |
N1—N2—C12 | 109.28 (16) | C2—C7—H7C | 109.468 |
N1—N2—B1 | 120.56 (19) | H7A—C7—H7B | 109.470 |
C12—N2—B1 | 130.2 (2) | H7A—C7—H7C | 109.491 |
C2—C1—C6 | 119.7 (3) | H7B—C7—H7C | 109.463 |
C2—C1—C10 | 120.3 (3) | C4—C8—H8A | 109.467 |
C6—C1—C10 | 120.1 (3) | C4—C8—H8B | 109.464 |
C1—C2—C3 | 118.9 (3) | C4—C8—H8C | 109.478 |
C1—C2—C7 | 121.2 (3) | H8A—C8—H8B | 109.473 |
C3—C2—C7 | 119.8 (3) | H8A—C8—H8C | 109.468 |
C2—C3—C4 | 122.1 (3) | H8B—C8—H8C | 109.477 |
C3—C4—C5 | 118.2 (3) | C6—C9—H9A | 109.484 |
C3—C4—C8 | 121.0 (4) | C6—C9—H9B | 109.478 |
C5—C4—C8 | 120.8 (4) | C6—C9—H9C | 109.466 |
C4—C5—C6 | 122.0 (4) | H9A—C9—H9B | 109.458 |
C1—C6—C5 | 119.0 (4) | H9A—C9—H9C | 109.471 |
C1—C6—C9 | 120.9 (3) | H9B—C9—H9C | 109.469 |
C5—C6—C9 | 120.0 (4) | C10—C11—H11 | 126.977 |
N1—C10—C1 | 119.16 (19) | C12—C11—H11 | 126.963 |
N1—C10—C11 | 109.9 (2) | C12—C13—H13A | 109.454 |
C1—C10—C11 | 130.94 (18) | C12—C13—H13B | 109.463 |
C10—C11—C12 | 106.06 (19) | C12—C13—H13C | 109.464 |
N2—C12—C11 | 107.9 (2) | H13A—C13—H13B | 109.486 |
N2—C12—C13 | 123.2 (2) | H13A—C13—H13C | 109.486 |
C11—C12—C13 | 128.8 (2) | H13B—C13—H13C | 109.475 |
N2—B1—N2i | 109.99 (19) | N2—B1—H1 | 108.949 |
N2—B1—N2ii | 109.98 (19) | N2i—B1—H1 | 108.956 |
N2i—B1—N2ii | 109.99 (19) | N2ii—B1—H1 | 108.952 |
| | | |
N1—Tl1—N1i—N2i | 43.20 (17) | B1—N2—C12—C11 | −179.5 (2) |
N1—Tl1—N1i—C10i | −147.6 (2) | B1—N2—C12—C13 | 3.1 (5) |
N1i—Tl1—N1—N2 | −33.91 (17) | C2—C1—C6—C5 | 3.2 (3) |
N1i—Tl1—N1—C10 | 135.3 (2) | C2—C1—C6—C9 | −177.01 (19) |
N1—Tl1—N1ii—N2ii | −33.91 (17) | C6—C1—C2—C3 | −2.6 (3) |
N1—Tl1—N1ii—C10ii | 135.3 (2) | C6—C1—C2—C7 | 176.4 (2) |
N1ii—Tl1—N1—N2 | 43.20 (17) | C2—C1—C10—N1 | −97.3 (3) |
N1ii—Tl1—N1—C10 | −147.6 (2) | C2—C1—C10—C11 | 82.4 (4) |
N1i—Tl1—N1ii—N2ii | 43.20 (17) | C10—C1—C2—C3 | 176.86 (17) |
N1i—Tl1—N1ii—C10ii | −147.6 (2) | C10—C1—C2—C7 | −4.1 (3) |
N1ii—Tl1—N1i—N2i | −33.91 (17) | C6—C1—C10—N1 | 82.1 (3) |
N1ii—Tl1—N1i—C10i | 135.3 (2) | C6—C1—C10—C11 | −98.2 (3) |
Tl1—N1—N2—C12 | 171.33 (14) | C10—C1—C6—C5 | −176.24 (18) |
Tl1—N1—N2—B1 | −8.9 (3) | C10—C1—C6—C9 | 3.6 (3) |
Tl1—N1—C10—C1 | 8.5 (4) | C1—C2—C3—C4 | −0.2 (3) |
Tl1—N1—C10—C11 | −171.24 (15) | C7—C2—C3—C4 | −179.2 (2) |
N2—N1—C10—C1 | 179.2 (2) | C2—C3—C4—C5 | 2.2 (4) |
N2—N1—C10—C11 | −0.5 (3) | C2—C3—C4—C8 | −177.6 (2) |
C10—N1—N2—C12 | 0.2 (3) | C3—C4—C5—C6 | −1.6 (4) |
C10—N1—N2—B1 | 180.0 (2) | C8—C4—C5—C6 | 178.3 (2) |
N1—N2—C12—C11 | 0.3 (3) | C4—C5—C6—C1 | −1.1 (4) |
N1—N2—C12—C13 | −177.1 (2) | C4—C5—C6—C9 | 179.1 (2) |
N1—N2—B1—N2i | 66.0 (3) | N1—C10—C11—C12 | 0.7 (4) |
N1—N2—B1—N2ii | −55.3 (3) | C1—C10—C11—C12 | −179.0 (3) |
C12—N2—B1—N2i | −114.3 (3) | C10—C11—C12—N2 | −0.6 (4) |
C12—N2—B1—N2ii | 124.4 (3) | C10—C11—C12—C13 | 176.6 (3) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) −x+2/3, −y+1/3, −z+1/3; (iv) y+2/3, −x+y+1/3, −z+1/3; (v) x−y+2/3, x+1/3, −z+1/3; (vi) −x+1, −y, −z; (vii) −x+y, −x, z; (viii) −y, x−y, z; (ix) −x+y+1, −x, z; (x) −y, x−y−1, z; (xi) x−y−1/3, x−2/3, −z+1/3; (xii) x−y, x, −z; (xiii) y, −x+y, −z. |
(20150127_l65stl_51) [Bis(3-mesityl-5-methyl-1
H-pyrazol-1-yl-
κN2)(5-mesityl-3-methyl-1
H-pyrazol-1-yl-
κN2)hydroborato]thallium(I)
top
Crystal data top
[Tl(C39H46BN6)] | Z = 2 |
Mr = 814.01 | F(000) = 816.00 |
Triclinic, P1 | Dx = 1.479 Mg m−3 |
a = 11.5262 (13) Å | Mo Kα radiation, λ = 0.71075 Å |
b = 11.8485 (15) Å | Cell parameters from 7445 reflections |
c = 14.523 (2) Å | θ = 3.0–27.5° |
α = 108.735 (4)° | µ = 4.45 mm−1 |
β = 100.095 (3)° | T = 178 K |
γ = 94.933 (9)° | Block, colourless |
V = 1827.5 (4) Å3 | 0.15 × 0.12 × 0.05 mm |
Data collection top
Rigaku XtaLAB P200 diffractometer | 7951 reflections with F2 > 2.0σ(F2) |
Detector resolution: 5.814 pixels mm-1 | Rint = 0.037 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: numerical (NUMABS; Rigaku, 1999) | h = −14→14 |
Tmin = 0.666, Tmax = 0.801 | k = −15→15 |
60831 measured reflections | l = −18→18 |
8362 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.015 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.038 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0238P)2 + 0.2336P] where P = (Fo2 + 2Fc2)/3 |
8362 reflections | (Δ/σ)max = 0.006 |
436 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.90 e Å−3 |
Primary atom site location: structure-invariant direct methods | |
Special details top
Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and
goodness of fit (S) are based on F2. R-factor (gt) are based on F. The
threshold expression of F2 > 2.0 sigma(F2) is used only for calculating
R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Tl1 | 0.44371 (2) | 0.93688 (2) | 0.86593 (2) | 0.02442 (3) | |
N1 | 0.40415 (12) | 0.85258 (11) | 0.68070 (10) | 0.0229 (2) | |
N2 | 0.34606 (11) | 0.74042 (11) | 0.62334 (9) | 0.0208 (2) | |
N3 | 0.22260 (11) | 0.84883 (12) | 0.80193 (10) | 0.0234 (2) | |
N4 | 0.17855 (11) | 0.75103 (12) | 0.71742 (10) | 0.0221 (2) | |
N6 | 0.33767 (11) | 0.62869 (11) | 0.74862 (9) | 0.0214 (2) | |
N5 | 0.42807 (12) | 0.70509 (12) | 0.82292 (10) | 0.0241 (3) | |
C1 | 0.51816 (14) | 1.02572 (13) | 0.66778 (11) | 0.0224 (3) | |
C2 | 0.45621 (15) | 1.12030 (14) | 0.70932 (12) | 0.0271 (3) | |
C3 | 0.52019 (18) | 1.23562 (15) | 0.76029 (13) | 0.0329 (4) | |
C4 | 0.64314 (18) | 1.25981 (15) | 0.77212 (13) | 0.0330 (4) | |
C5 | 0.70196 (16) | 1.16648 (15) | 0.72785 (13) | 0.0299 (3) | |
C6 | 0.64164 (14) | 1.04969 (14) | 0.67494 (12) | 0.0249 (3) | |
C7 | 0.32274 (17) | 1.10045 (18) | 0.69996 (17) | 0.0391 (4) | |
C8 | 0.7112 (2) | 1.38388 (18) | 0.83432 (17) | 0.0517 (5) | |
C9 | 0.70989 (16) | 0.95199 (16) | 0.62730 (14) | 0.0338 (4) | |
C10 | 0.45279 (13) | 0.90030 (14) | 0.62197 (11) | 0.0216 (3) | |
C11 | 0.42666 (14) | 0.81784 (14) | 0.52461 (12) | 0.0249 (3) | |
C12 | 0.35860 (14) | 0.71781 (14) | 0.52815 (11) | 0.0232 (3) | |
C13 | 0.30481 (18) | 0.60299 (17) | 0.44451 (13) | 0.0367 (4) | |
C14 | 0.15125 (14) | 0.99775 (15) | 0.92919 (13) | 0.0269 (3) | |
C15 | 0.20802 (15) | 0.98207 (15) | 1.01715 (13) | 0.0283 (3) | |
C16 | 0.23829 (16) | 1.08138 (16) | 1.10541 (14) | 0.0332 (4) | |
C17 | 0.21166 (17) | 1.19468 (16) | 1.10897 (15) | 0.0362 (4) | |
C18 | 0.14949 (17) | 1.20673 (17) | 1.02283 (16) | 0.0390 (4) | |
C19 | 0.11863 (16) | 1.11092 (17) | 0.93269 (15) | 0.0337 (4) | |
C20 | 0.23364 (19) | 0.86002 (17) | 1.01996 (14) | 0.0363 (4) | |
C21 | 0.2531 (2) | 1.30266 (19) | 1.20422 (18) | 0.0495 (5) | |
C22 | 0.0519 (2) | 1.1297 (2) | 0.84056 (18) | 0.0503 (5) | |
C23 | 0.12938 (14) | 0.89480 (15) | 0.83384 (12) | 0.0257 (3) | |
C24 | 0.02309 (15) | 0.82697 (17) | 0.76900 (14) | 0.0314 (3) | |
C25 | 0.05738 (14) | 0.73564 (15) | 0.69716 (12) | 0.0267 (3) | |
C26 | −0.01756 (16) | 0.63087 (17) | 0.61370 (14) | 0.0359 (4) | |
C27 | 0.21015 (15) | 0.42956 (14) | 0.70710 (13) | 0.0270 (3) | |
C28 | 0.10173 (17) | 0.41902 (16) | 0.73752 (15) | 0.0341 (4) | |
C29 | 0.01052 (17) | 0.32614 (17) | 0.67728 (16) | 0.0391 (4) | |
C30 | 0.02355 (17) | 0.24358 (16) | 0.58879 (16) | 0.0381 (4) | |
C31 | 0.13180 (17) | 0.25466 (16) | 0.56061 (15) | 0.0354 (4) | |
C32 | 0.22575 (15) | 0.34659 (14) | 0.61787 (13) | 0.0293 (3) | |
C33 | 0.0815 (2) | 0.5086 (2) | 0.83190 (17) | 0.0488 (5) | |
C34 | −0.0785 (2) | 0.1461 (2) | 0.5228 (2) | 0.0534 (6) | |
C35 | 0.34086 (17) | 0.35648 (17) | 0.58332 (15) | 0.0374 (4) | |
C36 | 0.30832 (14) | 0.52791 (14) | 0.77050 (12) | 0.0243 (3) | |
C37 | 0.38234 (15) | 0.53885 (15) | 0.85990 (13) | 0.0293 (3) | |
C38 | 0.45525 (14) | 0.65047 (15) | 0.89005 (12) | 0.0253 (3) | |
C39 | 0.54929 (17) | 0.70990 (18) | 0.98312 (14) | 0.0355 (4) | |
B1 | 0.26482 (15) | 0.66948 (15) | 0.66755 (13) | 0.0208 (3) | |
H1 | 0.21718 | 0.5969 | 0.61278 | 0.0250* | |
H3 | 0.47846 | 1.29968 | 0.7878 | 0.0395* | |
H5 | 0.78562 | 1.18235 | 0.73364 | 0.0358* | |
H7A | 0.30376 | 1.05901 | 0.74523 | 0.0469* | |
H7B | 0.28398 | 1.051 | 0.63132 | 0.0469* | |
H7C | 0.29395 | 1.17846 | 0.71728 | 0.0469* | |
H8A | 0.77826 | 1.40147 | 0.8054 | 0.0620* | |
H8B | 0.7413 | 1.3862 | 0.90243 | 0.0620* | |
H8C | 0.65794 | 1.44429 | 0.8354 | 0.0620* | |
H9A | 0.68067 | 0.87695 | 0.63636 | 0.0406* | |
H9B | 0.7949 | 0.97617 | 0.65853 | 0.0406* | |
H9C | 0.69848 | 0.93932 | 0.55602 | 0.0406* | |
H11 | 0.45054 | 0.82827 | 0.46812 | 0.0298* | |
H13A | 0.33189 | 0.53453 | 0.46144 | 0.0440* | |
H13B | 0.32965 | 0.60469 | 0.38374 | 0.0440* | |
H13C | 0.21769 | 0.59455 | 0.4336 | 0.0440* | |
H16 | 0.27817 | 1.07115 | 1.16458 | 0.0398* | |
H18 | 0.12715 | 1.2828 | 1.02525 | 0.0468* | |
H20A | 0.2889 | 0.83065 | 0.97665 | 0.0435* | |
H20B | 0.15906 | 0.80307 | 0.9967 | 0.0435* | |
H20C | 0.26956 | 0.86725 | 1.08835 | 0.0435* | |
H21A | 0.3297 | 1.34474 | 1.20343 | 0.0594* | |
H21B | 0.26239 | 1.27522 | 1.26161 | 0.0594* | |
H21C | 0.19384 | 1.35771 | 1.20912 | 0.0594* | |
H22A | 0.08755 | 1.09151 | 0.78399 | 0.0603* | |
H22B | 0.05677 | 1.21627 | 0.85197 | 0.0603* | |
H22C | −0.03189 | 1.09346 | 0.82608 | 0.0603* | |
H24 | −0.05596 | 0.84099 | 0.7736 | 0.0377* | |
H26A | −0.0036 | 0.55584 | 0.62566 | 0.0431* | |
H26B | 0.00377 | 0.62888 | 0.55083 | 0.0431* | |
H26C | −0.10195 | 0.63925 | 0.60992 | 0.0431* | |
H29 | −0.06298 | 0.31926 | 0.6976 | 0.0469* | |
H31 | 0.1423 | 0.19793 | 0.5005 | 0.0425* | |
H33A | 0.09895 | 0.59059 | 0.83086 | 0.0586* | |
H33B | 0.13417 | 0.50073 | 0.88955 | 0.0586* | |
H33C | −0.00175 | 0.49277 | 0.83654 | 0.0586* | |
H34A | −0.07439 | 0.07367 | 0.54128 | 0.0641* | |
H34B | −0.07265 | 0.12675 | 0.45309 | 0.0641* | |
H34C | −0.1545 | 0.17474 | 0.53144 | 0.0641* | |
H35A | 0.32632 | 0.31492 | 0.51121 | 0.0449* | |
H35B | 0.39912 | 0.31927 | 0.6171 | 0.0449* | |
H35C | 0.372 | 0.44169 | 0.59918 | 0.0449* | |
H37 | 0.3834 | 0.48227 | 0.89376 | 0.0352* | |
H39A | 0.58911 | 0.7852 | 0.98094 | 0.0426* | |
H39B | 0.60796 | 0.65587 | 0.98831 | 0.0426* | |
H39C | 0.51236 | 0.72754 | 1.04104 | 0.0426* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tl1 | 0.02931 (4) | 0.02252 (4) | 0.01744 (4) | −0.00006 (2) | 0.00217 (2) | 0.00401 (2) |
N1 | 0.0300 (6) | 0.0192 (6) | 0.0188 (6) | −0.0012 (5) | 0.0067 (5) | 0.0062 (5) |
N2 | 0.0260 (6) | 0.0183 (6) | 0.0164 (6) | −0.0007 (5) | 0.0042 (5) | 0.0048 (5) |
N3 | 0.0246 (6) | 0.0239 (6) | 0.0205 (6) | 0.0036 (5) | 0.0054 (5) | 0.0054 (5) |
N4 | 0.0231 (6) | 0.0225 (6) | 0.0197 (6) | 0.0004 (5) | 0.0039 (5) | 0.0072 (5) |
N6 | 0.0253 (6) | 0.0189 (6) | 0.0205 (6) | 0.0012 (5) | 0.0062 (5) | 0.0073 (5) |
N5 | 0.0265 (6) | 0.0237 (6) | 0.0218 (6) | 0.0024 (5) | 0.0037 (5) | 0.0086 (5) |
C1 | 0.0303 (7) | 0.0208 (7) | 0.0186 (7) | 0.0015 (6) | 0.0063 (6) | 0.0100 (6) |
C2 | 0.0362 (8) | 0.0241 (8) | 0.0262 (8) | 0.0058 (6) | 0.0098 (7) | 0.0137 (7) |
C3 | 0.0535 (11) | 0.0208 (8) | 0.0291 (9) | 0.0091 (7) | 0.0146 (8) | 0.0112 (7) |
C4 | 0.0517 (10) | 0.0216 (8) | 0.0239 (8) | −0.0042 (7) | 0.0070 (7) | 0.0083 (7) |
C5 | 0.0351 (8) | 0.0281 (8) | 0.0250 (8) | −0.0055 (7) | 0.0056 (7) | 0.0104 (7) |
C6 | 0.0310 (8) | 0.0251 (8) | 0.0209 (7) | 0.0008 (6) | 0.0081 (6) | 0.0103 (6) |
C7 | 0.0387 (10) | 0.0348 (10) | 0.0531 (12) | 0.0154 (8) | 0.0155 (9) | 0.0221 (9) |
C8 | 0.0746 (15) | 0.0260 (9) | 0.0432 (12) | −0.0104 (10) | 0.0100 (11) | 0.0027 (9) |
C9 | 0.0318 (8) | 0.0318 (9) | 0.0364 (10) | 0.0030 (7) | 0.0121 (7) | 0.0075 (8) |
C10 | 0.0252 (7) | 0.0219 (7) | 0.0201 (7) | 0.0036 (6) | 0.0065 (6) | 0.0098 (6) |
C11 | 0.0305 (8) | 0.0270 (8) | 0.0181 (7) | 0.0014 (6) | 0.0066 (6) | 0.0093 (6) |
C12 | 0.0269 (7) | 0.0244 (7) | 0.0177 (7) | 0.0024 (6) | 0.0059 (6) | 0.0064 (6) |
C13 | 0.0504 (11) | 0.0321 (9) | 0.0195 (8) | −0.0072 (8) | 0.0079 (7) | 0.0012 (7) |
C14 | 0.0268 (7) | 0.0269 (8) | 0.0293 (9) | 0.0063 (6) | 0.0132 (6) | 0.0086 (7) |
C15 | 0.0336 (8) | 0.0265 (8) | 0.0264 (8) | 0.0049 (6) | 0.0150 (7) | 0.0067 (7) |
C16 | 0.0385 (9) | 0.0328 (9) | 0.0280 (9) | 0.0025 (7) | 0.0146 (7) | 0.0068 (7) |
C17 | 0.0390 (9) | 0.0282 (9) | 0.0391 (10) | 0.0015 (7) | 0.0214 (8) | 0.0024 (8) |
C18 | 0.0411 (10) | 0.0275 (9) | 0.0536 (12) | 0.0113 (7) | 0.0238 (9) | 0.0123 (9) |
C19 | 0.0326 (8) | 0.0328 (9) | 0.0417 (10) | 0.0112 (7) | 0.0160 (8) | 0.0150 (8) |
C20 | 0.0553 (11) | 0.0313 (9) | 0.0265 (9) | 0.0099 (8) | 0.0133 (8) | 0.0124 (7) |
C21 | 0.0591 (13) | 0.0317 (10) | 0.0494 (13) | −0.0049 (9) | 0.0259 (11) | −0.0017 (9) |
C22 | 0.0549 (13) | 0.0472 (12) | 0.0560 (14) | 0.0244 (10) | 0.0110 (10) | 0.0237 (11) |
C23 | 0.0263 (7) | 0.0288 (8) | 0.0261 (8) | 0.0066 (6) | 0.0102 (6) | 0.0118 (7) |
C24 | 0.0228 (7) | 0.0383 (9) | 0.0342 (9) | 0.0048 (7) | 0.0089 (7) | 0.0125 (8) |
C25 | 0.0234 (7) | 0.0311 (8) | 0.0259 (8) | −0.0002 (6) | 0.0034 (6) | 0.0121 (7) |
C26 | 0.0275 (8) | 0.0391 (10) | 0.0339 (10) | −0.0037 (7) | −0.0006 (7) | 0.0089 (8) |
C27 | 0.0334 (8) | 0.0196 (7) | 0.0315 (9) | 0.0033 (6) | 0.0073 (7) | 0.0134 (7) |
C28 | 0.0387 (9) | 0.0295 (9) | 0.0404 (10) | 0.0027 (7) | 0.0141 (8) | 0.0182 (8) |
C29 | 0.0370 (9) | 0.0342 (9) | 0.0515 (12) | −0.0015 (7) | 0.0114 (8) | 0.0230 (9) |
C30 | 0.0378 (9) | 0.0247 (8) | 0.0511 (12) | −0.0000 (7) | −0.0001 (8) | 0.0182 (8) |
C31 | 0.0408 (9) | 0.0224 (8) | 0.0386 (10) | 0.0073 (7) | 0.0015 (8) | 0.0077 (7) |
C32 | 0.0337 (8) | 0.0202 (7) | 0.0350 (9) | 0.0075 (6) | 0.0059 (7) | 0.0107 (7) |
C33 | 0.0498 (12) | 0.0500 (12) | 0.0470 (12) | −0.0018 (10) | 0.0254 (10) | 0.0118 (10) |
C34 | 0.0440 (11) | 0.0350 (11) | 0.0696 (16) | −0.0076 (9) | −0.0023 (11) | 0.0134 (11) |
C35 | 0.0380 (9) | 0.0329 (9) | 0.0385 (10) | 0.0107 (8) | 0.0110 (8) | 0.0055 (8) |
C36 | 0.0308 (8) | 0.0198 (7) | 0.0262 (8) | 0.0063 (6) | 0.0107 (6) | 0.0102 (6) |
C37 | 0.0369 (9) | 0.0266 (8) | 0.0311 (9) | 0.0091 (7) | 0.0094 (7) | 0.0166 (7) |
C38 | 0.0288 (7) | 0.0278 (8) | 0.0235 (8) | 0.0091 (6) | 0.0082 (6) | 0.0116 (7) |
C39 | 0.0381 (9) | 0.0409 (10) | 0.0290 (9) | 0.0069 (8) | 0.0023 (7) | 0.0165 (8) |
B1 | 0.0246 (8) | 0.0182 (7) | 0.0189 (8) | −0.0004 (6) | 0.0050 (6) | 0.0061 (6) |
Geometric parameters (Å, º) top
Tl1—N1 | 2.4915 (14) | C32—C35 | 1.507 (3) |
Tl1—N3 | 2.5567 (12) | C36—C37 | 1.384 (2) |
Tl1—N5 | 2.5959 (15) | C37—C38 | 1.398 (2) |
N1—N2 | 1.3596 (15) | C38—C39 | 1.497 (2) |
N1—C10 | 1.336 (2) | C3—H3 | 0.950 |
N2—C12 | 1.357 (2) | C5—H5 | 0.950 |
N2—B1 | 1.555 (2) | C7—H7A | 0.980 |
N3—N4 | 1.3688 (16) | C7—H7B | 0.980 |
N3—C23 | 1.334 (2) | C7—H7C | 0.980 |
N4—C25 | 1.359 (2) | C8—H8A | 0.980 |
N4—B1 | 1.554 (2) | C8—H8B | 0.980 |
N6—N5 | 1.3732 (15) | C8—H8C | 0.980 |
N6—C36 | 1.361 (2) | C9—H9A | 0.980 |
N6—B1 | 1.554 (2) | C9—H9B | 0.980 |
N5—C38 | 1.342 (3) | C9—H9C | 0.980 |
C1—C2 | 1.409 (2) | C11—H11 | 0.950 |
C1—C6 | 1.406 (2) | C13—H13A | 0.980 |
C1—C10 | 1.488 (2) | C13—H13B | 0.980 |
C2—C3 | 1.394 (2) | C13—H13C | 0.980 |
C2—C7 | 1.511 (3) | C16—H16 | 0.950 |
C3—C4 | 1.390 (3) | C18—H18 | 0.950 |
C4—C5 | 1.386 (3) | C20—H20A | 0.980 |
C4—C8 | 1.514 (2) | C20—H20B | 0.980 |
C5—C6 | 1.397 (2) | C20—H20C | 0.980 |
C6—C9 | 1.507 (2) | C21—H21A | 0.980 |
C10—C11 | 1.399 (2) | C21—H21B | 0.980 |
C11—C12 | 1.384 (2) | C21—H21C | 0.980 |
C12—C13 | 1.497 (2) | C22—H22A | 0.980 |
C14—C15 | 1.405 (3) | C22—H22B | 0.980 |
C14—C19 | 1.411 (3) | C22—H22C | 0.980 |
C14—C23 | 1.486 (2) | C24—H24 | 0.950 |
C15—C16 | 1.398 (2) | C26—H26A | 0.980 |
C15—C20 | 1.512 (3) | C26—H26B | 0.980 |
C16—C17 | 1.390 (3) | C26—H26C | 0.980 |
C17—C18 | 1.385 (3) | C29—H29 | 0.950 |
C17—C21 | 1.518 (3) | C31—H31 | 0.950 |
C18—C19 | 1.393 (2) | C33—H33A | 0.980 |
C19—C22 | 1.514 (3) | C33—H33B | 0.980 |
C23—C24 | 1.405 (2) | C33—H33C | 0.980 |
C24—C25 | 1.382 (2) | C34—H34A | 0.980 |
C25—C26 | 1.496 (2) | C34—H34B | 0.980 |
C27—C28 | 1.405 (3) | C34—H34C | 0.980 |
C27—C32 | 1.404 (2) | C35—H35A | 0.980 |
C27—C36 | 1.485 (2) | C35—H35B | 0.980 |
C28—C29 | 1.393 (2) | C35—H35C | 0.980 |
C28—C33 | 1.510 (3) | C37—H37 | 0.950 |
C29—C30 | 1.384 (3) | C39—H39A | 0.980 |
C30—C31 | 1.388 (3) | C39—H39B | 0.980 |
C30—C34 | 1.515 (3) | C39—H39C | 0.980 |
C31—C32 | 1.396 (2) | B1—H1 | 1.000 |
| | | |
Tl1···C1 | 3.5752 (19) | C26···H31iii | 3.2801 |
N1···N4 | 2.976 (2) | C26···H34Biii | 3.4495 |
N1···N5 | 3.193 (2) | C27···H7Cxi | 3.2455 |
N1···C2 | 3.055 (2) | C28···H22Bxi | 3.3845 |
N1···C6 | 3.473 (2) | C29···H5xii | 3.3425 |
N1···C7 | 3.102 (3) | C29···H8Axii | 3.5378 |
N2···N3 | 3.142 (2) | C29···H13Ciii | 3.2105 |
N2···N6 | 3.059 (2) | C29···H22Bxi | 3.1909 |
N2···C1 | 3.574 (2) | C29···H26Biii | 3.4992 |
N3···N5 | 2.9698 (19) | C30···H13Ciii | 3.5379 |
N3···C15 | 3.058 (2) | C30···H26Biii | 2.8846 |
N3···C19 | 3.512 (2) | C31···H7Bxi | 3.4121 |
N3···C20 | 3.106 (3) | C31···H7Cxi | 3.0991 |
N4···N6 | 3.1899 (19) | C31···H9Cix | 3.3782 |
N4···C14 | 3.581 (2) | C31···H26Biii | 2.8079 |
N4···C36 | 3.377 (2) | C31···H26Ciii | 3.0996 |
N6···C28 | 3.467 (2) | C32···H7Cxi | 2.8965 |
N6···C32 | 3.2809 (18) | C32···H26Biii | 3.3769 |
N6···C35 | 3.353 (2) | C32···H26Ciii | 3.4280 |
C1···C4 | 2.813 (2) | C33···H8Axii | 3.5254 |
C2···C5 | 2.787 (3) | C33···H22Bxi | 3.5601 |
C3···C6 | 2.781 (3) | C34···H7Biii | 3.1472 |
C6···C11 | 3.3960 (19) | C34···H9Cxii | 3.5987 |
C7···C10 | 2.939 (3) | C34···H13Ciii | 3.5176 |
C9···C10 | 2.956 (2) | C34···H26Biii | 3.2797 |
C9···C11 | 3.359 (2) | C34···H34Axiii | 3.2494 |
C13···B1 | 3.205 (3) | C35···H3xi | 3.4064 |
C14···C17 | 2.814 (2) | C35···H7Cxi | 3.3668 |
C15···C18 | 2.781 (3) | C35···H9Aix | 3.4389 |
C16···C19 | 2.784 (3) | C35···H9Cix | 3.3813 |
C19···C24 | 3.390 (2) | C35···H11ix | 3.4081 |
C20···C23 | 2.930 (3) | C35···H26Ciii | 3.5871 |
C22···C23 | 2.973 (3) | C36···H3xi | 3.5210 |
C22···C24 | 3.367 (3) | C37···H3xi | 3.0651 |
C26···B1 | 3.168 (2) | C37···H8Cxi | 3.4964 |
C27···C30 | 2.809 (2) | C38···H8Cxi | 3.5273 |
C27···B1 | 3.111 (3) | C38···H21Aii | 3.0324 |
C28···C31 | 2.780 (3) | C39···H3ii | 3.4341 |
C28···C37 | 3.348 (2) | C39···H21Aii | 3.1714 |
C29···C32 | 2.782 (3) | C39···H37xiv | 3.3788 |
C32···C37 | 3.568 (2) | H1···H26Biii | 3.4513 |
C33···C36 | 2.920 (3) | H1···H26Ciii | 3.4778 |
C33···C37 | 3.394 (3) | H3···C35v | 3.4064 |
C35···C36 | 2.932 (2) | H3···C36v | 3.5210 |
C17···C24i | 3.519 (3) | H3···C37v | 3.0651 |
C17···C39ii | 3.519 (3) | H3···C39ii | 3.4341 |
C18···C39ii | 3.551 (3) | H3···H35Bv | 2.5783 |
C21···C24i | 3.552 (3) | H3···H37v | 2.6663 |
C24···C17i | 3.519 (3) | H3···H39Bii | 3.4594 |
C24···C21i | 3.552 (3) | H3···H39Cii | 2.5928 |
C26···C31iii | 3.365 (3) | H5···C22vi | 3.3911 |
C31···C26iii | 3.365 (3) | H5···C29vii | 3.3425 |
C39···C17ii | 3.519 (3) | H5···H11iv | 3.5943 |
C39···C18ii | 3.551 (3) | H5···H20Cii | 2.9869 |
Tl1···H7A | 2.9679 | H5···H22Bvi | 3.2156 |
Tl1···H20A | 3.0453 | H5···H22Cvi | 2.7632 |
Tl1···H39A | 3.2083 | H5···H29vii | 2.5158 |
N1···H1 | 3.3177 | H5···H34Avii | 3.4195 |
N1···H7A | 2.7557 | H5···H34Cvii | 3.1079 |
N1···H7B | 3.0422 | H7A···H34Biii | 3.5307 |
N1···H9A | 3.3671 | H7A···H39Cii | 3.5003 |
N1···H11 | 3.1519 | H7B···C31v | 3.4121 |
N2···H11 | 3.1399 | H7B···C34iii | 3.1472 |
N2···H13A | 2.7602 | H7B···H9Civ | 2.8010 |
N2···H13B | 3.2943 | H7B···H31v | 3.2914 |
N2···H13C | 2.8002 | H7B···H34Aiii | 3.0309 |
N2···H35C | 3.4873 | H7B···H34Biii | 2.8782 |
N3···H1 | 3.3317 | H7B···H34Ciii | 2.9973 |
N3···H7A | 2.9902 | H7B···H35Bv | 3.4205 |
N3···H20A | 2.6017 | H7C···C27v | 3.2455 |
N3···H20B | 3.2365 | H7C···C31v | 3.0991 |
N3···H22A | 3.4449 | H7C···C32v | 2.8965 |
N3···H24 | 3.1540 | H7C···C35v | 3.3668 |
N3···H33A | 3.4432 | H7C···H31v | 3.4098 |
N4···H20A | 3.5376 | H7C···H35Bv | 2.8635 |
N4···H24 | 3.1334 | H7C···H39Cii | 3.5858 |
N4···H26A | 2.7815 | H8A···C13iv | 3.5696 |
N4···H26B | 2.7472 | H8A···C21viii | 3.5992 |
N4···H26C | 3.2879 | H8A···C29vii | 3.5378 |
N4···H33A | 3.0678 | H8A···C33vii | 3.5254 |
N6···H20A | 3.5781 | H8A···H13Biv | 2.7849 |
N6···H33A | 3.2382 | H8A···H13Civ | 3.4948 |
N6···H35C | 2.6719 | H8A···H21Aviii | 3.3827 |
N6···H37 | 3.1381 | H8A···H21Cviii | 2.9227 |
N5···H1 | 3.3490 | H8A···H29vii | 2.6608 |
N5···H20A | 3.0501 | H8A···H33Cvii | 2.5722 |
N5···H37 | 3.1607 | H8B···C20ii | 3.4652 |
N5···H39A | 2.5333 | H8B···H20Aii | 3.5729 |
N5···H39B | 3.1258 | H8B···H20Bii | 3.2338 |
N5···H39C | 3.0634 | H8B···H20Cii | 3.0416 |
C1···H3 | 3.2687 | H8B···H33Bii | 2.9208 |
C1···H5 | 3.2718 | H8B···H33Cvii | 3.5225 |
C1···H7A | 2.8956 | H8B···H37ii | 3.4884 |
C1···H7B | 2.7195 | H8B···H39Cii | 3.4515 |
C1···H7C | 3.3302 | H8C···C21viii | 3.3405 |
C1···H9A | 2.6786 | H8C···C37v | 3.4964 |
C1···H9B | 3.3104 | H8C···C38v | 3.5273 |
C1···H9C | 2.9126 | H8C···H13Biv | 3.0779 |
C1···H11 | 3.0042 | H8C···H21Aviii | 2.7311 |
C3···H5 | 3.2401 | H8C···H21Cviii | 3.0843 |
C3···H7A | 3.0441 | H8C···H37v | 3.4459 |
C3···H7B | 3.2034 | H8C···H39Bv | 2.9443 |
C3···H7C | 2.5500 | H9A···C16ii | 3.5615 |
C3···H8A | 3.2593 | H9A···C35ix | 3.4389 |
C3···H8B | 2.9912 | H9A···H16ii | 2.6996 |
C3···H8C | 2.6094 | H9A···H21Bii | 2.7306 |
C5···H3 | 3.2385 | H9A···H24vi | 3.4664 |
C5···H8A | 2.6479 | H9A···H31ix | 3.0825 |
C5···H8B | 2.9266 | H9A···H35Aix | 2.5585 |
C5···H8C | 3.2855 | H9A···H35Bix | 3.5705 |
C5···H9A | 3.2260 | H9B···C22vi | 3.5086 |
C5···H9B | 2.5653 | H9B···H16ii | 3.0374 |
C5···H9C | 3.0174 | H9B···H21Bii | 3.5781 |
C6···H11 | 3.5187 | H9B···H22Avi | 3.4668 |
C7···H3 | 2.6373 | H9B···H22Cvi | 2.7360 |
C7···H22A | 3.1690 | H9B···H24vi | 3.0821 |
C8···H3 | 2.6678 | H9B···H31ix | 2.8099 |
C8···H5 | 2.6694 | H9B···H34Avii | 2.8927 |
C9···H5 | 2.6470 | H9B···H34Cvii | 3.4948 |
C9···H11 | 3.3281 | H9B···H35Aix | 3.5251 |
C10···H7A | 3.0269 | H9C···C7iv | 3.5551 |
C10···H7B | 2.7435 | H9C···C31ix | 3.3782 |
C10···H9A | 2.6436 | H9C···C34vii | 3.5987 |
C10···H9C | 3.1876 | H9C···C35ix | 3.3813 |
C11···H7B | 3.4151 | H9C···H7Biv | 2.8010 |
C11···H9A | 2.9913 | H9C···H11iv | 3.4465 |
C11···H9C | 3.2245 | H9C···H31ix | 2.6211 |
C11···H13A | 3.2160 | H9C···H34Avii | 3.0219 |
C11···H13B | 2.6846 | H9C···H34Cvii | 3.2891 |
C11···H13C | 3.1764 | H9C···H35Aix | 2.8238 |
C12···H1 | 2.7662 | H9C···H35Bix | 3.2313 |
C13···H1 | 2.8220 | H11···C1iv | 3.0585 |
C13···H11 | 2.9160 | H11···C2iv | 3.1677 |
C13···H35C | 3.4206 | H11···C3iv | 3.2425 |
C14···H16 | 3.2713 | H11···C4iv | 3.2519 |
C14···H18 | 3.2712 | H11···C5iv | 3.0939 |
C14···H20A | 2.8188 | H11···C6iv | 2.9928 |
C14···H20B | 2.7835 | H11···C35ix | 3.4081 |
C14···H20C | 3.3387 | H11···H5iv | 3.5943 |
C14···H22A | 2.7060 | H11···H9Civ | 3.4465 |
C14···H22B | 3.3270 | H11···H34Ciii | 3.4105 |
C14···H22C | 2.8946 | H11···H35Aix | 3.2234 |
C14···H24 | 2.9848 | H11···H35Bix | 2.7338 |
C16···H18 | 3.2372 | H13A···H21Bxv | 3.3967 |
C16···H20A | 3.1264 | H13A···H21Cxv | 3.5777 |
C16···H20B | 3.1357 | H13A···H26Ciii | 3.0109 |
C16···H20C | 2.5324 | H13B···C4iv | 3.2088 |
C16···H21A | 2.9881 | H13B···C5iv | 3.5911 |
C16···H21B | 2.6116 | H13B···C8iv | 3.1675 |
C16···H21C | 3.2622 | H13B···H8Aiv | 2.7849 |
C18···H16 | 3.2376 | H13B···H8Civ | 3.0779 |
C18···H21A | 2.9358 | H13B···H21Axv | 3.3412 |
C18···H21B | 3.2873 | H13B···H21Cxv | 3.2401 |
C18···H21C | 2.6514 | H13B···H29iii | 3.3974 |
C18···H22A | 3.2136 | H13B···H34Ciii | 3.4834 |
C18···H22B | 2.5658 | H13B···H35Bix | 3.1814 |
C18···H22C | 3.0490 | H13B···H35Cix | 3.5075 |
C19···H24 | 3.4833 | H13C···C26iii | 3.1832 |
C20···H16 | 2.6379 | H13C···C29iii | 3.2105 |
C20···H33A | 3.4878 | H13C···C30iii | 3.5379 |
C21···H16 | 2.6683 | H13C···C34iii | 3.5176 |
C21···H18 | 2.6727 | H13C···H8Aiv | 3.4948 |
C22···H7A | 3.4827 | H13C···H21Cxv | 3.5007 |
C22···H18 | 2.6506 | H13C···H26Aiii | 2.7421 |
C22···H24 | 3.3016 | H13C···H26Ciii | 2.7923 |
C23···H7A | 3.3651 | H13C···H29iii | 2.8680 |
C23···H20A | 2.8594 | H13C···H34Ciii | 2.8002 |
C23···H20B | 2.8852 | H16···Tl1ii | 3.3174 |
C23···H22A | 2.7099 | H16···C6ii | 3.1547 |
C23···H22C | 3.1397 | H16···C9ii | 3.1021 |
C23···H33A | 3.5769 | H16···H9Aii | 2.6996 |
C24···H20B | 3.5118 | H16···H9Bii | 3.0374 |
C24···H22A | 3.0868 | H16···H22Ci | 3.3516 |
C24···H22C | 3.1473 | H16···H24i | 3.0189 |
C24···H26A | 3.1714 | H16···H39Aii | 3.5637 |
C24···H26B | 3.2378 | H18···H20Bi | 3.2963 |
C24···H26C | 2.7097 | H18···H33Ci | 3.3821 |
C24···H33A | 3.3433 | H18···H39Aii | 3.4442 |
C25···H1 | 2.7594 | H18···H39Bii | 3.1321 |
C25···H33A | 2.9854 | H20A···H8Bii | 3.5729 |
C26···H1 | 2.7712 | H20B···C18i | 3.5066 |
C26···H24 | 2.9364 | H20B···H8Bii | 3.2338 |
C26···H33A | 3.4015 | H20B···H18i | 3.2963 |
C27···H1 | 2.7514 | H20B···H22Ci | 3.1433 |
C27···H26A | 3.2337 | H20C···C3ii | 3.5429 |
C27···H29 | 3.2653 | H20C···C4ii | 2.9817 |
C27···H31 | 3.2657 | H20C···C5ii | 2.7917 |
C27···H33A | 2.7457 | H20C···C6ii | 3.2022 |
C27···H33B | 2.8292 | H20C···C8ii | 3.5124 |
C27···H33C | 3.3286 | H20C···H5ii | 2.9869 |
C27···H35A | 3.3011 | H20C···H8Bii | 3.0416 |
C27···H35B | 2.9241 | H20C···H22Ci | 3.2104 |
C27···H35C | 2.6610 | H21A···N5ii | 2.9670 |
C27···H37 | 2.9201 | H21A···C8viii | 3.4877 |
C28···H1 | 3.5086 | H21A···C38ii | 3.0324 |
C28···H26A | 2.8425 | H21A···C39ii | 3.1714 |
C28···H37 | 3.4867 | H21A···H8Aviii | 3.3827 |
C29···H26A | 3.0561 | H21A···H8Cviii | 2.7311 |
C29···H31 | 3.2349 | H21A···H13Bxvi | 3.3412 |
C29···H33A | 3.1616 | H21A···H39Aii | 2.9822 |
C29···H33B | 3.1097 | H21A···H39Bii | 2.9933 |
C29···H33C | 2.5489 | H21B···C9ii | 3.5651 |
C29···H34A | 2.9717 | H21B···C24i | 3.3087 |
C29···H34B | 3.2675 | H21B···H9Aii | 2.7306 |
C29···H34C | 2.6234 | H21B···H9Bii | 3.5781 |
C31···H29 | 3.2353 | H21B···H13Axvi | 3.3967 |
C31···H34A | 2.9713 | H21B···H24i | 2.5252 |
C31···H34B | 2.6199 | H21B···H26Ci | 2.8714 |
C31···H34C | 3.2681 | H21B···H35Axvi | 3.4370 |
C31···H35A | 2.5824 | H21C···C8viii | 3.4464 |
C31···H35B | 3.0096 | H21C···C24i | 3.3053 |
C31···H35C | 3.2394 | H21C···C26i | 3.5248 |
C32···H1 | 3.0000 | H21C···H8Aviii | 2.9227 |
C33···H20B | 3.4710 | H21C···H8Cviii | 3.0843 |
C33···H26A | 3.2228 | H21C···H13Axvi | 3.5777 |
C33···H29 | 2.6495 | H21C···H13Bxvi | 3.2401 |
C33···H37 | 3.5050 | H21C···H13Cxvi | 3.5007 |
C34···H29 | 2.6679 | H21C···H24i | 2.8297 |
C34···H31 | 2.6662 | H21C···H26Ai | 3.5024 |
C35···H1 | 3.2341 | H21C···H26Ci | 2.9919 |
C35···H13A | 3.1570 | H21C···H33Ai | 3.4639 |
C35···H31 | 2.6566 | H21C···H33Ci | 3.0651 |
C36···H1 | 2.7432 | H22A···H9Bx | 3.4668 |
C36···H33A | 2.7884 | H22A···H34Biii | 3.5452 |
C36···H33B | 2.9301 | H22B···C28v | 3.3845 |
C36···H35B | 3.1455 | H22B···C29v | 3.1909 |
C36···H35C | 2.6286 | H22B···C33v | 3.5601 |
C37···H33A | 3.3542 | H22B···H5x | 3.2156 |
C37···H33B | 2.9843 | H22B···H29v | 3.0631 |
C37···H35C | 3.5630 | H22B···H33Bv | 3.2533 |
C37···H39A | 3.3658 | H22B···H33Cv | 3.4694 |
C37···H39B | 2.8604 | H22C···C5x | 3.4510 |
C37···H39C | 2.9032 | H22C···C15i | 3.5669 |
C38···H20A | 3.1049 | H22C···C16i | 3.4996 |
C39···H20A | 3.4336 | H22C···C20i | 3.4587 |
C39···H37 | 2.9341 | H22C···H5x | 2.7632 |
B1···H13A | 3.1723 | H22C···H9Bx | 2.7360 |
B1···H13C | 3.1559 | H22C···H16i | 3.3516 |
B1···H26A | 3.1389 | H22C···H20Bi | 3.1433 |
B1···H26B | 3.0980 | H22C···H20Ci | 3.2104 |
B1···H33A | 3.5862 | H24···C16i | 2.9898 |
B1···H35C | 3.0130 | H24···C17i | 2.7773 |
H1···H13A | 2.6960 | H24···C18i | 3.5084 |
H1···H13C | 2.5945 | H24···C21i | 2.8471 |
H1···H26A | 2.6000 | H24···H9Ax | 3.4664 |
H1···H26B | 2.5704 | H24···H9Bx | 3.0821 |
H1···H35C | 2.6571 | H24···H16i | 3.0189 |
H3···H7A | 3.1642 | H24···H21Bi | 2.5252 |
H3···H7B | 3.4129 | H24···H21Ci | 2.8297 |
H3···H7C | 2.3240 | H26A···C26iii | 3.5338 |
H3···H8A | 3.4981 | H26A···H13Ciii | 2.7421 |
H3···H8B | 3.0987 | H26A···H21Ci | 3.5024 |
H3···H8C | 2.4128 | H26A···H26Aiii | 3.4788 |
H5···H8A | 2.4829 | H26A···H26Biii | 2.7846 |
H5···H8B | 2.9919 | H26B···C26iii | 3.2711 |
H5···H8C | 3.5474 | H26B···C29iii | 3.4992 |
H5···H9A | 3.4521 | H26B···C30iii | 2.8846 |
H5···H9B | 2.3544 | H26B···C31iii | 2.8079 |
H5···H9C | 3.1269 | H26B···C32iii | 3.3769 |
H7A···H22A | 2.6820 | H26B···C34iii | 3.2797 |
H7B···H22A | 3.3964 | H26B···H1iii | 3.4513 |
H7C···H22A | 2.9474 | H26B···H26Aiii | 2.7846 |
H9A···H11 | 3.1461 | H26B···H26Biii | 2.9202 |
H9C···H11 | 2.9195 | H26B···H31iii | 2.9560 |
H11···H13A | 3.5932 | H26B···H34Biii | 2.9569 |
H11···H13B | 2.6725 | H26B···H34Ciii | 3.4174 |
H11···H13C | 3.5329 | H26C···C13iii | 3.3272 |
H13A···H35A | 2.9143 | H26C···C21i | 3.3845 |
H13A···H35C | 2.5695 | H26C···C31iii | 3.0996 |
H13C···H26B | 3.2160 | H26C···C32iii | 3.4280 |
H16···H20A | 3.2814 | H26C···C35iii | 3.5871 |
H16···H20B | 3.3197 | H26C···H1iii | 3.4778 |
H16···H20C | 2.2966 | H26C···H13Aiii | 3.0109 |
H16···H21A | 3.0912 | H26C···H13Ciii | 2.7923 |
H16···H21B | 2.4170 | H26C···H21Bi | 2.8714 |
H16···H21C | 3.5026 | H26C···H21Ci | 2.9919 |
H18···H21A | 3.0088 | H26C···H31iii | 2.8965 |
H18···H21B | 3.5451 | H26C···H35Aiii | 3.0558 |
H18···H21C | 2.4799 | H29···C5xii | 3.3008 |
H18···H22A | 3.4325 | H29···C8xii | 3.5333 |
H18···H22B | 2.3479 | H29···C13iii | 3.5389 |
H18···H22C | 3.1663 | H29···H5xii | 2.5158 |
H20A···H33A | 3.2866 | H29···H8Axii | 2.6608 |
H20A···H39A | 3.5403 | H29···H13Biii | 3.3974 |
H20A···H39C | 3.0711 | H29···H13Ciii | 2.8680 |
H20B···H33A | 2.7998 | H29···H22Bxi | 3.0631 |
H20B···H33B | 3.3797 | H31···C9ix | 3.0023 |
H20C···H39C | 3.4328 | H31···C26iii | 3.2801 |
H22A···H24 | 3.2171 | H31···H7Bxi | 3.2914 |
H22C···H24 | 2.8151 | H31···H7Cxi | 3.4098 |
H24···H26A | 3.5408 | H31···H9Aix | 3.0825 |
H24···H26C | 2.7084 | H31···H9Bix | 2.8099 |
H26A···H29 | 3.3496 | H31···H9Cix | 2.6211 |
H26A···H33A | 2.8881 | H31···H26Biii | 2.9560 |
H26A···H33C | 3.3747 | H31···H26Ciii | 2.8965 |
H29···H33A | 3.3570 | H31···H34Axiii | 3.0794 |
H29···H33B | 3.2629 | H33A···H21Ci | 3.4639 |
H29···H33C | 2.3200 | H33B···H8Bii | 2.9208 |
H29···H34A | 3.0372 | H33B···H22Bxi | 3.2533 |
H29···H34B | 3.5269 | H33C···C8xii | 3.4376 |
H29···H34C | 2.4517 | H33C···H8Axii | 2.5722 |
H31···H34A | 3.0336 | H33C···H8Bxii | 3.5225 |
H31···H34B | 2.4481 | H33C···H18i | 3.3821 |
H31···H34C | 3.5266 | H33C···H21Ci | 3.0651 |
H31···H35A | 2.3843 | H33C···H22Bxi | 3.4694 |
H31···H35B | 3.1055 | H34A···C9xii | 3.3839 |
H31···H35C | 3.4786 | H34A···C34xiii | 3.2494 |
H33B···H37 | 2.8912 | H34A···H5xii | 3.4195 |
H37···H39B | 2.9732 | H34A···H7Biii | 3.0309 |
H37···H39C | 3.0626 | H34A···H9Bxii | 2.8927 |
Tl1···H16ii | 3.3174 | H34A···H9Cxii | 3.0219 |
Tl1···H39Aii | 3.4260 | H34A···H31xiii | 3.0794 |
N2···H34Ciii | 3.3214 | H34A···H34Axiii | 2.7050 |
N4···H34Biii | 3.3567 | H34A···H34Bxiii | 3.0474 |
N5···H21Aii | 2.9670 | H34B···N4iii | 3.3567 |
C1···H11iv | 3.0585 | H34B···C24iii | 3.5719 |
C2···H11iv | 3.1677 | H34B···C25iii | 3.1340 |
C2···H35Bv | 3.1258 | H34B···C26iii | 3.4495 |
C2···H39Cii | 3.4285 | H34B···H7Aiii | 3.5307 |
C3···H11iv | 3.2425 | H34B···H7Biii | 2.8782 |
C3···H20Cii | 3.5429 | H34B···H22Aiii | 3.5452 |
C3···H35Bv | 2.7926 | H34B···H26Biii | 2.9569 |
C3···H39Cii | 2.8731 | H34B···H34Axiii | 3.0474 |
C4···H11iv | 3.2519 | H34C···N2iii | 3.3214 |
C4···H13Biv | 3.2088 | H34C···C5xii | 3.5622 |
C4···H20Cii | 2.9817 | H34C···C11iii | 3.1160 |
C4···H35Bv | 3.5518 | H34C···C12iii | 2.9006 |
C4···H39Cii | 3.4767 | H34C···C13iii | 3.2350 |
C5···H11iv | 3.0939 | H34C···H5xii | 3.1079 |
C5···H13Biv | 3.5911 | H34C···H7Biii | 2.9973 |
C5···H20Cii | 2.7917 | H34C···H9Bxii | 3.4948 |
C5···H22Cvi | 3.4510 | H34C···H9Cxii | 3.2891 |
C5···H29vii | 3.3008 | H34C···H11iii | 3.4105 |
C5···H34Cvii | 3.5622 | H34C···H13Biii | 3.4834 |
C6···H11iv | 2.9928 | H34C···H13Ciii | 2.8002 |
C6···H16ii | 3.1547 | H34C···H26Biii | 3.4174 |
C6···H20Cii | 3.2022 | H35A···C9ix | 3.1007 |
C7···H9Civ | 3.5551 | H35A···C11ix | 3.4081 |
C7···H35Bv | 3.3058 | H35A···H9Aix | 2.5585 |
C8···H13Biv | 3.1675 | H35A···H9Bix | 3.5251 |
C8···H20Cii | 3.5124 | H35A···H9Cix | 2.8238 |
C8···H21Aviii | 3.4877 | H35A···H11ix | 3.2234 |
C8···H21Cviii | 3.4464 | H35A···H21Bxv | 3.4370 |
C8···H29vii | 3.5333 | H35A···H26Ciii | 3.0558 |
C8···H33Cvii | 3.4376 | H35B···C2xi | 3.1258 |
C9···H16ii | 3.1021 | H35B···C3xi | 2.7926 |
C9···H21Bii | 3.5651 | H35B···C4xi | 3.5518 |
C9···H31ix | 3.0023 | H35B···C7xi | 3.3058 |
C9···H34Avii | 3.3839 | H35B···C11ix | 3.2817 |
C9···H35Aix | 3.1007 | H35B···H3xi | 2.5783 |
C11···H34Ciii | 3.1160 | H35B···H7Bxi | 3.4205 |
C11···H35Aix | 3.4081 | H35B···H7Cxi | 2.8635 |
C11···H35Bix | 3.2817 | H35B···H9Aix | 3.5705 |
C12···H34Ciii | 2.9006 | H35B···H9Cix | 3.2313 |
C13···H8Aiv | 3.5696 | H35B···H11ix | 2.7338 |
C13···H26Ciii | 3.3272 | H35B···H13Bix | 3.1814 |
C13···H29iii | 3.5389 | H35C···H13Bix | 3.5075 |
C13···H34Ciii | 3.2350 | H37···C39xiv | 3.3788 |
C14···H39Aii | 3.5248 | H37···H3xi | 2.6663 |
C15···H22Ci | 3.5669 | H37···H8Bii | 3.4884 |
C15···H39Aii | 3.4484 | H37···H8Cxi | 3.4459 |
C16···H9Aii | 3.5615 | H37···H39Bxiv | 2.7187 |
C16···H22Ci | 3.4996 | H37···H39Cxiv | 3.1854 |
C16···H24i | 2.9898 | H39A···Tl1ii | 3.4260 |
C16···H39Aii | 3.1043 | H39A···C14ii | 3.5248 |
C17···H24i | 2.7773 | H39A···C15ii | 3.4484 |
C17···H39Aii | 2.8622 | H39A···C16ii | 3.1043 |
C17···H39Bii | 3.3849 | H39A···C17ii | 2.8622 |
C18···H20Bi | 3.5066 | H39A···C18ii | 3.0169 |
C18···H24i | 3.5084 | H39A···C19ii | 3.3541 |
C18···H39Aii | 3.0169 | H39A···C21ii | 3.4447 |
C18···H39Bii | 3.1682 | H39A···H16ii | 3.5637 |
C19···H39Aii | 3.3541 | H39A···H18ii | 3.4442 |
C20···H8Bii | 3.4652 | H39A···H21Aii | 2.9822 |
C20···H22Ci | 3.4587 | H39B···C17ii | 3.3849 |
C21···H8Aviii | 3.5992 | H39B···C18ii | 3.1682 |
C21···H8Cviii | 3.3405 | H39B···C21ii | 3.5976 |
C21···H24i | 2.8471 | H39B···H3ii | 3.4594 |
C21···H26Ci | 3.3845 | H39B···H8Cxi | 2.9443 |
C21···H39Aii | 3.4447 | H39B···H18ii | 3.1321 |
C21···H39Bii | 3.5976 | H39B···H21Aii | 2.9933 |
C22···H5x | 3.3911 | H39B···H37xiv | 2.7187 |
C22···H9Bx | 3.5086 | H39C···C2ii | 3.4285 |
C24···H21Bi | 3.3087 | H39C···C3ii | 2.8731 |
C24···H21Ci | 3.3053 | H39C···C4ii | 3.4767 |
C24···H34Biii | 3.5719 | H39C···H3ii | 2.5928 |
C25···H34Biii | 3.1340 | H39C···H7Aii | 3.5003 |
C26···H13Ciii | 3.1832 | H39C···H7Cii | 3.5858 |
C26···H21Ci | 3.5248 | H39C···H8Bii | 3.4515 |
C26···H26Aiii | 3.5338 | H39C···H37xiv | 3.1854 |
C26···H26Biii | 3.2711 | | |
| | | |
N1—Tl1—N3 | 71.99 (5) | C6—C5—H5 | 119.085 |
N1—Tl1—N5 | 75.00 (5) | C2—C7—H7A | 109.464 |
N3—Tl1—N5 | 72.92 (5) | C2—C7—H7B | 109.472 |
Tl1—N1—N2 | 125.48 (11) | C2—C7—H7C | 109.473 |
Tl1—N1—C10 | 125.98 (8) | H7A—C7—H7B | 109.468 |
N2—N1—C10 | 107.65 (12) | H7A—C7—H7C | 109.469 |
N1—N2—C12 | 109.27 (14) | H7B—C7—H7C | 109.481 |
N1—N2—B1 | 119.51 (12) | C4—C8—H8A | 109.473 |
C12—N2—B1 | 130.48 (11) | C4—C8—H8B | 109.473 |
Tl1—N3—N4 | 123.98 (10) | C4—C8—H8C | 109.472 |
Tl1—N3—C23 | 128.27 (9) | H8A—C8—H8B | 109.472 |
N4—N3—C23 | 107.22 (11) | H8A—C8—H8C | 109.476 |
N3—N4—C25 | 109.67 (13) | H8B—C8—H8C | 109.462 |
N3—N4—B1 | 119.88 (11) | C6—C9—H9A | 109.471 |
C25—N4—B1 | 130.06 (11) | C6—C9—H9B | 109.467 |
N5—N6—C36 | 109.69 (13) | C6—C9—H9C | 109.467 |
N5—N6—B1 | 122.21 (13) | H9A—C9—H9B | 109.479 |
C36—N6—B1 | 126.68 (12) | H9A—C9—H9C | 109.474 |
Tl1—N5—N6 | 120.44 (10) | H9B—C9—H9C | 109.470 |
Tl1—N5—C38 | 124.46 (9) | C10—C11—H11 | 127.347 |
N6—N5—C38 | 106.71 (13) | C12—C11—H11 | 127.350 |
C2—C1—C6 | 119.82 (13) | C12—C13—H13A | 109.462 |
C2—C1—C10 | 119.22 (14) | C12—C13—H13B | 109.474 |
C6—C1—C10 | 120.86 (14) | C12—C13—H13C | 109.477 |
C1—C2—C3 | 118.84 (16) | H13A—C13—H13B | 109.470 |
C1—C2—C7 | 121.96 (14) | H13A—C13—H13C | 109.467 |
C3—C2—C7 | 119.20 (16) | H13B—C13—H13C | 109.478 |
C2—C3—C4 | 122.08 (17) | C15—C16—H16 | 119.100 |
C3—C4—C5 | 118.21 (14) | C17—C16—H16 | 119.105 |
C3—C4—C8 | 120.77 (18) | C17—C18—H18 | 118.935 |
C5—C4—C8 | 121.00 (19) | C19—C18—H18 | 118.923 |
C4—C5—C6 | 121.84 (17) | C15—C20—H20A | 109.474 |
C1—C6—C5 | 119.10 (15) | C15—C20—H20B | 109.469 |
C1—C6—C9 | 121.33 (13) | C15—C20—H20C | 109.473 |
C5—C6—C9 | 119.58 (15) | H20A—C20—H20B | 109.472 |
N1—C10—C1 | 117.58 (13) | H20A—C20—H20C | 109.467 |
N1—C10—C11 | 109.69 (14) | H20B—C20—H20C | 109.472 |
C1—C10—C11 | 132.70 (17) | C17—C21—H21A | 109.472 |
C10—C11—C12 | 105.30 (16) | C17—C21—H21B | 109.470 |
N2—C12—C11 | 108.09 (12) | C17—C21—H21C | 109.472 |
N2—C12—C13 | 123.75 (16) | H21A—C21—H21B | 109.473 |
C11—C12—C13 | 128.16 (16) | H21A—C21—H21C | 109.480 |
C15—C14—C19 | 119.63 (15) | H21B—C21—H21C | 109.460 |
C15—C14—C23 | 118.91 (16) | C19—C22—H22A | 109.465 |
C19—C14—C23 | 121.45 (17) | C19—C22—H22B | 109.471 |
C14—C15—C16 | 119.10 (17) | C19—C22—H22C | 109.469 |
C14—C15—C20 | 121.96 (14) | H22A—C22—H22B | 109.479 |
C16—C15—C20 | 118.91 (17) | H22A—C22—H22C | 109.467 |
C15—C16—C17 | 121.79 (19) | H22B—C22—H22C | 109.476 |
C16—C17—C18 | 118.22 (16) | C23—C24—H24 | 127.142 |
C16—C17—C21 | 120.59 (19) | C25—C24—H24 | 127.138 |
C18—C17—C21 | 121.17 (19) | C25—C26—H26A | 109.476 |
C17—C18—C19 | 122.14 (19) | C25—C26—H26B | 109.476 |
C14—C19—C18 | 118.94 (19) | C25—C26—H26C | 109.475 |
C14—C19—C22 | 121.21 (16) | H26A—C26—H26B | 109.467 |
C18—C19—C22 | 119.86 (19) | H26A—C26—H26C | 109.469 |
N3—C23—C14 | 118.73 (13) | H26B—C26—H26C | 109.463 |
N3—C23—C24 | 109.71 (13) | C28—C29—H29 | 118.933 |
C14—C23—C24 | 131.44 (16) | C30—C29—H29 | 118.943 |
C23—C24—C25 | 105.72 (15) | C30—C31—H31 | 118.974 |
N4—C25—C24 | 107.66 (12) | C32—C31—H31 | 118.978 |
N4—C25—C26 | 122.65 (15) | C28—C33—H33A | 109.471 |
C24—C25—C26 | 129.59 (15) | C28—C33—H33B | 109.472 |
C28—C27—C32 | 120.06 (14) | C28—C33—H33C | 109.475 |
C28—C27—C36 | 119.57 (15) | H33A—C33—H33B | 109.469 |
C32—C27—C36 | 120.36 (16) | H33A—C33—H33C | 109.467 |
C27—C28—C29 | 118.89 (17) | H33B—C33—H33C | 109.474 |
C27—C28—C33 | 121.18 (15) | C30—C34—H34A | 109.473 |
C29—C28—C33 | 119.90 (19) | C30—C34—H34B | 109.475 |
C28—C29—C30 | 122.1 (2) | C30—C34—H34C | 109.468 |
C29—C30—C31 | 118.12 (15) | H34A—C34—H34B | 109.470 |
C29—C30—C34 | 121.1 (2) | H34A—C34—H34C | 109.467 |
C31—C30—C34 | 120.78 (18) | H34B—C34—H34C | 109.474 |
C30—C31—C32 | 122.05 (17) | C32—C35—H35A | 109.470 |
C27—C32—C31 | 118.75 (17) | C32—C35—H35B | 109.468 |
C27—C32—C35 | 121.06 (13) | C32—C35—H35C | 109.470 |
C31—C32—C35 | 120.19 (16) | H35A—C35—H35B | 109.474 |
N6—C36—C27 | 123.17 (15) | H35A—C35—H35C | 109.469 |
N6—C36—C37 | 107.76 (13) | H35B—C35—H35C | 109.477 |
C27—C36—C37 | 129.04 (18) | C36—C37—H37 | 127.145 |
C36—C37—C38 | 105.71 (17) | C38—C37—H37 | 127.140 |
N5—C38—C37 | 110.12 (14) | C38—C39—H39A | 109.471 |
N5—C38—C39 | 121.31 (16) | C38—C39—H39B | 109.475 |
C37—C38—C39 | 128.54 (19) | C38—C39—H39C | 109.474 |
N2—B1—N4 | 109.76 (14) | H39A—C39—H39B | 109.475 |
N2—B1—N6 | 112.23 (12) | H39A—C39—H39C | 109.467 |
N4—B1—N6 | 107.22 (13) | H39B—C39—H39C | 109.465 |
C2—C3—H3 | 118.965 | N2—B1—H1 | 109.194 |
C4—C3—H3 | 118.959 | N4—B1—H1 | 109.195 |
C4—C5—H5 | 119.076 | N5—B1—H1 | 109.186 |
| | | |
N1—Tl1—N3—N4 | 32.04 (10) | C10—C1—C2—C3 | 174.04 (14) |
N1—Tl1—N3—C23 | −138.50 (13) | C10—C1—C2—C7 | −6.1 (2) |
N3—Tl1—N1—N2 | −49.87 (10) | C6—C1—C10—N1 | 114.93 (17) |
N3—Tl1—N1—C10 | 142.27 (11) | C6—C1—C10—C11 | −67.4 (2) |
N1—Tl1—N5—N6 | −45.35 (10) | C10—C1—C6—C5 | −173.18 (14) |
N1—Tl1—N5—C38 | 170.77 (11) | C10—C1—C6—C9 | 6.5 (3) |
N5—Tl1—N1—N2 | 26.67 (9) | C1—C2—C3—C4 | −0.6 (3) |
N5—Tl1—N1—C10 | −141.19 (11) | C7—C2—C3—C4 | 179.58 (17) |
N3—Tl1—N5—N6 | 30.03 (9) | C2—C3—C4—C5 | 2.7 (3) |
N3—Tl1—N5—C38 | −113.85 (11) | C2—C3—C4—C8 | −175.43 (16) |
N5—Tl1—N3—N4 | −47.30 (11) | C3—C4—C5—C6 | −1.9 (3) |
N5—Tl1—N3—C23 | 142.16 (13) | C8—C4—C5—C6 | 176.28 (18) |
Tl1—N1—N2—C12 | −169.63 (7) | C4—C5—C6—C1 | −1.1 (3) |
Tl1—N1—N2—B1 | 19.22 (17) | C4—C5—C6—C9 | 179.29 (16) |
Tl1—N1—C10—C1 | −12.43 (19) | N1—C10—C11—C12 | 0.39 (18) |
Tl1—N1—C10—C11 | 169.35 (8) | C1—C10—C11—C12 | −177.46 (16) |
N2—N1—C10—C1 | 177.92 (11) | C10—C11—C12—N2 | −0.34 (18) |
N2—N1—C10—C11 | −0.30 (17) | C10—C11—C12—C13 | 179.10 (14) |
C10—N1—N2—C12 | 0.08 (16) | C15—C14—C19—C18 | 3.5 (3) |
C10—N1—N2—B1 | −171.07 (11) | C15—C14—C19—C22 | −176.92 (15) |
N1—N2—C12—C11 | 0.17 (17) | C19—C14—C15—C16 | −4.3 (3) |
N1—N2—C12—C13 | −179.30 (13) | C19—C14—C15—C20 | 173.61 (15) |
N1—N2—B1—N4 | 49.49 (17) | C15—C14—C23—N3 | −60.7 (2) |
N1—N2—B1—N6 | −69.63 (17) | C15—C14—C23—C24 | 114.7 (2) |
C12—N2—B1—N4 | −119.50 (16) | C23—C14—C15—C16 | 174.37 (14) |
C12—N2—B1—N6 | 121.38 (16) | C23—C14—C15—C20 | −7.7 (2) |
B1—N2—C12—C11 | 170.03 (14) | C19—C14—C23—N3 | 117.90 (19) |
B1—N2—C12—C13 | −9.4 (3) | C19—C14—C23—C24 | −66.6 (3) |
Tl1—N3—N4—C25 | −172.69 (9) | C23—C14—C19—C18 | −175.13 (15) |
Tl1—N3—N4—B1 | 13.8 (2) | C23—C14—C19—C22 | 4.5 (3) |
Tl1—N3—C23—C14 | −12.3 (2) | C14—C15—C16—C17 | 1.3 (3) |
Tl1—N3—C23—C24 | 171.27 (9) | C20—C15—C16—C17 | −176.65 (16) |
N4—N3—C23—C14 | 175.85 (14) | C15—C16—C17—C18 | 2.4 (3) |
N4—N3—C23—C24 | −0.5 (2) | C15—C16—C17—C21 | −175.81 (16) |
C23—N3—N4—C25 | −0.46 (19) | C16—C17—C18—C19 | −3.3 (3) |
C23—N3—N4—B1 | −173.95 (14) | C21—C17—C18—C19 | 174.96 (18) |
N3—N4—C25—C24 | 1.3 (2) | C17—C18—C19—C14 | 0.3 (3) |
N3—N4—C25—C26 | −175.35 (15) | C17—C18—C19—C22 | −179.27 (17) |
N3—N4—B1—N2 | −67.91 (19) | N3—C23—C24—C25 | 1.3 (2) |
N3—N4—B1—N6 | 54.24 (19) | C14—C23—C24—C25 | −174.49 (19) |
C25—N4—B1—N2 | 120.10 (19) | C23—C24—C25—N4 | −1.5 (2) |
C25—N4—B1—N6 | −117.74 (19) | C23—C24—C25—C26 | 174.78 (18) |
B1—N4—C25—C24 | 173.88 (16) | C28—C27—C32—C31 | 0.2 (3) |
B1—N4—C25—C26 | −2.7 (3) | C28—C27—C32—C35 | 179.59 (16) |
N5—N6—C36—C27 | 177.38 (13) | C32—C27—C28—C29 | −0.7 (3) |
N5—N6—C36—C37 | −0.83 (17) | C32—C27—C28—C33 | −178.57 (16) |
C36—N6—N5—Tl1 | −148.81 (11) | C28—C27—C36—N6 | −104.2 (2) |
C36—N6—N5—C38 | 0.70 (16) | C28—C27—C36—C37 | 73.6 (2) |
N5—N6—B1—N2 | 46.00 (18) | C36—C27—C28—C29 | −179.91 (16) |
N5—N6—B1—N4 | −74.60 (17) | C36—C27—C28—C33 | 2.2 (3) |
B1—N6—N5—Tl1 | 18.40 (19) | C32—C27—C36—N6 | 76.6 (2) |
B1—N6—N5—C38 | 167.91 (12) | C32—C27—C36—C37 | −105.6 (2) |
C36—N6—B1—N2 | −149.06 (13) | C36—C27—C32—C31 | 179.44 (15) |
C36—N6—B1—N4 | 90.34 (16) | C36—C27—C32—C35 | −1.2 (3) |
B1—N6—C36—C27 | 10.9 (2) | C27—C28—C29—C30 | 0.4 (3) |
B1—N6—C36—C37 | −167.34 (13) | C33—C28—C29—C30 | 178.3 (2) |
Tl1—N5—C38—C37 | 147.67 (9) | C28—C29—C30—C31 | 0.4 (3) |
Tl1—N5—C38—C39 | −30.7 (2) | C28—C29—C30—C34 | −177.81 (19) |
N6—N5—C38—C37 | −0.29 (17) | C29—C30—C31—C32 | −0.8 (3) |
N6—N5—C38—C39 | −178.63 (12) | C34—C30—C31—C32 | 177.3 (2) |
C2—C1—C6—C5 | 3.2 (3) | C30—C31—C32—C27 | 0.6 (3) |
C2—C1—C6—C9 | −177.11 (15) | C30—C31—C32—C35 | −178.82 (18) |
C6—C1—C2—C3 | −2.4 (3) | N6—C36—C37—C38 | 0.63 (18) |
C6—C1—C2—C7 | 177.38 (15) | C27—C36—C37—C38 | −177.44 (15) |
C2—C1—C10—N1 | −61.5 (2) | C36—C37—C38—N5 | −0.21 (19) |
C2—C1—C10—C11 | 116.21 (19) | C36—C37—C38—C39 | 177.98 (15) |
Symmetry codes: (i) −x, −y+2, −z+2; (ii) −x+1, −y+2, −z+2; (iii) −x, −y+1, −z+1; (iv) −x+1, −y+2, −z+1; (v) x, y+1, z; (vi) x+1, y, z; (vii) x+1, y+1, z; (viii) −x+1, −y+3, −z+2; (ix) −x+1, −y+1, −z+1; (x) x−1, y, z; (xi) x, y−1, z; (xii) x−1, y−1, z; (xiii) −x, −y, −z+1; (xiv) −x+1, −y+1, −z+2; (xv) x, y−1, z−1; (xvi) x, y+1, z+1. |
Selected bond lengths (Å) and angles (°) in (I) and (II) top | (I) | | (II) |
Tl1—N1 | 2.5342 (19) | Tl1—N1 | 2.4915 (14) |
| | Tl1—N3 | 2.5567 (12) |
| | Tl1—N5 | 2.5959 (15) |
N2—B1 | 1.548 (2) | N2—B1 | 1.555 (2) |
| | N4—B1 | 1.554 (2) |
| | N6—B1 | 1.554 (2) |
N1—Tl1—N1i | 73.32 (7) | N1—Tl1—N3 | 71.99 (5) |
| | N1—Tl1— N5 | 75.00 (5) |
| | N3—Tl1—N5 | 72.92 (5) |
N2—B1—N2ii | 109.99 (19) | N2–B1–N4 | 109.76 (14) |
| | N2—B1—N6 | 112.23 (12) |
| | N4—B1—N6 | 107.22 (13) |
Symmetry codes: (i) -y+1, x-y, z;
(ii) -x+y+1, -x+1, z. |