metal-organic compounds
Caesium tetramethylammonium dodecahydrido-closo-dodecaborate monohydrate
aInstitut für Anorganische Chemie, Universität Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart, Germany
*Correspondence e-mail: schleid@iac.uni-stuttgart.de
In the +·[N(CH3)4]+·[B12H12]2−·H2O, the contains one caesium and one tetramethylammonium cation, one dodecahydrido-closo-dodecaborate anion and one water molecule. The Cs+ cation is coordinated tetrahedrally by four [B12H12]2− clusters, with the water molecule completing the coordination sphere. The tetramethylammonium cation is surrounded distorted octahedrally by six [B12H12]2− anions. The is stabilized by a three-dimensional network of O—H⋯H—B and C—H⋯H—B dihydrogen bonds.
of the hydrated double salt, CsKeywords: crystal structure; caesium salt; tetramethylammonium salt; dodecahydrido-closo-dodecaborate; hydrate.
CCDC reference: 1454125
Structure description
The crystal structures of dodecahydrido-closo-dodecaborates with heavier alkali metals M2[B12H12] (M = K, Rb, Cs) have been elucidated by single-crystal X-ray data [for the dicaesium salt, see: Tiritiris et al. (2000); for the dirubidium and dipotassium salts, see: Tiritiris & Schleid (2003)]. The crystal structures of the solvent-free and the acetonitrile-solvated bis(tetramethylammonium) salts have been also reported (Hofmann & Albert, 2001). In contrast, data for cationic mixed compounds with closo-borate anions are scarce. Until now, only two examples, namely Cs[Na(NH3)6][B10H10]·NH3 (Kraus & Albert, 2005) and the rare-earth-metal-containing compound [La(H2O)9](H3O)Cl2[B12H12]·H2O (Tiritiris & Schleid, 2008), have been published. The title compound is the second in our series to have been structurally characterized (Fig. 1). The B—B bond lengths and the B—B—B angles are in typical ranges for a [B12H12]2− anion [1.771 (5)–1.795 (5) Å and 59.6 (2)–60.5 (2)°] and comparable with those of Cs2[B12H12] (Tiritiris et al., 2000). Two anions are coordinating via triangular faces and another two via edges of H atoms to the caesium cation [Cs—H = 2.99 (4)–3.55 (3) Å]. The water molecule completes the coordination sphere of caesium, yielding a of 11 (Fig. 2). Every dodecahydrido-closo-dodecaborate anion is surrounded by four caesium and four tetramethylammonium cations, forming a slightly distorted cube.
The 12H12]2− anions (Fig. 3 and Table 1). O—H⋯H—B dihydrogen-bonding interactions between the cluster anions and the water molecules were also observed in the of (NH4)2[B10H10]·1.5H2O (Yisgedu et al., 2010), there ranging from 2.12 (3) to 2.23 (3) Å. Taking additional C—H⋯H—B dihydrogen-bonding interactions between the anions and the tetramethylammonium cations into account, a three-dimensional network structure results (Fig. 4 and Table 1).
is mainly stabilized by O—H⋯H—B dihydrogen bonds between the water molecules and the [BSynthesis and crystallization
The title compound was obtained by reaction of dicaesium dodecahydrido-closo-dodecaborate (Tiritiris et al., 2000) with one equivalent of tetramethylammonium chloride in water. The crude product was recrystallized from an aqueous solution. After slow evaporation of the solvent at ambient temperature, colorless single crystals suitable for X-ray analysis emerged.
Refinement
Crystal data, data collection and structure . The residual electron-density peak of 1.585 e Å−3 is located 0.80 Å from the Cs atom.
details are summarized in Table 2
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Structural data
CCDC reference: 1454125
https://doi.org/10.1107/S2414314616002911/wm4007sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314616002911/wm4007Isup2.hkl
Data collection: COLLECT (Hooft, 2004); cell
DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).Cs+·C4H12N+·B12H122−·H2O | Dx = 1.450 Mg m−3 |
Mr = 366.89 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 3552 reflections |
a = 8.9771 (5) Å | θ = 2.1–30.0° |
b = 12.8680 (8) Å | µ = 2.18 mm−1 |
c = 14.5449 (9) Å | T = 173 K |
V = 1680.19 (17) Å3 | Needle, colorless |
Z = 4 | 0.55 × 0.15 × 0.10 mm |
F(000) = 720 |
Bruker–Nonius KappaCCD diffractometer | 3279 independent reflections |
Radiation source: fine-focus sealed tube | 3143 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ scans, and ω scans | θmax = 30.0°, θmin = 2.1° |
Absorption correction: multi-scan (Blessing, 1995) | h = −12→12 |
Tmin = 0.70, Tmax = 0.80 | k = −18→18 |
3552 measured reflections | l = −20→20 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.024 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.063 | w = 1/[σ2(Fo2) + (0.0426P)2 + 0.3622P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
3279 reflections | Δρmax = 1.59 e Å−3 |
231 parameters | Δρmin = −0.76 e Å−3 |
3 restraints | Absolute structure: Classical Flack method preferred over Parsons because s.u. lower |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (2) |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Cs | 0.46732 (2) | −0.05439 (2) | 0.08106 (2) | 0.02735 (7) | |
N | 0.0367 (4) | 0.24156 (19) | 0.20442 (17) | 0.0211 (4) | |
C1 | 0.1556 (4) | 0.2290 (3) | 0.1332 (2) | 0.0294 (7) | |
H1A | 0.1203 | 0.1821 | 0.0848 | 0.044* | |
H1B | 0.2451 | 0.1998 | 0.1617 | 0.044* | |
H1C | 0.1792 | 0.2969 | 0.1064 | 0.044* | |
C2 | 0.0955 (5) | 0.3074 (3) | 0.2815 (2) | 0.0311 (7) | |
H2A | 0.1245 | 0.3757 | 0.2575 | 0.047* | |
H2B | 0.1824 | 0.2735 | 0.3090 | 0.047* | |
H2C | 0.0179 | 0.3162 | 0.3282 | 0.047* | |
C3 | −0.0051 (4) | 0.1366 (3) | 0.2403 (3) | 0.0321 (7) | |
H3A | 0.0835 | 0.1023 | 0.2655 | 0.048* | |
H3B | −0.0460 | 0.0945 | 0.1902 | 0.048* | |
H3C | −0.0800 | 0.1442 | 0.2889 | 0.048* | |
C4 | −0.0966 (5) | 0.2926 (3) | 0.1634 (3) | 0.0366 (8) | |
H4A | −0.1771 | 0.2946 | 0.2088 | 0.055* | |
H4B | −0.1293 | 0.2531 | 0.1094 | 0.055* | |
H4C | −0.0710 | 0.3636 | 0.1448 | 0.055* | |
B1 | 0.3945 (4) | −0.0349 (2) | 0.4200 (3) | 0.0221 (6) | |
H1 | 0.319 (6) | −0.088 (4) | 0.424 (3) | 0.046 (14)* | |
B2 | 0.5537 (4) | −0.0493 (3) | 0.3474 (2) | 0.0212 (6) | |
H2 | 0.576 (5) | −0.116 (3) | 0.307 (2) | 0.014 (9)* | |
B3 | 0.5763 (4) | −0.0442 (3) | 0.4691 (2) | 0.0194 (6) | |
H3 | 0.612 (6) | −0.116 (3) | 0.508 (3) | 0.027 (11)* | |
B4 | 0.3427 (4) | 0.0984 (3) | 0.4197 (2) | 0.0196 (5) | |
H4 | 0.223 (5) | 0.121 (3) | 0.427 (3) | 0.026 (11)* | |
B5 | 0.4688 (5) | 0.1664 (3) | 0.3468 (2) | 0.0216 (6) | |
H5 | 0.432 (6) | 0.230 (4) | 0.306 (3) | 0.031 (12)* | |
B6 | 0.4908 (4) | 0.1712 (2) | 0.4688 (2) | 0.0193 (6) | |
H6 | 0.469 (5) | 0.243 (3) | 0.511 (3) | 0.017 (8)* | |
B7 | 0.5994 (4) | 0.0747 (3) | 0.3028 (2) | 0.0204 (6) | |
H7 | 0.657 (4) | 0.084 (3) | 0.237 (2) | 0.007 (7)* | |
B8 | 0.7029 (4) | 0.0239 (3) | 0.3968 (2) | 0.0195 (6) | |
H8 | 0.823 (5) | 0.002 (3) | 0.390 (3) | 0.019 (9)* | |
B9 | 0.6352 (4) | 0.0829 (3) | 0.4998 (2) | 0.0174 (6) | |
H9 | 0.710 (5) | 0.102 (3) | 0.559 (3) | 0.022 (10)* | |
B10 | 0.4091 (4) | 0.0385 (3) | 0.3175 (2) | 0.0217 (6) | |
H10 | 0.341 (4) | 0.019 (3) | 0.260 (3) | 0.016 (9)* | |
B11 | 0.6495 (4) | 0.1574 (3) | 0.3959 (2) | 0.0194 (6) | |
H11 | 0.736 (5) | 0.219 (3) | 0.382 (3) | 0.023 (10)* | |
B12 | 0.4455 (4) | 0.0463 (3) | 0.5141 (2) | 0.0176 (5) | |
H12 | 0.386 (5) | 0.037 (3) | 0.588 (3) | 0.028 (10)* | |
O | 0.5166 (5) | 0.1878 (2) | 0.0878 (2) | 0.0446 (8) | |
H13 | 0.521 (7) | 0.2572 (11) | 0.077 (3) | 0.050* | |
H14 | 0.536 (8) | 0.186 (3) | 0.1489 (12) | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs | 0.02633 (10) | 0.02544 (9) | 0.03026 (10) | 0.00137 (8) | −0.00146 (9) | −0.00831 (7) |
N | 0.0214 (11) | 0.0215 (10) | 0.0204 (9) | 0.0031 (11) | −0.0029 (12) | −0.0024 (9) |
C1 | 0.0323 (16) | 0.0317 (15) | 0.0242 (14) | −0.0050 (15) | 0.0087 (13) | −0.0039 (13) |
C2 | 0.0313 (17) | 0.0370 (17) | 0.0250 (15) | 0.0055 (16) | −0.0081 (14) | −0.0105 (12) |
C3 | 0.0290 (17) | 0.0291 (14) | 0.0383 (16) | −0.0020 (12) | 0.0050 (14) | 0.0048 (14) |
C4 | 0.0323 (18) | 0.0396 (19) | 0.0380 (19) | 0.0146 (17) | −0.0126 (17) | −0.0078 (15) |
B1 | 0.0217 (13) | 0.0206 (13) | 0.0239 (13) | −0.0072 (11) | −0.0002 (15) | 0.0005 (13) |
B2 | 0.0222 (15) | 0.0185 (12) | 0.0230 (13) | −0.0011 (14) | −0.0019 (12) | −0.0028 (11) |
B3 | 0.0193 (13) | 0.0167 (12) | 0.0223 (13) | 0.0014 (11) | −0.0026 (11) | 0.0017 (11) |
B4 | 0.0164 (12) | 0.0252 (13) | 0.0172 (12) | 0.0035 (11) | 0.0015 (13) | 0.0025 (13) |
B5 | 0.0221 (14) | 0.0233 (13) | 0.0193 (12) | 0.0015 (16) | 0.0020 (15) | 0.0044 (11) |
B6 | 0.0219 (16) | 0.0166 (12) | 0.0195 (12) | 0.0017 (12) | 0.0021 (11) | 0.0007 (10) |
B7 | 0.0201 (14) | 0.0250 (15) | 0.0159 (12) | 0.0009 (13) | 0.0027 (12) | −0.0018 (11) |
B8 | 0.0178 (13) | 0.0214 (13) | 0.0193 (13) | 0.0002 (11) | −0.0003 (11) | −0.0016 (11) |
B9 | 0.0170 (13) | 0.0189 (12) | 0.0163 (12) | −0.0011 (11) | −0.0010 (11) | −0.0022 (11) |
B10 | 0.0194 (14) | 0.0281 (16) | 0.0176 (12) | −0.0011 (14) | −0.0015 (12) | −0.0013 (12) |
B11 | 0.0217 (14) | 0.0166 (12) | 0.0201 (13) | −0.0008 (12) | 0.0035 (12) | 0.0001 (11) |
B12 | 0.0171 (13) | 0.0174 (12) | 0.0185 (11) | 0.0020 (12) | −0.0010 (10) | 0.0035 (11) |
O | 0.062 (2) | 0.0283 (11) | 0.0440 (14) | 0.0055 (14) | 0.0030 (19) | 0.0019 (12) |
Cs—O | 3.149 (3) | B3—B9 | 1.776 (5) |
Cs—B6i | 3.624 (3) | B3—B12 | 1.778 (5) |
Cs—B10 | 3.678 (3) | B3—B8 | 1.780 (5) |
Cs—B4ii | 3.684 (3) | B3—H3 | 1.13 (4) |
Cs—B9iii | 3.777 (3) | B4—B6 | 1.776 (5) |
Cs—B5i | 3.786 (3) | B4—B10 | 1.778 (5) |
Cs—B7 | 3.816 (3) | B4—B5 | 1.782 (5) |
Cs—B12ii | 3.833 (3) | B4—B12 | 1.785 (5) |
Cs—B11i | 3.868 (3) | B4—Csiv | 3.684 (3) |
Cs—B2 | 3.951 (3) | B4—H4 | 1.12 (5) |
Cs—H7 | 3.35 (3) | B5—B11 | 1.776 (6) |
Cs—H10 | 2.99 (4) | B5—B7 | 1.783 (5) |
Cs—H14 | 3.30 (4) | B5—B10 | 1.783 (5) |
N—C4 | 1.490 (5) | B5—B6 | 1.786 (5) |
N—C3 | 1.496 (4) | B5—Csv | 3.786 (3) |
N—C1 | 1.496 (4) | B5—H5 | 1.06 (5) |
N—C2 | 1.501 (4) | B6—B9 | 1.782 (5) |
C1—H1A | 0.9800 | B6—B11 | 1.785 (5) |
C1—H1B | 0.9800 | B6—B12 | 1.785 (5) |
C1—H1C | 0.9800 | B6—Csv | 3.624 (3) |
C2—H2A | 0.9800 | B6—H6 | 1.12 (4) |
C2—H2B | 0.9800 | B7—B8 | 1.778 (5) |
C2—H2C | 0.9800 | B7—B11 | 1.780 (5) |
C3—H3A | 0.9800 | B7—B10 | 1.784 (6) |
C3—H3B | 0.9800 | B7—H7 | 1.09 (3) |
C3—H3C | 0.9800 | B8—B11 | 1.784 (5) |
C4—H4A | 0.9800 | B8—B9 | 1.786 (5) |
C4—H4B | 0.9800 | B8—H8 | 1.11 (4) |
C4—H4C | 0.9800 | B9—B12 | 1.779 (5) |
B1—B10 | 1.771 (5) | B9—B11 | 1.795 (5) |
B1—B4 | 1.778 (5) | B9—Csvi | 3.777 (3) |
B1—B12 | 1.781 (5) | B9—H9 | 1.12 (4) |
B1—B3 | 1.785 (5) | B10—H10 | 1.07 (4) |
B1—B2 | 1.787 (5) | B11—Csv | 3.868 (3) |
B1—H1 | 0.97 (5) | B11—H11 | 1.13 (4) |
B2—B7 | 1.771 (5) | B12—Csiv | 3.833 (3) |
B2—B10 | 1.775 (5) | B12—H12 | 1.21 (4) |
B2—B3 | 1.784 (5) | O—H13 | 0.908 (11) |
B2—B8 | 1.789 (5) | O—H14 | 0.906 (11) |
B2—H2 | 1.05 (4) | ||
O—Cs—B6i | 162.90 (9) | B1—B4—Csiv | 92.75 (17) |
O—Cs—B10 | 70.69 (8) | B5—B4—Csiv | 159.22 (19) |
B6i—Cs—B10 | 121.23 (8) | B12—B4—Csiv | 80.98 (15) |
O—Cs—B4ii | 106.14 (9) | B6—B4—H4 | 123 (2) |
B6i—Cs—B4ii | 78.53 (7) | B10—B4—H4 | 121 (2) |
B10—Cs—B4ii | 122.55 (8) | B1—B4—H4 | 120 (2) |
O—Cs—B9iii | 88.46 (9) | B5—B4—H4 | 123 (2) |
B6i—Cs—B9iii | 75.21 (7) | B12—B4—H4 | 121 (2) |
B10—Cs—B9iii | 117.29 (8) | B11—B5—B4 | 108.0 (2) |
B4ii—Cs—B9iii | 119.97 (7) | B11—B5—B7 | 60.0 (2) |
O—Cs—B5i | 155.38 (9) | B4—B5—B7 | 107.8 (2) |
B6i—Cs—B5i | 27.78 (7) | B11—B5—B10 | 108.1 (2) |
B10—Cs—B5i | 94.07 (7) | B4—B5—B10 | 59.8 (2) |
B4ii—Cs—B5i | 98.34 (8) | B7—B5—B10 | 60.0 (2) |
B9iii—Cs—B5i | 81.46 (8) | B11—B5—B6 | 60.1 (2) |
O—Cs—B7 | 59.96 (8) | B4—B5—B6 | 59.72 (19) |
B6i—Cs—B7 | 124.11 (7) | B7—B5—B6 | 107.9 (3) |
B10—Cs—B7 | 27.46 (8) | B10—B5—B6 | 107.6 (2) |
B4ii—Cs—B7 | 147.12 (8) | B11—B5—Csv | 79.17 (16) |
B9iii—Cs—B7 | 90.75 (7) | B4—B5—Csv | 113.42 (17) |
B5i—Cs—B7 | 97.57 (7) | B7—B5—Csv | 128.9 (2) |
O—Cs—B12ii | 96.70 (9) | B10—B5—Csv | 171.0 (2) |
B6i—Cs—B12ii | 94.36 (7) | B6—B5—Csv | 71.04 (15) |
B10—Cs—B12ii | 95.23 (7) | B11—B5—H5 | 124 (3) |
B4ii—Cs—B12ii | 27.38 (7) | B4—B5—H5 | 121 (3) |
B9iii—Cs—B12ii | 146.78 (7) | B7—B5—H5 | 121 (3) |
B5i—Cs—B12ii | 104.05 (8) | B10—B5—H5 | 119 (3) |
B7—Cs—B12ii | 120.21 (7) | B6—B5—H5 | 124 (2) |
O—Cs—B11i | 169.75 (8) | Csv—B5—H5 | 58 (2) |
B6i—Cs—B11i | 27.32 (7) | B4—B6—B9 | 108.0 (2) |
B10—Cs—B11i | 101.07 (8) | B4—B6—B11 | 107.9 (2) |
B4ii—Cs—B11i | 72.72 (7) | B9—B6—B11 | 60.43 (19) |
B9iii—Cs—B11i | 100.97 (7) | B4—B6—B12 | 60.16 (18) |
B5i—Cs—B11i | 26.81 (8) | B9—B6—B12 | 59.81 (18) |
B7—Cs—B11i | 115.35 (7) | B11—B6—B12 | 108.2 (2) |
B12ii—Cs—B11i | 77.64 (7) | B4—B6—B5 | 60.0 (2) |
O—Cs—B2 | 85.74 (8) | B9—B6—B5 | 108.1 (2) |
B6i—Cs—B2 | 101.06 (7) | B11—B6—B5 | 59.7 (2) |
B10—Cs—B2 | 26.60 (8) | B12—B6—B5 | 108.1 (2) |
B4ii—Cs—B2 | 140.83 (8) | B4—B6—Csv | 120.77 (17) |
B9iii—Cs—B2 | 97.07 (7) | B9—B6—Csv | 126.64 (19) |
B5i—Cs—B2 | 73.40 (7) | B11—B6—Csv | 83.99 (15) |
B7—Cs—B2 | 26.28 (7) | B12—B6—Csv | 167.23 (18) |
B12ii—Cs—B2 | 116.00 (7) | B5—B6—Csv | 81.17 (16) |
B11i—Cs—B2 | 89.09 (7) | B4—B6—H6 | 121 (2) |
O—Cs—H7 | 51.8 (6) | B9—B6—H6 | 121 (2) |
B6i—Cs—H7 | 126.9 (6) | B11—B6—H6 | 123 (2) |
B10—Cs—H7 | 42.7 (6) | B12—B6—H6 | 120 (2) |
B4ii—Cs—H7 | 153.8 (6) | B5—B6—H6 | 123 (2) |
B9iii—Cs—H7 | 77.6 (6) | Csv—B6—H6 | 48 (2) |
B5i—Cs—H7 | 103.8 (6) | B2—B7—B8 | 60.54 (19) |
B7—Cs—H7 | 15.8 (6) | B2—B7—B11 | 108.6 (2) |
B12ii—Cs—H7 | 130.4 (6) | B8—B7—B11 | 60.17 (19) |
B11i—Cs—H7 | 126.0 (6) | B2—B7—B5 | 108.2 (2) |
B2—Cs—H7 | 39.3 (6) | B8—B7—B5 | 108.1 (2) |
O—Cs—H10 | 73.3 (7) | B11—B7—B5 | 59.8 (2) |
B6i—Cs—H10 | 121.4 (7) | B2—B7—B10 | 59.9 (2) |
B10—Cs—H10 | 14.1 (8) | B8—B7—B10 | 108.2 (2) |
B4ii—Cs—H10 | 108.4 (8) | B11—B7—B10 | 107.9 (2) |
B9iii—Cs—H10 | 131.4 (8) | B5—B7—B10 | 60.0 (2) |
B5i—Cs—H10 | 96.7 (7) | B2—B7—Cs | 81.10 (15) |
B7—Cs—H10 | 41.0 (8) | B8—B7—Cs | 130.72 (18) |
B12ii—Cs—H10 | 81.1 (8) | B11—B7—Cs | 168.97 (19) |
B11i—Cs—H10 | 97.2 (7) | B5—B7—Cs | 112.79 (19) |
B2—Cs—H10 | 38.4 (7) | B10—B7—Cs | 71.96 (15) |
H7—Cs—H10 | 55.5 (9) | B2—B7—H7 | 121.9 (17) |
O—Cs—H14 | 15.9 (3) | B8—B7—H7 | 117.7 (19) |
B6i—Cs—H14 | 162.2 (11) | B11—B7—H7 | 118.7 (18) |
B10—Cs—H14 | 56.2 (6) | B5—B7—H7 | 123.5 (18) |
B4ii—Cs—H14 | 118.4 (8) | B10—B7—H7 | 125.9 (19) |
B9iii—Cs—H14 | 90.4 (12) | Cs—B7—H7 | 57.0 (18) |
B5i—Cs—H14 | 141.0 (5) | B7—B8—B3 | 107.6 (2) |
B7—Cs—H14 | 44.1 (3) | B7—B8—B11 | 59.99 (19) |
B12ii—Cs—H14 | 103.4 (11) | B3—B8—B11 | 107.9 (2) |
B11i—Cs—H14 | 157.2 (6) | B7—B8—B9 | 108.1 (2) |
B2—Cs—H14 | 69.8 (3) | B3—B8—B9 | 59.74 (19) |
H7—Cs—H14 | 37.3 (8) | B11—B8—B9 | 60.37 (19) |
H10—Cs—H14 | 61.0 (11) | B7—B8—B2 | 59.54 (19) |
C4—N—C3 | 109.7 (3) | B3—B8—B2 | 59.99 (19) |
C4—N—C1 | 110.1 (3) | B11—B8—B2 | 107.7 (2) |
C3—N—C1 | 108.8 (3) | B9—B8—B2 | 107.8 (2) |
C4—N—C2 | 109.4 (3) | B7—B8—H8 | 122 (2) |
C3—N—C2 | 109.7 (3) | B3—B8—H8 | 123 (2) |
C1—N—C2 | 109.1 (3) | B11—B8—H8 | 120 (2) |
N—C1—H1A | 109.5 | B9—B8—H8 | 121 (2) |
N—C1—H1B | 109.5 | B2—B8—H8 | 124 (2) |
H1A—C1—H1B | 109.5 | B3—B9—B12 | 60.04 (18) |
N—C1—H1C | 109.5 | B3—B9—B6 | 107.9 (2) |
H1A—C1—H1C | 109.5 | B12—B9—B6 | 60.18 (18) |
H1B—C1—H1C | 109.5 | B3—B9—B8 | 59.96 (18) |
N—C2—H2A | 109.5 | B12—B9—B8 | 108.1 (2) |
N—C2—H2B | 109.5 | B6—B9—B8 | 107.8 (2) |
H2A—C2—H2B | 109.5 | B3—B9—B11 | 107.6 (2) |
N—C2—H2C | 109.5 | B12—B9—B11 | 108.0 (2) |
H2A—C2—H2C | 109.5 | B6—B9—B11 | 59.86 (19) |
H2B—C2—H2C | 109.5 | B8—B9—B11 | 59.74 (18) |
N—C3—H3A | 109.5 | B3—B9—Csvi | 105.67 (17) |
N—C3—H3B | 109.5 | B12—B9—Csvi | 147.34 (16) |
H3A—C3—H3B | 109.5 | B6—B9—Csvi | 145.92 (18) |
N—C3—H3C | 109.5 | B8—B9—Csvi | 84.24 (16) |
H3A—C3—H3C | 109.5 | B11—B9—Csvi | 104.33 (17) |
H3B—C3—H3C | 109.5 | B3—B9—H9 | 125 (2) |
N—C4—H4A | 109.5 | B12—B9—H9 | 123 (2) |
N—C4—H4B | 109.5 | B6—B9—H9 | 119 (2) |
H4A—C4—H4B | 109.5 | B8—B9—H9 | 122 (2) |
N—C4—H4C | 109.5 | B11—B9—H9 | 119 (2) |
H4A—C4—H4C | 109.5 | B1—B10—B2 | 60.5 (2) |
H4B—C4—H4C | 109.5 | B1—B10—B4 | 60.13 (19) |
B10—B1—B4 | 60.1 (2) | B2—B10—B4 | 108.4 (2) |
B10—B1—B12 | 108.4 (2) | B1—B10—B7 | 108.1 (2) |
B4—B1—B12 | 60.21 (18) | B2—B10—B7 | 59.7 (2) |
B10—B1—B3 | 107.8 (2) | B4—B10—B7 | 108.0 (2) |
B4—B1—B3 | 107.8 (2) | B1—B10—B5 | 108.3 (2) |
B12—B1—B3 | 59.82 (18) | B2—B10—B5 | 108.0 (3) |
B10—B1—B2 | 59.9 (2) | B4—B10—B5 | 60.05 (19) |
B4—B1—B2 | 107.9 (2) | B7—B10—B5 | 60.0 (2) |
B12—B1—B2 | 108.0 (2) | B1—B10—Cs | 128.64 (19) |
B3—B1—B2 | 59.92 (19) | B2—B10—Cs | 85.29 (16) |
B10—B1—H1 | 119 (3) | B4—B10—Cs | 166.1 (2) |
B4—B1—H1 | 120 (3) | B7—B10—Cs | 80.58 (15) |
B12—B1—H1 | 123 (3) | B5—B10—Cs | 118.74 (18) |
B3—B1—H1 | 125 (3) | B1—B10—H10 | 120 (2) |
B2—B1—H1 | 122 (3) | B2—B10—H10 | 117 (2) |
B7—B2—B10 | 60.4 (2) | B4—B10—H10 | 125 (2) |
B7—B2—B3 | 107.7 (2) | B7—B10—H10 | 121 (2) |
B10—B2—B3 | 107.6 (2) | B5—B10—H10 | 125 (2) |
B7—B2—B8 | 59.9 (2) | B5—B11—B7 | 60.2 (2) |
B10—B2—B8 | 108.1 (2) | B5—B11—B8 | 108.1 (2) |
B3—B2—B8 | 59.77 (19) | B7—B11—B8 | 59.84 (19) |
B7—B2—B1 | 108.0 (2) | B5—B11—B6 | 60.19 (18) |
B10—B2—B1 | 59.61 (19) | B7—B11—B6 | 108.0 (2) |
B3—B2—B1 | 60.0 (2) | B8—B11—B6 | 107.8 (2) |
B8—B2—B1 | 107.9 (2) | B5—B11—B9 | 107.9 (2) |
B7—B2—Cs | 72.62 (14) | B7—B11—B9 | 107.6 (2) |
B10—B2—Cs | 68.11 (14) | B8—B11—B9 | 59.88 (18) |
B3—B2—Cs | 175.1 (2) | B6—B11—B9 | 59.71 (18) |
B8—B2—Cs | 123.34 (18) | B5—B11—Csv | 74.01 (15) |
B1—B2—Cs | 115.14 (18) | B7—B11—Csv | 124.80 (18) |
B7—B2—H2 | 119 (2) | B8—B11—Csv | 174.59 (19) |
B10—B2—H2 | 121 (2) | B6—B11—Csv | 68.69 (14) |
B3—B2—H2 | 124 (2) | B9—B11—Csv | 114.82 (17) |
B8—B2—H2 | 120 (2) | B5—B11—H11 | 121 (2) |
B1—B2—H2 | 124 (2) | B7—B11—H11 | 117 (2) |
Cs—B2—H2 | 59 (2) | B8—B11—H11 | 120 (2) |
B9—B3—B12 | 60.05 (19) | B6—B11—H11 | 126 (2) |
B9—B3—B8 | 60.31 (19) | B9—B11—H11 | 125 (2) |
B12—B3—B8 | 108.4 (2) | Csv—B11—H11 | 62 (2) |
B9—B3—B2 | 108.5 (2) | B3—B12—B9 | 59.91 (18) |
B12—B3—B2 | 108.3 (2) | B3—B12—B1 | 60.21 (19) |
B8—B3—B2 | 60.24 (19) | B9—B12—B1 | 108.2 (2) |
B9—B3—B1 | 108.1 (2) | B3—B12—B4 | 107.8 (2) |
B12—B3—B1 | 59.97 (19) | B9—B12—B4 | 107.8 (2) |
B8—B3—B1 | 108.3 (2) | B1—B12—B4 | 59.80 (18) |
B2—B3—B1 | 60.1 (2) | B3—B12—B6 | 107.7 (2) |
B9—B3—H3 | 123 (2) | B9—B12—B6 | 60.01 (18) |
B12—B3—H3 | 123 (2) | B1—B12—B6 | 107.6 (2) |
B8—B3—H3 | 121 (2) | B4—B12—B6 | 59.67 (18) |
B2—B3—H3 | 120 (2) | B3—B12—Csiv | 138.56 (19) |
B1—B3—H3 | 121 (2) | B9—B12—Csiv | 161.41 (18) |
B6—B4—B10 | 108.3 (2) | B1—B12—Csiv | 87.86 (16) |
B6—B4—B1 | 108.2 (2) | B4—B12—Csiv | 71.64 (14) |
B10—B4—B1 | 59.7 (2) | B6—B12—Csiv | 106.82 (16) |
B6—B4—B5 | 60.26 (19) | B3—B12—H12 | 124 (2) |
B10—B4—B5 | 60.11 (19) | B9—B12—H12 | 124 (2) |
B1—B4—B5 | 108.0 (2) | B1—B12—H12 | 121 (2) |
B6—B4—B12 | 60.17 (19) | B4—B12—H12 | 120 (2) |
B10—B4—B12 | 107.9 (2) | B6—B12—H12 | 121.6 (19) |
B1—B4—B12 | 59.99 (19) | Csiv—B12—H12 | 49 (2) |
B5—B4—B12 | 108.3 (2) | Cs—O—H13 | 168 (3) |
B6—B4—Csiv | 113.02 (18) | Cs—O—H14 | 92 (3) |
B10—B4—Csiv | 136.02 (19) | H13—O—H14 | 100.6 (16) |
B10—B1—B2—B7 | 37.6 (2) | B2—B1—B10—B5 | −100.8 (3) |
B4—B1—B2—B7 | 0.1 (3) | B4—B1—B10—Cs | −166.9 (3) |
B12—B1—B2—B7 | −63.6 (3) | B12—B1—B10—Cs | 155.69 (19) |
B3—B1—B2—B7 | −100.5 (3) | B3—B1—B10—Cs | 92.4 (3) |
B4—B1—B2—B10 | −37.5 (2) | B2—B1—B10—Cs | 55.1 (2) |
B12—B1—B2—B10 | −101.2 (2) | B7—B2—B10—B1 | −138.1 (2) |
B3—B1—B2—B10 | −138.1 (3) | B3—B2—B10—B1 | −37.4 (2) |
B10—B1—B2—B3 | 138.1 (3) | B8—B2—B10—B1 | −100.5 (2) |
B4—B1—B2—B3 | 100.6 (3) | Cs—B2—B10—B1 | 140.03 (18) |
B12—B1—B2—B3 | 36.9 (2) | B7—B2—B10—B4 | −100.5 (3) |
B10—B1—B2—B8 | 100.9 (3) | B3—B2—B10—B4 | 0.3 (3) |
B4—B1—B2—B8 | 63.4 (3) | B8—B2—B10—B4 | −62.8 (3) |
B12—B1—B2—B8 | −0.3 (3) | B1—B2—B10—B4 | 37.7 (2) |
B3—B1—B2—B8 | −37.2 (2) | Cs—B2—B10—B4 | 177.7 (2) |
B10—B1—B2—Cs | −41.18 (18) | B3—B2—B10—B7 | 100.8 (3) |
B4—B1—B2—Cs | −78.7 (2) | B8—B2—B10—B7 | 37.6 (2) |
B12—B1—B2—Cs | −142.37 (18) | B1—B2—B10—B7 | 138.1 (2) |
B3—B1—B2—Cs | −179.3 (2) | Cs—B2—B10—B7 | −81.83 (15) |
B7—B2—B3—B9 | 0.3 (3) | B7—B2—B10—B5 | −36.9 (2) |
B10—B2—B3—B9 | −63.5 (3) | B3—B2—B10—B5 | 63.9 (3) |
B8—B2—B3—B9 | 37.6 (2) | B8—B2—B10—B5 | 0.7 (3) |
B1—B2—B3—B9 | −100.7 (2) | B1—B2—B10—B5 | 101.2 (2) |
B7—B2—B3—B12 | 63.9 (3) | Cs—B2—B10—B5 | −118.7 (2) |
B10—B2—B3—B12 | 0.2 (3) | B7—B2—B10—Cs | 81.83 (15) |
B8—B2—B3—B12 | 101.2 (3) | B3—B2—B10—Cs | −177.4 (2) |
B1—B2—B3—B12 | −37.0 (2) | B8—B2—B10—Cs | 119.46 (19) |
B7—B2—B3—B8 | −37.3 (2) | B1—B2—B10—Cs | −140.03 (18) |
B10—B2—B3—B8 | −101.1 (3) | B6—B4—B10—B1 | 100.8 (2) |
B1—B2—B3—B8 | −138.3 (2) | B5—B4—B10—B1 | 138.5 (3) |
B7—B2—B3—B1 | 100.9 (3) | B12—B4—B10—B1 | 37.2 (2) |
B10—B2—B3—B1 | 37.2 (2) | Csiv—B4—B10—B1 | −58.4 (3) |
B8—B2—B3—B1 | 138.3 (2) | B6—B4—B10—B2 | 63.0 (3) |
B10—B1—B3—B9 | 64.0 (3) | B1—B4—B10—B2 | −37.8 (2) |
B4—B1—B3—B9 | 0.5 (3) | B5—B4—B10—B2 | 100.6 (3) |
B12—B1—B3—B9 | −37.3 (2) | B12—B4—B10—B2 | −0.6 (3) |
B2—B1—B3—B9 | 101.3 (3) | Csiv—B4—B10—B2 | −96.2 (3) |
B10—B1—B3—B12 | 101.3 (2) | B6—B4—B10—B7 | −0.2 (3) |
B4—B1—B3—B12 | 37.8 (2) | B1—B4—B10—B7 | −101.0 (3) |
B2—B1—B3—B12 | 138.7 (3) | B5—B4—B10—B7 | 37.5 (2) |
B10—B1—B3—B8 | 0.2 (3) | B12—B4—B10—B7 | −63.8 (3) |
B4—B1—B3—B8 | −63.3 (3) | Csiv—B4—B10—B7 | −159.4 (2) |
B12—B1—B3—B8 | −101.2 (2) | B6—B4—B10—B5 | −37.6 (2) |
B2—B1—B3—B8 | 37.5 (2) | B1—B4—B10—B5 | −138.5 (3) |
B10—B1—B3—B2 | −37.3 (2) | B12—B4—B10—B5 | −101.3 (3) |
B4—B1—B3—B2 | −100.8 (3) | Csiv—B4—B10—B5 | 163.2 (3) |
B12—B1—B3—B2 | −138.7 (3) | B6—B4—B10—Cs | −126.6 (8) |
B10—B1—B4—B6 | −101.0 (3) | B1—B4—B10—Cs | 132.5 (9) |
B12—B1—B4—B6 | 37.4 (2) | B5—B4—B10—Cs | −89.0 (9) |
B3—B1—B4—B6 | −0.3 (3) | B12—B4—B10—Cs | 169.7 (7) |
B2—B1—B4—B6 | −63.5 (3) | Csiv—B4—B10—Cs | 74.2 (9) |
B12—B1—B4—B10 | 138.3 (3) | B2—B7—B10—B1 | 37.7 (2) |
B3—B1—B4—B10 | 100.7 (3) | B8—B7—B10—B1 | −0.2 (3) |
B2—B1—B4—B10 | 37.4 (2) | B11—B7—B10—B1 | −63.9 (3) |
B10—B1—B4—B5 | −37.2 (2) | B5—B7—B10—B1 | −101.1 (2) |
B12—B1—B4—B5 | 101.1 (3) | Cs—B7—B10—B1 | 127.7 (2) |
B3—B1—B4—B5 | 63.5 (3) | B8—B7—B10—B2 | −37.9 (2) |
B2—B1—B4—B5 | 0.2 (3) | B11—B7—B10—B2 | −101.6 (2) |
B10—B1—B4—B12 | −138.3 (3) | B5—B7—B10—B2 | −138.8 (2) |
B3—B1—B4—B12 | −37.6 (2) | Cs—B7—B10—B2 | 90.04 (15) |
B2—B1—B4—B12 | −100.9 (3) | B2—B7—B10—B4 | 101.3 (2) |
B10—B1—B4—Csiv | 143.71 (19) | B8—B7—B10—B4 | 63.3 (3) |
B12—B1—B4—Csiv | −77.94 (16) | B11—B7—B10—B4 | −0.3 (3) |
B3—B1—B4—Csiv | −115.6 (2) | B5—B7—B10—B4 | −37.5 (2) |
B2—B1—B4—Csiv | −178.88 (19) | Cs—B7—B10—B4 | −168.7 (2) |
B6—B4—B5—B11 | 37.3 (2) | B2—B7—B10—B5 | 138.8 (2) |
B10—B4—B5—B11 | −100.9 (3) | B8—B7—B10—B5 | 100.8 (2) |
B1—B4—B5—B11 | −63.8 (3) | B11—B7—B10—B5 | 37.2 (2) |
B12—B4—B5—B11 | −0.3 (3) | Cs—B7—B10—B5 | −131.21 (17) |
Csiv—B4—B5—B11 | 113.6 (5) | B2—B7—B10—Cs | −90.04 (15) |
B6—B4—B5—B7 | 100.7 (3) | B8—B7—B10—Cs | −127.97 (19) |
B10—B4—B5—B7 | −37.4 (2) | B11—B7—B10—Cs | 168.4 (2) |
B1—B4—B5—B7 | −0.4 (3) | B5—B7—B10—Cs | 131.21 (17) |
B12—B4—B5—B7 | 63.1 (3) | B11—B5—B10—B1 | 63.5 (3) |
Csiv—B4—B5—B7 | 177.0 (5) | B4—B5—B10—B1 | −37.3 (2) |
B6—B4—B5—B10 | 138.1 (3) | B7—B5—B10—B1 | 100.8 (3) |
B1—B4—B5—B10 | 37.0 (2) | B6—B5—B10—B1 | −0.1 (4) |
B12—B4—B5—B10 | 100.5 (2) | B11—B5—B10—B2 | −0.6 (3) |
Csiv—B4—B5—B10 | −145.5 (6) | B4—B5—B10—B2 | −101.3 (3) |
B10—B4—B5—B6 | −138.1 (3) | B7—B5—B10—B2 | 36.8 (2) |
B1—B4—B5—B6 | −101.1 (3) | B6—B5—B10—B2 | −64.1 (3) |
B12—B4—B5—B6 | −37.6 (2) | B11—B5—B10—B4 | 100.7 (2) |
Csiv—B4—B5—B6 | 76.3 (6) | B7—B5—B10—B4 | 138.1 (2) |
B6—B4—B5—Csv | −48.48 (17) | B6—B5—B10—B4 | 37.2 (2) |
B10—B4—B5—Csv | 173.4 (2) | B11—B5—B10—B7 | −37.4 (2) |
B1—B4—B5—Csv | −149.57 (19) | B4—B5—B10—B7 | −138.1 (2) |
B12—B4—B5—Csv | −86.1 (2) | B6—B5—B10—B7 | −100.9 (3) |
Csiv—B4—B5—Csv | 27.9 (7) | B11—B5—B10—Cs | −95.2 (2) |
B10—B4—B6—B9 | −63.3 (3) | B4—B5—B10—Cs | 164.1 (2) |
B1—B4—B6—B9 | −0.1 (3) | B7—B5—B10—Cs | −57.8 (2) |
B5—B4—B6—B9 | −100.9 (3) | B6—B5—B10—Cs | −158.7 (2) |
B12—B4—B6—B9 | 37.2 (2) | B4—B5—B11—B7 | 100.6 (3) |
Csiv—B4—B6—B9 | 101.1 (2) | B10—B5—B11—B7 | 37.4 (2) |
B10—B4—B6—B11 | 0.5 (3) | B6—B5—B11—B7 | 137.7 (2) |
B1—B4—B6—B11 | 63.8 (3) | Csv—B5—B11—B7 | −148.06 (17) |
B5—B4—B6—B11 | −37.0 (2) | B4—B5—B11—B8 | 63.5 (3) |
B12—B4—B6—B11 | 101.1 (2) | B7—B5—B11—B8 | −37.1 (2) |
Csiv—B4—B6—B11 | 164.99 (17) | B10—B5—B11—B8 | 0.2 (3) |
B10—B4—B6—B12 | −100.6 (2) | B6—B5—B11—B8 | 100.6 (2) |
B1—B4—B6—B12 | −37.3 (2) | Csv—B5—B11—B8 | 174.8 (2) |
B5—B4—B6—B12 | −138.1 (2) | B4—B5—B11—B6 | −37.1 (2) |
Csiv—B4—B6—B12 | 63.90 (17) | B7—B5—B11—B6 | −137.7 (2) |
B10—B4—B6—B5 | 37.5 (2) | B10—B5—B11—B6 | −100.3 (2) |
B1—B4—B6—B5 | 100.8 (3) | Csv—B5—B11—B6 | 74.24 (15) |
B12—B4—B6—B5 | 138.1 (2) | B4—B5—B11—B9 | 0.2 (3) |
Csiv—B4—B6—B5 | −158.0 (2) | B7—B5—B11—B9 | −100.5 (2) |
B10—B4—B6—Csv | 94.2 (2) | B10—B5—B11—B9 | −63.1 (3) |
B1—B4—B6—Csv | 157.45 (18) | B6—B5—B11—B9 | 37.2 (2) |
B5—B4—B6—Csv | 56.7 (2) | Csv—B5—B11—B9 | 111.49 (19) |
B12—B4—B6—Csv | −165.2 (2) | B4—B5—B11—Csv | −111.3 (2) |
Csiv—B4—B6—Csv | −101.34 (16) | B7—B5—B11—Csv | 148.06 (17) |
B11—B5—B6—B4 | −138.4 (2) | B10—B5—B11—Csv | −174.6 (2) |
B7—B5—B6—B4 | −100.6 (3) | B6—B5—B11—Csv | −74.24 (15) |
B10—B5—B6—B4 | −37.3 (3) | B2—B7—B11—B5 | −100.7 (3) |
Csv—B5—B6—B4 | 133.41 (17) | B8—B7—B11—B5 | −138.4 (2) |
B11—B5—B6—B9 | −37.6 (2) | B10—B7—B11—B5 | −37.3 (2) |
B4—B5—B6—B9 | 100.8 (2) | Cs—B7—B11—B5 | 50.0 (11) |
B7—B5—B6—B9 | 0.2 (3) | B2—B7—B11—B8 | 37.7 (2) |
B10—B5—B6—B9 | 63.5 (3) | B5—B7—B11—B8 | 138.4 (2) |
Csv—B5—B6—B9 | −125.8 (2) | B10—B7—B11—B8 | 101.2 (2) |
B4—B5—B6—B11 | 138.4 (2) | Cs—B7—B11—B8 | −171.6 (11) |
B7—B5—B6—B11 | 37.8 (2) | B2—B7—B11—B6 | −62.8 (3) |
B10—B5—B6—B11 | 101.1 (3) | B8—B7—B11—B6 | −100.5 (2) |
Csv—B5—B6—B11 | −88.18 (15) | B5—B7—B11—B6 | 37.9 (2) |
B11—B5—B6—B12 | −100.9 (2) | B10—B7—B11—B6 | 0.6 (3) |
B4—B5—B6—B12 | 37.5 (2) | Cs—B7—B11—B6 | 87.9 (11) |
B7—B5—B6—B12 | −63.1 (3) | B2—B7—B11—B9 | 0.2 (3) |
B10—B5—B6—B12 | 0.3 (4) | B8—B7—B11—B9 | −37.5 (2) |
Csv—B5—B6—B12 | 171.0 (2) | B5—B7—B11—B9 | 100.9 (3) |
B11—B5—B6—Csv | 88.18 (15) | B10—B7—B11—B9 | 63.7 (3) |
B4—B5—B6—Csv | −133.41 (17) | Cs—B7—B11—B9 | 151.0 (10) |
B7—B5—B6—Csv | 126.0 (2) | B2—B7—B11—Csv | −139.0 (2) |
B10—B5—B6—Csv | −170.7 (3) | B8—B7—B11—Csv | −176.7 (2) |
B10—B2—B7—B8 | 137.9 (2) | B5—B7—B11—Csv | −38.3 (2) |
B3—B2—B7—B8 | 37.3 (2) | B10—B7—B11—Csv | −75.5 (2) |
B1—B2—B7—B8 | 100.6 (3) | Cs—B7—B11—Csv | 11.7 (12) |
Cs—B2—B7—B8 | −147.87 (18) | B7—B8—B11—B5 | 37.3 (2) |
B10—B2—B7—B11 | 100.3 (3) | B3—B8—B11—B5 | −63.1 (3) |
B3—B2—B7—B11 | −0.3 (3) | B9—B8—B11—B5 | −100.6 (2) |
B8—B2—B7—B11 | −37.6 (2) | B2—B8—B11—B5 | 0.2 (3) |
B1—B2—B7—B11 | 63.1 (3) | B3—B8—B11—B7 | −100.4 (3) |
Cs—B2—B7—B11 | 174.6 (2) | B9—B8—B11—B7 | −137.9 (3) |
B10—B2—B7—B5 | 36.9 (2) | B2—B8—B11—B7 | −37.0 (2) |
B3—B2—B7—B5 | −63.7 (3) | B7—B8—B11—B6 | 100.9 (3) |
B8—B2—B7—B5 | −100.9 (3) | B3—B8—B11—B6 | 0.5 (3) |
B1—B2—B7—B5 | −0.3 (3) | B9—B8—B11—B6 | −37.0 (2) |
Cs—B2—B7—B5 | 111.2 (2) | B2—B8—B11—B6 | 63.9 (3) |
B3—B2—B7—B10 | −100.6 (3) | B7—B8—B11—B9 | 137.9 (3) |
B8—B2—B7—B10 | −137.9 (2) | B3—B8—B11—B9 | 37.5 (2) |
B1—B2—B7—B10 | −37.2 (2) | B2—B8—B11—B9 | 100.8 (3) |
Cs—B2—B7—B10 | 74.25 (15) | B4—B6—B11—B5 | 37.2 (2) |
B10—B2—B7—Cs | −74.25 (15) | B9—B6—B11—B5 | 138.2 (2) |
B3—B2—B7—Cs | −174.9 (2) | B12—B6—B11—B5 | 100.8 (2) |
B8—B2—B7—Cs | 147.87 (18) | Csv—B6—B11—B5 | −83.27 (16) |
B1—B2—B7—Cs | −111.5 (2) | B4—B6—B11—B7 | −0.7 (3) |
B11—B5—B7—B2 | 101.3 (2) | B9—B6—B11—B7 | 100.3 (2) |
B4—B5—B7—B2 | 0.4 (3) | B12—B6—B11—B7 | 62.9 (3) |
B10—B5—B7—B2 | −36.9 (2) | B5—B6—B11—B7 | −37.9 (2) |
B6—B5—B7—B2 | 63.5 (3) | Csv—B6—B11—B7 | −121.1 (2) |
Csv—B5—B7—B2 | 143.25 (19) | B4—B6—B11—B8 | −63.9 (3) |
B11—B5—B7—B8 | 37.3 (2) | B9—B6—B11—B8 | 37.1 (2) |
B4—B5—B7—B8 | −63.6 (3) | B12—B6—B11—B8 | −0.3 (3) |
B10—B5—B7—B8 | −101.0 (2) | B5—B6—B11—B8 | −101.1 (3) |
B6—B5—B7—B8 | −0.5 (3) | Csv—B6—B11—B8 | 175.6 (2) |
Csv—B5—B7—B8 | 79.2 (3) | B4—B6—B11—B9 | −101.0 (2) |
B4—B5—B7—B11 | −100.9 (2) | B12—B6—B11—B9 | −37.4 (2) |
B10—B5—B7—B11 | −138.3 (2) | B5—B6—B11—B9 | −138.2 (2) |
B6—B5—B7—B11 | −37.8 (2) | Csv—B6—B11—B9 | 138.57 (17) |
Csv—B5—B7—B11 | 41.9 (2) | B4—B6—B11—Csv | 120.4 (2) |
B11—B5—B7—B10 | 138.3 (2) | B9—B6—B11—Csv | −138.57 (17) |
B4—B5—B7—B10 | 37.4 (2) | B12—B6—B11—Csv | −176.0 (2) |
B6—B5—B7—B10 | 100.4 (3) | B5—B6—B11—Csv | 83.27 (16) |
Csv—B5—B7—B10 | −179.8 (2) | B3—B9—B11—B5 | 63.5 (3) |
B11—B5—B7—Cs | −170.8 (2) | B12—B9—B11—B5 | 0.1 (3) |
B4—B5—B7—Cs | 88.2 (2) | B6—B9—B11—B5 | −37.5 (2) |
B10—B5—B7—Cs | 50.89 (17) | B8—B9—B11—B5 | 101.0 (2) |
B6—B5—B7—Cs | 151.3 (2) | Csvi—B9—B11—B5 | 175.38 (17) |
Csv—B5—B7—Cs | −128.94 (16) | B3—B9—B11—B7 | −0.1 (3) |
B2—B7—B8—B3 | −37.3 (2) | B12—B9—B11—B7 | −63.5 (3) |
B11—B7—B8—B3 | 100.9 (2) | B6—B9—B11—B7 | −101.0 (3) |
B5—B7—B8—B3 | 63.8 (3) | B8—B9—B11—B7 | 37.5 (2) |
B10—B7—B8—B3 | 0.3 (3) | Csvi—B9—B11—B7 | 111.9 (2) |
Cs—B7—B8—B3 | −81.2 (3) | B3—B9—B11—B8 | −37.5 (2) |
B2—B7—B8—B11 | −138.2 (2) | B12—B9—B11—B8 | −100.9 (2) |
B5—B7—B8—B11 | −37.1 (2) | B6—B9—B11—B8 | −138.4 (2) |
B10—B7—B8—B11 | −100.6 (2) | Csvi—B9—B11—B8 | 74.39 (17) |
Cs—B7—B8—B11 | 177.9 (3) | B3—B9—B11—B6 | 100.9 (2) |
B2—B7—B8—B9 | −100.4 (3) | B12—B9—B11—B6 | 37.5 (2) |
B11—B7—B8—B9 | 37.8 (2) | B8—B9—B11—B6 | 138.4 (2) |
B5—B7—B8—B9 | 0.7 (3) | Csvi—B9—B11—B6 | −147.16 (19) |
B10—B7—B8—B9 | −62.8 (3) | B3—B9—B11—Csv | 143.70 (18) |
Cs—B7—B8—B9 | −144.3 (2) | B12—B9—B11—Csv | 80.3 (2) |
B11—B7—B8—B2 | 138.2 (2) | B6—B9—B11—Csv | 42.79 (18) |
B5—B7—B8—B2 | 101.1 (3) | B8—B9—B11—Csv | −178.8 (2) |
B10—B7—B8—B2 | 37.7 (2) | Csvi—B9—B11—Csv | −104.37 (13) |
Cs—B7—B8—B2 | −43.9 (2) | B8—B3—B12—B9 | −37.4 (2) |
B9—B3—B8—B7 | −101.1 (2) | B2—B3—B12—B9 | −101.2 (3) |
B12—B3—B8—B7 | −63.9 (3) | B1—B3—B12—B9 | −138.3 (2) |
B2—B3—B8—B7 | 37.1 (2) | B9—B3—B12—B1 | 138.3 (2) |
B1—B3—B8—B7 | −0.3 (3) | B8—B3—B12—B1 | 100.9 (2) |
B9—B3—B8—B11 | −37.8 (2) | B2—B3—B12—B1 | 37.1 (2) |
B12—B3—B8—B11 | −0.5 (3) | B9—B3—B12—B4 | 100.7 (2) |
B2—B3—B8—B11 | 100.4 (3) | B8—B3—B12—B4 | 63.3 (3) |
B1—B3—B8—B11 | 63.0 (3) | B2—B3—B12—B4 | −0.5 (3) |
B12—B3—B8—B9 | 37.3 (2) | B1—B3—B12—B4 | −37.6 (2) |
B2—B3—B8—B9 | 138.2 (3) | B9—B3—B12—B6 | 37.7 (2) |
B1—B3—B8—B9 | 100.8 (2) | B8—B3—B12—B6 | 0.3 (3) |
B9—B3—B8—B2 | −138.2 (3) | B2—B3—B12—B6 | −63.5 (3) |
B12—B3—B8—B2 | −101.0 (3) | B1—B3—B12—B6 | −100.6 (2) |
B1—B3—B8—B2 | −37.4 (2) | B9—B3—B12—Csiv | −177.2 (3) |
B10—B2—B8—B7 | −37.8 (2) | B8—B3—B12—Csiv | 145.4 (2) |
B3—B2—B8—B7 | −138.1 (3) | B2—B3—B12—Csiv | 81.6 (3) |
B1—B2—B8—B7 | −100.9 (3) | B1—B3—B12—Csiv | 44.5 (3) |
Cs—B2—B8—B7 | 37.4 (2) | B6—B9—B12—B3 | 137.7 (2) |
B7—B2—B8—B3 | 138.1 (2) | B8—B9—B12—B3 | 37.2 (2) |
B10—B2—B8—B3 | 100.3 (3) | B11—B9—B12—B3 | 100.3 (2) |
B1—B2—B8—B3 | 37.3 (2) | Csvi—B9—B12—B3 | −71.2 (3) |
Cs—B2—B8—B3 | 175.5 (2) | B3—B9—B12—B1 | −37.4 (2) |
B7—B2—B8—B11 | 37.2 (2) | B6—B9—B12—B1 | 100.3 (2) |
B10—B2—B8—B11 | −0.6 (3) | B8—B9—B12—B1 | −0.3 (3) |
B3—B2—B8—B11 | −100.9 (3) | B11—B9—B12—B1 | 62.9 (3) |
B1—B2—B8—B11 | −63.6 (3) | Csvi—B9—B12—B1 | −108.7 (3) |
Cs—B2—B8—B11 | 74.7 (3) | B3—B9—B12—B4 | −100.6 (2) |
B7—B2—B8—B9 | 101.0 (3) | B6—B9—B12—B4 | 37.1 (2) |
B10—B2—B8—B9 | 63.1 (3) | B8—B9—B12—B4 | −63.5 (3) |
B3—B2—B8—B9 | −37.2 (2) | B11—B9—B12—B4 | −0.3 (3) |
B1—B2—B8—B9 | 0.1 (3) | Csvi—B9—B12—B4 | −171.9 (2) |
Cs—B2—B8—B9 | 138.38 (19) | B3—B9—B12—B6 | −137.7 (2) |
B8—B3—B9—B12 | 138.5 (2) | B8—B9—B12—B6 | −100.6 (2) |
B2—B3—B9—B12 | 100.9 (2) | B11—B9—B12—B6 | −37.4 (2) |
B1—B3—B9—B12 | 37.3 (2) | Csvi—B9—B12—B6 | 151.0 (3) |
B12—B3—B9—B6 | −37.8 (2) | B3—B9—B12—Csiv | 174.2 (5) |
B8—B3—B9—B6 | 100.6 (2) | B6—B9—B12—Csiv | −48.1 (5) |
B2—B3—B9—B6 | 63.1 (3) | B8—B9—B12—Csiv | −148.6 (4) |
B1—B3—B9—B6 | −0.6 (3) | B11—B9—B12—Csiv | −85.5 (5) |
B12—B3—B9—B8 | −138.5 (2) | Csvi—B9—B12—Csiv | 103.0 (5) |
B2—B3—B9—B8 | −37.6 (2) | B10—B1—B12—B3 | −100.3 (3) |
B1—B3—B9—B8 | −101.2 (2) | B4—B1—B12—B3 | −137.7 (2) |
B12—B3—B9—B11 | −101.0 (2) | B2—B1—B12—B3 | −37.0 (2) |
B8—B3—B9—B11 | 37.4 (2) | B10—B1—B12—B9 | −63.0 (3) |
B2—B3—B9—B11 | −0.1 (3) | B4—B1—B12—B9 | −100.4 (2) |
B1—B3—B9—B11 | −63.7 (3) | B3—B1—B12—B9 | 37.3 (2) |
B12—B3—B9—Csvi | 147.95 (17) | B2—B1—B12—B9 | 0.3 (3) |
B8—B3—B9—Csvi | −73.58 (17) | B10—B1—B12—B4 | 37.4 (2) |
B2—B3—B9—Csvi | −111.1 (2) | B3—B1—B12—B4 | 137.7 (2) |
B1—B3—B9—Csvi | −174.76 (17) | B2—B1—B12—B4 | 100.8 (3) |
B4—B6—B9—B3 | 0.4 (3) | B10—B1—B12—B6 | 0.4 (3) |
B11—B6—B9—B3 | −100.3 (2) | B4—B1—B12—B6 | −37.0 (2) |
B12—B6—B9—B3 | 37.8 (2) | B3—B1—B12—B6 | 100.7 (2) |
B5—B6—B9—B3 | −63.1 (3) | B2—B1—B12—B6 | 63.7 (3) |
Csv—B6—B9—B3 | −155.45 (17) | B10—B1—B12—Csiv | 107.3 (2) |
B4—B6—B9—B12 | −37.4 (2) | B4—B1—B12—Csiv | 69.94 (15) |
B11—B6—B9—B12 | −138.1 (2) | B3—B1—B12—Csiv | −152.35 (17) |
B5—B6—B9—B12 | −100.9 (3) | B2—B1—B12—Csiv | 170.7 (2) |
Csv—B6—B9—B12 | 166.8 (2) | B6—B4—B12—B3 | −100.5 (2) |
B4—B6—B9—B8 | 63.7 (3) | B10—B4—B12—B3 | 0.7 (3) |
B11—B6—B9—B8 | −37.0 (2) | B1—B4—B12—B3 | 37.8 (2) |
B12—B6—B9—B8 | 101.1 (2) | B5—B4—B12—B3 | −62.9 (3) |
B5—B6—B9—B8 | 0.3 (3) | Csiv—B4—B12—B3 | 136.3 (2) |
Csv—B6—B9—B8 | −92.1 (2) | B6—B4—B12—B9 | −37.3 (2) |
B4—B6—B9—B11 | 100.7 (2) | B10—B4—B12—B9 | 64.0 (3) |
B12—B6—B9—B11 | 138.1 (2) | B1—B4—B12—B9 | 101.1 (2) |
B5—B6—B9—B11 | 37.3 (2) | B5—B4—B12—B9 | 0.4 (3) |
Csv—B6—B9—B11 | −55.1 (2) | Csiv—B4—B12—B9 | −160.45 (19) |
B4—B6—B9—Csvi | 170.4 (2) | B6—B4—B12—B1 | −138.3 (2) |
B11—B6—B9—Csvi | 69.7 (3) | B10—B4—B12—B1 | −37.1 (2) |
B12—B6—B9—Csvi | −152.2 (3) | B5—B4—B12—B1 | −100.7 (3) |
B5—B6—B9—Csvi | 106.9 (3) | Csiv—B4—B12—B1 | 98.49 (16) |
Csv—B6—B9—Csvi | 14.6 (4) | B10—B4—B12—B6 | 101.2 (3) |
B7—B8—B9—B3 | 100.2 (3) | B1—B4—B12—B6 | 138.3 (2) |
B11—B8—B9—B3 | 137.9 (2) | B5—B4—B12—B6 | 37.6 (2) |
B2—B8—B9—B3 | 37.3 (2) | Csiv—B4—B12—B6 | −123.19 (16) |
B7—B8—B9—B12 | 63.0 (3) | B6—B4—B12—Csiv | 123.19 (16) |
B3—B8—B9—B12 | −37.2 (2) | B10—B4—B12—Csiv | −135.6 (2) |
B11—B8—B9—B12 | 100.7 (2) | B1—B4—B12—Csiv | −98.49 (16) |
B2—B8—B9—B12 | 0.1 (3) | B5—B4—B12—Csiv | 160.8 (2) |
B7—B8—B9—B6 | −0.6 (3) | B4—B6—B12—B3 | 100.6 (2) |
B3—B8—B9—B6 | −100.8 (2) | B9—B6—B12—B3 | −37.7 (2) |
B11—B8—B9—B6 | 37.1 (2) | B11—B6—B12—B3 | 0.0 (3) |
B2—B8—B9—B6 | −63.5 (3) | B5—B6—B12—B3 | 63.1 (3) |
B7—B8—B9—B11 | −37.7 (2) | Csv—B6—B12—B3 | −161.5 (8) |
B3—B8—B9—B11 | −137.9 (2) | B4—B6—B12—B9 | 138.3 (2) |
B2—B8—B9—B11 | −100.6 (3) | B11—B6—B12—B9 | 37.7 (2) |
B7—B8—B9—Csvi | −148.0 (2) | B5—B6—B12—B9 | 100.8 (3) |
B3—B8—B9—Csvi | 111.84 (16) | Csv—B6—B12—B9 | −123.8 (9) |
B11—B8—B9—Csvi | −110.30 (17) | B4—B6—B12—B1 | 37.1 (2) |
B2—B8—B9—Csvi | 149.1 (2) | B9—B6—B12—B1 | −101.2 (2) |
B4—B1—B10—B2 | 138.1 (2) | B11—B6—B12—B1 | −63.5 (3) |
B12—B1—B10—B2 | 100.6 (3) | B5—B6—B12—B1 | −0.4 (3) |
B3—B1—B10—B2 | 37.4 (2) | Csv—B6—B12—B1 | 135.0 (8) |
B12—B1—B10—B4 | −37.4 (2) | B9—B6—B12—B4 | −138.3 (2) |
B3—B1—B10—B4 | −100.7 (2) | B11—B6—B12—B4 | −100.6 (2) |
B2—B1—B10—B4 | −138.1 (2) | B5—B6—B12—B4 | −37.5 (2) |
B4—B1—B10—B7 | 100.8 (3) | Csv—B6—B12—B4 | 97.9 (9) |
B12—B1—B10—B7 | 63.3 (3) | B4—B6—B12—Csiv | −56.07 (16) |
B3—B1—B10—B7 | 0.1 (3) | B9—B6—B12—Csiv | 165.66 (18) |
B2—B1—B10—B7 | −37.3 (2) | B11—B6—B12—Csiv | −156.68 (17) |
B4—B1—B10—B5 | 37.2 (2) | B5—B6—B12—Csiv | −93.6 (2) |
B12—B1—B10—B5 | −0.2 (4) | Csv—B6—B12—Csiv | 41.8 (9) |
B3—B1—B10—B5 | −63.4 (3) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1/2, −y, z−1/2; (iii) −x+3/2, −y, z−1/2; (iv) −x+1/2, −y, z+1/2; (v) −x+1, y+1/2, −z+1/2; (vi) −x+3/2, −y, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O—H14···H7 | 0.91 (1) | 2.11 (3) | 2.86 (3) | 135 (4) |
O—H13···H1v | 0.91 (1) | 2.45 (3) | 3.24 (3) | 146 (4) |
O—H13···H2v | 0.91 (1) | 2.47 (3) | 3.07 (3) | 124 (4) |
O—H13···H3v | 0.91 (1) | 2.39 (3) | 3.11 (3) | 136 (4) |
C1—H1A···H3ii | 0.98 | 2.49 | 3.35 (5) | 143 |
C2—H2B···H5 | 0.98 | 2.33 | 3.20 (5) | 151 |
C2—H2C···H6vii | 0.98 | 2.49 | 3.29 (4) | 138 |
C2—H2B···H9vii | 0.98 | 2.51 | 2.79 (4) | 96 |
C3—H3C···H8viii | 0.98 | 2.51 | 3.18 (4) | 126 |
C3—H3C···H11viii | 0.98 | 2.33 | 3.28 (4) | 160 |
C4—H4B···H3ii | 0.98 | 2.30 | 3.21 (4) | 152 |
C4—H4C···H1ix | 0.98 | 2.52 | 2.82 (5) | 98 |
Symmetry codes: (ii) −x+1/2, −y, z−1/2; (v) −x+1, y+1/2, −z+1/2; (vii) x−1/2, −y+1/2, −z+1; (viii) x−1, y, z; (ix) −x, y+1/2, −z+1/2. |
Acknowledgements
The authors thank Dr F. Lissner (Institut für Anorganische Chemie, Universität Stuttgart) for recording the diffraction data. This work was supported by the state of Baden–Württemberg (Stuttgart) and the Deutsche Forschungsgemeinschaft (DFG; Frankfurt/Main) within the funding program Open Access Publishing.
References
Blessing, R. H. (1995). Acta Cryst. A51, 33–38. CrossRef CAS Web of Science IUCr Journals Google Scholar
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Hofmann, K. & Albert, B. (2001). Z. Anorg. Allg. Chem. 627, 1055–1058. CSD CrossRef CAS Google Scholar
Hooft, R. W. W. (2004). COLLECT. Bruker–Nonius BV, Delft, The Netherlands. Google Scholar
Kraus, F. & Albert, B. (2005). Z. Anorg. Allg. Chem. 631, 152–154. CrossRef CAS Google Scholar
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Tiritiris, I. & Schleid, Th. (2003). Z. Anorg. Allg. Chem. 629, 1390–1402. CSD CrossRef CAS Google Scholar
Tiritiris, I. & Schleid, Th. (2008). Z. Anorg. Allg. Chem. 634, 1353–1360. CrossRef CAS Google Scholar
Tiritiris, I., Schleid, Th., Müller, K. & Preetz, W. (2000). Z. Anorg. Allg. Chem. 626, 323–325. CrossRef CAS Google Scholar
Yisgedu, T. B., Chen, X., Lingam, H. K., Huang, Z., Meyers, E. A., Shore, S. G. & Zhao, J.-C. (2010). Acta Cryst. C66, m1–m3. CSD CrossRef IUCr Journals Google Scholar
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