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The title compound, poly­[[rubidium-μ-5-sulfonosalicylic acid] monohydrate], Rb+·C7H5O6S·H2O, the 5-sulfosalicylic acid anion (3-carboxy-4-hydroxy­benzene­sulfonate) has lost the proton of —SO3H group, but retains the usual intermolecular hydrogen bond between the phenolic and carboxyl­ic O atoms. The Rb+ cation is surrounded by eight O atoms. The crystal packing is stabilized by intermolecular O—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031290/br6173sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031290/br6173Isup2.hkl
Contains datablock I

CCDC reference: 262225

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.045
  • wR factor = 0.141
  • Data-to-parameter ratio = 11.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O7 - H2 ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.03 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT416_ALERT_2_C Short Intra D-H..H-D H2 .. H5 .. 1.92 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.67 Ratio
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
Rb+·C7H5O6S·H2OF(000) = 632
Mr = 320.66Dx = 2.099 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2007 reflections
a = 11.779 (11) Åθ = 3.3–27.7°
b = 7.363 (7) ŵ = 5.10 mm1
c = 12.025 (11) ÅT = 273 K
β = 103.359 (12)°Block, colourless
V = 1014.7 (16) Å30.45 × 0.39 × 0.12 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
1764 independent reflections
Radiation source: fine-focus sealed tube1438 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
φ and ω scansθmax = 25.0°, θmin = 3.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 148
Tmin = 0.116, Tmax = 0.542k = 88
4884 measured reflectionsl = 1314
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.141H atoms treated by a mixture of independent and constrained refinement
S = 0.98 w = 1/[σ2(Fo2) + (0.0973P)2 + 3.1685P]
where P = (Fo2 + 2Fc2)/3
1766 reflections(Δ/σ)max = 0.001
153 parametersΔρmax = 1.07 e Å3
3 restraintsΔρmin = 0.53 e Å3
Special details top

Experimental. The chemical composition was determined by C, H, N element analysis and Rb+ by Tas-986 atomic absorption spectrometric at a wavelength of 852.1 nm.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Rb10.90569 (5)0.57370 (8)0.74921 (5)0.0355 (3)
O10.1637 (3)0.9417 (5)0.5299 (3)0.0240 (9)
O20.9503 (3)0.3030 (5)0.5771 (3)0.0295 (9)
O30.0676 (4)0.7243 (5)0.6283 (3)0.0291 (9)
O40.6582 (3)0.5444 (5)0.6836 (3)0.0278 (9)
O50.5799 (3)0.8174 (5)0.6388 (3)0.0245 (8)
H50.64830.84890.65880.037*
O60.5239 (4)0.2584 (5)0.6404 (3)0.0272 (9)
H60.58600.31350.65770.041*
O70.8036 (4)0.9442 (6)0.6824 (4)0.0322 (10)
S10.12198 (11)0.75430 (17)0.53187 (10)0.0171 (3)
C10.5727 (5)0.6395 (7)0.6491 (4)0.0190 (11)
C20.4526 (4)0.5676 (7)0.6152 (4)0.0166 (11)
C30.4356 (5)0.3775 (7)0.6134 (4)0.0192 (11)
C40.3222 (5)0.3075 (7)0.5815 (4)0.0212 (11)
H40.31070.18250.57840.025*
C50.2282 (5)0.4219 (7)0.5549 (4)0.0207 (11)
H5A0.15290.37480.53460.025*
C60.2460 (4)0.6126 (7)0.5585 (4)0.0166 (10)
C70.3566 (4)0.6821 (7)0.5878 (4)0.0176 (11)
H70.36760.80720.58930.021*
H10.814 (6)0.959 (9)0.616 (3)0.05 (2)*
H20.767 (6)1.030 (7)0.705 (5)0.04 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0330 (4)0.0361 (4)0.0383 (4)0.0030 (2)0.0098 (3)0.0022 (2)
O10.025 (2)0.0163 (18)0.033 (2)0.0066 (15)0.0101 (17)0.0016 (14)
O20.026 (2)0.034 (2)0.024 (2)0.0027 (18)0.0040 (16)0.0061 (17)
O30.033 (2)0.029 (2)0.034 (2)0.0025 (17)0.0256 (18)0.0013 (17)
O40.019 (2)0.035 (2)0.029 (2)0.0019 (17)0.0034 (16)0.0007 (17)
O50.0201 (19)0.026 (2)0.028 (2)0.0101 (16)0.0060 (16)0.0034 (16)
O60.029 (2)0.023 (2)0.028 (2)0.0059 (17)0.0044 (17)0.0050 (16)
O70.039 (3)0.035 (2)0.027 (2)0.012 (2)0.0140 (19)0.0006 (18)
S10.0165 (6)0.0188 (6)0.0174 (6)0.0031 (5)0.0065 (5)0.0011 (5)
C10.021 (3)0.025 (3)0.012 (2)0.002 (2)0.006 (2)0.002 (2)
C20.019 (3)0.021 (3)0.011 (2)0.005 (2)0.005 (2)0.0019 (18)
C30.026 (3)0.021 (2)0.011 (2)0.001 (2)0.005 (2)0.0005 (19)
C40.034 (3)0.015 (2)0.016 (3)0.006 (2)0.009 (2)0.0008 (19)
C50.022 (3)0.023 (3)0.018 (3)0.008 (2)0.007 (2)0.000 (2)
C60.020 (3)0.018 (2)0.013 (2)0.000 (2)0.005 (2)0.0018 (19)
C70.020 (3)0.018 (2)0.016 (2)0.005 (2)0.007 (2)0.0025 (19)
Geometric parameters (Å, º) top
Rb1—O42.847 (5)O5—H50.8200
Rb1—O3i2.875 (4)O6—C31.342 (7)
Rb1—O2ii2.907 (4)O6—H60.8200
Rb1—O3iii2.945 (5)O7—Rb1ii3.466 (5)
Rb1—O23.005 (4)O7—H10.84 (6)
Rb1—O73.014 (5)O7—H20.85 (6)
Rb1—O1iii3.110 (5)S1—O2v1.451 (4)
Rb1—O7iv3.466 (5)S1—C61.763 (5)
Rb1—S1iii3.601 (3)S1—Rb1vii3.601 (3)
Rb1—C5v3.633 (6)S1—Rb1ix3.956 (3)
Rb1—S1vi3.956 (3)C1—C21.477 (7)
Rb1—Rb1ii4.298 (3)C2—C71.387 (7)
O1—S11.466 (4)C2—C31.413 (7)
O1—Rb1vii3.110 (5)C3—C41.400 (8)
O2—S1v1.451 (4)C4—C51.370 (8)
O2—Rb1iv2.907 (4)C4—H40.9300
O3—S11.465 (4)C5—C61.419 (7)
O3—Rb1viii2.875 (4)C5—Rb1v3.633 (6)
O3—Rb1vii2.945 (4)C5—H5A0.9300
O4—C11.218 (7)C6—C71.368 (7)
O5—C11.320 (7)C7—H70.9300
O4—Rb1—O3i130.23 (13)H1—O7—H2114 (4)
O4—Rb1—O2ii129.29 (12)O2v—S1—O3113.5 (3)
O3i—Rb1—O2ii78.11 (13)O2v—S1—O1112.8 (2)
O4—Rb1—O3iii93.24 (12)O3—S1—O1111.4 (2)
O3i—Rb1—O3iii125.69 (9)O2v—S1—C6106.3 (2)
O2ii—Rb1—O3iii99.84 (13)O3—S1—C6105.2 (2)
O4—Rb1—O295.15 (11)O1—S1—C6107.0 (2)
O3i—Rb1—O270.47 (13)O4—C1—O5122.5 (5)
O2ii—Rb1—O2135.55 (7)O4—C1—C2123.5 (5)
O3iii—Rb1—O275.49 (13)O5—C1—C2114.1 (4)
O4—Rb1—O771.01 (12)C7—C2—C3119.6 (5)
O3i—Rb1—O777.69 (13)C7—C2—C1121.6 (4)
O2ii—Rb1—O778.26 (12)C3—C2—C1118.8 (5)
O3iii—Rb1—O7156.01 (11)O6—C3—C4117.5 (5)
O2—Rb1—O7122.63 (12)O6—C3—C2123.0 (5)
O4—Rb1—O1iii76.03 (11)C4—C3—C2119.5 (5)
O3i—Rb1—O1iii152.69 (11)C5—C4—C3120.4 (5)
O2ii—Rb1—O1iii78.05 (12)C5—C4—H4119.8
O3iii—Rb1—O1iii47.03 (10)C3—C4—H4119.8
O2—Rb1—O1iii120.19 (12)C4—C5—C6119.7 (5)
O7—Rb1—O1iii110.06 (11)C4—C5—Rb1v112.3 (3)
O4—Rb1—O7iv159.61 (11)C6—C5—Rb1v92.8 (3)
O3i—Rb1—O7iv59.43 (12)C4—C5—H5A120.2
O2ii—Rb1—O7iv66.97 (11)C6—C5—H5A120.2
O3iii—Rb1—O7iv69.85 (11)Rb1v—C5—H5A64.7
O2—Rb1—O7iv70.16 (10)C7—C6—C5120.2 (5)
O7—Rb1—O7iv128.60 (11)C6—C7—C2120.6 (5)
O1iii—Rb1—O7iv98.72 (11)C6—C7—H7119.7
C1—O5—H5109.5C2—C7—H7119.7
C3—O6—H6109.5
O4—C1—C2—C35.4 (7)
Symmetry codes: (i) x+1, y, z; (ii) x+2, y+1/2, z+3/2; (iii) x+1, y1/2, z+3/2; (iv) x+2, y1/2, z+3/2; (v) x+1, y+1, z+1; (vi) x+1, y+3/2, z+1/2; (vii) x+1, y+1/2, z+3/2; (viii) x1, y, z; (ix) x1, y+3/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O70.821.922.729 (6)171
O6—H6···O40.821.892.613 (6)146
O7—H1···O1x0.84 (4)1.97 (4)2.797 (8)166 (1)
Symmetry code: (x) x+1, y+2, z+1.
 

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