Buy article online - an online subscription or single-article purchase is required to access this article.
share
share
Issue contentsclose
Statistics
close
Download citation
closeDownload citation
Format BIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Text
Plain Text
Supporting information
Supporting informationclose
Download PDF of article
Download PDF of articleclose
Acta Cryst. (2005). E61, m1957-m1959
https://doi.org/10.1107/S1600536805028151
Download PDF of article
Download PDF of articleclose
Supporting information
Supporting informationclose
Download citation
closeDownload citation
Format BIBTeX
EndNote
RefMan
Refer
Medline
CIF
SGML
Text
Plain Text
Statistics
close
Issue contentsclose
share
link to html

Bis[hexa­aqua­cadmium(II)] 25,26,27,28-tetra­hydr­oxy-2,8,14,19-tetra­thia­calix[4]arene-5,11,17,23-tetra­sulfonate monohydrate clathrate

B.-T. Zhao, P.-Z. Hu, J.-G. Wang, L.-F. Ma, L.-Y. Wang and S. W. Ng
The title compound, [Cd(H2O)6]2(C24H2O16S8)·H2O, the bis­[hexa­aqua­cadmium(II)] salt of the p-sulfonatothia­calix[4]arene tetra­anion, crystallizes as a hydrate; two symmetry-independent cations inter­act with the tetra­anion via their coordinated water mol­ecules. The Cd atoms and water O atom lie on special positions of site symmetry m and the complete calixarene anion is generated by mirror symmetry. The water mol­ecule is weakly associated with the calixarene cavity by way of long O—H...O hydrogen bonds.
Read articleSimilar articles

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805028151/hb6262sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805028151/hb6262Isup2.hkl
Contains datablock I

CCDC reference: 287566

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.041
  • wR factor = 0.130
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found




Alert level B
PLAT731_ALERT_1_B Bond    Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O3W  -H3W2    1.555   1.555
PLAT731_ALERT_1_B Bond    Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O4W  -H4W1    1.555   1.555
PLAT731_ALERT_1_B Bond    Calc     0.86(6), Rep   0.850(10) ......       6.00 su-Rat
              O4W  -H4W2    1.555   1.555
PLAT731_ALERT_1_B Bond    Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O7W  -H7W1    1.555   1.555
PLAT731_ALERT_1_B Bond    Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O8W  -H8W2    1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O3W  -H4#     1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O4W  -H5#     1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.86(6), Rep   0.850(10) ......       6.00 su-Rat
              O4W  -H6#     1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O7W  -H9#     1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.85(5), Rep   0.850(10) ......       5.00 su-Rat
              O8W  -H12#    1.555   1.555
PLAT736_ALERT_1_B H...A   Calc     1.91(5), Rep   1.910(10) ......       5.00 su-Rat
              H4#  -O3      1.555   1.455
PLAT736_ALERT_1_B H...A   Calc     1.92(6), Rep   1.930(10) ......       6.00 su-Rat
              H6#  -O8      1.555   3.666
PLAT736_ALERT_1_B H...A   Calc     1.95(5), Rep   1.960(10) ......       5.00 su-Rat
              H12# -O6      1.555   3.766


Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.556     0.703
            Tmin(prime) and Tmax expected:      0.603     0.685
            RR(prime) =      0.897
            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 .............       0.88
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.97
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cd1
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cd2
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         13
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O1W  -H1W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.84(3), Rep   0.840(10) ......       3.00 su-Rat
              O2W  -H2W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H3W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O5W  -H5W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O6W  -H6W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O7W  -H7W2    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O8W  -H8W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.860(10) ......       3.00 su-Rat
              O9W  -H9W1    1.555   1.555
PLAT732_ALERT_1_C Angle   Calc      125(4), Rep   125.0(10) ......       4.00 su-Rat
              CD1  -O1W  -H1W1    1.555   1.555   1.555
PLAT732_ALERT_1_C Angle   Calc      109(6), Rep      109(2) ......       3.00 su-Rat
              H4W1 -O4W  -H4W2    1.555   1.555   1.555
PLAT732_ALERT_1_C Angle   Calc      125(4), Rep   125.0(10) ......       4.00 su-Rat
              CD2  -O5W  -H5W1    1.555   1.555   1.555
PLAT732_ALERT_1_C Angle   Calc      125(4), Rep   125.0(10) ......       4.00 su-Rat
              CD2  -O6W  -H6W1    1.555   1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O1W  -H1#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(3), Rep   0.840(10) ......       3.00 su-Rat
              O2W  -H2#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H3#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O5W  -H7#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O6W  -H8#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O7W  -H10#    1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O8W  -H11#    1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.860(10) ......       3.00 su-Rat
              O9W  -H13#    1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.92(3), Rep   1.920(10) ......       3.00 su-Rat
              H1#  -O6      1.555   3.666
PLAT736_ALERT_1_C H...A   Calc     1.97(4), Rep   1.970(10) ......       4.00 su-Rat
              H3#  -O8      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.91(5), Rep     1.91(2) ......       2.50 su-Rat
              H5#  -O4      1.555   3.766
PLAT736_ALERT_1_C H...A   Calc     1.97(3), Rep   1.980(10) ......       3.00 su-Rat
              H7#  -O4      1.555   3.766
PLAT736_ALERT_1_C H...A   Calc     1.94(3), Rep   1.940(10) ......       3.00 su-Rat
              H8#  -O3      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.93(4), Rep   1.930(10) ......       4.00 su-Rat
              H10# -O5      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.96(5), Rep     1.96(2) ......       2.50 su-Rat
              H9#  -O7      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.94(4), Rep   1.940(10) ......       4.00 su-Rat
              H11# -O5      1.555   3.766
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          4
              H2 O


   0 ALERT level A = In general: serious problem
  13 ALERT level B = Potentially serious problem
  37 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

  43 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
   5 ALERT type 4 Improvement, methodology, query or suggestion
Comment top

The p-sulfonatocalix[4]arene (see scheme) tetraanion adopts a bowl-shaped conformation with the negatively charged sulfonate groups at the upper rim and the neutral/deprotonated hydroxyl groups at the lower rim. As such, it is capable of forming inclusion compounds through π-stacking, hydrogen-bonding and coordinative interactions (Atwood et al., 2001). A manganese(II) derivative of this species has been described (Gao et al., 2003) in which the hexaaquamanganese cations interact with the anionic p-sulfonatocalix[4]arene indirectly, via their coordinated water molecules. The compound was formulated as [Mn(H2O)6]2(C24H2O16S8)·0.5H2O.

The present cadmium complex, (I) (Fig. 1), is essentially isostructural with the manganese analogue (same cell dimensions and space group), but was modelled as [Cd(H2O)6]2(C24H2O16S8)·H2O, i.e. with full occupancy of the non-coordinatd water molecule. The hexaaquacadmium(II) species possess typical geometrical parameters (Table 1).

An extensive network of O—H···O hydrogen bonds (Table 2) help to stabilize the crystal packing in (I). The non-coordinated water molecule (O9w) lies on a special position of site symmetry m; as it forms long hydrogen bonds [H···O = 2.44 (2) Å] to neighboring acceptor calixarene hydroxide O atoms, its displacement factor is relatively large.

Experimental top

Tetrasodium p-sulfonatocalix[4]arene (Gao et al., 2003; Iki et al., 1998) (0.18 g, 0.2 mmol) was dissolved in water (10 ml) and cadmium nitrate (0.08 g, 0.4 mmol) was added to the solution. The filtered solution was set aside for several days resulting in the growth of colourless plates of (I).

Refinement top

The C-bound H atoms were positioned geometrically (C—H = 0.93 Å) and were included in the refinement in the riding-model approximation, with Uiso(H) = 1.2Ueq(C). The water H atoms were located in difference maps and were refined with the distance restraints O—H = 0.85 (1) Å and H···H = 1.39 (1) Å, and with Uiso(H) = 1.2Ueq(O). The two hydroxy H atoms of the anion are disordered over two positions. Two H-atom sites (H11 and H12 attached to O1 and H21 and H22 attached to O2), each of 50% occupancy, were generated for each O atom in idealized positions (O—H = 0.85 Å) and refined as riding with Uiso(H) = 1.2Ueq(O). This arrangment for the two orientations of the hydroxy groups leads to the formation of either a clockwise or an anticlockwise ring of O—H···O hydrogen bonds (Fig. 2 and Table 2). The deepest difference hole is 0.65 Å from atom Cd1 and the highest difference peak is 2.77 Å from atom H8, in a possible solvent-accessible void. Attempts to refine the electron density as an O atom were unsuccessful.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; 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.

Figures top
[Figure 1] Fig. 1. View of (I), showing 50% displacement ellipsoids (arbitrary spheres for H atoms). [Symmetry codes: (i) x, 3/2 − y, z; (ii) x, 1/2 − y, z.]
[Figure 2] Fig. 2. Detail of (I), showing one possible `clockwise' cyclic arrangement of O—H···O hydrogen bonds within the calixarene moiety. As a result of the positional disorder of the hydroxy H atoms (not shown), the hydrogen bonds can also propagate in the reverse (anticlockwise) sense.
Bis[hexaaquacadmium(II)] 25,26,27,28-tetrahydroxy-2,8,14,19-tetrathiacalix[4]arene-5,11,17,23- tetrasulfonate monohydrate clathrate top
Crystal data top
[Cd(H2O)6]2(C24H2O16S8)·H2OF(000) = 1276
Mr = 1271.82Dx = 1.868 Mg m−3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 8025 reflections
a = 13.1183 (5) Åθ = 2.8–28.4°
b = 14.2581 (6) ŵ = 1.40 mm−1
c = 13.1854 (5) ÅT = 295 K
β = 113.563 (1)°Block, colorless
V = 2260.6 (2) Å30.35 × 0.33 × 0.27 mm
Z = 2
Data collection top
Bruker APEX2 area-detector
diffractometer		5380 independent reflections
Radiation source: fine-focus sealed tube5106 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ϕ and ω scansθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −17→17
Tmin = 0.556, Tmax = 0.703k = −18→18
19302 measured reflectionsl = −17→17
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.130H atoms treated by a mixture of independent and constrained refinement
S = 1.11 w = 1/[σ2(Fo2) + (0.0599P)2 + 6.3407P]
where P = (Fo2 + 2Fc2)/3
5380 reflections(Δ/σ)max = 0.001
337 parametersΔρmax = 1.76 e Å−3
22 restraintsΔρmin = −1.74 e Å−3
Crystal data top
[Cd(H2O)6]2(C24H2O16S8)·H2OV = 2260.6 (2) Å3
Mr = 1271.82Z = 2
Monoclinic, P21/mMo Kα radiation
a = 13.1183 (5) ŵ = 1.40 mm−1
b = 14.2581 (6) ÅT = 295 K
c = 13.1854 (5) Å0.35 × 0.33 × 0.27 mm
β = 113.563 (1)°
Data collection top
Bruker APEX2 area-detector
diffractometer		5380 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		5106 reflections with I > 2σ(I)
Tmin = 0.556, Tmax = 0.703Rint = 0.019
19302 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04122 restraints
wR(F2) = 0.130H atoms treated by a mixture of independent and constrained refinement
S = 1.11Δρmax = 1.76 e Å−3
5380 reflectionsΔρmin = −1.74 e Å−3
337 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd10.47481 (3)0.75000.44903 (4)0.0371 (1)
Cd20.99024 (3)0.75000.48290 (4)0.0402 (1)
S11.12673 (7)0.49239 (6)0.33671 (7)0.0298 (2)
S21.04713 (12)0.2500−0.0102 (1)0.0386 (3)
S30.73831 (7)0.52185 (8)−0.03325 (8)0.0408 (2)
S40.43955 (10)0.2500−0.0273 (1)0.0363 (3)
S50.62754 (7)0.48790 (6)0.32418 (7)0.03002 (19)
O10.8270 (2)0.3504 (3)−0.1018 (2)0.0509 (8)
O20.5892 (3)0.3531 (2)−0.1125 (2)0.0461 (7)
O31.1734 (2)0.5838 (2)0.3294 (3)0.0422 (6)
O41.2104 (2)0.4194 (2)0.3828 (2)0.0399 (6)
O51.0520 (2)0.4983 (2)0.3944 (2)0.0410 (6)
O60.7017 (2)0.4178 (2)0.3976 (2)0.0397 (6)
O70.6779 (2)0.5810 (2)0.3416 (3)0.0421 (6)
O80.5180 (2)0.4868 (2)0.3282 (3)0.0414 (6)
O1w0.3633 (5)0.75000.5411 (7)0.075 (2)
O2w0.5880 (6)0.75000.3588 (7)0.082 (2)
O3w0.3760 (3)0.6346 (2)0.3296 (3)0.0499 (8)
O4w0.5741 (3)0.6351 (3)0.5675 (4)0.078 (1)
O5w0.8631 (5)0.75000.5598 (7)0.077 (2)
O6w1.1035 (6)0.75000.3926 (7)0.079 (2)
O7w0.8917 (3)0.6326 (2)0.3690 (3)0.0556 (8)
O8w1.0974 (3)0.6417 (2)0.6080 (3)0.0504 (8)
O9w1.1889 (18)0.75000.8388 (10)0.184 (5)
C11.0427 (3)0.4555 (3)0.2005 (3)0.0311 (7)
C21.0746 (3)0.3801 (3)0.1536 (3)0.0314 (7)
C31.0040 (3)0.3460 (3)0.0501 (3)0.0323 (7)
C40.8993 (3)0.3876 (3)−0.0058 (3)0.0347 (8)
C50.8698 (3)0.4668 (3)0.0398 (3)0.0342 (8)
C60.9418 (3)0.5007 (3)0.1423 (3)0.0345 (8)
C70.6085 (3)0.4536 (2)0.1891 (3)0.0292 (7)
C80.5393 (3)0.3784 (2)0.1392 (3)0.0296 (7)
C90.5307 (3)0.3452 (3)0.0371 (3)0.0309 (7)
C100.5935 (3)0.3876 (3)−0.0159 (3)0.0331 (7)
C110.6604 (3)0.4651 (3)0.0336 (3)0.0321 (7)
C120.6670 (3)0.4979 (2)0.1354 (3)0.0319 (7)
H1w10.339 (5)0.7013 (4)0.561 (5)0.090*
H2w10.624 (3)0.7012 (4)0.358 (6)0.099*
H3w10.416 (3)0.589 (2)0.327 (5)0.060*
H3w20.317 (3)0.615 (3)0.335 (5)0.060*
H4w10.638 (3)0.617 (4)0.573 (6)0.093*
H4w20.547 (5)0.594 (3)0.597 (6)0.093*
H5w10.834 (4)0.7012 (4)0.574 (6)0.093*
H6w11.124 (5)0.7012 (4)0.369 (5)0.094*
H7w10.833 (3)0.614 (3)0.376 (5)0.067*
H7w20.934 (3)0.586 (2)0.375 (5)0.067*
H8w11.052 (3)0.598 (2)0.605 (5)0.060*
H8w21.154 (3)0.618 (3)0.601 (5)0.060*
H9w11.176 (12)0.7013 (4)0.798 (2)0.221*
H21.14350.35210.19130.038*
H60.92270.55360.17200.041*
H80.49850.35020.17450.036*
H1210.71090.54980.16770.038*
H110.84490.3019−0.12840.061*0.50
H120.76360.3756−0.13560.061*0.50
H210.62730.3785−0.14420.055*0.50
H220.54840.3060−0.14190.055*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0303 (2)0.0309 (2)0.0554 (3)0.0000.02266 (18)0.000
Cd20.0288 (2)0.0337 (2)0.0603 (3)0.0000.02012 (18)0.000
S10.0252 (4)0.0308 (4)0.0354 (4)0.0003 (3)0.0143 (3)0.0017 (3)
S20.0415 (7)0.0496 (8)0.0348 (6)0.0000.0260 (6)0.000
S30.0312 (4)0.0483 (6)0.0437 (5)0.0083 (4)0.0160 (4)0.0262 (4)
S40.0241 (6)0.0410 (7)0.0364 (6)0.0000.0045 (5)0.000
S50.0285 (4)0.0265 (4)0.0371 (4)0.0023 (3)0.0153 (3)0.0005 (3)
O10.042 (2)0.071 (2)0.031 (1)0.001 (2)0.006 (1)0.004 (1)
O20.051 (2)0.055 (2)0.035 (1)−0.006 (1)0.021 (1)−0.001 (1)
O30.043 (2)0.035 (1)0.053 (2)−0.008 (1)0.024 (1)−0.001 (1)
O40.032 (1)0.041 (2)0.042 (1)0.008 (1)0.010 (1)0.001 (1)
O50.036 (1)0.050 (2)0.044 (2)0.000 (1)0.024 (1)0.001 (1)
O60.040 (1)0.038 (1)0.039 (1)0.007 (1)0.014 (1)0.006 (1)
O70.043 (2)0.029 (1)0.056 (2)−0.003 (1)0.023 (1)−0.006 (1)
O80.037 (1)0.045 (2)0.051 (2)0.004 (1)0.026 (1)0.000 (1)
O1w0.090 (4)0.036 (2)0.15 (6)0.0000.095 (4)0.000
O2w0.100 (5)0.029 (2)0.172 (7)0.0000.112 (5)0.000
O3w0.038 (2)0.038 (2)0.078 (2)−0.005 (1)0.029 (2)−0.009 (2)
O4w0.049 (2)0.083 (3)0.116 (3)0.030 (2)0.048 (2)0.057 (3)
O5w0.088 (4)0.037 (2)0.150 (6)0.0000.093 (4)0.000
O6w0.097 (4)0.039 (3)0.144 (6)0.0000.095 (5)0.000
O7w0.036 (2)0.047 (2)0.082 (2)−0.003 (1)0.021 (2)−0.011 (2)
O8w0.040 (2)0.039 (2)0.076 (2)0.004 (1)0.027 (2)0.009 (2)
O9w0.27 (2)0.15 (1)0.15 (1)0.0000.10 (1)0.000
C10.026 (2)0.033 (2)0.035 (2)0.000 (1)0.014 (1)0.007 (1)
C20.026 (2)0.035 (2)0.035 (2)0.002 (1)0.013 (1)0.007 (1)
C30.034 (2)0.038 (2)0.032 (2)0.001 (1)0.020 (1)0.007 (1)
C40.033 (2)0.045 (2)0.028 (2)−0.002 (2)0.014 (1)0.012 (2)
C50.027 (2)0.040 (2)0.039 (2)0.004 (1)0.016 (1)0.018 (2)
C60.030 (2)0.034 (2)0.043 (2)0.003 (1)0.018 (2)0.008 (2)
C70.025 (2)0.028 (2)0.034 (2)0.005 (1)0.012 (1)0.006 (1)
C80.027 (2)0.030 (2)0.034 (2)0.003 (1)0.014 (1)0.006 (1)
C90.024 (2)0.033 (2)0.033 (2)0.004 (1)0.008 (1)0.005 (1)
C100.028 (2)0.040 (2)0.029 (2)0.009 (1)0.009 (1)0.009 (1)
C110.025 (2)0.036 (2)0.038 (2)0.007 (1)0.014 (1)0.017 (2)
C120.025 (2)0.030 (2)0.040 (2)0.003 (1)0.012 (1)0.008 (1)
Geometric parameters (Å, º) top
Cd1—O1w2.243 (5)C3—C41.405 (5)
Cd1—O2w2.243 (5)C4—C51.404 (6)
Cd1—O3w2.288 (3)C5—C61.390 (6)
Cd1—O3wi2.288 (3)C7—C121.386 (5)
Cd1—O4w2.279 (4)C7—C81.388 (5)
Cd1—O4wi2.279 (4)C8—C91.388 (5)
Cd2—O5w2.272 (5)C9—C101.411 (5)
Cd2—O6w2.245 (5)C10—C111.401 (5)
Cd2—O7w2.275 (3)C11—C121.391 (5)
Cd2—O7wi2.275 (3)O1—H110.85
Cd2—O8w2.287 (3)O1—H120.85
Cd2—O8wi2.287 (3)O2—H210.85
S1—O41.458 (3)O2—H220.85
S1—O31.459 (3)O1w—H1w10.85 (1)
S1—O51.464 (3)O2w—H2w10.84 (1)
S1—C11.770 (4)O3w—H3w10.85 (1)
S2—C31.785 (4)O3w—H3w20.85 (1)
S2—C3ii1.785 (4)O4w—H4w10.85 (1)
S3—C51.786 (4)O4w—H4w20.85 (1)
S3—C111.788 (3)O5w—H5w10.85 (1)
S4—C91.784 (4)O6w—H6w10.85 (1)
S4—C9ii1.784 (4)O7w—H7w10.85 (1)
S5—O61.459 (3)O7w—H7w20.85 (1)
S5—O71.459 (3)O8w—H8w10.85 (1)
S5—O81.459 (3)O8w—H8w20.85 (1)
S5—C71.767 (4)O9w—H9w10.86 (1)
O1—C41.349 (5)C2—H20.93
O2—C101.346 (5)C6—H60.93
C1—C61.394 (5)C8—H80.93
C1—C21.386 (5)C12—H1210.93
C2—C31.394 (5)
O1w—Cd1—O2w179.3 (3)O1—C4—C3120.0 (4)
O1w—Cd1—O3w93.4 (2)O1—C4—C5120.4 (3)
O1w—Cd1—O3wi93.4 (2)C3—C4—C5119.6 (3)
O1w—Cd1—O4w87.0 (2)C6—C5—C4119.9 (3)
O1w—Cd1—O4wi87.0 (2)C6—C5—S3120.4 (3)
O2w—Cd1—O3w87.0 (2)C4—C5—S3119.6 (3)
O2w—Cd1—O3wi87.0 (2)C5—C6—C1120.1 (4)
O2w—Cd1—O4w92.6 (2)C12—C7—C8120.1 (3)
O2w—Cd1—O4wi92.6 (2)C12—C7—S5120.3 (3)
O3w—Cd1—O3wi92.0 (2)C8—C7—S5119.6 (3)
O3w—Cd1—O4w88.1 (2)C9—C8—C7120.4 (3)
O3w—Cd1—O4wi179.6 (1)C8—C9—C10119.8 (3)
O3wi—Cd1—O4w179.6 (1)C8—C9—S4120.0 (3)
O3wi—Cd1—O4wi88.1 (2)C10—C9—S4120.2 (3)
O4w—Cd1—O4wi91.9 (3)O2—C10—C11120.7 (3)
O5w—Cd2—O6w175.1 (3)O2—C10—C9120.1 (3)
O5w—Cd2—O7w88.3 (2)C11—C10—C9119.2 (3)
O5w—Cd2—O7wi88.3 (2)C12—C11—C10120.0 (3)
O5w—Cd2—O8w91.5 (2)C12—C11—S3119.8 (3)
O5w—Cd2—O8wi91.5 (2)C10—C11—S3120.2 (3)
O6w—Cd2—O7w88.4 (2)C11—C12—C7120.4 (3)
O6w—Cd2—O7wi88.4 (2)C4—O1—H11120.0
O6w—Cd2—O8w92.1 (2)C4—O1—H12120.0
O6w—Cd2—O8wi92.1 (2)H11—O1—H12120.0
O7w—Cd2—O7wi94.7 (2)C10—O2—H21120.0
O7w—Cd2—O8w90.2 (1)C10—O2—H22120.0
O7w—Cd2—O8wi175.1 (1)H21—O2—H22120.0
O7wi—Cd2—O8w175.1 (1)Cd1—O1w—H1w1125 (1)
O7wi—Cd2—O8wi90.2 (1)Cd1—O2w—H2w1120 (3)
O8w—Cd2—O8wi85.0 (2)Cd1—O3w—H3w1113 (3)
O4—S1—O3113.5 (2)Cd1—O3w—H3w2117 (4)
O4—S1—O5111.9 (2)H3w1—O3w—H3w2110 (2)
O3—S1—O5111.6 (2)Cd1—O4w—H4w1123 (4)
O4—S1—C1105.7 (2)Cd1—O4w—H4w2125 (4)
O3—S1—C1107.8 (2)H4w1—O4w—H4w2109 (2)
O5—S1—C1105.6 (2)Cd2—O5w—H5w1125 (1)
C3—S2—C3ii100.2 (2)Cd2—O6w—H6w1125 (1)
C5—S3—C1198.9 (2)Cd2—O7w—H7w1117 (4)
C9—S4—C9ii99.1 (2)Cd2—O7w—H7w2110 (4)
O6—S5—O7112.3 (2)H7w1—O7w—H7w2109 (2)
O6—S5—O8111.9 (2)Cd2—O8w—H8w1104 (4)
O7—S5—O8113.2 (2)Cd2—O8w—H8w2120 (4)
O6—S5—C7105.5 (2)H8w1—O8w—H8w2110 (2)
O7—S5—C7106.4 (2)C1—C2—H2119.8
O8—S5—C7106.8 (2)C3—C2—H2119.8
C6—C1—C2120.1 (3)C5—C6—H6119.9
C6—C1—S1119.4 (3)C1—C6—H6119.9
C2—C1—S1120.4 (3)C9—C8—H8119.8
C1—C2—C3120.5 (3)C7—C8—H8119.8
C2—C3—C4119.6 (3)C11—C12—H121119.8
C2—C3—S2119.9 (3)C7—C12—H121119.8
C4—C3—S2120.5 (3)
O4—S1—C1—C6167.1 (3)O6—S5—C7—C12−100.9 (3)
O3—S1—C1—C6−71.1 (3)O7—S5—C7—C1218.5 (3)
O5—S1—C1—C648.4 (3)O8—S5—C7—C12139.8 (3)
O4—S1—C1—C2−10.4 (3)O6—S5—C7—C875.5 (3)
O3—S1—C1—C2111.3 (3)O7—S5—C7—C8−165.0 (3)
O5—S1—C1—C2−129.2 (3)O8—S5—C7—C8−43.8 (3)
C6—C1—C2—C3−3.0 (5)C12—C7—C8—C92.0 (5)
S1—C1—C2—C3174.5 (3)S5—C7—C8—C9−174.4 (3)
C1—C2—C3—C4−1.1 (5)C7—C8—C9—C100.6 (5)
C1—C2—C3—S2179.1 (3)C7—C8—C9—S4−178.9 (3)
C3ii—S2—C3—C286.5 (3)C9ii—S4—C9—C8−86.0 (3)
C3ii—S2—C3—C4−93.4 (3)C9ii—S4—C9—C1094.6 (3)
C2—C3—C4—O1−174.8 (3)C8—C9—C10—O2177.1 (3)
S2—C3—C4—O15.1 (5)S4—C9—C10—O2−3.5 (5)
C2—C3—C4—C54.2 (5)C8—C9—C10—C11−2.5 (5)
S2—C3—C4—C5−175.9 (3)S4—C9—C10—C11176.9 (3)
O1—C4—C5—C6175.7 (3)O2—C10—C11—C12−177.7 (3)
C3—C4—C5—C6−3.3 (5)C9—C10—C11—C121.9 (5)
O1—C4—C5—S3−2.9 (5)O2—C10—C11—S31.8 (5)
C3—C4—C5—S3178.1 (3)C9—C10—C11—S3−178.6 (3)
C11—S3—C5—C6−83.3 (3)C5—S3—C11—C1281.7 (3)
C11—S3—C5—C495.4 (3)C5—S3—C11—C10−97.8 (3)
C4—C5—C6—C1−0.8 (5)C10—C11—C12—C70.6 (5)
S3—C5—C6—C1177.8 (3)S3—C11—C12—C7−178.9 (3)
C2—C1—C6—C53.9 (5)C8—C7—C12—C11−2.6 (5)
S1—C1—C6—C5−173.6 (3)S5—C7—C12—C11173.8 (3)
Symmetry codes: (i) x, −y+3/2, z; (ii) x, −y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O6iii0.85 (1)1.92 (1)2.767 (4)172 (3)
O2w—H2w1···O70.84 (1)1.90 (1)2.732 (4)169 (4)
O3w—H3w1···O80.85 (1)1.97 (1)2.817 (4)176 (5)
O3w—H3w2···O3iv0.85 (1)1.91 (1)2.754 (4)171 (5)
O4w—H4w1···O4v0.85 (1)1.91 (2)2.746 (4)168 (7)
O4w—H4w2···O8iii0.85 (1)1.93 (1)2.775 (5)174 (7)
O5w—H5w1···O4v0.85 (1)1.98 (1)2.814 (4)172 (6)
O6w—H6w1···O30.85 (1)1.94 (1)2.786 (4)175 (4)
O7w—H7w2···O50.85 (1)1.93 (1)2.764 (4)169 (5)
O7w—H7w1···O70.85 (1)1.96 (2)2.781 (4)162 (6)
O8w—H8w1···O5v0.85 (1)1.94 (1)2.788 (4)176 (5)
O8w—H8w2···O6v0.85 (1)1.96 (1)2.798 (4)170 (5)
O9w—H9w1···O8w0.86 (1)2.44 (2)3.188 (12)146 (3)
O1—H11···O1ii0.852.232.864 (7)132
O1—H12···O20.852.453.066 (5)130
O2—H21···O10.852.483.066 (4)127
O2—H22···O2ii0.852.332.940 (4)129
Symmetry codes: (ii) x, −y+1/2, z; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z; (v) −x+2, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula[Cd(H2O)6]2(C24H2O16S8)·H2O
Mr1271.82
Crystal system, space groupMonoclinic, P21/m
Temperature (K)295
a, b, c (Å)13.1183 (5), 14.2581 (6), 13.1854 (5)
β (°) 113.563 (1)
V (Å3)2260.6 (2)
Z2
Radiation typeMo Kα
µ (mm−1)1.40
Crystal size (mm)0.35 × 0.33 × 0.27
Data collection
DiffractometerBruker APEX2 area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.556, 0.703
No. of measured, independent and
observed [I > 2σ(I)] reflections		19302, 5380, 5106
Rint0.019
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.130, 1.11
No. of reflections5380
No. of parameters337
No. of restraints22
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.76, −1.74

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected bond lengths (Å) top
Cd1—O1w2.243 (5)Cd2—O5w2.272 (5)
Cd1—O2w2.243 (5)Cd2—O6w2.245 (5)
Cd1—O3w2.288 (3)Cd2—O7w2.275 (3)
Cd1—O4w2.279 (4)Cd2—O8w2.287 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O6i0.85 (1)1.92 (1)2.767 (4)172 (3)
O2w—H2w1···O70.84 (1)1.90 (1)2.732 (4)169 (4)
O3w—H3w1···O80.85 (1)1.97 (1)2.817 (4)176 (5)
O3w—H3w2···O3ii0.85 (1)1.91 (1)2.754 (4)171 (5)
O4w—H4w1···O4iii0.85 (1)1.91 (2)2.746 (4)168 (7)
O4w—H4w2···O8i0.85 (1)1.93 (1)2.775 (5)174 (7)
O5w—H5w1···O4iii0.85 (1)1.98 (1)2.814 (4)172 (6)
O6w—H6w1···O30.85 (1)1.94 (1)2.786 (4)175 (4)
O7w—H7w2···O50.85 (1)1.93 (1)2.764 (4)169 (5)
O7w—H7w1···O70.85 (1)1.96 (2)2.781 (4)162 (6)
O8w—H8w1···O5iii0.85 (1)1.94 (1)2.788 (4)176 (5)
O8w—H8w2···O6iii0.85 (1)1.96 (1)2.798 (4)170 (5)
O9w—H9w1···O8w0.86 (1)2.44 (2)3.188 (12)146 (3)
O1—H11···O1iv0.852.232.864 (7)132
O1—H12···O20.852.453.066 (5)130
O2—H21···O10.852.483.066 (4)127
O2—H22···O2iv0.852.332.940 (4)129
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z; (iii) −x+2, −y+1, −z+1; (iv) x, −y+1/2, z.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
E-alerts
Follow Acta Cryst. on Twitter
Twitter
Follow us on facebook
Facebook
Sign up for RSS feeds
RSS