metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 5| May 2011| Pages m613-m614

[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

(Received 28 March 2011; accepted 13 April 2011; online 22 April 2011)

The crystal structure 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-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 crystal structure 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.

Related literature

For a recent review on nine-atom group 14 clusters in solution, see: Scharfe & Fässler (2010[Scharfe, S. & Fässler, T. F. (2010). Philos. Trans. R. Soc. London Ser A, 368, 1265-1284.]). For Zintl clusters in the solid state see: Fässler (2001[Fässler, T. F. (2001). Coord. Chem. Rev. 215, 347-377.]); Hoch et al. (2003[Hoch, C., Wendorff, M. & Röhr, C. (2003). J. Alloys Compd, 361, 206-221.]). The coordination of two cations by 18-crown-6 usually results in two-dimensional layers (Hauptmann & Fässler, 2002[Hauptmann, R. & Fässler, T. F. (2002). Z. Anorg. Allg. Chem. 628, 1500-1504.], 2003a[Hauptmann, R. & Fässler, T. F. (2003a). Z. Kristallogr. New Cryst. Struct. 218, 455-457.],b[Hauptmann, R. & Fässler, T. F. (2003b). Z. Kristallogr. New Cryst. Struct. 218, 458-460.]), when three cations are coordinated by the latter, one-dimensional single strands are observed (Fässler & Hoffmann, 1999[Fässler, T. F. & Hoffmann, R. (1999). Angew. Chem. Int. Ed. 38, 543-546.]). The use of less [2.2.2]-cryptand gives two-dimensional double layers (Hauptmann et al., 2001[Hauptmann, R., Hoffmann, R. & Fässler, T. F. (2001). Z. Anorg. Allg. Chem. 627, 2220-2224.]), whereas larger amounts result in one-dimensional single strands (Burns & Corbett, 1985[Burns, R. C. & Corbett, J. D. (1985). Inorg. Chem. 24, 1489-1492.]) or isolated nona­stannide clusters without direct cation contacts (Corbett & Edwards, 1977[Corbett, J. D. & Edwards, P. A. (1977). J. Am. Chem. Soc. 99, 3313-3317.]).

[Scheme 1]

Experimental

Crystal data
  • [Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3

  • Mr = 2136.04

  • Monoclinic, P 21 /n

  • a = 10.790 (2) Å

  • b = 15.600 (3) Å

  • c = 36.960 (7) Å

  • β = 91.20 (3)°

  • V = 6220 (2) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 6.75 mm−1

  • T = 123 K

  • 0.25 × 0.2 × 0.15 mm

Data collection
  • Stoe IPDS diffractometer

  • Absorption correction: analytical (X-SHAPE; Stoe & Cie, 2002[Stoe & Cie (2002). X-AREA, X-RED and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]) Tmin = 0.057, Tmax = 0.119

  • 36425 measured reflections

  • 11435 independent reflections

  • 7473 reflections with I > 2σ(I)

  • Rint = 0.099

Refinement
  • R[F2 > 2σ(F2)] = 0.043

  • wR(F2) = 0.112

  • S = 0.84

  • 11435 reflections

  • 608 parameters

  • H-atom parameters constrained

  • Δρmax = 2.77 e Å−3

  • Δρmin = −1.18 e Å−3

Data collection: X-AREA (Stoe & Cie, 2002[Stoe & Cie (2002). X-AREA, X-RED and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2002[Stoe & Cie (2002). X-AREA, X-RED and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2001[Brandenburg, K. (2001). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

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).

Related literature top

For a recent review on nine-atom group 14 clusters in solution, see: Scharfe & Fassler (2010). For Zintl clusters in the solid state see: Fassler (2001); Hoch et al. (2003). 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).

Experimental top

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.

Refinement top

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.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: 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).

Figures top
[Figure 1] Fig. 1. : One-dimensionally extended double strands along the crystallographic a axis built by Rb12 and Rb13 (split position is not shown), 18-crown-6 molecules around Rb10 shield the strands. H atoms of 18-crown-6 are omitted; ellipsoids of all non-hydrogen atoms are given with a probability factor of 50%.
[Figure 2] Fig. 2. : The unit-cell content of [Rb(18-crown-6)][Rb([2.2.2]-cryptand)]Rb2Sn9 × 5NH3 shows the separation of the strands by [2.2.2]-cryptand molecules around Rb11; the coordination spheres of the Rb cations are saturated by ammonia molecules. H atoms of 18-crown-6 and [2.2.2]-cryptand are omitted; ellipsoids of all non-hydrogen atoms are given with a probability factor of 50%.
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-µ-rubidium-µ- nonastannide] pentaammonia] top
Crystal data top
[Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3F(000) = 3980
Mr = 2136.04Dx = 2.278 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.790 (2) ÅCell parameters from 11435 reflections
b = 15.600 (3) Åθ = 2.1–25.5°
c = 36.960 (7) ŵ = 6.75 mm1
β = 91.20 (3)°T = 123 K
V = 6220 (2) Å3Rod, dark red
Z = 40.25 × 0.2 × 0.15 mm
Data collection top
Stoe IPDS
diffractometer
11435 independent reflections
Radiation source: fine-focus sealed tube7473 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.099
rotation scansθmax = 25.5°, θmin = 2.1°
Absorption correction: analytical
(X-SHAPE; Stoe & Cie, 2002)
h = 1313
Tmin = 0.057, Tmax = 0.119k = 018
36425 measured reflectionsl = 044
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.112H-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 parametersΔρmax = 2.77 e Å3
0 restraintsΔρmin = 1.18 e Å3
Crystal data top
[Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3V = 6220 (2) Å3
Mr = 2136.04Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.790 (2) ŵ = 6.75 mm1
b = 15.600 (3) ÅT = 123 K
c = 36.960 (7) Å0.25 × 0.2 × 0.15 mm
β = 91.20 (3)°
Data collection top
Stoe IPDS
diffractometer
11435 independent reflections
Absorption correction: analytical
(X-SHAPE; Stoe & Cie, 2002)
7473 reflections with I > 2σ(I)
Tmin = 0.057, Tmax = 0.119Rint = 0.099
36425 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0430 restraints
wR(F2) = 0.112H-atom parameters constrained
S = 0.84Δρmax = 2.77 e Å3
11435 reflectionsΔρmin = 1.18 e Å3
608 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn10.86100 (7)0.23615 (4)0.907589 (19)0.04003 (16)
Sn20.98667 (7)0.39369 (5)0.931424 (17)0.03899 (16)
Sn31.02254 (6)0.31609 (4)0.854533 (17)0.03508 (15)
Sn40.71369 (7)0.30366 (4)0.846330 (18)0.03923 (16)
Sn50.69254 (6)0.37991 (5)0.923721 (18)0.04106 (17)
Sn61.03304 (7)0.50482 (4)0.86702 (2)0.04262 (17)
Sn70.87119 (7)0.43216 (5)0.809921 (18)0.04261 (17)
Sn80.66698 (7)0.48901 (5)0.856306 (19)0.04374 (18)
Sn90.82933 (7)0.54589 (5)0.91672 (2)0.04456 (18)
Rb100.57160 (8)0.40171 (5)0.75840 (2)0.03225 (19)
Rb110.66434 (8)0.09245 (5)0.09496 (2)0.03070 (18)
Rb120.81415 (13)0.45056 (9)0.01874 (3)0.0625 (3)
O10.5633 (6)0.2576 (4)0.11449 (18)0.0402 (15)
O20.4199 (6)0.2343 (4)0.74399 (16)0.0358 (14)
O30.6819 (6)0.0751 (4)0.12707 (17)0.0351 (14)
O40.3954 (7)0.5552 (4)0.74943 (18)0.0398 (15)
O50.6400 (7)0.5615 (4)0.72603 (18)0.0428 (16)
O60.7426 (6)0.4148 (4)0.69534 (18)0.0380 (15)
O70.3089 (6)0.3882 (4)0.7689 (2)0.0423 (16)
O80.8881 (6)0.0870 (4)0.05216 (17)0.0380 (15)
O90.7691 (6)0.1897 (4)0.15412 (19)0.0422 (16)
O100.4441 (6)0.0106 (4)0.10348 (18)0.0350 (14)
O110.6481 (7)0.1129 (4)0.01641 (17)0.0395 (15)
O120.6651 (7)0.2526 (4)0.72188 (18)0.0429 (16)
N10.4241 (8)0.1494 (5)0.0601 (2)0.0351 (17)
N20.9076 (7)0.0352 (5)0.1296 (2)0.0353 (17)
N30.8485 (13)0.2982 (8)0.0671 (3)0.077 (3)
H3C0.90340.31140.08530.115*
H3D0.87810.25350.05410.115*
H3E0.77440.28350.07670.115*
N40.7481 (11)0.7826 (7)0.0683 (3)0.068 (3)
H4C0.70620.82760.07790.102*
H4D0.73430.78100.04390.102*
H4E0.83070.78890.07310.102*
N50.8929 (11)0.7596 (9)0.0120 (3)0.076 (3)
N60.5861 (13)0.4400 (7)0.0693 (4)0.085 (4)
H6C0.62340.39660.08180.127*
H6D0.55820.42000.04740.127*
H6E0.52110.46040.08200.127*
N70.6387 (13)0.6110 (8)0.0138 (3)0.080 (4)
H7C0.55730.59560.01380.121*
H7D0.67380.59230.00700.121*
H7E0.64490.66910.01510.121*
C10.8604 (10)0.0730 (7)0.0140 (3)0.043 (2)
H1A0.82980.01380.01030.052*
H1B0.93660.08040.00010.052*
C20.9754 (10)0.0273 (7)0.0661 (3)0.044 (2)
H2A1.05120.02860.05140.053*
H2B0.94030.03130.06480.053*
C30.4776 (11)0.6220 (6)0.7593 (3)0.045 (3)
H3A0.52290.60660.78200.055*
H3B0.43010.67520.76380.055*
C40.7647 (9)0.1352 (7)0.0014 (2)0.037 (2)
H4A0.78860.19380.00910.045*
H4B0.75820.13430.02530.045*
C50.7776 (9)0.0840 (7)0.1535 (3)0.042 (2)
H5A0.78340.14460.16120.050*
H5B0.75810.04890.17490.050*
C60.5676 (11)0.6370 (7)0.7299 (3)0.048 (3)
H6A0.52270.65000.70700.058*
H6B0.62180.68620.73620.058*
C70.2302 (9)0.4614 (7)0.7664 (3)0.042 (2)
H7A0.16000.45510.78300.050*
H7B0.19650.46730.74140.050*
C80.3563 (9)0.0031 (7)0.0747 (3)0.043 (2)
H8A0.28100.03150.07880.051*
H8B0.39210.01500.05140.051*
C90.3235 (9)0.0957 (7)0.0731 (3)0.042 (2)
H9A0.25000.10320.05690.050*
H9B0.30070.11520.09760.050*
C100.4330 (10)0.2605 (7)0.1088 (2)0.039 (2)
H10A0.40160.31830.11480.047*
H10B0.39260.21850.12480.047*
C110.3289 (10)0.2381 (7)0.7713 (3)0.042 (2)
H11A0.36950.24720.79530.051*
H11B0.28230.18350.77200.051*
C120.5558 (10)0.1729 (7)0.0061 (3)0.043 (2)
H12A0.55160.17800.02060.052*
H12B0.57640.22990.01630.052*
C130.5999 (10)0.2839 (7)0.1511 (3)0.044 (2)
H13A0.55630.24790.16880.053*
H13B0.57520.34430.15500.053*
C140.4731 (10)0.0986 (6)0.1086 (3)0.046 (3)
H14A0.50450.12280.08580.055*
H14B0.39710.13030.11490.055*
C150.2431 (9)0.3100 (7)0.7630 (3)0.040 (2)
H15A0.21350.30650.73750.048*
H15B0.17030.30740.77880.048*
C160.7234 (10)0.5677 (7)0.6960 (3)0.041 (2)
H16A0.77070.62200.69730.050*
H16B0.67590.56650.67280.050*
C170.7518 (10)0.2623 (7)0.6930 (3)0.046 (3)
H17A0.70670.26420.66940.055*
H17B0.80930.21290.69280.055*
C180.7343 (10)0.2755 (7)0.1571 (3)0.042 (2)
H18A0.77840.31020.13900.050*
H18B0.75750.29730.18140.050*
C190.5680 (10)0.1097 (6)0.1379 (3)0.044 (2)
H19A0.54060.08040.16010.053*
H19B0.57830.17140.14340.053*
C200.4024 (12)0.2398 (7)0.0699 (3)0.052 (3)
H20A0.31410.25380.06490.062*
H20B0.45290.27680.05420.062*
C211.0067 (9)0.0497 (7)0.1044 (3)0.042 (2)
H21A1.07980.01570.11230.050*
H21B1.03050.11100.10540.050*
C220.5137 (10)0.1715 (6)0.7512 (3)0.043 (2)
H22A0.47560.11400.75310.052*
H22B0.55720.18460.77440.052*
C230.8992 (9)0.1786 (7)0.1595 (3)0.045 (3)
H23A0.92720.20970.18160.054*
H23B0.94380.20240.13870.054*
C240.8224 (10)0.3427 (7)0.6986 (3)0.044 (2)
H24A0.86240.34230.72290.052*
H24B0.88830.34670.68040.052*
C250.9278 (9)0.0843 (7)0.1635 (3)0.044 (2)
H25A1.01530.07750.17160.053*
H25B0.87490.05980.18250.053*
C260.3043 (10)0.5380 (7)0.7763 (3)0.044 (2)
H26A0.24880.58810.77860.053*
H26B0.34620.52850.80010.053*
C270.4310 (10)0.1429 (7)0.0200 (3)0.045 (2)
H27A0.36420.17800.00880.055*
H27B0.41720.08250.01270.055*
C280.8094 (9)0.4932 (6)0.6982 (3)0.040 (2)
H28A0.86980.49680.67850.048*
H28B0.85600.49480.72160.048*
C290.8976 (9)0.0564 (7)0.1388 (3)0.042 (2)
H29A0.96370.07050.15680.050*
H29B0.91350.09030.11680.050*
C300.6027 (10)0.1724 (6)0.7214 (3)0.044 (2)
H30A0.66320.12520.72450.053*
H30B0.55830.16450.69790.053*
Rb130.6569 (4)0.6145 (3)0.10223 (8)0.0558 (12)0.74 (2)
Rb140.6416 (11)0.6289 (8)0.1185 (15)0.130 (9)0.26 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0417 (4)0.0373 (4)0.0413 (4)0.0003 (3)0.0037 (3)0.0097 (3)
Sn20.0417 (4)0.0457 (4)0.0294 (3)0.0058 (3)0.0039 (3)0.0026 (3)
Sn30.0406 (4)0.0334 (3)0.0314 (3)0.0037 (3)0.0060 (3)0.0004 (3)
Sn40.0514 (4)0.0332 (3)0.0328 (3)0.0058 (3)0.0047 (3)0.0010 (3)
Sn50.0360 (4)0.0540 (4)0.0335 (3)0.0033 (3)0.0056 (3)0.0003 (3)
Sn60.0515 (4)0.0342 (3)0.0423 (4)0.0078 (3)0.0037 (3)0.0009 (3)
Sn70.0376 (4)0.0585 (4)0.0316 (3)0.0021 (3)0.0013 (3)0.0103 (3)
Sn80.0518 (4)0.0409 (4)0.0381 (4)0.0132 (3)0.0079 (3)0.0045 (3)
Sn90.0474 (4)0.0405 (4)0.0456 (4)0.0082 (3)0.0046 (3)0.0126 (3)
Rb100.0341 (5)0.0319 (4)0.0307 (4)0.0001 (3)0.0001 (3)0.0001 (3)
Rb110.0337 (5)0.0319 (4)0.0266 (4)0.0006 (3)0.0018 (3)0.0005 (3)
Rb120.0672 (8)0.0778 (8)0.0427 (6)0.0158 (6)0.0066 (5)0.0015 (6)
O10.039 (4)0.044 (4)0.038 (4)0.001 (3)0.007 (3)0.002 (3)
O20.040 (4)0.038 (3)0.029 (3)0.007 (3)0.000 (3)0.008 (3)
O30.027 (3)0.045 (4)0.033 (3)0.007 (3)0.000 (3)0.006 (3)
O40.050 (4)0.033 (3)0.036 (4)0.003 (3)0.000 (3)0.003 (3)
O50.052 (4)0.038 (4)0.038 (4)0.002 (3)0.008 (3)0.001 (3)
O60.033 (3)0.044 (4)0.037 (4)0.004 (3)0.005 (3)0.001 (3)
O70.037 (4)0.035 (4)0.055 (4)0.002 (3)0.008 (3)0.008 (3)
O80.039 (4)0.049 (4)0.026 (3)0.004 (3)0.001 (3)0.006 (3)
O90.041 (4)0.045 (4)0.042 (4)0.005 (3)0.003 (3)0.015 (3)
O100.028 (3)0.036 (3)0.041 (4)0.001 (3)0.000 (3)0.003 (3)
O110.049 (4)0.042 (4)0.027 (3)0.002 (3)0.002 (3)0.004 (3)
O120.055 (4)0.032 (4)0.042 (4)0.002 (3)0.010 (3)0.004 (3)
N10.042 (5)0.037 (4)0.027 (4)0.005 (3)0.001 (3)0.001 (3)
N20.030 (4)0.047 (5)0.028 (4)0.003 (3)0.005 (3)0.001 (3)
N30.101 (9)0.082 (8)0.047 (6)0.004 (7)0.002 (6)0.017 (6)
N40.063 (7)0.072 (7)0.068 (7)0.018 (6)0.014 (5)0.019 (6)
N50.058 (7)0.110 (10)0.061 (7)0.032 (7)0.007 (5)0.014 (7)
N60.095 (10)0.055 (7)0.107 (10)0.005 (6)0.041 (8)0.005 (7)
N70.085 (9)0.081 (8)0.076 (8)0.012 (7)0.019 (7)0.011 (7)
C10.043 (6)0.055 (6)0.031 (5)0.008 (5)0.010 (4)0.014 (4)
C20.044 (6)0.052 (6)0.037 (5)0.004 (5)0.006 (4)0.004 (5)
C30.065 (7)0.031 (5)0.040 (5)0.000 (5)0.014 (5)0.007 (4)
C40.030 (5)0.060 (6)0.022 (4)0.004 (4)0.002 (4)0.005 (4)
C50.032 (5)0.048 (6)0.045 (6)0.008 (4)0.002 (4)0.015 (5)
C60.070 (8)0.033 (5)0.041 (6)0.002 (5)0.013 (5)0.003 (4)
C70.035 (5)0.050 (6)0.041 (5)0.007 (4)0.000 (4)0.011 (5)
C80.032 (5)0.054 (6)0.041 (5)0.006 (4)0.012 (4)0.005 (5)
C90.031 (5)0.051 (6)0.041 (5)0.001 (4)0.006 (4)0.003 (5)
C100.044 (6)0.044 (5)0.029 (5)0.011 (4)0.003 (4)0.000 (4)
C110.041 (6)0.053 (6)0.033 (5)0.007 (5)0.002 (4)0.003 (4)
C120.056 (7)0.046 (6)0.026 (5)0.006 (5)0.000 (4)0.003 (4)
C130.052 (6)0.046 (6)0.035 (5)0.001 (5)0.008 (5)0.014 (4)
C140.037 (6)0.031 (5)0.070 (7)0.002 (4)0.010 (5)0.006 (5)
C150.035 (5)0.049 (6)0.037 (5)0.010 (4)0.011 (4)0.007 (4)
C160.051 (6)0.041 (5)0.032 (5)0.011 (5)0.003 (4)0.004 (4)
C170.049 (6)0.047 (6)0.043 (6)0.015 (5)0.016 (5)0.012 (5)
C180.049 (6)0.042 (6)0.034 (5)0.008 (5)0.002 (4)0.010 (4)
C190.045 (6)0.035 (5)0.052 (6)0.001 (4)0.016 (5)0.012 (5)
C200.069 (8)0.042 (6)0.045 (6)0.016 (5)0.014 (5)0.003 (5)
C210.031 (5)0.063 (7)0.030 (5)0.005 (5)0.001 (4)0.008 (4)
C220.050 (6)0.039 (5)0.040 (5)0.005 (4)0.008 (5)0.003 (4)
C230.033 (5)0.063 (7)0.039 (5)0.015 (5)0.003 (4)0.012 (5)
C240.041 (6)0.053 (6)0.036 (5)0.004 (5)0.002 (4)0.008 (4)
C250.026 (5)0.072 (7)0.034 (5)0.007 (5)0.002 (4)0.007 (5)
C260.054 (7)0.047 (6)0.031 (5)0.017 (5)0.003 (4)0.005 (4)
C270.051 (6)0.050 (6)0.035 (5)0.014 (5)0.003 (5)0.000 (5)
C280.038 (5)0.044 (6)0.038 (5)0.012 (4)0.002 (4)0.004 (4)
C290.031 (5)0.057 (6)0.037 (5)0.015 (4)0.006 (4)0.009 (5)
C300.049 (6)0.034 (5)0.049 (6)0.002 (4)0.015 (5)0.004 (4)
Rb130.0371 (13)0.0645 (18)0.066 (2)0.0003 (10)0.0051 (8)0.0027 (10)
Rb140.035 (4)0.075 (5)0.28 (3)0.011 (3)0.002 (9)0.026 (10)
Geometric parameters (Å, º) top
Sn1—Sn32.9295 (12)N6—H6C0.9100
Sn1—Sn22.9334 (11)N6—H6D0.9100
Sn1—Sn42.9344 (12)N6—H6E0.9100
Sn1—Sn52.9553 (11)N7—H7C0.9100
Sn2—Sn92.9623 (11)N7—H7D0.9100
Sn2—Sn62.9954 (11)N7—H7E0.9100
Sn2—Sn33.1206 (11)C1—C41.484 (15)
Sn2—Sn53.1877 (12)C1—H1A0.9900
Sn2—Rb12i3.7080 (16)C1—H1B0.9900
Sn2—Rb12ii3.8625 (17)C2—C211.490 (13)
Sn2—Rb13i4.069 (5)C2—H2A0.9900
Sn3—Sn72.9243 (11)C2—H2B0.9900
Sn3—Sn62.9819 (11)C3—C61.491 (17)
Sn3—Rb14i3.835 (16)C3—H3A0.9900
Sn3—Rb13i3.932 (3)C3—H3B0.9900
Sn4—Sn82.9594 (11)C4—H4A0.9900
Sn4—Sn72.9687 (11)C4—H4B0.9900
Sn4—Sn53.1106 (11)C5—C291.478 (14)
Sn4—Rb103.8784 (14)C5—H5A0.9900
Sn4—Rb14iii4.21 (2)C5—H5B0.9900
Sn5—Sn92.9942 (12)C6—H6A0.9900
Sn5—Sn83.0252 (11)C6—H6B0.9900
Sn5—Rb13iii3.872 (4)C7—C261.479 (15)
Sn5—Rb12ii3.8829 (17)C7—H7A0.9900
Sn5—Rb14iii3.90 (2)C7—H7B0.9900
Sn6—Sn72.9382 (13)C8—C91.489 (15)
Sn6—Sn92.9642 (14)C8—H8A0.9900
Sn6—Sn83.9689 (14)C8—H8B0.9900
Sn6—Rb13i3.974 (5)C9—H9A0.9900
Sn6—Rb14i4.109 (11)C9—H9B0.9900
Sn7—Sn82.9561 (13)C10—C201.503 (15)
Sn7—Rb103.7474 (15)C10—H10A0.9900
Sn8—Rb14iii3.93 (2)C10—H10B0.9900
Sn8—Rb103.9814 (14)C11—C151.483 (15)
Sn8—Rb13iii4.171 (4)C11—H11A0.9900
Sn9—Rb12ii4.0597 (16)C11—H11B0.9900
Rb10—O52.869 (7)C12—C271.525 (16)
Rb10—O72.876 (7)C12—H12A0.9900
Rb10—O122.882 (7)C12—H12B0.9900
Rb10—O63.010 (6)C13—C181.467 (15)
Rb10—O43.071 (7)C13—H13A0.9900
Rb10—O23.122 (7)C13—H13B0.9900
Rb11—O92.873 (7)C14—C191.483 (15)
Rb11—O32.875 (6)C14—H14A0.9900
Rb11—O102.891 (6)C14—H14B0.9900
Rb11—O12.896 (7)C15—H15A0.9900
Rb11—O82.915 (7)C15—H15B0.9900
Rb11—O112.922 (6)C16—C281.488 (15)
Rb11—N13.004 (8)C16—H16A0.9900
Rb11—N23.032 (8)C16—H16B0.9900
Rb12—N32.992 (12)C17—C241.479 (15)
Rb12—Sn2i3.7080 (16)C17—H17A0.9900
Rb12—Sn2iv3.8625 (17)C17—H17B0.9900
Rb12—Sn5iv3.8829 (17)C18—H18A0.9900
Rb12—Sn9iv4.0597 (16)C18—H18B0.9900
O1—C101.418 (12)C19—H19A0.9900
O1—C131.460 (12)C19—H19B0.9900
O2—C111.425 (12)C20—H20A0.9900
O2—C221.430 (12)C20—H20B0.9900
O3—C191.407 (12)C21—H21A0.9900
O3—C51.412 (11)C21—H21B0.9900
O4—C31.413 (12)C22—C301.477 (16)
O4—C261.437 (12)C22—H22A0.9900
O5—C61.421 (13)C22—H22B0.9900
O5—C161.448 (12)C23—C251.511 (16)
O6—C241.420 (12)C23—H23A0.9900
O6—C281.423 (12)C23—H23B0.9900
O7—C71.426 (12)C24—H24A0.9900
O7—C151.426 (12)C24—H24B0.9900
O8—C21.414 (12)C25—H25A0.9900
O8—C11.450 (11)C25—H25B0.9900
O9—C181.396 (12)C26—H26A0.9900
O9—C231.425 (13)C26—H26B0.9900
O10—C141.421 (11)C27—H27A0.9900
O10—C81.426 (11)C27—H27B0.9900
O11—C121.413 (12)C28—H28A0.9900
O11—C41.428 (12)C28—H28B0.9900
O12—C301.421 (12)C29—H29A0.9900
O12—C171.442 (12)C29—H29B0.9900
N1—C91.460 (13)C30—H30A0.9900
N1—C201.476 (13)C30—H30B0.9900
N1—C271.489 (12)Rb13—Sn5iii3.872 (4)
N2—C211.453 (13)Rb13—Sn3i3.932 (3)
N2—C291.473 (13)Rb13—Sn6i3.974 (5)
N2—C251.480 (12)Rb13—Sn2i4.069 (5)
N3—H3C0.9100Rb13—Sn8iii4.171 (4)
N3—H3D0.9100Rb14—Sn3i3.835 (15)
N3—H3E0.9100Rb14—Sn5iii3.90 (2)
N4—Rb133.077 (13)Rb14—Sn8iii3.933 (19)
N4—H4C0.9100Rb14—Sn6i4.109 (11)
N4—H4D0.9100Rb14—Sn4iii4.21 (2)
N4—H4E0.9100
Sn3—Sn1—Sn264.32 (3)C18—O9—C23111.8 (8)
Sn3—Sn1—Sn469.57 (3)C18—O9—Rb11117.6 (6)
Sn2—Sn1—Sn499.82 (3)C23—O9—Rb11114.4 (5)
Sn3—Sn1—Sn5100.90 (3)C14—O10—C8112.7 (8)
Sn2—Sn1—Sn565.55 (3)C14—O10—Rb11111.9 (5)
Sn4—Sn1—Sn563.76 (3)C8—O10—Rb11111.7 (5)
Sn1—Sn2—Sn9110.91 (3)C12—O11—C4110.9 (7)
Sn1—Sn2—Sn6109.27 (3)C12—O11—Rb11111.6 (5)
Sn9—Sn2—Sn659.67 (3)C4—O11—Rb11112.1 (5)
Sn1—Sn2—Sn357.78 (3)C30—O12—C17113.4 (8)
Sn9—Sn2—Sn3103.03 (3)C30—O12—Rb10123.1 (6)
Sn6—Sn2—Sn358.32 (3)C17—O12—Rb10120.1 (5)
Sn1—Sn2—Sn557.56 (3)C9—N1—C20110.1 (8)
Sn9—Sn2—Sn558.13 (3)C9—N1—C27109.9 (8)
Sn6—Sn2—Sn598.66 (4)C20—N1—C27108.7 (8)
Sn3—Sn2—Sn591.99 (4)C9—N1—Rb11109.3 (5)
Sn1—Sn2—Rb12i163.26 (3)C20—N1—Rb11108.5 (7)
Sn9—Sn2—Rb12i83.68 (4)C27—N1—Rb11110.2 (6)
Sn6—Sn2—Rb12i84.88 (3)C21—N2—C29111.0 (8)
Sn3—Sn2—Rb12i128.68 (4)C21—N2—C25111.5 (8)
Sn5—Sn2—Rb12i130.86 (4)C29—N2—C25108.5 (8)
Sn1—Sn2—Rb12ii102.44 (3)C21—N2—Rb11108.9 (5)
Sn9—Sn2—Rb12ii71.63 (3)C29—N2—Rb11108.4 (5)
Sn6—Sn2—Rb12ii128.50 (4)C25—N2—Rb11108.4 (6)
Sn3—Sn2—Rb12ii157.10 (3)Rb12—N3—H3C109.5
Sn5—Sn2—Rb12ii66.03 (4)Rb12—N3—H3D109.5
Rb12i—Sn2—Rb12ii73.68 (4)H3C—N3—H3D109.5
Sn1—Sn2—Rb13i108.41 (7)Rb12—N3—H3E109.5
Sn9—Sn2—Rb13i120.72 (7)H3C—N3—H3E109.5
Sn6—Sn2—Rb13i66.46 (6)H3D—N3—H3E109.5
Sn3—Sn2—Rb13i64.74 (5)Rb13—N4—H4C109.5
Sn5—Sn2—Rb13i156.38 (5)Rb13—N4—H4D109.5
Rb12i—Sn2—Rb13i68.33 (6)H4C—N4—H4D109.5
Rb12ii—Sn2—Rb13i137.55 (5)Rb13—N4—H4E109.5
Sn7—Sn3—Sn1107.93 (3)H4C—N4—H4E109.5
Sn7—Sn3—Sn659.66 (3)H4D—N4—H4E109.5
Sn1—Sn3—Sn6109.75 (3)H6C—N6—H6D109.5
Sn7—Sn3—Sn2101.23 (3)H6C—N6—H6E109.5
Sn1—Sn3—Sn257.90 (3)H6D—N6—H6E109.5
Sn6—Sn3—Sn258.74 (2)H7C—N7—H7D109.5
Sn7—Sn3—Rb14i121.4 (4)H7C—N7—H7E109.5
Sn1—Sn3—Rb14i119.6 (8)H7D—N7—H7E109.5
Sn6—Sn3—Rb14i72.9 (2)O8—C1—C4109.5 (8)
Sn2—Sn3—Rb14i79.1 (8)O8—C1—Rb1146.7 (4)
Sn7—Sn3—Rb13i122.33 (7)C4—C1—Rb1178.2 (5)
Sn1—Sn3—Rb13i112.08 (5)O8—C1—H1A109.8
Sn6—Sn3—Rb13i68.59 (8)C4—C1—H1A109.8
Sn2—Sn3—Rb13i69.38 (7)Rb11—C1—H1A89.7
Rb14i—Sn3—Rb13i9.7 (7)O8—C1—H1B109.8
Sn1—Sn4—Sn8110.21 (3)C4—C1—H1B109.8
Sn1—Sn4—Sn7106.63 (3)Rb11—C1—H1B155.4
Sn8—Sn4—Sn759.82 (3)H1A—C1—H1B108.2
Sn1—Sn4—Sn558.45 (3)O8—C2—C21109.1 (8)
Sn8—Sn4—Sn559.73 (2)O8—C2—Rb1147.1 (4)
Sn7—Sn4—Sn5102.26 (3)C21—C2—Rb1181.4 (6)
Sn1—Sn4—Rb10170.49 (3)O8—C2—H2A109.9
Sn8—Sn4—Rb1069.74 (2)C21—C2—H2A109.9
Sn7—Sn4—Rb1064.78 (3)Rb11—C2—H2A156.9
Sn5—Sn4—Rb10125.76 (3)O8—C2—H2B109.9
Sn1—Sn4—Rb14iii109.5 (7)C21—C2—H2B109.9
Sn8—Sn4—Rb14iii63.80 (18)Rb11—C2—H2B85.3
Sn7—Sn4—Rb14iii120.3 (3)H2A—C2—H2B108.3
Sn5—Sn4—Rb14iii62.3 (7)O4—C3—C6110.0 (8)
Rb10—Sn4—Rb14iii79.2 (7)O4—C3—Rb1057.7 (5)
Sn1—Sn5—Sn9109.42 (3)C6—C3—Rb1087.4 (6)
Sn1—Sn5—Sn8107.85 (3)O4—C3—H3A109.7
Sn9—Sn5—Sn858.60 (3)C6—C3—H3A109.7
Sn1—Sn5—Sn457.79 (3)Rb10—C3—H3A68.9
Sn9—Sn5—Sn4101.86 (3)O4—C3—H3B109.7
Sn8—Sn5—Sn457.65 (3)C6—C3—H3B109.7
Sn1—Sn5—Sn256.90 (2)Rb10—C3—H3B162.2
Sn9—Sn5—Sn257.16 (2)H3A—C3—H3B108.2
Sn8—Sn5—Sn296.26 (4)O11—C4—C1109.4 (8)
Sn4—Sn5—Sn290.91 (4)O11—C4—Rb1147.0 (4)
Sn1—Sn5—Rb13iii124.54 (8)C1—C4—Rb1178.7 (5)
Sn9—Sn5—Rb13iii116.00 (7)O11—C4—H4A109.8
Sn8—Sn5—Rb13iii73.25 (5)C1—C4—H4A109.8
Sn4—Sn5—Rb13iii82.57 (7)Rb11—C4—H4A88.7
Sn2—Sn5—Rb13iii169.45 (5)O11—C4—H4B109.8
Sn1—Sn5—Rb12ii101.55 (4)C1—C4—H4B109.8
Sn9—Sn5—Rb12ii71.02 (3)Rb11—C4—H4B156.0
Sn8—Sn5—Rb12ii127.48 (4)H4A—C4—H4B108.2
Sn4—Sn5—Rb12ii155.55 (3)O3—C5—C29110.6 (8)
Sn2—Sn5—Rb12ii65.36 (4)O3—C5—Rb1145.1 (4)
Rb13iii—Sn5—Rb12ii121.77 (7)C29—C5—Rb1181.4 (5)
Sn1—Sn5—Rb14iii117.4 (5)O3—C5—H5A109.5
Sn9—Sn5—Rb14iii116.7 (3)C29—C5—H5A109.5
Sn8—Sn5—Rb14iii67.8 (6)Rb11—C5—H5A154.1
Sn4—Sn5—Rb14iii72.7 (7)O3—C5—H5B109.5
Sn2—Sn5—Rb14iii161.5 (8)C29—C5—H5B109.5
Rb13iii—Sn5—Rb14iii9.8 (7)Rb11—C5—H5B89.0
Rb12ii—Sn5—Rb14iii131.6 (7)H5A—C5—H5B108.1
Sn7—Sn6—Sn995.23 (3)O5—C6—C3108.2 (8)
Sn7—Sn6—Sn359.20 (2)O5—C6—H6A110.1
Sn9—Sn6—Sn3106.44 (3)C3—C6—H6A110.1
Sn7—Sn6—Sn2103.94 (3)O5—C6—H6B110.1
Sn9—Sn6—Sn259.61 (3)C3—C6—H6B110.1
Sn3—Sn6—Sn262.94 (2)H6A—C6—H6B108.4
Sn7—Sn6—Sn847.87 (3)O7—C7—C26108.2 (8)
Sn9—Sn6—Sn847.62 (3)O7—C7—H7A110.1
Sn3—Sn6—Sn883.61 (2)C26—C7—H7A110.1
Sn2—Sn6—Sn882.00 (3)O7—C7—H7B110.1
Sn7—Sn6—Rb13i120.59 (7)C26—C7—H7B110.1
Sn9—Sn6—Rb13i123.69 (6)H7A—C7—H7B108.4
Sn3—Sn6—Rb13i67.09 (6)O10—C8—C9109.1 (8)
Sn2—Sn6—Rb13i69.83 (5)O10—C8—Rb1147.1 (4)
Sn8—Sn6—Rb13i146.05 (6)C9—C8—Rb1181.5 (5)
Sn7—Sn6—Rb14i113.0 (6)O10—C8—H8A109.9
Sn9—Sn6—Rb14i132.2 (7)C9—C8—H8A109.9
Sn3—Sn6—Rb14i63.2 (3)Rb11—C8—H8A156.9
Sn2—Sn6—Rb14i76.1 (6)O10—C8—H8B109.9
Sn8—Sn6—Rb14i145.81 (19)C9—C8—H8B109.9
Rb13i—Sn6—Rb14i9.3 (7)Rb11—C8—H8B85.3
Sn3—Sn7—Sn661.15 (3)H8A—C8—H8B108.3
Sn3—Sn7—Sn8105.84 (3)N1—C9—C8113.1 (8)
Sn6—Sn7—Sn884.65 (3)N1—C9—Rb1149.1 (4)
Sn3—Sn7—Sn469.18 (3)C8—C9—Rb1175.3 (5)
Sn6—Sn7—Sn4105.80 (3)N1—C9—H9A109.0
Sn8—Sn7—Sn459.93 (3)C8—C9—H9A109.0
Sn3—Sn7—Rb10132.34 (3)Rb11—C9—H9A154.3
Sn6—Sn7—Rb10155.13 (3)N1—C9—H9B109.0
Sn8—Sn7—Rb1071.77 (3)C8—C9—H9B109.0
Sn4—Sn7—Rb1069.44 (3)Rb11—C9—H9B93.9
Sn3—Sn7—Sn978.97 (3)H9A—C9—H9B107.8
Sn6—Sn7—Sn942.61 (2)O1—C10—C20109.4 (8)
Sn8—Sn7—Sn942.29 (3)O1—C10—Rb1147.3 (4)
Sn4—Sn7—Sn978.07 (3)C20—C10—Rb1181.4 (6)
Rb10—Sn7—Sn9114.02 (3)O1—C10—H10A109.8
Sn9—Sn8—Sn795.24 (3)C20—C10—H10A109.8
Sn9—Sn8—Sn4106.78 (3)Rb11—C10—H10A157.0
Sn7—Sn8—Sn460.25 (2)O1—C10—H10B109.8
Sn9—Sn8—Sn560.17 (3)C20—C10—H10B109.8
Sn7—Sn8—Sn5104.64 (3)Rb11—C10—H10B85.4
Sn4—Sn8—Sn562.62 (3)H10A—C10—H10B108.2
Sn9—Sn8—Rb14iii117.0 (8)O2—C11—C15108.7 (8)
Sn7—Sn8—Rb14iii129.9 (5)O2—C11—Rb1055.7 (5)
Sn4—Sn8—Rb14iii73.7 (3)C15—C11—Rb1083.8 (6)
Sn5—Sn8—Rb14iii66.7 (6)O2—C11—H11A110.0
Sn9—Sn8—Sn648.01 (3)C15—C11—H11A110.0
Sn7—Sn8—Sn647.48 (3)Rb10—C11—H11A73.4
Sn4—Sn8—Sn684.34 (2)O2—C11—H11B110.0
Sn5—Sn8—Sn683.08 (3)C15—C11—H11B110.0
Rb14iii—Sn8—Sn6148.3 (4)Rb10—C11—H11B163.7
Sn9—Sn8—Rb10158.47 (3)H11A—C11—H11B108.3
Sn7—Sn8—Rb1063.38 (3)O11—C12—C27109.1 (8)
Sn4—Sn8—Rb1066.05 (2)O11—C12—Rb1147.5 (4)
Sn5—Sn8—Rb10124.99 (3)C27—C12—Rb1182.0 (5)
Rb14iii—Sn8—Rb1081.4 (8)O11—C12—H12A109.9
Sn6—Sn8—Rb10110.47 (4)C27—C12—H12A109.9
Sn9—Sn8—Rb13iii109.12 (5)Rb11—C12—H12A157.4
Sn7—Sn8—Rb13iii137.51 (8)O11—C12—H12B109.9
Sn4—Sn8—Rb13iii79.26 (8)C27—C12—H12B109.9
Sn5—Sn8—Rb13iii62.75 (6)Rb11—C12—H12B84.3
Rb14iii—Sn8—Rb13iii8.8 (7)H12A—C12—H12B108.3
Sn6—Sn8—Rb13iii145.82 (5)O1—C13—C18111.2 (8)
Rb10—Sn8—Rb13iii89.94 (5)O1—C13—Rb1146.1 (4)
Sn8—Sn9—Sn2103.12 (3)C18—C13—Rb1179.4 (5)
Sn8—Sn9—Sn684.37 (3)O1—C13—H13A109.4
Sn2—Sn9—Sn660.72 (3)C18—C13—H13A109.4
Sn8—Sn9—Sn561.23 (3)Rb11—C13—H13A90.7
Sn2—Sn9—Sn564.71 (3)O1—C13—H13B109.4
Sn6—Sn9—Sn5103.88 (3)C18—C13—H13B109.4
Sn8—Sn9—Rb12ii123.97 (4)Rb11—C13—H13B154.2
Sn2—Sn9—Rb12ii64.54 (3)H13A—C13—H13B108.0
Sn6—Sn9—Rb12ii122.78 (4)O10—C14—C19110.9 (8)
Sn5—Sn9—Rb12ii64.75 (3)O10—C14—Rb1147.0 (4)
Sn8—Sn9—Sn742.47 (2)C19—C14—Rb1179.2 (5)
Sn2—Sn9—Sn776.71 (3)O10—C14—H14A109.5
Sn6—Sn9—Sn742.15 (3)C19—C14—H14A109.5
Sn5—Sn9—Sn777.70 (3)Rb11—C14—H14A89.4
Rb12ii—Sn9—Sn7134.33 (3)O10—C14—H14B109.5
O5—Rb10—O7112.5 (2)C19—C14—H14B109.5
O5—Rb10—O12114.23 (19)Rb11—C14—H14B155.5
O7—Rb10—O12111.1 (2)H14A—C14—H14B108.0
O5—Rb10—O656.70 (19)O7—C15—C11107.9 (8)
O7—Rb10—O6137.0 (2)O7—C15—H15A110.1
O12—Rb10—O657.70 (18)C11—C15—H15A110.1
O5—Rb10—O456.04 (19)O7—C15—H15B110.1
O7—Rb10—O457.46 (19)C11—C15—H15B110.1
O12—Rb10—O4143.19 (19)H15A—C15—H15B108.4
O6—Rb10—O4104.59 (18)O5—C16—C28107.6 (8)
O5—Rb10—O2142.60 (18)O5—C16—H16A110.2
O7—Rb10—O256.43 (18)C28—C16—H16A110.2
O12—Rb10—O255.43 (19)O5—C16—H16B110.2
O6—Rb10—O2104.61 (17)C28—C16—H16B110.2
O4—Rb10—O2108.20 (17)H16A—C16—H16B108.5
O5—Rb10—C341.0 (2)O12—C17—C24109.0 (8)
O7—Rb10—C377.8 (2)O12—C17—H17A109.9
O12—Rb10—C3151.7 (2)C24—C17—H17A109.9
O6—Rb10—C396.9 (2)O12—C17—H17B109.9
O4—Rb10—C322.9 (2)C24—C17—H17B109.9
O2—Rb10—C3131.0 (2)H17A—C17—H17B108.3
O5—Rb10—C2476.5 (2)O9—C18—C13109.9 (8)
O7—Rb10—C24144.0 (2)C13—C18—Rb1177.8 (5)
O12—Rb10—C2440.6 (2)O9—C18—H18A109.7
O6—Rb10—C2422.1 (2)C13—C18—H18A109.7
O4—Rb10—C24126.6 (2)Rb11—C18—H18A95.5
O2—Rb10—C2494.5 (2)O9—C18—H18B109.7
C3—Rb10—C24117.5 (3)C13—C18—H18B109.7
O5—Rb10—C22150.3 (2)Rb11—C18—H18B150.1
O7—Rb10—C2276.7 (2)H18A—C18—H18B108.2
O12—Rb10—C2240.0 (2)O3—C19—C14110.0 (8)
O6—Rb10—C2296.7 (2)O3—C19—Rb1145.2 (4)
O4—Rb10—C22130.8 (2)C14—C19—Rb1177.5 (5)
O2—Rb10—C2222.7 (2)O3—C19—H19A109.7
C3—Rb10—C22153.5 (3)C14—C19—H19A109.7
C24—Rb10—C2280.5 (2)Rb11—C19—H19A93.1
O5—Rb10—C2677.3 (2)O3—C19—H19B109.7
O7—Rb10—C2640.1 (2)C14—C19—H19B109.7
O12—Rb10—C26147.1 (2)Rb11—C19—H19B152.7
O6—Rb10—C26126.9 (2)H19A—C19—H19B108.2
O4—Rb10—C2622.6 (2)N1—C20—C10114.0 (9)
O2—Rb10—C2696.0 (2)N1—C20—Rb1149.5 (5)
C3—Rb10—C2638.4 (3)C10—C20—Rb1175.2 (6)
C24—Rb10—C26148.7 (2)N1—C20—H20A108.8
C22—Rb10—C26116.8 (3)C10—C20—H20A108.8
O5—Rb10—C11147.5 (2)Rb11—C20—H20A154.0
O7—Rb10—C1139.5 (2)N1—C20—H20B108.8
O12—Rb10—C1176.1 (2)C10—C20—H20B108.8
O6—Rb10—C11126.5 (2)Rb11—C20—H20B94.6
O4—Rb10—C1196.5 (2)H20A—C20—H20B107.7
O2—Rb10—C1122.1 (2)N2—C21—C2114.8 (8)
C3—Rb10—C11117.4 (3)N2—C21—H21A108.6
C24—Rb10—C11116.2 (2)C2—C21—H21A108.6
C22—Rb10—C1137.8 (2)N2—C21—H21B108.6
C26—Rb10—C1179.3 (2)C2—C21—H21B108.6
O5—Rb10—C2839.6 (2)H21A—C21—H21B107.5
O7—Rb10—C28143.5 (2)O2—C22—C30108.8 (8)
O12—Rb10—C2877.1 (2)O2—C22—Rb1057.3 (4)
O6—Rb10—C2821.3 (2)C30—C22—Rb1086.1 (6)
O4—Rb10—C2894.0 (2)O2—C22—H22A109.9
O2—Rb10—C28125.8 (2)C30—C22—H22A109.9
C3—Rb10—C2880.6 (3)Rb10—C22—H22A162.9
C24—Rb10—C2837.2 (2)O2—C22—H22B109.9
C22—Rb10—C28116.9 (2)C30—C22—H22B109.9
C26—Rb10—C28116.3 (2)Rb10—C22—H22B70.0
C11—Rb10—C28147.4 (2)H22A—C22—H22B108.3
O9—Rb11—O398.3 (2)O9—C23—C25109.3 (8)
O9—Rb11—O10121.43 (19)O9—C23—Rb1145.0 (4)
O3—Rb11—O1059.79 (18)C25—C23—Rb1181.0 (5)
O9—Rb11—O159.0 (2)O9—C23—H23A109.8
O3—Rb11—O1136.72 (18)C25—C23—H23A109.8
O10—Rb11—O198.80 (19)Rb11—C23—H23A154.5
O9—Rb11—O896.40 (19)O9—C23—H23B109.8
O3—Rb11—O898.59 (18)C25—C23—H23B109.8
O10—Rb11—O8137.29 (18)Rb11—C23—H23B88.3
O1—Rb11—O8118.80 (19)H23A—C23—H23B108.3
O9—Rb11—O11135.5 (2)O6—C24—C17110.5 (9)
O3—Rb11—O11120.77 (18)O6—C24—Rb1052.8 (4)
O10—Rb11—O1197.86 (19)C17—C24—Rb1084.9 (6)
O1—Rb11—O1197.78 (19)O6—C24—H24A109.6
O8—Rb11—O1159.82 (19)C17—C24—H24A109.6
O9—Rb11—N1119.5 (2)Rb10—C24—H24A76.5
O3—Rb11—N1119.6 (2)O6—C24—H24B109.6
O10—Rb11—N160.5 (2)C17—C24—H24B109.6
O1—Rb11—N161.2 (2)Rb10—C24—H24B161.3
O8—Rb11—N1119.54 (19)H24A—C24—H24B108.1
O11—Rb11—N160.6 (2)N2—C25—C23113.3 (8)
O9—Rb11—N260.7 (2)N2—C25—H25A108.9
O3—Rb11—N260.6 (2)C23—C25—H25A108.9
O10—Rb11—N2119.8 (2)N2—C25—H25B108.9
O1—Rb11—N2118.9 (2)C23—C25—H25B108.9
O8—Rb11—N260.08 (19)H25A—C25—H25B107.7
O11—Rb11—N2119.1 (2)O4—C26—C7110.6 (8)
N1—Rb11—N2179.6 (2)O4—C26—Rb1055.2 (4)
O9—Rb11—C1076.9 (2)C7—C26—Rb1084.8 (5)
O3—Rb11—C10129.2 (2)O4—C26—H26A109.5
O10—Rb11—C1079.5 (2)C7—C26—H26A109.5
O1—Rb11—C1021.1 (2)Rb10—C26—H26A163.0
O8—Rb11—C10132.2 (2)O4—C26—H26B109.5
O11—Rb11—C1091.9 (2)C7—C26—H26B109.5
N1—Rb11—C1042.6 (2)Rb10—C26—H26B74.1
N2—Rb11—C10137.6 (2)H26A—C26—H26B108.1
O9—Rb11—C14122.5 (2)N1—C27—C12112.3 (9)
O3—Rb11—C1440.2 (2)N1—C27—H27A109.2
O10—Rb11—C1421.1 (2)C12—C27—H27A109.2
O1—Rb11—C14118.2 (2)N1—C27—H27B109.2
O8—Rb11—C14121.7 (2)C12—C27—H27B109.2
O11—Rb11—C14101.8 (2)H27A—C27—H27B107.9
N1—Rb11—C1479.4 (2)O6—C28—C16110.7 (8)
N2—Rb11—C14100.8 (2)O6—C28—Rb1050.2 (4)
C10—Rb11—C14100.1 (2)C16—C28—Rb1084.0 (5)
O9—Rb11—C8134.1 (2)O6—C28—H28A109.5
O3—Rb11—C877.9 (2)C16—C28—H28A109.5
O10—Rb11—C821.2 (2)Rb10—C28—H28A159.5
O1—Rb11—C892.6 (2)O6—C28—H28B109.5
O8—Rb11—C8129.4 (2)C16—C28—H28B109.5
O11—Rb11—C878.7 (2)Rb10—C28—H28B80.3
N1—Rb11—C841.8 (2)H28A—C28—H28B108.1
N2—Rb11—C8138.4 (2)N2—C29—C5115.9 (8)
C10—Rb11—C871.5 (2)N2—C29—H29A108.3
C14—Rb11—C837.7 (2)C5—C29—H29A108.3
O9—Rb11—C12127.7 (2)N2—C29—H29B108.3
O3—Rb11—C12134.0 (2)C5—C29—H29B108.3
O10—Rb11—C1292.3 (2)H29A—C29—H29B107.4
O1—Rb11—C1278.7 (2)O12—C30—C22108.3 (8)
O8—Rb11—C1277.2 (2)O12—C30—H30A110.0
O11—Rb11—C1220.9 (2)C22—C30—H30A110.0
N1—Rb11—C1242.4 (2)O12—C30—H30B110.0
N2—Rb11—C12137.2 (2)C22—C30—H30B110.0
C10—Rb11—C1271.1 (2)H30A—C30—H30B108.4
C14—Rb11—C12103.3 (2)Rb14—Rb13—N499.7 (19)
C8—Rb11—C1271.2 (2)Rb14—Rb13—Sn5iii87.6 (17)
N3—Rb12—Sn2i99.2 (2)N4—Rb13—Sn5iii101.4 (2)
N3—Rb12—Sn2iv105.1 (2)Rb14—Rb13—Sn3i76.9 (14)
Sn2i—Rb12—Sn2iv106.32 (4)N4—Rb13—Sn3i69.2 (2)
N3—Rb12—Sn5iv110.5 (2)Sn5iii—Rb13—Sn3i159.77 (16)
Sn2i—Rb12—Sn5iv144.75 (4)Rb14—Rb13—Sn6i97 (2)
Sn2iv—Rb12—Sn5iv48.60 (2)N4—Rb13—Sn6i104.0 (2)
N3—Rb12—Sn9iv147.0 (2)Sn5iii—Rb13—Sn6i153.00 (12)
Sn2i—Rb12—Sn9iv100.78 (4)Sn3i—Rb13—Sn6i44.32 (5)
Sn2iv—Rb12—Sn9iv43.83 (2)Rb14—Rb13—Sn2i122.7 (14)
Sn5iv—Rb12—Sn9iv44.22 (2)N4—Rb13—Sn2i65.8 (2)
N3—Rb12—Rb1395.0 (2)Sn5iii—Rb13—Sn2i147.86 (8)
Sn2i—Rb12—Rb1359.74 (5)Sn3i—Rb13—Sn2i45.88 (5)
Sn2iv—Rb12—Rb13157.50 (6)Sn6i—Rb13—Sn2i43.71 (5)
Sn5iv—Rb12—Rb13132.44 (6)Rb14—Rb13—Sn8iii64.7 (13)
Sn9iv—Rb12—Rb13117.68 (6)N4—Rb13—Sn8iii139.2 (3)
N3—Rb12—Rb12v110.7 (3)Sn5iii—Rb13—Sn8iii43.99 (4)
Sn2i—Rb12—Rb12v54.72 (3)Sn3i—Rb13—Sn8iii133.95 (7)
Sn2iv—Rb12—Rb12v51.60 (3)Sn6i—Rb13—Sn8iii114.86 (9)
Sn5iv—Rb12—Rb12v95.99 (4)Sn2i—Rb13—Sn8iii154.80 (14)
Sn9iv—Rb12—Rb12v62.56 (4)Rb14—Rb13—Rb12160 (2)
Rb13—Rb12—Rb12v111.99 (6)N4—Rb13—Rb1294.5 (2)
N3—Rb12—Rb1492.5 (4)Sn5iii—Rb13—Rb12103.20 (8)
Sn2i—Rb12—Rb1459.39 (15)Sn3i—Rb13—Rb1295.55 (11)
Sn2iv—Rb12—Rb14159.3 (3)Sn6i—Rb13—Rb1265.89 (9)
Sn5iv—Rb12—Rb14134.4 (3)Sn2i—Rb13—Rb1251.93 (7)
Sn9iv—Rb12—Rb14120.2 (4)Sn8iii—Rb13—Rb12111.90 (10)
Rb13—Rb12—Rb142.6 (4)Rb13—Rb14—Sn3i93.4 (12)
Rb12v—Rb12—Rb14112.35 (15)Rb13—Rb14—Sn5iii83 (2)
C10—O1—C13112.2 (7)Sn3i—Rb14—Sn5iii166.4 (10)
C10—O1—Rb11111.6 (5)Rb13—Rb14—Sn8iii106.4 (15)
C13—O1—Rb11112.6 (6)Sn3i—Rb14—Sn8iii147.5 (13)
C11—O2—C22113.1 (7)Sn5iii—Rb14—Sn8iii45.43 (13)
C11—O2—Rb10102.2 (5)Rb13—Rb14—Sn6i73.7 (14)
C22—O2—Rb10100.1 (5)Sn3i—Rb14—Sn6i43.92 (13)
C19—O3—C5113.4 (7)Sn5iii—Rb14—Sn6i144.5 (8)
C19—O3—Rb11114.5 (5)Sn8iii—Rb14—Sn6i117.2 (5)
C5—O3—Rb11114.5 (6)Rb13—Rb14—Sn4iii127 (2)
C3—O4—C26113.2 (8)Sn3i—Rb14—Sn4iii136.6 (12)
C3—O4—Rb1099.4 (6)Sn5iii—Rb14—Sn4iii44.92 (14)
C26—O4—Rb10102.2 (5)Sn8iii—Rb14—Sn4iii42.5 (2)
C6—O5—C16112.0 (8)Sn6i—Rb14—Sn4iii150.3 (12)
C6—O5—Rb10122.0 (6)Sn3i—Rb14—Rb1287.2 (6)
C16—O5—Rb10123.2 (5)Sn5iii—Rb14—Rb1292.3 (9)
C24—O6—C28111.7 (7)Sn8iii—Rb14—Rb12104.1 (6)
C24—O6—Rb10105.1 (5)Sn6i—Rb14—Rb1258.9 (4)
C28—O6—Rb10108.5 (5)Sn4iii—Rb14—Rb12136.2 (8)
C7—O7—C15112.4 (7)Sn3i—Rb14—Rb10iii103.2 (11)
C7—O7—Rb10121.3 (6)Sn5iii—Rb14—Rb10iii85.7 (5)
C15—O7—Rb10122.1 (5)Sn8iii—Rb14—Rb10iii49.7 (5)
C2—O8—C1112.1 (7)Sn6i—Rb14—Rb10iii103.5 (9)
C2—O8—Rb11112.0 (5)Sn4iii—Rb14—Rb10iii47.6 (5)
C1—O8—Rb11112.0 (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, z1; (v) x+2, y+1, z.

Experimental details

Crystal data
Chemical formula[Rb(C12H24O6)][Rb3Sn9(C18H36N2O6)]·5NH3
Mr2136.04
Crystal system, space groupMonoclinic, P21/n
Temperature (K)123
a, b, c (Å)10.790 (2), 15.600 (3), 36.960 (7)
β (°) 91.20 (3)
V3)6220 (2)
Z4
Radiation typeMo Kα
µ (mm1)6.75
Crystal size (mm)0.25 × 0.2 × 0.15
Data collection
DiffractometerStoe IPDS
diffractometer
Absorption correctionAnalytical
(X-SHAPE; Stoe & Cie, 2002)
Tmin, Tmax0.057, 0.119
No. of measured, independent and
observed [I > 2σ(I)] reflections
36425, 11435, 7473
Rint0.099
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.112, 0.84
No. of reflections11435
No. of parameters608
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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

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ISSN: 2056-9890
Volume 67| Part 5| May 2011| Pages m613-m614
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