The Ba atom in the title compound, poly[[diaquabarium(II)]-μ6-1,5-naphthalenedisulfonato], [Ba(C10H6S2O6)(H2O)2]n, lies on a special position of site symmetry 2 and the dianion on an inversion centre. The Ba atom interacts with the O atoms of six different dianionic groups in the three-dimensional network and exhibits a square antiprismatic coordination.
Supporting information
CCDC reference: 269804
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.027
- wR factor = 0.065
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.245 0.530
Tmin' and Tmax expected: 0.282 0.530
RR' = 0.866
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.81
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H2# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.98(4), Rep 1.980(10) ...... 4.00 su-Rat
H2# -O2 1.555 2.656
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
poly[[diaquabarium(II)]-µ
6-1,5-naphthalenedisulfonato]
top
Crystal data top
[Ba(C10H6S2O6)(H2O)2] | F(000) = 888 |
Mr = 459.64 | Dx = 2.299 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6301 reflections |
a = 22.274 (4) Å | θ = 3.7–27.5° |
b = 5.715 (1) Å | µ = 3.34 mm−1 |
c = 10.443 (2) Å | T = 295 K |
β = 92.56 (3)° | Prism, colourless |
V = 1328.0 (4) Å3 | 0.37 × 0.24 × 0.19 mm |
Z = 4 | |
Data collection top
Rigaki R-AXIS RAPID IP diffractometer | 1525 independent reflections |
Radiation source: fine-focus sealed tube | 1495 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
ω scan | θmax = 27.5°, θmin = 3.7° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −28→28 |
Tmin = 0.245, Tmax = 0.530 | k = −7→7 |
6313 measured reflections | l = −13→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.065 | w = 1/[σ2(Fo2) + (0.0372P)2 + 1.6623P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.001 |
1525 reflections | Δρmax = 0.72 e Å−3 |
103 parameters | Δρmin = −1.38 e Å−3 |
3 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0071 (6) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ba1 | 0.5000 | 0.84452 (3) | 0.7500 | 0.0167 (1) | |
S1 | 0.59787 (3) | 0.6843 (1) | 0.44019 (6) | 0.0160 (2) | |
O1w | 0.4506 (1) | 1.1768 (3) | 0.8992 (3) | 0.0392 (6) | |
O1 | 0.5807 (1) | 0.6643 (3) | 0.5735 (2) | 0.0226 (4) | |
O2 | 0.5904 (1) | 0.9231 (3) | 0.3917 (2) | 0.0230 (4) | |
O3 | 0.5687 (1) | 0.5113 (3) | 0.3573 (2) | 0.0255 (4) | |
C1 | 0.6762 (1) | 0.6263 (4) | 0.4385 (2) | 0.0159 (5) | |
C2 | 0.6946 (1) | 0.4413 (4) | 0.3665 (2) | 0.0205 (5) | |
C3 | 0.7560 (1) | 0.3975 (4) | 0.3562 (3) | 0.0226 (5) | |
C4 | 0.7983 (1) | 0.5361 (4) | 0.4155 (2) | 0.0206 (5) | |
C5 | 0.7812 (1) | 0.7266 (4) | 0.4939 (2) | 0.0154 (4) | |
H1w1 | 0.436 (2) | 1.312 (4) | 0.885 (4) | 0.059* | |
H1w2 | 0.438 (2) | 1.122 (7) | 0.968 (3) | 0.059* | |
H2 | 0.6663 | 0.3450 | 0.3247 | 0.025* | |
H3 | 0.7681 | 0.2710 | 0.3076 | 0.027* | |
H4 | 0.8388 | 0.5063 | 0.4048 | 0.025* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ba1 | 0.0132 (2) | 0.0144 (2) | 0.0223 (2) | 0.000 | 0.0006 (1) | 0.000 |
S1 | 0.0141 (3) | 0.0146 (3) | 0.0191 (3) | −0.0012 (2) | −0.0003 (2) | −0.0013 (2) |
O1w | 0.048 (2) | 0.020 (1) | 0.052 (2) | 0.003 (1) | 0.026 (1) | 0.001 (1) |
O1 | 0.023 (1) | 0.022 (1) | 0.023 (1) | 0.000 (1) | 0.007 (1) | 0.000 (1) |
O2 | 0.023 (1) | 0.018 (1) | 0.028 (1) | 0.001 (1) | −0.003 (1) | 0.004 (1) |
O3 | 0.017 (1) | 0.025 (1) | 0.035 (1) | −0.004 (1) | −0.003 (1) | −0.010 (1) |
C1 | 0.014 (1) | 0.015 (1) | 0.019 (1) | 0.000 (1) | 0.000 (1) | 0.001 (1) |
C2 | 0.021 (1) | 0.018 (1) | 0.023 (1) | −0.002 (1) | 0.000 (1) | −0.006 (1) |
C3 | 0.025 (1) | 0.018 (1) | 0.025 (1) | 0.004 (1) | 0.002 (1) | −0.008 (1) |
C4 | 0.017 (1) | 0.020 (1) | 0.026 (1) | 0.005 (1) | −0.001 (1) | −0.004 (1) |
C5 | 0.016 (1) | 0.016 (1) | 0.015 (1) | 0.001 (1) | 0.002 (1) | 0.000 (1) |
Geometric parameters (Å, º) top
Ba1—O1 | 2.826 (2) | C1—C2 | 1.371 (3) |
Ba1—O1i | 2.826 (2) | C1—C5vi | 1.430 (3) |
Ba1—O2ii | 2.783 (2) | C2—C3 | 1.399 (3) |
Ba1—O2iii | 2.783 (2) | C3—C4 | 1.358 (4) |
Ba1—O3iv | 2.753 (2) | C4—C5 | 1.424 (3) |
Ba1—O3v | 2.752 (2) | C5—C5vi | 1.427 (4) |
Ba1—O1w | 2.720 (2) | C5—C1vi | 1.430 (3) |
Ba1—O1wi | 2.720 (2) | O1w—H1w1 | 0.85 (1) |
S1—O3 | 1.449 (2) | O1w—H1w2 | 0.85 (1) |
S1—O2 | 1.463 (2) | C2—H2 | 0.93 |
S1—O1 | 1.465 (2) | C3—H3 | 0.93 |
S1—C1 | 1.776 (3) | C4—H4 | 0.93 |
| | | |
O1—Ba1—O1i | 137.3 (1) | O3—S1—O2 | 112.9 (1) |
O1—Ba1—O2iii | 93.1 (1) | O3—S1—O1 | 112.7 (1) |
O1—Ba1—O2ii | 107.1 (1) | O2—S1—O1 | 111.8 (1) |
O1—Ba1—O3iv | 79.8 (1) | O3—S1—C1 | 106.4 (1) |
O1—Ba1—O3v | 68.8 (1) | O2—S1—C1 | 105.5 (1) |
O1—Ba1—O1w | 156.0 (1) | O1—S1—C1 | 107.0 (1) |
O1—Ba1—O1wi | 66.1 (1) | S1—O1—Ba1 | 142.4 (1) |
O1i—Ba1—O1w | 66.1 (1) | S1—O2—Ba1ii | 134.2 (1) |
O1i—Ba1—O1wi | 156.0 (1) | S1—O3—Ba1iv | 166.8 (1) |
O1i—Ba1—O3iv | 68.8 (1) | C2—C1—C5vi | 121.0 (2) |
O1i—Ba1—O2ii | 93.1 (1) | C2—C1—S1 | 117.9 (2) |
O1i—Ba1—O2iii | 107.1 (1) | C5vi—C1—S1 | 121.1 (2) |
O1i—Ba1—O3v | 79.8 (1) | C1—C2—C3 | 119.8 (2) |
O2ii—Ba1—O2iii | 123.0 (1) | C4—C3—C2 | 121.4 (2) |
O2ii—Ba1—O3iv | 76.1 (1) | C3—C4—C5 | 120.7 (2) |
O2ii—Ba1—O3v | 160.9 (1) | C5vi—C5—C4 | 118.7 (3) |
O2ii—Ba1—O1wi | 70.4 (1) | C5vi—C5—C1vi | 118.3 (3) |
O2ii—Ba1—O1w | 70.7 (1) | C4—C5—C1vi | 123.0 (2) |
O2iii—Ba1—O3iv | 160.9 (1) | Ba1—O1w—H1w1 | 134 (3) |
O2iii—Ba1—O3v | 76.1 (1) | Ba1—O1w—H1w2 | 113 (3) |
O2iii—Ba1—O1w | 70.4 (1) | H1w1—O1w—H1w2 | 110 (2) |
O2iii—Ba1—O1wi | 70.7 (1) | C1—C2—H2 | 120.1 |
O3iv—Ba1—O3v | 84.7 (1) | C3—C2—H2 | 120.1 |
O3iv—Ba1—O1w | 121.2 (1) | C4—C3—H3 | 119.3 |
O3iv—Ba1—O1wi | 120.9 (1) | C2—C3—H3 | 119.3 |
O3v—Ba1—O1w | 120.9 (1) | C3—C4—H4 | 119.6 |
O3v—Ba1—O1wi | 121.2 (1) | C5—C4—H4 | 119.6 |
O1w—Ba1—O1wi | 91.5 (1) | | |
| | | |
O3—S1—O1—Ba1 | −95.2 (2) | O1—S1—O3—Ba1iv | 3.8 (6) |
O2—S1—O1—Ba1 | 33.2 (2) | C1—S1—O3—Ba1iv | 120.7 (5) |
C1—S1—O1—Ba1 | 148.2 (2) | O3—S1—C1—C2 | −0.7 (2) |
O1wi—Ba1—O1—S1 | −43.0 (2) | O2—S1—C1—C2 | −120.9 (2) |
O1w—Ba1—O1—S1 | −65.2 (3) | O1—S1—C1—C2 | 119.9 (2) |
O3iv—Ba1—O1—S1 | 87.6 (2) | O3—S1—C1—C5vi | 176.8 (2) |
O3v—Ba1—O1—S1 | 175.8 (2) | O2—S1—C1—C5vi | 56.7 (2) |
O2iii—Ba1—O1—S1 | −110.4 (2) | O1—S1—C1—C5vi | −62.5 (2) |
O2ii—Ba1—O1—S1 | 15.6 (2) | C5vi—C1—C2—C3 | −1.4 (4) |
O1i—Ba1—O1—S1 | 130.2 (2) | S1—C1—C2—C3 | 176.2 (2) |
O3—S1—O2—Ba1ii | 32.2 (2) | C1—C2—C3—C4 | −0.5 (4) |
O1—S1—O2—Ba1ii | −96.1 (2) | C2—C3—C4—C5 | 2.1 (4) |
C1—S1—O2—Ba1ii | 148.0 (1) | C3—C4—C5—C5vi | −1.8 (4) |
O2—S1—O3—Ba1iv | −124.1 (5) | C3—C4—C5—C1vi | 178.2 (2) |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1, −y+2, −z+1; (iii) x, −y+2, z+1/2; (iv) −x+1, −y+1, −z+1; (v) x, −y+1, z+1/2; (vi) −x+3/2, −y+3/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1vii | 0.85 (1) | 2.10 (2) | 2.889 (3) | 155 (5) |
O1w—H1w2···O2i | 0.85 (1) | 1.98 (1) | 2.808 (3) | 167 (4) |
Symmetry codes: (i) −x+1, y, −z+3/2; (vii) −x+1, y+1, −z+3/2. |