Rb₂Sb₄O₁₁

The title compound, dirubidium tetra­anti­monate(V), Rb₂Sb₄O₁₁, has been synthesized by flux reaction. It is isotypic with known A₂Sb₄O₁₁ (A = K, Cs) structures and consists of an (Sb₄O₁₁)²⁻ skeleton and two Rb atoms as charge-compensating cations. Distorted SbO₆ octa­hedra share edges and corners, resulting in a layered assembly. Alternate stacking of the layers along the c axis leads to the formation of tunnels. The Rb⁺ ions, surrounded by nine and ten O atoms, respectively, are located in these tunnels. Some atoms in the structure are on special positions of m symmetry (two Sb atoms, both Rb atoms and four O atoms) and 2 symmetry (one O atom).

Related literature

Isotypic structures have been reported by Hong (1974) [K₂Sb₄O₁₁] and by Hirschle et al. (2001) [Cs₂Sb₄O₁₁]. For Rb—O distances in the crystal structure of Rb₃Ti₂(TiO)(PO₄)₃P₂O₇, see: Duhlev (1994).

Experimental

Crystal data

• Rb₂Sb₄O₁₁

• M_r = 833.94

• Monoclinic, C 2/m

• a = 19.5045 (11) Å

• b = 7.5681 (4) Å

• c = 7.2115 (4) Å

• β = 95.203 (3)°

• V = 1060.12 (10) ų

• Z = 4

• Mo Kα radiation

• μ = 19.26 mm⁻¹

• T = 120 K

• 0.12 × 0.12 × 0.11 mm

Data collection

• Nonius KappaCCD diffractometer

• Absorption correction: multi-scan (SADABS; Sheldrick, 2007) T_min = 0.110, T_max = 0.120

• 7605 measured reflections

• 1312 independent reflections

• 1234 reflections with I > 2σ(I)

• R_int = 0.038

Refinement

• R[F² > 2σ(F²)] = 0.028

• wR(F²) = 0.072

• S = 1.41

• 1312 reflections

• 91 parameters

• 18 restraints

• Δρ_max = 1.89 e Å⁻³

• Δρ_min = −1.91 e Å⁻³

Table 1
Selected bond lengths (Å)

Sb1—O4	1.940 (4)
Sb1—O3^i	1.956 (5)
Sb1—O1^ii	1.986 (3)
Sb1—O2	2.089 (5)
Sb2—O3^iii	1.903 (5)
Sb2—O6^iv	1.970 (3)
Sb2—O2^v	1.977 (5)
Sb2—O5^iii	1.993 (5)
Sb2—O2^iii	2.129 (5)
Sb3—O8	1.9281 (15)
Sb3—O4	1.959 (4)
Sb3—O7^vi	1.978 (4)
Sb3—O7	1.979 (4)
Sb3—O6	2.005 (4)
Sb3—O5	2.0261 (14)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+1; (iii) -x+1, -y, -z+1; (iv) -x+1, y, -z+1; (v) x-1, y, z; (vi) .

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT; data reduction: DENZO nd COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supporting information

S1. Comment

Single crystals of the title compound (1), were formed inadvertently during one of our flux syntheses aimed at producing new oxides in the quaternary Rb/Sb/B/O system. There are two A₂Sb₄O₁₁ (A = K, Cs) compounds known and their structures were determined by single-crystal X-ray diffraction (Hong, 1974 and Hirschle et al., 2001). A₂Sb₄O₁₁(A = K, Cs) crystallize in the centrosymmetric space group C2/m and have two-dimensional structures with Sb in octahedral coordination. In K₂Sb₄O₁₁, the K⁺ ions are mobile in the tunnels. The K⁺ ions have been ion-exchanged with Na⁺, Ag⁺, Rb⁺ and TI⁺ in molten salts, but neither their unit-cell parameters nor their crystal structures are available (Hong, 1974). In Cs₂Sb₄O₁₁, Cs⁺ ions are not mobile (Hirschle et al., 2001). Here, we report the crystal structure of Rb₂Sb₄O₁₁, confirming that it is isotypic with A₂Sb₄O₁₁ (A = K, Cs).

The crystal structure of compound (1) contains two Rb (Rb1 and Rb2), three Sb (Sb1, Sb2 and Sb3) and eight O (O1—O8) atoms (Fig.1). The atoms Sb1, O4, O6 and O7 are on general positions, all other atoms are on special positions, viz. mirror planes and twofold-rotation axes. Each antimony atom is coordinated to six oxygen atoms to form distorted octahedra with Sb—O distances ranging from 1.903 (4) to 2.129 (5) Å, comparable to those in the isotypic antimonates(V) (Hong, 1974; Hirschle et al., 2001). Rb1 is nine fold coordinated and Rb2 is ten fold coordinated to oxygen atoms (Fig. 2 (a) and 2(b)) with Rb—O distances ranging from 2.933 (4) - 3.473 (4) Å, comparable to Rb₃Ti₂(TiO)(PO₄)₃P₂O₇ (Duhlev, 1994). The coordination number of Rb⁺ ion differs from the the 11 coordinated A⁺ ions reported for the isotypic A₂Sb₄O₁₁ (A = K, Cs) compounds, where the non bonding distances of K—O; 3.78 (3) - 3.832 (4) Å, Cs—O; 3.721 (8) - 3.940 (9) Å were considered as bonds.

In the asymmetric unit of the title compound (1) all oxygen atoms are shared between two SbO₆ octahedra, except the oxygen atoms O(2) and O(4), that are common to all three Sb(1)O₆, Sb(2)O₆ and Sb(3)O₆ octahedra (Fig. 1). In compound (1), there are two different layers (1 and 2) formed by edge-sharing of Sb(1)—Sb(1), Sb(2)—Sb(2) and Sb(3)—Sb(3) octahedra to form three types of Sb₂O₁₀ dimers (Fig. 3). Layer 1 is formed by edge-sharing of the Sb₂(2)O₁₀ and Sb₂(3)O₁₀ dimers and layer 2 is formed by Sb₂(1)O₁₀ dimers sharing corners with the layer 1. Alternate stacking of these two layers along the c axis leads to formation of tunnels and Rb⁺ ions are located in these tunnels. The single-crystal data was measured at 123 K and the displacement parameters observed for Rb⁺ are roughly isotropic, indicating that they are not mobile in the channels.

Related literature

Isotypic structures have been reported by Hong (1974) [K₂Sb₄O₁₁] and by Hirschle et al. (2001) [Cs₂Sb₄O₁₁]. For Rb—O distances in the crystal structure of Rb₃Ti₂(TiO)(PO₄)₃P₂O₇, see: Duhlev (1994).

S2. Experimental

A mixture of Rb₂CO₃ (Aldrich, 0.6224 g; 2.70 mmol), Sb₂O₃ (Aldrich, 0.3143 g; 1.08 mmol) and H₃BO₃ (Aldrich,0.5000 g; 8.09 mmol) was ground in a mortar and pestle. The ground mixture was then added into a platinum crucible. The furnace temperature was slowly raised from room temperature and heated at 773 K for 12 hrs, 923 K for a further 12 hrs, and then kept at 1273 K for 24 hrs. The furnace was cooled to room temperature over a period of 48 hrs. The melt was washed with hot water to remove the excess boric acid, filtered and dried in an oven at 353 K. Colourless crystals of compound (1) were obtained from the melt.

S3. Refinement

All atoms were refined anisotropically. It was necessary to apply SHELX ISOR restraints to O2, O5 and O1; a value of 0.001 Ų was used. The highest peak and the deepest hole of the final Fourier map are located at 1.85 Šfrom Rb1 and 0.85 Šfrom the Sb2 atom, respectively.

Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998); data reduction: DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures

	Fig. 1. ORTEP plot of the asymmetric unit of compound (1) Thermal ellipsoids are given at the 50% probability level. [Symmetry codes: (i) x, -y, z; (ii) -x + 2, -y, -z + 2; (iii) -x + 2, -y - 1, -z + 2; (iv) -x + 2, y - 1, -z + 1; (v) -x + 2, -y - 1, -z + 1; (vi) x, y - 1, z; (vii) -x + 3/2, -y - 1/2, -z + 1].
	Fig. 2. ORTEP diagrams of the coordination environment of (a) Rb1 and (b) Rb2 atoms of compound (1). Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes (i) x, -y, z; (ii) -x + 2, -y, -z + 2; iii) -x + 2, -y - 1, -z + 2; (iv) -x + 2, y - 1, -z + 1; (v) -x + 2, -y - 1, -z + 1].
	Fig. 3. Polyhedral representation of compound (1) along the ac plane: blue octahedra, red spheres, green spheres represent SbO6, O and Rb atoms respectively

Dirubidium tetraantimonate(V)

Crystal data

Rb2Sb4O11	F(000) = 1464
Mr = 833.94	Dx = 5.225 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2y	Cell parameters from 1307 reflections
a = 19.5045 (11) Å	θ = 2.9–27.5°
b = 7.5681 (4) Å	µ = 19.26 mm^−1
c = 7.2115 (4) Å	T = 120 K
β = 95.203 (3)°	Block, colourless
V = 1060.12 (10) Å^3	0.12 × 0.12 × 0.11 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	1312 independent reflections
Radiation source: Nonius FR591 Rotating Anode	1234 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
Detector resolution: 9.091 pixels mm^-1	θmax = 27.6°, θmin = 3.7°
ϕ and ω scans	h = −25→25
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	k = −9→9
Tmin = 0.110, Tmax = 0.120	l = −9→8
7605 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	w = 1/[σ^2(Fo^2) + (0.029P)^2 + 1.4332P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.072	(Δ/σ)max = 0.001
S = 1.41	Δρmax = 1.89 e Å^−3
1312 reflections	Δρmin = −1.91 e Å^−3
91 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
18 restraints	Extinction coefficient: 0.00092 (9)

Special details

Experimental. SADABS was used to perform the Absorption correction

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 (Ų)

	x	y	z	Uiso*/Ueq
Sb1	0.92822 (2)	0.0000	0.90178 (6)	0.00457 (16)
Sb2	0.07568 (2)	0.0000	0.61748 (6)	0.00476 (16)
Sb3	0.825607 (17)	−0.25714 (4)	0.56390 (5)	0.00453 (15)
Rb1	0.99190 (4)	−0.5000	0.74518 (10)	0.0115 (2)
Rb2	0.73468 (4)	0.0000	0.00596 (10)	0.0128 (2)
O1	0.0000	0.1704 (7)	0.0000	0.0060 (10)
O2	0.9765 (3)	0.0000	0.6548 (7)	0.0045 (10)
O3	0.8831 (3)	0.0000	0.1331 (7)	0.0080 (11)
O4	0.8715 (2)	−0.1971 (5)	0.8087 (5)	0.0081 (8)
O5	0.8339 (3)	0.0000	0.4910 (7)	0.0072 (10)
O6	0.9112 (2)	−0.2537 (4)	0.4296 (5)	0.0061 (8)
O7	0.7364 (2)	−0.2127 (5)	0.6665 (5)	0.0069 (8)
O8	0.8392 (3)	−0.5000	0.6392 (7)	0.0070 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb1	0.0050 (3)	0.0049 (3)	0.0039 (3)	0.000	0.00008 (18)	0.000
Sb2	0.0046 (3)	0.0052 (3)	0.0045 (3)	0.000	0.00049 (18)	0.000
Sb3	0.0045 (2)	0.0042 (2)	0.0049 (2)	−0.00016 (12)	0.00030 (15)	−0.00009 (11)
Rb1	0.0108 (4)	0.0125 (4)	0.0111 (4)	0.000	0.0012 (3)	0.000
Rb2	0.0155 (4)	0.0137 (4)	0.0096 (4)	0.000	0.0027 (3)	0.000
O1	0.0054 (13)	0.0058 (13)	0.0067 (13)	0.000	0.0007 (9)	0.000
O2	0.0041 (13)	0.0048 (13)	0.0047 (13)	0.000	0.0004 (9)	0.000
O3	0.012 (3)	0.010 (3)	0.002 (2)	0.000	0.001 (2)	0.000
O4	0.011 (2)	0.0064 (18)	0.0073 (19)	−0.0017 (16)	0.0009 (15)	0.0001 (14)
O5	0.0067 (13)	0.0076 (13)	0.0073 (13)	0.000	0.0009 (9)	0.000
O6	0.0042 (19)	0.005 (2)	0.009 (2)	0.0001 (13)	0.0008 (15)	0.0010 (13)
O7	0.006 (2)	0.0095 (18)	0.0050 (18)	0.0001 (16)	0.0024 (14)	−0.0001 (14)
O8	0.009 (3)	0.006 (2)	0.006 (2)	0.000	−0.001 (2)	0.000

Geometric parameters (Å, º)

Sb1—O4	1.940 (4)	Rb1—O8	3.007 (5)
Sb1—O4^i	1.940 (4)	Rb1—O6^x	3.011 (4)
Sb1—O3^ii	1.956 (5)	Rb1—O6^xi	3.011 (4)
Sb1—O1^iii	1.986 (3)	Rb1—O1^iv	3.094 (4)
Sb1—O1^iv	1.986 (3)	Rb1—O1^xii	3.094 (4)
Sb1—O2	2.089 (5)	Rb1—O6^xiii	3.238 (4)
Sb1—Sb1^v	3.0211 (10)	Rb1—O6	3.238 (4)
Sb2—O3^iv	1.903 (5)	Rb1—O4^xiii	3.343 (4)
Sb2—O6^vi	1.970 (3)	Rb1—O4	3.343 (4)
Sb2—O6^iv	1.970 (3)	Rb1—Rb1^xi	3.5787 (14)
Sb2—O2^vii	1.977 (5)	Rb1—Rb1^xiv	3.6602 (14)
Sb2—O5^iv	1.993 (5)	Rb2—O7^xv	2.933 (4)
Sb2—O2^iv	2.129 (5)	Rb2—O7^xvi	2.933 (4)
Sb2—Sb3^iv	3.1084 (5)	Rb2—O3	2.956 (5)
Sb2—Sb3^vi	3.1084 (5)	Rb2—O8^ix	3.048 (5)
Sb2—Sb2^viii	3.2679 (10)	Rb2—O7^xvii	3.222 (4)
Sb3—O8	1.9281 (15)	Rb2—O7^ix	3.222 (4)
Sb3—O4	1.959 (4)	Rb2—O4^ix	3.440 (4)
Sb3—O7^ix	1.978 (4)	Rb2—O4^xvii	3.440 (4)
Sb3—O7	1.979 (4)	Rb2—O4^xvi	3.473 (4)
Sb3—O6	2.005 (4)	Rb2—O4^xv	3.473 (4)
Sb3—O5	2.0261 (14)	Rb2—Rb2^xviii	3.8331 (3)
Sb3—Sb3^ix	3.0111 (7)	Rb2—Rb2^xix	3.8331 (3)
Sb3—Sb2^iv	3.1084 (5)
O4—Sb1—O4^i	100.5 (2)	O6^xiii—Rb1—O6	70.31 (13)
O4—Sb1—O3^ii	90.47 (15)	O8—Rb1—O4^xiii	48.93 (8)
O4^i—Sb1—O3^ii	90.47 (15)	O6^x—Rb1—O4^xiii	163.20 (9)
O4—Sb1—O1^iii	169.68 (15)	O6^xi—Rb1—O4^xiii	96.20 (9)
O4^i—Sb1—O1^iii	89.17 (16)	O1^iv—Rb1—O4^xiii	118.05 (7)
O3^ii—Sb1—O1^iii	93.05 (12)	O1^xii—Rb1—O4^xiii	50.52 (7)
O4—Sb1—O1^iv	89.17 (16)	O6^xiii—Rb1—O4^xiii	53.05 (9)
O4^i—Sb1—O1^iv	169.68 (16)	O6—Rb1—O4^xiii	100.87 (10)
O3^ii—Sb1—O1^iv	93.05 (12)	O8—Rb1—O4	48.93 (8)
O1^iii—Sb1—O1^iv	81.0 (2)	O6^x—Rb1—O4	96.20 (9)
O4—Sb1—O2	89.55 (13)	O6^xi—Rb1—O4	163.20 (9)
O4^i—Sb1—O2	89.55 (14)	O1^iv—Rb1—O4	50.52 (7)
O3^ii—Sb1—O2	180.0 (2)	O1^xii—Rb1—O4	118.05 (7)
O1^iii—Sb1—O2	86.92 (11)	O6^xiii—Rb1—O4	100.87 (10)
O1^iv—Sb1—O2	86.92 (11)	O6—Rb1—O4	53.05 (9)
O4—Sb1—Sb1^v	129.58 (11)	O4^xiii—Rb1—O4	86.60 (13)
O4^i—Sb1—Sb1^v	129.58 (11)	O7^xv—Rb2—O7^xvi	66.58 (15)
O3^ii—Sb1—Sb1^v	94.01 (16)	O7^xv—Rb2—O3	100.00 (11)
O1^iii—Sb1—Sb1^v	40.48 (11)	O7^xvi—Rb2—O3	100.00 (11)
O1^iv—Sb1—Sb1^v	40.48 (11)	O7^xv—Rb2—O8^ix	137.98 (10)
O2—Sb1—Sb1^v	85.95 (14)	O7^xvi—Rb2—O8^ix	137.98 (10)
O3^iv—Sb2—O6^vi	96.46 (12)	O3—Rb2—O8^ix	105.29 (14)
O3^iv—Sb2—O6^iv	96.46 (12)	O7^xv—Rb2—O7^xvii	165.42 (8)
O6^vi—Sb2—O6^iv	154.0 (2)	O7^xvi—Rb2—O7^xvii	103.13 (8)
O3^iv—Sb2—O2^vii	101.9 (2)	O3—Rb2—O7^xvii	70.82 (10)
O6^vi—Sb2—O2^vii	99.63 (12)	O8^ix—Rb2—O7^xvii	56.58 (9)
O6^iv—Sb2—O2^vii	99.63 (12)	O7^xv—Rb2—O7^ix	103.13 (8)
O3^iv—Sb2—O5^iv	93.3 (2)	O7^xvi—Rb2—O7^ix	165.42 (8)
O6^vi—Sb2—O5^iv	78.42 (12)	O3—Rb2—O7^ix	70.82 (10)
O6^iv—Sb2—O5^iv	78.42 (12)	O8^ix—Rb2—O7^ix	56.58 (9)
O2^vii—Sb2—O5^iv	164.8 (2)	O7^xvii—Rb2—O7^ix	84.86 (13)
O3^iv—Sb2—O2^iv	176.5 (2)	O7^xv—Rb2—O4^ix	90.66 (9)
O6^vi—Sb2—O2^iv	84.25 (12)	O7^xvi—Rb2—O4^ix	137.99 (10)
O6^iv—Sb2—O2^iv	84.25 (12)	O3—Rb2—O4^ix	119.13 (9)
O2^vii—Sb2—O2^iv	74.6 (2)	O8^ix—Rb2—O4^ix	47.69 (7)
O5^iv—Sb2—O2^iv	90.24 (19)	O7^xvii—Rb2—O4^ix	103.67 (9)
O3^iv—Sb2—Sb3^iv	99.95 (13)	O7^ix—Rb2—O4^ix	48.47 (9)
O6^vi—Sb2—Sb3^iv	116.27 (12)	O7^xv—Rb2—O4^xvii	137.99 (10)
O6^iv—Sb2—Sb3^iv	38.97 (12)	O7^xvi—Rb2—O4^xvii	90.66 (9)
O2^vii—Sb2—Sb3^iv	135.10 (7)	O3—Rb2—O4^xvii	119.13 (9)
O5^iv—Sb2—Sb3^iv	39.73 (3)	O8^ix—Rb2—O4^xvii	47.69 (7)
O2^iv—Sb2—Sb3^iv	82.79 (11)	O7^xvii—Rb2—O4^xvii	48.47 (9)
O3^iv—Sb2—Sb3^vi	99.95 (13)	O7^ix—Rb2—O4^xvii	103.67 (9)
O6^vi—Sb2—Sb3^vi	38.97 (12)	O4^ix—Rb2—O4^xvii	83.58 (13)
O6^iv—Sb2—Sb3^vi	116.27 (12)	O7^xv—Rb2—O4^xvi	80.00 (10)
O2^vii—Sb2—Sb3^vi	135.10 (7)	O7^xvi—Rb2—O4^xvi	49.82 (9)
O5^iv—Sb2—Sb3^vi	39.73 (3)	O3—Rb2—O4^xvi	50.19 (10)
O2^iv—Sb2—Sb3^vi	82.79 (11)	O8^ix—Rb2—O4^xvi	141.55 (9)
Sb3^iv—Sb2—Sb3^vi	77.522 (16)	O7^xvii—Rb2—O4^xvi	85.45 (9)
O3^iv—Sb2—Sb2^viii	140.79 (17)	O7^ix—Rb2—O4^xvi	120.02 (9)
O6^vi—Sb2—Sb2^viii	92.06 (12)	O4^ix—Rb2—O4^xvi	163.25 (10)
O6^iv—Sb2—Sb2^viii	92.06 (12)	O4^xvii—Rb2—O4^xvi	112.65 (7)
O2^vii—Sb2—Sb2^viii	38.89 (14)	O7^xv—Rb2—O4^xv	49.82 (9)
O5^iv—Sb2—Sb2^viii	125.90 (15)	O7^xvi—Rb2—O4^xv	80.00 (10)
O2^iv—Sb2—Sb2^viii	35.67 (14)	O3—Rb2—O4^xv	50.19 (10)
Sb3^iv—Sb2—Sb2^viii	110.286 (17)	O8^ix—Rb2—O4^xv	141.55 (9)
Sb3^vi—Sb2—Sb2^viii	110.286 (17)	O7^xvii—Rb2—O4^xv	120.02 (9)
O8—Sb3—O4	85.82 (18)	O7^ix—Rb2—O4^xv	85.45 (9)
O8—Sb3—O7^ix	100.65 (19)	O4^ix—Rb2—O4^xv	112.65 (7)
O4—Sb3—O7^ix	168.10 (15)	O4^xvii—Rb2—O4^xv	163.25 (10)
O8—Sb3—O7	99.2 (2)	O4^xvi—Rb2—O4^xv	50.88 (12)
O4—Sb3—O7	88.24 (15)	Rb2^xviii—Rb2—Rb2^xix	161.64 (5)
O7^ix—Sb3—O7	80.91 (16)	Sb3^ix—O7—Sb3	99.09 (16)
O8—Sb3—O6	92.83 (19)	Sb3^ix—O7—Rb2^ii	135.39 (17)
O4—Sb3—O6	95.72 (15)	Sb3—O7—Rb2^ii	118.83 (16)
O7^ix—Sb3—O6	93.94 (15)	Sb3^ix—O7—Rb2^ix	126.22 (16)
O7—Sb3—O6	167.60 (15)	Sb3—O7—Rb2^ix	93.33 (13)
O8—Sb3—O5	167.6 (2)	Rb2^ii—O7—Rb2^ix	76.87 (8)
O4—Sb3—O5	88.31 (18)	Sb2^iv—O6—Sb3	102.87 (16)
O7^ix—Sb3—O5	87.13 (18)	Sb2^iv—O6—Rb1^xi	115.79 (16)
O7—Sb3—O5	91.56 (18)	Sb3—O6—Rb1^xi	140.87 (15)
O6—Sb3—O5	76.85 (17)	Sb2^iv—O6—Rb1	128.30 (17)
O8—Sb3—Sb3^ix	103.08 (16)	Sb3—O6—Rb1	91.48 (12)
O4—Sb3—Sb3^ix	128.50 (11)	Rb1^xi—O6—Rb1	69.77 (8)
O7^ix—Sb3—Sb3^ix	40.47 (11)	Sb2^xx—O2—Sb1	129.7 (2)
O7—Sb3—Sb3^ix	40.43 (10)	Sb2^xx—O2—Sb2^iv	105.4 (2)
O6—Sb3—Sb3^ix	133.40 (11)	Sb1—O2—Sb2^iv	124.9 (2)
O5—Sb3—Sb3^ix	89.14 (15)	Sb2^iv—O3—Sb1^xv	128.4 (3)
O8—Sb3—Sb2^iv	129.85 (16)	Sb2^iv—O3—Rb2	127.7 (2)
O4—Sb3—Sb2^iv	89.09 (11)	Sb1^xv—O3—Rb2	103.86 (19)
O7^ix—Sb3—Sb2^iv	94.24 (11)	Sb2^iv—O5—Sb3^i	101.30 (15)
O7—Sb3—Sb2^iv	130.51 (11)	Sb2^iv—O5—Sb3	101.30 (15)
O6—Sb3—Sb2^iv	38.16 (9)	Sb3^i—O5—Sb3	147.7 (3)
O5—Sb3—Sb2^iv	38.97 (15)	Sb1^xxi—O1—Sb1^iv	99.0 (2)
Sb3^ix—Sb3—Sb2^iv	118.398 (18)	Sb1^xxi—O1—Rb1^iv	137.03 (6)
O8—Rb1—O6^x	122.58 (10)	Sb1^iv—O1—Rb1^iv	108.38 (6)
O8—Rb1—O6^xi	122.58 (10)	Sb1^xxi—O1—Rb1^xxii	108.38 (6)
O6^x—Rb1—O6^xi	76.51 (14)	Sb1^iv—O1—Rb1^xxii	137.03 (6)
O8—Rb1—O1^iv	98.45 (6)	Rb1^iv—O1—Rb1^xxii	72.53 (11)
O6^x—Rb1—O1^iv	75.47 (8)	Sb3^xiii—O8—Sb3	144.8 (3)
O6^xi—Rb1—O1^iv	138.39 (8)	Sb3^xiii—O8—Rb1	100.33 (16)
O8—Rb1—O1^xii	98.45 (6)	Sb3—O8—Rb1	100.33 (16)
O6^x—Rb1—O1^xii	138.39 (8)	Sb3^xiii—O8—Rb2^ix	99.97 (16)
O6^xi—Rb1—O1^xii	75.47 (8)	Sb3—O8—Rb2^ix	99.97 (16)
O1^iv—Rb1—O1^xii	107.47 (11)	Rb1—O8—Rb2^ix	108.63 (15)
O8—Rb1—O6^xiii	54.15 (10)	Sb1—O4—Sb3	133.59 (19)
O6^x—Rb1—O6^xiii	110.23 (8)	Sb1—O4—Rb1	100.91 (14)
O6^xi—Rb1—O6^xiii	68.45 (13)	Sb3—O4—Rb1	89.24 (12)
O1^iv—Rb1—O6^xiii	151.31 (8)	Sb1—O4—Rb2^ix	136.26 (15)
O1^xii—Rb1—O6^xiii	87.06 (8)	Sb3—O4—Rb2^ix	87.33 (12)
O8—Rb1—O6	54.15 (10)	Rb1—O4—Rb2^ix	92.95 (9)
O6^x—Rb1—O6	68.45 (13)	Sb1—O4—Rb2^ii	87.90 (12)
O6^xi—Rb1—O6	110.23 (8)	Sb3—O4—Rb2^ii	99.39 (14)
O1^iv—Rb1—O6	87.06 (8)	Rb1—O4—Rb2^ii	157.86 (12)
O1^xii—Rb1—O6	151.31 (8)	Rb2^ix—O4—Rb2^ii	67.35 (7)

Symmetry codes: (i) x, −y, z; (ii) x, y, z+1; (iii) x+1, y, z+1; (iv) −x+1, −y, −z+1; (v) −x+2, −y, −z+2; (vi) −x+1, y, −z+1; (vii) x−1, y, z; (viii) −x, −y, −z+1; (ix) −x+3/2, −y−1/2, −z+1; (x) −x+2, y, −z+1; (xi) −x+2, −y−1, −z+1; (xii) x+1, y−1, z+1; (xiii) x, −y−1, z; (xiv) −x+2, −y−1, −z+2; (xv) x, y, z−1; (xvi) x, −y, z−1; (xvii) −x+3/2, y+1/2, −z+1; (xviii) −x+3/2, −y+1/2, −z; (xix) −x+3/2, −y−1/2, −z; (xx) x+1, y, z; (xxi) x−1, y, z−1; (xxii) x−1, y+1, z−1.