metal-organic compounds
[Rb(18-crown-6)][Rb([2.2.2]-cryptand)]Rb2Sn9·5NH3
aInstitut für Anorganische Chemie, Universität Regensburg, Universitätsstrasse 31, 93053 Regensburg, Germany
*Correspondence e-mail: nikolaus.korber@chemie.uni-regensburg.de
The μ-rubidium-μ-nonastannide] pentaammonia], {[Rb(C18H36N2O6)][Rb3Sn9(C12H24O6)C12H24O6)]·5NH3}n represents the first ammoniate of a Zintl anion together with two different chelating substances, namely 18-crown-6 and [2.2.2]-cryptand. The involvement of these large molecules in the of [Rb(18-crown-6)][Rb([2.2.2]-cryptand)]Rb2Sn9·5NH3 leads to the formation of a new structural motif, namely one-dimensionally extended double strands running parallel to [100] and built by Sn94− cages and Rb+ cations. The double strands are shielded by 18-crown-6 and [2.2.2]-cryptand. The cations are additionally coordinated by ammonia molecules. One of the four independent Rb+ cations is disordered over two sets of sites in a 0.74 (2):0.26 (2) ratio.
of the title compound, poly[[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)rubidium] [[(1,4,7,10,13,16-hexaoxacyclooctadecane)rubidium]di-Related literature
For a recent review on nine-atom group 14 clusters in solution, see: Scharfe & Fässler (2010). For Zintl clusters in the solid state see: Fässler (2001); Hoch et al. (2003). The coordination of two cations by 18-crown-6 usually results in two-dimensional layers (Hauptmann & Fässler, 2002, 2003a,b), when three cations are coordinated by the latter, one-dimensional single strands are observed (Fässler & Hoffmann, 1999). The use of less [2.2.2]-cryptand gives two-dimensional double layers (Hauptmann et al., 2001), whereas larger amounts result in one-dimensional single strands (Burns & Corbett, 1985) or isolated nonastannide clusters without direct cation contacts (Corbett & Edwards, 1977).
Experimental
Crystal data
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Data collection: X-AREA (Stoe & Cie, 2002); cell X-AREA; data reduction: X-RED (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
10.1107/S1600536811013997/hp2005sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536811013997/hp2005Isup2.hkl
0.36 g Rb12Sn17 (0.115 mmol), 0.06 g 18-crown-6 (0.25 mmol) and 0.09 g [2.2.2]-cryptand (0.25 mmol) were placed under Argon atmosphere in a baked out reaction vessel. Afterwards, 15 ml of dry liquid ammonia were condensed onto the reaction mixture, which yielded a dark red solution. After storage for five months at 236 K, dark red crystals could be obtained.
For one Rubidium atom a split model was applied due to large anisotropic displacement, yielding refined sof values of 0.874 (Rb13) respectively 0.126 (Rb14). The H atoms of four ammonia molecules were constructed at geometrically reasonable positions using a riding model (HFIX). For one ammonia molecule, which does not show contacts to cations, it did not seem reasonable to construct H atoms. Due to the extreme sensitivity towards moisture the implacement of a water molecule can be excluded. The H atoms of 18-crown-6 and [2.2.2]-cryptand were also located by using the HFIX instructions.
Data collection: X-AREA (Stoe & Cie, 2002); cell
X-AREA (Stoe & Cie, 2002); data reduction: X-RED (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).[Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3 | F(000) = 3980 |
Mr = 2136.04 | Dx = 2.278 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.790 (2) Å | Cell parameters from 11435 reflections |
b = 15.600 (3) Å | θ = 2.1–25.5° |
c = 36.960 (7) Å | µ = 6.75 mm−1 |
β = 91.20 (3)° | T = 123 K |
V = 6220 (2) Å3 | Rod, dark red |
Z = 4 | 0.25 × 0.2 × 0.15 mm |
Stoe IPDS diffractometer | 11435 independent reflections |
Radiation source: fine-focus sealed tube | 7473 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.099 |
rotation scans | θmax = 25.5°, θmin = 2.1° |
Absorption correction: analytical (X-SHAPE; Stoe & Cie, 2002) | h = −13→13 |
Tmin = 0.057, Tmax = 0.119 | k = 0→18 |
36425 measured reflections | l = 0→44 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 0.84 | w = 1/[σ2(Fo2) + (0.0671P)2] where P = (Fo2 + 2Fc2)/3 |
11435 reflections | (Δ/σ)max = 0.001 |
608 parameters | Δρmax = 2.77 e Å−3 |
0 restraints | Δρmin = −1.18 e Å−3 |
[Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3 | V = 6220 (2) Å3 |
Mr = 2136.04 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.790 (2) Å | µ = 6.75 mm−1 |
b = 15.600 (3) Å | T = 123 K |
c = 36.960 (7) Å | 0.25 × 0.2 × 0.15 mm |
β = 91.20 (3)° |
Stoe IPDS diffractometer | 11435 independent reflections |
Absorption correction: analytical (X-SHAPE; Stoe & Cie, 2002) | 7473 reflections with I > 2σ(I) |
Tmin = 0.057, Tmax = 0.119 | Rint = 0.099 |
36425 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 0.84 | Δρmax = 2.77 e Å−3 |
11435 reflections | Δρmin = −1.18 e Å−3 |
608 parameters |
Experimental. crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement 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 > σ(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 | Occ. (<1) | |
Sn1 | 0.86100 (7) | 0.23615 (4) | 0.907589 (19) | 0.04003 (16) | |
Sn2 | 0.98667 (7) | 0.39369 (5) | 0.931424 (17) | 0.03899 (16) | |
Sn3 | 1.02254 (6) | 0.31609 (4) | 0.854533 (17) | 0.03508 (15) | |
Sn4 | 0.71369 (7) | 0.30366 (4) | 0.846330 (18) | 0.03923 (16) | |
Sn5 | 0.69254 (6) | 0.37991 (5) | 0.923721 (18) | 0.04106 (17) | |
Sn6 | 1.03304 (7) | 0.50482 (4) | 0.86702 (2) | 0.04262 (17) | |
Sn7 | 0.87119 (7) | 0.43216 (5) | 0.809921 (18) | 0.04261 (17) | |
Sn8 | 0.66698 (7) | 0.48901 (5) | 0.856306 (19) | 0.04374 (18) | |
Sn9 | 0.82933 (7) | 0.54589 (5) | 0.91672 (2) | 0.04456 (18) | |
Rb10 | 0.57160 (8) | 0.40171 (5) | 0.75840 (2) | 0.03225 (19) | |
Rb11 | 0.66434 (8) | 0.09245 (5) | 0.09496 (2) | 0.03070 (18) | |
Rb12 | 0.81415 (13) | 0.45056 (9) | 0.01874 (3) | 0.0625 (3) | |
O1 | 0.5633 (6) | 0.2576 (4) | 0.11449 (18) | 0.0402 (15) | |
O2 | 0.4199 (6) | 0.2343 (4) | 0.74399 (16) | 0.0358 (14) | |
O3 | 0.6819 (6) | −0.0751 (4) | 0.12707 (17) | 0.0351 (14) | |
O4 | 0.3954 (7) | 0.5552 (4) | 0.74943 (18) | 0.0398 (15) | |
O5 | 0.6400 (7) | 0.5615 (4) | 0.72603 (18) | 0.0428 (16) | |
O6 | 0.7426 (6) | 0.4148 (4) | 0.69534 (18) | 0.0380 (15) | |
O7 | 0.3089 (6) | 0.3882 (4) | 0.7689 (2) | 0.0423 (16) | |
O8 | 0.8881 (6) | 0.0870 (4) | 0.05216 (17) | 0.0380 (15) | |
O9 | 0.7691 (6) | 0.1897 (4) | 0.15412 (19) | 0.0422 (16) | |
O10 | 0.4441 (6) | −0.0106 (4) | 0.10348 (18) | 0.0350 (14) | |
O11 | 0.6481 (7) | 0.1129 (4) | 0.01641 (17) | 0.0395 (15) | |
O12 | 0.6651 (7) | 0.2526 (4) | 0.72188 (18) | 0.0429 (16) | |
N1 | 0.4241 (8) | 0.1494 (5) | 0.0601 (2) | 0.0351 (17) | |
N2 | 0.9076 (7) | 0.0352 (5) | 0.1296 (2) | 0.0353 (17) | |
N3 | 0.8485 (13) | 0.2982 (8) | 0.0671 (3) | 0.077 (3) | |
H3C | 0.9034 | 0.3114 | 0.0853 | 0.115* | |
H3D | 0.8781 | 0.2535 | 0.0541 | 0.115* | |
H3E | 0.7744 | 0.2835 | 0.0767 | 0.115* | |
N4 | 0.7481 (11) | 0.7826 (7) | 0.0683 (3) | 0.068 (3) | |
H4C | 0.7062 | 0.8276 | 0.0779 | 0.102* | |
H4D | 0.7343 | 0.7810 | 0.0439 | 0.102* | |
H4E | 0.8307 | 0.7889 | 0.0731 | 0.102* | |
N5 | 0.8929 (11) | 0.7596 (9) | −0.0120 (3) | 0.076 (3) | |
N6 | 0.5861 (13) | 0.4400 (7) | 0.0693 (4) | 0.085 (4) | |
H6C | 0.6234 | 0.3966 | 0.0818 | 0.127* | |
H6D | 0.5582 | 0.4200 | 0.0474 | 0.127* | |
H6E | 0.5211 | 0.4604 | 0.0820 | 0.127* | |
N7 | 0.6387 (13) | 0.6110 (8) | 0.0138 (3) | 0.080 (4) | |
H7C | 0.5573 | 0.5956 | 0.0138 | 0.121* | |
H7D | 0.6738 | 0.5923 | −0.0070 | 0.121* | |
H7E | 0.6449 | 0.6691 | 0.0151 | 0.121* | |
C1 | 0.8604 (10) | 0.0730 (7) | 0.0140 (3) | 0.043 (2) | |
H1A | 0.8298 | 0.0138 | 0.0103 | 0.052* | |
H1B | 0.9366 | 0.0804 | −0.0001 | 0.052* | |
C2 | 0.9754 (10) | 0.0273 (7) | 0.0661 (3) | 0.044 (2) | |
H2A | 1.0512 | 0.0286 | 0.0514 | 0.053* | |
H2B | 0.9403 | −0.0313 | 0.0648 | 0.053* | |
C3 | 0.4776 (11) | 0.6220 (6) | 0.7593 (3) | 0.045 (3) | |
H3A | 0.5229 | 0.6066 | 0.7820 | 0.055* | |
H3B | 0.4301 | 0.6752 | 0.7638 | 0.055* | |
C4 | 0.7647 (9) | 0.1352 (7) | 0.0014 (2) | 0.037 (2) | |
H4A | 0.7886 | 0.1938 | 0.0091 | 0.045* | |
H4B | 0.7582 | 0.1343 | −0.0253 | 0.045* | |
C5 | 0.7776 (9) | −0.0840 (7) | 0.1535 (3) | 0.042 (2) | |
H5A | 0.7834 | −0.1446 | 0.1612 | 0.050* | |
H5B | 0.7581 | −0.0489 | 0.1749 | 0.050* | |
C6 | 0.5676 (11) | 0.6370 (7) | 0.7299 (3) | 0.048 (3) | |
H6A | 0.5227 | 0.6500 | 0.7070 | 0.058* | |
H6B | 0.6218 | 0.6862 | 0.7362 | 0.058* | |
C7 | 0.2302 (9) | 0.4614 (7) | 0.7664 (3) | 0.042 (2) | |
H7A | 0.1600 | 0.4551 | 0.7830 | 0.050* | |
H7B | 0.1965 | 0.4673 | 0.7414 | 0.050* | |
C8 | 0.3563 (9) | 0.0031 (7) | 0.0747 (3) | 0.043 (2) | |
H8A | 0.2810 | −0.0315 | 0.0788 | 0.051* | |
H8B | 0.3921 | −0.0150 | 0.0514 | 0.051* | |
C9 | 0.3235 (9) | 0.0957 (7) | 0.0731 (3) | 0.042 (2) | |
H9A | 0.2500 | 0.1032 | 0.0569 | 0.050* | |
H9B | 0.3007 | 0.1152 | 0.0976 | 0.050* | |
C10 | 0.4330 (10) | 0.2605 (7) | 0.1088 (2) | 0.039 (2) | |
H10A | 0.4016 | 0.3183 | 0.1148 | 0.047* | |
H10B | 0.3926 | 0.2185 | 0.1248 | 0.047* | |
C11 | 0.3289 (10) | 0.2381 (7) | 0.7713 (3) | 0.042 (2) | |
H11A | 0.3695 | 0.2472 | 0.7953 | 0.051* | |
H11B | 0.2823 | 0.1835 | 0.7720 | 0.051* | |
C12 | 0.5558 (10) | 0.1729 (7) | 0.0061 (3) | 0.043 (2) | |
H12A | 0.5516 | 0.1780 | −0.0206 | 0.052* | |
H12B | 0.5764 | 0.2299 | 0.0163 | 0.052* | |
C13 | 0.5999 (10) | 0.2839 (7) | 0.1511 (3) | 0.044 (2) | |
H13A | 0.5563 | 0.2479 | 0.1688 | 0.053* | |
H13B | 0.5752 | 0.3443 | 0.1550 | 0.053* | |
C14 | 0.4731 (10) | −0.0986 (6) | 0.1086 (3) | 0.046 (3) | |
H14A | 0.5045 | −0.1228 | 0.0858 | 0.055* | |
H14B | 0.3971 | −0.1303 | 0.1149 | 0.055* | |
C15 | 0.2431 (9) | 0.3100 (7) | 0.7630 (3) | 0.040 (2) | |
H15A | 0.2135 | 0.3065 | 0.7375 | 0.048* | |
H15B | 0.1703 | 0.3074 | 0.7788 | 0.048* | |
C16 | 0.7234 (10) | 0.5677 (7) | 0.6960 (3) | 0.041 (2) | |
H16A | 0.7707 | 0.6220 | 0.6973 | 0.050* | |
H16B | 0.6759 | 0.5665 | 0.6728 | 0.050* | |
C17 | 0.7518 (10) | 0.2623 (7) | 0.6930 (3) | 0.046 (3) | |
H17A | 0.7067 | 0.2642 | 0.6694 | 0.055* | |
H17B | 0.8093 | 0.2129 | 0.6928 | 0.055* | |
C18 | 0.7343 (10) | 0.2755 (7) | 0.1571 (3) | 0.042 (2) | |
H18A | 0.7784 | 0.3102 | 0.1390 | 0.050* | |
H18B | 0.7575 | 0.2973 | 0.1814 | 0.050* | |
C19 | 0.5680 (10) | −0.1097 (6) | 0.1379 (3) | 0.044 (2) | |
H19A | 0.5406 | −0.0804 | 0.1601 | 0.053* | |
H19B | 0.5783 | −0.1714 | 0.1434 | 0.053* | |
C20 | 0.4024 (12) | 0.2398 (7) | 0.0699 (3) | 0.052 (3) | |
H20A | 0.3141 | 0.2538 | 0.0649 | 0.062* | |
H20B | 0.4529 | 0.2768 | 0.0542 | 0.062* | |
C21 | 1.0067 (9) | 0.0497 (7) | 0.1044 (3) | 0.042 (2) | |
H21A | 1.0798 | 0.0157 | 0.1123 | 0.050* | |
H21B | 1.0305 | 0.1110 | 0.1054 | 0.050* | |
C22 | 0.5137 (10) | 0.1715 (6) | 0.7512 (3) | 0.043 (2) | |
H22A | 0.4756 | 0.1140 | 0.7531 | 0.052* | |
H22B | 0.5572 | 0.1846 | 0.7744 | 0.052* | |
C23 | 0.8992 (9) | 0.1786 (7) | 0.1595 (3) | 0.045 (3) | |
H23A | 0.9272 | 0.2097 | 0.1816 | 0.054* | |
H23B | 0.9438 | 0.2024 | 0.1387 | 0.054* | |
C24 | 0.8224 (10) | 0.3427 (7) | 0.6986 (3) | 0.044 (2) | |
H24A | 0.8624 | 0.3423 | 0.7229 | 0.052* | |
H24B | 0.8883 | 0.3467 | 0.6804 | 0.052* | |
C25 | 0.9278 (9) | 0.0843 (7) | 0.1635 (3) | 0.044 (2) | |
H25A | 1.0153 | 0.0775 | 0.1716 | 0.053* | |
H25B | 0.8749 | 0.0598 | 0.1825 | 0.053* | |
C26 | 0.3043 (10) | 0.5380 (7) | 0.7763 (3) | 0.044 (2) | |
H26A | 0.2488 | 0.5881 | 0.7786 | 0.053* | |
H26B | 0.3462 | 0.5285 | 0.8001 | 0.053* | |
C27 | 0.4310 (10) | 0.1429 (7) | 0.0200 (3) | 0.045 (2) | |
H27A | 0.3642 | 0.1780 | 0.0088 | 0.055* | |
H27B | 0.4172 | 0.0825 | 0.0127 | 0.055* | |
C28 | 0.8094 (9) | 0.4932 (6) | 0.6982 (3) | 0.040 (2) | |
H28A | 0.8698 | 0.4968 | 0.6785 | 0.048* | |
H28B | 0.8560 | 0.4948 | 0.7216 | 0.048* | |
C29 | 0.8976 (9) | −0.0564 (7) | 0.1388 (3) | 0.042 (2) | |
H29A | 0.9637 | −0.0705 | 0.1568 | 0.050* | |
H29B | 0.9135 | −0.0903 | 0.1168 | 0.050* | |
C30 | 0.6027 (10) | 0.1724 (6) | 0.7214 (3) | 0.044 (2) | |
H30A | 0.6632 | 0.1252 | 0.7245 | 0.053* | |
H30B | 0.5583 | 0.1645 | 0.6979 | 0.053* | |
Rb13 | 0.6569 (4) | 0.6145 (3) | 0.10223 (8) | 0.0558 (12) | 0.74 (2) |
Rb14 | 0.6416 (11) | 0.6289 (8) | 0.1185 (15) | 0.130 (9) | 0.26 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0417 (4) | 0.0373 (4) | 0.0413 (4) | 0.0003 (3) | 0.0037 (3) | 0.0097 (3) |
Sn2 | 0.0417 (4) | 0.0457 (4) | 0.0294 (3) | 0.0058 (3) | −0.0039 (3) | −0.0026 (3) |
Sn3 | 0.0406 (4) | 0.0334 (3) | 0.0314 (3) | 0.0037 (3) | 0.0060 (3) | 0.0004 (3) |
Sn4 | 0.0514 (4) | 0.0332 (3) | 0.0328 (3) | −0.0058 (3) | −0.0047 (3) | 0.0010 (3) |
Sn5 | 0.0360 (4) | 0.0540 (4) | 0.0335 (3) | 0.0033 (3) | 0.0056 (3) | −0.0003 (3) |
Sn6 | 0.0515 (4) | 0.0342 (3) | 0.0423 (4) | −0.0078 (3) | 0.0037 (3) | −0.0009 (3) |
Sn7 | 0.0376 (4) | 0.0585 (4) | 0.0316 (3) | −0.0021 (3) | −0.0013 (3) | 0.0103 (3) |
Sn8 | 0.0518 (4) | 0.0409 (4) | 0.0381 (4) | 0.0132 (3) | −0.0079 (3) | −0.0045 (3) |
Sn9 | 0.0474 (4) | 0.0405 (4) | 0.0456 (4) | 0.0082 (3) | −0.0046 (3) | −0.0126 (3) |
Rb10 | 0.0341 (5) | 0.0319 (4) | 0.0307 (4) | 0.0001 (3) | 0.0001 (3) | 0.0001 (3) |
Rb11 | 0.0337 (5) | 0.0319 (4) | 0.0266 (4) | 0.0006 (3) | 0.0018 (3) | −0.0005 (3) |
Rb12 | 0.0672 (8) | 0.0778 (8) | 0.0427 (6) | −0.0158 (6) | 0.0066 (5) | 0.0015 (6) |
O1 | 0.039 (4) | 0.044 (4) | 0.038 (4) | 0.001 (3) | 0.007 (3) | −0.002 (3) |
O2 | 0.040 (4) | 0.038 (3) | 0.029 (3) | 0.007 (3) | 0.000 (3) | 0.008 (3) |
O3 | 0.027 (3) | 0.045 (4) | 0.033 (3) | 0.007 (3) | 0.000 (3) | 0.006 (3) |
O4 | 0.050 (4) | 0.033 (3) | 0.036 (4) | −0.003 (3) | 0.000 (3) | −0.003 (3) |
O5 | 0.052 (4) | 0.038 (4) | 0.038 (4) | 0.002 (3) | 0.008 (3) | 0.001 (3) |
O6 | 0.033 (3) | 0.044 (4) | 0.037 (4) | −0.004 (3) | 0.005 (3) | −0.001 (3) |
O7 | 0.037 (4) | 0.035 (4) | 0.055 (4) | −0.002 (3) | 0.008 (3) | −0.008 (3) |
O8 | 0.039 (4) | 0.049 (4) | 0.026 (3) | 0.004 (3) | 0.001 (3) | −0.006 (3) |
O9 | 0.041 (4) | 0.045 (4) | 0.042 (4) | −0.005 (3) | 0.003 (3) | −0.015 (3) |
O10 | 0.028 (3) | 0.036 (3) | 0.041 (4) | 0.001 (3) | 0.000 (3) | 0.003 (3) |
O11 | 0.049 (4) | 0.042 (4) | 0.027 (3) | −0.002 (3) | 0.002 (3) | 0.004 (3) |
O12 | 0.055 (4) | 0.032 (4) | 0.042 (4) | −0.002 (3) | 0.010 (3) | −0.004 (3) |
N1 | 0.042 (5) | 0.037 (4) | 0.027 (4) | 0.005 (3) | −0.001 (3) | 0.001 (3) |
N2 | 0.030 (4) | 0.047 (5) | 0.028 (4) | 0.003 (3) | −0.005 (3) | −0.001 (3) |
N3 | 0.101 (9) | 0.082 (8) | 0.047 (6) | −0.004 (7) | −0.002 (6) | −0.017 (6) |
N4 | 0.063 (7) | 0.072 (7) | 0.068 (7) | 0.018 (6) | −0.014 (5) | −0.019 (6) |
N5 | 0.058 (7) | 0.110 (10) | 0.061 (7) | 0.032 (7) | 0.007 (5) | 0.014 (7) |
N6 | 0.095 (10) | 0.055 (7) | 0.107 (10) | −0.005 (6) | 0.041 (8) | −0.005 (7) |
N7 | 0.085 (9) | 0.081 (8) | 0.076 (8) | 0.012 (7) | 0.019 (7) | 0.011 (7) |
C1 | 0.043 (6) | 0.055 (6) | 0.031 (5) | −0.008 (5) | 0.010 (4) | −0.014 (4) |
C2 | 0.044 (6) | 0.052 (6) | 0.037 (5) | 0.004 (5) | 0.006 (4) | −0.004 (5) |
C3 | 0.065 (7) | 0.031 (5) | 0.040 (5) | 0.000 (5) | −0.014 (5) | −0.007 (4) |
C4 | 0.030 (5) | 0.060 (6) | 0.022 (4) | −0.004 (4) | −0.002 (4) | −0.005 (4) |
C5 | 0.032 (5) | 0.048 (6) | 0.045 (6) | 0.008 (4) | −0.002 (4) | 0.015 (5) |
C6 | 0.070 (8) | 0.033 (5) | 0.041 (6) | −0.002 (5) | −0.013 (5) | −0.003 (4) |
C7 | 0.035 (5) | 0.050 (6) | 0.041 (5) | 0.007 (4) | 0.000 (4) | −0.011 (5) |
C8 | 0.032 (5) | 0.054 (6) | 0.041 (5) | −0.006 (4) | −0.012 (4) | 0.005 (5) |
C9 | 0.031 (5) | 0.051 (6) | 0.041 (5) | −0.001 (4) | −0.006 (4) | 0.003 (5) |
C10 | 0.044 (6) | 0.044 (5) | 0.029 (5) | 0.011 (4) | 0.003 (4) | 0.000 (4) |
C11 | 0.041 (6) | 0.053 (6) | 0.033 (5) | −0.007 (5) | 0.002 (4) | 0.003 (4) |
C12 | 0.056 (7) | 0.046 (6) | 0.026 (5) | 0.006 (5) | 0.000 (4) | 0.003 (4) |
C13 | 0.052 (6) | 0.046 (6) | 0.035 (5) | −0.001 (5) | 0.008 (5) | −0.014 (4) |
C14 | 0.037 (6) | 0.031 (5) | 0.070 (7) | −0.002 (4) | −0.010 (5) | 0.006 (5) |
C15 | 0.035 (5) | 0.049 (6) | 0.037 (5) | −0.010 (4) | 0.011 (4) | −0.007 (4) |
C16 | 0.051 (6) | 0.041 (5) | 0.032 (5) | −0.011 (5) | 0.003 (4) | 0.004 (4) |
C17 | 0.049 (6) | 0.047 (6) | 0.043 (6) | 0.015 (5) | 0.016 (5) | −0.012 (5) |
C18 | 0.049 (6) | 0.042 (6) | 0.034 (5) | −0.008 (5) | 0.002 (4) | −0.010 (4) |
C19 | 0.045 (6) | 0.035 (5) | 0.052 (6) | −0.001 (4) | 0.016 (5) | 0.012 (5) |
C20 | 0.069 (8) | 0.042 (6) | 0.045 (6) | 0.016 (5) | 0.014 (5) | 0.003 (5) |
C21 | 0.031 (5) | 0.063 (7) | 0.030 (5) | 0.005 (5) | −0.001 (4) | −0.008 (4) |
C22 | 0.050 (6) | 0.039 (5) | 0.040 (5) | −0.005 (4) | −0.008 (5) | 0.003 (4) |
C23 | 0.033 (5) | 0.063 (7) | 0.039 (5) | −0.015 (5) | 0.003 (4) | −0.012 (5) |
C24 | 0.041 (6) | 0.053 (6) | 0.036 (5) | 0.004 (5) | 0.002 (4) | −0.008 (4) |
C25 | 0.026 (5) | 0.072 (7) | 0.034 (5) | −0.007 (5) | −0.002 (4) | −0.007 (5) |
C26 | 0.054 (7) | 0.047 (6) | 0.031 (5) | 0.017 (5) | 0.003 (4) | −0.005 (4) |
C27 | 0.051 (6) | 0.050 (6) | 0.035 (5) | 0.014 (5) | −0.003 (5) | 0.000 (5) |
C28 | 0.038 (5) | 0.044 (6) | 0.038 (5) | −0.012 (4) | 0.002 (4) | 0.004 (4) |
C29 | 0.031 (5) | 0.057 (6) | 0.037 (5) | 0.015 (4) | −0.006 (4) | 0.009 (5) |
C30 | 0.049 (6) | 0.034 (5) | 0.049 (6) | 0.002 (4) | −0.015 (5) | −0.004 (4) |
Rb13 | 0.0371 (13) | 0.0645 (18) | 0.066 (2) | −0.0003 (10) | −0.0051 (8) | −0.0027 (10) |
Rb14 | 0.035 (4) | 0.075 (5) | 0.28 (3) | 0.011 (3) | −0.002 (9) | −0.026 (10) |
Sn1—Sn3 | 2.9295 (12) | N6—H6C | 0.9100 |
Sn1—Sn2 | 2.9334 (11) | N6—H6D | 0.9100 |
Sn1—Sn4 | 2.9344 (12) | N6—H6E | 0.9100 |
Sn1—Sn5 | 2.9553 (11) | N7—H7C | 0.9100 |
Sn2—Sn9 | 2.9623 (11) | N7—H7D | 0.9100 |
Sn2—Sn6 | 2.9954 (11) | N7—H7E | 0.9100 |
Sn2—Sn3 | 3.1206 (11) | C1—C4 | 1.484 (15) |
Sn2—Sn5 | 3.1877 (12) | C1—H1A | 0.9900 |
Sn2—Rb12i | 3.7080 (16) | C1—H1B | 0.9900 |
Sn2—Rb12ii | 3.8625 (17) | C2—C21 | 1.490 (13) |
Sn2—Rb13i | 4.069 (5) | C2—H2A | 0.9900 |
Sn3—Sn7 | 2.9243 (11) | C2—H2B | 0.9900 |
Sn3—Sn6 | 2.9819 (11) | C3—C6 | 1.491 (17) |
Sn3—Rb14i | 3.835 (16) | C3—H3A | 0.9900 |
Sn3—Rb13i | 3.932 (3) | C3—H3B | 0.9900 |
Sn4—Sn8 | 2.9594 (11) | C4—H4A | 0.9900 |
Sn4—Sn7 | 2.9687 (11) | C4—H4B | 0.9900 |
Sn4—Sn5 | 3.1106 (11) | C5—C29 | 1.478 (14) |
Sn4—Rb10 | 3.8784 (14) | C5—H5A | 0.9900 |
Sn4—Rb14iii | 4.21 (2) | C5—H5B | 0.9900 |
Sn5—Sn9 | 2.9942 (12) | C6—H6A | 0.9900 |
Sn5—Sn8 | 3.0252 (11) | C6—H6B | 0.9900 |
Sn5—Rb13iii | 3.872 (4) | C7—C26 | 1.479 (15) |
Sn5—Rb12ii | 3.8829 (17) | C7—H7A | 0.9900 |
Sn5—Rb14iii | 3.90 (2) | C7—H7B | 0.9900 |
Sn6—Sn7 | 2.9382 (13) | C8—C9 | 1.489 (15) |
Sn6—Sn9 | 2.9642 (14) | C8—H8A | 0.9900 |
Sn6—Sn8 | 3.9689 (14) | C8—H8B | 0.9900 |
Sn6—Rb13i | 3.974 (5) | C9—H9A | 0.9900 |
Sn6—Rb14i | 4.109 (11) | C9—H9B | 0.9900 |
Sn7—Sn8 | 2.9561 (13) | C10—C20 | 1.503 (15) |
Sn7—Rb10 | 3.7474 (15) | C10—H10A | 0.9900 |
Sn8—Rb14iii | 3.93 (2) | C10—H10B | 0.9900 |
Sn8—Rb10 | 3.9814 (14) | C11—C15 | 1.483 (15) |
Sn8—Rb13iii | 4.171 (4) | C11—H11A | 0.9900 |
Sn9—Rb12ii | 4.0597 (16) | C11—H11B | 0.9900 |
Rb10—O5 | 2.869 (7) | C12—C27 | 1.525 (16) |
Rb10—O7 | 2.876 (7) | C12—H12A | 0.9900 |
Rb10—O12 | 2.882 (7) | C12—H12B | 0.9900 |
Rb10—O6 | 3.010 (6) | C13—C18 | 1.467 (15) |
Rb10—O4 | 3.071 (7) | C13—H13A | 0.9900 |
Rb10—O2 | 3.122 (7) | C13—H13B | 0.9900 |
Rb11—O9 | 2.873 (7) | C14—C19 | 1.483 (15) |
Rb11—O3 | 2.875 (6) | C14—H14A | 0.9900 |
Rb11—O10 | 2.891 (6) | C14—H14B | 0.9900 |
Rb11—O1 | 2.896 (7) | C15—H15A | 0.9900 |
Rb11—O8 | 2.915 (7) | C15—H15B | 0.9900 |
Rb11—O11 | 2.922 (6) | C16—C28 | 1.488 (15) |
Rb11—N1 | 3.004 (8) | C16—H16A | 0.9900 |
Rb11—N2 | 3.032 (8) | C16—H16B | 0.9900 |
Rb12—N3 | 2.992 (12) | C17—C24 | 1.479 (15) |
Rb12—Sn2i | 3.7080 (16) | C17—H17A | 0.9900 |
Rb12—Sn2iv | 3.8625 (17) | C17—H17B | 0.9900 |
Rb12—Sn5iv | 3.8829 (17) | C18—H18A | 0.9900 |
Rb12—Sn9iv | 4.0597 (16) | C18—H18B | 0.9900 |
O1—C10 | 1.418 (12) | C19—H19A | 0.9900 |
O1—C13 | 1.460 (12) | C19—H19B | 0.9900 |
O2—C11 | 1.425 (12) | C20—H20A | 0.9900 |
O2—C22 | 1.430 (12) | C20—H20B | 0.9900 |
O3—C19 | 1.407 (12) | C21—H21A | 0.9900 |
O3—C5 | 1.412 (11) | C21—H21B | 0.9900 |
O4—C3 | 1.413 (12) | C22—C30 | 1.477 (16) |
O4—C26 | 1.437 (12) | C22—H22A | 0.9900 |
O5—C6 | 1.421 (13) | C22—H22B | 0.9900 |
O5—C16 | 1.448 (12) | C23—C25 | 1.511 (16) |
O6—C24 | 1.420 (12) | C23—H23A | 0.9900 |
O6—C28 | 1.423 (12) | C23—H23B | 0.9900 |
O7—C7 | 1.426 (12) | C24—H24A | 0.9900 |
O7—C15 | 1.426 (12) | C24—H24B | 0.9900 |
O8—C2 | 1.414 (12) | C25—H25A | 0.9900 |
O8—C1 | 1.450 (11) | C25—H25B | 0.9900 |
O9—C18 | 1.396 (12) | C26—H26A | 0.9900 |
O9—C23 | 1.425 (13) | C26—H26B | 0.9900 |
O10—C14 | 1.421 (11) | C27—H27A | 0.9900 |
O10—C8 | 1.426 (11) | C27—H27B | 0.9900 |
O11—C12 | 1.413 (12) | C28—H28A | 0.9900 |
O11—C4 | 1.428 (12) | C28—H28B | 0.9900 |
O12—C30 | 1.421 (12) | C29—H29A | 0.9900 |
O12—C17 | 1.442 (12) | C29—H29B | 0.9900 |
N1—C9 | 1.460 (13) | C30—H30A | 0.9900 |
N1—C20 | 1.476 (13) | C30—H30B | 0.9900 |
N1—C27 | 1.489 (12) | Rb13—Sn5iii | 3.872 (4) |
N2—C21 | 1.453 (13) | Rb13—Sn3i | 3.932 (3) |
N2—C29 | 1.473 (13) | Rb13—Sn6i | 3.974 (5) |
N2—C25 | 1.480 (12) | Rb13—Sn2i | 4.069 (5) |
N3—H3C | 0.9100 | Rb13—Sn8iii | 4.171 (4) |
N3—H3D | 0.9100 | Rb14—Sn3i | 3.835 (15) |
N3—H3E | 0.9100 | Rb14—Sn5iii | 3.90 (2) |
N4—Rb13 | 3.077 (13) | Rb14—Sn8iii | 3.933 (19) |
N4—H4C | 0.9100 | Rb14—Sn6i | 4.109 (11) |
N4—H4D | 0.9100 | Rb14—Sn4iii | 4.21 (2) |
N4—H4E | 0.9100 | ||
Sn3—Sn1—Sn2 | 64.32 (3) | C18—O9—C23 | 111.8 (8) |
Sn3—Sn1—Sn4 | 69.57 (3) | C18—O9—Rb11 | 117.6 (6) |
Sn2—Sn1—Sn4 | 99.82 (3) | C23—O9—Rb11 | 114.4 (5) |
Sn3—Sn1—Sn5 | 100.90 (3) | C14—O10—C8 | 112.7 (8) |
Sn2—Sn1—Sn5 | 65.55 (3) | C14—O10—Rb11 | 111.9 (5) |
Sn4—Sn1—Sn5 | 63.76 (3) | C8—O10—Rb11 | 111.7 (5) |
Sn1—Sn2—Sn9 | 110.91 (3) | C12—O11—C4 | 110.9 (7) |
Sn1—Sn2—Sn6 | 109.27 (3) | C12—O11—Rb11 | 111.6 (5) |
Sn9—Sn2—Sn6 | 59.67 (3) | C4—O11—Rb11 | 112.1 (5) |
Sn1—Sn2—Sn3 | 57.78 (3) | C30—O12—C17 | 113.4 (8) |
Sn9—Sn2—Sn3 | 103.03 (3) | C30—O12—Rb10 | 123.1 (6) |
Sn6—Sn2—Sn3 | 58.32 (3) | C17—O12—Rb10 | 120.1 (5) |
Sn1—Sn2—Sn5 | 57.56 (3) | C9—N1—C20 | 110.1 (8) |
Sn9—Sn2—Sn5 | 58.13 (3) | C9—N1—C27 | 109.9 (8) |
Sn6—Sn2—Sn5 | 98.66 (4) | C20—N1—C27 | 108.7 (8) |
Sn3—Sn2—Sn5 | 91.99 (4) | C9—N1—Rb11 | 109.3 (5) |
Sn1—Sn2—Rb12i | 163.26 (3) | C20—N1—Rb11 | 108.5 (7) |
Sn9—Sn2—Rb12i | 83.68 (4) | C27—N1—Rb11 | 110.2 (6) |
Sn6—Sn2—Rb12i | 84.88 (3) | C21—N2—C29 | 111.0 (8) |
Sn3—Sn2—Rb12i | 128.68 (4) | C21—N2—C25 | 111.5 (8) |
Sn5—Sn2—Rb12i | 130.86 (4) | C29—N2—C25 | 108.5 (8) |
Sn1—Sn2—Rb12ii | 102.44 (3) | C21—N2—Rb11 | 108.9 (5) |
Sn9—Sn2—Rb12ii | 71.63 (3) | C29—N2—Rb11 | 108.4 (5) |
Sn6—Sn2—Rb12ii | 128.50 (4) | C25—N2—Rb11 | 108.4 (6) |
Sn3—Sn2—Rb12ii | 157.10 (3) | Rb12—N3—H3C | 109.5 |
Sn5—Sn2—Rb12ii | 66.03 (4) | Rb12—N3—H3D | 109.5 |
Rb12i—Sn2—Rb12ii | 73.68 (4) | H3C—N3—H3D | 109.5 |
Sn1—Sn2—Rb13i | 108.41 (7) | Rb12—N3—H3E | 109.5 |
Sn9—Sn2—Rb13i | 120.72 (7) | H3C—N3—H3E | 109.5 |
Sn6—Sn2—Rb13i | 66.46 (6) | H3D—N3—H3E | 109.5 |
Sn3—Sn2—Rb13i | 64.74 (5) | Rb13—N4—H4C | 109.5 |
Sn5—Sn2—Rb13i | 156.38 (5) | Rb13—N4—H4D | 109.5 |
Rb12i—Sn2—Rb13i | 68.33 (6) | H4C—N4—H4D | 109.5 |
Rb12ii—Sn2—Rb13i | 137.55 (5) | Rb13—N4—H4E | 109.5 |
Sn7—Sn3—Sn1 | 107.93 (3) | H4C—N4—H4E | 109.5 |
Sn7—Sn3—Sn6 | 59.66 (3) | H4D—N4—H4E | 109.5 |
Sn1—Sn3—Sn6 | 109.75 (3) | H6C—N6—H6D | 109.5 |
Sn7—Sn3—Sn2 | 101.23 (3) | H6C—N6—H6E | 109.5 |
Sn1—Sn3—Sn2 | 57.90 (3) | H6D—N6—H6E | 109.5 |
Sn6—Sn3—Sn2 | 58.74 (2) | H7C—N7—H7D | 109.5 |
Sn7—Sn3—Rb14i | 121.4 (4) | H7C—N7—H7E | 109.5 |
Sn1—Sn3—Rb14i | 119.6 (8) | H7D—N7—H7E | 109.5 |
Sn6—Sn3—Rb14i | 72.9 (2) | O8—C1—C4 | 109.5 (8) |
Sn2—Sn3—Rb14i | 79.1 (8) | O8—C1—Rb11 | 46.7 (4) |
Sn7—Sn3—Rb13i | 122.33 (7) | C4—C1—Rb11 | 78.2 (5) |
Sn1—Sn3—Rb13i | 112.08 (5) | O8—C1—H1A | 109.8 |
Sn6—Sn3—Rb13i | 68.59 (8) | C4—C1—H1A | 109.8 |
Sn2—Sn3—Rb13i | 69.38 (7) | Rb11—C1—H1A | 89.7 |
Rb14i—Sn3—Rb13i | 9.7 (7) | O8—C1—H1B | 109.8 |
Sn1—Sn4—Sn8 | 110.21 (3) | C4—C1—H1B | 109.8 |
Sn1—Sn4—Sn7 | 106.63 (3) | Rb11—C1—H1B | 155.4 |
Sn8—Sn4—Sn7 | 59.82 (3) | H1A—C1—H1B | 108.2 |
Sn1—Sn4—Sn5 | 58.45 (3) | O8—C2—C21 | 109.1 (8) |
Sn8—Sn4—Sn5 | 59.73 (2) | O8—C2—Rb11 | 47.1 (4) |
Sn7—Sn4—Sn5 | 102.26 (3) | C21—C2—Rb11 | 81.4 (6) |
Sn1—Sn4—Rb10 | 170.49 (3) | O8—C2—H2A | 109.9 |
Sn8—Sn4—Rb10 | 69.74 (2) | C21—C2—H2A | 109.9 |
Sn7—Sn4—Rb10 | 64.78 (3) | Rb11—C2—H2A | 156.9 |
Sn5—Sn4—Rb10 | 125.76 (3) | O8—C2—H2B | 109.9 |
Sn1—Sn4—Rb14iii | 109.5 (7) | C21—C2—H2B | 109.9 |
Sn8—Sn4—Rb14iii | 63.80 (18) | Rb11—C2—H2B | 85.3 |
Sn7—Sn4—Rb14iii | 120.3 (3) | H2A—C2—H2B | 108.3 |
Sn5—Sn4—Rb14iii | 62.3 (7) | O4—C3—C6 | 110.0 (8) |
Rb10—Sn4—Rb14iii | 79.2 (7) | O4—C3—Rb10 | 57.7 (5) |
Sn1—Sn5—Sn9 | 109.42 (3) | C6—C3—Rb10 | 87.4 (6) |
Sn1—Sn5—Sn8 | 107.85 (3) | O4—C3—H3A | 109.7 |
Sn9—Sn5—Sn8 | 58.60 (3) | C6—C3—H3A | 109.7 |
Sn1—Sn5—Sn4 | 57.79 (3) | Rb10—C3—H3A | 68.9 |
Sn9—Sn5—Sn4 | 101.86 (3) | O4—C3—H3B | 109.7 |
Sn8—Sn5—Sn4 | 57.65 (3) | C6—C3—H3B | 109.7 |
Sn1—Sn5—Sn2 | 56.90 (2) | Rb10—C3—H3B | 162.2 |
Sn9—Sn5—Sn2 | 57.16 (2) | H3A—C3—H3B | 108.2 |
Sn8—Sn5—Sn2 | 96.26 (4) | O11—C4—C1 | 109.4 (8) |
Sn4—Sn5—Sn2 | 90.91 (4) | O11—C4—Rb11 | 47.0 (4) |
Sn1—Sn5—Rb13iii | 124.54 (8) | C1—C4—Rb11 | 78.7 (5) |
Sn9—Sn5—Rb13iii | 116.00 (7) | O11—C4—H4A | 109.8 |
Sn8—Sn5—Rb13iii | 73.25 (5) | C1—C4—H4A | 109.8 |
Sn4—Sn5—Rb13iii | 82.57 (7) | Rb11—C4—H4A | 88.7 |
Sn2—Sn5—Rb13iii | 169.45 (5) | O11—C4—H4B | 109.8 |
Sn1—Sn5—Rb12ii | 101.55 (4) | C1—C4—H4B | 109.8 |
Sn9—Sn5—Rb12ii | 71.02 (3) | Rb11—C4—H4B | 156.0 |
Sn8—Sn5—Rb12ii | 127.48 (4) | H4A—C4—H4B | 108.2 |
Sn4—Sn5—Rb12ii | 155.55 (3) | O3—C5—C29 | 110.6 (8) |
Sn2—Sn5—Rb12ii | 65.36 (4) | O3—C5—Rb11 | 45.1 (4) |
Rb13iii—Sn5—Rb12ii | 121.77 (7) | C29—C5—Rb11 | 81.4 (5) |
Sn1—Sn5—Rb14iii | 117.4 (5) | O3—C5—H5A | 109.5 |
Sn9—Sn5—Rb14iii | 116.7 (3) | C29—C5—H5A | 109.5 |
Sn8—Sn5—Rb14iii | 67.8 (6) | Rb11—C5—H5A | 154.1 |
Sn4—Sn5—Rb14iii | 72.7 (7) | O3—C5—H5B | 109.5 |
Sn2—Sn5—Rb14iii | 161.5 (8) | C29—C5—H5B | 109.5 |
Rb13iii—Sn5—Rb14iii | 9.8 (7) | Rb11—C5—H5B | 89.0 |
Rb12ii—Sn5—Rb14iii | 131.6 (7) | H5A—C5—H5B | 108.1 |
Sn7—Sn6—Sn9 | 95.23 (3) | O5—C6—C3 | 108.2 (8) |
Sn7—Sn6—Sn3 | 59.20 (2) | O5—C6—H6A | 110.1 |
Sn9—Sn6—Sn3 | 106.44 (3) | C3—C6—H6A | 110.1 |
Sn7—Sn6—Sn2 | 103.94 (3) | O5—C6—H6B | 110.1 |
Sn9—Sn6—Sn2 | 59.61 (3) | C3—C6—H6B | 110.1 |
Sn3—Sn6—Sn2 | 62.94 (2) | H6A—C6—H6B | 108.4 |
Sn7—Sn6—Sn8 | 47.87 (3) | O7—C7—C26 | 108.2 (8) |
Sn9—Sn6—Sn8 | 47.62 (3) | O7—C7—H7A | 110.1 |
Sn3—Sn6—Sn8 | 83.61 (2) | C26—C7—H7A | 110.1 |
Sn2—Sn6—Sn8 | 82.00 (3) | O7—C7—H7B | 110.1 |
Sn7—Sn6—Rb13i | 120.59 (7) | C26—C7—H7B | 110.1 |
Sn9—Sn6—Rb13i | 123.69 (6) | H7A—C7—H7B | 108.4 |
Sn3—Sn6—Rb13i | 67.09 (6) | O10—C8—C9 | 109.1 (8) |
Sn2—Sn6—Rb13i | 69.83 (5) | O10—C8—Rb11 | 47.1 (4) |
Sn8—Sn6—Rb13i | 146.05 (6) | C9—C8—Rb11 | 81.5 (5) |
Sn7—Sn6—Rb14i | 113.0 (6) | O10—C8—H8A | 109.9 |
Sn9—Sn6—Rb14i | 132.2 (7) | C9—C8—H8A | 109.9 |
Sn3—Sn6—Rb14i | 63.2 (3) | Rb11—C8—H8A | 156.9 |
Sn2—Sn6—Rb14i | 76.1 (6) | O10—C8—H8B | 109.9 |
Sn8—Sn6—Rb14i | 145.81 (19) | C9—C8—H8B | 109.9 |
Rb13i—Sn6—Rb14i | 9.3 (7) | Rb11—C8—H8B | 85.3 |
Sn3—Sn7—Sn6 | 61.15 (3) | H8A—C8—H8B | 108.3 |
Sn3—Sn7—Sn8 | 105.84 (3) | N1—C9—C8 | 113.1 (8) |
Sn6—Sn7—Sn8 | 84.65 (3) | N1—C9—Rb11 | 49.1 (4) |
Sn3—Sn7—Sn4 | 69.18 (3) | C8—C9—Rb11 | 75.3 (5) |
Sn6—Sn7—Sn4 | 105.80 (3) | N1—C9—H9A | 109.0 |
Sn8—Sn7—Sn4 | 59.93 (3) | C8—C9—H9A | 109.0 |
Sn3—Sn7—Rb10 | 132.34 (3) | Rb11—C9—H9A | 154.3 |
Sn6—Sn7—Rb10 | 155.13 (3) | N1—C9—H9B | 109.0 |
Sn8—Sn7—Rb10 | 71.77 (3) | C8—C9—H9B | 109.0 |
Sn4—Sn7—Rb10 | 69.44 (3) | Rb11—C9—H9B | 93.9 |
Sn3—Sn7—Sn9 | 78.97 (3) | H9A—C9—H9B | 107.8 |
Sn6—Sn7—Sn9 | 42.61 (2) | O1—C10—C20 | 109.4 (8) |
Sn8—Sn7—Sn9 | 42.29 (3) | O1—C10—Rb11 | 47.3 (4) |
Sn4—Sn7—Sn9 | 78.07 (3) | C20—C10—Rb11 | 81.4 (6) |
Rb10—Sn7—Sn9 | 114.02 (3) | O1—C10—H10A | 109.8 |
Sn9—Sn8—Sn7 | 95.24 (3) | C20—C10—H10A | 109.8 |
Sn9—Sn8—Sn4 | 106.78 (3) | Rb11—C10—H10A | 157.0 |
Sn7—Sn8—Sn4 | 60.25 (2) | O1—C10—H10B | 109.8 |
Sn9—Sn8—Sn5 | 60.17 (3) | C20—C10—H10B | 109.8 |
Sn7—Sn8—Sn5 | 104.64 (3) | Rb11—C10—H10B | 85.4 |
Sn4—Sn8—Sn5 | 62.62 (3) | H10A—C10—H10B | 108.2 |
Sn9—Sn8—Rb14iii | 117.0 (8) | O2—C11—C15 | 108.7 (8) |
Sn7—Sn8—Rb14iii | 129.9 (5) | O2—C11—Rb10 | 55.7 (5) |
Sn4—Sn8—Rb14iii | 73.7 (3) | C15—C11—Rb10 | 83.8 (6) |
Sn5—Sn8—Rb14iii | 66.7 (6) | O2—C11—H11A | 110.0 |
Sn9—Sn8—Sn6 | 48.01 (3) | C15—C11—H11A | 110.0 |
Sn7—Sn8—Sn6 | 47.48 (3) | Rb10—C11—H11A | 73.4 |
Sn4—Sn8—Sn6 | 84.34 (2) | O2—C11—H11B | 110.0 |
Sn5—Sn8—Sn6 | 83.08 (3) | C15—C11—H11B | 110.0 |
Rb14iii—Sn8—Sn6 | 148.3 (4) | Rb10—C11—H11B | 163.7 |
Sn9—Sn8—Rb10 | 158.47 (3) | H11A—C11—H11B | 108.3 |
Sn7—Sn8—Rb10 | 63.38 (3) | O11—C12—C27 | 109.1 (8) |
Sn4—Sn8—Rb10 | 66.05 (2) | O11—C12—Rb11 | 47.5 (4) |
Sn5—Sn8—Rb10 | 124.99 (3) | C27—C12—Rb11 | 82.0 (5) |
Rb14iii—Sn8—Rb10 | 81.4 (8) | O11—C12—H12A | 109.9 |
Sn6—Sn8—Rb10 | 110.47 (4) | C27—C12—H12A | 109.9 |
Sn9—Sn8—Rb13iii | 109.12 (5) | Rb11—C12—H12A | 157.4 |
Sn7—Sn8—Rb13iii | 137.51 (8) | O11—C12—H12B | 109.9 |
Sn4—Sn8—Rb13iii | 79.26 (8) | C27—C12—H12B | 109.9 |
Sn5—Sn8—Rb13iii | 62.75 (6) | Rb11—C12—H12B | 84.3 |
Rb14iii—Sn8—Rb13iii | 8.8 (7) | H12A—C12—H12B | 108.3 |
Sn6—Sn8—Rb13iii | 145.82 (5) | O1—C13—C18 | 111.2 (8) |
Rb10—Sn8—Rb13iii | 89.94 (5) | O1—C13—Rb11 | 46.1 (4) |
Sn8—Sn9—Sn2 | 103.12 (3) | C18—C13—Rb11 | 79.4 (5) |
Sn8—Sn9—Sn6 | 84.37 (3) | O1—C13—H13A | 109.4 |
Sn2—Sn9—Sn6 | 60.72 (3) | C18—C13—H13A | 109.4 |
Sn8—Sn9—Sn5 | 61.23 (3) | Rb11—C13—H13A | 90.7 |
Sn2—Sn9—Sn5 | 64.71 (3) | O1—C13—H13B | 109.4 |
Sn6—Sn9—Sn5 | 103.88 (3) | C18—C13—H13B | 109.4 |
Sn8—Sn9—Rb12ii | 123.97 (4) | Rb11—C13—H13B | 154.2 |
Sn2—Sn9—Rb12ii | 64.54 (3) | H13A—C13—H13B | 108.0 |
Sn6—Sn9—Rb12ii | 122.78 (4) | O10—C14—C19 | 110.9 (8) |
Sn5—Sn9—Rb12ii | 64.75 (3) | O10—C14—Rb11 | 47.0 (4) |
Sn8—Sn9—Sn7 | 42.47 (2) | C19—C14—Rb11 | 79.2 (5) |
Sn2—Sn9—Sn7 | 76.71 (3) | O10—C14—H14A | 109.5 |
Sn6—Sn9—Sn7 | 42.15 (3) | C19—C14—H14A | 109.5 |
Sn5—Sn9—Sn7 | 77.70 (3) | Rb11—C14—H14A | 89.4 |
Rb12ii—Sn9—Sn7 | 134.33 (3) | O10—C14—H14B | 109.5 |
O5—Rb10—O7 | 112.5 (2) | C19—C14—H14B | 109.5 |
O5—Rb10—O12 | 114.23 (19) | Rb11—C14—H14B | 155.5 |
O7—Rb10—O12 | 111.1 (2) | H14A—C14—H14B | 108.0 |
O5—Rb10—O6 | 56.70 (19) | O7—C15—C11 | 107.9 (8) |
O7—Rb10—O6 | 137.0 (2) | O7—C15—H15A | 110.1 |
O12—Rb10—O6 | 57.70 (18) | C11—C15—H15A | 110.1 |
O5—Rb10—O4 | 56.04 (19) | O7—C15—H15B | 110.1 |
O7—Rb10—O4 | 57.46 (19) | C11—C15—H15B | 110.1 |
O12—Rb10—O4 | 143.19 (19) | H15A—C15—H15B | 108.4 |
O6—Rb10—O4 | 104.59 (18) | O5—C16—C28 | 107.6 (8) |
O5—Rb10—O2 | 142.60 (18) | O5—C16—H16A | 110.2 |
O7—Rb10—O2 | 56.43 (18) | C28—C16—H16A | 110.2 |
O12—Rb10—O2 | 55.43 (19) | O5—C16—H16B | 110.2 |
O6—Rb10—O2 | 104.61 (17) | C28—C16—H16B | 110.2 |
O4—Rb10—O2 | 108.20 (17) | H16A—C16—H16B | 108.5 |
O5—Rb10—C3 | 41.0 (2) | O12—C17—C24 | 109.0 (8) |
O7—Rb10—C3 | 77.8 (2) | O12—C17—H17A | 109.9 |
O12—Rb10—C3 | 151.7 (2) | C24—C17—H17A | 109.9 |
O6—Rb10—C3 | 96.9 (2) | O12—C17—H17B | 109.9 |
O4—Rb10—C3 | 22.9 (2) | C24—C17—H17B | 109.9 |
O2—Rb10—C3 | 131.0 (2) | H17A—C17—H17B | 108.3 |
O5—Rb10—C24 | 76.5 (2) | O9—C18—C13 | 109.9 (8) |
O7—Rb10—C24 | 144.0 (2) | C13—C18—Rb11 | 77.8 (5) |
O12—Rb10—C24 | 40.6 (2) | O9—C18—H18A | 109.7 |
O6—Rb10—C24 | 22.1 (2) | C13—C18—H18A | 109.7 |
O4—Rb10—C24 | 126.6 (2) | Rb11—C18—H18A | 95.5 |
O2—Rb10—C24 | 94.5 (2) | O9—C18—H18B | 109.7 |
C3—Rb10—C24 | 117.5 (3) | C13—C18—H18B | 109.7 |
O5—Rb10—C22 | 150.3 (2) | Rb11—C18—H18B | 150.1 |
O7—Rb10—C22 | 76.7 (2) | H18A—C18—H18B | 108.2 |
O12—Rb10—C22 | 40.0 (2) | O3—C19—C14 | 110.0 (8) |
O6—Rb10—C22 | 96.7 (2) | O3—C19—Rb11 | 45.2 (4) |
O4—Rb10—C22 | 130.8 (2) | C14—C19—Rb11 | 77.5 (5) |
O2—Rb10—C22 | 22.7 (2) | O3—C19—H19A | 109.7 |
C3—Rb10—C22 | 153.5 (3) | C14—C19—H19A | 109.7 |
C24—Rb10—C22 | 80.5 (2) | Rb11—C19—H19A | 93.1 |
O5—Rb10—C26 | 77.3 (2) | O3—C19—H19B | 109.7 |
O7—Rb10—C26 | 40.1 (2) | C14—C19—H19B | 109.7 |
O12—Rb10—C26 | 147.1 (2) | Rb11—C19—H19B | 152.7 |
O6—Rb10—C26 | 126.9 (2) | H19A—C19—H19B | 108.2 |
O4—Rb10—C26 | 22.6 (2) | N1—C20—C10 | 114.0 (9) |
O2—Rb10—C26 | 96.0 (2) | N1—C20—Rb11 | 49.5 (5) |
C3—Rb10—C26 | 38.4 (3) | C10—C20—Rb11 | 75.2 (6) |
C24—Rb10—C26 | 148.7 (2) | N1—C20—H20A | 108.8 |
C22—Rb10—C26 | 116.8 (3) | C10—C20—H20A | 108.8 |
O5—Rb10—C11 | 147.5 (2) | Rb11—C20—H20A | 154.0 |
O7—Rb10—C11 | 39.5 (2) | N1—C20—H20B | 108.8 |
O12—Rb10—C11 | 76.1 (2) | C10—C20—H20B | 108.8 |
O6—Rb10—C11 | 126.5 (2) | Rb11—C20—H20B | 94.6 |
O4—Rb10—C11 | 96.5 (2) | H20A—C20—H20B | 107.7 |
O2—Rb10—C11 | 22.1 (2) | N2—C21—C2 | 114.8 (8) |
C3—Rb10—C11 | 117.4 (3) | N2—C21—H21A | 108.6 |
C24—Rb10—C11 | 116.2 (2) | C2—C21—H21A | 108.6 |
C22—Rb10—C11 | 37.8 (2) | N2—C21—H21B | 108.6 |
C26—Rb10—C11 | 79.3 (2) | C2—C21—H21B | 108.6 |
O5—Rb10—C28 | 39.6 (2) | H21A—C21—H21B | 107.5 |
O7—Rb10—C28 | 143.5 (2) | O2—C22—C30 | 108.8 (8) |
O12—Rb10—C28 | 77.1 (2) | O2—C22—Rb10 | 57.3 (4) |
O6—Rb10—C28 | 21.3 (2) | C30—C22—Rb10 | 86.1 (6) |
O4—Rb10—C28 | 94.0 (2) | O2—C22—H22A | 109.9 |
O2—Rb10—C28 | 125.8 (2) | C30—C22—H22A | 109.9 |
C3—Rb10—C28 | 80.6 (3) | Rb10—C22—H22A | 162.9 |
C24—Rb10—C28 | 37.2 (2) | O2—C22—H22B | 109.9 |
C22—Rb10—C28 | 116.9 (2) | C30—C22—H22B | 109.9 |
C26—Rb10—C28 | 116.3 (2) | Rb10—C22—H22B | 70.0 |
C11—Rb10—C28 | 147.4 (2) | H22A—C22—H22B | 108.3 |
O9—Rb11—O3 | 98.3 (2) | O9—C23—C25 | 109.3 (8) |
O9—Rb11—O10 | 121.43 (19) | O9—C23—Rb11 | 45.0 (4) |
O3—Rb11—O10 | 59.79 (18) | C25—C23—Rb11 | 81.0 (5) |
O9—Rb11—O1 | 59.0 (2) | O9—C23—H23A | 109.8 |
O3—Rb11—O1 | 136.72 (18) | C25—C23—H23A | 109.8 |
O10—Rb11—O1 | 98.80 (19) | Rb11—C23—H23A | 154.5 |
O9—Rb11—O8 | 96.40 (19) | O9—C23—H23B | 109.8 |
O3—Rb11—O8 | 98.59 (18) | C25—C23—H23B | 109.8 |
O10—Rb11—O8 | 137.29 (18) | Rb11—C23—H23B | 88.3 |
O1—Rb11—O8 | 118.80 (19) | H23A—C23—H23B | 108.3 |
O9—Rb11—O11 | 135.5 (2) | O6—C24—C17 | 110.5 (9) |
O3—Rb11—O11 | 120.77 (18) | O6—C24—Rb10 | 52.8 (4) |
O10—Rb11—O11 | 97.86 (19) | C17—C24—Rb10 | 84.9 (6) |
O1—Rb11—O11 | 97.78 (19) | O6—C24—H24A | 109.6 |
O8—Rb11—O11 | 59.82 (19) | C17—C24—H24A | 109.6 |
O9—Rb11—N1 | 119.5 (2) | Rb10—C24—H24A | 76.5 |
O3—Rb11—N1 | 119.6 (2) | O6—C24—H24B | 109.6 |
O10—Rb11—N1 | 60.5 (2) | C17—C24—H24B | 109.6 |
O1—Rb11—N1 | 61.2 (2) | Rb10—C24—H24B | 161.3 |
O8—Rb11—N1 | 119.54 (19) | H24A—C24—H24B | 108.1 |
O11—Rb11—N1 | 60.6 (2) | N2—C25—C23 | 113.3 (8) |
O9—Rb11—N2 | 60.7 (2) | N2—C25—H25A | 108.9 |
O3—Rb11—N2 | 60.6 (2) | C23—C25—H25A | 108.9 |
O10—Rb11—N2 | 119.8 (2) | N2—C25—H25B | 108.9 |
O1—Rb11—N2 | 118.9 (2) | C23—C25—H25B | 108.9 |
O8—Rb11—N2 | 60.08 (19) | H25A—C25—H25B | 107.7 |
O11—Rb11—N2 | 119.1 (2) | O4—C26—C7 | 110.6 (8) |
N1—Rb11—N2 | 179.6 (2) | O4—C26—Rb10 | 55.2 (4) |
O9—Rb11—C10 | 76.9 (2) | C7—C26—Rb10 | 84.8 (5) |
O3—Rb11—C10 | 129.2 (2) | O4—C26—H26A | 109.5 |
O10—Rb11—C10 | 79.5 (2) | C7—C26—H26A | 109.5 |
O1—Rb11—C10 | 21.1 (2) | Rb10—C26—H26A | 163.0 |
O8—Rb11—C10 | 132.2 (2) | O4—C26—H26B | 109.5 |
O11—Rb11—C10 | 91.9 (2) | C7—C26—H26B | 109.5 |
N1—Rb11—C10 | 42.6 (2) | Rb10—C26—H26B | 74.1 |
N2—Rb11—C10 | 137.6 (2) | H26A—C26—H26B | 108.1 |
O9—Rb11—C14 | 122.5 (2) | N1—C27—C12 | 112.3 (9) |
O3—Rb11—C14 | 40.2 (2) | N1—C27—H27A | 109.2 |
O10—Rb11—C14 | 21.1 (2) | C12—C27—H27A | 109.2 |
O1—Rb11—C14 | 118.2 (2) | N1—C27—H27B | 109.2 |
O8—Rb11—C14 | 121.7 (2) | C12—C27—H27B | 109.2 |
O11—Rb11—C14 | 101.8 (2) | H27A—C27—H27B | 107.9 |
N1—Rb11—C14 | 79.4 (2) | O6—C28—C16 | 110.7 (8) |
N2—Rb11—C14 | 100.8 (2) | O6—C28—Rb10 | 50.2 (4) |
C10—Rb11—C14 | 100.1 (2) | C16—C28—Rb10 | 84.0 (5) |
O9—Rb11—C8 | 134.1 (2) | O6—C28—H28A | 109.5 |
O3—Rb11—C8 | 77.9 (2) | C16—C28—H28A | 109.5 |
O10—Rb11—C8 | 21.2 (2) | Rb10—C28—H28A | 159.5 |
O1—Rb11—C8 | 92.6 (2) | O6—C28—H28B | 109.5 |
O8—Rb11—C8 | 129.4 (2) | C16—C28—H28B | 109.5 |
O11—Rb11—C8 | 78.7 (2) | Rb10—C28—H28B | 80.3 |
N1—Rb11—C8 | 41.8 (2) | H28A—C28—H28B | 108.1 |
N2—Rb11—C8 | 138.4 (2) | N2—C29—C5 | 115.9 (8) |
C10—Rb11—C8 | 71.5 (2) | N2—C29—H29A | 108.3 |
C14—Rb11—C8 | 37.7 (2) | C5—C29—H29A | 108.3 |
O9—Rb11—C12 | 127.7 (2) | N2—C29—H29B | 108.3 |
O3—Rb11—C12 | 134.0 (2) | C5—C29—H29B | 108.3 |
O10—Rb11—C12 | 92.3 (2) | H29A—C29—H29B | 107.4 |
O1—Rb11—C12 | 78.7 (2) | O12—C30—C22 | 108.3 (8) |
O8—Rb11—C12 | 77.2 (2) | O12—C30—H30A | 110.0 |
O11—Rb11—C12 | 20.9 (2) | C22—C30—H30A | 110.0 |
N1—Rb11—C12 | 42.4 (2) | O12—C30—H30B | 110.0 |
N2—Rb11—C12 | 137.2 (2) | C22—C30—H30B | 110.0 |
C10—Rb11—C12 | 71.1 (2) | H30A—C30—H30B | 108.4 |
C14—Rb11—C12 | 103.3 (2) | Rb14—Rb13—N4 | 99.7 (19) |
C8—Rb11—C12 | 71.2 (2) | Rb14—Rb13—Sn5iii | 87.6 (17) |
N3—Rb12—Sn2i | 99.2 (2) | N4—Rb13—Sn5iii | 101.4 (2) |
N3—Rb12—Sn2iv | 105.1 (2) | Rb14—Rb13—Sn3i | 76.9 (14) |
Sn2i—Rb12—Sn2iv | 106.32 (4) | N4—Rb13—Sn3i | 69.2 (2) |
N3—Rb12—Sn5iv | 110.5 (2) | Sn5iii—Rb13—Sn3i | 159.77 (16) |
Sn2i—Rb12—Sn5iv | 144.75 (4) | Rb14—Rb13—Sn6i | 97 (2) |
Sn2iv—Rb12—Sn5iv | 48.60 (2) | N4—Rb13—Sn6i | 104.0 (2) |
N3—Rb12—Sn9iv | 147.0 (2) | Sn5iii—Rb13—Sn6i | 153.00 (12) |
Sn2i—Rb12—Sn9iv | 100.78 (4) | Sn3i—Rb13—Sn6i | 44.32 (5) |
Sn2iv—Rb12—Sn9iv | 43.83 (2) | Rb14—Rb13—Sn2i | 122.7 (14) |
Sn5iv—Rb12—Sn9iv | 44.22 (2) | N4—Rb13—Sn2i | 65.8 (2) |
N3—Rb12—Rb13 | 95.0 (2) | Sn5iii—Rb13—Sn2i | 147.86 (8) |
Sn2i—Rb12—Rb13 | 59.74 (5) | Sn3i—Rb13—Sn2i | 45.88 (5) |
Sn2iv—Rb12—Rb13 | 157.50 (6) | Sn6i—Rb13—Sn2i | 43.71 (5) |
Sn5iv—Rb12—Rb13 | 132.44 (6) | Rb14—Rb13—Sn8iii | 64.7 (13) |
Sn9iv—Rb12—Rb13 | 117.68 (6) | N4—Rb13—Sn8iii | 139.2 (3) |
N3—Rb12—Rb12v | 110.7 (3) | Sn5iii—Rb13—Sn8iii | 43.99 (4) |
Sn2i—Rb12—Rb12v | 54.72 (3) | Sn3i—Rb13—Sn8iii | 133.95 (7) |
Sn2iv—Rb12—Rb12v | 51.60 (3) | Sn6i—Rb13—Sn8iii | 114.86 (9) |
Sn5iv—Rb12—Rb12v | 95.99 (4) | Sn2i—Rb13—Sn8iii | 154.80 (14) |
Sn9iv—Rb12—Rb12v | 62.56 (4) | Rb14—Rb13—Rb12 | 160 (2) |
Rb13—Rb12—Rb12v | 111.99 (6) | N4—Rb13—Rb12 | 94.5 (2) |
N3—Rb12—Rb14 | 92.5 (4) | Sn5iii—Rb13—Rb12 | 103.20 (8) |
Sn2i—Rb12—Rb14 | 59.39 (15) | Sn3i—Rb13—Rb12 | 95.55 (11) |
Sn2iv—Rb12—Rb14 | 159.3 (3) | Sn6i—Rb13—Rb12 | 65.89 (9) |
Sn5iv—Rb12—Rb14 | 134.4 (3) | Sn2i—Rb13—Rb12 | 51.93 (7) |
Sn9iv—Rb12—Rb14 | 120.2 (4) | Sn8iii—Rb13—Rb12 | 111.90 (10) |
Rb13—Rb12—Rb14 | 2.6 (4) | Rb13—Rb14—Sn3i | 93.4 (12) |
Rb12v—Rb12—Rb14 | 112.35 (15) | Rb13—Rb14—Sn5iii | 83 (2) |
C10—O1—C13 | 112.2 (7) | Sn3i—Rb14—Sn5iii | 166.4 (10) |
C10—O1—Rb11 | 111.6 (5) | Rb13—Rb14—Sn8iii | 106.4 (15) |
C13—O1—Rb11 | 112.6 (6) | Sn3i—Rb14—Sn8iii | 147.5 (13) |
C11—O2—C22 | 113.1 (7) | Sn5iii—Rb14—Sn8iii | 45.43 (13) |
C11—O2—Rb10 | 102.2 (5) | Rb13—Rb14—Sn6i | 73.7 (14) |
C22—O2—Rb10 | 100.1 (5) | Sn3i—Rb14—Sn6i | 43.92 (13) |
C19—O3—C5 | 113.4 (7) | Sn5iii—Rb14—Sn6i | 144.5 (8) |
C19—O3—Rb11 | 114.5 (5) | Sn8iii—Rb14—Sn6i | 117.2 (5) |
C5—O3—Rb11 | 114.5 (6) | Rb13—Rb14—Sn4iii | 127 (2) |
C3—O4—C26 | 113.2 (8) | Sn3i—Rb14—Sn4iii | 136.6 (12) |
C3—O4—Rb10 | 99.4 (6) | Sn5iii—Rb14—Sn4iii | 44.92 (14) |
C26—O4—Rb10 | 102.2 (5) | Sn8iii—Rb14—Sn4iii | 42.5 (2) |
C6—O5—C16 | 112.0 (8) | Sn6i—Rb14—Sn4iii | 150.3 (12) |
C6—O5—Rb10 | 122.0 (6) | Sn3i—Rb14—Rb12 | 87.2 (6) |
C16—O5—Rb10 | 123.2 (5) | Sn5iii—Rb14—Rb12 | 92.3 (9) |
C24—O6—C28 | 111.7 (7) | Sn8iii—Rb14—Rb12 | 104.1 (6) |
C24—O6—Rb10 | 105.1 (5) | Sn6i—Rb14—Rb12 | 58.9 (4) |
C28—O6—Rb10 | 108.5 (5) | Sn4iii—Rb14—Rb12 | 136.2 (8) |
C7—O7—C15 | 112.4 (7) | Sn3i—Rb14—Rb10iii | 103.2 (11) |
C7—O7—Rb10 | 121.3 (6) | Sn5iii—Rb14—Rb10iii | 85.7 (5) |
C15—O7—Rb10 | 122.1 (5) | Sn8iii—Rb14—Rb10iii | 49.7 (5) |
C2—O8—C1 | 112.1 (7) | Sn6i—Rb14—Rb10iii | 103.5 (9) |
C2—O8—Rb11 | 112.0 (5) | Sn4iii—Rb14—Rb10iii | 47.6 (5) |
C1—O8—Rb11 | 112.0 (5) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x, y, z+1; (iii) −x+1, −y+1, −z+1; (iv) x, y, z−1; (v) −x+2, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3 |
Mr | 2136.04 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 123 |
a, b, c (Å) | 10.790 (2), 15.600 (3), 36.960 (7) |
β (°) | 91.20 (3) |
V (Å3) | 6220 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.75 |
Crystal size (mm) | 0.25 × 0.2 × 0.15 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Analytical (X-SHAPE; Stoe & Cie, 2002) |
Tmin, Tmax | 0.057, 0.119 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 36425, 11435, 7473 |
Rint | 0.099 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.112, 0.84 |
No. of reflections | 11435 |
No. of parameters | 608 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.77, −1.18 |
Computer programs: X-AREA (Stoe & Cie, 2002), X-RED (Stoe & Cie, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2001), publCIF (Westrip, 2010).
References
Brandenburg, K. (2001). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Burns, R. C. & Corbett, J. D. (1985). Inorg. Chem. 24, 1489–1492. CrossRef CAS Google Scholar
Corbett, J. D. & Edwards, P. A. (1977). J. Am. Chem. Soc. 99, 3313–3317. CrossRef CAS Google Scholar
Fässler, T. F. (2001). Coord. Chem. Rev. 215, 347–377. Google Scholar
Fässler, T. F. & Hoffmann, R. (1999). Angew. Chem. Int. Ed. 38, 543–546. Google Scholar
Hauptmann, R. & Fässler, T. F. (2002). Z. Anorg. Allg. Chem. 628, 1500–1504. CrossRef CAS Google Scholar
Hauptmann, R. & Fässler, T. F. (2003a). Z. Kristallogr. New Cryst. Struct. 218, 455-457. CAS Google Scholar
Hauptmann, R. & Fässler, T. F. (2003b). Z. Kristallogr. New Cryst. Struct. 218, 458-460. CAS Google Scholar
Hauptmann, R., Hoffmann, R. & Fässler, T. F. (2001). Z. Anorg. Allg. Chem. 627, 2220–2224. CrossRef CAS Google Scholar
Hoch, C., Wendorff, M. & Röhr, C. (2003). J. Alloys Compd, 361, 206–221. Web of Science CrossRef CAS Google Scholar
Scharfe, S. & Fässler, T. F. (2010). Philos. Trans. R. Soc. London Ser A, 368, 1265–1284. CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2002). X-AREA, X-RED and X-SHAPE. Stoe & Cie, Darmstadt, Germany. Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
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Compounds which contain elements of group 14 elements in negative oxidation states can be obtained by reacting an electropositive metal with the favoured element in solid state reactions at high temperatures. Some of these Zintl phases contain molecular homoatomic clusters preformed in solid state (Hoch et al., 2003, Fassler, 2001). The dissolution of these cluster containing Zintl compounds in an appropriate solvent is a common route to obtain homoatomic building blocks in solution (Scharfe & Fassler, 2010). Dissolving the binary material Rb12Sn17, which contains four and nine atom clusters of tin, in liquid ammonia in presence of 18-crown-6 and [2.2.2]-cryptand yields a dark red solution, the colour of which is characteristic for polystannides in solution. After storage at 236 K for five months dark red, rod shaped crystals could be isolated, which only include the nine atom clusters Sn94- and four Rb+, of which one Rb cation is coordinated by 18-crown-6 and one Rb+ is situated in the cavity of a [2.2.2]-cryptand molecule. The coordiantion of two cations by 18-crown-6 usually results in two-dimensional layers (Hauptmann & Fassler, 2003a,b; Hauptmann & Fassler, 2002), when three cations are coordinated by the latter, one-dimensional single strands are observed (Fassler & Hoffmann, 1999). The use of less [2.2.2]-cryptand gives two-dimensional double layers (Hauptmann et al., 2001), whereas larger amounts result in one-dimensional single strands (Burns & Corbett, 1985) or isolated nonastannide clusters without direct cation contacts (Corbett & Edwards, 1977). The presence of the two different chelating compounds offers the possibility of a new structral motif in nonastannide compounds. Here, one-dimensional double strands of nonastannide cages linked by Rb+ (Rb10, Rb12, Rb13) along the crystallographic a axis are observed. These double strands are shielded by 18-crown-6 molecules, which surround Rb10 (Fig.1). [2.2.2]-cryptand molecules around Rb11 isolate the double strands from each other. The coordination spheres of the Rb cations are saturated by ammonia molecules, additionally one ammonia molecule of crystallization is found (Fig. 2).