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In the title compound, [Cd(C8H3O7S)(C6H13N2)(H2O)]n, the Cd atom is coordinated by one O atom of a carboxyl­ate group of a 5-sulfatoisophthalato ligand, two O atoms of the carboxyl­ate group group of an adjacent symmetry-related 5-sulfo­isophthalato entity, one O atom of the sulfonyl group of yet another adjacent 5-sulfatooisophthalato entity, a water mol­ecule and the N atom of the 1-aza-4-azoniabi­cyclo­[2.2.2]­octane cation in a six-coordinate octahedral geometry. Thus, the mode of coordination of the 5-sulfatoisophthalato ligand leads to the formation of a linear ribbon motif; adjacent ribbons are linked by hydrogen-bonding interactions, giving rise to a three-dimensional network structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803013230/ya6165sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803013230/ya6165Isup2.hkl
Contains datablock I

CCDC reference: 202766

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.025
  • wR factor = 0.056
  • Data-to-parameter ratio = 15.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.20 From the CIF: _reflns_number_total 3750 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 4037 Completeness (_total/calc) 92.89% Alert C: < 95% complete
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

The 5-sulfoisophthalato monoanion, [C6H3-1,3-(CO2H)2-5-SO3], reacts with copper nitrate in the presence of hexamine to form C6H3-1,3-(CO2)2-5-SO3H](H2O)3Cu·6H2O·0.5(CH2)6N4. In the crystal structure, the [C6H3-1,3-(CO2)2-5-SO3H]2− dianion links adjacent Cu atoms through both monodentate –CO2 groups into a linear chain, and adjacent chains are linked by hydrogen bonds to the water and hexamine molecules into a network motif. The piperazine guest-host analog, [C6H3-1,3-(CO2)2-5-SO3H](H2O)2Cu·6H2O·0.5 N(CH2)4N, follows the similar pattern (Sun et al., 2003). The other known metal complex of 5-sulfoisophthalic acid is also a copper derivative, [C6H3(CO2)2(SO3)]2Cu3, whose Cu atoms are coordinated by pyridine ligands (Kulynych & Shimizu, 2002).

We have employed the anion to react with Cd2+ in the presence of 1,4-diazabicyclo[2.2.2]octane in the hope of synthesizing a similar guest–host hydrate, i.e. [C6H3-1,3-(CO2)2-5-SO3H]Cd–N(CH2CH2)3N.nH2O, (I), using a hydrothermal synthetic procedure. However, in the water-coordinated product, the H atom of the sulfonate group has protonated one of the N atoms of the 1,4-diazabicyclo[2.2.2]octane; the resulting 1-aza-4-azoniabicyclo[2.2.2]octane cation then engages its free N atom to coordinate to the Cd atom, and a zwitterionic compound results (Fig. 1).

The [C6H3-1,3-(CO2)2-5-SO3]3− trianion uses both –CO2 groups to link to adjacent Cd atoms to form a chain, but one of them is monodentate [Cd—O = 2.190 (2) Å] whereas the other is chelating [Cd—O = 2.331 (2) and 2.399 (2) Å]. Two chains are then linked by a sulfonate bridge [Cd—O = 2.349 (2) Å] to furnish a ribbon motif (Fig. 2). The ribbons are further linked by hydrogen-bonding interactions (Table 2) to give rise to a three-dimensional network structure. Protonation of one of the two N atoms of the 1,4-diazabicyclo[2.2.2]octane probably raises the Lewis basicity of the other N atom to permit it to bind to Cd [Cd1—N1 = 2.437 (2) Å]; a Cd N interaction of a similar length [Cd N 2.446 (3) Å] is also found in {[NH(CH2CH2)N]2Cd}{Ni(CN)4}2·4C6H5NH2 (Yuge & Iwamoto, 1995).

Experimental top

A 1/1 water–ethanol solution (8 ml) of cadmium nitrate tetrahydrate (0.15 g, 0.5 mmol), the monosodium salt of 5-sulfoisophthalic acid (0.13 g, 0.5 mmol) and diazabicyclo[2.2.2]octane (0.22 g, 2.0 mmol) was placed in a 23 ml Teflon-lined stainless vessel. The vessel was sealed and then heated at 433 K for 60 h, after which it was allowed to cool to room temperature. The crystals that deposited from the solution were collected and washed with water. CHN analysis for C14H18CdN2O8S: found C 34.22, H 3.79, N 6.02%; calculated C 34.54, H 3.73, N 5.75%. IR: 2983 (m), 2882 (w), 2808 (w), 2659 (m), 1683 (w), 1598 (s), 1555 (s), 1465 (m), 1434 (s), 1360 (s), 1240 (s), 1170 (s), 1092 (m), 1037 (s), 924 (w), 839 (m), 800 (m), 776 (s), 730 (s), 671 (m), 621 (s), 578 (m), 519 (w), 461 (w), 449 (w) cm−1.

Refinement top

The water and ammonium H atoms were located and refined subject to constraints of O—H = N—H = 0.85±0.01 and H···H = 1.39±0.01 Å. The C-bound H atoms were generated geometrically (C—H = 0.95 Å for the aromatic H atoms and 0.97 Å for the aliphatic H atoms) and were included in the refinement in the riding-model approximation; their displacement parameters were set at 1.2 times those of the equivalent isotropic displacement parameters of the parent C atoms.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); 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. ORTEPII (Johnson, 1976) plot of a segment of the structure of the title compound at the 50% probability level. [Symmetry codes: (i) x − 1/2, 1/2 − y, 1/2 + z; (ii) 3/2 − x, 1/2 − y, 1 − z.
[Figure 2] Fig. 2. ORTEPII (Johnson, 1976) plot of the ribbon structure running along the b axis.
Poly[[aqua(1-aza-4-azoniabicyclo[2.2.2]octane)cadmate(II)]-µ-5- sulfoisophthalato] top
Crystal data top
[Cd(C8H3O7S)(C6H13N2)(H2O)]F(000) = 1952
Mr = 486.76Dx = 1.974 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 18.5885 (8) ÅCell parameters from 6969 reflections
b = 8.8265 (4) Åθ = 2.0–28.2°
c = 21.7607 (9) ŵ = 1.51 mm1
β = 113.408 (1)°T = 298 K
V = 3276.5 (2) Å3Plate, colorless
Z = 80.40 × 0.08 × 0.04 mm
Data collection top
Bruker AXS area-detector
diffractometer
3750 independent reflections
Radiation source: fine-focus sealed tube3207 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ϕ and ω scansθmax = 28.2°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2424
Tmin = 0.689, Tmax = 0.941k = 1111
9529 measured reflectionsl = 1928
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H atoms treated by a mixture of independent and constrained refinement
S = 0.93 w = 1/[σ2(Fo2) + (0.0278P)2]
where P = (Fo2 + 2Fc2)/3
3750 reflections(Δ/σ)max = 0.001
247 parametersΔρmax = 0.63 e Å3
4 restraintsΔρmin = 0.42 e Å3
Crystal data top
[Cd(C8H3O7S)(C6H13N2)(H2O)]V = 3276.5 (2) Å3
Mr = 486.76Z = 8
Monoclinic, C2/cMo Kα radiation
a = 18.5885 (8) ŵ = 1.51 mm1
b = 8.8265 (4) ÅT = 298 K
c = 21.7607 (9) Å0.40 × 0.08 × 0.04 mm
β = 113.408 (1)°
Data collection top
Bruker AXS area-detector
diffractometer
3750 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3207 reflections with I > 2σ(I)
Tmin = 0.689, Tmax = 0.941Rint = 0.024
9529 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0254 restraints
wR(F2) = 0.056H atoms treated by a mixture of independent and constrained refinement
S = 0.93Δρmax = 0.63 e Å3
3750 reflectionsΔρmin = 0.42 e Å3
247 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd10.632505 (9)0.53351 (2)0.360303 (8)0.02357 (6)
S10.99060 (3)0.28780 (7)0.63378 (3)0.0249 (1)
O10.7530 (1)0.4692 (2)0.4242 (1)0.0372 (4)
O20.7544 (1)0.3492 (2)0.3350 (1)0.0348 (4)
O31.0194 (1)0.1558 (2)0.3560 (1)0.0295 (4)
O41.1077 (1)0.1047 (2)0.4565 (1)0.0357 (4)
O51.0671 (1)0.2185 (2)0.6640 (1)0.0341 (4)
O60.9296 (1)0.2006 (2)0.6446 (1)0.0338 (4)
O70.9888 (1)0.4447 (2)0.6507 (1)0.0370 (4)
O1w0.5949 (1)0.5180 (2)0.2491 (1)0.0326 (4)
N10.6818 (1)0.7819 (2)0.3470 (1)0.0252 (4)
N20.7300 (1)1.0435 (2)0.3346 (1)0.0268 (4)
C10.7862 (1)0.3909 (3)0.3946 (1)0.0261 (5)
C20.8675 (1)0.3353 (3)0.4372 (1)0.0245 (5)
C30.9159 (1)0.2746 (3)0.4088 (1)0.0259 (5)
C40.9889 (1)0.2183 (3)0.4494 (1)0.0244 (5)
C51.0129 (1)0.2203 (3)0.5182 (1)0.0264 (5)
C60.9647 (1)0.2815 (3)0.5463 (1)0.0239 (5)
C70.8927 (1)0.3403 (3)0.5056 (1)0.0273 (5)
C81.0423 (1)0.1545 (3)0.4190 (1)0.0256 (5)
C90.7527 (2)0.7727 (3)0.3325 (2)0.0448 (8)
C100.7820 (2)0.9292 (3)0.3233 (2)0.0351 (6)
C110.6211 (2)0.8659 (3)0.2923 (1)0.0365 (6)
C120.6479 (2)1.0242 (3)0.2840 (1)0.0363 (6)
C130.7016 (2)0.8702 (3)0.4091 (1)0.0402 (7)
C140.7322 (2)1.0263 (3)0.4034 (1)0.0366 (6)
H1w10.589 (2)0.429 (1)0.233 (1)0.05 (1)*
H1w20.560 (1)0.574 (2)0.221 (1)0.06 (1)*
H2n0.746 (1)1.134 (2)0.332 (1)0.03 (1)*
H30.89930.27160.36240.031*
H51.06140.18040.54560.032*
H70.86090.38380.52470.033*
H9a0.74120.71360.29210.054*
H9b0.79370.72090.36910.054*
H10a0.83560.94380.35500.042*
H10b0.78040.93920.27840.042*
H11a0.57420.87290.30140.044*
H11b0.60790.81040.25070.044*
H12a0.64611.03700.23920.044*
H12b0.61381.09930.29110.044*
H13a0.74100.81610.44600.048*
H13b0.65520.88030.41890.048*
H14a0.70001.10340.41170.044*
H14b0.78561.03780.43620.044*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0195 (1)0.0277 (1)0.0247 (1)0.0044 (1)0.0100 (1)0.0003 (1)
S10.0257 (3)0.0268 (3)0.0238 (3)0.0030 (2)0.0115 (2)0.0009 (2)
O10.025 (1)0.044 (1)0.040 (1)0.014 (1)0.011 (1)0.000 (1)
O20.031 (1)0.035 (1)0.031 (1)0.003 (1)0.003 (1)0.005 (1)
O30.026 (1)0.038 (1)0.027 (1)0.002 (1)0.013 (1)0.004 (1)
O40.025 (1)0.052 (1)0.033 (1)0.013 (1)0.014 (1)0.000 (1)
O50.029 (1)0.044 (1)0.027 (1)0.011 (1)0.009 (1)0.007 (1)
O60.037 (1)0.035 (1)0.036 (1)0.005 (1)0.022 (1)0.000 (1)
O70.048 (1)0.028 (1)0.038 (1)0.002 (1)0.020 (1)0.006 (1)
O1w0.035 (1)0.032 (1)0.027 (1)0.006 (1)0.008 (1)0.003 (1)
N10.024 (1)0.026 (1)0.028 (1)0.003 (1)0.013 (1)0.001 (1)
N20.029 (1)0.023 (1)0.033 (1)0.001 (1)0.016 (1)0.001 (1)
C10.021 (1)0.025 (1)0.031 (1)0.006 (1)0.009 (1)0.006 (1)
C20.021 (1)0.026 (1)0.027 (1)0.004 (1)0.010 (1)0.002 (1)
C30.025 (1)0.032 (1)0.021 (1)0.002 (1)0.010 (1)0.001 (1)
C40.023 (1)0.026 (1)0.028 (1)0.002 (1)0.014 (1)0.002 (1)
C50.020 (1)0.032 (1)0.027 (1)0.006 (1)0.009 (1)0.001 (1)
C60.023 (1)0.028 (1)0.022 (1)0.002 (1)0.010 (1)0.000 (1)
C70.023 (1)0.032 (2)0.030 (1)0.006 (1)0.014 (1)0.001 (1)
C80.023 (1)0.027 (1)0.030 (1)0.001 (1)0.015 (1)0.004 (1)
C90.040 (2)0.034 (2)0.076 (2)0.006 (1)0.039 (2)0.001 (2)
C100.033 (1)0.032 (2)0.050 (2)0.004 (1)0.027 (1)0.001 (1)
C110.033 (1)0.032 (2)0.037 (2)0.000 (1)0.004 (1)0.004 (1)
C120.031 (1)0.035 (2)0.039 (2)0.005 (1)0.009 (1)0.008 (1)
C130.055 (2)0.040 (2)0.029 (2)0.014 (1)0.019 (1)0.005 (1)
C140.052 (2)0.033 (2)0.032 (2)0.005 (1)0.024 (1)0.005 (1)
Geometric parameters (Å, º) top
Cd1—O12.190 (2)C4—C81.503 (3)
Cd1—O3i2.331 (2)C5—C61.379 (3)
Cd1—O4i2.399 (2)C6—C71.380 (3)
Cd1—O6ii2.349 (2)C9—C101.527 (4)
Cd1—O1w2.241 (2)C11—C121.518 (4)
Cd1—N12.437 (2)C13—C141.515 (4)
S1—O71.437 (2)O1w—H1w10.85 (1)
S1—O51.445 (2)O1w—H1w20.85 (1)
S1—O61.465 (2)N2—H2n0.86 (1)
S1—C61.769 (2)C3—H30.93
O1—C11.261 (3)C5—H50.93
O2—C11.248 (3)C7—H70.93
O3—C81.265 (3)C9—H9a0.97
O4—C81.244 (3)C9—H9b0.97
N1—C111.474 (3)C10—H10a0.97
N1—C91.474 (3)C10—H10b0.97
N1—C131.475 (3)C11—H11a0.97
N2—C101.484 (3)C11—H11b0.97
N2—C141.488 (3)C12—H12a0.97
N2—C121.495 (3)C12—H12b0.97
C1—C21.506 (3)C13—H13a0.97
C2—C71.372 (3)C13—H13b0.97
C2—C31.386 (3)C14—H14a0.97
C3—C41.384 (3)C14—H14b0.97
C4—C51.384 (3)
O1—Cd1—O3i145.5 (1)O4—C8—C4119.2 (2)
O1—Cd1—O4i91.0 (1)O3—C8—C4118.5 (2)
O1—Cd1—O6ii99.3 (1)N1—C9—C10112.0 (2)
O1—Cd1—O1w118.1 (1N2—C10—C9107.7 (2)
O1—Cd1—N188.3 (1)N1—C11—C12112.1 (2)
O3i—Cd1—O4i55.3 (1)N2—C12—C11107.7 (2)
O3i—Cd1—O6ii89.2 (1)N1—C13—C14111.7 (2)
O3i—Cd1—O1w95.5 (1)N2—C14—C13108.4 (2)
O3i—Cd1—N187.4 (1)Cd1—O1w—H1w1116 (2)
O4i—Cd1—O6ii90.5 (1)Cd1—O1w—H1w2124 (2)
O4i—Cd1—O1w150.8 (1)H1w1—O1w—H1w2108 (2)
O4i—Cd1—N194.6 (1)C10—N2—H2n111 (2)
O6ii—Cd1—O1w87.7 (1)C14—N2—H2n106 (2)
O6ii—Cd1—N1170.8 (1)C12—N2—H2n110 (2)
O1w—Cd1—N184.1 (1)C4—C3—H3120.0
O7—S1—O5114.2 (1)C2—C3—H3120.0
O7—S1—O6111.6 (1)C6—C5—H5120.1
O5—S1—O6112.9 (1)C4—C5—H5120.1
O7—S1—C6106.4 (1)C2—C7—H7119.6
O5—S1—C6106.0 (1)C6—C7—H7119.6
O6—S1—C6105.0 (1)N1—C9—H9a109.2
C1—O1—Cd1113.7 (2)C10—C9—H9a109.2
C8—O3—Cd1iii92.5 (1)N1—C9—H9b109.2
C8—O4—Cd1iii89.9 (1)C10—C9—H9b109.2
S1—O6—Cd1ii148.5 (1)H9a—C9—H9b107.9
C11—N1—C9108.5 (2)N2—C10—H10a110.2
C11—N1—C13107.9 (2)C9—C10—H10a110.2
C9—N1—C13107.9 (2)N2—C10—H10b110.2
C11—N1—Cd1110.2 (1)C9—C10—H10b110.2
C9—N1—Cd1112.7 (2)H10a—C10—H10b108.5
C13—N1—Cd1109.5 (2)N1—C11—H11a109.2
C10—N2—C14109.7 (2)C12—C11—H11a109.2
C10—N2—C12110.0 (2)N1—C11—H11b109.2
C14—N2—C12110.0 (2)C12—C11—H11b109.2
O2—C1—O1124.5 (2)H11a—C11—H11b107.9
O2—C1—C2119.2 (2)N2—C12—H12a110.2
O1—C1—C2116.0 (2)C11—C12—H12a110.2
C7—C2—C3119.6 (2)N2—C12—H12b110.2
C7—C2—C1118.9 (2)C11—C12—H12b110.2
C3—C2—C1121.4 (2)H12a—C12—H12b108.5
C4—C3—C2120.0 (2)N1—C13—H13a109.3
C5—C4—C3120.0 (2)C14—C13—H13a109.3
C5—C4—C8119.7 (2)N1—C13—H13b109.3
C3—C4—C8120.3 (2)C14—C13—H13b109.3
C6—C5—C4119.9 (2)H13a—C13—H13b107.9
C5—C6—C7119.9 (2)N2—C14—H14a110.0
C5—C6—S1122.8 (2)C13—C14—H14a110.0
C7—C6—S1117.4 (2)N2—C14—H14b110.0
C2—C7—C6120.7 (2)C13—C14—H14b110.0
O4—C8—O3122.2 (2)H14a—C14—H14b108.4
O1w—Cd1—O1—C117.7 (2)C4—C5—C6—S1179.7 (2)
O3i—Cd1—O1—C1177.0 (2)O7—S1—C6—C5121.7 (2)
O6ii—Cd1—O1—C174.7 (2)O5—S1—C6—C50.2 (2)
O4i—Cd1—O1—C1165.3 (2)O6—S1—C6—C5119.9 (2)
N1—Cd1—O1—C1100.1 (2)O7—S1—C6—C758.7 (2)
C8i—Cd1—O1—C1168.6 (2)O5—S1—C6—C7179.4 (2)
O7—S1—O6—Cd1ii179.4 (2)O6—S1—C6—C759.6 (2)
O5—S1—O6—Cd1ii50.4 (2)C3—C2—C7—C61.9 (4)
C6—S1—O6—Cd1ii64.6 (2)C1—C2—C7—C6175.8 (2)
O1—Cd1—N1—C11167.1 (2)C5—C6—C7—C21.6 (4)
O1w—Cd1—N1—C1148.7 (2)S1—C6—C7—C2178.0 (2)
O3i—Cd1—N1—C1147.1 (2)Cd1iii—O4—C8—O33.2 (3)
O4i—Cd1—N1—C11102.0 (2)Cd1iii—O4—C8—C4178.0 (2)
C8i—Cd1—N1—C1174.7 (2)Cd1iii—O3—C8—O43.3 (3)
O1—Cd1—N1—C945.8 (2)Cd1iii—O3—C8—C4177.9 (2)
O1w—Cd1—N1—C972.7 (2)C5—C4—C8—O40.2 (4)
O3i—Cd1—N1—C9168.5 (2)C3—C4—C8—O4179.9 (2)
O4i—Cd1—N1—C9136.6 (2)C5—C4—C8—O3179.1 (2)
C8i—Cd1—N1—C9164.0 (2)C3—C4—C8—O31.1 (4)
O1—Cd1—N1—C1374.3 (2)C11—N1—C9—C1056.8 (3)
O1w—Cd1—N1—C13167.2 (2)C13—N1—C9—C1059.8 (3)
O3i—Cd1—N1—C1371.4 (2)Cd1—N1—C9—C10179.1 (2)
O4i—Cd1—N1—C1316.5 (2)C14—N2—C10—C959.3 (3)
C8i—Cd1—N1—C1343.9 (2)C12—N2—C10—C961.9 (3)
Cd1—O1—C1—O21.5 (3)N1—C9—C10—N22.1 (3)
Cd1—O1—C1—C2176.4 (2)C9—N1—C11—C1258.6 (3)
O2—C1—C2—C7159.9 (2)C13—N1—C11—C1258.0 (3)
O1—C1—C2—C715.3 (4)Cd1—N1—C11—C12177.5 (2)
O2—C1—C2—C317.7 (4)C10—N2—C12—C1160.3 (3)
O1—C1—C2—C3167.1 (2)C14—N2—C12—C1160.7 (3)
C7—C2—C3—C40.5 (4)N1—C11—C12—N21.0 (3)
C1—C2—C3—C4177.1 (2)C11—N1—C13—C1459.8 (3)
C2—C3—C4—C51.1 (4)C9—N1—C13—C1457.3 (3)
C2—C3—C4—C8179.0 (2)Cd1—N1—C13—C14179.7 (2)
C3—C4—C5—C61.5 (4)C10—N2—C14—C1362.0 (3)
C8—C4—C5—C6178.7 (2)C12—N2—C14—C1359.1 (3)
C4—C5—C6—C70.1 (4)N1—C13—C14—N22.0 (3)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x+3/2, y+1/2, z+1; (iii) x+1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O5iv0.85 (1)1.91 (2)2.700 (3)155 (3)
O1w—H1w2···O3v0.85 (1)1.88 (1)2.714 (2)165 (3)
N2—H2n···O2vi0.86 (1)1.91 (1)2.736 (3)161 (3)
Symmetry codes: (iv) x1/2, y+1/2, z1/2; (v) x+3/2, y+1/2, z+1/2; (vi) x, y+1, z.

Experimental details

Crystal data
Chemical formula[Cd(C8H3O7S)(C6H13N2)(H2O)]
Mr486.76
Crystal system, space groupMonoclinic, C2/c
Temperature (K)298
a, b, c (Å)18.5885 (8), 8.8265 (4), 21.7607 (9)
β (°) 113.408 (1)
V3)3276.5 (2)
Z8
Radiation typeMo Kα
µ (mm1)1.51
Crystal size (mm)0.40 × 0.08 × 0.04
Data collection
DiffractometerBruker AXS area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.689, 0.941
No. of measured, independent and
observed [I > 2σ(I)] reflections
9529, 3750, 3207
Rint0.024
(sin θ/λ)max1)0.665
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.056, 0.93
No. of reflections3750
No. of parameters247
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.63, 0.42

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Cd1—O12.190 (2)Cd1—O6ii2.349 (2)
Cd1—O3i2.331 (2)Cd1—O1w2.241 (2)
Cd1—O4i2.399 (2)Cd1—N12.437 (2)
O1—Cd1—O3i145.5 (1)O3i—Cd1—N187.4 (1)
O1—Cd1—O4i91.0 (1)O4i—Cd1—O6ii90.5 (1)
O1—Cd1—O6ii99.3 (1)O4i—Cd1—O1w150.8 (1)
O1—Cd1—O1w118.1 (1O4i—Cd1—N194.6 (1)
O1—Cd1—N188.3 (1)O6ii—Cd1—O1w87.7 (1)
O3i—Cd1—O4i55.3 (1)O6ii—Cd1—N1170.8 (1)
O3i—Cd1—O6ii89.2 (1)O1w—Cd1—N184.1 (1)
O3i—Cd1—O1w95.5 (1)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x+3/2, y+1/2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O5iii0.85 (1)1.91 (2)2.700 (3)155 (3)
O1w—H1w2···O3iv0.85 (1)1.88 (1)2.714 (2)165 (3)
N2—H2n···O2v0.86 (1)1.91 (1)2.736 (3)161 (3)
Symmetry codes: (iii) x1/2, y+1/2, z1/2; (iv) x+3/2, y+1/2, z+1/2; (v) x, y+1, z.
 

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