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The introduction of poly(1
H-pyrazolyl)borate anions, better known as scorpionates, as negatively charged ligands for a great diversity of metal cations has had a tremendous influence in coordination chemistry. The structures of two salts of tetrakispyrazolylborate, namely [tetrakis(3-phenyl-1
H-pyrazol-1-yl)borato]thallium(I), [Tl(C
36H
28BN
8)], and
catena-poly[potassium-[
2-tetrakis(3-cyclopropyl-1
H-pyrazol-1-yl)borato]], [K(C
24H
28BN
8)]
n, have been determined at 296 K in the monoclinic
P2
1/
c and
C2/
c space groups, respectively. In their crystal structures, the thallium salt presents discrete molecular motifs, while the potassium salt shows infinite polymeric chains. The
13C and
15N CPMAS (cross polarization magic angle spinning) NMR spectra of these compounds were recorded and the chemical shifts compared with theoretically calculated ones at the GIAO/B3LYP/6-311++G(d,p) level. Both techniques are complementary and mutually consistent.
Supporting information
CCDC references: 1457065; 1457064
For both compounds, data collection: APEX2 (Bruker, 2013); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SIR2014 (Burla et al., 2015); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: Mercury (Macrae et al., 2008) and ORTEP-3 for Windows (Farrugia , 2012).
(comp1) [Tetrakis(3-phenyl-1
H-pyrazol-1-yl)borato]thallium(I)
top
Crystal data top
[Tl(C36H28BN8)] | F(000) = 1544 |
Mr = 787.85 | Dx = 1.61 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -P 2ybc | Cell parameters from 9879 reflections |
a = 9.9552 (6) Å | θ = 3.6–74.3° |
b = 13.1693 (8) Å | µ = 9.86 mm−1 |
c = 24.7993 (14) Å | T = 296 K |
β = 91.463 (2)° | Prism, colourless |
V = 3250.2 (3) Å3 | 0.06 × 0.02 × 0.02 mm |
Z = 4 | |
Data collection top
Bruker APEXII CCD diffractometer | 5748 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.045 |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | θmax = 74.5°, θmin = 3.6° |
Tmin = 0.218, Tmax = 0.754 | h = −12→12 |
45124 measured reflections | k = −16→16 |
6614 independent reflections | l = −30→30 |
Refinement top
Refinement on F2 | 28 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
wR(F2) = 0.072 | w = 1/[σ2(Fo2) + (0.0358P)2 + 1.7721P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.003 |
6614 reflections | Δρmax = 0.42 e Å−3 |
470 parameters | Δρmin = −1.27 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Tl1 | 0.14310 (2) | 0.04696 (2) | 0.13345 (2) | 0.05693 (6) | |
B1 | 0.0505 (3) | 0.1455 (3) | 0.26229 (12) | 0.0426 (7) | |
N1 | −0.0280 (2) | 0.14475 (18) | 0.35851 (9) | 0.0439 (5) | |
N2 | 0.0314 (2) | 0.19608 (19) | 0.31732 (9) | 0.0442 (5) | |
C1 | 0.0931 (3) | 0.2809 (3) | 0.33641 (13) | 0.0555 (8) | |
H1 | 0.1411 | 0.3272 | 0.3161 | 0.067* | |
C2 | 0.0728 (4) | 0.2868 (3) | 0.39028 (13) | 0.0589 (8) | |
H2 | 0.1027 | 0.3373 | 0.4139 | 0.071* | |
C3 | −0.0029 (3) | 0.2005 (2) | 0.40278 (11) | 0.0452 (6) | |
C4 | −0.0498 (3) | 0.1690 (2) | 0.45605 (11) | 0.0484 (7) | |
C5 | −0.1287 (5) | 0.0862 (4) | 0.46254 (16) | 0.0809 (12) | |
H5 | −0.1581 | 0.0498 | 0.4324 | 0.097* | |
C6 | −0.1662 (6) | 0.0548 (4) | 0.5134 (2) | 0.0971 (16) | |
H6 | −0.2172 | −0.0039 | 0.517 | 0.117* | |
C7 | −0.1289 (5) | 0.1093 (4) | 0.55790 (16) | 0.0828 (13) | |
H7 | −0.1568 | 0.0898 | 0.5919 | 0.099* | |
C8 | −0.0515 (6) | 0.1914 (4) | 0.55210 (15) | 0.0964 (16) | |
H8 | −0.0243 | 0.2283 | 0.5825 | 0.116* | |
C9 | −0.0113 (5) | 0.2225 (3) | 0.50173 (14) | 0.0821 (13) | |
H9 | 0.0423 | 0.28 | 0.4986 | 0.098* | |
N1A | −0.0851 (3) | 0.0801 (2) | 0.18346 (9) | 0.0472 (6) | |
N2A | −0.0821 (2) | 0.10520 (19) | 0.23705 (9) | 0.0442 (5) | |
C1A | −0.2042 (3) | 0.0907 (3) | 0.25772 (13) | 0.0523 (7) | |
H1A | −0.2273 | 0.103 | 0.2932 | 0.063* | |
C2A | −0.2885 (3) | 0.0548 (3) | 0.21775 (14) | 0.0559 (8) | |
H2A | −0.3787 | 0.0376 | 0.2206 | 0.067* | |
C3A | −0.2107 (3) | 0.0495 (2) | 0.17183 (12) | 0.0462 (7) | |
C4A | −0.2507 (3) | 0.0167 (2) | 0.11696 (12) | 0.0494 (7) | |
C5A | −0.1837 (4) | 0.0510 (3) | 0.07217 (14) | 0.0622 (9) | |
H5A | −0.1131 | 0.0968 | 0.0765 | 0.075* | |
C6A | −0.2211 (4) | 0.0177 (4) | 0.02101 (15) | 0.0776 (11) | |
H6A | −0.1749 | 0.0409 | −0.0087 | 0.093* | |
C7A | −0.3251 (5) | −0.0487 (4) | 0.01375 (17) | 0.0845 (13) | |
H7A | −0.3494 | −0.0711 | −0.0207 | 0.101* | |
C8A | −0.3933 (4) | −0.0823 (4) | 0.05747 (17) | 0.0779 (11) | |
H8A | −0.4642 | −0.1277 | 0.0526 | 0.093* | |
C9A | −0.3582 (4) | −0.0494 (3) | 0.10894 (15) | 0.0619 (9) | |
H9A | −0.4066 | −0.0716 | 0.1382 | 0.074* | |
N1B | 0.1877 (2) | −0.00706 (19) | 0.23031 (9) | 0.0421 (5) | |
N2B | 0.1539 (2) | 0.05854 (17) | 0.27058 (9) | 0.0420 (5) | |
C1B | 0.2282 (3) | 0.0377 (2) | 0.31547 (12) | 0.0501 (7) | |
H1B | 0.2235 | 0.0717 | 0.3482 | 0.06* | |
C2B | 0.3117 (3) | −0.0417 (3) | 0.30479 (13) | 0.0551 (8) | |
H2B | 0.3737 | −0.072 | 0.3284 | 0.066* | |
C3B | 0.2844 (3) | −0.0680 (2) | 0.25089 (12) | 0.0442 (6) | |
C4B | 0.3480 (3) | −0.1468 (2) | 0.21797 (12) | 0.0452 (6) | |
C5B | 0.2896 (3) | −0.1823 (2) | 0.17041 (14) | 0.0528 (7) | |
H5B | 0.2059 | −0.1576 | 0.1592 | 0.063* | |
C6B | 0.3536 (4) | −0.2541 (3) | 0.13897 (15) | 0.0621 (9) | |
H6B | 0.3145 | −0.2756 | 0.1065 | 0.075* | |
C7B | 0.4759 (4) | −0.2932 (3) | 0.15651 (17) | 0.0705 (10) | |
H7B | 0.5193 | −0.3414 | 0.1358 | 0.085* | |
C8B | 0.5335 (4) | −0.2610 (3) | 0.20452 (17) | 0.0704 (10) | |
H8B | 0.6142 | −0.2894 | 0.2168 | 0.084* | |
C9B | 0.4720 (3) | −0.1867 (3) | 0.23473 (14) | 0.0587 (8) | |
H9B | 0.5136 | −0.1633 | 0.2664 | 0.07* | |
N1C | 0.2122 (2) | 0.20837 (19) | 0.19175 (10) | 0.0464 (5) | |
N2C | 0.1052 (2) | 0.22658 (19) | 0.22339 (9) | 0.0443 (5) | |
C1C | 0.0520 (4) | 0.3186 (2) | 0.21191 (14) | 0.0563 (8) | |
H1C | −0.0226 | 0.347 | 0.228 | 0.068* | |
C2C | 0.1258 (4) | 0.3627 (3) | 0.17292 (14) | 0.0599 (8) | |
H2C | 0.1124 | 0.4262 | 0.1573 | 0.072* | |
C3C | 0.2261 (3) | 0.2923 (2) | 0.16144 (13) | 0.0526 (7) | |
C4C | 0.3363 (12) | 0.3032 (13) | 0.1237 (4) | 0.064 (5) | 0.397 (18) |
C5C | 0.422 (2) | 0.226 (2) | 0.1133 (8) | 0.059 (5) | 0.397 (18) |
H5C | 0.4134 | 0.1643 | 0.1307 | 0.071* | 0.397 (18) |
C6C | 0.525 (2) | 0.2413 (19) | 0.0756 (9) | 0.069 (5) | 0.397 (18) |
H6C | 0.5829 | 0.1888 | 0.0673 | 0.083* | 0.397 (18) |
C7C | 0.5359 (18) | 0.3295 (17) | 0.0528 (8) | 0.092 (6) | 0.397 (18) |
H7C | 0.6045 | 0.3394 | 0.0286 | 0.11* | 0.397 (18) |
C8C | 0.4540 (14) | 0.4057 (18) | 0.0626 (8) | 0.110 (7) | 0.397 (18) |
H8C | 0.4636 | 0.4671 | 0.0446 | 0.132* | 0.397 (18) |
C9C | 0.3533 (12) | 0.3942 (14) | 0.1000 (8) | 0.087 (6) | 0.397 (18) |
H9C | 0.2984 | 0.4487 | 0.1085 | 0.104* | 0.397 (18) |
C4D | 0.3282 (10) | 0.2899 (8) | 0.1192 (4) | 0.064 (3) | 0.603 (18) |
C5D | 0.4437 (15) | 0.2330 (12) | 0.1254 (6) | 0.058 (3) | 0.603 (18) |
H5D | 0.4574 | 0.196 | 0.157 | 0.069* | 0.603 (18) |
C6D | 0.539 (2) | 0.2290 (13) | 0.0867 (8) | 0.082 (4) | 0.603 (18) |
H6D | 0.6148 | 0.1886 | 0.0922 | 0.098* | 0.603 (18) |
C7D | 0.5227 (14) | 0.2870 (9) | 0.0373 (5) | 0.080 (3) | 0.603 (18) |
H7D | 0.5882 | 0.2864 | 0.0113 | 0.096* | 0.603 (18) |
C8D | 0.4087 (13) | 0.3422 (10) | 0.0305 (5) | 0.108 (5) | 0.603 (18) |
H8D | 0.3953 | 0.3794 | −0.0011 | 0.13* | 0.603 (18) |
C9D | 0.3122 (12) | 0.3443 (9) | 0.0691 (5) | 0.091 (4) | 0.603 (18) |
H9D | 0.2344 | 0.3819 | 0.0627 | 0.109* | 0.603 (18) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tl1 | 0.07118 (10) | 0.06286 (10) | 0.03707 (8) | 0.00501 (6) | 0.00786 (6) | −0.00129 (5) |
B1 | 0.0456 (16) | 0.0458 (17) | 0.0367 (14) | 0.0003 (14) | 0.0067 (12) | −0.0027 (13) |
N1 | 0.0494 (13) | 0.0463 (13) | 0.0363 (11) | −0.0030 (11) | 0.0051 (9) | −0.0047 (10) |
N2 | 0.0484 (13) | 0.0464 (13) | 0.0380 (11) | −0.0046 (11) | 0.0058 (9) | −0.0057 (10) |
C1 | 0.0639 (19) | 0.0528 (18) | 0.0498 (16) | −0.0143 (16) | 0.0055 (14) | −0.0040 (14) |
C2 | 0.071 (2) | 0.059 (2) | 0.0467 (16) | −0.0150 (17) | 0.0038 (14) | −0.0147 (14) |
C3 | 0.0479 (15) | 0.0490 (16) | 0.0386 (14) | −0.0007 (13) | 0.0009 (11) | −0.0046 (12) |
C4 | 0.0531 (16) | 0.0540 (18) | 0.0380 (14) | 0.0051 (14) | 0.0019 (12) | −0.0029 (12) |
C5 | 0.103 (3) | 0.094 (3) | 0.0460 (19) | −0.033 (3) | 0.0108 (19) | −0.0048 (19) |
C6 | 0.112 (4) | 0.119 (4) | 0.060 (3) | −0.038 (3) | 0.017 (2) | 0.013 (2) |
C7 | 0.107 (3) | 0.094 (3) | 0.048 (2) | 0.016 (3) | 0.018 (2) | 0.011 (2) |
C8 | 0.174 (5) | 0.079 (3) | 0.0362 (18) | 0.007 (3) | 0.003 (2) | −0.0063 (18) |
C9 | 0.141 (4) | 0.064 (2) | 0.0409 (17) | −0.012 (3) | −0.002 (2) | −0.0039 (17) |
N1A | 0.0525 (14) | 0.0545 (14) | 0.0348 (12) | 0.0006 (12) | 0.0017 (10) | −0.0046 (10) |
N2A | 0.0484 (13) | 0.0489 (14) | 0.0355 (11) | 0.0019 (11) | 0.0035 (9) | −0.0043 (10) |
C1A | 0.0491 (16) | 0.0642 (19) | 0.0441 (15) | −0.0030 (15) | 0.0110 (12) | −0.0087 (14) |
C2A | 0.0460 (16) | 0.073 (2) | 0.0489 (17) | −0.0018 (15) | 0.0049 (13) | −0.0057 (15) |
C3A | 0.0533 (16) | 0.0450 (16) | 0.0401 (15) | 0.0040 (13) | −0.0026 (12) | −0.0006 (12) |
C4A | 0.0553 (17) | 0.0519 (17) | 0.0408 (15) | 0.0071 (14) | −0.0044 (12) | −0.0007 (13) |
C5A | 0.064 (2) | 0.077 (2) | 0.0451 (17) | −0.0010 (18) | −0.0044 (14) | 0.0051 (15) |
C6A | 0.081 (3) | 0.112 (3) | 0.0392 (17) | 0.005 (3) | −0.0019 (16) | 0.0031 (19) |
C7A | 0.088 (3) | 0.117 (4) | 0.048 (2) | −0.003 (3) | −0.0152 (19) | −0.012 (2) |
C8A | 0.078 (3) | 0.093 (3) | 0.062 (2) | −0.012 (2) | −0.0157 (19) | −0.010 (2) |
C9A | 0.065 (2) | 0.071 (2) | 0.0488 (18) | −0.0037 (17) | −0.0073 (15) | −0.0019 (15) |
N1B | 0.0445 (12) | 0.0427 (12) | 0.0392 (12) | 0.0030 (10) | 0.0050 (9) | −0.0002 (10) |
N2B | 0.0473 (13) | 0.0441 (13) | 0.0348 (11) | −0.0008 (10) | 0.0043 (9) | −0.0007 (9) |
C1B | 0.0527 (17) | 0.0601 (19) | 0.0375 (14) | −0.0016 (15) | 0.0009 (12) | 0.0020 (12) |
C2B | 0.0549 (18) | 0.066 (2) | 0.0447 (16) | 0.0078 (16) | −0.0024 (13) | 0.0067 (14) |
C3B | 0.0407 (14) | 0.0472 (16) | 0.0450 (15) | −0.0044 (12) | 0.0056 (11) | 0.0059 (12) |
C4B | 0.0409 (14) | 0.0444 (15) | 0.0507 (15) | −0.0008 (12) | 0.0085 (11) | 0.0068 (12) |
C5B | 0.0443 (16) | 0.0493 (17) | 0.0647 (19) | 0.0016 (14) | 0.0018 (14) | −0.0023 (15) |
C6B | 0.060 (2) | 0.064 (2) | 0.063 (2) | −0.0008 (17) | 0.0062 (15) | −0.0111 (16) |
C7B | 0.061 (2) | 0.068 (2) | 0.084 (3) | 0.0122 (18) | 0.0167 (18) | −0.013 (2) |
C8B | 0.0521 (19) | 0.078 (3) | 0.081 (2) | 0.0204 (18) | 0.0037 (17) | −0.004 (2) |
C9B | 0.0499 (17) | 0.066 (2) | 0.0597 (18) | 0.0075 (16) | −0.0015 (14) | 0.0029 (16) |
N1C | 0.0442 (13) | 0.0448 (13) | 0.0506 (13) | 0.0022 (11) | 0.0089 (10) | 0.0061 (11) |
N2C | 0.0475 (13) | 0.0446 (13) | 0.0410 (12) | 0.0037 (11) | 0.0069 (10) | 0.0009 (10) |
C1C | 0.0631 (19) | 0.0504 (18) | 0.0558 (18) | 0.0138 (16) | 0.0107 (15) | 0.0041 (14) |
C2C | 0.067 (2) | 0.0494 (18) | 0.0632 (19) | 0.0087 (16) | 0.0083 (16) | 0.0136 (16) |
C3C | 0.0474 (16) | 0.0499 (17) | 0.0607 (18) | 0.0003 (14) | 0.0059 (13) | 0.0127 (14) |
C4C | 0.049 (9) | 0.072 (10) | 0.070 (10) | −0.005 (8) | −0.007 (7) | 0.042 (7) |
C5C | 0.051 (7) | 0.074 (8) | 0.052 (9) | −0.009 (6) | 0.001 (6) | 0.000 (6) |
C6C | 0.049 (7) | 0.090 (10) | 0.071 (9) | 0.004 (7) | 0.023 (6) | 0.009 (7) |
C7C | 0.062 (7) | 0.128 (18) | 0.087 (12) | −0.018 (11) | 0.018 (7) | 0.022 (11) |
C8C | 0.089 (9) | 0.127 (15) | 0.115 (14) | −0.011 (10) | 0.030 (8) | 0.063 (13) |
C9C | 0.075 (7) | 0.090 (10) | 0.097 (11) | 0.013 (7) | 0.025 (7) | 0.049 (9) |
C4D | 0.058 (7) | 0.052 (5) | 0.083 (7) | 0.000 (5) | 0.028 (5) | 0.014 (5) |
C5D | 0.055 (6) | 0.069 (5) | 0.049 (5) | 0.008 (4) | 0.006 (4) | 0.008 (4) |
C6D | 0.077 (7) | 0.084 (6) | 0.085 (7) | 0.018 (5) | 0.016 (5) | 0.020 (5) |
C7D | 0.085 (7) | 0.072 (6) | 0.087 (7) | −0.004 (5) | 0.050 (5) | 0.002 (5) |
C8D | 0.115 (8) | 0.118 (9) | 0.095 (7) | 0.031 (7) | 0.055 (6) | 0.059 (7) |
C9D | 0.089 (6) | 0.093 (7) | 0.092 (7) | 0.032 (6) | 0.045 (5) | 0.042 (6) |
Geometric parameters (Å, º) top
Tl1—N1B | 2.533 (2) | C1B—C2B | 1.365 (5) |
Tl1—N1C | 2.652 (3) | C1B—H1B | 0.93 |
Tl1—N1A | 2.652 (3) | C2B—C3B | 1.401 (4) |
B1—N2 | 1.535 (4) | C2B—H2B | 0.93 |
B1—N2A | 1.541 (4) | C3B—C4B | 1.473 (4) |
B1—N2C | 1.547 (4) | C4B—C5B | 1.383 (4) |
B1—N2B | 1.550 (4) | C4B—C9B | 1.396 (4) |
N1—C3 | 1.339 (4) | C5B—C6B | 1.391 (5) |
N1—N2 | 1.371 (3) | C5B—H5B | 0.93 |
N2—C1 | 1.354 (4) | C6B—C7B | 1.382 (5) |
C1—C2 | 1.358 (4) | C6B—H6B | 0.93 |
C1—H1 | 0.93 | C7B—C8B | 1.375 (6) |
C2—C3 | 1.402 (5) | C7B—H7B | 0.93 |
C2—H2 | 0.93 | C8B—C9B | 1.384 (5) |
C3—C4 | 1.472 (4) | C8B—H8B | 0.93 |
C4—C5 | 1.355 (5) | C9B—H9B | 0.93 |
C4—C9 | 1.380 (5) | N1C—C3C | 1.346 (4) |
C5—C6 | 1.387 (6) | N1C—N2C | 1.360 (3) |
C5—H5 | 0.93 | N2C—C1C | 1.350 (4) |
C6—C7 | 1.361 (7) | C1C—C2C | 1.360 (5) |
C6—H6 | 0.93 | C1C—H1C | 0.93 |
C7—C8 | 1.338 (7) | C2C—C3C | 1.398 (5) |
C7—H7 | 0.93 | C2C—H2C | 0.93 |
C8—C9 | 1.384 (5) | C3C—C4C | 1.467 (13) |
C8—H8 | 0.93 | C3C—C4D | 1.479 (9) |
C9—H9 | 0.93 | C4C—C9C | 1.348 (18) |
N1A—C3A | 1.339 (4) | C4C—C5C | 1.35 (2) |
N1A—N2A | 1.369 (3) | C5C—C6C | 1.42 (2) |
N2A—C1A | 1.344 (4) | C5C—H5C | 0.93 |
C1A—C2A | 1.367 (5) | C6C—C7C | 1.30 (2) |
C1A—H1A | 0.93 | C6C—H6C | 0.93 |
C2A—C3A | 1.395 (4) | C7C—C8C | 1.32 (2) |
C2A—H2A | 0.93 | C7C—H7C | 0.93 |
C3A—C4A | 1.473 (4) | C8C—C9C | 1.390 (16) |
C4A—C5A | 1.386 (5) | C8C—H8C | 0.93 |
C4A—C9A | 1.390 (5) | C9C—H9C | 0.93 |
C5A—C6A | 1.385 (5) | C4D—C5D | 1.378 (15) |
C5A—H5A | 0.93 | C4D—C9D | 1.438 (15) |
C6A—C7A | 1.364 (6) | C5D—C6D | 1.366 (17) |
C6A—H6A | 0.93 | C5D—H5D | 0.93 |
C7A—C8A | 1.367 (6) | C6D—C7D | 1.450 (19) |
C7A—H7A | 0.93 | C6D—H6D | 0.93 |
C8A—C9A | 1.384 (5) | C7D—C8D | 1.355 (15) |
C8A—H8A | 0.93 | C7D—H7D | 0.93 |
C9A—H9A | 0.93 | C8D—C9D | 1.374 (10) |
N1B—C3B | 1.344 (4) | C8D—H8D | 0.93 |
N1B—N2B | 1.369 (3) | C9D—H9D | 0.93 |
N2B—C1B | 1.349 (4) | | |
| | | |
N1B—Tl1—N1C | 70.82 (8) | N2B—C1B—H1B | 125.7 |
N1B—Tl1—N1A | 74.60 (7) | C2B—C1B—H1B | 125.7 |
N1C—Tl1—N1A | 80.00 (7) | C1B—C2B—C3B | 105.7 (3) |
N2—B1—N2A | 112.7 (2) | C1B—C2B—H2B | 127.1 |
N2—B1—N2C | 108.0 (2) | C3B—C2B—H2B | 127.1 |
N2A—B1—N2C | 107.2 (2) | N1B—C3B—C2B | 109.5 (3) |
N2—B1—N2B | 107.5 (2) | N1B—C3B—C4B | 121.6 (3) |
N2A—B1—N2B | 111.0 (2) | C2B—C3B—C4B | 128.9 (3) |
N2C—B1—N2B | 110.5 (2) | C5B—C4B—C9B | 118.4 (3) |
C3—N1—N2 | 105.4 (2) | C5B—C4B—C3B | 122.3 (3) |
C1—N2—N1 | 110.3 (2) | C9B—C4B—C3B | 119.3 (3) |
C1—N2—B1 | 127.1 (3) | C4B—C5B—C6B | 121.3 (3) |
N1—N2—B1 | 120.9 (2) | C4B—C5B—H5B | 119.4 |
N2—C1—C2 | 108.2 (3) | C6B—C5B—H5B | 119.4 |
N2—C1—H1 | 125.9 | C7B—C6B—C5B | 119.3 (3) |
C2—C1—H1 | 125.9 | C7B—C6B—H6B | 120.3 |
C1—C2—C3 | 105.4 (3) | C5B—C6B—H6B | 120.3 |
C1—C2—H2 | 127.3 | C8B—C7B—C6B | 120.2 (3) |
C3—C2—H2 | 127.3 | C8B—C7B—H7B | 119.9 |
N1—C3—C2 | 110.7 (3) | C6B—C7B—H7B | 119.9 |
N1—C3—C4 | 121.6 (3) | C7B—C8B—C9B | 120.4 (3) |
C2—C3—C4 | 127.7 (3) | C7B—C8B—H8B | 119.8 |
C5—C4—C9 | 117.6 (3) | C9B—C8B—H8B | 119.8 |
C5—C4—C3 | 122.1 (3) | C8B—C9B—C4B | 120.3 (3) |
C9—C4—C3 | 120.3 (3) | C8B—C9B—H9B | 119.8 |
C4—C5—C6 | 121.2 (4) | C4B—C9B—H9B | 119.8 |
C4—C5—H5 | 119.4 | C3C—N1C—N2C | 105.7 (2) |
C6—C5—H5 | 119.4 | C3C—N1C—Tl1 | 112.5 (2) |
C7—C6—C5 | 120.4 (4) | N2C—N1C—Tl1 | 105.06 (17) |
C7—C6—H6 | 119.8 | C1C—N2C—N1C | 110.2 (2) |
C5—C6—H6 | 119.8 | C1C—N2C—B1 | 127.5 (3) |
C8—C7—C6 | 119.0 (4) | N1C—N2C—B1 | 122.1 (2) |
C8—C7—H7 | 120.5 | N2C—C1C—C2C | 108.5 (3) |
C6—C7—H7 | 120.5 | N2C—C1C—H1C | 125.7 |
C7—C8—C9 | 121.1 (4) | C2C—C1C—H1C | 125.7 |
C7—C8—H8 | 119.4 | C1C—C2C—C3C | 105.2 (3) |
C9—C8—H8 | 119.4 | C1C—C2C—H2C | 127.4 |
C4—C9—C8 | 120.6 (4) | C3C—C2C—H2C | 127.4 |
C4—C9—H9 | 119.7 | N1C—C3C—C2C | 110.3 (3) |
C8—C9—H9 | 119.7 | N1C—C3C—C4C | 121.7 (8) |
C3A—N1A—N2A | 106.2 (2) | C2C—C3C—C4C | 127.9 (8) |
C3A—N1A—Tl1 | 131.04 (19) | N1C—C3C—C4D | 117.4 (6) |
N2A—N1A—Tl1 | 119.75 (17) | C2C—C3C—C4D | 131.8 (6) |
C1A—N2A—N1A | 109.8 (2) | C9C—C4C—C5C | 119.7 (16) |
C1A—N2A—B1 | 131.9 (2) | C9C—C4C—C3C | 118.0 (13) |
N1A—N2A—B1 | 118.3 (2) | C5C—C4C—C3C | 122.3 (15) |
N2A—C1A—C2A | 108.5 (3) | C4C—C5C—C6C | 119.4 (19) |
N2A—C1A—H1A | 125.7 | C4C—C5C—H5C | 120.3 |
C2A—C1A—H1A | 125.7 | C6C—C5C—H5C | 120.3 |
C1A—C2A—C3A | 105.4 (3) | C7C—C6C—C5C | 118.9 (19) |
C1A—C2A—H2A | 127.3 | C7C—C6C—H6C | 120.5 |
C3A—C2A—H2A | 127.3 | C5C—C6C—H6C | 120.5 |
N1A—C3A—C2A | 110.1 (3) | C6C—C7C—C8C | 123 (2) |
N1A—C3A—C4A | 121.1 (3) | C6C—C7C—H7C | 118.7 |
C2A—C3A—C4A | 128.8 (3) | C8C—C7C—H7C | 118.7 |
C5A—C4A—C9A | 118.3 (3) | C7C—C8C—C9C | 120.0 (13) |
C5A—C4A—C3A | 121.4 (3) | C7C—C8C—H8C | 120 |
C9A—C4A—C3A | 120.3 (3) | C9C—C8C—H8C | 120 |
C6A—C5A—C4A | 120.5 (4) | C4C—C9C—C8C | 119.2 (13) |
C6A—C5A—H5A | 119.8 | C4C—C9C—H9C | 120.4 |
C4A—C5A—H5A | 119.8 | C8C—C9C—H9C | 120.4 |
C7A—C6A—C5A | 120.7 (4) | C5D—C4D—C9D | 116.2 (10) |
C7A—C6A—H6A | 119.7 | C5D—C4D—C3C | 121.3 (12) |
C5A—C6A—H6A | 119.7 | C9D—C4D—C3C | 122.6 (10) |
C6A—C7A—C8A | 119.6 (4) | C6D—C5D—C4D | 122.3 (12) |
C6A—C7A—H7A | 120.2 | C6D—C5D—H5D | 118.8 |
C8A—C7A—H7A | 120.2 | C4D—C5D—H5D | 118.8 |
C7A—C8A—C9A | 120.7 (4) | C5D—C6D—C7D | 120.5 (14) |
C7A—C8A—H8A | 119.6 | C5D—C6D—H6D | 119.7 |
C9A—C8A—H8A | 119.6 | C7D—C6D—H6D | 119.7 |
C8A—C9A—C4A | 120.2 (4) | C8D—C7D—C6D | 117.6 (12) |
C8A—C9A—H9A | 119.9 | C8D—C7D—H7D | 121.2 |
C4A—C9A—H9A | 119.9 | C6D—C7D—H7D | 121.2 |
C3B—N1B—N2B | 106.7 (2) | C7D—C8D—C9D | 121.4 (9) |
C3B—N1B—Tl1 | 129.37 (18) | C7D—C8D—H8D | 119.3 |
N2B—N1B—Tl1 | 118.29 (17) | C9D—C8D—H8D | 119.3 |
C1B—N2B—N1B | 109.5 (2) | C8D—C9D—C4D | 121.9 (8) |
C1B—N2B—B1 | 127.5 (2) | C8D—C9D—H9D | 119.1 |
N1B—N2B—B1 | 123.0 (2) | C4D—C9D—H9D | 119.1 |
N2B—C1B—C2B | 108.6 (3) | | |
| | | |
C3—N1—N2—C1 | 0.8 (3) | N1B—N2B—C1B—C2B | 0.2 (3) |
C3—N1—N2—B1 | 167.0 (3) | B1—N2B—C1B—C2B | −176.7 (3) |
N2A—B1—N2—C1 | −140.7 (3) | N2B—C1B—C2B—C3B | 0.1 (4) |
N2C—B1—N2—C1 | −22.5 (4) | N2B—N1B—C3B—C2B | 0.5 (3) |
N2B—B1—N2—C1 | 96.7 (3) | Tl1—N1B—C3B—C2B | 152.9 (2) |
N2A—B1—N2—N1 | 55.6 (4) | N2B—N1B—C3B—C4B | −178.3 (2) |
N2C—B1—N2—N1 | 173.8 (2) | Tl1—N1B—C3B—C4B | −25.9 (4) |
N2B—B1—N2—N1 | −67.0 (3) | C1B—C2B—C3B—N1B | −0.4 (4) |
N1—N2—C1—C2 | −1.0 (4) | C1B—C2B—C3B—C4B | 178.2 (3) |
B1—N2—C1—C2 | −166.1 (3) | N1B—C3B—C4B—C5B | −18.5 (4) |
N2—C1—C2—C3 | 0.7 (4) | C2B—C3B—C4B—C5B | 163.0 (3) |
N2—N1—C3—C2 | −0.4 (3) | N1B—C3B—C4B—C9B | 160.8 (3) |
N2—N1—C3—C4 | −179.2 (3) | C2B—C3B—C4B—C9B | −17.7 (5) |
C1—C2—C3—N1 | −0.2 (4) | C9B—C4B—C5B—C6B | −1.7 (5) |
C1—C2—C3—C4 | 178.6 (3) | C3B—C4B—C5B—C6B | 177.7 (3) |
N1—C3—C4—C5 | −4.9 (5) | C4B—C5B—C6B—C7B | 2.2 (5) |
C2—C3—C4—C5 | 176.5 (4) | C5B—C6B—C7B—C8B | −0.2 (6) |
N1—C3—C4—C9 | 173.6 (3) | C6B—C7B—C8B—C9B | −2.3 (6) |
C2—C3—C4—C9 | −5.1 (5) | C7B—C8B—C9B—C4B | 2.8 (6) |
C9—C4—C5—C6 | −1.8 (7) | C5B—C4B—C9B—C8B | −0.8 (5) |
C3—C4—C5—C6 | 176.7 (4) | C3B—C4B—C9B—C8B | 179.8 (3) |
C4—C5—C6—C7 | 2.8 (9) | C3C—N1C—N2C—C1C | 1.6 (3) |
C5—C6—C7—C8 | −2.4 (8) | Tl1—N1C—N2C—C1C | −117.6 (2) |
C6—C7—C8—C9 | 1.2 (8) | C3C—N1C—N2C—B1 | 176.5 (3) |
C5—C4—C9—C8 | 0.5 (7) | Tl1—N1C—N2C—B1 | 57.3 (3) |
C3—C4—C9—C8 | −178.0 (4) | N2—B1—N2C—C1C | −53.7 (4) |
C7—C8—C9—C4 | −0.3 (8) | N2A—B1—N2C—C1C | 68.0 (4) |
C3A—N1A—N2A—C1A | −0.3 (3) | N2B—B1—N2C—C1C | −170.9 (3) |
Tl1—N1A—N2A—C1A | −162.8 (2) | N2—B1—N2C—N1C | 132.3 (3) |
C3A—N1A—N2A—B1 | −178.9 (3) | N2A—B1—N2C—N1C | −106.0 (3) |
Tl1—N1A—N2A—B1 | 18.7 (3) | N2B—B1—N2C—N1C | 15.0 (4) |
N2—B1—N2A—C1A | −13.1 (5) | N1C—N2C—C1C—C2C | −1.1 (4) |
N2C—B1—N2A—C1A | −131.8 (3) | B1—N2C—C1C—C2C | −175.7 (3) |
N2B—B1—N2A—C1A | 107.5 (4) | N2C—C1C—C2C—C3C | 0.1 (4) |
N2—B1—N2A—N1A | 165.1 (2) | N2C—N1C—C3C—C2C | −1.5 (4) |
N2C—B1—N2A—N1A | 46.4 (3) | Tl1—N1C—C3C—C2C | 112.6 (3) |
N2B—B1—N2A—N1A | −74.3 (3) | N2C—N1C—C3C—C4C | 177.0 (3) |
N1A—N2A—C1A—C2A | 0.6 (4) | Tl1—N1C—C3C—C4C | −68.9 (4) |
B1—N2A—C1A—C2A | 178.9 (3) | N2C—N1C—C3C—C4D | −174.4 (4) |
N2A—C1A—C2A—C3A | −0.6 (4) | Tl1—N1C—C3C—C4D | −60.3 (5) |
N2A—N1A—C3A—C2A | 0.0 (3) | C1C—C2C—C3C—N1C | 0.9 (4) |
Tl1—N1A—C3A—C2A | 159.6 (2) | C1C—C2C—C3C—C4C | −177.5 (4) |
N2A—N1A—C3A—C4A | 179.8 (3) | C1C—C2C—C3C—C4D | 172.4 (5) |
Tl1—N1A—C3A—C4A | −20.5 (4) | N1C—C3C—C4C—C9C | −171.7 (9) |
C1A—C2A—C3A—N1A | 0.4 (4) | C2C—C3C—C4C—C9C | 6.5 (9) |
C1A—C2A—C3A—C4A | −179.4 (3) | N1C—C3C—C4C—C5C | 6.6 (9) |
N1A—C3A—C4A—C5A | −25.4 (5) | C2C—C3C—C4C—C5C | −175.2 (9) |
C2A—C3A—C4A—C5A | 154.4 (3) | C9C—C4C—C5C—C6C | −2.9 (8) |
N1A—C3A—C4A—C9A | 155.1 (3) | C3C—C4C—C5C—C6C | 178.8 (5) |
C2A—C3A—C4A—C9A | −25.1 (5) | C4C—C5C—C6C—C7C | 1.6 (12) |
C9A—C4A—C5A—C6A | −1.7 (5) | C5C—C6C—C7C—C8C | −1.2 (17) |
C3A—C4A—C5A—C6A | 178.7 (3) | C6C—C7C—C8C—C9C | 2.2 (17) |
C4A—C5A—C6A—C7A | 0.5 (6) | C5C—C4C—C9C—C8C | 3.9 (11) |
C5A—C6A—C7A—C8A | 0.4 (7) | C3C—C4C—C9C—C8C | −177.8 (7) |
C6A—C7A—C8A—C9A | 0.1 (7) | C7C—C8C—C9C—C4C | −3.5 (15) |
C7A—C8A—C9A—C4A | −1.4 (7) | N1C—C3C—C4D—C5D | −30.9 (9) |
C5A—C4A—C9A—C8A | 2.2 (5) | C2C—C3C—C4D—C5D | 158.0 (8) |
C3A—C4A—C9A—C8A | −178.3 (4) | N1C—C3C—C4D—C9D | 147.7 (8) |
C3B—N1B—N2B—C1B | −0.4 (3) | C2C—C3C—C4D—C9D | −23.4 (9) |
Tl1—N1B—N2B—C1B | −156.38 (19) | C9D—C4D—C5D—C6D | 0.8 (12) |
C3B—N1B—N2B—B1 | 176.6 (2) | C3C—C4D—C5D—C6D | 179.5 (9) |
Tl1—N1B—N2B—B1 | 20.6 (3) | C4D—C5D—C6D—C7D | 1.2 (17) |
N2—B1—N2B—C1B | −8.1 (4) | C5D—C6D—C7D—C8D | −2.0 (19) |
N2A—B1—N2B—C1B | −131.7 (3) | C6D—C7D—C8D—C9D | 0.8 (18) |
N2C—B1—N2B—C1B | 109.5 (3) | C7D—C8D—C9D—C4D | 1.2 (17) |
N2—B1—N2B—N1B | 175.4 (2) | C5D—C4D—C9D—C8D | −2.0 (13) |
N2A—B1—N2B—N1B | 51.8 (3) | C3C—C4D—C9D—C8D | 179.3 (8) |
N2C—B1—N2B—N1B | −67.0 (3) | | |
(comp2)
catena-Poly[potassium-[µ
2-tetrakis(3-cyclopropyl-1
H-pyrazol-1-yl)borato]]
top
Crystal data top
[K(C24H28BN8)] | F(000) = 1008 |
Mr = 478.45 | Dx = 1.269 Mg m−3 |
Monoclinic, C2/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -C 2yc | Cell parameters from 5460 reflections |
a = 19.547 (8) Å | θ = 5.1–70.2° |
b = 8.391 (3) Å | µ = 2.08 mm−1 |
c = 17.153 (8) Å | T = 296 K |
β = 117.111 (12)° | Prism, colourless |
V = 2504.2 (18) Å3 | 0.19 × 0.06 × 0.06 mm |
Z = 4 | |
Data collection top
Bruker APEXII CCD diffractometer | 1361 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.085 |
Absorption correction: multi-scan (SADABS; Bruker, 2013) | θmax = 66.7°, θmin = 5.1° |
Tmin = 0.511, Tmax = 0.754 | h = −23→23 |
21173 measured reflections | k = −9→9 |
2126 independent reflections | l = −20→20 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.051 | H-atom parameters constrained |
wR(F2) = 0.135 | w = 1/[σ2(Fo2) + (0.0534P)2 + 1.8736P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
2126 reflections | Δρmax = 0.14 e Å−3 |
155 parameters | Δρmin = −0.24 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0 | 0.67908 (11) | 0.25 | 0.0794 (4) | |
B1 | 0 | 1.1765 (5) | 0.25 | 0.0448 (11) | |
N1A | 0.04126 (13) | 1.0712 (2) | 0.21159 (14) | 0.0460 (6) | |
N2A | 0.08779 (14) | 0.9490 (3) | 0.25887 (15) | 0.0562 (7) | |
C1A | 0.11582 (17) | 0.8846 (3) | 0.20838 (19) | 0.0524 (7) | |
C2A | 0.0885 (2) | 0.9637 (4) | 0.1296 (2) | 0.0726 (10) | |
H2A | 0.0994 | 0.9421 | 0.0833 | 0.087* | |
C3A | 0.0420 (2) | 1.0805 (4) | 0.1341 (2) | 0.0659 (9) | |
H3A | 0.0152 | 1.1547 | 0.0904 | 0.079* | |
C4A | 0.16749 (19) | 0.7446 (4) | 0.2416 (2) | 0.0720 (10) | |
H4A | 0.1909 | 0.7297 | 0.3052 | 0.086* | |
C5A | 0.1484 (3) | 0.5948 (5) | 0.1900 (3) | 0.1159 (16) | |
H5A1 | 0.1581 | 0.4948 | 0.2217 | 0.139* | |
H5A2 | 0.1036 | 0.5949 | 0.133 | 0.139* | |
C6A | 0.2141 (3) | 0.6889 (5) | 0.2005 (3) | 0.0999 (14) | |
H6A1 | 0.2104 | 0.7471 | 0.1499 | 0.12* | |
H6A2 | 0.2648 | 0.6471 | 0.2384 | 0.12* | |
N1B | 0.05869 (13) | 1.2815 (2) | 0.32347 (15) | 0.0483 (6) | |
N2B | 0.03531 (14) | 1.4085 (3) | 0.35488 (17) | 0.0591 (7) | |
C1B | 0.09807 (17) | 1.4670 (3) | 0.42155 (19) | 0.0550 (8) | |
C2B | 0.1610 (2) | 1.3764 (4) | 0.4340 (2) | 0.0880 (12) | |
H2B | 0.2116 | 1.3909 | 0.4763 | 0.106* | |
C3B | 0.13353 (19) | 1.2608 (4) | 0.3712 (2) | 0.0760 (10) | |
H3B | 0.1626 | 1.1806 | 0.3634 | 0.091* | |
C4B | 0.0927 (2) | 1.6112 (4) | 0.4678 (2) | 0.0705 (9) | |
H4B | 0.0428 | 1.6275 | 0.4672 | 0.085* | |
C5B | 0.1331 (3) | 1.7605 (4) | 0.4646 (2) | 0.0961 (13) | |
H5B1 | 0.1646 | 1.7567 | 0.4343 | 0.115* | |
H5B2 | 0.1071 | 1.8612 | 0.46 | 0.115* | |
C6B | 0.1593 (2) | 1.6707 (4) | 0.5465 (2) | 0.0797 (11) | |
H6B1 | 0.2072 | 1.6122 | 0.5669 | 0.096* | |
H6B2 | 0.1498 | 1.7165 | 0.5926 | 0.096* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0980 (9) | 0.0358 (5) | 0.0960 (9) | 0 | 0.0369 (7) | 0 |
B1 | 0.057 (3) | 0.028 (2) | 0.050 (3) | 0 | 0.025 (3) | 0 |
N1A | 0.0590 (15) | 0.0361 (11) | 0.0439 (14) | 0.0011 (10) | 0.0242 (12) | 0.0038 (10) |
N2A | 0.0783 (18) | 0.0400 (12) | 0.0561 (15) | 0.0138 (12) | 0.0356 (15) | 0.0043 (11) |
C1A | 0.065 (2) | 0.0430 (15) | 0.0561 (19) | 0.0003 (14) | 0.0332 (17) | −0.0075 (13) |
C2A | 0.094 (3) | 0.078 (2) | 0.062 (2) | 0.017 (2) | 0.050 (2) | 0.0041 (18) |
C3A | 0.085 (2) | 0.0629 (19) | 0.055 (2) | 0.0120 (17) | 0.0368 (19) | 0.0129 (16) |
C4A | 0.085 (3) | 0.067 (2) | 0.066 (2) | 0.0195 (18) | 0.036 (2) | −0.0072 (17) |
C5A | 0.110 (4) | 0.072 (3) | 0.155 (4) | 0.015 (2) | 0.052 (3) | −0.037 (3) |
C6A | 0.092 (3) | 0.117 (3) | 0.102 (3) | 0.040 (3) | 0.054 (3) | 0.003 (3) |
N1B | 0.0518 (15) | 0.0348 (11) | 0.0536 (15) | 0.0048 (10) | 0.0200 (13) | −0.0021 (10) |
N2B | 0.0593 (16) | 0.0399 (13) | 0.0692 (18) | 0.0039 (11) | 0.0217 (15) | −0.0135 (12) |
C1B | 0.061 (2) | 0.0445 (15) | 0.0487 (19) | 0.0011 (14) | 0.0156 (17) | −0.0063 (13) |
C2B | 0.058 (2) | 0.082 (2) | 0.091 (3) | 0.0097 (18) | 0.005 (2) | −0.038 (2) |
C3B | 0.053 (2) | 0.074 (2) | 0.085 (3) | 0.0126 (17) | 0.018 (2) | −0.026 (2) |
C4B | 0.077 (2) | 0.0542 (18) | 0.076 (2) | −0.0027 (17) | 0.031 (2) | −0.0197 (17) |
C5B | 0.154 (4) | 0.051 (2) | 0.079 (3) | −0.017 (2) | 0.049 (3) | −0.0122 (19) |
C6B | 0.099 (3) | 0.065 (2) | 0.064 (2) | −0.0076 (19) | 0.027 (2) | −0.0193 (18) |
Geometric parameters (Å, º) top
K1—N2Bi | 2.781 (3) | C4A—H4A | 0.98 |
K1—N2Bii | 2.781 (3) | C5A—C6A | 1.448 (5) |
K1—N2A | 2.804 (3) | C5A—H5A1 | 0.97 |
K1—N2Aiii | 2.804 (3) | C5A—H5A2 | 0.97 |
K1—C1A | 3.175 (3) | C6A—H6A1 | 0.97 |
K1—C1Aiii | 3.175 (3) | C6A—H6A2 | 0.97 |
K1—C1Bi | 3.218 (3) | N1B—C3B | 1.322 (4) |
K1—C1Bii | 3.218 (3) | N1B—N2B | 1.364 (3) |
K1—C4Bi | 3.375 (4) | N2B—C1B | 1.332 (3) |
K1—C4Bii | 3.375 (4) | N2B—K1iv | 2.781 (3) |
K1—C4Aiii | 3.387 (4) | C1B—C2B | 1.378 (4) |
K1—C4A | 3.387 (4) | C1B—C4B | 1.476 (4) |
B1—N1Aiii | 1.533 (3) | C1B—K1iv | 3.218 (3) |
B1—N1A | 1.533 (3) | C2B—C3B | 1.364 (4) |
B1—N1B | 1.537 (3) | C2B—H2B | 0.93 |
B1—N1Biii | 1.537 (3) | C3B—H3B | 0.93 |
N1A—C3A | 1.339 (3) | C4B—C6B | 1.472 (5) |
N1A—N2A | 1.365 (3) | C4B—C5B | 1.495 (5) |
N2A—C1A | 1.332 (3) | C4B—K1iv | 3.375 (4) |
C1A—C2A | 1.376 (4) | C4B—H4B | 0.98 |
C1A—C4A | 1.484 (4) | C5B—C6B | 1.466 (5) |
C2A—C3A | 1.362 (4) | C5B—K1iv | 3.472 (4) |
C2A—H2A | 0.93 | C5B—H5B1 | 0.97 |
C3A—H3A | 0.93 | C5B—H5B2 | 0.97 |
C4A—C6A | 1.459 (4) | C6B—H6B1 | 0.97 |
C4A—C5A | 1.484 (5) | C6B—H6B2 | 0.97 |
| | | |
N2Bi—K1—N2Bii | 70.57 (10) | N2A—C1A—C2A | 110.6 (3) |
N2Bi—K1—N2A | 131.29 (7) | N2A—C1A—C4A | 118.8 (3) |
N2Bii—K1—N2A | 131.23 (7) | C2A—C1A—C4A | 130.6 (3) |
N2Bi—K1—N2Aiii | 131.23 (7) | N2A—C1A—K1 | 61.81 (15) |
N2Bii—K1—N2Aiii | 131.29 (7) | C2A—C1A—K1 | 119.0 (2) |
N2A—K1—N2Aiii | 72.22 (10) | C4A—C1A—K1 | 85.06 (19) |
N2Bi—K1—C1A | 106.87 (7) | C3A—C2A—C1A | 105.2 (3) |
N2Bii—K1—C1A | 126.63 (8) | C3A—C2A—H2A | 127.4 |
N2A—K1—C1A | 24.76 (6) | C1A—C2A—H2A | 127.4 |
N2Aiii—K1—C1A | 91.74 (8) | N1A—C3A—C2A | 108.8 (3) |
N2Bi—K1—C1Aiii | 126.63 (8) | N1A—C3A—H3A | 125.6 |
N2Bii—K1—C1Aiii | 106.87 (7) | C2A—C3A—H3A | 125.6 |
N2A—K1—C1Aiii | 91.74 (8) | C6A—C4A—C1A | 122.3 (3) |
N2Aiii—K1—C1Aiii | 24.76 (6) | C6A—C4A—C5A | 58.9 (2) |
C1A—K1—C1Aiii | 114.20 (10) | C1A—C4A—C5A | 120.0 (3) |
N2Bi—K1—C1Bi | 24.28 (7) | C6A—C4A—K1 | 142.8 (3) |
N2Bii—K1—C1Bi | 90.51 (8) | C1A—C4A—K1 | 69.06 (17) |
N2A—K1—C1Bi | 126.23 (7) | C5A—C4A—K1 | 84.4 (2) |
N2Aiii—K1—C1Bi | 107.59 (7) | C6A—C4A—H4A | 114.8 |
C1A—K1—C1Bi | 106.46 (8) | C1A—C4A—H4A | 114.8 |
C1Aiii—K1—C1Bi | 108.50 (8) | C5A—C4A—H4A | 114.8 |
N2Bi—K1—C1Bii | 90.51 (8) | K1—C4A—H4A | 84.4 |
N2Bii—K1—C1Bii | 24.28 (7) | C6A—C5A—C4A | 59.7 (3) |
N2A—K1—C1Bii | 107.59 (7) | C6A—C5A—H5A1 | 117.8 |
N2Aiii—K1—C1Bii | 126.24 (7) | C4A—C5A—H5A1 | 117.8 |
C1A—K1—C1Bii | 108.50 (8) | C6A—C5A—H5A2 | 117.8 |
C1Aiii—K1—C1Bii | 106.46 (8) | C4A—C5A—H5A2 | 117.8 |
C1Bi—K1—C1Bii | 112.87 (10) | H5A1—C5A—H5A2 | 114.9 |
N2Bi—K1—C4Bi | 45.30 (7) | C5A—C6A—C4A | 61.4 (3) |
N2Bii—K1—C4Bi | 115.34 (8) | C5A—C6A—H6A1 | 117.6 |
N2A—K1—C4Bi | 101.71 (7) | C4A—C6A—H6A1 | 117.6 |
N2Aiii—K1—C4Bi | 93.99 (7) | C5A—C6A—H6A2 | 117.6 |
C1A—K1—C4Bi | 85.47 (8) | C4A—C6A—H6A2 | 117.6 |
C1Aiii—K1—C4Bi | 105.21 (8) | H6A1—C6A—H6A2 | 114.7 |
C1Bi—K1—C4Bi | 25.74 (7) | C3B—N1B—N2B | 109.5 (2) |
C1Bii—K1—C4Bi | 135.58 (8) | C3B—N1B—B1 | 129.4 (2) |
N2Bi—K1—C4Bii | 115.34 (8) | N2B—N1B—B1 | 120.8 (2) |
N2Bii—K1—C4Bii | 45.30 (7) | C1B—N2B—N1B | 106.5 (2) |
N2A—K1—C4Bii | 93.99 (7) | C1B—N2B—K1iv | 96.58 (17) |
N2Aiii—K1—C4Bii | 101.71 (7) | N1B—N2B—K1iv | 114.31 (17) |
C1A—K1—C4Bii | 105.20 (8) | N2B—C1B—C2B | 109.7 (3) |
C1Aiii—K1—C4Bii | 85.47 (8) | N2B—C1B—C4B | 120.0 (3) |
C1Bi—K1—C4Bii | 135.58 (8) | C2B—C1B—C4B | 130.3 (3) |
C1Bii—K1—C4Bii | 25.74 (7) | N2B—C1B—K1iv | 59.14 (15) |
C4Bi—K1—C4Bii | 160.58 (11) | C2B—C1B—K1iv | 124.4 (2) |
N2Bi—K1—C4Aiii | 101.56 (8) | C4B—C1B—K1iv | 83.07 (18) |
N2Bii—K1—C4Aiii | 93.71 (8) | C3B—C2B—C1B | 105.5 (3) |
N2A—K1—C4Aiii | 116.50 (8) | C3B—C2B—H2B | 127.2 |
N2Aiii—K1—C4Aiii | 44.89 (7) | C1B—C2B—H2B | 127.2 |
C1A—K1—C4Aiii | 136.34 (8) | N1B—C3B—C2B | 108.8 (3) |
C1Aiii—K1—C4Aiii | 25.87 (7) | N1B—C3B—H3B | 125.6 |
C1Bi—K1—C4Aiii | 86.80 (8) | C2B—C3B—H3B | 125.6 |
C1Bii—K1—C4Aiii | 103.61 (8) | C1B—C4B—C6B | 121.4 (3) |
C4Bi—K1—C4Aiii | 91.88 (9) | C1B—C4B—C5B | 120.0 (3) |
C4Bii—K1—C4Aiii | 91.26 (9) | C6B—C4B—C5B | 59.2 (2) |
N2Bi—K1—C4A | 93.71 (8) | C1B—C4B—K1iv | 71.19 (17) |
N2Bii—K1—C4A | 101.56 (8) | C6B—C4B—K1iv | 139.7 (2) |
N2A—K1—C4A | 44.89 (7) | C5B—C4B—K1iv | 81.1 (2) |
N2Aiii—K1—C4A | 116.50 (8) | C1B—C4B—H4B | 115 |
C1A—K1—C4A | 25.87 (7) | C6B—C4B—H4B | 115 |
C1Aiii—K1—C4A | 136.34 (8) | C5B—C4B—H4B | 115 |
C1Bi—K1—C4A | 103.61 (8) | K1iv—C4B—H4B | 86.3 |
C1Bii—K1—C4A | 86.80 (8) | C6B—C5B—C4B | 59.6 (2) |
C4Bi—K1—C4A | 91.26 (9) | C6B—C5B—K1iv | 132.9 (2) |
C4Bii—K1—C4A | 91.88 (9) | C4B—C5B—K1iv | 73.8 (2) |
C4Aiii—K1—C4A | 161.32 (11) | C6B—C5B—H5B1 | 117.8 |
N1Aiii—B1—N1A | 109.6 (3) | C4B—C5B—H5B1 | 117.8 |
N1Aiii—B1—N1B | 108.68 (12) | K1iv—C5B—H5B1 | 77.2 |
N1A—B1—N1B | 109.90 (12) | C6B—C5B—H5B2 | 117.8 |
N1Aiii—B1—N1Biii | 109.90 (12) | C4B—C5B—H5B2 | 117.8 |
N1A—B1—N1Biii | 108.68 (12) | K1iv—C5B—H5B2 | 88.5 |
N1B—B1—N1Biii | 110.1 (3) | H5B1—C5B—H5B2 | 114.9 |
C3A—N1A—N2A | 109.1 (2) | C4B—C6B—C5B | 61.2 (2) |
C3A—N1A—B1 | 129.7 (2) | C4B—C6B—H6B1 | 117.6 |
N2A—N1A—B1 | 121.08 (19) | C5B—C6B—H6B1 | 117.6 |
C1A—N2A—N1A | 106.2 (2) | C4B—C6B—H6B2 | 117.6 |
C1A—N2A—K1 | 93.43 (16) | C5B—C6B—H6B2 | 117.6 |
N1A—N2A—K1 | 110.42 (16) | H6B1—C6B—H6B2 | 114.8 |
| | | |
N1Aiii—B1—N1A—C3A | 132.8 (3) | N1Biii—B1—N1B—C3B | −141.4 (3) |
N1B—B1—N1A—C3A | −107.8 (3) | N1Aiii—B1—N1B—N2B | −74.3 (3) |
N1Biii—B1—N1A—C3A | 12.7 (4) | N1A—B1—N1B—N2B | 165.8 (2) |
N1Aiii—B1—N1A—N2A | −49.62 (18) | N1Biii—B1—N1B—N2B | 46.10 (18) |
N1B—B1—N1A—N2A | 69.7 (3) | C3B—N1B—N2B—C1B | 1.5 (3) |
N1Biii—B1—N1A—N2A | −169.7 (2) | B1—N1B—N2B—C1B | 175.4 (2) |
C3A—N1A—N2A—C1A | −0.5 (3) | C3B—N1B—N2B—K1iv | 106.9 (2) |
B1—N1A—N2A—C1A | −178.5 (2) | B1—N1B—N2B—K1iv | −79.2 (2) |
C3A—N1A—N2A—K1 | −100.6 (2) | N1B—N2B—C1B—C2B | −1.2 (4) |
B1—N1A—N2A—K1 | 81.4 (2) | K1iv—N2B—C1B—C2B | −119.0 (3) |
N1A—N2A—C1A—C2A | 0.3 (3) | N1B—N2B—C1B—C4B | 177.3 (3) |
K1—N2A—C1A—C2A | 112.8 (2) | K1iv—N2B—C1B—C4B | 59.5 (3) |
N1A—N2A—C1A—C4A | −178.5 (3) | N1B—N2B—C1B—K1iv | 117.8 (2) |
K1—N2A—C1A—C4A | −66.1 (3) | N2B—C1B—C2B—C3B | 0.4 (4) |
N1A—N2A—C1A—K1 | −112.4 (2) | C4B—C1B—C2B—C3B | −177.8 (3) |
N2A—C1A—C2A—C3A | 0.0 (4) | K1iv—C1B—C2B—C3B | −65.1 (4) |
C4A—C1A—C2A—C3A | 178.6 (3) | N2B—N1B—C3B—C2B | −1.3 (4) |
K1—C1A—C2A—C3A | 68.4 (3) | B1—N1B—C3B—C2B | −174.5 (3) |
N2A—N1A—C3A—C2A | 0.5 (4) | C1B—C2B—C3B—N1B | 0.5 (4) |
B1—N1A—C3A—C2A | 178.3 (3) | N2B—C1B—C4B—C6B | 174.4 (3) |
C1A—C2A—C3A—N1A | −0.3 (4) | C2B—C1B—C4B—C6B | −7.5 (6) |
N2A—C1A—C4A—C6A | −165.9 (3) | K1iv—C1B—C4B—C6B | −137.4 (3) |
C2A—C1A—C4A—C6A | 15.5 (6) | N2B—C1B—C4B—C5B | −115.5 (4) |
K1—C1A—C4A—C6A | 140.1 (3) | C2B—C1B—C4B—C5B | 62.6 (5) |
N2A—C1A—C4A—C5A | 124.0 (4) | K1iv—C1B—C4B—C5B | −67.3 (3) |
C2A—C1A—C4A—C5A | −54.6 (5) | N2B—C1B—C4B—K1iv | −48.2 (2) |
K1—C1A—C4A—C5A | 70.0 (3) | C2B—C1B—C4B—K1iv | 129.9 (4) |
N2A—C1A—C4A—K1 | 54.0 (2) | C1B—C4B—C5B—C6B | −110.9 (4) |
C2A—C1A—C4A—K1 | −124.6 (4) | K1iv—C4B—C5B—C6B | −173.0 (2) |
C1A—C4A—C5A—C6A | 111.8 (4) | C1B—C4B—C5B—K1iv | 62.1 (3) |
K1—C4A—C5A—C6A | 173.7 (3) | C6B—C4B—C5B—K1iv | 173.0 (2) |
C1A—C4A—C6A—C5A | −108.0 (4) | C1B—C4B—C6B—C5B | 108.5 (4) |
K1—C4A—C6A—C5A | −10.4 (5) | K1iv—C4B—C6B—C5B | 10.7 (4) |
N1Aiii—B1—N1B—C3B | 98.2 (3) | K1iv—C5B—C6B—C4B | −9.1 (3) |
N1A—B1—N1B—C3B | −21.7 (4) | | |
Symmetry codes: (i) −x, y−1, −z+1/2; (ii) x, y−1, z; (iii) −x, y, −z+1/2; (iv) x, y+1, z. |
Frequency of the 11 motifs found in the CSD for tetrakis scorpionate
derivatives (title compounds have also been included) topMotif | A | B | C | D | E | F | G | H | I | J | K |
No. of structures | 2 | 3 | 37 | 73 | 14 | 2 | 7 | 19 | 5 | 2 | 2 |
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