Literature DB >> 28217330

Crystal structure of tris[(4,7,13,16,21,24-hexa-oxa-1,10-di-aza-bicyclo-[8.8.8]hexa-cosane-κ8N2,O6)rubidium] rubidium nona-stannide.

Wilhelm Klein1, Haiyan He1, Thomas F Fässler1.   

Abstract

The crystal structure of the title compound, [Rb(C18H36N2O6)]3RbSn9, consists of deltahedral [Sn9]4- cluster anions, Rb+ cations and cryptand mol-ecules, which partially sequester the cations. Those cations, which are not coordinated by cryptand mol-ecules, are neighboured directly to the [Sn9]4- clusters and inter-connect them to form ∞1[RbSn9]3- chains. These chains extend parallel to [001] and are arranged in a pseudo-hexa-gonal rod packing, separated by the Rb-cryptand complex cations.

Entities:  

Keywords:  Zintl anions; cage compounds; crystal structure; isotypism; stannides; tin

Year:  2017        PMID: 28217330      PMCID: PMC5290553          DOI: 10.1107/S2056989017000172

Source DB:  PubMed          Journal:  Acta Crystallogr E Crystallogr Commun


Chemical context

The dissolution of elemental tin in alkali metal ammonia solutions was reported first by Joannis (1891 ▸). Since then Zintl compounds containing tetrel elements, particularly the remarkably stable nine-membered cluster compounds, have been studied intensively. Plenty of chemical reactions such as reduction, oligomerization, functionalization, and even filling of the nine-membered clusters with transition metal atoms, have been investigated (Scharfe et al., 2011 ▸). For enabling this extended variety of chemical reactions, dissolution of solid Zintl cluster compounds in organic solvents is often helpful or even necessary. To achieve this, the addition of sequestering agents like crown ethers or cryptands has been successfully applied (Corbett & Edwards, 1975 ▸). During our experiments including the Zintl cluster compound Rb4Sn9 in ethyl­enedi­amine in the presence of 2.2.2-cryptand, single crystals of the title compound, [Rb(2.2.2)-crypt]3RbSn9, have been obtained.

Structural commentary

The title compound crystallizes in space group P with all atoms at general sites except for Rb1 and Rb2, which are located on inversion centres (Wyckoff sites 1a and 1b). The crystal structure consists of five rubidium cations, partially sequestered by cryptand-[2.2.2], and nine-atomic Sn clusters, see Fig. 1 ▸. The composition of four Rb+ cations per Sn9 cluster anion indicate a fourfold negative charge and, thus, 22 skeleton electrons for [Sn9]. According to the Wade–Mingos electron-counting rules, the shape of such a [Sn9]4– anion is predicted to be a nido cage, a mono-capped square anti­prism with C 4 symmetry (Fässler, 2001 ▸). Indeed, the cluster Sn atoms form an almost C 4 symmetric mono-capped square anti­prism, as indicated e.g. by the planarity and equal diagonal lengths of the square formed by atoms Sn1, Sn2, Sn3, and Sn4 [ratio of diagonals 1.03, dihedral angle between the two triangle halves of the square 3.59 (3)°]. However, larger devi­ations from the ideal C 4 symmetry are frequent, e.g. in the closely related compound [K(2.2.2)-crypt][K(18-crown-6)]2KSn9 (He et al., 2014a ▸) where the [Sn9]4– cluster exhibits a shape close to D 3 symmetry. The Sn9 clusters are capped by two crystallographically independent rubidium cations (Rb1 and Rb2) with SnRb distances in the range between 3.5976 (10) Å and 3.8357 (10) Å; for both cations a third longer distance of more than 4 Å indicates an inter­mediate between edge-coordination and face-coordination at two opposite sites (Fig. 1 ▸). Both the cations are located at special crystallographic sites, Rb1 at 1a and Rb2 at 1b, so their surroundings, although irregular, are centrosymmetric. The title compound represents the fourth member of this structure type; however, it is the first one to contain Rb. The same type of ion packing has been found in the isotypic crystal structures of [K(2.2.2)-crypt]3KSn9 (Burns & Corbett, 1985 ▸), [K(2.2.2)-crypt]3K[Co0.68@Sn9] (He et al., 2014b ▸), and [K(2.2.2)-crypt]3K[Ni@Sn9] (Gillett-Kunnath et al., 2011 ▸). This structure type includes both empty Sn9 clusters and Sn9 clusters partly or completely filled with Co and Ni, respectively. As expected, the SnSn bond lengths of the title compound are shorter than those in the filled cluster compounds. However, they are even slightly shorter than those of the empty [Sn9]4– clusters in the potassium analogue [K(2.2.2)-crypt]3KSn9. A similar effect, namely decreasing homoatomic bond lengths with increasing size of the counter-cations, has been found for other homoatomic anions, e.g. [Sn4]4– (Baitinger et al., 1999a ▸,b ▸) and [O3]− (Klein & Jansen, 2000 ▸). In the present case, this effect compensates the increase of inter­atomic distances resulting from the larger ionic radius of Rb+ compared to that of K+, so the unit-cell volume does even decrease slightly from 4186 Å3 (K+; Burns & Corbett, 1985 ▸) to 4166 Å3 (Rb+; title compound).
Figure 1

The main structural components of the title compound, showing a section of the ∞ 1[RbSn9]3− chain. Anisotropic displacement ellipsoids are drawn at the 50% probability level. H atoms of the cryptand mol­ecules have been omitted; labelled sections represent the asymmetric unit.

Supra­molecular features

The [Sn9]4– cluster anions are linked by rubidium cations formally into infinite ∞ 1[RbSn9]3− chains parallel to [001]. The shortest distances between Rb+ cations and Sn9 clusters are similar to those for related compounds, e.g. [Rb(18-crown-6)]2Rb2Sn9·1.5C2N2H8 (3.679 Å; Hauptmann & Fässler, 2002 ▸), [Rb(2.2.2)-crypt][Rb(18-crown-6)]Rb2Sn9·2NH3 (3.708 Å; Gaertner & Korber, 2011 ▸) or Rb12Sn17 (3.582 Å; Hoch et al., 2003 ▸). The dimensionality of structural entities is influenced by the ratio of sequestered to unsequestered cations, and the formation of one-dimensional strands in Zintl phases of nine-atomic clusters with three sequestered cations has been observed previously (Fässler & Hoffmann, 1999 ▸; He et al., 2014a ▸), while a lower content of sequestering agents promotes the formation of double strands (Gaertner & Korber, 2011 ▸), or of a layered arrangement (Hauptmann & Fässler, 2002 ▸, 2003a ▸,b ▸) or double layers (Hauptmann et al., 2001 ▸). A complete coordination of all the cations finally leads to isolated clusters without direct contacts between clusters and cations. In the title compound, the chains form a pseudo-hexa­gonal rod packing separated by the [Rb(2.2.2)-crypt]+ complexes, as can be seen in Fig. 2 ▸ b.
Figure 2

Crystal structure of the title compound: (a) in a view along [110]; (b) in a view along [001]. [Sn9]4– clusters are drawn as polyhedra and Rb+ cations as grey spheres. H atoms of the cryptand mol­ecules have been omitted for clarity.

Database survey

Nine-atomic Zintl cluster compounds and their chemistry have been reviewed by Fässler (2001 ▸) and by Scharfe et al. (2011 ▸). Rb4Sn9 has been crystallized in the presence of sequestering agents previously by Hauptmann & Fässler (2002 ▸) and Gaertner & Korber (2011 ▸). Binary phases of the elements Rb and Sn are known as the Zintl phases including [Sn4]4– clusters, Rb4Sn4 (Baitinger et al., 1999b ▸) and Rb12Sn17 (Hoch et al., 2003 ▸), as well as the clathrate Rb8Sn44 (Dubois & Fässler, 2005 ▸). The structure type of the title compound has been reported previously by Burns & Corbett (1985 ▸), Gillett-Kunnath et al. (2011 ▸) and He et al. (2014b ▸).

Synthesis and crystallization

All manipulations were carried out under anhydrous and oxygen-free conditions using a glove-box or a Schlenk line. Ethyl­enedi­amine (Alfa–Aesar, 99%) and toluene were distilled over CaH2 and stored in a gas-tight Schlenk tube. Cryptand-[2.2.2] (4,7,13,16,21,24-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]-hexa­cosane, Acros, 98%) was dried under vacuum for 8 h. Rb4Sn9 was obtained from a stoichiometric mixture of the elements in a steel container, which was held at 823 K for 3 d under argon in a corundum tube. Rb4Sn9 (65 mg, 0.046 mmol) and cryptand-[2.2.2] (50 mg, 0.13 mmol) were dissolved in 1.5 ml ethyl­enedi­amine in a Schlenk tube. The brown solution was stirred at ambient temperature for 1 h, then filtered and layered with 3.5 ml toluene. The solution was warmed in an oil bath to 323 K for 1 h, then stored at room temperature for crystallization. After 3 d, dark-brown plate-shaped crystals together with a small amount of elemental tin were found on the wall of the glass tube.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1 ▸. All H atoms were included in calculated positions and treated as riding atoms with C—H = 0.99 Å and U iso(H) = 1.2U eq(C). The anisotropic displacement parameters of nine C atoms (C5, C8, C26, C29, C33, C45, C48, C50, C53) had to be restrained using the ISOR option (Sheldrick, 2015 ▸).
Table 1

Experimental details

Crystal data
Chemical formula[Rb(C18H36N2O6)]3RbSn9
M r 2539.55
Crystal system, space groupTriclinic, P
Temperature (K)123
a, b, c (Å)15.7287 (8), 16.153 (1), 20.2896 (8)
α, β, γ (°)98.782 (4), 104.350 (4), 118.407 (6)
V3)4165.4 (4)
Z 2
Radiation typeMo Kα
μ (mm−1)5.03
Crystal size (mm)0.15 × 0.12 × 0.05
 
Data collection
DiffractometerOxford Diffraction Xcalibur 3
Absorption correctionMulti-scan (CrysAlis RED; Oxford Diffraction, 2009)
T min, T max 0.832, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections29013, 15902, 4724
R int 0.112
(sin θ/λ)max−1)0.617
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.054, 0.094, 0.62
No. of reflections15902
No. of parameters823
No. of restraints60
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)2.85, −2.19

Computer programs: CrysAlis CCD and CrysAlis RED (Oxford Diffraction, 2009 ▸), SHELXS97 (Sheldrick, 2008 ▸), SHELXL2014/7 (Sheldrick, 2015 ▸), DIAMOND (Brandenburg, 2012 ▸) and publCIF (Westrip, 2010 ▸).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989017000172/wm5352sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989017000172/wm5352Isup2.hkl Click here for additional data file. Supporting information file. DOI: 10.1107/S2056989017000172/wm5352Isup3.cdx CCDC reference: 1525634 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Rb(C18H36N2O6)]3RbSn9Z = 2
Mr = 2539.55F(000) = 2432
Triclinic, P1Dx = 2.025 Mg m3
a = 15.7287 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.153 (1) ÅCell parameters from 2671 reflections
c = 20.2896 (8) Åθ = 2.9–32.9°
α = 98.782 (4)°µ = 5.03 mm1
β = 104.350 (4)°T = 123 K
γ = 118.407 (6)°Plate, brown
V = 4165.4 (4) Å30.15 × 0.12 × 0.05 mm
Oxford Diffraction Xcalibur 3 diffractometer15902 independent reflections
Radiation source: fine-focus sealed tube4724 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.112
Detector resolution: 16.0238 pixels mm-1θmax = 26.0°, θmin = 2.9°
ω and π scansh = −17→19
Absorption correction: multi-scan (CrysAlisRED; Oxford Diffraction, 2009)k = −19→19
Tmin = 0.832, Tmax = 1.000l = −20→25
29013 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 0.62w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3
15902 reflections(Δ/σ)max = 0.001
823 parametersΔρmax = 2.85 e Å3
60 restraintsΔρmin = −2.19 e Å3
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.
xyzUiso*/Ueq
Sn10.08357 (8)0.16103 (7)0.39428 (5)0.0410 (3)
Sn20.16023 (7)0.25708 (7)0.29264 (5)0.0299 (3)
Sn30.12360 (7)0.07394 (7)0.20224 (5)0.0328 (3)
Sn40.05539 (8)−0.02245 (8)0.30783 (5)0.0416 (3)
Sn5−0.04374 (7)0.21046 (7)0.29624 (5)0.0355 (3)
Sn6−0.01767 (8)0.14432 (7)0.15343 (5)0.0343 (3)
Sn7−0.09899 (8)−0.07686 (7)0.16271 (5)0.0386 (3)
Sn8−0.12916 (8)−0.01594 (7)0.30748 (5)0.0419 (3)
Sn9−0.20912 (8)0.02659 (8)0.17892 (5)0.0430 (3)
Rb10.00000.00000.00000.0586 (7)
Rb20.00000.00000.50000.1214 (13)
Rb30.61092 (10)0.39675 (10)0.17403 (7)0.0318 (4)
N10.4557 (8)0.2336 (7)0.0330 (5)0.028 (3)
N20.7700 (9)0.5604 (9)0.3164 (6)0.039 (3)
O10.5734 (7)0.4486 (7)0.0473 (4)0.039 (3)
O20.7466 (7)0.5961 (6)0.1754 (5)0.042 (3)
O30.3993 (6)0.2728 (6)0.1544 (4)0.031 (2)
O40.5387 (8)0.4516 (7)0.2800 (5)0.042 (3)
O50.6478 (7)0.2466 (7)0.1151 (5)0.043 (3)
O60.7708 (7)0.3809 (7)0.2619 (5)0.042 (3)
C10.4354 (9)0.2790 (9)−0.0236 (6)0.032 (4)
H1A0.38450.2967−0.01850.039*
H1B0.40450.2296−0.07160.039*
C20.5381 (11)0.3749 (11)−0.0178 (7)0.053 (5)
H2A0.59190.3596−0.01850.063*
H2B0.52390.3988−0.05880.063*
C30.6589 (10)0.5372 (10)0.0478 (7)0.035 (4)
H3A0.63630.55820.00700.042*
H3B0.71400.52590.04310.042*
C40.7011 (11)0.6183 (10)0.1191 (7)0.048 (4)
H4A0.75310.68330.11740.058*
H4B0.64350.62310.12660.058*
C50.7826 (11)0.6677 (10)0.2414 (8)0.057 (5)
H5A0.72280.66740.24940.068*
H5B0.83050.73430.23970.068*
C60.8390 (11)0.6477 (10)0.3040 (8)0.056 (5)
H6A0.89380.64060.29340.067*
H6B0.87320.70510.34800.067*
C70.3610 (10)0.1695 (10)0.0410 (7)0.047 (4)
H7A0.37010.12420.06560.057*
H7B0.30610.1284−0.00720.057*
C80.3253 (10)0.2235 (10)0.0829 (7)0.041 (4)
H8A0.32000.27230.06090.049*
H8B0.25600.17580.08270.049*
C90.3669 (10)0.3255 (10)0.1942 (7)0.041 (4)
H9A0.29500.27970.19070.049*
H9B0.36840.37850.17460.049*
C100.4416 (11)0.3711 (11)0.2729 (8)0.047 (4)
H10A0.41190.39420.30340.056*
H10B0.45100.32020.28920.056*
C110.6091 (12)0.4900 (11)0.3483 (7)0.044 (4)
H11A0.62280.43930.36030.053*
H11B0.57970.50720.38200.053*
C120.7103 (12)0.5817 (11)0.3572 (8)0.062 (5)
H12A0.69510.62950.34050.074*
H12B0.75460.61360.40880.074*
C130.4980 (10)0.1743 (10)0.0100 (7)0.046 (5)
H13A0.44020.1099−0.02600.055*
H13B0.54660.2099−0.01320.055*
C140.5522 (10)0.1562 (10)0.0701 (7)0.039 (4)
H14A0.50780.13050.09820.047*
H14B0.56660.10570.05190.047*
C150.7082 (11)0.2306 (10)0.1697 (7)0.049 (5)
H15A0.73270.19110.14820.059*
H15B0.66520.19290.19540.059*
C160.8002 (11)0.3285 (10)0.2217 (7)0.041 (4)
H16A0.84820.31660.25460.049*
H16B0.83790.36920.19480.049*
C170.8587 (11)0.4697 (12)0.3131 (7)0.057 (5)
H17A0.89940.51250.28850.068*
H17B0.90390.45440.34540.068*
C180.8242 (10)0.5226 (11)0.3557 (7)0.043 (4)
H18A0.77840.47650.37620.052*
H18B0.88610.57860.39630.052*
Rb40.63019 (10)0.24191 (10)0.48979 (7)0.0307 (4)
N30.4697 (9)0.2786 (8)0.5135 (6)0.035 (3)
N40.7945 (9)0.2050 (8)0.4680 (5)0.034 (3)
O70.4670 (7)0.2095 (7)0.3686 (4)0.034 (2)
O80.5935 (7)0.1347 (6)0.3462 (4)0.038 (3)
O90.6892 (7)0.4381 (6)0.5596 (4)0.035 (3)
O100.8322 (6)0.4092 (6)0.5085 (4)0.036 (3)
O110.5135 (7)0.1394 (6)0.5733 (5)0.040 (3)
O120.6924 (7)0.1374 (6)0.5723 (4)0.032 (2)
C190.4044 (9)0.2752 (10)0.4456 (6)0.036 (4)
H19A0.44230.33880.43620.043*
H19B0.34000.26730.45020.043*
C200.3762 (11)0.1911 (10)0.3831 (6)0.039 (4)
H20A0.34540.12810.39440.047*
H20B0.32400.18460.34020.047*
C210.4405 (9)0.1419 (9)0.3066 (6)0.031 (4)
H21A0.39620.14800.26600.038*
H21B0.40060.07400.30930.038*
C220.5395 (10)0.1599 (9)0.2945 (7)0.034 (4)
H22A0.52120.11890.24570.040*
H22B0.58440.23060.29890.040*
C230.6872 (10)0.1476 (10)0.3405 (7)0.042 (4)
H23A0.73160.21600.34010.050*
H23B0.67010.10120.29440.050*
C240.7461 (10)0.1303 (9)0.3996 (6)0.031 (4)
H24A0.69840.06560.40400.037*
H24B0.80070.12540.38670.037*
C250.5207 (11)0.3747 (10)0.5659 (7)0.044 (4)
H25A0.54860.37060.61390.053*
H25B0.46840.39210.56650.053*
C260.6076 (10)0.4564 (10)0.5531 (7)0.037 (4)
H26A0.58180.45980.50450.045*
H26B0.63440.52080.58850.045*
C270.7740 (12)0.5146 (10)0.5454 (7)0.051 (5)
H27A0.79950.58090.57750.061*
H27B0.74920.51330.49520.061*
C280.8625 (10)0.4949 (11)0.5584 (7)0.043 (4)
H28A0.92430.55130.55560.051*
H28B0.88190.48940.60710.051*
C290.9102 (10)0.3877 (10)0.5277 (6)0.034 (4)
H29A0.91710.37510.57440.041*
H29B0.97780.44510.53260.041*
C300.8821 (10)0.2979 (10)0.4711 (7)0.043 (4)
H30A0.86570.30820.42380.052*
H30B0.94340.29210.47960.052*
C310.4037 (10)0.2025 (11)0.5402 (7)0.046 (4)
H31A0.35600.13960.49990.055*
H31B0.36060.22300.55710.055*
C320.4622 (11)0.1839 (11)0.5995 (7)0.039 (4)
H32A0.51450.24730.63850.046*
H32B0.41370.13900.61920.046*
C330.5677 (11)0.1164 (10)0.6260 (7)0.040 (4)
H33A0.51830.06880.64380.048*
H33B0.61990.17750.66700.048*
C340.6205 (10)0.0730 (10)0.5979 (7)0.035 (4)
H34A0.65710.05750.63650.042*
H34B0.56800.01010.55850.042*
C350.7387 (12)0.0917 (11)0.5435 (7)0.050 (5)
H35A0.68560.03410.50030.060*
H35B0.76770.06750.57930.060*
C360.8262 (10)0.1680 (10)0.5237 (7)0.036 (4)
H36A0.87740.22530.56750.044*
H36B0.86240.13710.50830.044*
Rb50.76177 (10)0.32954 (9)0.86626 (7)0.0300 (4)
N50.7359 (9)0.1513 (8)0.9045 (6)0.041 (3)
N60.7851 (8)0.5051 (8)0.8284 (6)0.031 (3)
O130.8244 (7)0.2143 (6)0.7948 (5)0.037 (3)
O140.8891 (6)0.4026 (6)0.7829 (5)0.033 (2)
O150.5564 (6)0.1735 (6)0.8469 (4)0.033 (2)
O160.5787 (6)0.3200 (6)0.7796 (4)0.034 (2)
O170.8618 (7)0.3529 (7)1.0154 (4)0.036 (3)
O180.8401 (6)0.5092 (6)0.9782 (4)0.032 (2)
C370.7556 (11)0.0977 (10)0.8552 (7)0.040 (4)
H37A0.69080.05510.81240.048*
H37B0.77030.05290.87730.048*
C380.8434 (12)0.1553 (10)0.8296 (8)0.049 (5)
H38A0.90990.19690.87120.058*
H38B0.84970.10820.79680.058*
C390.8988 (11)0.2580 (10)0.7645 (7)0.041 (4)
H39A0.89230.20600.72690.049*
H39B0.96940.29320.80190.049*
C400.8837 (10)0.3292 (10)0.7326 (6)0.035 (4)
H40A0.93770.36090.71220.041*
H40B0.81510.29260.69300.041*
C410.8807 (10)0.4729 (11)0.7549 (7)0.043 (4)
H41A0.81690.43880.71130.051*
H41B0.94100.50930.74090.051*
C420.8769 (10)0.5446 (10)0.8074 (7)0.039 (4)
H42A0.93980.57580.85130.047*
H42B0.88080.59770.78710.047*
C430.6326 (10)0.0921 (9)0.9057 (6)0.033 (4)
H43A0.63090.12350.95090.039*
H43B0.61870.02560.90590.039*
C440.5489 (10)0.0800 (10)0.8449 (7)0.036 (4)
H44A0.55270.05260.79940.043*
H44B0.48070.03200.84620.043*
C450.4793 (10)0.1614 (9)0.7896 (7)0.037 (4)
H45A0.41090.11430.79100.044*
H45B0.48330.13240.74460.044*
C460.4873 (9)0.2567 (9)0.7893 (6)0.030 (4)
H46A0.42640.24420.75020.036*
H46B0.48780.28820.83540.036*
C470.5921 (10)0.4135 (9)0.7803 (6)0.028 (4)
H47A0.59510.44680.82680.034*
H47B0.53300.40450.74150.034*
C480.6920 (9)0.4754 (9)0.7695 (6)0.027 (3)
H48A0.69040.43740.72550.032*
H48B0.69590.53580.76140.032*
C490.8130 (10)0.1830 (11)0.9768 (8)0.044 (4)
H49A0.79330.12450.99370.053*
H49B0.88150.20530.97270.053*
C500.8251 (11)0.2625 (10)1.0317 (7)0.044 (4)
H50A0.75720.24101.03660.052*
H50B0.87460.27401.07840.052*
C510.8655 (11)0.4296 (11)1.0631 (7)0.050 (5)
H51A0.90810.44171.11270.060*
H51B0.79420.40771.06120.060*
C520.9099 (11)0.5238 (10)1.0454 (8)0.049 (5)
H52A0.91970.57761.08330.058*
H52B0.97850.54321.04260.058*
C530.8794 (10)0.5975 (8)0.9598 (6)0.027 (3)
H53A0.94730.61720.95560.033*
H53B0.88990.65170.99780.033*
C540.8060 (10)0.5816 (10)0.8918 (7)0.040 (4)
H54A0.83250.64550.88150.048*
H54B0.73910.56300.89750.048*
U11U22U33U12U13U23
Sn10.0433 (7)0.0303 (7)0.0357 (6)0.0122 (6)0.0073 (5)0.0139 (5)
Sn20.0253 (6)0.0228 (6)0.0318 (6)0.0083 (5)0.0088 (5)0.0032 (5)
Sn30.0321 (7)0.0283 (6)0.0368 (6)0.0170 (5)0.0111 (5)0.0071 (5)
Sn40.0408 (7)0.0433 (7)0.0478 (7)0.0261 (6)0.0149 (6)0.0223 (6)
Sn50.0318 (7)0.0330 (7)0.0396 (7)0.0195 (6)0.0094 (5)0.0050 (5)
Sn60.0375 (7)0.0319 (6)0.0299 (6)0.0185 (6)0.0077 (5)0.0088 (5)
Sn70.0331 (7)0.0208 (6)0.0463 (7)0.0102 (5)0.0050 (5)0.0025 (5)
Sn80.0334 (7)0.0333 (7)0.0536 (7)0.0129 (6)0.0171 (6)0.0161 (6)
Sn90.0251 (6)0.0373 (7)0.0527 (7)0.0137 (6)0.0043 (5)0.0069 (6)
Rb10.0697 (18)0.0670 (17)0.0312 (13)0.0357 (15)0.0161 (12)0.0037 (12)
Rb20.095 (2)0.167 (3)0.126 (3)0.064 (2)0.052 (2)0.112 (2)
Rb30.0273 (9)0.0260 (8)0.0358 (9)0.0116 (7)0.0087 (7)0.0083 (7)
N10.033 (8)0.014 (7)0.030 (7)0.010 (6)0.013 (6)−0.001 (6)
N20.022 (8)0.045 (9)0.036 (8)0.008 (7)0.012 (6)0.010 (7)
O10.051 (7)0.040 (7)0.025 (6)0.020 (6)0.022 (5)0.011 (5)
O20.037 (6)0.035 (6)0.031 (6)0.008 (5)0.004 (5)0.010 (5)
O30.041 (6)0.029 (6)0.029 (6)0.026 (5)0.009 (5)0.000 (5)
O40.047 (7)0.053 (7)0.026 (6)0.027 (6)0.008 (5)0.017 (5)
O50.042 (7)0.041 (7)0.033 (6)0.014 (6)0.010 (5)0.011 (5)
O60.033 (6)0.056 (7)0.034 (6)0.029 (6)0.006 (5)0.003 (6)
C10.013 (8)0.017 (8)0.035 (9)−0.009 (7)0.001 (7)0.003 (7)
C20.062 (12)0.068 (13)0.038 (10)0.042 (11)0.023 (9)0.007 (10)
C30.048 (10)0.034 (9)0.045 (10)0.028 (9)0.023 (8)0.034 (8)
C40.045 (11)0.035 (10)0.055 (11)0.017 (9)0.013 (9)0.018 (9)
C50.058 (8)0.030 (7)0.064 (8)0.012 (6)0.016 (7)0.017 (7)
C60.036 (11)0.036 (10)0.062 (12)−0.003 (9)0.012 (9)0.017 (9)
C70.029 (10)0.033 (10)0.043 (10)−0.003 (8)0.008 (8)−0.006 (8)
C80.023 (7)0.037 (7)0.047 (8)0.011 (6)0.006 (6)0.007 (6)
C90.037 (10)0.029 (9)0.047 (10)0.012 (8)0.003 (8)0.026 (8)
C100.055 (12)0.051 (11)0.070 (12)0.044 (10)0.045 (10)0.021 (10)
C110.076 (13)0.060 (12)0.040 (10)0.062 (11)0.026 (10)0.026 (9)
C120.053 (13)0.045 (12)0.063 (12)0.021 (11)−0.005 (10)0.019 (10)
C130.020 (9)0.030 (10)0.054 (11)−0.005 (8)0.000 (8)0.018 (9)
C140.046 (11)0.036 (10)0.037 (9)0.020 (9)0.027 (8)0.007 (8)
C150.047 (11)0.050 (11)0.048 (10)0.019 (9)0.017 (9)0.034 (9)
C160.044 (11)0.037 (10)0.032 (9)0.011 (9)0.018 (8)0.018 (8)
C170.049 (12)0.071 (13)0.044 (11)0.044 (11)−0.012 (9)0.010 (10)
C180.030 (10)0.052 (11)0.036 (10)0.020 (9)0.001 (8)0.012 (9)
Rb40.0284 (9)0.0277 (9)0.0312 (8)0.0145 (7)0.0075 (7)0.0053 (7)
N30.051 (9)0.028 (7)0.040 (8)0.028 (7)0.018 (7)0.021 (7)
N40.058 (9)0.025 (7)0.020 (7)0.018 (7)0.022 (6)0.012 (6)
O70.038 (7)0.045 (7)0.021 (6)0.025 (6)0.010 (5)0.008 (5)
O80.053 (7)0.037 (6)0.036 (6)0.033 (6)0.014 (5)0.015 (5)
O90.030 (6)0.019 (6)0.046 (6)0.009 (5)0.007 (5)0.005 (5)
O100.025 (6)0.019 (6)0.032 (6)0.001 (5)−0.005 (5)−0.006 (5)
O110.040 (7)0.031 (6)0.036 (6)0.011 (5)0.014 (5)0.005 (5)
O120.033 (6)0.022 (6)0.038 (6)0.007 (5)0.017 (5)0.016 (5)
C190.018 (8)0.056 (11)0.026 (8)0.020 (8)0.003 (7)0.001 (8)
C200.045 (11)0.044 (10)0.023 (9)0.030 (9)−0.001 (8)0.001 (8)
C210.027 (9)0.022 (8)0.024 (8)0.000 (7)0.011 (7)−0.001 (7)
C220.029 (9)0.019 (8)0.046 (10)0.013 (7)0.008 (8)0.003 (8)
C230.028 (10)0.037 (10)0.064 (11)0.012 (8)0.036 (9)0.016 (9)
C240.035 (9)0.031 (9)0.035 (9)0.020 (8)0.015 (7)0.019 (8)
C250.051 (11)0.042 (10)0.039 (9)0.034 (10)0.005 (8)−0.004 (9)
C260.043 (8)0.033 (7)0.041 (7)0.032 (6)0.005 (6)−0.001 (6)
C270.066 (13)0.016 (9)0.035 (9)0.015 (9)−0.014 (9)0.003 (8)
C280.023 (9)0.039 (10)0.046 (10)0.007 (8)0.005 (8)0.011 (9)
C290.041 (8)0.034 (7)0.024 (7)0.012 (6)0.017 (6)0.020 (6)
C300.042 (10)0.042 (10)0.056 (11)0.017 (9)0.037 (9)0.032 (9)
C310.031 (10)0.056 (11)0.039 (10)0.019 (9)0.011 (8)0.000 (9)
C320.046 (10)0.048 (11)0.032 (9)0.025 (9)0.028 (8)0.016 (8)
C330.041 (8)0.044 (8)0.019 (7)0.012 (6)0.016 (6)0.005 (6)
C340.024 (9)0.036 (10)0.041 (9)0.015 (8)0.007 (7)0.014 (8)
C350.082 (14)0.049 (11)0.039 (10)0.046 (11)0.027 (9)0.017 (9)
C360.053 (11)0.037 (10)0.043 (10)0.039 (9)0.022 (8)0.015 (8)
Rb50.0317 (9)0.0231 (8)0.0315 (8)0.0122 (7)0.0120 (7)0.0075 (7)
N50.037 (8)0.023 (7)0.035 (8)0.007 (7)−0.001 (7)−0.007 (6)
N60.029 (8)0.032 (8)0.045 (8)0.024 (6)0.014 (6)0.021 (7)
O130.037 (6)0.019 (6)0.056 (7)0.013 (5)0.025 (5)0.010 (5)
O140.039 (6)0.024 (6)0.048 (6)0.028 (5)0.011 (5)0.010 (5)
O150.017 (5)0.038 (6)0.030 (6)0.010 (5)0.000 (4)0.008 (5)
O160.027 (6)0.028 (6)0.042 (6)0.015 (5)0.011 (5)0.007 (5)
O170.048 (7)0.039 (6)0.017 (5)0.024 (6)0.010 (5)0.000 (5)
O180.041 (6)0.019 (6)0.026 (6)0.013 (5)0.004 (5)0.004 (5)
C370.053 (11)0.037 (10)0.053 (11)0.035 (9)0.034 (9)0.013 (9)
C380.073 (13)0.026 (10)0.057 (11)0.038 (10)0.022 (10)0.001 (9)
C390.041 (10)0.023 (9)0.042 (10)0.007 (8)0.017 (8)−0.001 (8)
C400.042 (10)0.029 (9)0.024 (8)0.012 (8)0.016 (7)0.006 (7)
C410.040 (10)0.065 (12)0.042 (10)0.041 (10)0.016 (8)0.018 (9)
C420.018 (9)0.031 (9)0.060 (11)0.013 (8)0.002 (8)0.015 (8)
C430.042 (10)0.022 (8)0.014 (8)0.002 (8)0.007 (7)0.009 (7)
C440.055 (11)0.033 (9)0.043 (10)0.031 (9)0.034 (9)0.021 (8)
C450.031 (7)0.017 (7)0.052 (8)0.002 (5)0.023 (6)0.007 (6)
C460.009 (8)0.039 (10)0.022 (8)0.001 (7)0.002 (6)0.011 (7)
C470.035 (9)0.016 (8)0.029 (8)0.014 (7)0.007 (7)0.003 (7)
C480.032 (7)0.023 (7)0.033 (7)0.023 (6)0.005 (5)0.011 (5)
C490.039 (10)0.061 (12)0.076 (12)0.040 (9)0.042 (9)0.050 (10)
C500.052 (8)0.028 (7)0.055 (8)0.026 (6)0.010 (6)0.024 (6)
C510.029 (10)0.084 (14)0.025 (9)0.023 (10)0.007 (8)0.022 (10)
C520.055 (11)0.025 (9)0.063 (12)0.014 (9)0.026 (10)0.027 (9)
C530.036 (7)0.010 (6)0.029 (7)0.006 (5)0.017 (6)0.003 (5)
C540.033 (10)0.036 (10)0.050 (10)0.016 (8)0.010 (8)0.029 (9)
Sn1—Sn22.9229 (14)O11—C331.407 (14)
Sn1—Sn52.9387 (14)O11—C321.448 (14)
Sn1—Sn42.9724 (15)O12—C341.403 (14)
Sn1—Sn82.9850 (14)O12—C351.416 (15)
Sn1—Rb23.5976 (10)C19—C201.508 (15)
Sn1—Sn34.2360 (14)C19—H19A0.9900
Sn2—Sn32.9404 (14)C19—H19B0.9900
Sn2—Sn52.9493 (14)C20—H20A0.9900
Sn2—Sn62.9644 (13)C20—H20B0.9900
Sn2—Sn44.0981 (14)C21—C221.533 (16)
Sn3—Sn72.9549 (14)C21—H21A0.9900
Sn3—Sn42.9552 (14)C21—H21B0.9900
Sn3—Sn62.9777 (14)C22—H22A0.9900
Sn3—Rb13.7925 (9)C22—H22B0.9900
Sn4—Sn82.9527 (15)C23—C241.472 (15)
Sn4—Sn72.9957 (14)C23—H23A0.9900
Sn4—Rb24.2008 (11)C23—H23B0.9900
Sn5—Sn92.9453 (14)C24—H24A0.9900
Sn5—Sn63.1249 (14)C24—H24B0.9900
Sn5—Sn83.3110 (15)C25—C261.496 (17)
Sn6—Sn92.9283 (15)C25—H25A0.9900
Sn6—Sn73.2267 (14)C25—H25B0.9900
Sn6—Rb13.7460 (10)C26—H26A0.9900
Sn7—Sn92.9613 (15)C26—H26B0.9900
Sn7—Sn83.1741 (15)C27—C281.540 (17)
Sn7—Rb14.1017 (11)C27—H27A0.9900
Sn8—Sn92.9327 (14)C27—H27B0.9900
Sn8—Rb23.8357 (10)C28—H28A0.9900
Rb3—O32.830 (9)C28—H28B0.9900
Rb3—O12.834 (8)C29—C301.499 (16)
Rb3—O62.847 (9)C29—H29A0.9900
Rb3—O42.877 (9)C29—H29B0.9900
Rb3—O22.886 (9)C30—H30A0.9900
Rb3—O52.907 (10)C30—H30B0.9900
Rb3—N13.034 (10)C31—C321.487 (16)
Rb3—N23.063 (11)C31—H31A0.9900
N1—C71.422 (15)C31—H31B0.9900
N1—C131.483 (16)C32—H32A0.9900
N1—C11.502 (14)C32—H32B0.9900
N2—C61.420 (15)C33—C341.474 (17)
N2—C181.430 (15)C33—H33A0.9900
N2—C121.514 (18)C33—H33B0.9900
O1—C21.413 (14)C34—H34A0.9900
O1—C31.420 (13)C34—H34B0.9900
O2—C41.382 (13)C35—C361.545 (17)
O2—C51.407 (14)C35—H35A0.9900
O3—C81.423 (12)C35—H35B0.9900
O3—C91.429 (15)C36—H36A0.9900
O4—C111.362 (13)C36—H36B0.9900
O4—C101.411 (15)Rb5—O132.858 (9)
O5—C151.411 (13)Rb5—O152.875 (8)
O5—C141.432 (13)Rb5—O182.880 (8)
O6—C161.392 (15)Rb5—O142.882 (9)
O6—C171.412 (15)Rb5—O162.897 (8)
C1—C21.579 (16)Rb5—O172.915 (8)
C1—H1A0.9900Rb5—N62.929 (10)
C1—H1B0.9900Rb5—N52.963 (11)
C2—H2A0.9900N5—C371.411 (14)
C2—H2B0.9900N5—C431.451 (15)
C3—C41.539 (16)N5—C491.477 (14)
C3—H3A0.9900N6—C481.446 (13)
C3—H3B0.9900N6—C421.479 (15)
C4—H4A0.9900N6—C541.487 (15)
C4—H4B0.9900O13—C381.367 (14)
C5—C61.532 (16)O13—C391.396 (14)
C5—H5A0.9900O14—C411.389 (14)
C5—H5B0.9900O14—C401.396 (13)
C6—H6A0.9900O15—C451.366 (13)
C6—H6B0.9900O15—C441.452 (13)
C7—C81.508 (17)O16—C461.398 (13)
C7—H7A0.9900O16—C471.419 (13)
C7—H7B0.9900O17—C511.419 (15)
C8—H8A0.9900O17—C501.420 (14)
C8—H8B0.9900O18—C531.412 (13)
C9—C101.537 (15)O18—C521.427 (13)
C9—H9A0.9900C37—C381.524 (17)
C9—H9B0.9900C37—H37A0.9900
C10—H10A0.9900C37—H37B0.9900
C10—H10B0.9900C38—H38A0.9900
C11—C121.514 (18)C38—H38B0.9900
C11—H11A0.9900C39—C401.486 (16)
C11—H11B0.9900C39—H39A0.9900
C12—H12A0.9900C39—H39B0.9900
C12—H12B0.9900C40—H40A0.9900
C13—C141.460 (15)C40—H40B0.9900
C13—H13A0.9900C41—C421.483 (16)
C13—H13B0.9900C41—H41A0.9900
C14—H14A0.9900C41—H41B0.9900
C14—H14B0.9900C42—H42A0.9900
C15—C161.504 (16)C42—H42B0.9900
C15—H15A0.9900C43—C441.472 (15)
C15—H15B0.9900C43—H43A0.9900
C16—H16A0.9900C43—H43B0.9900
C16—H16B0.9900C44—H44A0.9900
C17—C181.492 (17)C44—H44B0.9900
C17—H17A0.9900C45—C461.484 (16)
C17—H17B0.9900C45—H45A0.9900
C18—H18A0.9900C45—H45B0.9900
C18—H18B0.9900C46—H46A0.9900
Rb4—O92.845 (8)C46—H46B0.9900
Rb4—O72.848 (8)C47—C481.504 (15)
Rb4—O122.869 (8)C47—H47A0.9900
Rb4—O102.909 (8)C47—H47B0.9900
Rb4—O112.914 (9)C48—H48A0.9900
Rb4—O82.914 (9)C48—H48B0.9900
Rb4—N32.983 (11)C49—C501.466 (16)
Rb4—N43.030 (12)C49—H49A0.9900
N3—C251.440 (14)C49—H49B0.9900
N3—C311.465 (15)C50—H50A0.9900
N3—C191.476 (13)C50—H50B0.9900
N4—C241.433 (14)C51—C521.488 (17)
N4—C361.447 (13)C51—H51A0.9900
N4—C301.455 (14)C51—H51B0.9900
O7—C211.355 (12)C52—H52A0.9900
O7—C201.431 (15)C52—H52B0.9900
O8—C221.415 (13)C53—C541.457 (14)
O8—C231.425 (14)C53—H53A0.9900
O9—C261.428 (13)C53—H53B0.9900
O9—C271.456 (15)C54—H54A0.9900
O10—C281.370 (14)C54—H54B0.9900
O10—C291.411 (14)
Sn2—Sn1—Sn560.42 (3)O9—Rb4—O8135.0 (3)
Sn2—Sn1—Sn488.07 (4)O7—Rb4—O859.5 (3)
Sn5—Sn1—Sn4106.08 (4)O12—Rb4—O8100.6 (2)
Sn2—Sn1—Sn8105.93 (4)O10—Rb4—O894.1 (3)
Sn5—Sn1—Sn867.96 (3)O11—Rb4—O8120.8 (2)
Sn4—Sn1—Sn859.42 (3)O9—Rb4—N360.5 (3)
Sn2—Sn1—Rb2166.42 (4)O7—Rb4—N361.1 (3)
Sn5—Sn1—Rb2126.75 (4)O12—Rb4—N3118.4 (3)
Sn4—Sn1—Rb278.86 (3)O10—Rb4—N3119.4 (3)
Sn8—Sn1—Rb270.58 (3)O11—Rb4—N360.7 (3)
Sn2—Sn1—Sn343.91 (3)O8—Rb4—N3119.3 (3)
Sn5—Sn1—Sn379.76 (3)O9—Rb4—N4119.3 (3)
Sn4—Sn1—Sn344.23 (3)O7—Rb4—N4119.7 (3)
Sn8—Sn1—Sn379.25 (3)O12—Rb4—N461.0 (3)
Rb2—Sn1—Sn3123.08 (3)O10—Rb4—N460.6 (3)
Sn1—Sn2—Sn392.51 (4)O11—Rb4—N4118.7 (3)
Sn1—Sn2—Sn560.06 (3)O8—Rb4—N461.5 (3)
Sn3—Sn2—Sn5106.10 (4)N3—Rb4—N4179.2 (3)
Sn1—Sn2—Sn6105.01 (4)C25—N3—C31109.2 (11)
Sn3—Sn2—Sn660.57 (3)C25—N3—C19109.6 (10)
Sn5—Sn2—Sn663.80 (3)C31—N3—C19109.2 (11)
Sn1—Sn2—Sn446.46 (3)C25—N3—Rb4109.1 (8)
Sn3—Sn2—Sn446.11 (3)C31—N3—Rb4109.7 (8)
Sn5—Sn2—Sn482.44 (3)C19—N3—Rb4110.1 (8)
Sn6—Sn2—Sn481.83 (3)C24—N4—C36109.4 (10)
Sn2—Sn3—Sn7105.68 (4)C24—N4—C30112.4 (10)
Sn2—Sn3—Sn488.07 (4)C36—N4—C30110.9 (11)
Sn7—Sn3—Sn460.91 (3)C24—N4—Rb4106.5 (8)
Sn2—Sn3—Sn660.12 (3)C36—N4—Rb4108.9 (8)
Sn7—Sn3—Sn665.90 (3)C30—N4—Rb4108.5 (8)
Sn4—Sn3—Sn6104.91 (4)C21—O7—C20110.4 (9)
Sn2—Sn3—Rb1119.31 (3)C21—O7—Rb4116.7 (8)
Sn7—Sn3—Rb173.70 (3)C20—O7—Rb4113.2 (7)
Sn4—Sn3—Rb1132.27 (4)C22—O8—C23114.9 (11)
Sn6—Sn3—Rb165.91 (3)C22—O8—Rb4109.8 (7)
Sn2—Sn3—Sn143.58 (3)C23—O8—Rb4111.3 (7)
Sn7—Sn3—Sn180.14 (3)C26—O9—C27111.2 (10)
Sn4—Sn3—Sn144.55 (3)C26—O9—Rb4117.0 (7)
Sn6—Sn3—Sn178.59 (3)C27—O9—Rb4113.6 (7)
Rb1—Sn3—Sn1142.08 (3)C28—O10—C29108.5 (10)
Sn8—Sn4—Sn3105.57 (4)C28—O10—Rb4113.6 (8)
Sn8—Sn4—Sn160.50 (4)C29—O10—Rb4111.3 (7)
Sn3—Sn4—Sn191.22 (4)C33—O11—C32113.4 (10)
Sn8—Sn4—Sn764.49 (4)C33—O11—Rb4114.6 (8)
Sn3—Sn4—Sn759.54 (3)C32—O11—Rb4114.0 (8)
Sn1—Sn4—Sn7104.90 (4)C34—O12—C35110.2 (10)
Sn8—Sn4—Sn282.24 (3)C34—O12—Rb4117.2 (7)
Sn3—Sn4—Sn245.81 (3)C35—O12—Rb4116.1 (8)
Sn1—Sn4—Sn245.47 (3)N3—C19—C20111.9 (11)
Sn7—Sn4—Sn281.35 (3)N3—C19—H19A109.2
Sn8—Sn4—Rb261.98 (3)C20—C19—H19A109.2
Sn3—Sn4—Rb2148.37 (4)N3—C19—H19B109.2
Sn1—Sn4—Rb257.17 (3)C20—C19—H19B109.2
Sn7—Sn4—Rb2125.08 (4)H19A—C19—H19B107.9
Sn2—Sn4—Rb2102.56 (3)O7—C20—C19109.9 (11)
Sn1—Sn5—Sn9107.87 (4)O7—C20—H20A109.7
Sn1—Sn5—Sn259.53 (3)C19—C20—H20A109.7
Sn9—Sn5—Sn2109.20 (4)O7—C20—H20B109.7
Sn1—Sn5—Sn6100.73 (4)C19—C20—H20B109.7
Sn9—Sn5—Sn657.60 (3)H20A—C20—H20B108.2
Sn2—Sn5—Sn658.34 (3)O7—C21—C22109.2 (10)
Sn1—Sn5—Sn856.68 (3)O7—C21—H21A109.8
Sn9—Sn5—Sn855.54 (3)C22—C21—H21A109.8
Sn2—Sn5—Sn897.60 (4)O7—C21—H21B109.8
Sn6—Sn5—Sn889.13 (4)C22—C21—H21B109.8
Sn9—Sn6—Sn2109.25 (4)H21A—C21—H21B108.3
Sn9—Sn6—Sn3108.76 (4)O8—C22—C21109.2 (11)
Sn2—Sn6—Sn359.32 (3)O8—C22—H22A109.8
Sn9—Sn6—Sn558.12 (3)C21—C22—H22A109.8
Sn2—Sn6—Sn557.87 (3)O8—C22—H22B109.8
Sn3—Sn6—Sn5100.91 (4)C21—C22—H22B109.8
Sn9—Sn6—Sn757.27 (3)H22A—C22—H22B108.3
Sn2—Sn6—Sn798.65 (4)O8—C23—C24113.0 (11)
Sn3—Sn6—Sn756.71 (3)O8—C23—H23A109.0
Sn5—Sn6—Sn791.74 (4)C24—C23—H23A109.0
Sn9—Sn6—Rb1112.40 (3)O8—C23—H23B109.0
Sn2—Sn6—Rb1120.07 (4)C24—C23—H23B109.0
Sn3—Sn6—Rb167.56 (3)H23A—C23—H23B107.8
Sn5—Sn6—Rb1163.05 (4)N4—C24—C23115.1 (11)
Sn7—Sn6—Rb171.63 (3)N4—C24—H24A108.5
Sn3—Sn7—Sn9108.48 (4)C23—C24—H24A108.5
Sn3—Sn7—Sn459.55 (3)N4—C24—H24B108.5
Sn9—Sn7—Sn4107.75 (4)C23—C24—H24B108.5
Sn3—Sn7—Sn8100.23 (4)H24A—C24—H24B107.5
Sn9—Sn7—Sn856.98 (3)N3—C25—C26114.6 (12)
Sn4—Sn7—Sn857.10 (3)N3—C25—H25A108.6
Sn3—Sn7—Sn657.39 (3)C26—C25—H25A108.6
Sn9—Sn7—Sn656.29 (3)N3—C25—H25B108.6
Sn4—Sn7—Sn698.16 (4)C26—C25—H25B108.6
Sn8—Sn7—Sn689.80 (4)H25A—C25—H25B107.6
Sn3—Sn7—Rb162.56 (3)O9—C26—C25109.6 (11)
Sn9—Sn7—Rb1102.78 (3)O9—C26—H26A109.8
Sn4—Sn7—Rb1120.29 (4)C25—C26—H26A109.8
Sn8—Sn7—Rb1149.75 (4)O9—C26—H26B109.8
Sn6—Sn7—Rb160.08 (2)C25—C26—H26B109.8
Sn9—Sn8—Sn4109.68 (4)H26A—C26—H26B108.2
Sn9—Sn8—Sn1106.97 (4)O9—C27—C28108.7 (10)
Sn4—Sn8—Sn160.08 (4)O9—C27—H27A109.9
Sn9—Sn8—Sn757.85 (3)C28—C27—H27A109.9
Sn4—Sn8—Sn758.41 (3)O9—C27—H27B109.9
Sn1—Sn8—Sn7100.35 (4)C28—C27—H27B109.9
Sn9—Sn8—Sn555.90 (3)H27A—C27—H27B108.3
Sn4—Sn8—Sn597.73 (4)O10—C28—C27110.6 (11)
Sn1—Sn8—Sn555.36 (3)O10—C28—H28A109.5
Sn7—Sn8—Sn589.32 (4)C27—C28—H28A109.5
Sn9—Sn8—Rb2164.75 (4)O10—C28—H28B109.5
Sn4—Sn8—Rb275.20 (3)C27—C28—H28B109.5
Sn1—Sn8—Rb262.20 (3)H28A—C28—H28B108.1
Sn7—Sn8—Rb2132.01 (4)O10—C29—C30109.4 (11)
Sn5—Sn8—Rb2109.68 (3)O10—C29—H29A109.8
Sn6—Sn9—Sn8100.87 (4)C30—C29—H29A109.8
Sn6—Sn9—Sn564.28 (3)O10—C29—H29B109.8
Sn8—Sn9—Sn568.57 (3)C30—C29—H29B109.8
Sn6—Sn9—Sn766.44 (4)H29A—C29—H29B108.2
Sn8—Sn9—Sn765.17 (4)N4—C30—C29114.8 (11)
Sn5—Sn9—Sn7101.06 (4)N4—C30—H30A108.6
Sn6—Rb1—Sn6i180.0C29—C30—H30A108.6
Sn6—Rb1—Sn346.53 (2)N4—C30—H30B108.6
Sn6i—Rb1—Sn3133.47 (2)C29—C30—H30B108.6
Sn6—Rb1—Sn3i133.47 (2)H30A—C30—H30B107.5
Sn6i—Rb1—Sn3i46.53 (2)N3—C31—C32114.2 (11)
Sn3—Rb1—Sn3i180.0N3—C31—H31A108.7
Sn6—Rb1—Sn748.29 (2)C32—C31—H31A108.7
Sn6i—Rb1—Sn7131.71 (2)N3—C31—H31B108.7
Sn3—Rb1—Sn743.75 (2)C32—C31—H31B108.7
Sn3i—Rb1—Sn7136.26 (2)H31A—C31—H31B107.6
Sn6—Rb1—Sn7i131.71 (2)O11—C32—C31110.0 (11)
Sn6i—Rb1—Sn7i48.29 (2)O11—C32—H32A109.7
Sn3—Rb1—Sn7i136.25 (2)C31—C32—H32A109.7
Sn3i—Rb1—Sn7i43.75 (2)O11—C32—H32B109.7
Sn7—Rb1—Sn7i180.0C31—C32—H32B109.7
Sn1—Rb2—Sn1ii180.0H32A—C32—H32B108.2
Sn1—Rb2—Sn8ii132.78 (2)O11—C33—C34111.9 (11)
Sn1ii—Rb2—Sn8ii47.22 (2)O11—C33—H33A109.2
Sn1—Rb2—Sn847.22 (2)C34—C33—H33A109.2
Sn1ii—Rb2—Sn8132.78 (2)O11—C33—H33B109.2
Sn8ii—Rb2—Sn8180.0C34—C33—H33B109.2
Sn1—Rb2—Sn4ii136.03 (2)H33A—C33—H33B107.9
Sn1ii—Rb2—Sn4ii43.97 (2)O12—C34—C33112.0 (11)
Sn8ii—Rb2—Sn4ii42.81 (2)O12—C34—H34A109.2
Sn8—Rb2—Sn4ii137.19 (2)C33—C34—H34A109.2
Sn1—Rb2—Sn443.97 (2)O12—C34—H34B109.2
Sn1ii—Rb2—Sn4136.03 (2)C33—C34—H34B109.2
Sn8ii—Rb2—Sn4137.19 (2)H34A—C34—H34B107.9
Sn8—Rb2—Sn442.81 (2)O12—C35—C36109.2 (11)
Sn4ii—Rb2—Sn4180.0O12—C35—H35A109.8
O3—Rb3—O196.0 (3)C36—C35—H35A109.8
O3—Rb3—O6122.5 (3)O12—C35—H35B109.8
O1—Rb3—O6136.2 (3)C36—C35—H35B109.8
O3—Rb3—O461.8 (3)H35A—C35—H35B108.3
O1—Rb3—O4117.3 (3)N4—C36—C35116.3 (11)
O6—Rb3—O4100.2 (3)N4—C36—H36A108.2
O3—Rb3—O2137.2 (3)C35—C36—H36A108.2
O1—Rb3—O260.4 (3)N4—C36—H36B108.2
O6—Rb3—O295.8 (3)C35—C36—H36B108.2
O4—Rb3—O295.9 (3)H36A—C36—H36B107.4
O3—Rb3—O599.3 (2)O13—Rb5—O1599.4 (3)
O1—Rb3—O595.7 (3)O13—Rb5—O18143.0 (3)
O6—Rb3—O560.9 (3)O15—Rb5—O18113.2 (3)
O4—Rb3—O5142.3 (3)O13—Rb5—O1458.0 (3)
O2—Rb3—O5117.0 (3)O15—Rb5—O14139.6 (2)
O3—Rb3—N159.1 (3)O18—Rb5—O14101.6 (2)
O1—Rb3—N160.9 (3)O13—Rb5—O16115.9 (2)
O6—Rb3—N1119.4 (3)O15—Rb5—O1658.8 (2)
O4—Rb3—N1120.0 (3)O18—Rb5—O1696.4 (2)
O2—Rb3—N1120.3 (3)O14—Rb5—O1698.7 (2)
O5—Rb3—N159.7 (3)O13—Rb5—O17100.7 (3)
O3—Rb3—N2121.5 (3)O15—Rb5—O1796.8 (2)
O1—Rb3—N2119.4 (3)O18—Rb5—O1759.8 (3)
O6—Rb3—N259.8 (3)O14—Rb5—O17118.8 (2)
O4—Rb3—N260.8 (3)O16—Rb5—O17137.8 (3)
O2—Rb3—N259.8 (3)O13—Rb5—N6119.2 (3)
O5—Rb3—N2119.5 (3)O15—Rb5—N6117.9 (3)
N1—Rb3—N2179.1 (3)O18—Rb5—N660.5 (3)
C7—N1—C13108.6 (10)O14—Rb5—N662.6 (3)
C7—N1—C1109.7 (11)O16—Rb5—N660.9 (3)
C13—N1—C1108.9 (11)O17—Rb5—N6118.8 (3)
C7—N1—Rb3110.1 (7)O13—Rb5—N561.3 (3)
C13—N1—Rb3110.0 (8)O15—Rb5—N561.5 (3)
C1—N1—Rb3109.5 (7)O18—Rb5—N5119.5 (3)
C6—N2—C18111.6 (11)O14—Rb5—N5117.9 (3)
C6—N2—C12110.1 (13)O16—Rb5—N5118.5 (3)
C18—N2—C12109.3 (11)O17—Rb5—N561.4 (3)
C6—N2—Rb3110.6 (8)N6—Rb5—N5179.4 (3)
C18—N2—Rb3107.5 (8)C37—N5—C43112.2 (11)
C12—N2—Rb3107.5 (8)C37—N5—C49108.2 (12)
C2—O1—C3107.1 (10)C43—N5—C49108.6 (11)
C2—O1—Rb3116.2 (8)C37—N5—Rb5108.9 (9)
C3—O1—Rb3114.4 (7)C43—N5—Rb5109.9 (8)
C4—O2—C5111.0 (11)C49—N5—Rb5109.1 (8)
C4—O2—Rb3112.0 (7)C48—N6—C42111.3 (10)
C5—O2—Rb3112.5 (7)C48—N6—C54111.6 (10)
C8—O3—C9108.4 (10)C42—N6—C54108.7 (10)
C8—O3—Rb3117.7 (7)C48—N6—Rb5108.9 (7)
C9—O3—Rb3111.0 (7)C42—N6—Rb5105.8 (7)
C11—O4—C10111.6 (11)C54—N6—Rb5110.4 (7)
C11—O4—Rb3113.3 (8)C38—O13—C39110.0 (11)
C10—O4—Rb3110.7 (7)C38—O13—Rb5115.5 (8)
C15—O5—C14111.8 (10)C39—O13—Rb5119.9 (7)
C15—O5—Rb3111.5 (8)C41—O14—C40112.9 (10)
C14—O5—Rb3111.2 (8)C41—O14—Rb5114.4 (8)
C16—O6—C17111.1 (11)C40—O14—Rb5114.7 (7)
C16—O6—Rb3112.1 (8)C45—O15—C44111.1 (10)
C17—O6—Rb3116.7 (8)C45—O15—Rb5114.1 (7)
N1—C1—C2111.9 (10)C44—O15—Rb5112.4 (7)
N1—C1—H1A109.2C46—O16—C47112.5 (10)
C2—C1—H1A109.2C46—O16—Rb5114.6 (7)
N1—C1—H1B109.2C47—O16—Rb5114.8 (7)
C2—C1—H1B109.2C51—O17—C50115.1 (11)
H1A—C1—H1B107.9C51—O17—Rb5111.3 (7)
O1—C2—C1108.0 (11)C50—O17—Rb5114.3 (7)
O1—C2—H2A110.1C53—O18—C52110.3 (9)
C1—C2—H2A110.1C53—O18—Rb5116.3 (7)
O1—C2—H2B110.1C52—O18—Rb5115.4 (7)
C1—C2—H2B110.1N5—C37—C38118.6 (12)
H2A—C2—H2B108.4N5—C37—H37A107.7
O1—C3—C4108.4 (11)C38—C37—H37A107.7
O1—C3—H3A110.0N5—C37—H37B107.7
C4—C3—H3A110.0C38—C37—H37B107.7
O1—C3—H3B110.0H37A—C37—H37B107.1
C4—C3—H3B110.0O13—C38—C37110.4 (12)
H3A—C3—H3B108.4O13—C38—H38A109.6
O2—C4—C3110.1 (11)C37—C38—H38A109.6
O2—C4—H4A109.6O13—C38—H38B109.6
C3—C4—H4A109.6C37—C38—H38B109.6
O2—C4—H4B109.6H38A—C38—H38B108.1
C3—C4—H4B109.6O13—C39—C40109.7 (12)
H4A—C4—H4B108.2O13—C39—H39A109.7
O2—C5—C6111.6 (12)C40—C39—H39A109.7
O2—C5—H5A109.3O13—C39—H39B109.7
C6—C5—H5A109.3C40—C39—H39B109.7
O2—C5—H5B109.3H39A—C39—H39B108.2
C6—C5—H5B109.3O14—C40—C39112.2 (11)
H5A—C5—H5B108.0O14—C40—H40A109.2
N2—C6—C5111.9 (12)C39—C40—H40A109.2
N2—C6—H6A109.2O14—C40—H40B109.2
C5—C6—H6A109.2C39—C40—H40B109.2
N2—C6—H6B109.2H40A—C40—H40B107.9
C5—C6—H6B109.2O14—C41—C42111.9 (11)
H6A—C6—H6B107.9O14—C41—H41A109.2
N1—C7—C8113.7 (11)C42—C41—H41A109.2
N1—C7—H7A108.8O14—C41—H41B109.2
C8—C7—H7A108.8C42—C41—H41B109.2
N1—C7—H7B108.8H41A—C41—H41B107.9
C8—C7—H7B108.8N6—C42—C41116.9 (11)
H7A—C7—H7B107.7N6—C42—H42A108.1
O3—C8—C7108.0 (11)C41—C42—H42A108.1
O3—C8—H8A110.1N6—C42—H42B108.1
C7—C8—H8A110.1C41—C42—H42B108.1
O3—C8—H8B110.1H42A—C42—H42B107.3
C7—C8—H8B110.1N5—C43—C44114.3 (10)
H8A—C8—H8B108.4N5—C43—H43A108.7
O3—C9—C10108.2 (11)C44—C43—H43A108.7
O3—C9—H9A110.1N5—C43—H43B108.7
C10—C9—H9A110.1C44—C43—H43B108.7
O3—C9—H9B110.1H43A—C43—H43B107.6
C10—C9—H9B110.1O15—C44—C43111.7 (11)
H9A—C9—H9B108.4O15—C44—H44A109.3
O4—C10—C9109.9 (11)C43—C44—H44A109.3
O4—C10—H10A109.7O15—C44—H44B109.3
C9—C10—H10A109.7C43—C44—H44B109.3
O4—C10—H10B109.7H44A—C44—H44B107.9
C9—C10—H10B109.7O15—C45—C46112.0 (11)
H10A—C10—H10B108.2O15—C45—H45A109.2
O4—C11—C12111.4 (12)C46—C45—H45A109.2
O4—C11—H11A109.3O15—C45—H45B109.2
C12—C11—H11A109.3C46—C45—H45B109.2
O4—C11—H11B109.3H45A—C45—H45B107.9
C12—C11—H11B109.3O16—C46—C45109.7 (11)
H11A—C11—H11B108.0O16—C46—H46A109.7
N2—C12—C11113.5 (13)C45—C46—H46A109.7
N2—C12—H12A108.9O16—C46—H46B109.7
C11—C12—H12A108.9C45—C46—H46B109.7
N2—C12—H12B108.9H46A—C46—H46B108.2
C11—C12—H12B108.9O16—C47—C48108.1 (10)
H12A—C12—H12B107.7O16—C47—H47A110.1
C14—C13—N1112.1 (12)C48—C47—H47A110.1
C14—C13—H13A109.2O16—C47—H47B110.1
N1—C13—H13A109.2C48—C47—H47B110.1
C14—C13—H13B109.2H47A—C47—H47B108.4
N1—C13—H13B109.2N6—C48—C47114.7 (10)
H13A—C13—H13B107.9N6—C48—H48A108.6
O5—C14—C13109.9 (11)C47—C48—H48A108.6
O5—C14—H14A109.7N6—C48—H48B108.6
C13—C14—H14A109.7C47—C48—H48B108.6
O5—C14—H14B109.7H48A—C48—H48B107.6
C13—C14—H14B109.7C50—C49—N5116.2 (11)
H14A—C14—H14B108.2C50—C49—H49A108.2
O5—C15—C16110.0 (11)N5—C49—H49A108.2
O5—C15—H15A109.7C50—C49—H49B108.2
C16—C15—H15A109.7N5—C49—H49B108.2
O5—C15—H15B109.7H49A—C49—H49B107.4
C16—C15—H15B109.7O17—C50—C49112.7 (12)
H15A—C15—H15B108.2O17—C50—H50A109.1
O6—C16—C15112.2 (13)C49—C50—H50A109.1
O6—C16—H16A109.2O17—C50—H50B109.1
C15—C16—H16A109.2C49—C50—H50B109.1
O6—C16—H16B109.2H50A—C50—H50B107.8
C15—C16—H16B109.2O17—C51—C52112.4 (12)
H16A—C16—H16B107.9O17—C51—H51A109.1
O6—C17—C18109.4 (12)C52—C51—H51A109.1
O6—C17—H17A109.8O17—C51—H51B109.1
C18—C17—H17A109.8C52—C51—H51B109.1
O6—C17—H17B109.8H51A—C51—H51B107.9
C18—C17—H17B109.8O18—C52—C51108.6 (11)
H17A—C17—H17B108.2O18—C52—H52A110.0
N2—C18—C17114.9 (12)C51—C52—H52A110.0
N2—C18—H18A108.5O18—C52—H52B110.0
C17—C18—H18A108.5C51—C52—H52B110.0
N2—C18—H18B108.5H52A—C52—H52B108.3
C17—C18—H18B108.5O18—C53—C54109.4 (10)
H18A—C18—H18B107.5O18—C53—H53A109.8
O9—Rb4—O794.6 (3)C54—C53—H53A109.8
O9—Rb4—O12119.1 (2)O18—C53—H53B109.8
O7—Rb4—O12141.6 (2)C54—C53—H53B109.8
O9—Rb4—O1060.3 (3)H53A—C53—H53B108.2
O7—Rb4—O10112.6 (2)C53—C54—N6116.3 (11)
O12—Rb4—O10100.5 (2)C53—C54—H54A108.2
O9—Rb4—O1198.7 (3)N6—C54—H54A108.2
O7—Rb4—O11101.1 (3)C53—C54—H54B108.2
O12—Rb4—O1158.7 (3)N6—C54—H54B108.2
O10—Rb4—O11140.8 (2)H54A—C54—H54B107.4
  7 in total

1.  Metal-centered deltahedral Zintl ions: synthesis of [Ni@Sn9]4- by direct extraction from intermetallic precursors and of the vertex-fused dimer [{Ni@Sn8(μ-Ge)(1/2)}2]4-.

Authors:  Miriam M Gillett-Kunnath; Joseph I Paik; Sara M Jensen; Jacob D Taylor; Slavi C Sevov
Journal:  Inorg Chem       Date:  2011-10-25       Impact factor: 5.165

2.  Ordering of vacancies in type-I tin clathrate: superstructure of Rb8Sn44 square2.

Authors:  Franck Dubois; Thomas F Fässler
Journal:  J Am Chem Soc       Date:  2005-03-16       Impact factor: 15.419

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Zintl ions, cage compounds, and intermetalloid clusters of Group 14 and Group 15 elements.

Authors:  Sandra Scharfe; Florian Kraus; Saskia Stegmaier; Annette Schier; Thomas F Fässler
Journal:  Angew Chem Int Ed Engl       Date:  2011-03-31       Impact factor: 15.336

5.  Easy Access to Soluble Polyanions-Stabilization of the One-Dimensional Chain 1 [K4 Sn9 ] by [18]Crown-6 in [K4 Sn9 ([18]crown-6)3 ]⋅ethylenediamine.

Authors:  Thomas F Fässler; Rudolf Hoffmann
Journal:  Angew Chem Int Ed Engl       Date:  1999-02-15       Impact factor: 15.336

6.  [Rb(18-crown-6)][Rb([2.2.2]-cryptand)]Rb(2)Sn(9)·5NH(3).

Authors:  Stefanie Gaertner; Nikolaus Korber
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-04-22

7.  Crystal structure refinement with SHELXL.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr C Struct Chem       Date:  2015-01-01       Impact factor: 1.172

  7 in total

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