Face-to-face stacking of quinoid rings of alkali salts of bromanilic acid

A series of alkali salts of hydrogen bromanilic acid trihydrates (K⁺, Rb⁺ and Cs⁺, potassium, rubidium and caesium 2,5-dibromo-4-hydroxy-3,6-dioxocyclohexa-1,4-dien-1-olate trihydrate), bromanilic acid tetrahydrate (Na⁺, disodium 2,5-dibromo-3,6-dioxocyclohexa-1,4-diene-1,4-diolate tetrahydrate) and bromanilic acid dihydrates (K⁺, Rb⁺ and Cs⁺, dipotasium, dirubidium and dicaesium 2,5-dibromo-3,6-dioxo­cyclohexa-1,4-diene-1,4-diolate dihydrate) were prepared and studied by single-crystal X-ray diffraction. Their crystal packings are dominated by quinoid ring stacking. The monoanionic quinoid rings pack face-to-face without offset and with short centroid separations (3.25–3.30 Å), while the dianionic rings form offset stacks (1.4–1.8 Å) with a larger centroid separation (3.8–4.1 Å).

Computing details

Data collection: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) for Cs2BAx2H2O, Rb2BAx2H2O; CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) for K2BAx2H2O, Na2BAx4H2O; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) for RbHBAx3H2O, CsHBAx3H2O. Cell refinement: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) for Cs2BAx2H2O, Rb2BAx2H2O; CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) for K2BAx2H2O, Na2BAx4H2O; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) for RbHBAx3H2O, CsHBAx3H2O. Data reduction: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) for Cs2BAx2H2O, Rb2BAx2H2O; CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) for K2BAx2H2O, Na2BAx4H2O; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) for RbHBAx3H2O, CsHBAx3H2O. Program(s) used to solve structure: SHELXS86 (Sheldrick, 1986) for Cs2BAx2H2O, K2BAx2H2O, Rb2BAx2H2O; SHELXS97 (Sheldrick, 1997) for RbHBAx3H2O, Na2BAx4H2O; SIR92 (Giacovazzo et al., 1993) for CsHBAx3H2O. For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

(Cs2BAx2H2O)

Crystal data

C6H2Br2Cs2O6	F(000) = 536
Mr = 597.73	Dx = 3.134 Mg m^−3
Monoclinic, P21/n	Cu Kα radiation, λ = 1.54179 Å
a = 4.3380 (1) Å	Cell parameters from 1393 reflections
b = 9.7036 (3) Å	θ = 2.9–75.4°
c = 15.1253 (5) Å	µ = 52.40 mm^−1
β = 95.793 (3)°	T = 293 K
V = 633.44 (3) Å^3	Prism, red
Z = 2	0.15 × 0.10 × 0.05 mm

Data collection

Oxford Xcalibur Nova diffractometer	1315 independent reflections
Radiation source: Enhance (Cu) X-ray Source	1226 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.073
Detector resolution: 10.4323 pixels mm^-1	θmax = 75.8°, θmin = 5.4°
CCD detector, ω scans	h = −5→4
Absorption correction: multi-scan	k = −12→11
Tmin = 0.118, Tmax = 1	l = −18→18
2628 measured reflections

Refinement

Refinement on F^2	4 restraints
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.074	w = 1/[σ^2(Fo^2) + (0.1689P)^2 + 1.3043P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.204	(Δ/σ)max < 0.001
S = 1.05	Δρmax = 2.24 e Å^−3
1315 reflections	Δρmin = −2.70 e Å^−3
81 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
O1	−0.3416 (18)	0.3870 (8)	0.3592 (4)	0.0332 (15)
C1	−0.1934 (19)	0.4353 (9)	0.4268 (5)	0.0205 (15)
C3	−0.110 (2)	0.3626 (8)	0.5056 (5)	0.0209 (16)
C2	0.0690 (19)	0.4152 (8)	0.5801 (5)	0.0192 (15)
O2	0.1401 (18)	0.3553 (7)	0.6502 (5)	0.0297 (15)
O3	0.6740 (17)	−0.0691 (9)	0.3070 (4)	0.0369 (18)
Cs1	0.19316 (12)	0.15932 (6)	0.30117 (4)	0.0301 (4)
Br1	−0.2536 (3)	0.17834 (11)	0.51276 (7)	0.0367 (4)
H3A	0.74 (2)	−0.138 (6)	0.349 (4)	0.01 (2)*
H3B	0.66 (2)	−0.118 (9)	0.252 (3)	0.04 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.056 (4)	0.028 (3)	0.012 (3)	−0.014 (3)	−0.014 (3)	0.005 (2)
C1	0.028 (4)	0.021 (4)	0.011 (3)	−0.002 (3)	−0.005 (3)	−0.003 (3)
C3	0.044 (5)	0.010 (3)	0.008 (3)	−0.004 (3)	0.004 (3)	−0.002 (3)
C2	0.029 (4)	0.019 (4)	0.009 (3)	0.002 (3)	−0.002 (3)	0.002 (3)
O2	0.044 (4)	0.021 (3)	0.021 (4)	−0.003 (3)	−0.008 (3)	0.008 (2)
O3	0.062 (5)	0.026 (4)	0.022 (3)	0.008 (3)	0.002 (3)	0.007 (3)
Cs1	0.0287 (5)	0.0250 (5)	0.0350 (6)	−0.00105 (16)	−0.0046 (3)	−0.00379 (18)
Br1	0.0622 (8)	0.0198 (6)	0.0257 (7)	−0.0132 (4)	−0.0076 (5)	0.0044 (3)

Geometric parameters (Å, º)

O1—C1	1.243 (10)	O3—Cs1^vi	3.167 (8)
O1—Cs1^i	3.061 (7)	O3—Cs1^vii	3.411 (8)
O1—Cs1	3.383 (8)	O3—H3A	0.95 (2)
O1—Cs1^ii	3.800 (7)	O3—H3B	0.95 (2)
C1—C3	1.401 (11)	Cs1—O1^vi	3.061 (7)
C1—C2^iii	1.554 (12)	Cs1—O2^viii	3.144 (8)
C1—Cs1	3.773 (8)	Cs1—O2^ix	3.145 (8)
C3—C2	1.399 (11)	Cs1—O3^i	3.167 (8)
C3—Br1	1.900 (8)	Cs1—O3^x	3.411 (8)
C2—O2	1.222 (10)	Cs1—O1^xi	3.800 (7)
C2—C1^iii	1.554 (12)	Cs1—Br1^vi	3.8062 (13)
O2—Cs1^iv	3.144 (8)	Cs1—Br1	3.9096 (14)
O2—Cs1^v	3.145 (8)	Br1—Cs1^i	3.8062 (13)
O3—Cs1	3.039 (8)
C1—O1—Cs1^i	141.2 (6)	O3^i—Cs1—O3^x	104.78 (6)
C1—O1—Cs1	98.5 (6)	O1—Cs1—O3^x	47.19 (15)
Cs1^i—O1—Cs1	84.47 (18)	O3—Cs1—C1	147.32 (17)
C1—O1—Cs1^ii	113.8 (6)	O1^vi—Cs1—C1	69.9 (2)
Cs1^i—O1—Cs1^ii	96.22 (16)	O2^viii—Cs1—C1	93.00 (17)
Cs1—O1—Cs1^ii	122.01 (19)	O2^ix—Cs1—C1	137.36 (17)
O1—C1—C3	125.3 (8)	O3^i—Cs1—C1	97.43 (19)
O1—C1—C2^iii	116.8 (7)	O1—Cs1—C1	19.01 (16)
C3—C1—C2^iii	117.7 (7)	O3^x—Cs1—C1	58.89 (17)
O1—C1—Cs1	62.5 (5)	O3—Cs1—O1^xi	75.02 (18)
C3—C1—Cs1	88.9 (5)	O1^vi—Cs1—O1^xi	153.56 (4)
C2^iii—C1—Cs1	117.0 (5)	O2^viii—Cs1—O1^xi	43.73 (16)
C2—C3—C1	125.2 (8)	O2^ix—Cs1—O1^xi	75.07 (17)
C2—C3—Br1	117.1 (6)	O3^i—Cs1—O1^xi	44.81 (17)
C1—C3—Br1	117.7 (6)	O1—Cs1—O1^xi	112.22 (7)
O2—C2—C3	126.6 (8)	O3^x—Cs1—O1^xi	95.35 (15)
O2—C2—C1^iii	116.3 (7)	C1—Cs1—O1^xi	130.14 (17)
C3—C2—C1^iii	117.1 (7)	O3—Cs1—Br1^vi	68.79 (13)
C2—O2—Cs1^iv	139.4 (6)	O1^vi—Cs1—Br1^vi	51.85 (12)
C2—O2—Cs1^v	122.1 (6)	O2^viii—Cs1—Br1^vi	169.46 (15)
Cs1^iv—O2—Cs1^v	87.23 (19)	O2^ix—Cs1—Br1^vi	103.31 (14)
Cs1—O3—Cs1^vi	88.7 (2)	O3^i—Cs1—Br1^vi	113.59 (12)
Cs1—O3—Cs1^vii	105.3 (2)	O1—Cs1—Br1^vi	98.10 (10)
Cs1^vi—O3—Cs1^vii	145.7 (2)	O3^x—Cs1—Br1^vi	126.17 (12)
Cs1—O3—H3A	134 (5)	C1—Cs1—Br1^vi	79.45 (12)
Cs1^vi—O3—H3A	111 (6)	O1^xi—Cs1—Br1^vi	138.48 (10)
Cs1^vii—O3—H3A	82 (5)	O3—Cs1—Br1	113.96 (13)
Cs1—O3—H3B	110 (3)	O1^vi—Cs1—Br1	95.64 (14)
Cs1^vi—O3—H3B	109 (8)	O2^viii—Cs1—Br1	101.06 (15)
Cs1^vii—O3—H3B	37 (8)	O2^ix—Cs1—Br1	171.71 (14)
H3A—O3—H3B	103 (4)	O3^i—Cs1—Br1	66.27 (13)
O3—Cs1—O1^vi	95.0 (2)	O1—Cs1—Br1	49.26 (11)
O3—Cs1—O2^viii	117.35 (18)	O3^x—Cs1—Br1	96.32 (12)
O1^vi—Cs1—O2^viii	132.34 (18)	C1—Cs1—Br1	43.29 (13)
O3—Cs1—O2^ix	61.08 (18)	O1^xi—Cs1—Br1	110.80 (12)
O1^vi—Cs1—O2^ix	78.68 (19)	Br1^vi—Cs1—Br1	68.40 (2)
O2^viii—Cs1—O2^ix	87.23 (19)	O3—Cs1—Cs1^i	133.12 (16)
O3—Cs1—O3^i	88.7 (2)	O1^vi—Cs1—Cs1^i	129.09 (16)
O1^vi—Cs1—O3^i	161.32 (17)	O2^viii—Cs1—Cs1^i	46.39 (15)
O2^viii—Cs1—O3^i	59.74 (17)	O2^ix—Cs1—Cs1^i	133.62 (14)
O2^ix—Cs1—O3^i	118.75 (18)	O3^i—Cs1—Cs1^i	44.45 (14)
O3—Cs1—O1	162.85 (15)	O1—Cs1—Cs1^i	44.61 (11)
O1^vi—Cs1—O1	84.47 (18)	O3^x—Cs1—Cs1^i	65.25 (13)
O2^viii—Cs1—O1	74.04 (16)	C1—Cs1—Cs1^i	60.31 (12)
O2^ix—Cs1—O1	134.99 (17)	O1^xi—Cs1—Cs1^i	70.31 (12)
O3^i—Cs1—O1	86.66 (18)	Br1^vi—Cs1—Cs1^i	123.07 (2)
O3—Cs1—O3^x	149.71 (5)	Br1—Cs1—Cs1^i	54.67 (2)
O1^vi—Cs1—O3^x	80.92 (18)	C3—Br1—Cs1^i	100.4 (3)
O2^viii—Cs1—O3^x	53.22 (16)	C3—Br1—Cs1	78.8 (3)
O2^ix—Cs1—O3^x	88.79 (18)	Cs1^i—Br1—Cs1	68.40 (2)
Cs1^i—O1—C1—C3	25.1 (16)	Cs1^ii—O1—Cs1—O1^xi	−72.7 (3)
Cs1—O1—C1—C3	−66.7 (9)	C1—O1—Cs1—Br1^vi	11.2 (5)
Cs1^ii—O1—C1—C3	162.6 (7)	Cs1^i—O1—Cs1—Br1^vi	−129.83 (9)
Cs1^i—O1—C1—C2^iii	−160.2 (7)	Cs1^ii—O1—Cs1—Br1^vi	136.27 (18)
Cs1—O1—C1—C2^iii	108.0 (7)	C1—O1—Cs1—Br1	63.3 (5)
Cs1^ii—O1—C1—C2^iii	−22.7 (9)	Cs1^i—O1—Cs1—Br1	−77.66 (14)
Cs1^i—O1—C1—Cs1	91.8 (9)	Cs1^ii—O1—Cs1—Br1	−171.6 (3)
Cs1^ii—O1—C1—Cs1	−130.7 (5)	C1—O1—Cs1—Cs1^i	141.0 (6)
O1—C1—C3—C2	176.8 (9)	Cs1^ii—O1—Cs1—Cs1^i	−93.9 (2)
C2^iii—C1—C3—C2	2.1 (14)	O1—C1—Cs1—O3	−155.2 (5)
Cs1—C1—C3—C2	122.3 (9)	C3—C1—Cs1—O3	−23.8 (7)
O1—C1—C3—Br1	−3.7 (13)	C2^iii—C1—Cs1—O3	97.0 (6)
C2^iii—C1—C3—Br1	−178.5 (6)	O1—C1—Cs1—O1^vi	138.2 (6)
Cs1—C1—C3—Br1	−58.3 (6)	C3—C1—Cs1—O1^vi	−90.4 (5)
C1—C3—C2—O2	178.4 (9)	C2^iii—C1—Cs1—O1^vi	30.4 (5)
Br1—C3—C2—O2	−1.0 (13)	O1—C1—Cs1—O2^viii	3.8 (5)
C1—C3—C2—C1^iii	−2.1 (14)	C3—C1—Cs1—O2^viii	135.2 (5)
Br1—C3—C2—C1^iii	178.5 (6)	C2^iii—C1—Cs1—O2^viii	−104.0 (5)
C3—C2—O2—Cs1^iv	146.7 (7)	O1—C1—Cs1—O2^ix	93.0 (6)
C1^iii—C2—O2—Cs1^iv	−32.8 (13)	C3—C1—Cs1—O2^ix	−135.6 (5)
C3—C2—O2—Cs1^v	−83.1 (10)	C2^iii—C1—Cs1—O2^ix	−14.8 (6)
C1^iii—C2—O2—Cs1^v	97.4 (8)	O1—C1—Cs1—O3^i	−56.0 (5)
Cs1^vi—O3—Cs1—O1^vi	−18.35 (16)	C3—C1—Cs1—O3^i	75.4 (5)
Cs1^vii—O3—Cs1—O1^vi	−166.61 (19)	C2^iii—C1—Cs1—O3^i	−163.8 (5)
Cs1^vi—O3—Cs1—O2^viii	125.41 (19)	C3—C1—Cs1—O1	131.4 (8)
Cs1^vii—O3—Cs1—O2^viii	−22.8 (3)	C2^iii—C1—Cs1—O1	−107.8 (8)
Cs1^vi—O3—Cs1—O2^ix	55.78 (18)	O1—C1—Cs1—O3^x	46.8 (5)
Cs1^vii—O3—Cs1—O2^ix	−92.5 (2)	C3—C1—Cs1—O3^x	178.2 (6)
Cs1^vi—O3—Cs1—O3^i	180	C2^iii—C1—Cs1—O3^x	−61.0 (5)
Cs1^vii—O3—Cs1—O3^i	31.7 (2)	O1—C1—Cs1—O1^xi	−21.7 (6)
Cs1^vi—O3—Cs1—O1	−105.8 (6)	C3—C1—Cs1—O1^xi	109.7 (5)
Cs1^vii—O3—Cs1—O1	105.9 (6)	C2^iii—C1—Cs1—O1^xi	−129.5 (5)
Cs1^vi—O3—Cs1—O3^x	62.2 (4)	O1—C1—Cs1—Br1^vi	−168.8 (5)
Cs1^vii—O3—Cs1—O3^x	−86.0 (4)	C3—C1—Cs1—Br1^vi	−37.4 (5)
Cs1^vi—O3—Cs1—C1	−78.3 (4)	C2^iii—C1—Cs1—Br1^vi	83.4 (5)
Cs1^vii—O3—Cs1—C1	133.5 (3)	O1—C1—Cs1—Br1	−99.1 (6)
Cs1^vi—O3—Cs1—O1^xi	136.75 (18)	C3—C1—Cs1—Br1	32.3 (4)
Cs1^vii—O3—Cs1—O1^xi	−11.51 (17)	C2^iii—C1—Cs1—Br1	153.1 (6)
Cs1^vi—O3—Cs1—Br1^vi	−63.99 (11)	O1—C1—Cs1—Cs1^i	−30.6 (5)
Cs1^vii—O3—Cs1—Br1^vi	147.7 (2)	C3—C1—Cs1—Cs1^i	100.8 (5)
Cs1^vi—O3—Cs1—Br1	−116.79 (11)	C2^iii—C1—Cs1—Cs1^i	−138.4 (5)
Cs1^vii—O3—Cs1—Br1	94.95 (15)	C2—C3—Br1—Cs1^i	171.0 (6)
Cs1^vi—O3—Cs1—Cs1^i	180	C1—C3—Br1—Cs1^i	−8.5 (7)
Cs1^vii—O3—Cs1—Cs1^i	31.7 (2)	C2—C3—Br1—Cs1	−123.7 (7)
C1—O1—Cs1—O3	50.1 (10)	C1—C3—Br1—Cs1	56.8 (7)
Cs1^i—O1—Cs1—O3	−90.9 (7)	O3—Cs1—Br1—C3	127.0 (3)
Cs1^ii—O1—Cs1—O3	175.2 (6)	O1^vi—Cs1—Br1—C3	28.9 (3)
C1—O1—Cs1—O1^vi	−39.0 (6)	O2^viii—Cs1—Br1—C3	−106.2 (3)
Cs1^i—O1—Cs1—O1^vi	180	O2^ix—Cs1—Br1—C3	75.3 (9)
Cs1^ii—O1—Cs1—O1^vi	86.1 (2)	O3^i—Cs1—Br1—C3	−155.9 (3)
C1—O1—Cs1—O2^viii	−176.0 (6)	O1—Cs1—Br1—C3	−48.8 (3)
Cs1^i—O1—Cs1—O2^viii	42.99 (17)	O3^x—Cs1—Br1—C3	−52.5 (3)
Cs1^ii—O1—Cs1—O2^viii	−50.9 (2)	C1—Cs1—Br1—C3	−23.7 (3)
C1—O1—Cs1—O2^ix	−106.9 (5)	O1^xi—Cs1—Br1—C3	−150.7 (3)
Cs1^i—O1—Cs1—O2^ix	112.1 (2)	Br1^vi—Cs1—Br1—C3	74.0 (3)
Cs1^ii—O1—Cs1—O2^ix	18.2 (3)	Cs1^i—Cs1—Br1—C3	−106.0 (3)
C1—O1—Cs1—O3^i	124.5 (5)	O3—Cs1—Br1—Cs1^i	−127.00 (17)
Cs1^i—O1—Cs1—O3^i	−16.46 (14)	O1^vi—Cs1—Br1—Cs1^i	134.96 (14)
Cs1^ii—O1—Cs1—O3^i	−110.4 (2)	O2^viii—Cs1—Br1—Cs1^i	−0.19 (12)
C1—O1—Cs1—O3^x	−121.7 (6)	O2^ix—Cs1—Br1—Cs1^i	−178.7 (8)
Cs1^i—O1—Cs1—O3^x	97.3 (2)	O3^i—Cs1—Br1—Cs1^i	−49.89 (14)
Cs1^ii—O1—Cs1—O3^x	3.37 (18)	O1—Cs1—Br1—Cs1^i	57.24 (15)
Cs1^i—O1—Cs1—C1	−141.0 (6)	O3^x—Cs1—Br1—Cs1^i	53.50 (12)
Cs1^ii—O1—Cs1—C1	125.1 (6)	C1—Cs1—Br1—Cs1^i	82.36 (17)
C1—O1—Cs1—O1^xi	162.2 (5)	O1^xi—Cs1—Br1—Cs1^i	−44.68 (11)
Cs1^i—O1—Cs1—O1^xi	21.22 (15)	Br1^vi—Cs1—Br1—Cs1^i	180

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

(K2BAx2H2O)

Crystal data

C6H4Br2K2O6	F(000) = 392
Mr = 410.11	Dx = 2.509 Mg m^−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54179 Å
a = 3.8441 (2) Å	Cell parameters from 1580 reflections
b = 9.4171 (4) Å	θ = 3.0–75.9°
c = 15.1001 (6) Å	µ = 16.50 mm^−1
β = 96.813 (4)°	T = 293 K
V = 542.77 (4) Å^3	Prism, red
Z = 2	0.20 × 0.15 × 0.05 mm

Data collection

Oxford Xcalibur Nova diffractometer	1112 independent reflections
Radiation source: Enhance (Cu) X-ray Source	956 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 10.4323 pixels mm^-1	θmax = 76.1°, θmin = 5.6°
CCD detector, ω scans	h = −3→4
Absorption correction: multi-scan	k = −11→10
Tmin = 0.242, Tmax = 1	l = −18→17
2213 measured reflections

Refinement

Refinement on F^2	3 restraints
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.041	w = 1/[σ^2(Fo^2) + (0.0818P)^2 + 0.287P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.122	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 0.80 e Å^−3
1112 reflections	Δρmin = −0.6 e Å^−3
80 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.8935 (3)	0.67047 (10)	0.20849 (7)	0.0362 (3)
Br1	0.22706 (13)	0.83316 (5)	0.49510 (3)	0.0360 (2)
O1	0.6912 (9)	0.3778 (3)	0.35130 (18)	0.0349 (7)
O2	0.4778 (9)	0.6497 (3)	0.34675 (19)	0.0311 (6)
O3	1.3461 (10)	0.4562 (4)	0.1909 (2)	0.0442 (8)
H3A	1.442 (15)	0.456 (7)	0.2506 (16)	0.050 (16)*
H3B	1.445 (17)	0.379 (6)	0.164 (4)	0.06*
C1	0.6085 (9)	0.4293 (4)	0.4219 (2)	0.0220 (7)
C2	0.4807 (9)	0.5847 (4)	0.4190 (2)	0.0212 (7)
C3	0.3741 (10)	0.6428 (4)	0.4977 (2)	0.0223 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0291 (5)	0.0356 (5)	0.0456 (6)	0.0010 (3)	0.0126 (4)	0.0081 (3)
Br1	0.0440 (4)	0.0249 (3)	0.0401 (3)	0.00683 (15)	0.0092 (2)	0.00109 (14)
O1	0.0509 (18)	0.0316 (15)	0.0234 (13)	0.0142 (14)	0.0097 (11)	−0.0026 (11)
O2	0.0453 (18)	0.0276 (14)	0.0218 (13)	0.0037 (12)	0.0099 (11)	0.0049 (10)
O3	0.061 (2)	0.0371 (17)	0.0326 (14)	0.0140 (16)	−0.0018 (13)	−0.0087 (13)
C1	0.0234 (17)	0.0206 (16)	0.0222 (15)	0.0018 (13)	0.0042 (12)	−0.0012 (12)
C2	0.0237 (17)	0.0194 (16)	0.0200 (15)	−0.0003 (13)	0.0011 (11)	0.0006 (12)
C3	0.0268 (18)	0.0141 (14)	0.0265 (17)	0.0036 (14)	0.0048 (12)	−0.0021 (12)

Geometric parameters (Å, º)

K1—O1^i	2.742 (3)	O2—C2	1.250 (5)
K1—O1^ii	3.033 (4)	O3—K1	2.698 (3)
K1—O2	2.782 (3)	O3—K1^iii	2.905 (4)
K1—O2^iii	2.886 (3)	O3—K1^v	3.276 (4)
K1—O3^iv	2.905 (4)	O3—H3A	0.933 (19)
K1—O3^i	3.276 (4)	O3—H3B	0.93 (2)
Br1—C3	1.878 (4)	C1—C3^vii	1.386 (5)
O1—K1^v	2.742 (3)	C2—C1	1.542 (5)
O1—K1^vi	3.033 (4)	C2—C3	1.413 (5)
O1—C1	1.246 (4)	C3—C1^vii	1.386 (5)
O2—K1^iv	2.886 (3)
K1^iii—K1—K1^i	82.16 (2)	O2^iii—K1—Br1^viii	169.37 (7)
K1^iv—K1—K1^i	97.84 (2)	O2—K1—O1^ii	78.31 (8)
K1^iii—K1—Br1^viii	124.262 (15)	O2^iii—K1—O1^ii	138.13 (9)
K1^ix—Br1—K1^x	61.747 (18)	O2—K1—O2^iii	85.38 (8)
K1^iv—K1—Br1^viii	55.738 (15)	O2—K1—O3^iv	62.97 (9)
K1^v—O1—K1^vi	83.30 (9)	O2^iii—K1—O3^iv	120.82 (9)
K1—O2—K1^iv	85.38 (8)	O2—K1—O3^i	59.45 (8)
K1—O3—K1^iii	86.56 (10)	O2^iii—K1—O3^i	87.57 (9)
K1—O3—K1^v	110.40 (13)	O2—K1—H3A	104.5 (10)
K1^iii—O3—K1^v	140.23 (12)	O2^iii—K1—H3A	47.1 (8)
K1—O3—H3A	95 (4)	O2—C2—C1	117.3 (3)
K1^iii—O3—H3A	74 (4)	O2—C2—C3	124.8 (3)
K1^v—O3—H3A	69 (4)	O3—K1—K1^iii	48.96 (9)
K1—O3—H3B	158 (4)	O3^iv—K1—K1^iii	135.53 (7)
K1^iii—O3—H3B	104 (5)	O3^i—K1—K1^iii	109.64 (7)
K1^v—O3—H3B	74 (5)	O3—K1—K1^iv	131.04 (9)
Br1^xi—K1—K1^i	99.83 (3)	O3^iv—K1—K1^iv	44.47 (7)
Br1^viii—K1—K1^i	107.12 (3)	O3^i—K1—K1^iv	70.36 (7)
Br1^xi—K1—K1^iii	62.515 (18)	O3—K1—K1^i	130.66 (9)
Br1^xi—K1—K1^iv	117.485 (18)	O3^iv—K1—K1^i	141.78 (8)
Br1^xi—K1—Br1^viii	61.747 (18)	O3^i—K1—K1^i	30.95 (6)
O1^ii—K1—K1^iii	134.89 (6)	O3—K1—Br1^xi	66.61 (8)
O1^i—K1—K1^iv	128.41 (8)	O3^iv—K1—Br1^xi	104.01 (7)
O1^ii—K1—K1^iv	45.11 (6)	O3^i—K1—Br1^xi	124.86 (6)
O1^i—K1—K1^iii	51.59 (8)	O3—K1—Br1^viii	106.39 (7)
O1^i—K1—K1^i	46.84 (7)	O3^iv—K1—Br1^viii	61.12 (7)
O1^ii—K1—K1^i	63.54 (6)	O3^i—K1—Br1^viii	101.46 (6)
O1^i—K1—Br1^xi	55.25 (6)	O3—K1—O1^ii	156.34 (9)
O1^ii—K1—Br1^xi	93.99 (6)	O3^iv—K1—O1^ii	85.22 (9)
O1^i—K1—Br1^viii	94.92 (7)	O3—K1—O1^i	95.32 (12)
O1^ii—K1—Br1^viii	50.51 (6)	O3—K1—O2	117.12 (11)
O1^i—K1—O1^ii	83.30 (9)	O3—K1—O2^iii	64.21 (9)
O1^i—K1—O2	134.90 (10)	O3—K1—O3^iv	86.56 (10)
O1^i—K1—O2^iii	81.55 (9)	O3—K1—O3^i	151.66 (5)
O1^i—K1—O3^iv	155.27 (10)	O3^iv—K1—O3^i	111.88 (4)
O1^i—K1—O3^i	76.96 (9)	O3—K1—H3A	18.4 (6)
O1^ii—K1—O3^i	50.95 (8)	O3^iv—K1—H3A	92.0 (13)
O1^i—K1—H3A	97.5 (13)	O3^i—K1—H3A	134.4 (7)
O1^ii—K1—H3A	174.7 (6)	C1—O1—K1^v	140.9 (2)
O1—C1—C2	117.3 (3)	C1—O1—K1^vi	104.5 (2)
O1—C1—C3^vii	124.6 (3)	C1^vii—C3—Br1	118.0 (3)
O2—K1—K1^iii	131.55 (7)	C1^vii—C3—C2	123.9 (3)
O2^iii—K1—K1^iii	46.18 (6)	C2—O2—K1	138.0 (3)
O2—K1—K1^i	88.24 (7)	C2—O2—K1^iv	126.2 (3)
O2—K1—K1^iv	48.45 (7)	C2—C3—Br1	117.9 (3)
O2^iii—K1—K1^iv	133.82 (6)	C3—Br1—K1^ix	96.32 (12)
O2^iii—K1—K1^i	77.80 (7)	C3—Br1—K1^x	78.83 (12)
O2—K1—Br1^viii	103.98 (7)	C3^vii—C1—C2	118.2 (3)
O2—K1—Br1^xi	165.10 (8)	C3—C2—C1	117.9 (3)
O2^iii—K1—Br1^xi	108.48 (7)	H3A—O3—H3B	106 (4)
K1^iii—K1—O2—C2	−37.3 (4)	K1^v—O3—K1—O2	20.21 (14)
K1^iv—K1—O2—C2	142.7 (4)	K1^iii—O3—K1—O2^iii	−53.20 (8)
K1^i—K1—O2—C2	−115.2 (4)	K1^v—O3—K1—O2^iii	89.85 (12)
K1^iii—K1—O2—K1^iv	180	K1^iii—O3—K1—O3^iv	180
K1^i—K1—O2—K1^iv	102.10 (6)	K1^v—O3—K1—O3^iv	−36.95 (14)
K1^ix—Br1—C3—C1^vii	−13.4 (3)	K1^iii—O3—K1—O3^i	−47.53 (19)
K1^x—Br1—C3—C1^vii	46.1 (3)	K1^v—O3—K1—O3^i	95.5 (2)
K1^ix—Br1—C3—C2	170.4 (3)	Br1^viii—K1—O2—K1^iv	−5.12 (8)
K1^x—Br1—C3—C2	−130.1 (3)	Br1^xi—K1—O2—K1^iv	−21.2 (3)
K1^v—O1—C1—C2	154.7 (3)	Br1^xi—K1—O2—C2	121.5 (4)
K1^vi—O1—C1—C2	−108.0 (3)	Br1^viii—K1—O2—C2	137.6 (4)
K1^v—O1—C1—C3^vii	−24.8 (7)	O1^i—K1—O2—K1^iv	106.78 (13)
K1^vi—O1—C1—C3^vii	72.5 (4)	O1^ii—K1—O2—K1^iv	38.77 (8)
K1—O2—C2—C1	−39.0 (5)	O1^i—K1—O2—C2	−110.5 (4)
K1^iv—O2—C2—C1	92.6 (4)	O1^ii—K1—O2—C2	−178.6 (4)
K1—O2—C2—C3	141.4 (3)	O2^iii—K1—O2—K1^iv	180
K1^iv—O2—C2—C3	−87.1 (4)	O2^iii—K1—O2—C2	−37.3 (4)
K1^v—O3—K1—K1^iii	143.05 (14)	O2—C2—C1—O1	−1.9 (5)
K1^iii—O3—K1—K1^iv	180	O2—C2—C1—C3^vii	177.7 (3)
K1^v—O3—K1—K1^iv	−36.95 (14)	O2—C2—C3—Br1	−1.6 (5)
K1^iii—O3—K1—K1^i	−9.61 (14)	O2—C2—C3—C1^vii	−177.5 (4)
K1^v—O3—K1—K1^i	133.44 (9)	O3—K1—O2—K1^iv	−122.12 (10)
K1^iii—O3—K1—Br1^xi	73.13 (7)	O3^iv—K1—O2—K1^iv	−51.81 (9)
K1^v—O3—K1—Br1^xi	−143.82 (12)	O3^i—K1—O2—K1^iv	90.09 (9)
K1^iii—O3—K1—Br1^viii	121.47 (6)	O3—K1—O2—C2	20.5 (4)
K1^v—O3—K1—Br1^viii	−95.48 (9)	O3^iv—K1—O2—C2	90.9 (4)
K1^iii—O3—K1—O1^ii	110.2 (2)	O3^i—K1—O2—C2	−127.2 (4)
K1^v—O3—K1—O1^ii	−106.8 (2)	C1—C2—C3—Br1	178.8 (3)
K1^iii—O3—K1—O1^i	24.74 (10)	C1—C2—C3—C1^vii	2.8 (6)
K1^v—O3—K1—O1^i	167.79 (11)	C3—C2—C1—O1	177.8 (3)
K1^iii—O3—K1—O2	−122.84 (10)	C3—C2—C1—C3^vii	−2.7 (6)

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

(Rb2BAx2H2O)

Crystal data

C6H4Br2O6Rb2	F(000) = 464
Mr = 502.85	Dx = 2.892 Mg m^−3
Monoclinic, P21/n	Cu Kα radiation, λ = 1.54179 Å
a = 4.0228 (1) Å	Cell parameters from 3650 reflections
b = 9.5488 (3) Å	θ = 2.9–75.5°
c = 15.1307 (4) Å	µ = 19.25 mm^−1
β = 96.521 (2)°	T = 293 K
V = 577.45 (3) Å^3	Prism, red
Z = 2	0.30 × 0.16 × 0.03 mm

Data collection

Oxford Xcalibur Nova diffractometer	1181 independent reflections
Radiation source: Enhance (Cu) X-ray Source	1159 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 10.4323 pixels mm^-1	θmax = 75.7°, θmin = 5.5°
CCD detector, ω scans	h = −5→3
Absorption correction: multi-scan	k = −11→11
Tmin = 0.151, Tmax = 1	l = −15→18
3568 measured reflections

Refinement

Refinement on F^2	3 restraints
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.047	w = 1/[σ^2(Fo^2) + (0.0858P)^2 + 1.211P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.128	(Δ/σ)max = 0.001
S = 1.12	Δρmax = 0.77 e Å^−3
1181 reflections	Δρmin = −2.03 e Å^−3
81 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Rb1	0.18573 (11)	0.16602 (5)	0.29598 (3)	0.0342 (3)
Br1	−0.25701 (15)	0.17109 (5)	0.50657 (4)	0.0375 (3)
O1	−0.3435 (9)	0.3832 (4)	0.35487 (18)	0.0357 (7)
O2	0.1364 (9)	0.3510 (3)	0.65169 (19)	0.0330 (7)
O3	0.6604 (10)	−0.0562 (4)	0.3093 (2)	0.0426 (9)
H3A	0.62 (5)	−0.016 (10)	0.251 (3)	0.30 (11)*
H3B	0.673 (18)	−0.154 (3)	0.297 (5)	0.05 (2)*
C1	−0.1903 (10)	0.4320 (4)	0.4239 (2)	0.0218 (7)
C3	−0.1149 (10)	0.3585 (4)	0.5031 (3)	0.0230 (7)
C2	0.0650 (10)	0.4153 (4)	0.5798 (2)	0.0215 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rb1	0.0279 (4)	0.0366 (4)	0.0370 (4)	−0.00123 (13)	−0.0007 (2)	−0.00569 (15)
Br1	0.0508 (4)	0.0288 (4)	0.0317 (4)	−0.00875 (17)	−0.0008 (3)	0.00185 (15)
O1	0.0517 (19)	0.0353 (17)	0.0178 (13)	−0.0140 (15)	−0.0062 (12)	−0.0020 (12)
O2	0.051 (2)	0.0314 (16)	0.0145 (13)	−0.0022 (13)	−0.0054 (13)	0.0048 (11)
O3	0.063 (2)	0.040 (2)	0.0255 (15)	0.0099 (16)	0.0104 (15)	0.0081 (14)
C1	0.0283 (18)	0.0240 (18)	0.0131 (14)	−0.0022 (14)	0.0020 (13)	−0.0008 (13)
C3	0.032 (2)	0.0177 (17)	0.0191 (17)	−0.0020 (14)	0.0020 (15)	0.0009 (14)
C2	0.0289 (19)	0.0214 (19)	0.0144 (14)	0.0008 (14)	0.0031 (13)	0.0017 (13)

Geometric parameters (Å, º)

Br1—Rb1^i	3.6821 (7)	O2—Rb1^vii	2.997 (3)
Rb1—Br1^ii	3.6821 (7)	O3—Rb1	2.846 (4)
Rb1—Br1	3.8231 (8)	O3—Rb1^ii	3.017 (4)
Rb1—O1^ii	2.880 (3)	O3—Rb1^viii	3.318 (4)
Rb1—O2^iii	2.929 (3)	O3—H3A	0.95 (2)
Rb1—O2^iv	2.997 (3)	O3—H3B	0.95 (2)
Rb1—O3^i	3.017 (4)	C1—Rb1	3.627 (4)
Rb1—O3^v	3.318 (4)	C1—C2^ix	1.546 (5)
Rb1—H3A	2.62 (16)	C1—C3	1.392 (5)
O1—Rb1^i	2.880 (3)	C2—O2	1.254 (5)
O1—Rb1	3.171 (4)	C2—C1^ix	1.546 (5)
O1—C1	1.242 (5)	C3—Br1	1.881 (4)
O2—Rb1^vi	2.929 (3)	C3—C2	1.405 (5)
Rb1^i—Br1—Rb1	64.792 (12)	O2^iii—Rb1—O3^i	62.34 (9)
Rb1^i—Rb1—H3A	134 (4)	O2^iv—Rb1—O3^i	119.78 (9)
Rb1^ii—Rb1—H3A	46 (4)	O2^iii—Rb1—O3^v	56.41 (9)
Rb1^i—O1—Rb1	83.18 (9)	O2^iv—Rb1—O3^v	87.10 (9)
Rb1^vi—O2—Rb1^vii	85.50 (8)	O2^iii—Rb1—C1	96.41 (9)
Rb1—O3—Rb1^ii	86.59 (10)	O2^iv—Rb1—C1	138.64 (9)
Rb1—O3—Rb1^viii	108.70 (12)	O2^iii—Rb1—H3A	104 (3)
Rb1^ii—O3—Rb1^viii	142.11 (11)	O2^iv—Rb1—H3A	45.2 (17)
Rb1—O3—H3A	66 (9)	O2—C2—C1^ix	116.7 (3)
Rb1^ii—O3—H3A	73 (10)	O2—C2—C3	125.0 (4)
Rb1^viii—O3—H3A	82 (8)	O3—Rb1—Rb1^i	131.52 (8)
Rb1—O3—H3B	140 (4)	O3^i—Rb1—Rb1^i	44.93 (7)
Rb1^ii—O3—H3B	129 (4)	O3^v—Rb1—Rb1^i	68.58 (7)
Rb1^viii—O3—H3B	32 (5)	O3—Rb1—Rb1^ii	48.48 (8)
Br1^ii—Rb1—Rb1^ii	59.300 (12)	O3^i—Rb1—Rb1^ii	135.07 (7)
Br1—Rb1—Rb1^ii	124.092 (11)	O3^v—Rb1—Rb1^ii	111.42 (7)
Br1^ii—Rb1—Rb1^i	120.700 (12)	O3—Rb1—Br1^ii	67.11 (7)
Br1—Rb1—Rb1^i	55.908 (11)	O3^i—Rb1—Br1^ii	108.29 (6)
Br1^ii—Rb1—Br1	64.792 (12)	O3^v—Rb1—Br1^ii	125.87 (6)
Br1^ii—Rb1—H3A	83 (2)	O3—Rb1—Br1	108.84 (7)
Br1—Rb1—H3A	127.9 (12)	O3^i—Rb1—Br1	63.72 (6)
O1^ii—Rb1—Rb1^i	128.49 (8)	O3^v—Rb1—Br1	100.37 (6)
O1—Rb1—Rb1^i	45.31 (6)	O3—Rb1—O1^ii	95.89 (12)
O1^ii—Rb1—Rb1^ii	51.51 (8)	O3—Rb1—O1	159.07 (8)
O1—Rb1—Rb1^ii	134.69 (6)	O3^i—Rb1—O1	86.75 (9)
O1^ii—Rb1—Br1^ii	53.74 (6)	O3—Rb1—O2^iii	117.03 (10)
O1—Rb1—Br1^ii	96.34 (5)	O3—Rb1—O2^iv	63.54 (9)
O1^ii—Rb1—Br1	94.89 (6)	O3—Rb1—O3^i	86.59 (10)
O1—Rb1—Br1	50.68 (5)	O3—Rb1—O3^v	150.63 (3)
O1^ii—Rb1—O1	83.18 (9)	O3^i—Rb1—O3^v	109.59 (3)
O1^ii—Rb1—O2^iii	133.19 (9)	O3—Rb1—C1	143.28 (9)
O1^ii—Rb1—O2^iv	80.42 (9)	O3^i—Rb1—C1	96.84 (9)
O1^ii—Rb1—O3^i	157.89 (8)	O3^v—Rb1—C1	61.22 (8)
O1^ii—Rb1—O3^v	78.36 (9)	O3—Rb1—H3A	19.5 (5)
O1—Rb1—O3^v	49.73 (8)	O3^i—Rb1—H3A	93 (4)
O1^ii—Rb1—C1	68.30 (10)	O3^v—Rb1—H3A	131.7 (11)
O1—Rb1—C1	19.62 (8)	C1—Rb1—Rb1^ii	118.54 (6)
O1^ii—Rb1—H3A	97 (4)	C1—Rb1—Rb1^i	61.46 (6)
O1—Rb1—H3A	178.6 (10)	C1—Rb1—Br1	44.29 (6)
O1—C1—Rb1	59.0 (2)	C1—Rb1—Br1^ii	77.21 (6)
O1—C1—C2^ix	117.1 (3)	C1—Rb1—H3A	160 (3)
O1—C1—C3	125.0 (4)	C1—O1—Rb1^i	140.9 (3)
O2^iii—Rb1—Rb1^i	47.95 (7)	C1—O1—Rb1	101.4 (3)
O2^iv—Rb1—Rb1^i	133.46 (7)	C1—C3—Br1	117.8 (3)
O2^iii—Rb1—Rb1^ii	132.05 (7)	C1—C3—C2	123.9 (4)
O2^iv—Rb1—Rb1^ii	46.54 (7)	C2—O2—Rb1^vi	138.9 (3)
O2^iii—Rb1—Br1^ii	168.33 (7)	C2—O2—Rb1^vii	124.1 (3)
O2^iv—Rb1—Br1^ii	105.78 (7)	C2^ix—C1—Rb1	118.9 (2)
O2^iii—Rb1—Br1	103.80 (7)	C2—C3—Br1	118.3 (3)
O2^iv—Rb1—Br1	170.27 (7)	C3—C1—Rb1	92.5 (2)
O2^iii—Rb1—O1	76.82 (8)	C3—C2—C1^ix	118.3 (3)
O2^iv—Rb1—O1	136.16 (8)	C3—C1—C2^ix	117.8 (3)
O2^iii—Rb1—O2^iv	85.50 (8)	H3A—O3—H3B	103 (4)
Rb1^ii—Rb1—Br1—Rb1^i	180	O1—C1—C3—Br1	−0.4 (6)
Rb1^i—Rb1—Br1—C3	−104.55 (13)	O1—C1—C3—C2	178.6 (4)
Rb1^ii—Rb1—Br1—C3	75.45 (13)	O2^iii—Rb1—Br1—Rb1^i	−2.61 (6)
Rb1^i—O1—Rb1—Rb1^ii	180	O2^iv—Rb1—Br1—Rb1^i	−165.2 (4)
Rb1^i—O1—Rb1—Br1^ii	−127.78 (5)	O2^iii—Rb1—Br1—C3	−107.16 (14)
Rb1^i—O1—Rb1—Br1	−77.94 (7)	O2^iv—Rb1—Br1—C3	90.3 (4)
Rb1^i—O1—Rb1—O1^ii	180	O3—Rb1—Br1—Rb1^i	−127.94 (9)
Rb1^i—O1—Rb1—O2^iii	42.61 (8)	O3^i—Rb1—Br1—Rb1^i	−51.74 (8)
Rb1^i—O1—Rb1—O2^iv	111.51 (11)	O3^v—Rb1—Br1—Rb1^i	55.10 (7)
Rb1^i—O1—Rb1—O3^i	−19.72 (8)	O3—Rb1—Br1—C3	127.52 (16)
Rb1^i—O1—Rb1—O3^v	99.50 (11)	O3^i—Rb1—Br1—C3	−156.28 (15)
Rb1^i—O1—Rb1—O3	−91.3 (3)	O3^v—Rb1—Br1—C3	−49.44 (15)
Rb1^i—O1—Rb1—C1	−140.7 (3)	C1—Rb1—Br1—Rb1^i	82.40 (8)
Rb1^i—O1—C1—Rb1	93.2 (4)	C1—Rb1—Br1—C3	−22.15 (16)
Rb1^i—O1—C1—C2^ix	−157.8 (3)	C1—O1—Rb1—Rb1^i	140.7 (3)
Rb1—O1—C1—C2^ix	109.0 (3)	C1—O1—Rb1—Rb1^ii	−39.3 (3)
Rb1^i—O1—C1—C3	24.2 (7)	C1—O1—Rb1—Br1^ii	12.9 (2)
Rb1—O1—C1—C3	−68.9 (4)	C1—O1—Rb1—Br1	62.7 (2)
Rb1^ii—O3—Rb1—Rb1^i	180	C1—O1—Rb1—O1^ii	−39.3 (3)
Rb1^viii—O3—Rb1—Rb1^i	35.47 (13)	C1—O1—Rb1—O2^iii	−176.7 (3)
Rb1^viii—O3—Rb1—Rb1^ii	−144.53 (13)	C1—O1—Rb1—O2^iv	−107.8 (2)
Rb1^ii—O3—Rb1—Br1^ii	−68.50 (6)	C1—O1—Rb1—O3^i	121.0 (3)
Rb1^viii—O3—Rb1—Br1^ii	146.96 (11)	C1—O1—Rb1—O3^v	−119.8 (3)
Rb1^ii—O3—Rb1—Br1	−119.27 (5)	C1—O1—Rb1—O3	49.3 (4)
Rb1^viii—O3—Rb1—Br1	96.20 (8)	C1^ix—C2—O2—Rb1^vi	−35.1 (6)
Rb1^ii—O3—Rb1—O1^ii	−22.05 (8)	C1^ix—C2—O2—Rb1^vii	94.1 (4)
Rb1^viii—O3—Rb1—O1^ii	−166.58 (10)	C1—C3—Br1—Rb1^i	−11.4 (3)
Rb1^ii—O3—Rb1—O1	−108.3 (3)	C1—C3—Br1—Rb1	50.9 (3)
Rb1^viii—O3—Rb1—O1	107.1 (3)	C1—C3—C2—O2	−179.8 (4)
Rb1^ii—O3—Rb1—O2^iii	123.54 (10)	C1—C3—C2—C1^ix	−0.6 (7)
Rb1^viii—O3—Rb1—O2^iii	−20.99 (14)	C2^ix—C1—Rb1—Rb1^i	−136.9 (3)
Rb1^ii—O3—Rb1—O2^iv	54.17 (9)	C2^ix—C1—Rb1—Rb1^ii	43.1 (3)
Rb1^viii—O3—Rb1—O2^iv	−90.36 (11)	C2^ix—C1—Rb1—Br1	154.0 (3)
Rb1^ii—O3—Rb1—O3^i	180	C2^ix—C1—Rb1—Br1^ii	87.1 (2)
Rb1^viii—O3—Rb1—O3^i	35.47 (13)	C2^ix—C1—Rb1—O1^ii	31.3 (2)
Rb1^ii—O3—Rb1—O3^v	54.63 (18)	C2^ix—C1—Rb1—O1	−106.0 (4)
Rb1^viii—O3—Rb1—O3^v	−89.9 (2)	C2^ix—C1—Rb1—O2^iii	−102.8 (3)
Rb1^ii—O3—Rb1—C1	−83.13 (16)	C2^ix—C1—Rb1—O2^iv	−12.3 (3)
Rb1^viii—O3—Rb1—C1	132.34 (13)	C2^ix—C1—Rb1—O3	100.9 (3)
Rb1—C1—C3—Br1	−53.6 (3)	C2^ix—C1—Rb1—O3^v	−57.0 (2)
Rb1—C1—C3—C2	125.4 (4)	C2^ix—C1—Rb1—O3^i	−165.6 (2)
Br1^ii—Rb1—Br1—Rb1^i	180	C2^ix—C1—C3—Br1	−178.3 (3)
Br1^ii—Rb1—Br1—C3	75.45 (13)	C2^ix—C1—C3—C2	0.6 (7)
Br1—C3—C2—O2	−0.9 (6)	C2—C3—Br1—Rb1^i	169.6 (3)
Br1—C3—C2—C1^ix	178.3 (3)	C2—C3—Br1—Rb1	−128.2 (3)
O1^ii—Rb1—Br1—Rb1^i	134.13 (7)	C3—C1—Rb1—Rb1^ii	−80.8 (2)
O1—Rb1—Br1—Rb1^i	57.09 (7)	C3—C1—Rb1—Rb1^i	99.2 (2)
O1—Rb1—Br1—C3	−47.46 (15)	C3—C1—Rb1—Br1	30.1 (2)
O1^ii—Rb1—Br1—C3	29.59 (15)	C3—C1—Rb1—Br1^ii	−36.8 (2)
O1—C1—Rb1—Rb1^i	−30.9 (2)	C3—C1—Rb1—O1^ii	−92.5 (3)
O1—C1—Rb1—Rb1^ii	149.1 (2)	C3—C1—Rb1—O1	130.1 (4)
O1—C1—Rb1—Br1^ii	−166.9 (2)	C3—C1—Rb1—O2^iii	133.3 (2)
O1—C1—Rb1—Br1	−100.0 (3)	C3—C1—Rb1—O2^iv	−136.2 (2)
O1—C1—Rb1—O1^ii	137.4 (3)	C3—C1—Rb1—O3	−23.0 (3)
O1—C1—Rb1—O2^iii	3.2 (3)	C3—C1—Rb1—O3^v	179.1 (3)
O1—C1—Rb1—O2^iv	93.7 (3)	C3—C1—Rb1—O3^i	70.5 (2)
O1—C1—Rb1—O3^i	−59.6 (3)	C3—C2—O2—Rb1^vi	144.1 (3)
O1—C1—Rb1—O3^v	49.0 (2)	C3—C2—O2—Rb1^vii	−86.7 (5)
O1—C1—Rb1—O3	−153.0 (2)

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

(RbHBAx3H2O)

Crystal data

C6H5Br2O6Rb·H2O	Dx = 2.557 Mg m^−3
Mr = 436.39	Cu Kα radiation, λ = 1.54179 Å
Tetragonal, P42/n	Cell parameters from 12733 reflections
a = 18.6351 (1) Å	θ = 2.4–76.0°
c = 6.528 (1) Å	µ = 14.50 mm^−1
V = 2266.96 (2) Å^3	T = 293 K
Z = 8	Prism, dark red
F(000) = 2100	0.23 × 0.20 × 0.09 mm

Data collection

Oxford Xcalibur Nova diffractometer	2330 independent reflections
Radiation source: Enhance (Cu) X-ray Source	2232 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
Detector resolution: 10.4323 pixels mm^-1	θmax = 76.1°, θmin = 3.4°
CCD detector, ω scans	h = −23→23
Absorption correction: multi-scan	k = −23→23
Tmin = 0.488, Tmax = 1	l = −7→7
20373 measured reflections

Refinement

Refinement on F^2	13 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.044	w = 1/[σ^2(Fo^2) + (0.0741P)^2 + 3.9255P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.136	(Δ/σ)max = 0.001
S = 1.21	Δρmax = 1.00 e Å^−3
2330 reflections	Δρmin = −0.95 e Å^−3
167 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Rb1	0.65825 (3)	0.50015 (2)	1.24068 (8)	0.0466 (2)
Br1	0.83118 (4)	0.40736 (3)	0.99888 (8)	0.0469 (2)
Br2	0.59254 (3)	0.66886 (4)	1.50009 (8)	0.0465 (2)
O1	0.6707 (2)	0.3701 (2)	1.0027 (5)	0.0383 (8)
O2	0.6031 (2)	0.2446 (2)	0.9987 (5)	0.0391 (9)
H2	0.5676	0.2858	0.9971	0.1*	0.5
O3	0.6302 (2)	0.8294 (2)	1.4983 (5)	0.0371 (8)
O4	0.7437 (2)	0.6039 (2)	1.5018 (5)	0.0375 (8)
H4	0.7852	0.5892	1.5027	0.056*	0.5
O5	0.5011 (2)	0.3566 (2)	1.0001 (6)	0.0435 (9)
H5A	0.473 (5)	0.381 (5)	0.904 (10)	0.13 (4)*
H5B	0.473 (5)	0.364 (6)	1.120 (9)	0.15 (5)*
O6	0.6507 (2)	0.49982 (15)	1.7463 (5)	0.0387 (9)
H6A	0.674 (4)	0.544 (2)	1.759 (4)	0.11 (4)*
H6B	0.681 (5)	0.461 (3)	1.760 (4)	0.22 (8)*
O7	0.4996 (4)	0.4991 (6)	1.269 (2)	0.136 (4)
H7A	0.532 (9)	0.528 (9)	1.34 (3)	0.25*
H7B	0.504 (10)	0.506 (11)	1.127 (6)	0.25*
C1	0.7099 (3)	0.3161 (3)	1.0005 (6)	0.0302 (10)
C3	0.7865 (3)	0.3179 (2)	0.9989 (6)	0.0283 (9)
C2	0.6731 (3)	0.2432 (3)	0.9992 (6)	0.0308 (10)
C4	0.6836 (2)	0.7902 (3)	1.5001 (5)	0.0278 (9)
C5	0.7437 (3)	0.6724 (3)	1.5015 (6)	0.0301 (9)
C6	0.6826 (2)	0.7136 (3)	1.5010 (6)	0.0274 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rb1	0.0594 (4)	0.0282 (3)	0.0520 (4)	0.0003 (2)	−0.0002 (2)	0.00028 (19)
Br1	0.0550 (4)	0.0325 (3)	0.0533 (4)	−0.0062 (2)	0.0020 (2)	0.00005 (19)
Br2	0.0320 (3)	0.0549 (4)	0.0525 (4)	−0.0076 (2)	−0.00126 (19)	−0.0016 (2)
O1	0.042 (2)	0.0280 (17)	0.045 (2)	0.0087 (14)	−0.0029 (13)	−0.0033 (12)
O2	0.0314 (17)	0.0378 (19)	0.048 (2)	0.0051 (15)	−0.0038 (12)	−0.0042 (13)
O3	0.0258 (16)	0.0394 (19)	0.046 (2)	0.0074 (14)	−0.0037 (12)	−0.0019 (13)
O4	0.0371 (19)	0.0292 (17)	0.046 (2)	0.0042 (14)	−0.0019 (13)	−0.0033 (12)
O5	0.0305 (18)	0.052 (2)	0.048 (2)	−0.0021 (17)	−0.0016 (13)	0.0047 (15)
O6	0.053 (2)	0.0133 (14)	0.050 (2)	−0.0007 (13)	0.0063 (15)	0.0005 (12)
O7	0.054 (4)	0.200 (11)	0.152 (9)	−0.001 (5)	0.010 (4)	0.003 (6)
C1	0.042 (3)	0.028 (2)	0.021 (2)	0.0095 (19)	−0.0025 (15)	−0.0018 (13)
C2	0.035 (2)	0.037 (2)	0.020 (2)	0.007 (2)	−0.0023 (14)	−0.0018 (15)
C3	0.036 (2)	0.025 (2)	0.024 (2)	−0.0029 (18)	−0.0001 (14)	−0.0004 (13)
C4	0.0216 (19)	0.039 (2)	0.022 (2)	0.0089 (18)	−0.0013 (13)	−0.0004 (14)
C5	0.031 (2)	0.035 (2)	0.023 (2)	0.0017 (19)	−0.0002 (14)	−0.0014 (15)
C6	0.0209 (19)	0.033 (2)	0.028 (2)	−0.0025 (17)	0.0001 (13)	−0.0014 (14)

Geometric parameters (Å, º)

Rb1—Br1	3.9833 (9)	O4—H4	0.82
Rb1—Br1^i	3.7749 (8)	O5—H5A	0.94 (2)
Rb1—Br2^ii	3.9768 (9)	O5—H5B	0.95 (2)
Rb1—O2^iii	3.022 (4)	O6—Rb1^viii	3.231 (4)
Rb1—O3^ii	2.892 (3)	O6—Rb1	3.303 (4)
Rb1—O6^iv	3.231 (4)	O6—H6B	0.92 (2)
Rb1—O7	2.963 (7)	O6—H6A	0.93 (2)
Rb1—H7B	2.96 (19)	O7—H7A	0.93 (19)
Rb1—H7A	2.50 (19)	O7—H7B	0.94 (2)
Br1—Rb1^v	3.7749 (8)	C1—C2	1.522 (7)
Br2—Rb1	3.7751 (8)	C1—C2	1.522 (7)
Br2—Rb1^vi	3.9768 (9)	C2—C3^ix	1.364 (7)
Br2—C6	1.875 (5)	C3—Br1	1.863 (5)
O1—Rb1	2.888 (4)	C3—C1	1.429 (7)
O1—C1	1.244 (6)	C3—C2^ix	1.364 (7)
O2—Rb1^vii	3.022 (4)	C4—O3	1.234 (6)
O2—C2	1.305 (6)	C4—C5^x	1.522 (7)
O2—H2	1.014 (4)	C4—C6	1.428 (7)
O3—Rb1^vi	2.892 (3)	C5—C4^x	1.522 (7)
O4—C5	1.277 (6)	C6—C5	1.373 (7)
Rb1^v—Br1—Rb1	172.91 (2)	O3^ii—Rb1—O7	96.9 (2)
Rb1—Br2—Rb1^vi	129.632 (15)	O3—C4—C5^x	116.5 (5)
Rb1^vii—O2—H2	88.9 (2)	O3—C4—C6	125.5 (5)
Rb1^viii—O6—Rb1	175.09 (14)	O4—C5—C4^x	117.3 (5)
Rb1^viii—O6—H6A	83.5 (17)	O4—C5—C6	123.9 (5)
Rb1—O6—H6A	94.1 (16)	O6^iv—Rb1—Br1	68.80 (7)
Rb1^viii—O6—H6B	82.8 (17)	O6—Rb1—Br1	115.43 (7)
Rb1—O6—H6B	94.4 (17)	O6^iv—Rb1—Br1^i	115.50 (5)
Rb1—O7—H7A	52 (10)	O6—Rb1—Br1^i	62.53 (5)
Rb1—O7—H7B	81 (10)	O6^iv—Rb1—Br2	115.83 (5)
Br1^i—Rb1—Br1	94.41 (2)	O6—Rb1—Br2	62.59 (5)
Br1^i—Rb1—Br2^ii	143.13 (2)	O6^iv—Rb1—Br2^ii	68.96 (7)
Br1^i—Rb1—Br2	112.912 (19)	O6—Rb1—Br2^ii	115.46 (7)
Br2—Rb1—Br1	143.29 (2)	O6^iv—Rb1—O6	175.09 (14)
Br2^ii—Rb1—Br1	51.382 (14)	O6^iv—Rb1—H7A	103 (3)
Br2—Rb1—Br2^ii	94.56 (2)	O6—Rb1—H7A	73 (3)
O1—Rb1—Br1	50.04 (8)	O6^iv—Rb1—H7B	73.0 (10)
O1—Rb1—Br1^i	64.29 (7)	O6—Rb1—H7B	102.1 (10)
O1—Rb1—Br2	165.06 (8)	O7—Rb1—Br1^i	69.1 (2)
O1—Rb1—Br2^ii	94.92 (8)	O7—Rb1—Br1	146.0 (2)
O1—Rb1—O2^iii	73.90 (10)	O7—Rb1—Br2^ii	146.8 (2)
O1—Rb1—O3^ii	114.00 (10)	O7—Rb1—Br2	69.7 (2)
O1—Rb1—O6^iv	57.62 (8)	O7—Rb1—O2^iii	119.5 (2)
O1—Rb1—O6	122.64 (8)	O7—Rb1—O6^iv	91.1 (3)
O1—Rb1—O7	96.2 (3)	O7—Rb1—O6	84.0 (3)
O1—Rb1—H7A	113 (2)	O7—Rb1—H7A	17.1 (18)
O1—Rb1—H7B	89 (4)	O7—Rb1—H7B	18.3 (8)
O1—C1—C2	117.3 (5)	C1—O1—Rb1	137.1 (3)
O1—C1—C3	124.6 (5)	C1—C3—Br1	117.9 (4)
O2^iii—Rb1—Br1^i	52.59 (7)	C2—O2—Rb1^vii	128.8 (3)
O2^iii—Rb1—Br1	60.89 (7)	C2—O2—H2	132.0 (4)
O2^iii—Rb1—Br2	116.95 (7)	C2^ix—C3—Br1	120.0 (4)
O2^iii—Rb1—Br2^ii	93.70 (7)	C2^ix—C3—C1	122.1 (4)
O2^iii—Rb1—O6^iv	125.36 (9)	C3—Br1—Rb1^v	94.75 (15)
O2^iii—Rb1—O6	57.62 (9)	C3—Br1—Rb1	91.55 (15)
O2^iii—Rb1—H7B	133 (3)	C3^ix—C2—C1	119.8 (5)
O2^iii—Rb1—H7A	119 (4)	C3—C1—C2	118.1 (4)
O2—C2—C1	115.5 (5)	C4—O3—Rb1^vi	136.7 (3)
O2—C2—C3^ix	124.6 (5)	C4—C6—Br2	117.2 (3)
O3^ii—Rb1—Br1^i	165.00 (8)	C5—O4—H4	109.5
O3^ii—Rb1—Br1	94.90 (8)	C5—C6—Br2	119.6 (4)
O3^ii—Rb1—O2^iii	142.37 (11)	C5—C6—C4	123.2 (4)
O3^ii—Rb1—O6^iv	57.73 (8)	C6—Br2—Rb1	94.67 (14)
O3^ii—Rb1—H7A	92 (4)	C6—Br2—Rb1^vi	91.64 (15)
O3^ii—Rb1—H7B	85 (3)	C6—C4—C5^x	118.0 (4)
O3^ii—Rb1—Br2	64.52 (7)	C6—C5—C4^x	118.8 (5)
O3^ii—Rb1—Br2^ii	50.15 (8)	H5A—O5—H5B	100 (5)
O3^ii—Rb1—O6	122.95 (8)	H6B—O6—H6A	114 (6)
O3^ii—Rb1—O6	122.95 (8)	H7B—O7—H7A	110 (6)
Rb1^vi—Br2—Rb1—Br1^i	−130.82 (2)	O3—C4—C6—Br2	−0.1 (5)
Rb1^vi—Br2—Rb1—Br1	94.23 (3)	O3—C4—C6—C5	179.5 (4)
Rb1^vi—Br2—Rb1—Br2^ii	74.36 (2)	O6^iv—Rb1—Br1—Rb1^v	63.33 (19)
Rb1^vi—Br2—Rb1—O1	−54.9 (3)	O6—Rb1—Br1—Rb1^v	−119.40 (19)
Rb1^vi—Br2—Rb1—O2^iii	170.86 (8)	O6^iv—Rb1—Br1—C3	−89.32 (14)
Rb1^vi—Br2—Rb1—O3^ii	32.97 (8)	O6—Rb1—Br1—C3	87.95 (14)
Rb1^vi—Br2—Rb1—O6^iv	5.56 (8)	O7—Rb1—Br1—Rb1^v	120.8 (5)
Rb1^vi—Br2—Rb1—O6	−169.24 (8)	O7—Rb1—Br1—C3	−31.9 (4)
Rb1^vi—Br2—Rb1—O7	−75.5 (3)	C1—O1—Rb1—Br1^i	−74.7 (5)
Rb1—Br2—C6—C4	152.9 (3)	C1—O1—Rb1—Br1	46.3 (5)
Rb1^vi—Br2—C6—C4	22.9 (3)	C1—O1—Rb1—Br2	−157.3 (4)
Rb1—Br2—C6—C5	−26.8 (3)	C1—O1—Rb1—Br2^ii	73.5 (5)
Rb1^vi—Br2—C6—C5	−156.8 (3)	C1—O1—Rb1—O2^iii	−18.9 (5)
Rb1—O1—C1—C2	129.0 (4)	C1—O1—Rb1—O3^ii	121.8 (5)
Rb1—O1—C1—C3	−51.1 (6)	C1—O1—Rb1—O6^iv	134.8 (5)
Rb1^vii—O2—C2—C1	134.8 (3)	C1—O1—Rb1—O6	−51.1 (5)
Rb1^vii—O2—C2—C3^ix	−45.4 (6)	C1—O1—Rb1—O7	−137.9 (5)
Rb1^viii—O6—Rb1—Br1^i	112.6 (12)	C1—C3—Br1—Rb1^v	−153.9 (3)
Rb1^viii—O6—Rb1—Br1	31.3 (12)	C1—C3—Br1—Rb1	22.9 (3)
Rb1^viii—O6—Rb1—Br2	−107.6 (11)	C2^ix—C3—C1—O1	179.2 (4)
Rb1^viii—O6—Rb1—Br2^ii	−26.1 (12)	C2^ix—C3—C1—C2	−1.0 (5)
Rb1^viii—O6—Rb1—O1	88.6 (11)	C2^ix—C3—Br1—Rb1^v	26.7 (3)
Rb1^viii—O6—Rb1—O2^iii	51.3 (11)	C2^ix—C3—Br1—Rb1	−156.6 (3)
Rb1^viii—O6—Rb1—O3^ii	−83.6 (12)	C3—C1—C2—O2	−179.4 (3)
Rb1^viii—O6—Rb1—O6^iv	180.000 (4)	C3—C1—C2—C3^ix	0.8 (5)
Rb1^viii—O6—Rb1—O7	−177.9 (12)	C4—C6—C5—O4	−179.8 (4)
Br1^i—Rb1—Br1—Rb1^v	179.00 (17)	C4—C6—C5—C4^x	−0.2 (5)
Br1^i—Rb1—Br1—C3	26.35 (13)	C5^x—C4—O3—Rb1^vi	129.1 (4)
Br1—C3—C1—O1	−0.3 (5)	C5^x—C4—C6—Br2	179.8 (2)
Br1—C3—C1—C2	179.6 (3)	C5^x—C4—C6—C5	−0.5 (5)
Br2—Rb1—Br1—Rb1^v	−41.8 (2)	C6—Br2—Rb1—Br1	−1.79 (13)
Br2^ii—Rb1—Br1—Rb1^v	−16.13 (18)	C6—Br2—Rb1—Br1^i	133.16 (12)
Br2—Rb1—Br1—C3	165.52 (13)	C6—Br2—Rb1—Br2^ii	−21.66 (12)
Br2^ii—Rb1—Br1—C3	−168.78 (13)	C6—Br2—Rb1—O1	−150.9 (3)
Br2—C6—C5—O4	−0.2 (5)	C6—Br2—Rb1—O2^iii	74.83 (15)
Br2—C6—C5—C4^x	179.4 (2)	C6—Br2—Rb1—O3^ii	−63.06 (15)
O1—Rb1—Br1—Rb1^v	128.2 (2)	C6—Br2—Rb1—O6	94.73 (14)
O1—Rb1—Br1—C3	−24.43 (15)	C6—Br2—Rb1—O7	−171.5 (3)
O1—C1—C2—O2	0.5 (5)	C6—Br2—Rb1—O6^iv	−90.47 (14)
O1—C1—C2—C3^ix	−179.3 (4)	C6—C4—O3—Rb1^vi	−51.0 (6)
O2^iii—Rb1—Br1—Rb1^v	−138.8 (2)	PLAT113_ALERT_2_A—PROBLEM:—ADDSYM—Suggests	Possible
O2^iii—Rb1—Br1—C3	68.58 (14)	Hydrogen—bromanilate—anions—are	disordered,
O3^ii—Rb1—Br1—Rb1^v	10.8 (2)	hydrogen—atom—bound—to	every
O3^ii—Rb1—Br1—C3	−141.87 (14)

Symmetry codes: (i) −y+1, x−1/2, z+1/2; (ii) −y+3/2, x, −z+5/2; (iii) y+1/2, −x+1, z+1/2; (iv) x, y, z−1; (v) y+1/2, −x+1, z−1/2; (vi) y, −x+3/2, −z+5/2; (vii) −y+1, x−1/2, z−1/2; (viii) x, y, z+1; (ix) −x+3/2, −y+1/2, z; (x) −x+3/2, −y+3/2, z.

(CsHBAx3H2O)

Crystal data

C6H5Br2CsO6·H2O	Dx = 2.684 Mg m^−3
Mr = 483.83	Cu Kα radiation, λ = 1.54179 Å
Tetragonal, P42/n	Cell parameters from 4266 reflections
a = 18.9442 (1) Å	θ = 2.3–76.1°
c = 6.6730 (1) Å	µ = 32.16 mm^−1
V = 2394.82 (4) Å^3	T = 293 K
Z = 8	Prism, dark red
F(000) = 2688	0.15 × 0.06 × 0.03 mm

Data collection

Oxford Xcalibur Nova diffractometer	2425 independent reflections
Radiation source: Enhance (Cu) X-ray Source	2129 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.028
Detector resolution: 10.4323 pixels mm^-1	θmax = 76.3°, θmin = 3.3°
CCD detector, ω scans	h = −19→22
Absorption correction: multi-scan	k = −22→23
Tmin = 0.207, Tmax = 1	l = −7→7
6509 measured reflections

Refinement

Refinement on F^2	19 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.046	w = 1/[σ^2(Fo^2) + (0.0816P)^2 + 4.2315P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.139	(Δ/σ)max = 0.001
S = 1.15	Δρmax = 1.42 e Å^−3
2425 reflections	Δρmin = −0.94 e Å^−3
161 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cs1	0.65188 (3)	0.50018 (2)	1.23457 (8)	0.0499 (2)
Br1	0.82631 (5)	0.40696 (4)	0.99677 (14)	0.0563 (3)
Br2	0.59297 (4)	0.67379 (5)	1.50255 (14)	0.0564 (3)
O1	0.6693 (3)	0.3654 (3)	0.9923 (8)	0.0491 (13)
O2	0.6044 (3)	0.2429 (3)	0.9996 (8)	0.0515 (14)
H2	0.5676	0.2858	0.9971	0.1*	0.5
O3	0.6343 (3)	0.8311 (3)	1.5052 (8)	0.0471 (13)
O4	0.7409 (3)	0.6067 (3)	1.5049 (8)	0.0487 (13)
H4	0.7814	0.5913	1.5057	0.073*	0.5
O5	0.5016 (3)	0.3544 (3)	0.9989 (8)	0.0498 (14)
H5A	0.492 (6)	0.4032 (17)	1.006 (19)	0.11 (5)*
H5B	0.458 (3)	0.332 (5)	0.972 (17)	0.08 (4)*
O6	0.6533 (3)	0.5000 (3)	1.7414 (9)	0.0522 (17)
H6A	0.687 (6)	0.537 (6)	1.738 (4)	0.22 (11)*
H6B	0.680 (6)	0.458 (4)	1.738 (4)	0.09 (4)*
O7	0.4898 (9)	0.5023 (10)	1.266 (3)	0.194 (8)
H7A	0.447	0.4957	1.2007	0.3*
H7B	0.4923	0.4663	1.3648	0.3*
C1	0.7091 (4)	0.3137 (4)	0.9937 (10)	0.0398 (15)
C2	0.6738 (4)	0.2422 (4)	0.9963 (10)	0.0406 (15)
C3	0.7844 (4)	0.3178 (4)	0.9961 (10)	0.0381 (15)
C4	0.6855 (4)	0.7908 (4)	1.5047 (9)	0.0378 (15)
C6	0.6822 (3)	0.7161 (4)	1.5046 (10)	0.0381 (14)
C5	0.7424 (4)	0.6739 (4)	1.5059 (10)	0.0403 (15)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cs1	0.0656 (4)	0.0320 (3)	0.0520 (4)	0.00045 (17)	0.0016 (2)	0.00063 (17)
Br1	0.0620 (5)	0.0382 (4)	0.0688 (7)	−0.0042 (3)	0.0067 (4)	−0.0013 (3)
Br2	0.0370 (4)	0.0627 (5)	0.0695 (7)	−0.0052 (3)	−0.0034 (3)	−0.0067 (4)
O1	0.051 (3)	0.035 (2)	0.062 (4)	0.010 (2)	−0.006 (2)	−0.006 (2)
O2	0.046 (3)	0.048 (3)	0.061 (4)	0.005 (2)	−0.006 (2)	−0.005 (2)
O3	0.030 (2)	0.046 (3)	0.065 (4)	0.008 (2)	−0.007 (2)	−0.003 (2)
O4	0.046 (3)	0.041 (3)	0.060 (4)	0.004 (2)	−0.002 (2)	−0.006 (2)
O5	0.034 (2)	0.070 (4)	0.045 (3)	−0.005 (2)	−0.004 (2)	0.007 (2)
O6	0.064 (4)	0.033 (3)	0.059 (4)	0.001 (2)	0.002 (2)	0.000 (2)
O7	0.194 (8)	0.195 (8)	0.194 (8)	0.0000 (12)	0.0004 (12)	0.0005 (12)
C1	0.051 (4)	0.035 (3)	0.034 (4)	0.007 (3)	−0.001 (3)	−0.004 (2)
C2	0.052 (4)	0.035 (3)	0.035 (4)	0.010 (3)	−0.005 (3)	−0.003 (3)
C3	0.047 (4)	0.030 (3)	0.038 (4)	0.004 (3)	0.004 (3)	0.000 (2)
C4	0.031 (3)	0.049 (4)	0.034 (4)	0.005 (3)	−0.003 (2)	0.000 (3)
C6	0.029 (3)	0.044 (3)	0.042 (4)	0.002 (3)	−0.002 (2)	−0.001 (3)
C5	0.036 (3)	0.049 (4)	0.036 (4)	0.006 (3)	−0.001 (2)	−0.004 (3)

Geometric parameters (Å, º)

Cs1—Br1^i	3.8926 (10)	O5—H5B	0.94 (2)
Cs1—O2^ii	3.167 (6)	O6—Cs1^viii	3.291 (6)
Cs1—O3^iii	3.021 (5)	O6—Cs1	3.382 (6)
Cs1—O6^iv	3.291 (6)	O6—H6B	0.95 (2)
Cs1—O7	3.077 (17)	O6—H6A	0.95 (2)
Cs1—H7B	3.2100 (5)	O7—H7B	0.952 (16)
Br1—Cs1^v	3.8926 (10)	O7—H7A	0.928 (15)
Br2—Cs1	3.9064 (11)	C1—C2	1.511 (11)
Br2—C6	1.871 (7)	C2—C3^ix	1.385 (10)
O1—Cs1	3.039 (5)	C3—Br1	1.866 (7)
O1—C1	1.236 (9)	C3—C1	1.429 (11)
O2—Cs1^vi	3.167 (6)	C3—C2^ix	1.385 (10)
O2—C2	1.315 (10)	C4—O3	1.233 (9)
O2—H2	1.071 (5)	C4—C5^x	1.520 (10)
O3—Cs1^vii	3.021 (5)	C4—C6	1.418 (11)
O4—C5	1.275 (10)	C5—C4^x	1.520 (10)
O4—H4	0.82	C6—C5	1.392 (10)
O5—H5A	0.94 (2)
Cs1^v—Br1—Cs1	170.66 (3)	O3^iii—Cs1—O7	97.5 (3)
Cs1—Br2—Cs1^vii	129.04 (2)	O3^iii—Cs1—H7B	114.36 (11)
Cs1^vi—O2—H2	89.8 (3)	O3—C4—C6	125.7 (7)
Cs1^viii—O6—Cs1	179.1 (2)	O3—C4—C5^x	115.8 (7)
Cs1^viii—O6—H6B	91.5 (16)	O4—C5—C4^x	117.3 (6)
Cs1—O6—H6B	89.1 (16)	O4—C5—C6	123.7 (7)
Cs1^viii—O6—H6A	91.5 (17)	O6^iv—Cs1—Br1^i	116.82 (10)
Cs1—O6—H6A	89.0 (16)	O6—Cs1—Br1^i	63.39 (9)
Cs1—O7—H7B	89.3 (10)	O6^iv—Cs1—Br1	66.60 (11)
Cs1—O7—H7A	147.0 (16)	O6—Cs1—Br1	112.52 (11)
Br1^i—Cs1—Br1	92.33 (2)	O6^iv—Cs1—Br2	117.44 (9)
Br1^i—Cs1—Br2	115.14 (2)	O6—Cs1—Br2	62.95 (9)
Br1^i—Cs1—Br2^iii	140.72 (2)	O6^iv—Cs1—Br2^iii	66.68 (11)
Br1^i—Cs1—H7B	55.897 (14)	O6—Cs1—Br2^iii	112.54 (11)
Br1—Cs1—H7B	141.580 (18)	O6^iv—Cs1—O6	179.1 (2)
Br2—Cs1—Br1	140.89 (2)	O6^iv—Cs1—H7B	106.17 (11)
Br2^iii—Cs1—Br1	51.362 (18)	O6—Cs1—H7B	74.73 (11)
Br2—Cs1—Br2^iii	92.65 (3)	O7—Cs1—Br1^i	72.2 (3)
Br2—Cs1—H7B	77.028 (16)	O7—Cs1—Br1	147.4 (4)
Br2^iii—Cs1—H7B	163.262 (19)	O7—Cs1—Br2	70.9 (4)
O1—Cs1—Br1^i	63.86 (11)	O7—Cs1—Br2^iii	146.3 (3)
O1—Cs1—Br1	48.70 (11)	O7—Cs1—O2^ii	120.9 (3)
O1—Cs1—Br2	168.98 (11)	O7—Cs1—O6^iv	94.3 (4)
O1—Cs1—Br2^iii	93.90 (12)	O7—Cs1—O6	86.6 (4)
O1—Cs1—O2^ii	73.29 (15)	O7—Cs1—H7B	17.2 (3)
O1—Cs1—O6^iv	57.76 (14)	C1—O1—Cs1	136.7 (5)
O1—Cs1—O6	122.02 (14)	C1—C3—Br1	118.3 (5)
O1—Cs1—O7	98.9 (4)	C2—O2—Cs1^vi	127.6 (4)
O1—C1—C3	124.5 (7)	C2—O2—H2	131.3 (6)
O1—C1—C2	116.2 (7)	C2^ix—C3—Br1	120.0 (6)
O1—Cs1—H7B	94.48 (11)	C2^ix—C3—C1	121.7 (6)
O2^ii—Cs1—Br1^i	51.36 (9)	C3—Br1—Cs1^v	95.7 (2)
O2^ii—Cs1—Br1	60.25 (10)	C3—Br1—Cs1	92.8 (2)
O2^ii—Cs1—Br2	115.26 (10)	C3—C1—C2	119.3 (6)
O2^ii—Cs1—Br2^iii	92.60 (10)	C3^ix—C2—C1	119.0 (7)
O2^ii—Cs1—O6^iv	123.60 (14)	C4—O3—Cs1^vii	136.6 (5)
O2^ii—Cs1—O6	55.71 (14)	C4—C6—Br2	117.9 (5)
O2—C2—C1	115.6 (6)	C5—C6—C4	122.5 (6)
O2—C2—C3^ix	125.5 (7)	C5—C6—Br2	119.7 (6)
O2^ii—Cs1—H7B	103.68 (10)	C5—O4—H4	109.5
O3^iii—Cs1—Br1^i	168.72 (10)	C6—Br2—Cs1	96.1 (2)
O3^iii—Cs1—Br1	94.12 (11)	C6—Br2—Cs1^vii	92.6 (2)
O3^iii—Cs1—Br2	64.18 (11)	C6—C4—C5^x	118.6 (6)
O3^iii—Cs1—Br2^iii	48.90 (11)	C6—C5—C4^x	119.0 (7)
O3^iii—Cs1—O1	114.42 (15)	H5A—O5—H5B	107 (5)
O3^iii—Cs1—O2^ii	139.82 (14)	H6B—O6—H6A	105 (5)
O3^iii—Cs1—O6^iv	58.01 (14)	H7B—O7—H7A	105.8 (16)
O3^iii—Cs1—O6	121.97 (14)
Cs1^vii—Br2—Cs1—Br1^i	−132.11 (3)	O3—C4—C6—Br2	0.6 (9)
Cs1^vii—Br2—Cs1—Br1	97.47 (4)	O3—C4—C6—C5	−179.4 (7)
Cs1^vii—Br2—Cs1—Br2^iii	76.52 (3)	O6^iv—Cs1—Br1—Cs1^v	64.1 (2)
Cs1^vii—Br2—Cs1—O1	−49.9 (6)	O6—Cs1—Br1—Cs1^v	−115.5 (2)
Cs1^vii—Br2—Cs1—O2^ii	170.65 (11)	O6^iv—Cs1—Br1—C3	−91.2 (2)
Cs1^vii—Br2—Cs1—O3^iii	35.41 (12)	O6—Cs1—Br1—C3	89.2 (2)
Cs1^vii—Br2—Cs1—O6^iv	11.52 (13)	O7—Cs1—Br1—Cs1^v	122.6 (6)
Cs1^vii—Br2—Cs1—O6	−169.45 (13)	O7—Cs1—Br1—C3	−32.7 (6)
Cs1^vii—Br2—Cs1—O7	−73.4 (3)	C1—O1—Cs1—Br1	46.3 (7)
Cs1—Br2—C6—C4	152.5 (5)	C1—O1—Cs1—Br1^i	−73.1 (7)
Cs1^vii—Br2—C6—C4	22.7 (5)	C1—O1—Cs1—Br2	−160.6 (6)
Cs1—Br2—C6—C5	−27.5 (6)	C1—O1—Cs1—Br2^iii	73.1 (7)
Cs1^vii—Br2—C6—C5	−157.3 (5)	C1—O1—Cs1—O2^ii	−18.5 (7)
Cs1—O1—C1—C2	127.9 (6)	C1—O1—Cs1—O3^iii	119.2 (7)
Cs1—O1—C1—C3	−51.1 (11)	C1—O1—Cs1—O6^iv	132.3 (8)
Cs1^vi—O2—C2—C1	133.9 (5)	C1—O1—Cs1—O6	−46.7 (8)
Cs1^vi—O2—C2—C3^ix	−46.5 (9)	C1—O1—Cs1—O7	−138.2 (8)
Cs1^viii—O6—Cs1—Br1^i	−77 (11)	C1—C3—Br1—Cs1^v	−152.5 (5)
Cs1^viii—O6—Cs1—Br1	−158 (11)	C1—C3—Br1—Cs1	23.6 (5)
Cs1^viii—O6—Cs1—Br2	65 (11)	C2^ix—C3—Br1—Cs1^v	27.0 (6)
Cs1^viii—O6—Cs1—Br2^iii	146 (11)	C2^ix—C3—Br1—Cs1	−156.9 (5)
Cs1^viii—O6—Cs1—O1	−103 (11)	C2^ix—C3—C1—O1	−179.6 (6)
Cs1^viii—O6—Cs1—O2^ii	−137 (11)	C2^ix—C3—C1—C2	1.4 (9)
Cs1^viii—O6—Cs1—O3^iii	92 (11)	C3—C1—C2—O2	178.2 (6)
Cs1^viii—O6—Cs1—O6^iv	180.00 (19)	C3—C1—C2—C3^ix	−1.5 (8)
Cs1^viii—O6—Cs1—O7	−5 (11)	C4—C6—C5—O4	−179.6 (6)
Br1^i—Cs1—Br1—Cs1^v	−177.54 (17)	C4—C6—C5—C4^x	−0.8 (9)
Br1^i—Cs1—Br1—C3	27.1 (2)	C5^x—C4—O3—Cs1^vii	129.8 (6)
Br1—C3—C1—O1	−0.1 (10)	C5^x—C4—C6—Br2	−179.9 (5)
Br1—C3—C1—C2	−179.1 (5)	C5^x—C4—C6—C5	0.1 (9)
Br2—Cs1—Br1—Cs1^v	−41.1 (2)	C6—Br2—Cs1—Br1^i	129.5 (2)
Br2^iii—Cs1—Br1—Cs1^v	−13.94 (18)	C6—Br2—Cs1—Br1	−0.9 (2)
Br2—Cs1—Br1—C3	163.5 (2)	C6—Br2—Cs1—Br2^iii	−21.8 (2)
Br2^iii—Cs1—Br1—C3	−169.3 (2)	C6—Br2—Cs1—O1	−148.3 (6)
Br2—C6—C5—O4	0.4 (10)	C6—Br2—Cs1—O2^ii	72.3 (2)
Br2—C6—C5—C4^x	179.2 (5)	C6—Br2—Cs1—O3^iii	−63.0 (2)
O1—Cs1—Br1—Cs1^v	131.0 (2)	C6—Br2—Cs1—O6^iv	−86.8 (2)
O1—Cs1—Br1—C3	−24.4 (3)	C6—Br2—Cs1—O6	92.2 (2)
O1—C1—C2—O2	−0.9 (9)	C6—Br2—Cs1—O7	−171.7 (4)
O1—C1—C2—C3^ix	179.4 (6)	C6—C4—O3—Cs1^vii	−50.7 (10)
O2^ii—Cs1—Br1—Cs1^v	−135.5 (2)	PLAT113_ALERT_2_A—PROBLEM:—ADDSYM—Suggests	Possible
O2^ii—Cs1—Br1—C3	69.1 (2)	Hydrogen—bromanilate—anions—are	disordered,
O3^iii—Cs1—Br1—Cs1^v	11.7 (2)	hydrogen—atom—bound—to	every
O3^iii—Cs1—Br1—C3	−143.6 (2)

Symmetry codes: (i) −y+1, x−1/2, z+1/2; (ii) y+1/2, −x+1, z+1/2; (iii) −y+3/2, x, −z+5/2; (iv) x, y, z−1; (v) y+1/2, −x+1, z−1/2; (vi) −y+1, x−1/2, z−1/2; (vii) y, −x+3/2, −z+5/2; (viii) x, y, z+1; (ix) −x+3/2, −y+1/2, z; (x) −x+3/2, −y+3/2, z.

(Na2BAx4H2O)

Crystal data

C6H8Br2Na2O8	Z = 2
Mr = 413.90	F(000) = 414
Triclinic, P1	Dx = 2.268 Mg m^−3
a = 8.0223 (6) Å	Cu Kα radiation, λ = 1.54179 Å
b = 8.6764 (6) Å	Cell parameters from 2696 reflections
c = 9.9131 (6) Å	θ = 5.1–75.9°
α = 108.113 (6)°	µ = 9.52 mm^−1
β = 110.543 (6)°	T = 293 K
γ = 91.991 (6)°	Prism, red
V = 606.03 (7) Å^3	0.25 × 0.05 × 0.05 mm

Data collection

Oxford Xcalibur Nova diffractometer	2459 independent reflections
Radiation source: Enhance (Cu) X-ray Source	1989 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 10.4323 pixels mm^-1	θmax = 76.1°, θmin = 5.1°
CCD detector, ω scans	h = −10→9
Absorption correction: multi-scan	k = −10→10
Tmin = 0.194, Tmax = 1	l = −12→10
4617 measured reflections

Refinement

Refinement on F^2	All H-atom parameters refined
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0531P)^2 + 0.0514P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.030	(Δ/σ)max = 0.001
wR(F^2) = 0.094	Δρmax = 0.58 e Å^−3
S = 1.03	Δρmin = −0.51 e Å^−3
2459 reflections	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
196 parameters	Extinction coefficient: 0.0021 (4)
15 restraints

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Na1	0.79693 (16)	0.53269 (14)	0.68730 (13)	0.0328 (3)
Na2	0.63882 (17)	0.65270 (15)	1.00292 (13)	0.0362 (3)
Br1	0.73381 (5)	1.03516 (4)	0.17219 (3)	0.03785 (15)
Br2	0.75597 (5)	0.96537 (4)	0.82555 (3)	0.03585 (15)
O1	0.7498 (3)	0.7022 (2)	0.5312 (3)	0.0380 (5)
O2	0.7467 (4)	0.7311 (3)	0.2714 (3)	0.0403 (6)
O3	0.7387 (3)	1.2968 (2)	0.4649 (2)	0.0331 (5)
O4	0.7663 (3)	1.2728 (2)	0.7332 (2)	0.0342 (5)
O5	1.0990 (3)	0.5507 (3)	0.7037 (3)	0.0363 (5)
H5A	1.134 (6)	0.611 (4)	0.654 (4)	0.063 (13)*
H5B	1.129 (6)	0.448 (3)	0.671 (5)	0.076 (15)*
O6	0.9278 (3)	0.6716 (3)	0.9812 (3)	0.0424 (5)
H6A	1.009 (8)	0.664 (7)	1.073 (5)	0.17 (3)*
H6B	0.973 (8)	0.775 (4)	0.985 (7)	0.13 (2)*
O7	0.6512 (3)	0.3758 (3)	0.9931 (3)	0.0376 (5)
H7A	0.678 (5)	0.313 (4)	0.914 (3)	0.065 (13)*
H7B	0.749 (5)	0.391 (6)	1.084 (3)	0.10 (2)*
O8	0.5214 (3)	0.5664 (3)	0.7288 (2)	0.0341 (5)
H8A	0.463 (6)	0.644 (4)	0.690 (5)	0.11 (2)*
H8B	0.442 (5)	0.468 (3)	0.684 (5)	0.073 (15)*
C1	0.7520 (4)	0.8425 (3)	0.5243 (3)	0.0247 (5)
C2	0.7488 (4)	0.8580 (3)	0.3728 (3)	0.0269 (6)
C3	0.7457 (4)	1.0143 (3)	0.3599 (3)	0.0267 (6)
C4	0.7463 (4)	1.1570 (3)	0.4757 (3)	0.0237 (5)
C5	0.7564 (4)	1.1434 (3)	0.6297 (3)	0.0234 (5)
C6	0.7534 (4)	0.9867 (3)	0.6399 (3)	0.0249 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.0393 (6)	0.0305 (6)	0.0338 (6)	0.0103 (5)	0.0180 (5)	0.0129 (5)
Na2	0.0401 (7)	0.0385 (6)	0.0314 (6)	0.0050 (5)	0.0176 (5)	0.0095 (5)
Br1	0.0658 (3)	0.0304 (2)	0.0243 (2)	0.00988 (16)	0.02289 (17)	0.01193 (15)
Br2	0.0574 (3)	0.0312 (2)	0.0253 (2)	0.00569 (15)	0.01992 (16)	0.01355 (15)
O1	0.0648 (15)	0.0193 (10)	0.0336 (11)	0.0110 (9)	0.0201 (11)	0.0122 (9)
O2	0.0712 (16)	0.0230 (11)	0.0285 (11)	0.0171 (10)	0.0216 (11)	0.0074 (9)
O3	0.0555 (13)	0.0193 (9)	0.0278 (10)	0.0102 (9)	0.0176 (10)	0.0101 (8)
O4	0.0590 (14)	0.0221 (10)	0.0259 (10)	0.0117 (9)	0.0206 (10)	0.0083 (8)
O5	0.0386 (12)	0.0337 (11)	0.0414 (12)	0.0093 (9)	0.0183 (10)	0.0154 (10)
O6	0.0374 (12)	0.0468 (14)	0.0386 (12)	0.0057 (10)	0.0131 (10)	0.0107 (10)
O7	0.0388 (12)	0.0394 (12)	0.0367 (11)	0.0116 (10)	0.0194 (10)	0.0098 (10)
O8	0.0338 (11)	0.0298 (10)	0.0340 (11)	0.0045 (9)	0.0076 (9)	0.0110 (9)
C1	0.0328 (13)	0.0212 (12)	0.0201 (12)	0.0073 (10)	0.0100 (10)	0.0071 (10)
C2	0.0362 (14)	0.0217 (13)	0.0236 (13)	0.0071 (11)	0.0120 (11)	0.0079 (11)
C3	0.0410 (15)	0.0240 (13)	0.0188 (12)	0.0084 (11)	0.0135 (11)	0.0094 (11)
C4	0.0330 (13)	0.0194 (12)	0.0201 (12)	0.0067 (10)	0.0111 (10)	0.0073 (10)
C5	0.0298 (13)	0.0220 (12)	0.0192 (12)	0.0075 (10)	0.0093 (10)	0.0078 (10)
C6	0.0355 (14)	0.0235 (13)	0.0191 (12)	0.0054 (10)	0.0123 (10)	0.0095 (10)

Geometric parameters (Å, º)

Na1—O3^i	2.382 (2)	O1—C1	1.240 (4)
Na1—O4^i	2.456 (2)	O2—Na2^iv	2.348 (2)
Na1—O5	2.368 (3)	O2—C2	1.233 (3)
Na1—O6	2.574 (3)	O3—Na1^v	2.382 (2)
Na1—O8	2.397 (3)	O3—C4	1.252 (3)
Na2—Na2^ii	3.375 (2)	O4—Na1^v	2.456 (2)
Na2—Br1^iii	3.1421 (12)	O4—C5	1.241 (3)
Na2—O2^iii	2.348 (2)	O5—H5A	0.921 (19)
Na2—O6	2.407 (3)	O5—H5B	0.918 (18)
Na2—O7^ii	2.347 (3)	O6—H6A	0.94 (2)
Na2—O7	2.381 (3)	O6—H6B	0.935 (19)
Na2—O8	2.392 (2)	O7—Na2^ii	2.347 (3)
Br1—Na2^iv	3.1421 (12)	O7—H7A	0.908 (18)
Br1—C3	1.895 (3)	O7—H7B	0.929 (19)
Br2—C6	1.899 (3)	O8—H8A	0.938 (14)
O1—Na1	2.396 (2)	O8—H8B	0.928 (14)
Na1—O5—H5A	118 (3)	O5—Na1—O1	87.19 (9)
Na1—O5—H5B	111 (3)	O5—Na1—O3^i	85.15 (9)
Na1—O6—H6A	144 (4)	O5—Na1—O4^i	99.54 (9)
Na1—O6—H6B	98 (4)	O5—Na1—O6	86.63 (9)
Na1—O8—H8A	112 (3)	O5—Na1—O8	166.31 (9)
Na1—O8—H8B	111 (3)	O6—Na1—Na2	41.10 (6)
Na2^ii—Na2—Na1	113.25 (5)	O6—Na2—Na1	44.68 (6)
Na2—O6—Na1	94.22 (9)	O6—Na2—Na2^ii	134.12 (9)
Na2—O6—H6A	104 (4)	O6—Na2—Br1^iii	86.15 (7)
Na2—O6—H6B	115 (4)	O7^ii—Na2—Na1	131.62 (7)
Na2^ii—O7—Na2	91.10 (9)	O7—Na2—Na1	84.54 (7)
Na2^ii—O7—H7A	122 (3)	O7^ii—Na2—Na2^ii	44.85 (6)
Na2—O7—H7A	113 (3)	O7—Na2—Na2^ii	44.05 (6)
Na2^ii—O7—H7B	118 (3)	O7^ii—Na2—Br1^iii	96.27 (7)
Na2—O7—H7B	101 (3)	O7—Na2—Br1^iii	153.36 (8)
Na2—O8—Na1	99.36 (8)	O7^ii—Na2—O2^iii	86.43 (10)
Na2—O8—H8A	114 (3)	O7^ii—Na2—O6	176.27 (10)
Na2—O8—H8B	112 (3)	O7—Na2—O6	90.18 (9)
Br1^iii—Na2—Na1	110.39 (4)	O7^ii—Na2—O7	88.90 (9)
Br1^iii—Na2—Na2^ii	134.95 (6)	O7^ii—Na2—O8	92.10 (9)
O1—Na1—Na2	116.87 (7)	O7—Na2—O8	90.95 (9)
O1—Na1—O4^i	154.48 (9)	O8—Na2—Na1	40.38 (6)
O1—Na1—O6	118.74 (9)	O8—Na1—Na2	40.26 (6)
O1—Na1—O8	94.47 (9)	O8—Na1—O4^i	84.78 (8)
O1—C1—C2	116.3 (2)	O8—Na1—O6	80.66 (8)
O1—C1—C6	126.2 (3)	O8—Na2—Na2^ii	92.13 (7)
O2^iii—Na2—Na1	140.84 (8)	O8—Na2—Br1^iii	114.85 (7)
O2^iii—Na2—Na2^ii	86.02 (8)	O8—Na2—O6	84.30 (9)
O2^iii—Na2—Br1^iii	66.49 (6)	C1—O1—Na1	148.1 (2)
O2^iii—Na2—O6	97.15 (10)	C1—C6—Br2	117.0 (2)
O2^iii—Na2—O7	87.88 (9)	C2—O2—Na2^iv	132.6 (2)
O2^iii—Na2—O8	178.14 (10)	C2—C3—Br1	118.3 (2)
O2—C2—C3	125.1 (3)	C3—Br1—Na2^iv	92.02 (9)
O2—C2—C1	117.3 (3)	C3—C2—C1	117.6 (2)
O3^i—Na1—Na2	136.17 (7)	C3—C4—C5	118.2 (2)
O3^i—Na1—O1	89.47 (8)	C4—O3—Na1^v	120.30 (18)
O3^i—Na1—O4^i	66.84 (8)	C4—C3—Br1	117.2 (2)
O3^i—Na1—O6	150.14 (9)	C4—C3—C2	124.4 (3)
O3^i—Na1—O8	108.43 (9)	C5—O4—Na1^v	118.02 (19)
O3—C4—C3	125.3 (3)	C5—C6—Br2	117.8 (2)
O3—C4—C5	116.4 (2)	C5—C6—C1	125.2 (3)
O4^i—Na1—Na2	78.31 (6)	C6—C1—C2	117.5 (2)
O4^i—Na1—O6	86.38 (9)	C6—C5—C4	117.0 (2)
O4—C5—C4	117.1 (2)	H5A—O5—H5B	107 (3)
O4—C5—C6	125.9 (3)	H6B—O6—H6A	102 (3)
O5—Na1—Na2	127.62 (7)	H7B—O7—H7A	108 (3)
O5—Na1—O1	87.19 (9)	H8A—O8—H8B	108 (3)
Na1—Na2—O7—Na2^ii	−132.00 (8)	O4—C5—C6—C1	−176.4 (3)
Na1—O1—C1—C6	−17.3 (6)	O5—Na1—O6—Na2	−176.13 (10)
Na1—O1—C1—C2	164.1 (3)	O5—Na1—O8—Na2	−31.1 (4)
Na1^v—O3—C4—C3	−168.4 (2)	O6—Na1—O8—Na2	−9.11 (9)
Na1^v—O3—C4—C5	11.9 (3)	O6—Na2—Na1—O1	−103.84 (12)
Na1^v—O4—C5—C4	−5.6 (3)	O6—Na2—Na1—O3^i	135.30 (14)
Na1^v—O4—C5—C6	174.5 (2)	O6—Na2—Na1—O4^i	97.99 (11)
Na2^ii—Na2—Na1—O1	126.13 (9)	O6—Na2—Na1—O5	4.88 (12)
Na2^ii—Na2—Na1—O3^i	5.28 (13)	O6—Na2—Na1—O8	−166.25 (13)
Na2^ii—Na2—Na1—O4^i	−32.03 (8)	O6—Na2—O7—Na2^ii	−176.39 (10)
Na2^ii—Na2—Na1—O5	−125.15 (9)	O6—Na2—O8—Na1	9.67 (9)
Na2^ii—Na2—Na1—O6	−130.02 (12)	O7^ii—Na2—Na1—O1	76.70 (13)
Na2^ii—Na2—Na1—O8	63.73 (10)	O7—Na2—Na1—O1	160.35 (10)
Na2^ii—Na2—O6—Na1	78.54 (13)	O7^ii—Na2—Na1—O3^i	−44.15 (15)
Na2^ii—Na2—O8—Na1	−124.47 (8)	O7—Na2—Na1—O3^i	39.49 (12)
Na2^iv—Br1—C3—C2	12.5 (2)	O7^ii—Na2—Na1—O4^i	−81.46 (12)
Na2^iv—Br1—C3—C4	−166.0 (2)	O7—Na2—Na1—O4^i	2.18 (9)
Na2^iv—O2—C2—C1	153.8 (2)	O7^ii—Na2—Na1—O5	−174.58 (12)
Na2^iv—O2—C2—C3	−25.2 (5)	O7—Na2—Na1—O5	−90.93 (10)
Br1^iii—Na2—Na1—O1	−42.38 (9)	O7^ii—Na2—Na1—O6	−179.45 (14)
Br1^iii—Na2—Na1—O3^i	−163.23 (9)	O7—Na2—Na1—O6	−95.81 (11)
Br1^iii—Na2—Na1—O4^i	159.46 (7)	O7^ii—Na2—Na1—O8	14.30 (12)
Br1^iii—Na2—Na1—O5	66.35 (9)	O7—Na2—Na1—O8	97.94 (11)
Br1^iii—Na2—Na1—O6	61.47 (10)	O7^ii—Na2—O6—Na1	6.3 (17)
Br1^iii—Na2—Na1—O8	−104.78 (9)	O7—Na2—O6—Na1	82.04 (9)
Br1^iii—Na2—O6—Na1	−124.37 (7)	O7^ii—Na2—O7—Na2^ii	0
Br1^iii—Na2—O7—Na2^ii	101.84 (16)	O7^ii—Na2—O8—Na1	−169.35 (9)
Br1^iii—Na2—O8—Na1	92.75 (8)	O7—Na2—O8—Na1	−80.42 (9)
Br1—C3—C2—C1	−178.00 (19)	O8—Na1—O6—Na2	8.96 (8)
Br1—C3—C2—O2	1.0 (4)	O8—Na2—Na1—O1	62.41 (11)
Br2—C6—C1—O1	1.1 (4)	O8—Na2—Na1—O3^i	−58.45 (13)
Br2—C6—C1—C2	179.63 (19)	O8—Na2—Na1—O4^i	−95.76 (11)
O1—C1—C2—O2	−1.0 (4)	O8—Na2—Na1—O5	171.13 (13)
O1—C1—C2—C3	178.1 (3)	O8—Na2—Na1—O6	166.25 (13)
O1—Na1—O6—Na2	98.94 (11)	O8—Na2—O6—Na1	−8.90 (8)
O1—Na1—O8—Na2	−127.54 (9)	O8—Na2—O7—Na2^ii	−92.08 (9)
O2^iii—Na2—Na1—O1	−119.80 (13)	C1—O1—Na1—O5	−90.1 (4)
O2^iii—Na2—Na1—O5	−11.08 (15)	C1—O1—Na1—O3^i	−175.3 (4)
O2^iii—Na2—Na1—O3^i	119.35 (14)	C1—O1—Na1—O8	76.3 (4)
O2^iii—Na2—Na1—O4^i	82.03 (13)	C1—O1—Na1—O4^i	163.5 (4)
O2^iii—Na2—Na1—O6	−15.96 (14)	C1—O1—Na1—O6	−5.5 (5)
O2^iii—Na2—Na1—O8	177.79 (15)	C1—O1—Na1—Na2	41.2 (5)
O2^iii—Na2—O6—Na1	169.92 (9)	C4—C3—C2—O2	179.3 (3)
O2^iii—Na2—O7—Na2^ii	86.47 (10)	C4—C3—C2—C1	0.4 (5)
O2^iii—Na2—O8—Na1	−132 (3)	C4—C5—C6—Br2	−177.53 (18)
O3^i—Na1—O6—Na2	−101.96 (19)	C4—C5—C6—C1	3.7 (4)
O3^i—Na1—O8—Na2	141.53 (9)	C5—C4—C3—Br1	−179.83 (19)
O3—C4—C3—Br1	0.4 (4)	C5—C4—C3—C2	1.8 (5)
O3—C4—C3—C2	−178.0 (3)	C6—C1—C2—O2	−179.7 (3)
O4^i—Na1—O6—Na2	−76.34 (10)	C6—C1—C2—C3	−0.6 (4)
O4^i—Na1—O8—Na2	78.07 (9)	C5—C6—C1—O1	179.8 (3)
O4—C5—C4—O3	−3.9 (4)	C5—C6—C1—C2	−1.6 (4)
O4—C5—C4—C3	176.4 (3)	C6—C5—C4—O3	176.0 (3)
O4—C5—C6—Br2	2.4 (4)	C6—C5—C4—C3	−3.7 (4)

Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+1, −z+2; (iii) x, y, z+1; (iv) x, y, z−1; (v) x, y+1, z.