Literature DB >> 21200590

catena-Poly[bis-(sulfamethoxazolium) [[trichloridocadmate(II)]-μ-chlorido] monohydrate].

Annamalai Subashini, Packianathan Thomas Muthiah, Gabriele Bocelli, Andrea Cantoni.   

Abstract

In the title compound, {(C(10)H(12)N(3)O(3)S)(2)[CdCl(4)]·H(2)O}(n), the Cd(II) atom is five-coordinate with a distorted trigonal-bipyramidal geometry formed by chloride ions. The Cd atom and two of the Cl atoms lie on a mirror plane. The cation is protonated on the amino group N atom; it is not coordinated to cadmium, but is hydrogen bonded to the chlorido ligands. Each water mol-ecule bridges two chlorido ligands, generating ring motifs along the -Cd-Cl-Cd- chains. The isoxazole unit and the amide groups are linked through a pair of N-H⋯N hydrogen bonds. The crystal structure is stabilized by N-H⋯O, O-H⋯Cl, C-H⋯N, N-H⋯Cl and C-H⋯O hydrogen bonds.

Entities:  

Year:  2007        PMID： 21200590      PMCID： PMC2915166          DOI： 10.1107/S1600536807067190

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related literature, see: Abramenko & Sergienko (2002 ▶); Bettinetti et al. (1982 ▶); Dai et al. (2002 ▶); Fawcett et al. (1978 ▶); Haridas et al. (1984 ▶); Kagi & Vallee (1960 ▶); Kálmán et al. (1981 ▶); Kendi et al. (2000 ▶); Schaffers & Keszler (1993 ▶); Singh et al. (1984 ▶); Subashini et al. (2007 ▶); Subha Nandhini et al. (2002 ▶); Takasuka & Nakai (2001 ▶); Tao et al. (2003 ▶); Yukawa et al. (1982 ▶).

Experimental

Crystal data

(C10H12N3O3S)2[CdCl4]·H2O M = 780.82 Orthorhombic, a = 15.088 (2) Å b = 35.028 (3) Å c = 5.562 (3) Å V = 2939.5 (17) Å3 Z = 4 Cu Kα radiation μ = 11.07 mm−1 T = 293 K 0.19 × 0.16 × 0.14 mm

Data collection

Siemens AED single-crystal diffractometer Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.227, T max = 0.306 (expected range = 0.157–0.212) 2834 measured reflections 2834 independent reflections 2470 reflections with I > 2σ(I)

Refinement

R[F 2 > 2σ(F 2)] = 0.041 wR(F 2) = 0.111 S = 1.05 2834 reflections 203 parameters 4 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.04 e Å−3 Δρmin = −0.64 e Å−3 Data collection: local program (Belletti et al., 1993 ▶); cell refinement: local program; data reduction: local program; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: PLATON (Spek, 2003 ▶); software used to prepare material for publication: PLATON. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807067190/fi2052sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067190/fi2052Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
(C10H12N3O3S)2[CdCl4]·H2OF000 = 1568
Mr = 780.82Dx = 1.764 Mg m−3
Orthorhombic, PnmaCu Kα radiation λ = 1.54178 Å
Hall symbol: -P 2ac 2nCell parameters from 45 reflections
a = 15.088 (2) Åθ = 5.1–70.1º
b = 35.028 (3) ŵ = 11.07 mm−1
c = 5.562 (3) ÅT = 293 K
V = 2939.5 (17) Å3Prism-like, light-brown
Z = 40.19 × 0.16 × 0.14 mm
Siemens AED single-crystal diffractometer2834 independent reflections
Radiation source: fine- focus sealed tube2470 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.0000
T = 293 Kθmax = 70.1º
ω–2θ scansθmin = 5.1º
Absorption correction: ψ scan(North et al., 1968)h = −2→18
Tmin = 0.227, Tmax = 0.306k = −2→42
2834 measured reflectionsl = −6→6
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.111  w = 1/[σ2(Fo2) + (0.0706P)2 + 2.0804P] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
2834 reflectionsΔρmax = 1.04 e Å−3
203 parametersΔρmin = −0.64 e Å−3
4 restraintsExtinction correction: shelxl, FC*=KFC[1+0.001XFC2Λ3/SIN(2Θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00108 (10)
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles
Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2> σ(F2) is used only for calculating -R-factor-obs 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.
xyzUiso*/Ueq
S10.47494 (5)0.09076 (2)0.89098 (17)0.0348 (3)
O10.54498 (17)0.11258 (8)0.7896 (6)0.0526 (9)
O20.47844 (16)0.07794 (8)1.1338 (5)0.0433 (8)
O30.34703 (17)−0.03052 (8)0.6783 (5)0.0465 (8)
N40.1435 (2)0.18175 (9)0.7834 (6)0.0367 (9)
N70.46903 (19)0.05310 (9)0.7171 (5)0.0383 (9)
N80.39733 (19)−0.00044 (9)0.5779 (6)0.0450 (10)
C10.3753 (2)0.11622 (9)0.8542 (6)0.0311 (8)
C20.3077 (2)0.11213 (9)1.0198 (6)0.0376 (9)
C30.2303 (2)0.13307 (10)0.9951 (6)0.0380 (10)
C40.2224 (2)0.15783 (9)0.8048 (6)0.0322 (9)
C50.2887 (2)0.16153 (10)0.6346 (7)0.0400 (10)
C60.3658 (2)0.14054 (10)0.6588 (6)0.0403 (10)
C80.4174 (2)0.02120 (9)0.7613 (6)0.0315 (8)
C90.3822 (2)0.00750 (9)0.9784 (6)0.0348 (9)
C100.3395 (2)−0.02479 (9)0.9160 (6)0.0345 (9)
C110.2894 (3)−0.05362 (11)1.0534 (8)0.0500 (11)
Cd10.47373 (2)0.250001.18772 (7)0.0430 (1)
Cl10.48401 (11)0.250000.7087 (2)0.0541 (5)
Cl20.54023 (7)0.18534 (3)1.21780 (16)0.0511 (3)
Cl30.31017 (11)0.250001.2016 (3)0.0795 (7)
O1W0.2295 (3)0.250001.7017 (8)0.0513 (14)
H20.314200.095301.147900.0450*
H30.184400.130401.105600.0460*
H4A0.119 (3)0.1815 (15)0.938 (10)0.073 (15)*
H4B0.165 (3)0.2055 (13)0.753 (7)0.046 (11)*
H4C0.118 (3)0.1707 (14)0.666 (7)0.076 (17)*
H50.281500.178000.505000.0480*
H60.410800.142700.545400.0480*
H70.500500.053200.588200.0460*
H90.387200.018301.130600.0420*
H11A0.22950−0.054600.995800.0750*
H11B0.28950−0.046901.220700.0750*
H11C0.31670−0.078201.033100.0750*
H1W0.267500.250001.839400.13 (4)*
H2W0.265300.250001.560400.08 (2)*
U11U22U33U12U13U23
S10.0272 (4)0.0305 (4)0.0468 (5)0.0038 (3)−0.0006 (3)−0.0050 (3)
O10.0300 (12)0.0449 (15)0.083 (2)−0.0033 (11)0.0069 (12)−0.0036 (14)
O20.0447 (13)0.0426 (14)0.0427 (13)0.0104 (11)−0.0108 (11)−0.0063 (11)
O30.0442 (14)0.0511 (15)0.0441 (14)−0.0099 (12)0.0004 (11)−0.0139 (11)
N40.0343 (15)0.0302 (15)0.0456 (18)0.0058 (12)−0.0034 (13)−0.0003 (13)
N70.0427 (16)0.0326 (15)0.0395 (15)0.0050 (11)0.0113 (12)−0.0059 (12)
N80.0426 (15)0.0549 (19)0.0374 (16)−0.0080 (14)0.0044 (13)−0.0087 (14)
C10.0283 (14)0.0255 (14)0.0394 (16)0.0020 (12)0.0004 (12)−0.0023 (12)
C20.0384 (16)0.0345 (16)0.0400 (17)0.0067 (14)0.0072 (14)0.0087 (14)
C30.0338 (16)0.0388 (17)0.0415 (17)0.0041 (13)0.0080 (14)0.0067 (14)
C40.0295 (15)0.0242 (15)0.0428 (17)0.0005 (11)−0.0017 (13)−0.0026 (12)
C50.0436 (18)0.0335 (16)0.0429 (17)0.0035 (14)0.0070 (15)0.0110 (15)
C60.0387 (17)0.0375 (18)0.0447 (19)0.0020 (14)0.0112 (15)0.0072 (15)
C80.0287 (14)0.0343 (15)0.0314 (15)0.0091 (12)−0.0009 (12)−0.0036 (13)
C90.0388 (16)0.0329 (16)0.0328 (16)0.0068 (13)−0.0004 (13)−0.0014 (13)
C100.0292 (14)0.0356 (16)0.0388 (17)0.0064 (12)−0.0008 (13)−0.0018 (14)
C110.0441 (19)0.045 (2)0.061 (2)−0.0010 (16)0.0025 (18)0.0030 (18)
Cd10.0368 (2)0.0306 (2)0.0615 (3)0.00000.0019 (2)0.0000
Cl10.0672 (9)0.0529 (8)0.0422 (7)0.00000.0054 (6)0.0000
Cl20.0724 (6)0.0427 (5)0.0383 (5)0.0192 (4)0.0009 (4)−0.0018 (4)
Cl30.0402 (7)0.1403 (19)0.0581 (9)0.00000.0057 (6)0.0000
O1W0.052 (2)0.037 (2)0.065 (3)0.00000.000 (2)0.0000
Cd1—Cl22.4828 (17)N7—H70.8599
Cd1—Cl32.469 (2)C1—C61.388 (5)
Cd1—Cl1i2.902 (2)C1—C21.382 (5)
Cd1—Cl2ii2.4828 (17)C2—C31.386 (4)
Cd1—Cl12.6688 (19)C3—C41.374 (5)
S1—C11.760 (3)C4—C51.383 (5)
S1—O11.421 (3)C5—C61.383 (5)
S1—O21.424 (3)C8—C91.404 (5)
S1—N71.638 (3)C9—C101.347 (4)
O3—N81.413 (4)C10—C111.475 (5)
O3—C101.342 (4)C2—H20.9299
O1W—H1W0.9567C3—H30.9306
O1W—H2W0.9536C5—H50.9296
N4—C41.461 (4)C6—H60.9298
N7—C81.384 (4)C9—H90.9303
N8—C81.306 (5)C11—H11A0.9595
N4—H4A0.94 (5)C11—H11B0.9598
N4—H4B0.91 (5)C11—H11C0.9611
N4—H4C0.85 (4)
Cd1···H1Wiii3.6654N8···H7xi2.5778
Cd1···H2W3.7665C3···O1xii3.293 (5)
Cd1···H4Aiv3.86 (5)C4···O1xii3.155 (4)
Cd1···H4Av3.86 (5)C4···O1Wvi3.281 (4)
Cd1···H1Wvi3.6654C4···O1Wiii3.281 (4)
Cd1···H2Wii3.7665C5···O1Wvi3.247 (4)
Cl1···Cd1iii2.902 (2)C5···O1Wiii3.247 (4)
Cl1···N4vii3.392 (4)C8···C11xv3.516 (6)
Cl1···N4viii3.392 (4)C8···N8xi3.450 (5)
Cl1···Cl2iii3.648 (2)C8···C9x3.500 (5)
Cl2···N4vii3.196 (4)C9···O22.991 (4)
Cl2···N4v3.184 (4)C9···N8i3.354 (5)
Cl3···O1Wiii3.035 (5)C9···C8x3.500 (5)
Cl3···O1Wvi3.035 (5)C10···O2x3.330 (4)
Cl3···O1Wii3.036 (5)C11···C8xvi3.516 (6)
Cl3···O1W3.036 (5)C11···N8xvi3.397 (6)
Cl2···H3v3.0659C11···O1x3.357 (5)
Cl2···H4Cvii2.49 (4)C8···H11Axv2.9089
Cl2···H4Av2.26 (5)H1W···H4Bi2.2477
Cl2···H6i3.0601H1W···Cd1i3.6654
Cl3···H1Wiii2.1149H1W···H4Bix2.2477
Cl3···H2W2.1074H1W···Cl3i2.1149
Cl3···H5i3.0652H1W···Cl3i2.1149
Cl3···H5ix3.0652H1W···Cd1i3.6654
Cl3···H2Wii2.1074H2···O22.5528
Cl3···H1Wvi2.1149H2···H11Axvi2.4923
S1···H93.1577H2W···Cd13.7665
O1···C11x3.357 (5)H2W···Cl32.1074
O1···C3vii3.293 (5)H2W···H4Bix2.4223
O1···N4vii2.871 (4)H2W···H5ix2.5525
O1···C4vii3.155 (4)H2W···Cl32.1074
O1W···N4i2.758 (4)H2W···H4Bi2.4223
O1W···C4i3.281 (4)H2W···H5i2.5525
O1W···Cl3i3.035 (5)H2W···Cd13.7665
O1W···Cl33.036 (5)H3···H4A2.2464
O1W···C5ix3.247 (4)H3···Cl2xiv3.0659
O1W···C5i3.247 (4)H4A···H32.2464
O1W···Cl3i3.035 (5)H4A···Cd1xiv3.86 (5)
O1W···N4ix2.758 (4)H4A···Cl2xiv2.26 (5)
O1W···Cl33.036 (5)H4A···Cd1xvii3.86 (5)
O1W···C4ix3.281 (4)H4B···H52.4332
O2···C92.991 (4)H4B···O1Wvi1.86 (5)
O2···C10x3.330 (4)H4B···O1Wiii1.86 (5)
O1···H4Cvii2.33 (5)H4B···H1Wiii2.2477
O1···H11Cx2.6035H4B···H2Wiii2.4223
O1···H62.6564H4B···H1Wvi2.2477
O1W···H5ix2.8589H4B···H2Wvi2.4223
O1W···H5i2.8589H4C···Cl2xii2.49 (4)
O1W···H4Bix1.86 (5)H4C···O1xii2.33 (5)
O1W···H4Bi1.86 (5)H5···H2Wiii2.5525
O2···H7i2.6925H5···Cl3iii3.0652
O2···H22.5528H5···O1Wiii2.8589
O2···H92.5019H5···Cl3vi3.0652
O3···H11Biii2.7496H5···O1Wvi2.8589
O3···H7xi2.8496H5···H4B2.4332
N4···Cl1xii3.392 (4)H5···H2Wvi2.5525
N4···Cl2xii3.196 (4)H6···O12.6564
N4···Cl1xiii3.392 (4)H6···Cl2iii3.0601
N4···O1xii2.871 (4)H7···O3xi2.8496
N4···O1Wvi2.758 (4)H7···N8xi2.5778
N4···Cl2xiv3.184 (4)H7···O2iii2.6925
N4···O1Wiii2.758 (4)H9···O22.5019
N7···N8xi3.188 (5)H9···N8i2.5776
N8···C8xi3.450 (5)H9···S13.1577
N8···C9iii3.354 (5)H11A···N8xvi2.7545
N8···N7xi3.188 (5)H11A···C8xvi2.9089
N8···C11xv3.397 (6)H11A···H2xv2.4923
N8···N8xi3.217 (4)H11B···O3i2.7496
N8···H11Axv2.7545H11C···O1x2.6035
N8···H9iii2.5776
Cl1—Cd1—Cl2ii92.51 (3)S1—C1—C2120.0 (2)
Cl2—Cd1—Cl3113.69 (3)C1—C2—C3120.1 (3)
Cl1i—Cd1—Cl284.90 (3)C2—C3—C4118.9 (3)
Cl2—Cd1—Cl2ii131.63 (4)N4—C4—C3119.7 (3)
Cl1—Cd1—Cl292.51 (3)C3—C4—C5121.6 (3)
Cl1—Cd1—Cl395.12 (5)N4—C4—C5118.7 (3)
Cl1—Cd1—Cl1i173.60 (5)C4—C5—C6119.5 (3)
Cl1i—Cd1—Cl2ii84.90 (3)C1—C6—C5119.3 (3)
Cl1i—Cd1—Cl391.27 (5)N7—C8—C9129.9 (3)
Cl2ii—Cd1—Cl3113.69 (3)N8—C8—C9112.7 (3)
Cd1—Cl1—Cd1vi173.60 (7)N7—C8—N8117.4 (3)
O1—S1—N7103.85 (17)C8—C9—C10104.3 (3)
O1—S1—C1108.46 (16)C9—C10—C11133.4 (3)
O2—S1—N7107.94 (16)O3—C10—C11116.8 (3)
O1—S1—O2121.22 (17)O3—C10—C9109.8 (3)
O2—S1—C1107.56 (16)C1—C2—H2119.91
N7—S1—C1107.03 (15)C3—C2—H2120.02
N8—O3—C10108.9 (3)C2—C3—H3120.56
H1W—O1W—H2W108.68C4—C3—H3120.52
S1—N7—C8125.2 (2)C6—C5—H5120.25
O3—N8—C8104.4 (3)C4—C5—H5120.28
H4A—N4—H4C121 (4)C1—C6—H6120.37
C4—N4—H4A104 (3)C5—C6—H6120.33
H4B—N4—H4C116 (4)C8—C9—H9127.81
H4A—N4—H4B109 (4)C10—C9—H9127.93
C4—N4—H4B104 (3)H11B—C11—H11C109.45
C4—N4—H4C100 (3)H11A—C11—H11B109.51
C8—N7—H7117.52H11A—C11—H11C109.42
S1—N7—H7117.31C10—C11—H11A109.53
S1—C1—C6119.3 (2)C10—C11—H11B109.49
C2—C1—C6120.6 (3)C10—C11—H11C109.44
O1—S1—N7—C8171.7 (3)O3—N8—C8—C9−0.8 (4)
O2—S1—N7—C841.8 (3)S1—C1—C6—C5−177.8 (3)
C1—S1—N7—C8−73.7 (3)S1—C1—C2—C3178.0 (3)
O1—S1—C1—C2−150.0 (3)C6—C1—C2—C3−1.5 (5)
O1—S1—C1—C629.6 (3)C2—C1—C6—C51.7 (5)
O2—S1—C1—C2−17.2 (3)C1—C2—C3—C4−0.2 (5)
O2—S1—C1—C6162.3 (3)C2—C3—C4—N4−176.5 (3)
N7—S1—C1—C298.6 (3)C2—C3—C4—C51.8 (5)
N7—S1—C1—C6−81.9 (3)C3—C4—C5—C6−1.6 (5)
N8—O3—C10—C11−179.5 (3)N4—C4—C5—C6176.7 (3)
C10—O3—N8—C80.5 (3)C4—C5—C6—C1−0.2 (5)
N8—O3—C10—C90.0 (4)N8—C8—C9—C100.8 (4)
S1—N7—C8—N8158.6 (3)N7—C8—C9—C10−178.6 (3)
S1—N7—C8—C9−22.0 (5)C8—C9—C10—O3−0.5 (4)
O3—N8—C8—N7178.7 (3)C8—C9—C10—C11178.9 (4)
D—H···AD—HH···AD···AD—H···A
O1W—H1W···Cl3i0.962.113.035 (5)161
O1W—H2W···Cl30.952.113.036 (5)164
N4—H4A···Cl2xiv0.94 (5)2.26 (5)3.184 (4)171 (4)
N4—H4B···O1Wiii0.91 (5)1.86 (5)2.758 (4)169 (4)
N4—H4B···O1Wvi0.91 (5)1.86 (5)2.758 (4)169 (4)
N4—H4C···Cl2xii0.85 (4)2.49 (4)3.196 (4)141 (4)
N4—H4C···O1xii0.85 (4)2.33 (5)2.871 (4)122 (4)
N7—H7···N8xi0.862.583.188 (5)129
C2—H2···O20.932.552.911 (4)103
C9—H9···O20.932.502.991 (4)113
C9—H9···N8i0.932.583.354 (5)141
Cd1—Cl22.4828 (17)
Cd1—Cl32.469 (2)
Cd1—Cl1i2.902 (2)
Cd1—Cl2ii2.4828 (17)
Cd1—Cl12.6688 (19)
Cl1—Cd1—Cl2ii92.51 (3)
Cl2—Cd1—Cl3113.69 (3)
Cl1i—Cd1—Cl284.90 (3)
Cl2—Cd1—Cl2ii131.63 (4)
Cl1—Cd1—Cl292.51 (3)
Cl1—Cd1—Cl395.12 (5)
Cl1—Cd1—Cl1i173.60 (5)
Cl1i—Cd1—Cl2ii84.90 (3)
Cl1i—Cd1—Cl391.27 (5)
Cl2ii—Cd1—Cl3113.69 (3)
Cd1—Cl1—Cd1iii173.60 (7)

Symmetry codes: (i) ; (ii) ; (iii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—H1W⋯Cl3i0.962.113.035 (5)161
O1W—H2W⋯Cl30.952.113.036 (5)164
N4—H4A⋯Cl2iv0.94 (5)2.26 (5)3.184 (4)171 (4)
N4—H4B⋯O1Wv0.91 (5)1.86 (5)2.758 (4)169 (4)
N4—H4B⋯O1Wiii0.91 (5)1.86 (5)2.758 (4)169 (4)
N4—H4C⋯Cl2vi0.85 (4)2.49 (4)3.196 (4)141 (4)
N4—H4C⋯O1vi0.85 (4)2.33 (5)2.871 (4)122 (4)
N7—H7⋯N8vii0.862.583.188 (5)129
C2—H2⋯O20.932.552.911 (4)103
C9—H9⋯O20.932.502.991 (4)113
C9—H9⋯N8i0.932.583.354 (5)141

Symmetry codes: (i) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

  3 in total

1.  Flavone-3'-sulfonamide.

Authors:  E Kendi; S Ozbey; O Bozdağ; R Ertan
Journal:  Acta Crystallogr C       Date:  2000-04-15       Impact factor: 1.172

2.  Metallothionein: a cadmium- and zinc-containing protein from equine renal cortex.

Authors:  J H KAGI; B L VALEE
Journal:  J Biol Chem       Date:  1960-12       Impact factor: 5.157

3.  Synthesis, structure, and fluorescence of the novel cadmium(II)-trimesate coordination polymers with different coordination architectures.

Authors:  Jing-Cao Dai; Xin-Tao Wu; Zhi-Yong Fu; Chuan-Peng Cui; Sheng-Min Hu; Wen-Xin Du; Li-Ming Wu; Han-Hui Zhang; Rui-Qing Sun
Journal:  Inorg Chem       Date:  2002-03-25       Impact factor: 5.165
  3 in total

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