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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.

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

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 m3
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 mm1
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 = 1717
Tmin = 0.556, Tmax = 0.703k = 1818
19302 measured reflectionsl = 1717
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 Å3
22 restraintsΔρmin = 1.74 e Å3
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 mm1
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 Å3
5380 reflectionsΔρmin = 1.74 e Å3
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)0.25000.0102 (1)0.0386 (3)
S30.73831 (7)0.52185 (8)0.03325 (8)0.0408 (2)
S40.43955 (10)0.25000.0273 (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*
H110.84490.30190.12840.061*0.50
H120.76360.37560.13560.061*0.50
H210.62730.37850.14420.055*0.50
H220.54840.30600.14190.055*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—C12100.9 (3)
O3—S1—C1—C671.1 (3)O7—S5—C7—C1218.5 (3)
O5—S1—C1—C648.4 (3)O8—S5—C7—C12139.8 (3)
O4—S1—C1—C210.4 (3)O6—S5—C7—C875.5 (3)
O3—S1—C1—C2111.3 (3)O7—S5—C7—C8165.0 (3)
O5—S1—C1—C2129.2 (3)O8—S5—C7—C843.8 (3)
C6—C1—C2—C33.0 (5)C12—C7—C8—C92.0 (5)
S1—C1—C2—C3174.5 (3)S5—C7—C8—C9174.4 (3)
C1—C2—C3—C41.1 (5)C7—C8—C9—C100.6 (5)
C1—C2—C3—S2179.1 (3)C7—C8—C9—S4178.9 (3)
C3ii—S2—C3—C286.5 (3)C9ii—S4—C9—C886.0 (3)
C3ii—S2—C3—C493.4 (3)C9ii—S4—C9—C1094.6 (3)
C2—C3—C4—O1174.8 (3)C8—C9—C10—O2177.1 (3)
S2—C3—C4—O15.1 (5)S4—C9—C10—O23.5 (5)
C2—C3—C4—C54.2 (5)C8—C9—C10—C112.5 (5)
S2—C3—C4—C5175.9 (3)S4—C9—C10—C11176.9 (3)
O1—C4—C5—C6175.7 (3)O2—C10—C11—C12177.7 (3)
C3—C4—C5—C63.3 (5)C9—C10—C11—C121.9 (5)
O1—C4—C5—S32.9 (5)O2—C10—C11—S31.8 (5)
C3—C4—C5—S3178.1 (3)C9—C10—C11—S3178.6 (3)
C11—S3—C5—C683.3 (3)C5—S3—C11—C1281.7 (3)
C11—S3—C5—C495.4 (3)C5—S3—C11—C1097.8 (3)
C4—C5—C6—C10.8 (5)C10—C11—C12—C70.6 (5)
S3—C5—C6—C1177.8 (3)S3—C11—C12—C7178.9 (3)
C2—C1—C6—C53.9 (5)C8—C7—C12—C112.6 (5)
S1—C1—C6—C5173.6 (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) x1, 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)
V3)2260.6 (2)
Z2
Radiation typeMo Kα
µ (mm1)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)max1)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 Å3)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) x1, y, z; (iii) x+2, y+1, z+1; (iv) x, y+1/2, z.
 

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