Cs5Sn9(OH)·4NH3

Friedrich, U.; Korber, N.

doi:10.1107/S1600536814011817

inorganic compounds

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ISSN: 2056-9890

Volume 70| Part 6| June 2014| Page i29

doi:10.1107/S1600536814011817

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Cs₅Sn₉(OH)·4NH₃

Ute Friedrich ^a and Nikolaus Korber ^a ^*

^aInstitut für Anorganische Chemie, Universität Regensburg, Universitätsstrasse 31, 93053 Regensburg, Germany
^*Correspondence e-mail: nikolaus.korber@chemie.uni-regensburg.de

(Received 25 April 2014; accepted 21 May 2014; online 31 May 2014)

The title compound, pentacaesium nonastannide hydroxide tetraammonia, crystallized from a solution of CsSnBi in liquid ammonia. The Sn₉⁴⁻ unit forms a monocapped quadratic antiprism. The hydroxide ion is surrounded by five caesium cations, which form a distorted quadratic pyramidal polyhedron. A three-dimensional network is formed by Cs—Sn [3.8881 (7) Å to 4.5284 (7) Å] and Cs—NH₃ [3.276 (7)–3.636 (7) Å] contacts.

CCDC reference: 1004528

Related literature

For the co-crystallization of Zintl anions and oxide or hydroxide ions see, for example: Boss et al. (2005 ), Röhr (1995 ) For the diagonal ratio value of the Sn₉⁴⁻ anion, see: Fässler & Hoffmann (1999 ).

Experimental

Crystal data

Cs₅Sn₉(OH)·4NH₃
M_r = 1817.90
Orthorhombic, P 2₁ 2₁ 2₁
a = 10.0935 (1) Å
b = 14.8256 (2) Å
c = 20.0419 (3) Å
V = 2999.11 (7) Å³
Z = 4
Mo Kα radiation
μ = 13.34 mm⁻¹
T = 123 K
0.32 × 0.15 × 0.06 mm

Data collection

Agilent SuperNova (single source at offset, Eos) diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012 ) T_min = 0.263, T_max = 1.000
34752 measured reflections
5910 independent reflections
5754 reflections with I > 2σ(I)
R_int = 0.045

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.037
S = 1.05
5910 reflections
191 parameters
H-atom parameters constrained
Δρ_max = 0.69 e Å⁻³
Δρ_min = −0.61 e Å⁻³
Absolute structure: Flack x determined using 2458 quotients [(I⁺)−(I⁻)]/[(I⁺)+(I⁻)] (Parsons & Flack, 2004 )
Absolute structure parameter: 0.037 (17)

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: OLEX2.SOLVE (Bourhis et al., 2014 ); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008 ); molecular graphics: DIAMOND (Brandenburg & Putz, 2011 ); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC reference: 1004528

Crystal structure: contains datablock I. DOI: 10.1107/S1600536814011817/ru2058sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814011817/ru2058Isup2.hkl

checkCIF report

Comment top

The crystal structure of Cs₅Sn₉(OH) × 4 NH₃ was determined in the course of solvation experiments on ternary alkali metal–Sn–Bi-phases.

The Sn₉^4- anion has a diagonal ratio value (Fässler et al., 1999) which is very close to 1, consequently it can be described as a monocapped quadratic antiprism (Fig. 1). Sn—Sn bond lengths range from 2.9310 (8) Å to 3.2457 (8) Å. The nonastannid cluster is surrounded by 15 caesium cations with distances ranging from 3.8881 (7) Å to 4.5284 (7) Å. The chemical origin of the hydroxide anion could not be determined, but it is likely that water was introduced to the system, which was deprotonated by the ammonia solvent. The caesium cations form a distorted quadratic pyramide around the hydroxide ion (Fig. 1). The distances d_Cs—O have values between 2.818 (5) Å and 3.080 (6) Å. Angles between neighbouring equatorial cations Cs_eq–O(1)–Cs_eq range from 86.43 (13)° to 95.28 (17)°, angles between the axial and the equatorial Cs cations Cs_ax–O(1)–Cs_eq have values between 85.15 (15)° and 101.89 (16)°. The ammonia molecules coordinate with distances from 3.276 (7) Å to 3.636 (7) Å to the caesium cations, forming a three dimensional network (Fig. 2).

Related literature top

For the co-crystallization of Zintl anions and oxide or hydroxide ions see, for example: Boss et al. (2005), Röhr (1995) For the diagonal ratio value of the Sn₉^4- anion, see: Fässler & Hoffmann (1999).

Experimental top

The educt material CsSnBi was synthesized in glas ampoules at 723 K from stochiometric amounts of the corresponding elements. 0.35 g (0.38 mmol) CsSnBi were weighed in a baked out reaction vessel, afterwards 10 ml of ammonia were condensed, leading to a brownish red solution. The solution was stored for four months at 236 K. The title compound formed as red plate-shaped crystals.

Computing details top

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO (Agilent, 2012); data reduction: CrysAlis PRO (Agilent, 2012); program(s) used to solve structure: OLEX2.SOLVE (Bourhis et al., 2014); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2011); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Figures top

	Fig. 1. : Asymmetric unit of the title compound; displacement ellipsoids drawn at the 50% probability level.
	Fig. 2. : Projection of the unit cell along the crystallographic a-axis; displacement ellipsoids drawn at the 50% probability level.

Pentacaesium nonastannide hydroxide tetraammonia top

Crystal data top

Cs₅Sn₉(OH)·4NH₃	D_x = 4.026 Mg m⁻³
M_r = 1817.90	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P2₁2₁2₁	Cell parameters from 21366 reflections
a = 10.0935 (1) Å	θ = 2.9–28.8°
b = 14.8256 (2) Å	µ = 13.34 mm⁻¹
c = 20.0419 (3) Å	T = 123 K
V = 2999.11 (7) Å³	Plate, red
Z = 4	0.32 × 0.15 × 0.06 mm
F(000) = 3096

Data collection top

Agilent SuperNova (single source at offset, Eos) diffractometer	5910 independent reflections
Radiation source: SuperNova (Mo) X-ray Source	5754 reflections with I > 2σ(I)
Detector resolution: 7.9851 pixels mm^-1	R_int = 0.045
ω scans	θ_max = 26.0°, θ_min = 2.9°
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	h = −12→12
T_min = 0.263, T_max = 1.000	k = −18→18
34752 measured reflections	l = −24→24

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.020	w = 1/[σ²(F_o²) + (0.0119P)² + 0.8162P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.037	(Δ/σ)_max = 0.002
S = 1.05	Δρ_max = 0.69 e Å⁻³
5910 reflections	Δρ_min = −0.61 e Å⁻³
191 parameters	Absolute structure: Flack x determined using 2458 quotients [(I⁺)-(I^-)]/[(I⁺)+(I^-)] (Parsons & Flack, 2004)
0 restraints	Absolute structure parameter: 0.037 (17)

Crystal data top

Cs₅Sn₉(OH)·4NH₃	V = 2999.11 (7) Å³
M_r = 1817.90	Z = 4
Orthorhombic, P2₁2₁2₁	Mo Kα radiation
a = 10.0935 (1) Å	µ = 13.34 mm⁻¹
b = 14.8256 (2) Å	T = 123 K
c = 20.0419 (3) Å	0.32 × 0.15 × 0.06 mm

Data collection top

Agilent SuperNova (single source at offset, Eos) diffractometer	5910 independent reflections
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	5754 reflections with I > 2σ(I)
T_min = 0.263, T_max = 1.000	R_int = 0.045
34752 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	H-atom parameters constrained
wR(F²) = 0.037	Δρ_max = 0.69 e Å⁻³
S = 1.05	Δρ_min = −0.61 e Å⁻³
5910 reflections	Absolute structure: Flack x determined using 2458 quotients [(I⁺)-(I^-)]/[(I⁺)+(I^-)] (Parsons & Flack, 2004)
191 parameters	Absolute structure parameter: 0.037 (17)
0 restraints

Special details top

Experimental. crystal mounting in perfluorether

Absorption correction: CrysAlisPro (Agilent Technologies, 2012), Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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

	x	y	z	U_iso*/U_eq
Cs1	0.69651 (4)	0.62993 (3)	0.52616 (3)	0.01745 (12)
Cs5	0.96022 (5)	0.55715 (3)	0.36506 (3)	0.01733 (12)
Cs2	0.77685 (5)	0.33699 (3)	0.47723 (3)	0.01964 (13)
Cs3	0.53343 (5)	0.64420 (3)	0.32331 (3)	0.01897 (12)
Cs4	0.70495 (5)	0.39111 (4)	0.27494 (3)	0.02169 (13)
Sn8	0.32179 (5)	0.57700 (4)	0.48243 (3)	0.01753 (13)
Sn9	0.33484 (5)	0.68860 (4)	0.60507 (3)	0.01726 (14)
Sn6	0.44704 (5)	0.53549 (4)	0.67889 (3)	0.01920 (14)
Sn4	0.15595 (5)	0.42149 (4)	0.51683 (3)	0.01634 (13)
Sn5	0.24692 (5)	0.38957 (4)	0.66732 (3)	0.01944 (14)
Sn3	0.07763 (5)	0.62769 (4)	0.55430 (3)	0.01715 (14)
Sn2	0.17196 (6)	0.59083 (4)	0.70575 (3)	0.02052 (14)
Sn7	0.43672 (5)	0.42314 (4)	0.55797 (3)	0.01669 (13)
Sn1	−0.00956 (5)	0.47064 (4)	0.63144 (3)	0.01970 (14)
O1	0.7008 (5)	0.5080 (3)	0.4020 (3)	0.0160 (13)
H1	0.6133	0.4914	0.4145	0.019*
N4	0.8001 (7)	0.6444 (5)	0.2302 (4)	0.0272 (19)
H4A	0.8659	0.6084	0.2143	0.041*
H4B	0.8275	0.7029	0.2296	0.041*
H4C	0.7269	0.6384	0.2041	0.041*
N3	0.9939 (7)	0.3306 (4)	0.3478 (4)	0.0249 (19)
H3A	1.0352	0.3496	0.3100	0.037*
H3B	0.9629	0.2735	0.3416	0.037*
H3C	1.0524	0.3310	0.3823	0.037*
N2	0.7994 (6)	0.2374 (4)	0.1655 (4)	0.0237 (18)
H2A	0.7623	0.2044	0.1321	0.036*
H2B	0.7658	0.2189	0.2054	0.036*
H2C	0.8888	0.2293	0.1653	0.036*
N1	0.4815 (7)	0.3126 (5)	0.3796 (4)	0.031 (2)
H1A	0.4909	0.2518	0.3834	0.046*
H1B	0.3990	0.3256	0.3640	0.046*
H1C	0.4929	0.3388	0.4202	0.046*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cs1	0.0134 (2)	0.0200 (3)	0.0189 (3)	−0.0008 (2)	0.0009 (2)	−0.0020 (2)
Cs5	0.0155 (2)	0.0163 (3)	0.0202 (3)	−0.0019 (2)	−0.0001 (2)	−0.0021 (2)
Cs2	0.0186 (3)	0.0152 (2)	0.0251 (4)	0.0012 (2)	0.0014 (2)	0.0016 (2)
Cs3	0.0175 (2)	0.0210 (3)	0.0185 (3)	0.0007 (2)	−0.0004 (2)	0.0003 (2)
Cs4	0.0192 (3)	0.0264 (3)	0.0194 (3)	0.0021 (2)	−0.0026 (2)	−0.0053 (2)
Sn8	0.0175 (3)	0.0204 (3)	0.0146 (4)	−0.0020 (2)	0.0026 (3)	0.0044 (3)
Sn9	0.0146 (3)	0.0119 (3)	0.0253 (4)	−0.0024 (2)	−0.0030 (3)	−0.0010 (3)
Sn6	0.0169 (3)	0.0215 (3)	0.0192 (4)	0.0014 (2)	−0.0077 (3)	−0.0012 (3)
Sn4	0.0154 (3)	0.0157 (3)	0.0179 (4)	−0.0031 (2)	−0.0020 (3)	−0.0035 (3)
Sn5	0.0221 (3)	0.0161 (3)	0.0201 (4)	0.0003 (2)	0.0027 (3)	0.0078 (3)
Sn3	0.0114 (3)	0.0154 (3)	0.0247 (4)	0.0013 (2)	−0.0036 (3)	0.0026 (3)
Sn2	0.0195 (3)	0.0238 (3)	0.0183 (4)	−0.0012 (2)	0.0058 (3)	−0.0072 (3)
Sn7	0.0129 (3)	0.0178 (3)	0.0194 (4)	0.0031 (2)	0.0017 (2)	−0.0013 (3)
Sn1	0.0141 (3)	0.0207 (3)	0.0243 (4)	−0.0038 (2)	0.0054 (3)	0.0000 (3)
O1	0.015 (3)	0.014 (3)	0.019 (4)	−0.004 (2)	0.001 (2)	0.000 (3)
N4	0.023 (4)	0.033 (4)	0.026 (5)	0.000 (3)	0.006 (4)	−0.004 (4)
N3	0.026 (4)	0.021 (4)	0.027 (5)	−0.001 (3)	0.000 (4)	0.001 (4)
N2	0.020 (4)	0.026 (4)	0.025 (5)	0.002 (3)	0.000 (3)	0.001 (4)
N1	0.029 (4)	0.030 (4)	0.034 (6)	−0.007 (4)	−0.007 (4)	0.001 (4)

Geometric parameters (Å, º) top

Cs1—N2ⁱ	3.417 (8)	Sn9—Sn6	2.9367 (8)
Cs1—Sn3ⁱⁱ	3.8881 (7)	Sn9—Sn2	2.9793 (9)
Cs1—Sn8	3.9609 (7)	Sn9—Cs1^xii	4.0131 (8)
Cs1—Sn9ⁱⁱⁱ	4.0132 (8)	Sn9—Cs5^xii	4.0210 (7)
Cs1—Sn9	4.0723 (7)	Sn9—Cs3^xii	4.1787 (8)
Cs1—Sn7	4.0843 (8)	Sn6—Sn7	2.9425 (9)
Cs1—Sn3ⁱⁱⁱ	4.1175 (8)	Sn6—Sn2	2.9449 (8)
Cs1—Sn6	4.2037 (9)	Sn6—Sn5	2.9688 (8)
Cs1—Cs5	4.3213 (8)	Sn6—Cs5ⁱ	4.0847 (9)
Cs1—Sn1ⁱⁱ	4.3395 (8)	Sn6—Cs4ⁱ	4.1507 (8)
Cs5—O1	2.817 (5)	Sn4—Sn1	2.9323 (9)
Cs5—N2^iv	3.661 (6)	Sn4—Sn7	2.9516 (7)
Cs5—Cs4	3.9951 (7)	Sn4—Sn5	3.1880 (9)
Cs5—Sn9ⁱⁱⁱ	4.0210 (7)	Sn4—Sn3	3.2457 (8)
Cs5—Sn6^v	4.0847 (9)	Sn4—Cs2^vii	4.0234 (7)
Cs5—Sn3ⁱⁱ	4.1089 (9)	Sn4—Cs2^xi	4.1038 (7)
Cs5—Sn4ⁱⁱ	4.1474 (8)	Sn4—Cs5^xi	4.1473 (8)
Cs5—Sn8ⁱⁱ	4.3519 (8)	Sn5—Sn1	2.9434 (8)
Cs5—Cs2	4.3741 (7)	Sn5—Sn7	2.9530 (9)
Cs2—Sn7	4.0045 (7)	Sn5—Sn2	3.1732 (8)
Cs2—Sn4^vi	4.0235 (7)	Sn5—Cs3^xiii	4.2463 (8)
Cs2—Sn4ⁱⁱ	4.1038 (7)	Sn5—Cs4^vii	4.3400 (8)
Cs2—Cs4	4.1961 (9)	Sn5—Cs2^vii	4.4459 (8)
Cs2—Sn7^vi	4.2398 (7)	Sn3—Sn1	2.9301 (8)
Cs2—Sn1ⁱⁱ	4.2575 (9)	Sn3—Sn2	3.2277 (9)
Cs2—Sn5^vi	4.4460 (8)	Sn3—Cs1^xi	3.8882 (7)
Cs2—Cs2^vii	5.7408 (5)	Sn3—Cs5^xi	4.1088 (9)
Cs2—Cs2^vi	5.7408 (5)	Sn3—Cs1^xii	4.1174 (8)
Cs3—N2^viii	3.639 (7)	Sn3—Cs3^xii	4.2017 (8)
Cs3—Sn8	3.9656 (8)	Sn2—Sn1	2.9581 (9)
Cs3—Sn9ⁱⁱⁱ	4.1786 (8)	Sn2—Cs4^xiii	4.0580 (8)
Cs3—Sn3ⁱⁱⁱ	4.2016 (8)	Sn2—Cs3^xii	4.2103 (7)
Cs3—Sn2ⁱⁱⁱ	4.2102 (7)	Sn7—Cs2^vii	4.2398 (7)
Cs3—Sn1^ix	4.2123 (9)	Sn1—Cs4^xiii	4.0449 (9)
Cs3—Cs4	4.2445 (7)	Sn1—Cs3^xiii	4.2122 (9)
Cs3—Sn5^ix	4.2463 (8)	Sn1—Cs2^xi	4.2576 (9)
Cs3—Cs4^viii	4.8028 (7)	Sn1—Cs1^xi	4.3396 (8)
Cs4—N1	3.292 (8)	O1—H1	0.9500
Cs4—Sn1^ix	4.0449 (9)	N4—H4A	0.9100
Cs4—Sn2^ix	4.0579 (8)	N4—H4B	0.9100
Cs4—Sn6^v	4.1507 (8)	N4—H4C	0.9100
Cs4—Sn5^vi	4.3399 (8)	N3—H3A	0.9100
Cs4—Cs3^x	4.8027 (7)	N3—H3B	0.9100
Sn8—Sn4	2.9314 (8)	N3—H3C	0.9100
Sn8—Sn3	2.9518 (8)	N2—H2A	0.9100
Sn8—Sn9	2.9658 (9)	N2—H2B	0.9100
Sn8—Sn7	2.9735 (8)	N2—H2C	0.9100
Sn8—Cs5^xi	4.3518 (8)	N1—H1A	0.9100
Sn8—Cs1^xii	4.5284 (7)	N1—H1B	0.9100
Sn9—Sn3	2.9310 (8)	N1—H1C	0.9100

N2ⁱ—Cs1—Sn3ⁱⁱ	82.78 (11)	Sn4—Sn8—Cs3	133.97 (2)
N2ⁱ—Cs1—Sn8	107.85 (11)	Sn3—Sn8—Cs3	141.10 (2)
Sn3ⁱⁱ—Cs1—Sn8	167.198 (19)	Sn9—Sn8—Cs3	120.16 (2)
N2ⁱ—Cs1—Sn9ⁱⁱⁱ	98.37 (12)	Sn7—Sn8—Cs3	113.08 (2)
Sn3ⁱⁱ—Cs1—Sn9ⁱⁱⁱ	75.913 (15)	Cs1—Sn8—Cs3	67.283 (14)
Sn8—Cs1—Sn9ⁱⁱⁱ	108.664 (18)	Sn4—Sn8—Cs5^xi	66.113 (17)
N2ⁱ—Cs1—Sn9	64.56 (11)	Sn3—Sn8—Cs5^xi	65.218 (18)
Sn3ⁱⁱ—Cs1—Sn9	146.35 (2)	Sn9—Sn8—Cs5^xi	121.53 (2)
Sn8—Cs1—Sn9	43.304 (13)	Sn7—Sn8—Cs5^xi	123.40 (2)
Sn9ⁱⁱⁱ—Cs1—Sn9	115.038 (15)	Cs1—Sn8—Cs5^xi	159.03 (2)
N2ⁱ—Cs1—Sn7	108.20 (12)	Cs3—Sn8—Cs5^xi	91.952 (17)
Sn3ⁱⁱ—Cs1—Sn7	127.309 (17)	Sn4—Sn8—Cs1^xii	127.17 (2)
Sn8—Cs1—Sn7	43.347 (12)	Sn3—Sn8—Cs1^xii	62.688 (16)
Sn9ⁱⁱⁱ—Cs1—Sn7	145.99 (2)	Sn9—Sn8—Cs1^xii	60.572 (16)
Sn9—Cs1—Sn7	61.588 (12)	Sn7—Sn8—Cs1^xii	149.81 (2)
N2ⁱ—Cs1—Sn3ⁱⁱⁱ	79.70 (12)	Cs1—Sn8—Cs1^xii	94.875 (13)
Sn3ⁱⁱ—Cs1—Sn3ⁱⁱⁱ	110.648 (15)	Cs3—Sn8—Cs1^xii	83.040 (14)
Sn8—Cs1—Sn3ⁱⁱⁱ	78.928 (14)	Cs5^xi—Sn8—Cs1^xii	79.056 (13)
Sn9ⁱⁱⁱ—Cs1—Sn3ⁱⁱⁱ	42.236 (12)	Sn3—Sn9—Sn6	106.16 (2)
Sn9—Cs1—Sn3ⁱⁱⁱ	72.811 (14)	Sn3—Sn9—Sn8	60.07 (2)
Sn7—Cs1—Sn3ⁱⁱⁱ	121.949 (15)	Sn6—Sn9—Sn8	90.20 (2)
N2ⁱ—Cs1—Sn6	66.66 (12)	Sn3—Sn9—Sn2	66.20 (2)
Sn3ⁱⁱ—Cs1—Sn6	118.956 (19)	Sn6—Sn9—Sn2	59.70 (2)
Sn8—Cs1—Sn6	61.522 (14)	Sn8—Sn9—Sn2	105.39 (2)
Sn9ⁱⁱⁱ—Cs1—Sn6	155.360 (17)	Sn3—Sn9—Cs1^xii	70.784 (18)
Sn9—Cs1—Sn6	41.531 (12)	Sn6—Sn9—Cs1^xii	169.28 (3)
Sn7—Cs1—Sn6	41.560 (13)	Sn8—Sn9—Cs1^xii	79.36 (2)
Sn3ⁱⁱⁱ—Cs1—Sn6	113.663 (16)	Sn2—Sn9—Cs1^xii	125.31 (2)
N2ⁱ—Cs1—Cs5	138.34 (11)	Sn3—Sn9—Cs5^xii	128.26 (2)
Sn3ⁱⁱ—Cs1—Cs5	59.790 (14)	Sn6—Sn9—Cs5^xii	121.89 (2)
Sn8—Cs1—Cs5	111.923 (17)	Sn8—Sn9—Cs5^xii	131.32 (2)
Sn9ⁱⁱⁱ—Cs1—Cs5	57.548 (12)	Sn2—Sn9—Cs5^xii	121.93 (2)
Sn9—Cs1—Cs5	153.592 (18)	Cs1^xii—Sn9—Cs5^xii	65.078 (14)
Sn7—Cs1—Cs5	108.945 (16)	Sn3—Sn9—Cs1	126.40 (2)
Sn3ⁱⁱⁱ—Cs1—Cs5	96.014 (16)	Sn6—Sn9—Cs1	71.633 (18)
Sn6—Cs1—Cs5	146.084 (16)	Sn8—Sn9—Cs1	66.348 (17)
N2ⁱ—Cs1—Sn1ⁱⁱ	84.70 (11)	Sn2—Sn9—Cs1	130.83 (2)
Sn3ⁱⁱ—Cs1—Sn1ⁱⁱ	41.268 (12)	Cs1^xii—Sn9—Cs1	101.571 (16)
Sn8—Cs1—Sn1ⁱⁱ	130.739 (17)	Cs5^xii—Sn9—Cs1	88.619 (15)
Sn9ⁱⁱⁱ—Cs1—Sn1ⁱⁱ	116.464 (15)	Sn3—Sn9—Cs3^xii	69.949 (18)
Sn9—Cs1—Sn1ⁱⁱ	122.702 (19)	Sn6—Sn9—Cs3^xii	124.49 (3)
Sn7—Cs1—Sn1ⁱⁱ	87.394 (15)	Sn8—Sn9—Cs3^xii	125.68 (2)
Sn3ⁱⁱⁱ—Cs1—Sn1ⁱⁱ	149.840 (16)	Sn2—Sn9—Cs3^xii	69.766 (18)
Sn6—Cs1—Sn1ⁱⁱ	82.772 (15)	Cs1^xii—Sn9—Cs3^xii	64.795 (14)
Cs5—Cs1—Sn1ⁱⁱ	78.830 (14)	Cs5^xii—Sn9—Cs3^xii	67.783 (13)
O1—Cs5—N2^iv	148.09 (15)	Cs1—Sn9—Cs3^xii	155.890 (17)
O1—Cs5—Cs4	50.21 (11)	Sn9—Sn6—Sn7	90.51 (2)
N2^iv—Cs5—Cs4	143.27 (13)	Sn9—Sn6—Sn2	60.87 (2)
O1—Cs5—Sn9ⁱⁱⁱ	84.88 (10)	Sn7—Sn6—Sn2	105.96 (2)
N2^iv—Cs5—Sn9ⁱⁱⁱ	63.22 (10)	Sn9—Sn6—Sn5	105.16 (2)
Cs4—Cs5—Sn9ⁱⁱⁱ	116.228 (16)	Sn7—Sn6—Sn5	59.94 (2)
O1—Cs5—Sn6^v	111.48 (12)	Sn2—Sn6—Sn5	64.902 (19)
N2^iv—Cs5—Sn6^v	86.59 (13)	Sn9—Sn6—Cs5ⁱ	143.95 (3)
Cs4—Cs5—Sn6^v	61.811 (14)	Sn7—Sn6—Cs5ⁱ	124.76 (2)
Sn9ⁱⁱⁱ—Cs5—Sn6^v	121.556 (19)	Sn2—Sn6—Cs5ⁱ	98.21 (2)
O1—Cs5—Sn3ⁱⁱ	95.23 (12)	Sn5—Sn6—Cs5ⁱ	88.99 (2)
N2^iv—Cs5—Sn3ⁱⁱ	77.16 (13)	Sn9—Sn6—Cs4ⁱ	110.94 (2)
Cs4—Cs5—Sn3ⁱⁱ	139.478 (18)	Sn7—Sn6—Cs4ⁱ	124.08 (2)
Sn9ⁱⁱⁱ—Cs5—Sn3ⁱⁱ	73.429 (15)	Sn2—Sn6—Cs4ⁱ	129.80 (2)
Sn6^v—Cs5—Sn3ⁱⁱ	149.616 (17)	Sn5—Sn6—Cs4ⁱ	143.42 (2)
O1—Cs5—Sn4ⁱⁱ	97.15 (11)	Cs5ⁱ—Sn6—Cs4ⁱ	58.034 (13)
N2^iv—Cs5—Sn4ⁱⁱ	99.27 (12)	Sn9—Sn6—Cs1	66.836 (19)
Cs4—Cs5—Sn4ⁱⁱ	109.876 (16)	Sn7—Sn6—Cs1	67.046 (18)
Sn9ⁱⁱⁱ—Cs5—Sn4ⁱⁱ	119.695 (19)	Sn2—Sn6—Cs1	127.23 (2)
Sn6^v—Cs5—Sn4ⁱⁱ	113.434 (16)	Sn5—Sn6—Cs1	126.39 (2)
Sn3ⁱⁱ—Cs5—Sn4ⁱⁱ	46.295 (12)	Cs5ⁱ—Sn6—Cs1	129.785 (16)
O1—Cs5—Cs1	45.22 (11)	Cs4ⁱ—Sn6—Cs1	75.135 (14)
N2^iv—Cs5—Cs1	110.56 (12)	Sn8—Sn4—Sn1	108.31 (2)
Cs4—Cs5—Cs1	95.417 (14)	Sn8—Sn4—Sn7	60.719 (19)
Sn9ⁱⁱⁱ—Cs5—Cs1	57.374 (13)	Sn1—Sn4—Sn7	109.03 (3)
Sn6^v—Cs5—Cs1	155.179 (17)	Sn8—Sn4—Sn5	100.07 (2)
Sn3ⁱⁱ—Cs5—Cs1	54.861 (13)	Sn1—Sn4—Sn5	57.31 (2)
Sn4ⁱⁱ—Cs5—Cs1	82.331 (15)	Sn7—Sn4—Sn5	57.344 (19)
O1—Cs5—Sn8ⁱⁱ	130.91 (12)	Sn8—Sn4—Sn3	56.818 (17)
N2^iv—Cs5—Sn8ⁱⁱ	59.02 (12)	Sn1—Sn4—Sn3	56.350 (19)
Cs4—Cs5—Sn8ⁱⁱ	145.780 (16)	Sn7—Sn4—Sn3	99.29 (2)
Sn9ⁱⁱⁱ—Cs5—Sn8ⁱⁱ	96.897 (15)	Sn5—Sn4—Sn3	89.49 (2)
Sn6^v—Cs5—Sn8ⁱⁱ	108.922 (16)	Sn8—Sn4—Cs2^vii	125.66 (2)
Sn3ⁱⁱ—Cs5—Sn8ⁱⁱ	40.711 (12)	Sn1—Sn4—Cs2^vii	112.72 (2)
Sn4ⁱⁱ—Cs5—Sn8ⁱⁱ	40.262 (11)	Sn7—Sn4—Cs2^vii	73.050 (17)
Cs1—Cs5—Sn8ⁱⁱ	95.499 (16)	Sn5—Sn4—Cs2^vii	75.125 (17)
O1—Cs5—Cs2	43.82 (10)	Sn3—Sn4—Cs2^vii	164.60 (3)
N2^iv—Cs5—Cs2	155.66 (13)	Sn8—Sn4—Cs2^xi	136.64 (2)
Cs4—Cs5—Cs2	59.978 (14)	Sn1—Sn4—Cs2^xi	72.311 (18)
Sn9ⁱⁱⁱ—Cs5—Cs2	119.331 (17)	Sn7—Sn4—Cs2^xi	162.15 (2)
Sn6^v—Cs5—Cs2	108.391 (15)	Sn5—Sn4—Cs2^xi	113.97 (2)
Sn3ⁱⁱ—Cs5—Cs2	80.651 (15)	Sn3—Sn4—Cs2^xi	96.036 (17)
Sn4ⁱⁱ—Cs5—Cs2	57.504 (12)	Cs2^vii—Sn4—Cs2^xi	89.873 (12)
Cs1—Cs5—Cs2	62.723 (12)	Sn8—Sn4—Cs5^xi	73.625 (18)
Sn8ⁱⁱ—Cs5—Cs2	97.327 (15)	Sn1—Sn4—Cs5^xi	100.52 (2)
Sn7—Cs2—Sn4^vi	91.823 (15)	Sn7—Sn4—Cs5^xi	131.17 (2)
Sn7—Cs2—Sn4ⁱⁱ	128.598 (19)	Sn5—Sn4—Cs5^xi	154.56 (2)
Sn4^vi—Cs2—Sn4ⁱⁱ	124.596 (16)	Sn3—Sn4—Cs5^xi	66.228 (17)
Sn7—Cs2—Cs4	100.440 (16)	Cs2^vii—Sn4—Cs5^xi	128.909 (19)
Sn4^vi—Cs2—Cs4	99.106 (17)	Cs2^xi—Sn4—Cs5^xi	64.025 (13)
Sn4ⁱⁱ—Cs2—Cs4	106.844 (17)	Sn1—Sn5—Sn7	108.69 (3)
Sn7—Cs2—Sn7^vi	133.131 (16)	Sn1—Sn5—Sn6	108.66 (2)
Sn4^vi—Cs2—Sn7^vi	41.753 (11)	Sn7—Sn5—Sn6	59.59 (2)
Sn4ⁱⁱ—Cs2—Sn7^vi	87.418 (14)	Sn1—Sn5—Sn2	57.697 (19)
Cs4—Cs2—Sn7^vi	94.530 (17)	Sn7—Sn5—Sn2	100.16 (2)
Sn7—Cs2—Sn1ⁱⁱ	89.560 (17)	Sn6—Sn5—Sn2	57.184 (18)
Sn4^vi—Cs2—Sn1ⁱⁱ	125.124 (19)	Sn1—Sn5—Sn4	56.97 (2)
Sn4ⁱⁱ—Cs2—Sn1ⁱⁱ	41.007 (13)	Sn7—Sn5—Sn4	57.300 (19)
Cs4—Cs2—Sn1ⁱⁱ	134.426 (17)	Sn6—Sn5—Sn4	99.31 (2)
Sn7^vi—Cs2—Sn1ⁱⁱ	110.573 (16)	Sn2—Sn5—Sn4	91.23 (2)
Sn7—Cs2—Cs5	109.417 (15)	Sn1—Sn5—Cs3^xiii	69.015 (19)
Sn4^vi—Cs2—Cs5	148.679 (19)	Sn7—Sn5—Cs3^xiii	176.91 (2)
Sn4ⁱⁱ—Cs2—Cs5	58.471 (13)	Sn6—Sn5—Cs3^xiii	118.80 (2)
Cs4—Cs2—Cs5	55.525 (13)	Sn2—Sn5—Cs3^xiii	76.893 (18)
Sn7^vi—Cs2—Cs5	115.608 (16)	Sn4—Sn5—Cs3^xiii	121.47 (2)
Sn1ⁱⁱ—Cs2—Cs5	79.136 (14)	Sn1—Sn5—Cs4^vii	111.766 (19)
Sn7—Cs2—Sn5^vi	116.490 (16)	Sn7—Sn5—Cs4^vii	115.01 (2)
Sn4^vi—Cs2—Sn5^vi	43.871 (13)	Sn6—Sn5—Cs4^vii	138.10 (2)
Sn4ⁱⁱ—Cs2—Sn5^vi	114.834 (16)	Sn2—Sn5—Cs4^vii	144.45 (2)
Cs4—Cs2—Sn5^vi	60.207 (13)	Sn4—Sn5—Cs4^vii	111.50 (2)
Sn7^vi—Cs2—Sn5^vi	39.663 (12)	Cs3^xiii—Sn5—Cs4^vii	68.012 (13)
Sn1ⁱⁱ—Cs2—Sn5^vi	149.209 (16)	Sn1—Sn5—Cs2^vii	102.07 (2)
Cs5—Cs2—Sn5^vi	104.930 (17)	Sn7—Sn5—Cs2^vii	66.404 (18)
Sn7—Cs2—Cs1	56.821 (12)	Sn6—Sn5—Cs2^vii	123.73 (2)
Sn4^vi—Cs2—Cs1	148.568 (16)	Sn2—Sn5—Cs2^vii	152.23 (2)
Sn4ⁱⁱ—Cs2—Cs1	80.342 (13)	Sn4—Sn5—Cs2^vii	61.004 (16)
Cs4—Cs2—Cs1	89.708 (14)	Cs3^xiii—Sn5—Cs2^vii	115.845 (16)
Sn7^vi—Cs2—Cs1	167.741 (16)	Cs4^vii—Sn5—Cs2^vii	57.042 (13)
Sn1ⁱⁱ—Cs2—Cs1	59.123 (12)	Sn1—Sn3—Sn9	109.13 (3)
Cs5—Cs2—Cs1	58.068 (11)	Sn1—Sn3—Sn8	107.82 (2)
Sn5^vi—Cs2—Cs1	148.656 (18)	Sn9—Sn3—Sn8	60.55 (2)
Sn7—Cs2—Cs2^vii	47.576 (10)	Sn1—Sn3—Sn2	57.17 (2)
Sn4^vi—Cs2—Cs2^vii	45.631 (12)	Sn9—Sn3—Sn2	57.62 (2)
Sn4ⁱⁱ—Cs2—Cs2^vii	157.83 (2)	Sn8—Sn3—Sn2	99.76 (2)
Cs4—Cs2—Cs2^vii	95.020 (15)	Sn1—Sn3—Sn4	56.415 (19)
Sn7^vi—Cs2—Cs2^vii	87.268 (15)	Sn9—Sn3—Sn4	98.90 (2)
Sn1ⁱⁱ—Cs2—Cs2^vii	122.60 (2)	Sn8—Sn3—Sn4	56.218 (17)
Cs5—Cs2—Cs2^vii	142.091 (16)	Sn2—Sn3—Sn4	89.22 (2)
Sn5^vi—Cs2—Cs2^vii	72.807 (14)	Sn1—Sn3—Cs1^xi	77.654 (18)
Cs1—Cs2—Cs2^vii	103.840 (12)	Sn9—Sn3—Cs1^xi	157.53 (2)
Sn7—Cs2—Cs2^vi	146.38 (2)	Sn8—Sn3—Cs1^xi	139.24 (3)
Sn4^vi—Cs2—Cs2^vi	80.443 (14)	Sn2—Sn3—Cs1^xi	115.45 (2)
Sn4ⁱⁱ—Cs2—Cs2^vi	44.495 (8)	Sn4—Sn3—Cs1^xi	102.444 (18)
Cs4—Cs2—Cs2^vi	113.053 (17)	Sn1—Sn3—Cs5^xi	101.43 (2)
Sn7^vi—Cs2—Cs2^vi	44.205 (11)	Sn9—Sn3—Cs5^xi	130.87 (2)
Sn1ⁱⁱ—Cs2—Cs2^vi	69.422 (13)	Sn8—Sn3—Cs5^xi	74.07 (2)
Cs5—Cs2—Cs2^vi	92.580 (11)	Sn2—Sn3—Cs5^xi	155.51 (2)
Sn5^vi—Cs2—Cs2^vi	79.856 (14)	Sn4—Sn3—Cs5^xi	67.477 (17)
Cs1—Cs2—Cs2^vi	123.659 (15)	Cs1^xi—Sn3—Cs5^xi	65.349 (14)
Cs2^vii—Cs2—Cs2^vi	123.070 (17)	Sn1—Sn3—Cs1^xii	170.99 (3)
N2^viii—Cs3—Sn8	63.17 (13)	Sn9—Sn3—Cs1^xii	66.980 (17)
N2^viii—Cs3—Sn9ⁱⁱⁱ	115.20 (10)	Sn8—Sn3—Cs1^xii	77.744 (18)
Sn8—Cs3—Sn9ⁱⁱⁱ	105.364 (18)	Sn2—Sn3—Cs1^xii	115.47 (2)
N2^viii—Cs3—Sn3ⁱⁱⁱ	75.92 (11)	Sn4—Sn3—Cs1^xii	131.33 (2)
Sn8—Cs3—Sn3ⁱⁱⁱ	77.873 (16)	Cs1^xi—Sn3—Cs1^xii	102.944 (15)
Sn9ⁱⁱⁱ—Cs3—Sn3ⁱⁱⁱ	40.943 (12)	Cs5^xi—Sn3—Cs1^xii	86.825 (17)
N2^viii—Cs3—Sn2ⁱⁱⁱ	87.77 (10)	Sn1—Sn3—Cs3^xii	107.44 (2)
Sn8—Cs3—Sn2ⁱⁱⁱ	121.638 (18)	Sn9—Sn3—Cs3^xii	69.109 (18)
Sn9ⁱⁱⁱ—Cs3—Sn2ⁱⁱⁱ	41.602 (12)	Sn8—Sn3—Cs3^xii	125.34 (2)
Sn3ⁱⁱⁱ—Cs3—Sn2ⁱⁱⁱ	45.128 (14)	Sn2—Sn3—Cs3^xii	67.578 (17)
N2^viii—Cs3—Sn1^ix	99.02 (13)	Sn4—Sn3—Cs3^xii	156.79 (2)
Sn8—Cs3—Sn1^ix	126.998 (17)	Cs1^xi—Sn3—Cs3^xii	88.437 (15)
Sn9ⁱⁱⁱ—Cs3—Sn1^ix	126.514 (18)	Cs5^xi—Sn3—Cs3^xii	135.489 (17)
Sn3ⁱⁱⁱ—Cs3—Sn1^ix	149.810 (19)	Cs1^xii—Sn3—Cs3^xii	63.713 (14)
Sn2ⁱⁱⁱ—Cs3—Sn1^ix	105.654 (18)	Sn6—Sn2—Sn1	108.91 (2)
N2^viii—Cs3—Cs4	136.56 (10)	Sn6—Sn2—Sn9	59.43 (2)
Sn8—Cs3—Cs4	100.445 (16)	Sn1—Sn2—Sn9	107.09 (3)
Sn9ⁱⁱⁱ—Cs3—Cs4	107.813 (15)	Sn6—Sn2—Sn5	57.914 (18)
Sn3ⁱⁱⁱ—Cs3—Cs4	143.281 (17)	Sn1—Sn2—Sn5	57.249 (18)
Sn2ⁱⁱⁱ—Cs3—Cs4	131.129 (17)	Sn9—Sn2—Sn5	99.29 (2)
Sn1^ix—Cs3—Cs4	57.148 (13)	Sn6—Sn2—Sn3	98.82 (2)
N2^viii—Cs3—Sn5^ix	58.32 (13)	Sn1—Sn2—Sn3	56.34 (2)
Sn8—Cs3—Sn5^ix	101.741 (16)	Sn9—Sn2—Sn3	56.183 (19)
Sn9ⁱⁱⁱ—Cs3—Sn5^ix	143.904 (18)	Sn5—Sn2—Sn3	90.07 (2)
Sn3ⁱⁱⁱ—Cs3—Sn5^ix	126.547 (16)	Sn6—Sn2—Cs4^xiii	164.74 (3)
Sn2ⁱⁱⁱ—Cs3—Sn5^ix	103.266 (17)	Sn1—Sn2—Cs4^xiii	68.353 (18)
Sn1^ix—Cs3—Sn5^ix	40.724 (12)	Sn9—Sn2—Cs4^xiii	135.78 (2)
Cs4—Cs3—Sn5^ix	89.967 (15)	Sn5—Sn2—Cs4^xiii	111.62 (2)
N2^viii—Cs3—Cs1	107.90 (13)	Sn3—Sn2—Cs4^xiii	91.928 (19)
Sn8—Cs3—Cs1	56.307 (13)	Sn6—Sn2—Cs3^xii	123.22 (2)
Sn9ⁱⁱⁱ—Cs3—Cs1	55.779 (13)	Sn1—Sn2—Cs3^xii	106.66 (2)
Sn3ⁱⁱⁱ—Cs3—Cs1	57.211 (13)	Sn9—Sn2—Cs3^xii	68.632 (17)
Sn2ⁱⁱⁱ—Cs3—Cs1	92.782 (15)	Sn5—Sn2—Cs3^xii	157.36 (3)
Sn1^ix—Cs3—Cs1	147.903 (16)	Sn3—Sn2—Cs3^xii	67.296 (17)
Cs4—Cs3—Cs1	90.915 (15)	Cs4^xiii—Sn2—Cs3^xii	70.996 (14)
Sn5^ix—Cs3—Cs1	157.780 (18)	Sn6—Sn7—Sn4	105.59 (2)
N2^viii—Cs3—Cs5	164.84 (13)	Sn6—Sn7—Sn5	60.47 (2)
Sn8—Cs3—Cs5	106.815 (17)	Sn4—Sn7—Sn5	65.36 (2)
Sn9ⁱⁱⁱ—Cs3—Cs5	54.469 (11)	Sn6—Sn7—Sn8	89.94 (2)
Sn3ⁱⁱⁱ—Cs3—Cs5	91.162 (14)	Sn4—Sn7—Sn8	59.306 (18)
Sn2ⁱⁱⁱ—Cs3—Cs5	88.612 (13)	Sn5—Sn7—Sn8	104.72 (2)
Sn1^ix—Cs3—Cs5	96.134 (15)	Sn6—Sn7—Cs2	118.88 (2)
Cs4—Cs3—Cs5	53.719 (11)	Sn4—Sn7—Cs2	135.04 (2)
Sn5^ix—Cs3—Cs5	136.804 (17)	Sn5—Sn7—Cs2	143.35 (2)
Cs1—Cs3—Cs5	57.588 (12)	Sn8—Sn7—Cs2	111.92 (2)
N2^viii—Cs3—Cs4^viii	43.41 (12)	Sn6—Sn7—Cs1	71.394 (18)
Sn8—Cs3—Cs4^viii	104.556 (15)	Sn4—Sn7—Cs1	125.38 (2)
Sn9ⁱⁱⁱ—Cs3—Cs4^viii	93.062 (13)	Sn5—Sn7—Cs1	131.21 (2)
Sn3ⁱⁱⁱ—Cs3—Cs4^viii	71.279 (13)	Sn8—Sn7—Cs1	66.117 (17)
Sn2ⁱⁱⁱ—Cs3—Cs4^viii	53.023 (12)	Cs2—Sn7—Cs1	68.033 (13)
Sn1^ix—Cs3—Cs4^viii	84.558 (15)	Sn6—Sn7—Cs2^vii	131.71 (2)
Cs4—Cs3—Cs4^viii	141.674 (15)	Sn4—Sn7—Cs2^vii	65.197 (16)
Sn5^ix—Cs3—Cs4^viii	56.920 (12)	Sn5—Sn7—Cs2^vii	73.933 (18)
Cs1—Cs3—Cs4^viii	127.162 (15)	Sn8—Sn7—Cs2^vii	117.69 (2)
Cs5—Cs3—Cs4^viii	139.627 (15)	Cs2—Sn7—Cs2^vii	88.220 (12)
N1—Cs4—Cs5	111.82 (14)	Cs1—Sn7—Cs2^vii	154.315 (19)
N1—Cs4—Sn1^ix	107.34 (13)	Sn3—Sn1—Sn4	67.23 (2)
Cs5—Cs4—Sn1^ix	108.886 (17)	Sn3—Sn1—Sn5	100.91 (2)
N1—Cs4—Sn2^ix	66.34 (14)	Sn4—Sn1—Sn5	65.72 (2)
Cs5—Cs4—Sn2^ix	135.927 (17)	Sn3—Sn1—Sn2	66.48 (2)
Sn1^ix—Cs4—Sn2^ix	42.824 (13)	Sn4—Sn1—Sn2	101.03 (2)
N1—Cs4—Sn6^v	165.43 (14)	Sn5—Sn1—Sn2	65.05 (2)
Cs5—Cs4—Sn6^v	60.155 (14)	Sn3—Sn1—Cs4^xiii	96.83 (2)
Sn1^ix—Cs4—Sn6^v	87.136 (17)	Sn4—Sn1—Cs4^xiii	163.88 (2)
Sn2^ix—Cs4—Sn6^v	128.14 (2)	Sn5—Sn1—Cs4^xiii	117.52 (3)
N1—Cs4—Cs2	55.63 (14)	Sn2—Sn1—Cs4^xiii	68.824 (19)
Cs5—Cs4—Cs2	64.497 (14)	Sn3—Sn1—Cs3^xiii	145.08 (2)
Sn1^ix—Cs4—Cs2	150.248 (18)	Sn4—Sn1—Cs3^xiii	130.33 (2)
Sn2^ix—Cs4—Cs2	120.324 (18)	Sn5—Sn1—Cs3^xiii	70.26 (2)
Sn6^v—Cs4—Cs2	110.600 (16)	Sn2—Sn1—Cs3^xiii	79.59 (2)
N1—Cs4—Cs3	83.55 (13)	Cs4^xiii—Sn1—Cs3^xiii	61.826 (14)
Cs5—Cs4—Cs3	67.362 (13)	Sn3—Sn1—Cs2^xi	97.98 (2)
Sn1^ix—Cs4—Cs3	61.026 (14)	Sn4—Sn1—Cs2^xi	66.681 (18)
Sn2^ix—Cs4—Cs3	68.737 (13)	Sn5—Sn1—Cs2^xi	115.64 (2)
Sn6^v—Cs4—Cs3	102.670 (15)	Sn2—Sn1—Cs2^xi	163.63 (3)
Cs2—Cs4—Cs3	91.084 (16)	Cs4^xiii—Sn1—Cs2^xi	120.338 (17)
N1—Cs4—Sn5^vi	63.77 (13)	Cs3^xiii—Sn1—Cs2^xi	116.465 (16)
Cs5—Cs4—Sn5^vi	114.035 (17)	Sn3—Sn1—Cs1^xi	61.077 (16)
Sn1^ix—Cs4—Sn5^vi	136.305 (18)	Sn4—Sn1—Cs1^xi	98.27 (2)
Sn2^ix—Cs4—Sn5^vi	104.233 (16)	Sn5—Sn1—Cs1^xi	160.44 (2)
Sn6^v—Cs4—Sn5^vi	107.003 (15)	Sn2—Sn1—Cs1^xi	109.90 (2)
Cs2—Cs4—Sn5^vi	62.751 (14)	Cs4^xiii—Sn1—Cs1^xi	74.730 (14)
Cs3—Cs4—Sn5^vi	145.75 (2)	Cs3^xiii—Sn1—Cs1^xi	128.664 (17)
N1—Cs4—Cs3^x	69.42 (14)	Cs2^xi—Sn1—Cs1^xi	63.520 (13)
Cs5—Cs4—Cs3^x	167.984 (17)	Cs5—O1—H1	180.0
Sn1^ix—Cs4—Cs3^x	81.400 (14)	H4A—N4—H4B	109.5
Sn2^ix—Cs4—Cs3^x	55.981 (12)	H4A—N4—H4C	109.5
Sn6^v—Cs4—Cs3^x	115.700 (17)	H4B—N4—H4C	109.5
Cs2—Cs4—Cs3^x	109.695 (15)	H3A—N3—H3B	109.5
Cs3—Cs4—Cs3^x	124.270 (12)	H3A—N3—H3C	109.5
Sn5^vi—Cs4—Cs3^x	55.068 (12)	H3B—N3—H3C	109.5
Sn4—Sn8—Sn3	66.964 (19)	H2A—N2—H2B	109.5
Sn4—Sn8—Sn9	105.62 (2)	H2A—N2—H2C	109.5
Sn3—Sn8—Sn9	59.38 (2)	H2B—N2—H2C	109.5
Sn4—Sn8—Sn7	59.975 (18)	Cs4—N1—H1A	109.5
Sn3—Sn8—Sn7	105.81 (2)	Cs4—N1—H1B	109.5
Sn9—Sn8—Sn7	89.35 (2)	H1A—N1—H1B	109.5
Sn4—Sn8—Cs1	130.47 (2)	Cs4—N1—H1C	109.5
Sn3—Sn8—Cs1	129.70 (2)	H1A—N1—H1C	109.5
Sn9—Sn8—Cs1	70.347 (17)	H1B—N1—H1C	109.5
Sn7—Sn8—Cs1	70.536 (17)

Symmetry codes: (i) −x+3/2, −y+1, z+1/2; (ii) x+1, y, z; (iii) x+1/2, −y+3/2, −z+1; (iv) −x+2, y+1/2, −z+1/2; (v) −x+3/2, −y+1, z−1/2; (vi) x+1/2, −y+1/2, −z+1; (vii) x−1/2, −y+1/2, −z+1; (viii) −x+1, y+1/2, −z+1/2; (ix) −x+1/2, −y+1, z−1/2; (x) −x+1, y−1/2, −z+1/2; (xi) x−1, y, z; (xii) x−1/2, −y+3/2, −z+1; (xiii) −x+1/2, −y+1, z+1/2.

Experimental details

Crystal data
Chemical formula	Cs₅Sn₉(OH)·4NH₃
M_r	1817.90
Crystal system, space group	Orthorhombic, P2₁2₁2₁
Temperature (K)	123
a, b, c (Å)	10.0935 (1), 14.8256 (2), 20.0419 (3)
V (Å³)	2999.11 (7)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	13.34
Crystal size (mm)	0.32 × 0.15 × 0.06

Data collection
Diffractometer	Agilent SuperNova (single source at offset, Eos) diffractometer
Absorption correction	Multi-scan (CrysAlis PRO; Agilent, 2012)
T_min, T_max	0.263, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	34752, 5910, 5754
R_int	0.045
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.037, 1.05
No. of reflections	5910
No. of parameters	191
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.69, −0.61
Absolute structure	Flack x determined using 2458 quotients [(I⁺)-(I^-)]/[(I⁺)+(I^-)] (Parsons & Flack, 2004)
Absolute structure parameter	0.037 (17)

Computer programs: CrysAlis PRO (Agilent, 2012), OLEX2.SOLVE (Bourhis et al., 2014), SHELXL2013 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2011), OLEX2 (Dolomanov et al., 2009).

Acknowledgements

UF thanks the Chemical Industry Fund for a scholarship.

References

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