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In the title compound, [Cd2(C7H4O6S)2(C12H8N2)4]·H2O, the CdII atoms are bridged by two 5-sulfonatosalicylate dianions, forming a centrosymmetric dinuclear complex. Each Cd atom is coordinated by four N atoms from two 1,10-phenanthroline mol­ecules and two O atoms from two 5-sulfonatosalicylate ligands in a distorted octa­hedral environment. A strong π–π stacking inter­action occurs between 1,10-phenanthroline ligands from neighboring dimers. Extensive hydrogen bonds give rise to a two-dimensional network and enhance the stability of the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805039437/is6151sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805039437/is6151Isup2.hkl
Contains datablock I

CCDC reference: 296583

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.031
  • wR factor = 0.072
  • Data-to-parameter ratio = 12.1

checkCIF/PLATON results

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Alert level C PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

5-Sulfosalicylic acid (5-H3ssal) has three functional groups, viz. hydroxy, carboxyl and sulfonic acid groups, and can be partly or fully deprotonated in the formation of metal complexes. Therefore, 5-sulfonatosalicylate metal complexes can exhibit interesting assembly structures (Fan, Cai et al., 2005; Fan & Zhu, 2005a,b), among which only one cyclic dimer was reported (Li et al., 2004). We present here the second 5-sulfonatosalicylate cyclic dimer, (I).

The title CdII complex is a centrosymmetric cyclic dimer, in which each Cd atom adopts a distorted octahedral geometry defined by four N atoms from two 1,10-phenanthroline ligands and two O atoms from one sulfonate and one carboxylate group of two 5-Hssal2− ligands (Fig. 1 and Table 1). The Cd—O(SO3) and Cd—N bond distances are similar to those in the cyclic dimer of bis[diaqua(1,10-phenanthroline)(µ-4-sulfonatobenzoato)cadmium(II)], (II) (Fan, Zhang et al., 2005). 5-Sulfosalicylic acid is doubly deprotonated and acts as a bridging ligand through its sulfonate and carboxylate groups. The Cd···Cd separation in the dimer is 8.1153 (5) Å, which is significantly shorter than 9.931 (1) Å in (II). In neighboring dimers, there is a strong ππ stacking interaction between symmetry-related N3/N4/C13–C24 1,10-phenanthroline groups (symmetry code: 1 − x, 1 − y, 2 − z), with an interplanar distance of 3.29 (2) Å. Moreover, intra- and intermolecular hydrogen bonds generate a two-dimensional extended network (Fig. 2 and Table 2) and stabilize the crystal packing.

Experimental top

A mixture of Cd(CH3COO)2·2H2O (0.053 g, 0.2 mmol), 5-sulfosalicylic acid dihydrate (0.050 g, 0.2 mmol) and 1,10-phenanthroline hydrate (0.040 g, 0.2 mmol) in an aqueous solution (10 ml) was stirred for 2 h, and then sealed in a 20 ml stainless steel reactor with a Teflon liner. The mixture was heated for 72 h at 423 K. Colorless plate-shaped crystals of (I) were obtained after cooling to room temperature and these were separated by suction filtration. Thermogravimetric measurement showed 1.35% weight loss between 377 and 441 K, which corresponds to one water molecule per Cd complex.

Refinement top

H atoms on C atoms were placed geometrically and refined as riding atoms with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C). The water and hydroxy H atoms were located from a difference Fourier map and were refined with a distance restraint of O—H = 0.85 (1) Å, and with Uiso(H) = 0.08 Å2. The occupancy of the water molecule O1w was initially refined and converged to 0.595 (12), and was then fixed at 0.5 in the final cycles of refinement.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. ORTEP-3 (Farrugia, 1997) view of (I). Displacement ellipsoids are drawn at the 40% probability level. H atoms are not shown for clarity [symmetry code (i): 1 − x, −y, 2 − z].
[Figure 2] Fig. 2. A view of the two-dimensional hydrogen-bonding network in (I). Hydrogen bonds are shown as dashed lines. 1,10-Phenanthroline ligands have been omitted for clarity.
Bis(µ-5-sulfonatosalicylato)bis[bis(1,10-phenanthroline)cadmium(II)] monohydrate top
Crystal data top
[Cd2(C7H4O6S)2(C12H8N2)4]·H2OF(000) = 1404
Mr = 1395.96Dx = 1.663 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7178 reflections
a = 15.1984 (7) Åθ = 2.3–27.9°
b = 9.8340 (4) ŵ = 0.91 mm1
c = 18.9902 (8) ÅT = 296 K
β = 100.778 (1)°Plate, colorless
V = 2788.2 (2) Å30.31 × 0.21 × 0.15 mm
Z = 2
Data collection top
Bruker APEX area-detector
diffractometer
4905 independent reflections
Radiation source: fine-focus sealed tube4600 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
ϕ and ω scansθmax = 25.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1817
Tmin = 0.765, Tmax = 0.875k = 1111
14180 measured reflectionsl = 2219
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0314P)2 + 2.1742P]
where P = (Fo2 + 2Fc2)/3
4905 reflections(Δ/σ)max = 0.001
406 parametersΔρmax = 0.39 e Å3
4 restraintsΔρmin = 0.33 e Å3
Crystal data top
[Cd2(C7H4O6S)2(C12H8N2)4]·H2OV = 2788.2 (2) Å3
Mr = 1395.96Z = 2
Monoclinic, P21/nMo Kα radiation
a = 15.1984 (7) ŵ = 0.91 mm1
b = 9.8340 (4) ÅT = 296 K
c = 18.9902 (8) Å0.31 × 0.21 × 0.15 mm
β = 100.778 (1)°
Data collection top
Bruker APEX area-detector
diffractometer
4905 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
4600 reflections with I > 2σ(I)
Tmin = 0.765, Tmax = 0.875Rint = 0.021
14180 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0314 restraints
wR(F2) = 0.072H-atom parameters constrained
S = 1.07Δρmax = 0.39 e Å3
4905 reflectionsΔρmin = 0.33 e Å3
406 parameters
Special details top

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*/UeqOcc. (<1)
Cd10.716876 (12)0.22732 (2)0.980272 (10)0.03252 (8)
S10.58041 (4)0.11818 (7)0.80855 (4)0.03517 (16)
N10.85396 (15)0.3304 (3)1.03881 (12)0.0399 (6)
N20.83530 (14)0.1325 (2)0.93496 (12)0.0375 (5)
N30.70536 (14)0.4285 (2)0.90958 (12)0.0360 (5)
N40.64130 (15)0.3972 (2)1.03419 (12)0.0368 (5)
O10.34167 (14)0.0890 (2)0.94857 (11)0.0465 (5)
O20.20607 (14)0.0316 (3)0.89132 (13)0.0652 (7)
O30.18930 (16)0.1432 (4)0.79092 (15)0.0816 (9)
O40.61524 (13)0.1302 (2)0.88582 (10)0.0491 (5)
O50.60269 (13)0.0135 (2)0.78217 (11)0.0484 (5)
O60.60394 (15)0.2308 (2)0.76750 (13)0.0546 (6)
O1W0.0108 (4)0.2434 (6)0.7480 (5)0.101 (2)0.50
C10.8636 (2)0.4279 (3)1.08740 (17)0.0505 (8)
H10.81250.46151.10160.061*
C20.9460 (2)0.4834 (4)1.11854 (18)0.0585 (9)
H20.94960.55181.15280.070*
C31.0205 (2)0.4356 (4)1.09788 (19)0.0612 (10)
H31.07620.47071.11850.073*
C41.0147 (2)0.3338 (4)1.04569 (17)0.0492 (8)
C51.0899 (2)0.2803 (4)1.0206 (2)0.0631 (10)
H51.14670.31311.03990.076*
C61.0815 (2)0.1845 (4)0.9702 (2)0.0613 (10)
H61.13230.15210.95500.074*
C70.99501 (19)0.1302 (3)0.93883 (17)0.0481 (8)
C80.9828 (2)0.0300 (4)0.88617 (19)0.0571 (9)
H81.03200.00460.86950.069*
C90.8995 (2)0.0177 (4)0.85898 (18)0.0552 (9)
H90.89090.08500.82400.066*
C100.8268 (2)0.0372 (3)0.88506 (16)0.0455 (7)
H100.76970.00490.86630.055*
C110.92857 (18)0.2831 (3)1.01692 (16)0.0395 (7)
C120.91869 (18)0.1798 (3)0.96226 (15)0.0391 (7)
C130.73720 (19)0.4448 (3)0.84968 (15)0.0433 (7)
H130.76340.37040.83140.052*
C140.7333 (2)0.5678 (4)0.81273 (16)0.0492 (8)
H140.75720.57510.77120.059*
C150.6940 (2)0.6771 (4)0.83823 (17)0.0504 (8)
H150.69020.75970.81390.060*
C160.65929 (18)0.6645 (3)0.90134 (16)0.0417 (7)
C170.6172 (2)0.7747 (3)0.93158 (19)0.0532 (8)
H170.61340.85940.90950.064*
C180.5831 (2)0.7577 (3)0.99141 (19)0.0535 (9)
H180.55470.83021.00930.064*
C190.58975 (19)0.6304 (3)1.02798 (16)0.0420 (7)
C200.5548 (2)0.6082 (3)1.09024 (17)0.0515 (8)
H200.52440.67761.10880.062*
C210.5652 (2)0.4855 (4)1.12357 (17)0.0514 (8)
H210.54300.47081.16530.062*
C220.60952 (19)0.3823 (3)1.09446 (16)0.0449 (7)
H220.61730.29921.11810.054*
C230.66689 (17)0.5372 (3)0.93577 (14)0.0345 (6)
C240.63275 (17)0.5197 (3)1.00127 (14)0.0347 (6)
C250.28959 (19)0.0286 (3)0.89914 (16)0.0404 (7)
C260.33121 (18)0.0502 (3)0.84613 (14)0.0363 (6)
C270.27890 (19)0.1348 (4)0.79563 (17)0.0503 (8)
C280.3187 (2)0.2132 (4)0.75002 (17)0.0540 (9)
H280.28370.27040.71720.065*
C290.4099 (2)0.2075 (3)0.75268 (15)0.0434 (7)
H290.43610.26050.72170.052*
C300.46250 (17)0.1222 (3)0.80172 (13)0.0329 (6)
C310.42321 (17)0.0449 (3)0.84784 (14)0.0328 (6)
H310.45870.01180.88070.039*
H1A0.0659 (12)0.265 (6)0.755 (5)0.080*0.50
H1B0.021 (3)0.315 (4)0.744 (4)0.080*0.50
H3A0.178 (3)0.088 (3)0.8223 (17)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02807 (12)0.03403 (13)0.03711 (13)0.00127 (8)0.01030 (8)0.00059 (8)
S10.0325 (3)0.0374 (4)0.0364 (4)0.0036 (3)0.0086 (3)0.0014 (3)
N10.0365 (13)0.0475 (15)0.0347 (13)0.0009 (11)0.0037 (10)0.0011 (11)
N20.0317 (12)0.0420 (14)0.0393 (13)0.0051 (10)0.0077 (10)0.0012 (11)
N30.0309 (12)0.0394 (14)0.0384 (13)0.0019 (10)0.0081 (10)0.0011 (10)
N40.0368 (12)0.0357 (13)0.0397 (13)0.0034 (10)0.0119 (10)0.0008 (10)
O10.0479 (12)0.0440 (12)0.0515 (13)0.0013 (10)0.0197 (10)0.0090 (10)
O20.0370 (12)0.0904 (19)0.0733 (16)0.0040 (12)0.0236 (11)0.0074 (14)
O30.0346 (13)0.125 (3)0.085 (2)0.0196 (15)0.0099 (12)0.0356 (18)
O40.0386 (11)0.0644 (15)0.0419 (12)0.0079 (10)0.0012 (9)0.0022 (10)
O50.0435 (11)0.0461 (13)0.0581 (13)0.0042 (10)0.0160 (10)0.0050 (10)
O60.0501 (13)0.0550 (14)0.0615 (15)0.0096 (10)0.0172 (11)0.0162 (11)
O1W0.064 (4)0.067 (4)0.160 (7)0.015 (3)0.005 (4)0.007 (4)
C10.0532 (19)0.053 (2)0.0433 (18)0.0021 (15)0.0036 (14)0.0004 (15)
C20.067 (2)0.058 (2)0.0448 (19)0.0137 (18)0.0053 (17)0.0012 (16)
C30.0462 (19)0.070 (2)0.059 (2)0.0201 (18)0.0122 (16)0.0145 (19)
C40.0368 (16)0.060 (2)0.0463 (18)0.0074 (15)0.0031 (13)0.0152 (16)
C50.0260 (16)0.086 (3)0.074 (3)0.0052 (16)0.0004 (16)0.019 (2)
C60.0291 (16)0.084 (3)0.073 (2)0.0095 (17)0.0156 (16)0.019 (2)
C70.0352 (16)0.058 (2)0.0540 (19)0.0133 (14)0.0142 (14)0.0167 (16)
C80.0461 (19)0.068 (2)0.063 (2)0.0188 (17)0.0249 (16)0.0054 (18)
C90.059 (2)0.056 (2)0.054 (2)0.0146 (17)0.0195 (16)0.0045 (16)
C100.0399 (16)0.0473 (18)0.0496 (18)0.0082 (14)0.0091 (13)0.0024 (15)
C110.0316 (15)0.0442 (17)0.0416 (16)0.0004 (12)0.0039 (12)0.0152 (13)
C120.0297 (14)0.0474 (17)0.0407 (16)0.0047 (12)0.0083 (12)0.0115 (13)
C130.0379 (15)0.0508 (19)0.0428 (17)0.0041 (13)0.0115 (13)0.0042 (14)
C140.0454 (17)0.064 (2)0.0401 (17)0.0110 (16)0.0141 (14)0.0074 (15)
C150.0459 (18)0.051 (2)0.0526 (19)0.0078 (15)0.0055 (15)0.0147 (16)
C160.0364 (15)0.0387 (17)0.0477 (17)0.0044 (13)0.0021 (13)0.0033 (14)
C170.060 (2)0.0339 (17)0.063 (2)0.0020 (15)0.0041 (17)0.0042 (15)
C180.064 (2)0.0328 (18)0.062 (2)0.0084 (15)0.0052 (17)0.0096 (15)
C190.0441 (16)0.0366 (17)0.0441 (17)0.0001 (13)0.0048 (13)0.0099 (13)
C200.060 (2)0.046 (2)0.0489 (19)0.0083 (15)0.0128 (15)0.0164 (15)
C210.0568 (19)0.063 (2)0.0389 (17)0.0030 (16)0.0194 (14)0.0082 (15)
C220.0461 (17)0.0492 (19)0.0412 (17)0.0028 (14)0.0129 (14)0.0038 (14)
C230.0289 (13)0.0339 (15)0.0387 (15)0.0019 (11)0.0017 (11)0.0014 (12)
C240.0306 (13)0.0351 (15)0.0377 (15)0.0006 (11)0.0046 (11)0.0036 (12)
C250.0418 (17)0.0401 (17)0.0418 (17)0.0010 (13)0.0143 (13)0.0060 (13)
C260.0368 (15)0.0385 (16)0.0345 (15)0.0012 (12)0.0086 (12)0.0028 (12)
C270.0353 (16)0.068 (2)0.0459 (18)0.0107 (15)0.0040 (13)0.0062 (16)
C280.0484 (19)0.067 (2)0.0435 (18)0.0166 (16)0.0017 (15)0.0174 (16)
C290.0489 (18)0.0489 (18)0.0326 (15)0.0039 (14)0.0085 (13)0.0069 (13)
C300.0339 (14)0.0348 (15)0.0301 (14)0.0002 (11)0.0064 (11)0.0029 (11)
C310.0363 (14)0.0311 (15)0.0309 (14)0.0042 (11)0.0057 (11)0.0003 (11)
Geometric parameters (Å, º) top
Cd1—O1i2.2177 (19)C7—C121.405 (4)
Cd1—O42.3407 (19)C8—C91.358 (5)
Cd1—N12.395 (2)C8—H80.9300
Cd1—N22.330 (2)C9—C101.400 (4)
Cd1—N32.379 (2)C9—H90.9300
Cd1—N42.366 (2)C10—H100.9300
S1—O41.469 (2)C11—C121.440 (4)
S1—O51.451 (2)C13—C141.394 (4)
S1—O61.437 (2)C13—H130.9300
S1—C301.773 (3)C14—C151.362 (5)
N1—C11.320 (4)C14—H140.9300
N1—C111.360 (4)C15—C161.402 (4)
N2—C101.322 (4)C15—H150.9300
N2—C121.359 (4)C16—C231.407 (4)
N3—C131.327 (4)C16—C171.432 (4)
N3—C231.356 (3)C17—C181.344 (5)
N4—C221.331 (4)C17—H170.9300
N4—C241.353 (4)C18—C191.425 (4)
O1—C251.258 (3)C18—H180.9300
O1—Cd1i2.2177 (19)C19—C201.401 (4)
O2—C251.251 (3)C19—C241.412 (4)
O3—C271.351 (4)C20—C211.358 (5)
O3—H3A0.85 (3)C20—H200.9300
O1W—H1A0.850 (10)C21—C221.388 (4)
O1W—H1B0.849 (10)C21—H210.9300
C1—C21.392 (5)C22—H220.9300
C1—H10.9300C23—C241.445 (4)
C2—C31.350 (5)C25—C261.500 (4)
C2—H20.9300C26—C311.394 (4)
C3—C41.400 (5)C26—C271.400 (4)
C3—H30.9300C27—C281.381 (5)
C4—C111.411 (4)C28—C291.378 (4)
C4—C51.420 (5)C28—H280.9300
C5—C61.332 (5)C29—C301.389 (4)
C5—H50.9300C29—H290.9300
C6—C71.440 (5)C30—C311.377 (4)
C6—H60.9300C31—H310.9300
C7—C81.392 (5)
O1i—Cd1—O486.23 (8)N2—C10—H10118.3
O1i—Cd1—N1112.96 (8)C9—C10—H10118.3
O1i—Cd1—N2113.91 (8)N1—C11—C4121.8 (3)
O1i—Cd1—N3149.14 (8)N1—C11—C12118.7 (2)
O1i—Cd1—N483.50 (8)C4—C11—C12119.5 (3)
O4—Cd1—N1156.97 (8)N2—C12—C7121.8 (3)
O4—Cd1—N289.91 (8)N2—C12—C11118.7 (2)
O4—Cd1—N386.47 (8)C7—C12—C11119.5 (3)
O4—Cd1—N4108.38 (8)N3—C13—C14123.2 (3)
N1—Cd1—N271.08 (8)N3—C13—H13118.4
N1—Cd1—N382.87 (8)C14—C13—H13118.4
N1—Cd1—N487.20 (8)C15—C14—C13119.1 (3)
N2—Cd1—N396.01 (8)C15—C14—H14120.4
N2—Cd1—N4155.99 (8)C13—C14—H14120.4
N3—Cd1—N470.53 (8)C14—C15—C16119.6 (3)
O5—S1—O4110.67 (13)C14—C15—H15120.2
O6—S1—O4113.57 (14)C16—C15—H15120.2
O6—S1—O5113.74 (13)C15—C16—C23117.7 (3)
O6—S1—C30107.08 (13)C15—C16—C17122.9 (3)
O5—S1—C30107.02 (12)C23—C16—C17119.4 (3)
O4—S1—C30103.99 (12)C18—C17—C16121.1 (3)
C1—N1—C11118.1 (3)C18—C17—H17119.5
C1—N1—Cd1127.3 (2)C16—C17—H17119.5
C11—N1—Cd1114.58 (19)C17—C18—C19121.2 (3)
C10—N2—C12118.4 (2)C17—C18—H18119.4
C10—N2—Cd1124.76 (19)C19—C18—H18119.4
C12—N2—Cd1116.88 (19)C20—C19—C24117.2 (3)
C13—N3—C23118.1 (3)C20—C19—C18123.0 (3)
C13—N3—Cd1125.7 (2)C24—C19—C18119.8 (3)
C23—N3—Cd1116.08 (17)C21—C20—C19120.2 (3)
C22—N4—C24118.4 (2)C21—C20—H20119.9
C22—N4—Cd1125.3 (2)C19—C20—H20119.9
C24—N4—Cd1116.19 (17)C20—C21—C22119.1 (3)
C25—O1—Cd1i118.44 (18)C20—C21—H21120.4
C27—O3—H3A105 (3)C22—C21—H21120.4
S1—O4—Cd1149.48 (13)N4—C22—C21122.9 (3)
H1A—O1W—H1B109.8 (18)N4—C22—H22118.5
N1—C1—C2123.8 (3)C21—C22—H22118.5
N1—C1—H1118.1N3—C23—C16122.3 (3)
C2—C1—H1118.1N3—C23—C24118.1 (2)
C3—C2—C1118.5 (3)C16—C23—C24119.6 (3)
C3—C2—H2120.8N4—C24—C19122.1 (3)
C1—C2—H2120.8N4—C24—C23119.0 (2)
C2—C3—C4120.6 (3)C19—C24—C23118.9 (3)
C2—C3—H3119.7O2—C25—O1124.1 (3)
C4—C3—H3119.7O2—C25—C26118.6 (3)
C3—C4—C11117.2 (3)O1—C25—C26117.3 (2)
C3—C4—C5123.7 (3)C31—C26—C27118.5 (3)
C11—C4—C5119.1 (3)C31—C26—C25120.8 (2)
C6—C5—C4121.9 (3)C27—C26—C25120.7 (3)
C6—C5—H5119.1O3—C27—C28118.6 (3)
C4—C5—H5119.1O3—C27—C26121.2 (3)
C5—C6—C7121.1 (3)C28—C27—C26120.1 (3)
C5—C6—H6119.4C29—C28—C27120.7 (3)
C7—C6—H6119.4C29—C28—H28119.7
C8—C7—C12117.8 (3)C27—C28—H28119.7
C8—C7—C6123.3 (3)C28—C29—C30119.8 (3)
C12—C7—C6118.9 (3)C28—C29—H29120.1
C9—C8—C7120.5 (3)C30—C29—H29120.1
C9—C8—H8119.8C31—C30—C29119.7 (3)
C7—C8—H8119.8C31—C30—S1119.6 (2)
C8—C9—C10118.3 (3)C29—C30—S1120.6 (2)
C8—C9—H9120.9C30—C31—C26121.1 (2)
C10—C9—H9120.9C30—C31—H31119.4
N2—C10—C9123.3 (3)C26—C31—H31119.4
O1i—Cd1—N1—C173.2 (3)Cd1—N2—C12—C7179.9 (2)
N2—Cd1—N1—C1178.1 (3)C10—N2—C12—C11179.7 (3)
O4—Cd1—N1—C1142.3 (2)Cd1—N2—C12—C110.4 (3)
N4—Cd1—N1—C18.5 (3)C8—C7—C12—N20.0 (4)
N3—Cd1—N1—C179.2 (3)C6—C7—C12—N2179.8 (3)
O1i—Cd1—N1—C11108.56 (19)C8—C7—C12—C11179.7 (3)
N2—Cd1—N1—C110.10 (18)C6—C7—C12—C110.1 (4)
O4—Cd1—N1—C1135.9 (3)N1—C11—C12—N20.5 (4)
N4—Cd1—N1—C11169.7 (2)C4—C11—C12—N2179.8 (3)
N3—Cd1—N1—C1199.0 (2)N1—C11—C12—C7179.8 (3)
O1i—Cd1—N2—C1072.5 (2)C4—C11—C12—C70.5 (4)
O4—Cd1—N2—C1013.3 (2)C23—N3—C13—C140.2 (4)
N4—Cd1—N2—C10153.8 (2)Cd1—N3—C13—C14176.0 (2)
N3—Cd1—N2—C1099.8 (2)N3—C13—C14—C150.9 (5)
N1—Cd1—N2—C10179.9 (3)C13—C14—C15—C160.7 (5)
O1i—Cd1—N2—C12107.6 (2)C14—C15—C16—C230.0 (4)
O4—Cd1—N2—C12166.6 (2)C14—C15—C16—C17179.9 (3)
N4—Cd1—N2—C1226.1 (3)C15—C16—C17—C18178.6 (3)
N3—Cd1—N2—C1280.2 (2)C23—C16—C17—C181.5 (5)
N1—Cd1—N2—C120.17 (19)C16—C17—C18—C191.7 (5)
O1i—Cd1—N3—C13146.6 (2)C17—C18—C19—C20179.7 (3)
N2—Cd1—N3—C1319.6 (2)C17—C18—C19—C240.0 (5)
O4—Cd1—N3—C1370.0 (2)C24—C19—C20—C211.9 (5)
N4—Cd1—N3—C13179.1 (2)C18—C19—C20—C21178.4 (3)
N1—Cd1—N3—C1389.6 (2)C19—C20—C21—C221.0 (5)
O1i—Cd1—N3—C2337.2 (3)C24—N4—C22—C212.4 (4)
N2—Cd1—N3—C23156.68 (18)Cd1—N4—C22—C21179.7 (2)
O4—Cd1—N3—C23113.78 (18)C20—C21—C22—N41.2 (5)
N4—Cd1—N3—C232.87 (17)C13—N3—C23—C160.5 (4)
N1—Cd1—N3—C2386.67 (18)Cd1—N3—C23—C16177.1 (2)
O1i—Cd1—N4—C2216.5 (2)C13—N3—C23—C24179.6 (2)
N2—Cd1—N4—C22121.8 (3)Cd1—N3—C23—C243.0 (3)
O4—Cd1—N4—C22100.3 (2)C15—C16—C23—N30.6 (4)
N3—Cd1—N4—C22179.5 (2)C17—C16—C23—N3179.5 (3)
N1—Cd1—N4—C2297.0 (2)C15—C16—C23—C24179.5 (3)
O1i—Cd1—N4—C24165.6 (2)C17—C16—C23—C240.4 (4)
N2—Cd1—N4—C2456.2 (3)C22—N4—C24—C191.4 (4)
O4—Cd1—N4—C2481.7 (2)Cd1—N4—C24—C19179.5 (2)
N3—Cd1—N4—C242.47 (18)C22—N4—C24—C23179.9 (2)
N1—Cd1—N4—C2480.95 (19)Cd1—N4—C24—C231.9 (3)
O6—S1—O4—Cd119.5 (3)C20—C19—C24—N40.7 (4)
O5—S1—O4—Cd1109.8 (3)C18—C19—C24—N4179.6 (3)
C30—S1—O4—Cd1135.6 (3)C20—C19—C24—C23177.8 (3)
O1i—Cd1—O4—S1175.6 (3)C18—C19—C24—C231.9 (4)
N2—Cd1—O4—S161.7 (3)N3—C23—C24—N40.8 (4)
N4—Cd1—O4—S1102.5 (3)C16—C23—C24—N4179.4 (2)
N3—Cd1—O4—S134.4 (3)N3—C23—C24—C19177.8 (2)
N1—Cd1—O4—S128.1 (4)C16—C23—C24—C192.0 (4)
C11—N1—C1—C21.3 (5)Cd1i—O1—C25—O26.8 (4)
Cd1—N1—C1—C2179.4 (2)Cd1i—O1—C25—C26172.38 (18)
N1—C1—C2—C30.3 (5)O2—C25—C26—C31173.0 (3)
C1—C2—C3—C40.8 (5)O1—C25—C26—C316.2 (4)
C2—C3—C4—C110.8 (5)O2—C25—C26—C279.5 (4)
C2—C3—C4—C5179.0 (3)O1—C25—C26—C27171.3 (3)
C3—C4—C5—C6179.2 (4)C31—C26—C27—O3179.4 (3)
C11—C4—C5—C60.6 (5)C25—C26—C27—O33.1 (5)
C4—C5—C6—C70.2 (6)C31—C26—C27—C281.5 (5)
C5—C6—C7—C8179.9 (4)C25—C26—C27—C28176.0 (3)
C5—C6—C7—C120.1 (5)O3—C27—C28—C29179.7 (3)
C12—C7—C8—C90.2 (5)C26—C27—C28—C291.1 (5)
C6—C7—C8—C9179.6 (3)C27—C28—C29—C300.1 (5)
C7—C8—C9—C100.3 (5)C28—C29—C30—C310.6 (4)
C12—N2—C10—C90.1 (5)C28—C29—C30—S1177.5 (2)
Cd1—N2—C10—C9180.0 (2)O6—S1—C30—C31166.0 (2)
C8—C9—C10—N20.3 (5)O5—S1—C30—C3171.7 (2)
C1—N1—C11—C41.2 (4)O4—S1—C30—C3145.5 (2)
Cd1—N1—C11—C4179.6 (2)O6—S1—C30—C2910.9 (3)
C1—N1—C11—C12178.0 (3)O5—S1—C30—C29111.4 (2)
Cd1—N1—C11—C120.4 (3)O4—S1—C30—C29131.4 (2)
C3—C4—C11—N10.2 (4)C29—C30—C31—C260.2 (4)
C5—C4—C11—N1180.0 (3)S1—C30—C31—C26177.1 (2)
C3—C4—C11—C12179.0 (3)C27—C26—C31—C300.9 (4)
C5—C4—C11—C120.8 (4)C25—C26—C31—C30176.7 (2)
C10—N2—C12—C70.0 (4)
Symmetry code: (i) x+1, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1B···O5ii0.85 (1)2.10 (2)2.940 (6)172 (8)
O1w—H1A···O30.85 (1)2.22 (5)2.858 (7)131 (5)
O3—H3A···O20.85 (3)1.75 (2)2.545 (4)154 (4)
Symmetry code: (ii) x+1/2, y+1/2, z+3/2.

Experimental details

Crystal data
Chemical formula[Cd2(C7H4O6S)2(C12H8N2)4]·H2O
Mr1395.96
Crystal system, space groupMonoclinic, P21/n
Temperature (K)296
a, b, c (Å)15.1984 (7), 9.8340 (4), 18.9902 (8)
β (°) 100.778 (1)
V3)2788.2 (2)
Z2
Radiation typeMo Kα
µ (mm1)0.91
Crystal size (mm)0.31 × 0.21 × 0.15
Data collection
DiffractometerBruker APEX area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2002)
Tmin, Tmax0.765, 0.875
No. of measured, independent and
observed [I > 2σ(I)] reflections
14180, 4905, 4600
Rint0.021
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.072, 1.07
No. of reflections4905
No. of parameters406
No. of restraints4
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.39, 0.33

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Cd1—O1i2.2177 (19)Cd1—N42.366 (2)
Cd1—O42.3407 (19)S1—O41.469 (2)
Cd1—N12.395 (2)S1—O51.451 (2)
Cd1—N22.330 (2)S1—O61.437 (2)
Cd1—N32.379 (2)
O1i—Cd1—O486.23 (8)N1—Cd1—N271.08 (8)
O1i—Cd1—N1112.96 (8)N1—Cd1—N382.87 (8)
O1i—Cd1—N2113.91 (8)N1—Cd1—N487.20 (8)
O1i—Cd1—N3149.14 (8)N2—Cd1—N396.01 (8)
O1i—Cd1—N483.50 (8)N2—Cd1—N4155.99 (8)
O4—Cd1—N1156.97 (8)N3—Cd1—N470.53 (8)
O4—Cd1—N289.91 (8)O5—S1—O4110.67 (13)
O4—Cd1—N386.47 (8)O6—S1—O4113.57 (14)
O4—Cd1—N4108.38 (8)O6—S1—O5113.74 (13)
Symmetry code: (i) x+1, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1B···O5ii0.849 (10)2.097 (16)2.940 (6)172 (8)
O1w—H1A···O30.850 (10)2.22 (5)2.858 (7)131 (5)
O3—H3A···O20.85 (3)1.75 (2)2.545 (4)154 (4)
Symmetry code: (ii) x+1/2, y+1/2, z+3/2.
 

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