μ-Hexa­thio­metadiphosphato-bis­[(1,4,7,10,13,16-hexa­oxa­cyclo­octa­decane-κ6O)rubidium] aceto­nitrile disolvate

Gjikaj, M.; Pook, N.-P.; Qarri, F.

doi:10.1107/S1600536813032121

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 69| Part 12| December 2013| Page m689

doi:10.1107/S1600536813032121

Open

access

μ-Hexathiometadiphosphato-bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ⁶O)rubidium] acetonitrile disolvate

Mimoza Gjikaj,^a ^* Niels-Patrick Pook ^a and Flora Qarri ^b

^aInstitute of Inorganic and Analytical Chemistry, Clausthal University of Technology, Paul-Ernst-Strasse 4, D-38678 Clausthal-Zellerfeld, Germany, and ^bChemistry Department, University of Vlora, Sheshi Pavaresia, 9401 Vlore, Albania
^*Correspondence e-mail: mimoza.gjikaj@tu-clausthal.de

(Received 20 November 2013; accepted 25 November 2013; online 30 November 2013)

The asymmetric unit of the title compound, [Rb₂(P₂S₆)(C₁₂H₂₄O₆)₂]·2CH₃CN, contains one half of an [Rb(18-crown-6)₂]₂[P₂S₆] unit and one acetonitrile solvent molecule. The [Rb(18-crown-6)]₂[P₂S₆] unit is completed by inversion symmetry. Its Rb⁺ ion is situated near the centre of the macrocyclic cavity, but is displaced by 0.8972 (1) Å from the O atoms of the crown in the direction of the [P₂S₆]²⁻ moiety. The overall coordination number of the cation is eight, defined by the six crown ether O atoms and by two terminal S atoms of the [P₂S₆]²⁻ anion. The hexathiometadiphosphate anion is built up from two tetrahedral PS₄ units joined together by a common edge. The crystal structure is characterized by alternating layers of [Rb(18-crown-6)]₂[P₂S₆] and acetonitrile solvent molecules stacked along [010].

CCDC reference: 973623

Related literature

For the synthesis of hexathiometadiphosphates, see: Thilo & Ladwig (1962 ). For the crystal structures of hexathiometadiphosphates, see: Toffoli et al. (1978 ); Brockner et al. (1985 ). For the crystal structures of alkali crown ether hexathiometadiphosphates, see: Gjikaj et al. (2005 , 2006 ).

Experimental

Crystal data

[Rb₂(P₂S₆)(C₁₂H₂₄O₆)₂]·2C₂H₃N
M_r = 1035.98
Monoclinic, P 2₁ /c
a = 8.2261 (9) Å
b = 17.1054 (15) Å
c = 16.5895 (18) Å
β = 95.520 (9)°
V = 2323.5 (4) Å³
Z = 2
Mo Kα radiation
μ = 2.50 mm⁻¹
T = 223 K
0.29 × 0.26 × 0.22 mm

Data collection

Stoe IPDSII diffractometer
Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 1999 , 2001 ) T_min = 0.490, T_max = 0.577
26056 measured reflections
4400 independent reflections
3450 reflections with I > 2σ(I)
R_int = 0.092

Refinement

R[F² > 2σ(F²)] = 0.047
wR(F²) = 0.074
S = 1.15
4400 reflections
343 parameters
All H-atom parameters refined
Δρ_max = 0.50 e Å⁻³
Δρ_min = −0.28 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2002 ); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ); software used to prepare material for publication: SHELXL97, PLATON (Spek, 2009 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 973623

Crystal structure: contains datablock I. DOI: 10.1107/S1600536813032121/wm2785sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813032121/wm2785Isup2.hkl

Supporting information file. DOI: 10.1107/S1600536813032121/wm2785Isup3.cdx

checkCIF report

Comment top

The first thiophosphates with empirical formula MPS₃ (M = Na, Ag and Tl), were described by Thilo & Ladwig (1962). However, the crystal structure determination of Ag₂P₂S₆ proved the presence of isolated P₂S₆^2- anions (Toffoli et al., 1978). The first alkali metal hexathiometadiphosphate structures, M₂P₂S₆ (M = K and Cs), were determined by Brockner et al. (1985). By using crown ether as complexing agent, alkali hexathiometadiphosphates, M₂P₂S₆ (M = Na and K), can be dissolved in CH₃CN. Such crown-ether-stabilized thiophosphates were obtained in crystalline form by Gjikaj et al. (2005, 2006).

The structure of the title compound, [Rb(18-crown-6)]₂[P₂S₆]^.2CH₃CN, is isotypic with [K(18-crown-6)]₂[P₂S₆]^.2CH₃CN (Gjikaj et al., 2005) and is characterized by alternating layers of [Rb(18-crown-6)]₂[P₂S₆] and acetonitrile molecules stacked along [010]. The asymmetric unit consists of one half of an [Rb(18-crown-6)]₂[P₂S₆] unit, which is located on a centre of inversion, and is completed by one acetonitrile molecule. The eightfold coordination environment of rubidium is defined by the six crown ether oxygen atoms and by two terminal sulfur atoms of the hexathiometadiphosphate anion (Fig. 2). The hexathiometadiphosphate anion is built up by two edge-sharing PS₄ units, each with a tetrahedral arrangement. The P–S bond lengths are ranging from 1.9630 (13) to 2.1419 (13) Å. All bond lengths and angles are comparable to those found for [K(18-crown-6)]₂[P₂S₆]^.2CH₃CN (Gjikaj et al., 2005).

Experimental top

Rubidium hexathiometadiphosphate was prepared by high-temperature element synthesis using the procedure reported by Brockner et al. (1985). A solution of bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ⁶O)rubidium] hexathiometadiphosphate was obtained by adding rubidium hexathiometadiphosphate to a solution of 18-crown-6 in dry acetonitrile.

Refinement top

All hydrogen atoms were located in a difference Fourier map and were refined isotropically with no restraints.

Related literature top

For the synthesis of hexathiometadiphosphates, see: Thilo & Ladwig (1962). For the crystal structures of hexathiometadiphosphates, see: Toffoli et al. (1978); Brockner et al. (1985). For the crystal structures of alkali crown ether hexathiometadiphosphates, see: Gjikaj et al. (2005, 2006).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA (Stoe & Cie, 2002); data reduction: X-AREA (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

Figures top

	Fig. 1. The crystal structure of the title compound. Displacement ellipsoids at the 50% probability level. The Rb—O and Rb—S bonds are shown as dashed lines.
	Fig. 2. The molecular structure of the title compound with atom labels and 50% probability displacement ellipsoids. The Rb—O and Rb—S bonds are shown as dashed lines. [Symmetry codes: (i) -x, -y + 1, -z - 1.]

µ-Hexathiometadiphosphato-bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ⁶O)rubidium] acetonitrile disolvate top

Crystal data top

[Rb₂(P₂S₆)(C₁₂H₂₄O₆)₂]·2C₂H₃N	F(000) = 1064
M_r = 1035.98	block, yellow
Monoclinic, P2₁/c	D_x = 1.481 Mg m⁻³
Hall symbol: -P 2yn	Mo Kα radiation, λ = 0.71073 Å
a = 8.2261 (9) Å	Cell parameters from 41621 reflections
b = 17.1054 (15) Å	θ = 2.4–25.7°
c = 16.5895 (18) Å	µ = 2.50 mm⁻¹
β = 95.520 (9)°	T = 223 K
V = 2323.5 (4) Å³	Block, yellow
Z = 2	0.29 × 0.26 × 0.22 mm

Data collection top

Stoe IPDSII diffractometer	4400 independent reflections
Radiation source: fine-focus sealed tube	3450 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.092
ω–scans	θ_max = 25.7°, θ_min = 2.4°
Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 1999, 2001)	h = −10→9
T_min = 0.490, T_max = 0.577	k = −20→20
26056 measured reflections	l = −20→20

Refinement top

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.074	All H-atom parameters refined
S = 1.15	w = 1/[σ²(F_o²) + (0.0188P)² + 1.1961P] where P = (F_o² + 2F_c²)/3
4400 reflections	(Δ/σ)_max < 0.001
343 parameters	Δρ_max = 0.50 e Å⁻³
0 restraints	Δρ_min = −0.28 e Å⁻³

Crystal data top

[Rb₂(P₂S₆)(C₁₂H₂₄O₆)₂]·2C₂H₃N	V = 2323.5 (4) Å³
M_r = 1035.98	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 8.2261 (9) Å	µ = 2.50 mm⁻¹
b = 17.1054 (15) Å	T = 223 K
c = 16.5895 (18) Å	0.29 × 0.26 × 0.22 mm
β = 95.520 (9)°

Data collection top

Stoe IPDSII diffractometer	4400 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 1999, 2001)	3450 reflections with I > 2σ(I)
T_min = 0.490, T_max = 0.577	R_int = 0.092
26056 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	0 restraints
wR(F²) = 0.074	All H-atom parameters refined
S = 1.15	Δρ_max = 0.50 e Å⁻³
4400 reflections	Δρ_min = −0.28 e Å⁻³
343 parameters

Special details top

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
Rb	0.01688 (5)	0.43425 (2)	−0.19589 (2)	0.03401 (10)
S1	0.01382 (16)	0.35946 (6)	−0.38945 (6)	0.0451 (3)
S2	−0.20728 (13)	0.51995 (6)	−0.36048 (6)	0.0374 (2)
S3	0.14602 (13)	0.53670 (6)	−0.44812 (5)	0.0348 (2)
P	−0.05739 (12)	0.46416 (5)	−0.42619 (5)	0.0290 (2)
O1	0.2674 (4)	0.54136 (15)	−0.23640 (16)	0.0410 (6)
O2	0.0200 (4)	0.60293 (16)	−0.14890 (16)	0.0415 (7)
O3	−0.2169 (4)	0.50147 (15)	−0.09188 (15)	0.0406 (6)
O4	−0.1161 (3)	0.34506 (15)	−0.06497 (16)	0.0394 (6)
O5	0.1325 (4)	0.27789 (15)	−0.14684 (15)	0.0412 (7)
O6	0.3663 (4)	0.38439 (16)	−0.19993 (16)	0.0416 (7)
C1	0.2628 (7)	0.6212 (3)	−0.2123 (3)	0.0509 (12)
C2	0.0893 (7)	0.6461 (3)	−0.2104 (3)	0.0482 (11)
C3	−0.1428 (7)	0.6269 (3)	−0.1389 (3)	0.0499 (11)
C4	−0.2044 (7)	0.5824 (3)	−0.0707 (3)	0.0479 (11)
C5	−0.2661 (7)	0.4551 (3)	−0.0274 (3)	0.0525 (12)
C6	−0.2744 (6)	0.3710 (3)	−0.0527 (3)	0.0540 (12)
C7	−0.1060 (6)	0.2626 (2)	−0.0796 (3)	0.0473 (11)
C8	0.0674 (6)	0.2404 (2)	−0.0800 (3)	0.0435 (10)
C9	0.3003 (6)	0.2593 (3)	−0.1507 (3)	0.0457 (10)
C10	0.3625 (7)	0.3033 (3)	−0.2188 (3)	0.0476 (11)
C11	0.4266 (6)	0.4296 (3)	−0.2630 (3)	0.0499 (11)
C12	0.4300 (6)	0.5138 (3)	−0.2389 (3)	0.0513 (11)
N13	−0.5159 (6)	0.2422 (3)	−0.4116 (3)	0.0750 (13)
C14	−0.5164 (6)	0.3022 (3)	−0.4407 (3)	0.0478 (10)
C15	−0.5201 (8)	0.3788 (3)	−0.4778 (4)	0.0580 (13)
H1A	0.324 (6)	0.633 (3)	−0.160 (3)	0.054 (13)*
H1B	0.323 (7)	0.652 (3)	−0.252 (3)	0.073 (16)*
H2A	0.026 (5)	0.639 (2)	−0.261 (3)	0.044 (12)*
H2B	0.098 (6)	0.702 (3)	−0.197 (3)	0.062 (14)*
H3A	−0.146 (6)	0.683 (3)	−0.125 (3)	0.065 (14)*
H3B	−0.212 (6)	0.618 (2)	−0.192 (3)	0.050 (13)*
H4A	−0.303 (6)	0.603 (3)	−0.056 (3)	0.054 (13)*
H4B	−0.129 (6)	0.590 (3)	−0.018 (3)	0.056 (13)*
H5A	−0.373 (7)	0.473 (3)	−0.016 (3)	0.077 (17)*
H5B	−0.179 (6)	0.463 (2)	0.019 (3)	0.052 (13)*
H6A	−0.308 (5)	0.342 (2)	−0.008 (3)	0.047 (12)*
H6B	−0.341 (6)	0.367 (3)	−0.106 (3)	0.062 (15)*
H7A	−0.143 (5)	0.237 (2)	−0.036 (2)	0.041 (11)*
H7B	−0.179 (7)	0.253 (3)	−0.132 (3)	0.077 (17)*
H8A	0.078 (5)	0.189 (3)	−0.083 (2)	0.041 (11)*
H8B	0.137 (5)	0.259 (2)	−0.027 (3)	0.050 (12)*
H9A	0.319 (6)	0.204 (3)	−0.158 (3)	0.056 (13)*
H9B	0.364 (5)	0.271 (2)	−0.097 (3)	0.046 (12)*
H10A	0.300 (6)	0.296 (3)	−0.267 (3)	0.050 (13)*
H10B	0.470 (6)	0.287 (3)	−0.229 (3)	0.054 (13)*
H11A	0.537 (6)	0.413 (3)	−0.269 (3)	0.054 (13)*
H11B	0.353 (6)	0.420 (3)	−0.314 (3)	0.061 (14)*
H12A	0.485 (6)	0.520 (3)	−0.186 (3)	0.052 (13)*
H12B	0.480 (6)	0.543 (2)	−0.282 (3)	0.051 (13)*
H15A	−0.451 (8)	0.411 (4)	−0.446 (4)	0.09 (2)*
H15B	−0.493 (7)	0.374 (3)	−0.531 (4)	0.083 (18)*
H15C	−0.630 (9)	0.396 (4)	−0.485 (4)	0.11 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb	0.0386 (2)	0.03336 (18)	0.03045 (17)	−0.00168 (18)	0.00526 (13)	0.00247 (16)
S1	0.0684 (8)	0.0288 (5)	0.0373 (5)	0.0062 (5)	0.0010 (5)	0.0021 (4)
S2	0.0354 (6)	0.0432 (5)	0.0349 (5)	0.0033 (4)	0.0099 (4)	−0.0027 (4)
S3	0.0333 (5)	0.0429 (5)	0.0282 (4)	−0.0058 (4)	0.0022 (4)	0.0005 (4)
P	0.0323 (6)	0.0286 (4)	0.0263 (4)	0.0002 (4)	0.0043 (4)	0.0010 (4)
O1	0.0347 (16)	0.0398 (15)	0.0487 (15)	−0.0043 (12)	0.0055 (12)	0.0030 (12)
O2	0.0426 (18)	0.0380 (15)	0.0440 (15)	0.0020 (13)	0.0046 (13)	0.0031 (12)
O3	0.0415 (17)	0.0390 (15)	0.0412 (15)	0.0022 (13)	0.0036 (12)	0.0018 (12)
O4	0.0361 (17)	0.0375 (15)	0.0453 (15)	−0.0053 (12)	0.0072 (12)	0.0027 (12)
O5	0.0460 (18)	0.0349 (14)	0.0427 (15)	0.0005 (13)	0.0048 (13)	0.0079 (11)
O6	0.0401 (17)	0.0418 (15)	0.0433 (15)	−0.0003 (13)	0.0063 (13)	0.0048 (12)
C1	0.058 (3)	0.038 (2)	0.058 (3)	−0.017 (2)	0.013 (2)	−0.002 (2)
C2	0.063 (3)	0.034 (2)	0.048 (3)	−0.003 (2)	0.008 (2)	0.0046 (19)
C3	0.056 (3)	0.034 (2)	0.059 (3)	0.005 (2)	0.003 (2)	−0.001 (2)
C4	0.045 (3)	0.047 (3)	0.053 (3)	0.005 (2)	0.008 (2)	−0.0113 (19)
C5	0.045 (3)	0.059 (3)	0.057 (3)	0.011 (2)	0.023 (2)	0.011 (2)
C6	0.036 (3)	0.060 (3)	0.068 (3)	−0.004 (2)	0.016 (2)	0.019 (3)
C7	0.059 (3)	0.033 (2)	0.050 (3)	−0.010 (2)	0.007 (2)	0.0054 (19)
C8	0.058 (3)	0.027 (2)	0.046 (2)	−0.002 (2)	0.009 (2)	0.0046 (17)
C9	0.047 (3)	0.040 (2)	0.050 (3)	0.011 (2)	0.002 (2)	0.0071 (19)
C10	0.052 (3)	0.042 (2)	0.050 (3)	0.010 (2)	0.009 (2)	−0.0009 (19)
C11	0.037 (3)	0.057 (3)	0.057 (3)	0.004 (2)	0.014 (2)	0.015 (2)
C12	0.035 (3)	0.056 (3)	0.064 (3)	−0.008 (2)	0.009 (2)	0.014 (2)
N13	0.086 (4)	0.058 (3)	0.081 (3)	0.012 (3)	0.011 (3)	0.009 (2)
C14	0.043 (3)	0.054 (3)	0.046 (2)	0.006 (2)	0.003 (2)	−0.008 (2)
C15	0.065 (4)	0.050 (3)	0.058 (3)	−0.010 (3)	−0.002 (3)	0.003 (2)

Geometric parameters (Å, º) top

Rb—O1	2.885 (3)	C3—C4	1.491 (7)
Rb—O5	2.928 (3)	C3—H3A	0.98 (5)
Rb—O3	2.939 (3)	C3—H3B	1.01 (5)
Rb—O4	2.949 (3)	C4—H4A	0.93 (5)
Rb—O2	2.988 (3)	C4—H4B	1.02 (5)
Rb—O6	3.005 (3)	C5—C6	1.499 (7)
Rb—S1	3.4544 (11)	C5—H5A	0.97 (6)
Rb—S2	3.4692 (11)	C5—H5B	1.01 (5)
S1—P	1.9630 (13)	C6—H6A	0.96 (4)
S2—P	1.9692 (13)	C6—H6B	1.00 (5)
S3—Pⁱ	2.1418 (13)	C7—C8	1.477 (7)
S3—P	2.1421 (14)	C7—H7A	0.92 (4)
P—S3ⁱ	2.1419 (13)	C7—H7B	1.02 (5)
O1—C12	1.423 (6)	C8—H8A	0.89 (4)
O1—C1	1.424 (5)	C8—H8B	1.05 (4)
O2—C2	1.422 (5)	C9—C10	1.489 (6)
O2—C3	1.425 (6)	C9—H9A	0.97 (5)
O3—C5	1.421 (5)	C9—H9B	1.01 (4)
O3—C4	1.430 (5)	C10—H10A	0.91 (5)
O4—C6	1.409 (5)	C10—H10B	0.96 (5)
O4—C7	1.435 (5)	C11—C12	1.495 (7)
O5—C9	1.423 (5)	C11—H11A	0.97 (5)
O5—C8	1.428 (5)	C11—H11B	1.01 (5)
O6—C10	1.422 (5)	C12—H12A	0.95 (5)
O6—C11	1.428 (5)	C12—H12B	1.00 (4)
C1—C2	1.493 (7)	N13—C14	1.135 (6)
C1—H1A	0.98 (5)	C14—C15	1.446 (7)
C1—H1B	1.01 (5)	C15—H15A	0.92 (7)
C2—H2A	0.96 (4)	C15—H15B	0.93 (6)
C2—H2B	0.97 (5)	C15—H15C	0.95 (7)

O1—Rb—O5	115.13 (8)	C4—C3—H3A	108 (3)
O1—Rb—O3	114.25 (8)	Rb—C3—H3A	160 (3)
O5—Rb—O3	114.06 (7)	O2—C3—H3B	108 (3)
O1—Rb—O4	145.48 (8)	C4—C3—H3B	113 (3)
O5—Rb—O4	57.07 (8)	Rb—C3—H3B	80 (2)
O3—Rb—O4	57.31 (7)	H3A—C3—H3B	108 (4)
O1—Rb—O2	57.26 (8)	O3—C4—C3	109.2 (4)
O5—Rb—O2	144.60 (8)	O3—C4—H4A	112 (3)
O3—Rb—O2	57.22 (8)	C3—C4—H4A	112 (3)
O4—Rb—O2	107.56 (7)	O3—C4—H4B	111 (3)
O1—Rb—O6	57.92 (8)	C3—C4—H4B	111 (3)
O5—Rb—O6	57.38 (8)	H4A—C4—H4B	102 (4)
O3—Rb—O6	143.65 (8)	O3—C5—C6	109.5 (4)
O4—Rb—O6	107.03 (7)	O3—C5—H5A	108 (3)
O2—Rb—O6	107.20 (8)	C6—C5—H5A	110 (3)
O1—Rb—S1	87.72 (6)	O3—C5—H5B	105 (3)
O5—Rb—S1	83.87 (5)	C6—C5—H5B	111 (3)
O3—Rb—S1	138.08 (6)	H5A—C5—H5B	113 (4)
O4—Rb—S1	121.53 (6)	O4—C6—C5	109.0 (4)
O2—Rb—S1	126.82 (5)	O4—C6—H6A	107 (3)
O6—Rb—S1	78.21 (6)	C5—C6—H6A	107 (3)
O1—Rb—S2	83.44 (6)	Rb—C6—H6A	155 (3)
O5—Rb—S2	137.62 (6)	O4—C6—H6B	107 (3)
O3—Rb—S2	88.20 (6)	C5—C6—H6B	109 (3)
O4—Rb—S2	126.26 (6)	Rb—C6—H6B	78 (3)
O2—Rb—S2	77.75 (6)	H6A—C6—H6B	118 (4)
O6—Rb—S2	122.65 (5)	O4—C7—C8	108.9 (4)
S1—Rb—S2	57.93 (3)	O4—C7—H7A	108 (3)
P—S1—Rb	85.75 (4)	C8—C7—H7A	106 (3)
P—S2—Rb	85.25 (4)	Rb—C7—H7A	156 (3)
Pⁱ—S3—P	87.88 (5)	O4—C7—H7B	105 (3)
S1—P—S2	117.02 (6)	C8—C7—H7B	116 (3)
S1—P—S3ⁱ	111.07 (6)	Rb—C7—H7B	82 (3)
S2—P—S3ⁱ	111.69 (6)	H7A—C7—H7B	112 (4)
S1—P—S3	111.50 (7)	O5—C8—C7	108.9 (4)
S2—P—S3	110.75 (6)	O5—C8—H8A	111 (3)
S3ⁱ—P—S3	92.12 (5)	C7—C8—H8A	111 (3)
S1—P—Rb	63.64 (4)	O5—C8—H8B	108 (2)
S2—P—Rb	64.06 (4)	C7—C8—H8B	111 (2)
S3ⁱ—P—Rb	166.70 (5)	H8A—C8—H8B	107 (3)
S3—P—Rb	101.17 (4)	O5—C9—C10	109.1 (4)
C12—O1—C1	112.1 (4)	O5—C9—H9A	113 (3)
C12—O1—Rb	119.4 (2)	C10—C9—H9A	110 (3)
C1—O1—Rb	120.3 (3)	O5—C9—H9B	110 (2)
C2—O2—C3	112.3 (3)	C10—C9—H9B	112 (2)
C2—O2—Rb	108.0 (2)	H9A—C9—H9B	103 (4)
C3—O2—Rb	108.9 (2)	O6—C10—C9	109.1 (4)
C5—O3—C4	112.0 (3)	O6—C10—H10A	109 (3)
C5—O3—Rb	118.3 (2)	C9—C10—H10A	113 (3)
C4—O3—Rb	119.2 (2)	Rb—C10—H10A	78 (3)
C6—O4—C7	113.8 (3)	O6—C10—H10B	109 (3)
C6—O4—Rb	110.9 (2)	C9—C10—H10B	112 (3)
C7—O4—Rb	110.6 (2)	Rb—C10—H10B	160 (3)
C9—O5—C8	111.9 (3)	H10A—C10—H10B	105 (4)
C9—O5—Rb	118.8 (2)	O6—C11—C12	108.9 (4)
C8—O5—Rb	119.3 (2)	O6—C11—H11A	108 (3)
C10—O6—C11	111.6 (3)	C12—C11—H11A	109 (3)
C10—O6—Rb	106.3 (3)	Rb—C11—H11A	160 (3)
C11—O6—Rb	105.3 (2)	O6—C11—H11B	108 (3)
O1—C1—C2	109.4 (4)	C12—C11—H11B	112 (3)
O1—C1—H1A	115 (3)	Rb—C11—H11B	76 (3)
C2—C1—H1A	109 (3)	H11A—C11—H11B	111 (4)
O1—C1—H1B	107 (3)	O1—C12—C11	109.5 (4)
C2—C1—H1B	113 (3)	O1—C12—H12A	108 (3)
H1A—C1—H1B	103 (4)	C11—C12—H12A	110 (3)
O2—C2—C1	108.5 (4)	O1—C12—H12B	108 (3)
O2—C2—H2A	110 (3)	C11—C12—H12B	107 (2)
C1—C2—H2A	113 (3)	H12A—C12—H12B	115 (4)
Rb—C2—H2A	82 (2)	N13—C14—C15	179.0 (6)
O2—C2—H2B	112 (3)	C14—C15—H15A	108 (4)
C1—C2—H2B	103 (3)	C14—C15—H15B	109 (4)
Rb—C2—H2B	162 (3)	H15A—C15—H15B	114 (5)
H2A—C2—H2B	110 (4)	C14—C15—H15C	109 (4)
O2—C3—C4	109.5 (4)	H15A—C15—H15C	115 (6)
O2—C3—H3A	111 (3)	H15B—C15—H15C	102 (5)

Symmetry code: (i) −x, −y+1, −z−1.

Experimental details

Crystal data
Chemical formula	[Rb₂(P₂S₆)(C₁₂H₂₄O₆)₂]·2C₂H₃N
M_r	1035.98
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	223
a, b, c (Å)	8.2261 (9), 17.1054 (15), 16.5895 (18)
β (°)	95.520 (9)
V (Å³)	2323.5 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.50
Crystal size (mm)	0.29 × 0.26 × 0.22

Data collection
Diffractometer	Stoe IPDSII diffractometer
Absorption correction	Numerical (X-SHAPE and X-RED; Stoe & Cie, 1999, 2001)
T_min, T_max	0.490, 0.577
No. of measured, independent and observed [I > 2σ(I)] reflections	26056, 4400, 3450
R_int	0.092
(sin θ/λ)_max (Å⁻¹)	0.610

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.047, 0.074, 1.15
No. of reflections	4400
No. of parameters	343
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.50, −0.28

Computer programs: X-AREA (Stoe & Cie, 2002), SHELXS97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 2012), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF (Westrip, 2010).

References

Brockner, W., Becker, R., Eisenmann, B. & Schäfer, H. (1985). Z. Anorg. Allg. Chem. 520, 51–58. CrossRef CAS Web of Science Google Scholar
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854. Web of Science CrossRef CAS IUCr Journals Google Scholar
Gjikaj, M., Adam, A. & Brockner, W. (2006). Z. Anorg. Allg. Chem. 632, 279–283. Web of Science CSD CrossRef CAS Google Scholar
Gjikaj, M., Adam, A., Duewel, M. & Brockner, W. (2005). Z. Kristallogr. New Cryst. Struct. 220, 67. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (1999). X-SHAPE. Stoe & Cie GmbH, Darmstadt, Germany. Google Scholar
Stoe & Cie (2001). X-RED. Stoe & Cie GmbH, Darmstadt, Germany. Google Scholar
Stoe & Cie (2002). X-AREA. Stoe & Cie GmbH, Darmstadt, Germany. Google Scholar
Thilo, E. & Ladwig, G. (1962). Monatsber. Dtsch Akad. Wiss. Berlin, 4, 720–724. CAS Google Scholar
Toffoli, P., Khodadad, P. & Rodier, N. (1978). Acta Cryst. B34, 3561–3564. CrossRef CAS IUCr Journals Web of Science Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 69| Part 12| December 2013| Page m689

doi:10.1107/S1600536813032121

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

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