Caesium tetra­methyl­ammonium dodeca­hydrido-closo-dodeca­borate monohydrate

Tiritiris, I.; Schleid, T.

doi:10.1107/S2414314616002911

metal-organic compounds

IUCrDATA

ISSN: 2414-3146

Volume 1| Part 2| February 2016| x160291

https://doi.org/10.1107/S2414314616002911

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Caesium tetramethylammonium dodecahydrido-closo-dodecaborate monohydrate

Ioannis Tiritiris ^a and Thomas Schleid ^a ^*

^aInstitut für Anorganische Chemie, Universität Stuttgart, Pfaffenwaldring 55, D-70569 Stuttgart, Germany
^*Correspondence e-mail: schleid@iac.uni-stuttgart.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 27 January 2016; accepted 17 February 2016; online 24 February 2016)

In the crystal structure of the hydrated double salt, Cs⁺·[N(CH₃)₄]⁺·[B₁₂H₁₂]²⁻·H₂O, the asymmetric unit 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 crystal structure is stabilized by a three-dimensional network of O—H⋯H—B and C—H⋯H—B dihydrogen bonds.

Keywords: 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 coordination number of 11 (Fig. 2). Every dodecahydrido-closo-dodecaborate anion is surrounded by four caesium and four tetramethylammonium cations, forming a slightly distorted cube.

Figure 1
The molecular components of the title compound, with displacement ellipsoids drawn at the 50% probability level.

Figure 2
Tetrahedral coordination of caesium by four dodecahydrido-closo-dodecaborate anions with the water molecule completing the coordination sphere of the cation.

The crystal structure is mainly stabilized by O—H⋯H—B dihydrogen bonds between the water molecules and the [B₁₂H₁₂]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 crystal structure 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).

Table 1
Hydrogen-bond geometry (Å, °)

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⋯H1ⁱ	0.91 (1)	2.45 (3)	3.24 (3)	146 (4)
O—H13⋯H2ⁱ	0.91 (1)	2.47 (3)	3.07 (3)	124 (4)
O—H13⋯H3ⁱ	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⋯H6ⁱⁱⁱ	0.98	2.49	3.29 (4)	138
C2—H2B⋯H9ⁱⁱⁱ	0.98	2.51	2.79 (4)	96
C3—H3C⋯H8^iv	0.98	2.51	3.18 (4)	126
C3—H3C⋯H11^iv	0.98	2.33	3.28 (4)	160
C4—H4B⋯H3ⁱⁱ	0.98	2.30	3.21 (4)	152
C4—H4C⋯H1^v	0.98	2.52	2.82 (5)	98
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y, z-{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (iv) x-1, y, z; (v) $[-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Figure 3
B—H⋯H—O dihydrogen bonds (depicted by grey dashed lines) between two [B₁₂H₁₂]²⁻ anions and a water molecule.

Figure 4
The molecular packing of the title compound (central projection with view along [100]). The O—H⋯H—B and C—H⋯H—B dihydrogen bonds are depicted by brown dashed lines.

Synthesis 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 refinement details are summarized in Table 2. The residual electron-density peak of 1.585 e Å⁻³ is located 0.80 Å from the Cs atom.

Table 2
Experimental details

Crystal data
Chemical formula	Cs⁺·C₄H₁₂N⁺·B₁₂H₁₂²⁻·H₂O
M_r	366.89
Crystal system, space group	Orthorhombic, P2₁2₁2₁
Temperature (K)	173
a, b, c (Å)	8.9771 (5), 12.8680 (8), 14.5449 (9)
V (Å³)	1680.19 (17)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	2.18
Crystal size (mm)	0.55 × 0.15 × 0.10

Data collection
Diffractometer	Bruker–Nonius KappaCCD
Absorption correction	Multi-scan (Blessing, 1995 )
T_min, T_max	0.70, 0.80
No. of measured, independent and observed [I > 2σ(I)] reflections	3552, 3279, 3143
R_int	0.017
(sin θ/λ)_max (Å⁻¹)	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.063, 1.05
No. of reflections	3279
No. of parameters	231
No. of restraints	3
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.59, −0.76
Absolute structure	Classical Flack method preferred over Parsons because s.u. lower
Absolute structure parameter	−0.02 (2)
Computer programs: COLLECT (Hooft, 2004 ), DENZO-SMN (Otwinowski & Minor, 1997 ), SHELXS97 (Sheldrick, 2008 ), SHELXL2014 (Sheldrick, 2015 ), DIAMOND (Brandenburg & Putz, 2005 ).

Structural data

CCDC reference: 1454125

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314616002911/wm4007sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314616002911/wm4007Isup2.hkl

checkCIF report

Computing details top

Data collection: COLLECT (Hooft, 2004); cell refinement: 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).

Caesium tetramethylammonium dodecahydro-closo-dodecaborate monohydrate top

Crystal data top

Cs⁺·C₄H₁₂N⁺·B₁₂H₁₂²⁻·H₂O	D_x = 1.450 Mg m⁻³
M_r = 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

Data collection top

Bruker–Nonius KappaCCD diffractometer	3279 independent reflections
Radiation source: fine-focus sealed tube	3143 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.017
φ scans, and ω scans	θ_max = 30.0°, θ_min = 2.1°
Absorption correction: multi-scan (Blessing, 1995)	h = −12→12
T_min = 0.70, T_max = 0.80	k = −18→18
3552 measured reflections	l = −20→20

Refinement top

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(F_o²) + (0.0426P)² + 0.3622P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max < 0.001
3279 reflections	Δρ_max = 1.59 e Å⁻³
231 parameters	Δρ_min = −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)

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.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—Cs^iv	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—Cs^v	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—Cs^v	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—Cs^vi	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—Cs^v	3.868 (3)
B1—H1	0.97 (5)	B11—H11	1.13 (4)
B2—B7	1.771 (5)	B12—Cs^iv	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—Cs^iv	92.75 (17)
O—Cs—B10	70.69 (8)	B5—B4—Cs^iv	159.22 (19)
B6ⁱ—Cs—B10	121.23 (8)	B12—B4—Cs^iv	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—Cs^v	79.17 (16)
B9ⁱⁱⁱ—Cs—B7	90.75 (7)	B4—B5—Cs^v	113.42 (17)
B5ⁱ—Cs—B7	97.57 (7)	B7—B5—Cs^v	128.9 (2)
O—Cs—B12ⁱⁱ	96.70 (9)	B10—B5—Cs^v	171.0 (2)
B6ⁱ—Cs—B12ⁱⁱ	94.36 (7)	B6—B5—Cs^v	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)	Cs^v—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—Cs^v	120.77 (17)
B9ⁱⁱⁱ—Cs—B2	97.07 (7)	B9—B6—Cs^v	126.64 (19)
B5ⁱ—Cs—B2	73.40 (7)	B11—B6—Cs^v	83.99 (15)
B7—Cs—B2	26.28 (7)	B12—B6—Cs^v	167.23 (18)
B12ⁱⁱ—Cs—B2	116.00 (7)	B5—B6—Cs^v	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)	Cs^v—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—Cs^vi	105.67 (17)
N—C3—H3B	109.5	B12—B9—Cs^vi	147.34 (16)
H3A—C3—H3B	109.5	B6—B9—Cs^vi	145.92 (18)
N—C3—H3C	109.5	B8—B9—Cs^vi	84.24 (16)
H3A—C3—H3C	109.5	B11—B9—Cs^vi	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—Cs^v	74.01 (15)
B1—B2—Cs	115.14 (18)	B7—B11—Cs^v	124.80 (18)
B7—B2—H2	119 (2)	B8—B11—Cs^v	174.59 (19)
B10—B2—H2	121 (2)	B6—B11—Cs^v	68.69 (14)
B3—B2—H2	124 (2)	B9—B11—Cs^v	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)	Cs^v—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—Cs^iv	138.56 (19)
B1—B3—H3	121 (2)	B9—B12—Cs^iv	161.41 (18)
B6—B4—B10	108.3 (2)	B1—B12—Cs^iv	87.86 (16)
B6—B4—B1	108.2 (2)	B4—B12—Cs^iv	71.64 (14)
B10—B4—B1	59.7 (2)	B6—B12—Cs^iv	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)	Cs^iv—B12—H12	49 (2)
B5—B4—B12	108.3 (2)	Cs—O—H13	168 (3)
B6—B4—Cs^iv	113.02 (18)	Cs—O—H14	92 (3)
B10—B4—Cs^iv	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)	Cs^iv—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)	Cs^iv—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)	Cs^iv—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)	Cs^iv—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)	Cs^iv—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—Cs^iv	143.71 (19)	B8—B7—B10—B4	63.3 (3)
B12—B1—B4—Cs^iv	−77.94 (16)	B11—B7—B10—B4	−0.3 (3)
B3—B1—B4—Cs^iv	−115.6 (2)	B5—B7—B10—B4	−37.5 (2)
B2—B1—B4—Cs^iv	−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)
Cs^iv—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)
Cs^iv—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)
Cs^iv—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)
Cs^iv—B4—B5—B6	76.3 (6)	B7—B5—B10—B4	138.1 (2)
B6—B4—B5—Cs^v	−48.48 (17)	B6—B5—B10—B4	37.2 (2)
B10—B4—B5—Cs^v	173.4 (2)	B11—B5—B10—B7	−37.4 (2)
B1—B4—B5—Cs^v	−149.57 (19)	B4—B5—B10—B7	−138.1 (2)
B12—B4—B5—Cs^v	−86.1 (2)	B6—B5—B10—B7	−100.9 (3)
Cs^iv—B4—B5—Cs^v	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)
Cs^iv—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)	Cs^v—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)
Cs^iv—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)	Cs^v—B5—B11—B8	174.8 (2)
B5—B4—B6—B12	−138.1 (2)	B4—B5—B11—B6	−37.1 (2)
Cs^iv—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)	Cs^v—B5—B11—B6	74.24 (15)
B12—B4—B6—B5	138.1 (2)	B4—B5—B11—B9	0.2 (3)
Cs^iv—B4—B6—B5	−158.0 (2)	B7—B5—B11—B9	−100.5 (2)
B10—B4—B6—Cs^v	94.2 (2)	B10—B5—B11—B9	−63.1 (3)
B1—B4—B6—Cs^v	157.45 (18)	B6—B5—B11—B9	37.2 (2)
B5—B4—B6—Cs^v	56.7 (2)	Cs^v—B5—B11—B9	111.49 (19)
B12—B4—B6—Cs^v	−165.2 (2)	B4—B5—B11—Cs^v	−111.3 (2)
Cs^iv—B4—B6—Cs^v	−101.34 (16)	B7—B5—B11—Cs^v	148.06 (17)
B11—B5—B6—B4	−138.4 (2)	B10—B5—B11—Cs^v	−174.6 (2)
B7—B5—B6—B4	−100.6 (3)	B6—B5—B11—Cs^v	−74.24 (15)
B10—B5—B6—B4	−37.3 (3)	B2—B7—B11—B5	−100.7 (3)
Cs^v—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)
Cs^v—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)
Cs^v—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)
Cs^v—B5—B6—B12	171.0 (2)	B5—B7—B11—B9	100.9 (3)
B11—B5—B6—Cs^v	88.18 (15)	B10—B7—B11—B9	63.7 (3)
B4—B5—B6—Cs^v	−133.41 (17)	Cs—B7—B11—B9	151.0 (10)
B7—B5—B6—Cs^v	126.0 (2)	B2—B7—B11—Cs^v	−139.0 (2)
B10—B5—B6—Cs^v	−170.7 (3)	B8—B7—B11—Cs^v	−176.7 (2)
B10—B2—B7—B8	137.9 (2)	B5—B7—B11—Cs^v	−38.3 (2)
B3—B2—B7—B8	37.3 (2)	B10—B7—B11—Cs^v	−75.5 (2)
B1—B2—B7—B8	100.6 (3)	Cs—B7—B11—Cs^v	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)	Cs^v—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)	Cs^v—B6—B11—B7	−121.1 (2)
Cs^v—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)	Cs^v—B6—B11—B8	175.6 (2)
Cs^v—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)	Cs^v—B6—B11—B9	138.57 (17)
Cs^v—B5—B7—B11	41.9 (2)	B4—B6—B11—Cs^v	120.4 (2)
B11—B5—B7—B10	138.3 (2)	B9—B6—B11—Cs^v	−138.57 (17)
B4—B5—B7—B10	37.4 (2)	B12—B6—B11—Cs^v	−176.0 (2)
B6—B5—B7—B10	100.4 (3)	B5—B6—B11—Cs^v	83.27 (16)
Cs^v—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)	Cs^vi—B9—B11—B5	175.38 (17)
Cs^v—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)	Cs^vi—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)	Cs^vi—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)	Cs^vi—B9—B11—B6	−147.16 (19)
B10—B7—B8—B9	−62.8 (3)	B3—B9—B11—Cs^v	143.70 (18)
Cs—B7—B8—B9	−144.3 (2)	B12—B9—B11—Cs^v	80.3 (2)
B11—B7—B8—B2	138.2 (2)	B6—B9—B11—Cs^v	42.79 (18)
B5—B7—B8—B2	101.1 (3)	B8—B9—B11—Cs^v	−178.8 (2)
B10—B7—B8—B2	37.7 (2)	Cs^vi—B9—B11—Cs^v	−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—Cs^iv	−177.2 (3)
B10—B2—B8—B7	−37.8 (2)	B8—B3—B12—Cs^iv	145.4 (2)
B3—B2—B8—B7	−138.1 (3)	B2—B3—B12—Cs^iv	81.6 (3)
B1—B2—B8—B7	−100.9 (3)	B1—B3—B12—Cs^iv	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)	Cs^vi—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)	Cs^vi—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)	Cs^vi—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)	Cs^vi—B9—B12—B6	151.0 (3)
B12—B3—B9—B6	−37.8 (2)	B3—B9—B12—Cs^iv	174.2 (5)
B8—B3—B9—B6	100.6 (2)	B6—B9—B12—Cs^iv	−48.1 (5)
B2—B3—B9—B6	63.1 (3)	B8—B9—B12—Cs^iv	−148.6 (4)
B1—B3—B9—B6	−0.6 (3)	B11—B9—B12—Cs^iv	−85.5 (5)
B12—B3—B9—B8	−138.5 (2)	Cs^vi—B9—B12—Cs^iv	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—Cs^vi	147.95 (17)	B2—B1—B12—B9	0.3 (3)
B8—B3—B9—Cs^vi	−73.58 (17)	B10—B1—B12—B4	37.4 (2)
B2—B3—B9—Cs^vi	−111.1 (2)	B3—B1—B12—B4	137.7 (2)
B1—B3—B9—Cs^vi	−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)
Cs^v—B6—B9—B3	−155.45 (17)	B10—B1—B12—Cs^iv	107.3 (2)
B4—B6—B9—B12	−37.4 (2)	B4—B1—B12—Cs^iv	69.94 (15)
B11—B6—B9—B12	−138.1 (2)	B3—B1—B12—Cs^iv	−152.35 (17)
B5—B6—B9—B12	−100.9 (3)	B2—B1—B12—Cs^iv	170.7 (2)
Cs^v—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)	Cs^iv—B4—B12—B3	136.3 (2)
Cs^v—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)
Cs^v—B6—B9—B11	−55.1 (2)	Cs^iv—B4—B12—B9	−160.45 (19)
B4—B6—B9—Cs^vi	170.4 (2)	B6—B4—B12—B1	−138.3 (2)
B11—B6—B9—Cs^vi	69.7 (3)	B10—B4—B12—B1	−37.1 (2)
B12—B6—B9—Cs^vi	−152.2 (3)	B5—B4—B12—B1	−100.7 (3)
B5—B6—B9—Cs^vi	106.9 (3)	Cs^iv—B4—B12—B1	98.49 (16)
Cs^v—B6—B9—Cs^vi	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)	Cs^iv—B4—B12—B6	−123.19 (16)
B7—B8—B9—B12	63.0 (3)	B6—B4—B12—Cs^iv	123.19 (16)
B3—B8—B9—B12	−37.2 (2)	B10—B4—B12—Cs^iv	−135.6 (2)
B11—B8—B9—B12	100.7 (2)	B1—B4—B12—Cs^iv	−98.49 (16)
B2—B8—B9—B12	0.1 (3)	B5—B4—B12—Cs^iv	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)	Cs^v—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—Cs^vi	−148.0 (2)	B5—B6—B12—B9	100.8 (3)
B3—B8—B9—Cs^vi	111.84 (16)	Cs^v—B6—B12—B9	−123.8 (9)
B11—B8—B9—Cs^vi	−110.30 (17)	B4—B6—B12—B1	37.1 (2)
B2—B8—B9—Cs^vi	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)	Cs^v—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)	Cs^v—B6—B12—B4	97.9 (9)
B12—B1—B10—B7	63.3 (3)	B4—B6—B12—Cs^iv	−56.07 (16)
B3—B1—B10—B7	0.1 (3)	B9—B6—B12—Cs^iv	165.66 (18)
B2—B1—B10—B7	−37.3 (2)	B11—B6—B12—Cs^iv	−156.68 (17)
B4—B1—B10—B5	37.2 (2)	B5—B6—B12—Cs^iv	−93.6 (2)
B12—B1—B10—B5	−0.2 (4)	Cs^v—B6—B12—Cs^iv	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.

Hydrogen-bond geometry (Å, º) top

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···H1^v	0.91 (1)	2.45 (3)	3.24 (3)	146 (4)
O—H13···H2^v	0.91 (1)	2.47 (3)	3.07 (3)	124 (4)
O—H13···H3^v	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···H6^vii	0.98	2.49	3.29 (4)	138
C2—H2B···H9^vii	0.98	2.51	2.79 (4)	96
C3—H3C···H8^viii	0.98	2.51	3.18 (4)	126
C3—H3C···H11^viii	0.98	2.33	3.28 (4)	160
C4—H4B···H3ⁱⁱ	0.98	2.30	3.21 (4)	152
C4—H4C···H1^ix	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.

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