Tetra­aqua­{1-[(1H-1,2,3-benzotriazol-1-yl)meth­yl]-1H-1,2,4-triazole}sulfato­cadmium dihydrate

Li, Y.; Li, D.; Zhao, D.

doi:10.1107/S1600536811032442

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 9| September 2011| Page m1251

doi:10.1107/S1600536811032442

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Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole}sulfatocadmium dihydrate

Yu-xian Li,^a ^* Da-wei Li ^b and Dong Zhao ^c

^aPharmacy College, Henan University of Traditional Chinese Medicine, Zhengzhou 450008, People's Republic of China, ^bZhengZhou Trade and Industry Schools, Zhengzhou 450000, People's Republic of China, and ^cDepartment of Chemistry, Zhengzhou University, Zhengzhou 450052, People's Republic of China
^*Correspondence e-mail: 13623712409@139.com

(Received 6 July 2011; accepted 10 August 2011; online 17 August 2011)

In the title complex, [Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O, the Cd^II ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand and by five O atoms from four water molecules and one monodentate sulfate anion in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.651 (12):0.349 (12) ratio. In the crystal, adjacent molecules are linked through O—H⋯O and O—H⋯N hydrogen bonds into a three-dimensional network.

Related literature

For background to complexes based on triazolyl or benzotriazolyl ligands, see: Meng et al. (2009 ); Yang et al. (2011 ).

Experimental

Crystal data

[Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M_r = 516.77
Triclinic, $[P \overline 1]$
a = 7.7154 (15) Å
b = 8.0667 (16) Å
c = 16.369 (3) Å
α = 100.12 (3)°
β = 91.64 (3)°
γ = 112.38 (3)°
V = 922.3 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.36 mm⁻¹
T = 293 K
0.19 × 0.17 × 0.14 mm

Data collection

Rigaku Saturn CCD diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ) T_min = 0.782, T_max = 0.832
8812 measured reflections
3608 independent reflections
3361 reflections with I > 2σ(I)
R_int = 0.020

Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.057
S = 1.05
3608 reflections
272 parameters
H-atom parameters constrained
Δρ_max = 0.56 e Å⁻³
Δρ_min = −0.32 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8W⋯O9	0.85	1.89	2.732 (3)	170
O6—H4W⋯O2′	0.85	2.39	2.905 (19)	119
O5—H1W⋯O4ⁱ	0.85	1.91	2.719 (4)	157
O5—H1W⋯O4′ⁱ	0.85	1.84	2.672 (7)	166
O5—H2W⋯O1ⁱⁱ	0.85	1.97	2.817 (3)	172
O8—H7W⋯O3ⁱⁱ	0.85	2.00	2.795 (4)	156
O8—H7W⋯O3′ⁱⁱ	0.85	2.38	3.127 (15)	147
O6—H3W⋯O10ⁱⁱⁱ	0.85	1.83	2.680 (3)	178
O6—H4W⋯N2^iv	0.85	2.27	3.025 (3)	148
O7—H5W⋯O3^v	0.85	1.93	2.730 (4)	157
O9—H9W⋯O4^v	0.85	2.00	2.795 (6)	155
O7—H5W⋯O3′^v	0.85	1.91	2.720 (8)	159
O9—H9W⋯O3′^v	0.85	2.06	2.844 (14)	155
O7—H6W⋯O9^vi	0.85	1.97	2.791 (3)	161
O9—H10W⋯O1^vii	0.85	2.06	2.906 (3)	175
O9—H10W⋯O4′^vii	0.85	2.48	3.030 (11)	123
O10—H11W⋯N6^viii	0.85	2.01	2.861 (3)	177
O10—H12W⋯O2^ix	0.85	2.02	2.809 (8)	155
O10—H12W⋯O4′^ix	0.85	2.19	2.944 (14)	148
O10—H12W⋯O2′^ix	0.85	2.51	3.280 (16)	151
Symmetry codes: (i) x-1, y, z; (ii) -x, -y+2, -z+1; (iii) x-1, y+1, z; (iv) x, y+1, z; (v) x-1, y-1, z; (vi) -x-1, -y+1, -z+1; (vii) -x, -y+1, -z+1; (viii) -x+1, -y+1, -z+2; (ix) x, y-1, z.

Data collection: CrystalClear (Rigaku/MSC, 2006 ); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811032442/pk2337sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811032442/pk2337Isup2.hkl

checkCIF report

Comment top

Numerous supramolecular complexes based on triazolyl or benzotriazolyl ligands which have abundant N-donor sites have been synthesized. These show a variety of discrete or infinite frameworks of one-, two-, and three-dimensional motifs (Meng et al., 2009; Yang et al., 2011). In order to further explore frameworks with new structures, we used 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole to react with CdSO₄ at room temperature and obtained the title complex [Cd(SO₄) (C₉H₈N₆) (H₂O)₄] (H₂O)₂, which is reported here. As shown in Fig. 1, the Cd^II ion is located in a distorted octahedral coordination environment and is coordinated to five oxygen atoms from four water molecules and one monodentate sulfate anion and one nitrogen atom from the 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand. Atoms O1, O6, O7, O8 and Cd1 are nearly co-planar (the mean deviation from the plane is 0.0473 Å), O5 and N1 atoms are located in the apical positions. The SO₄ tetrahedron is rotationally disordered about its S—O axis passing though O1 and S1 atoms. Intramolecular O—H···O hydrogen bonds stabilize the molecular configuration and O—H···O, O—H···N hydrogen bonds between adjacent molecules consolidate the crystal packing (Fig. 2).

Related literature top

For background to complexes based on triazolyl or benzotriazolyl ligands, see: Meng et al. (2009); Yang et al. (2011).

Experimental top

The ligand 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole (0.1 mmol) in methanol (4 ml) was added dropwise to an aqueous solution (3 ml) of cadmium sulfate (0.1 mmol). The resulting solution was allowed to stand at room temperature. After three weeks colourless crystals of good quality were obtained from the filtrate and dried in air.

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2006); cell refinement: CrystalClear (Rigaku/MSC, 2006); data reduction: CrystalClear (Rigaku/MSC, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. View of the title complex. Displacement ellipsoids are displayed at the 30% probability level. Only one orientation of the disordered SO₄^2- tetrahedron is shown.
	Fig. 2. View of hydrogen bonds in the title complex. Hydrogen bonds are indicated by dashed lines.

Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H- 1,2,4-triazole}sulfatocadmium dihydrate top

Crystal data top

[Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O	Z = 2
M_r = 516.77	F(000) = 520
Triclinic, P1	D_x = 1.861 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.7154 (15) Å	Cell parameters from 3156 reflections
b = 8.0667 (16) Å	θ = 2.5–27.9°
c = 16.369 (3) Å	µ = 1.36 mm⁻¹
α = 100.12 (3)°	T = 293 K
β = 91.64 (3)°	Prism, colourless
γ = 112.38 (3)°	0.19 × 0.17 × 0.14 mm
V = 922.3 (3) Å³

Data collection top

Rigaku Saturn CCD diffractometer	3608 independent reflections
Radiation source: fine-focus sealed tube	3361 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
Detector resolution: 28.6 pixels mm^-1	θ_max = 26.0°, θ_min = 2.5°
ω scans	h = −9→9
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −9→9
T_min = 0.782, T_max = 0.832	l = −19→20
8812 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.057	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0278P)² + 0.3915P] where P = (F_o² + 2F_c²)/3
3608 reflections	(Δ/σ)_max = 0.001
272 parameters	Δρ_max = 0.56 e Å⁻³
0 restraints	Δρ_min = −0.32 e Å⁻³

Crystal data top

[Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O	γ = 112.38 (3)°
M_r = 516.77	V = 922.3 (3) Å³
Triclinic, P1	Z = 2
a = 7.7154 (15) Å	Mo Kα radiation
b = 8.0667 (16) Å	µ = 1.36 mm⁻¹
c = 16.369 (3) Å	T = 293 K
α = 100.12 (3)°	0.19 × 0.17 × 0.14 mm
β = 91.64 (3)°

Data collection top

Rigaku Saturn CCD diffractometer	3608 independent reflections
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	3361 reflections with I > 2σ(I)
T_min = 0.782, T_max = 0.832	R_int = 0.020
8812 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.05	Δρ_max = 0.56 e Å⁻³
3608 reflections	Δρ_min = −0.32 e Å⁻³
272 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cd1	−0.08817 (2)	0.82498 (2)	0.629897 (11)	0.02758 (7)
N1	0.0196 (3)	0.6456 (3)	0.69209 (13)	0.0317 (5)
N2	0.0601 (3)	0.4169 (3)	0.73914 (14)	0.0350 (5)
N3	0.2076 (3)	0.5783 (3)	0.76785 (12)	0.0291 (4)
N4	0.3177 (3)	0.5906 (3)	0.90746 (13)	0.0326 (5)
N5	0.3149 (4)	0.7462 (3)	0.95407 (15)	0.0458 (6)
N6	0.2707 (4)	0.7145 (4)	1.02726 (15)	0.0490 (6)
O1	0.2166 (2)	0.9862 (2)	0.60171 (11)	0.0379 (4)
O2	0.3964 (14)	1.1563 (16)	0.7348 (7)	0.0486 (17)	0.651 (12)
O3	0.3456 (6)	1.3130 (5)	0.6316 (4)	0.0443 (13)	0.651 (12)
O4	0.5488 (4)	1.1527 (6)	0.6098 (3)	0.0417 (15)	0.651 (12)
O2'	0.345 (2)	1.183 (3)	0.7336 (12)	0.049 (3)	0.349 (12)
O3'	0.438 (2)	1.2932 (10)	0.6056 (5)	0.071 (4)	0.349 (12)
O4'	0.5348 (11)	1.0724 (17)	0.6482 (7)	0.078 (4)	0.349 (12)
O5	−0.1905 (3)	1.0094 (3)	0.56985 (11)	0.0386 (4)
H1W	−0.2870	1.0265	0.5864	0.058*
H2W	−0.1868	1.0155	0.5186	0.058*
O6	−0.0542 (3)	1.0205 (3)	0.75212 (11)	0.0434 (5)
H3W	−0.1547	1.0216	0.7718	0.065*
H4W	0.0211	1.1271	0.7482	0.065*
O7	−0.4009 (2)	0.6650 (3)	0.64632 (13)	0.0440 (5)
H5W	−0.4523	0.5516	0.6469	0.066*
H6W	−0.4706	0.7003	0.6187	0.066*
O8	−0.1160 (3)	0.6613 (3)	0.49667 (11)	0.0438 (5)
H7W	−0.1616	0.7013	0.4604	0.066*
H8W	−0.1814	0.5479	0.4928	0.066*
O9	−0.3463 (3)	0.2982 (3)	0.46744 (13)	0.0448 (5)
H9W	−0.4038	0.2670	0.5090	0.067*
H10W	−0.3156	0.2099	0.4472	0.067*
O10	0.6339 (3)	0.0317 (3)	0.81643 (12)	0.0507 (5)
H11W	0.6575	0.1056	0.8631	0.076*
H12W	0.5847	0.0689	0.7802	0.076*
C1	−0.0485 (4)	0.4643 (3)	0.69349 (16)	0.0334 (6)
H1A	−0.1625	0.3808	0.6645	0.040*
C2	0.1805 (4)	0.7115 (3)	0.73996 (16)	0.0351 (6)
H2A	0.2630	0.8340	0.7523	0.042*
C3	0.3661 (3)	0.5908 (4)	0.82319 (15)	0.0337 (6)
H3A	0.4006	0.4879	0.8038	0.040*
H3B	0.4740	0.7023	0.8218	0.040*
C4	0.2737 (3)	0.4545 (4)	0.95223 (15)	0.0310 (5)
C5	0.2629 (4)	0.2757 (4)	0.93464 (18)	0.0397 (6)
H5A	0.2844	0.2226	0.8828	0.048*
C6	0.2185 (4)	0.1827 (4)	0.9985 (2)	0.0536 (8)
H6A	0.2099	0.0626	0.9898	0.064*
C7	0.1853 (4)	0.2624 (5)	1.0768 (2)	0.0590 (9)
H7A	0.1538	0.1932	1.1180	0.071*
C8	0.1983 (4)	0.4385 (6)	1.09375 (19)	0.0569 (9)
H8A	0.1778	0.4914	1.1458	0.068*
C9	0.2439 (4)	0.5364 (4)	1.02929 (16)	0.0398 (6)
S1	0.38047 (8)	1.14858 (8)	0.64711 (4)	0.02752 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.02582 (10)	0.02909 (11)	0.02891 (11)	0.01048 (8)	0.00083 (7)	0.00959 (7)
N1	0.0320 (11)	0.0299 (11)	0.0327 (12)	0.0096 (9)	−0.0026 (9)	0.0116 (9)
N2	0.0355 (12)	0.0249 (11)	0.0421 (13)	0.0093 (9)	−0.0025 (10)	0.0070 (9)
N3	0.0284 (11)	0.0295 (11)	0.0292 (11)	0.0104 (9)	−0.0007 (9)	0.0081 (9)
N4	0.0379 (12)	0.0340 (12)	0.0274 (11)	0.0173 (10)	−0.0031 (9)	0.0037 (9)
N5	0.0579 (15)	0.0407 (14)	0.0426 (14)	0.0280 (12)	−0.0038 (12)	−0.0004 (11)
N6	0.0556 (15)	0.0610 (17)	0.0357 (14)	0.0349 (13)	−0.0019 (11)	−0.0035 (12)
O1	0.0281 (9)	0.0364 (10)	0.0360 (10)	0.0002 (8)	0.0014 (8)	0.0029 (8)
O2	0.052 (4)	0.061 (4)	0.030 (2)	0.019 (3)	−0.002 (3)	0.011 (2)
O3	0.050 (2)	0.0294 (17)	0.054 (3)	0.0158 (16)	−0.0026 (18)	0.0101 (17)
O4	0.0226 (15)	0.046 (2)	0.051 (3)	0.0101 (14)	0.0063 (14)	0.0032 (17)
O2'	0.051 (9)	0.055 (7)	0.027 (4)	0.014 (5)	0.002 (5)	−0.005 (4)
O3'	0.119 (10)	0.027 (4)	0.045 (4)	0.003 (5)	0.019 (5)	0.011 (3)
O4'	0.057 (5)	0.118 (8)	0.097 (7)	0.067 (5)	0.031 (5)	0.044 (7)
O5	0.0441 (11)	0.0479 (12)	0.0365 (10)	0.0281 (9)	0.0057 (8)	0.0174 (9)
O6	0.0446 (11)	0.0376 (11)	0.0372 (11)	0.0065 (9)	0.0068 (9)	0.0023 (8)
O7	0.0288 (10)	0.0359 (11)	0.0651 (13)	0.0060 (8)	0.0016 (9)	0.0205 (10)
O8	0.0536 (12)	0.0360 (11)	0.0327 (10)	0.0095 (9)	−0.0013 (9)	0.0029 (8)
O9	0.0456 (11)	0.0347 (10)	0.0569 (13)	0.0171 (9)	0.0098 (10)	0.0124 (9)
O10	0.0591 (13)	0.0506 (13)	0.0394 (11)	0.0218 (11)	0.0020 (10)	0.0013 (10)
C1	0.0322 (13)	0.0281 (13)	0.0366 (14)	0.0092 (11)	−0.0034 (11)	0.0058 (11)
C2	0.0347 (14)	0.0276 (13)	0.0388 (15)	0.0058 (11)	−0.0059 (11)	0.0123 (11)
C3	0.0294 (13)	0.0456 (16)	0.0292 (13)	0.0164 (12)	−0.0010 (11)	0.0119 (12)
C4	0.0257 (12)	0.0395 (15)	0.0285 (13)	0.0136 (11)	−0.0036 (10)	0.0078 (11)
C5	0.0399 (15)	0.0398 (15)	0.0390 (15)	0.0169 (13)	−0.0044 (12)	0.0056 (12)
C6	0.0485 (18)	0.0426 (18)	0.067 (2)	0.0112 (15)	−0.0058 (16)	0.0220 (16)
C7	0.0457 (18)	0.081 (3)	0.053 (2)	0.0164 (18)	0.0062 (15)	0.0389 (19)
C8	0.0487 (18)	0.099 (3)	0.0331 (16)	0.0346 (19)	0.0138 (14)	0.0239 (17)
C9	0.0332 (14)	0.0583 (19)	0.0291 (14)	0.0214 (14)	0.0001 (11)	0.0048 (13)
S1	0.0238 (3)	0.0256 (3)	0.0280 (3)	0.0054 (2)	0.0010 (2)	0.0029 (2)

Geometric parameters (Å, º) top

Cd1—O6	2.259 (2)	O5—H2W	0.8498
Cd1—O5	2.2733 (18)	O6—H3W	0.8501
Cd1—N1	2.282 (2)	O6—H4W	0.8500
Cd1—O8	2.300 (2)	O7—H5W	0.8500
Cd1—O7	2.3123 (19)	O7—H6W	0.8499
Cd1—O1	2.3190 (19)	O8—H7W	0.8500
N1—C2	1.317 (3)	O8—H8W	0.8500
N1—C1	1.358 (3)	O9—H9W	0.8464
N2—C1	1.309 (3)	O9—H10W	0.8508
N2—N3	1.356 (3)	O10—H11W	0.8499
N3—C2	1.322 (3)	O10—H12W	0.8500
N3—C3	1.462 (3)	C1—H1A	0.9300
N4—N5	1.357 (3)	C2—H2A	0.9300
N4—C4	1.368 (3)	C3—H3A	0.9700
N4—C3	1.440 (3)	C3—H3B	0.9700
N5—N6	1.297 (3)	C4—C9	1.385 (4)
N6—C9	1.378 (4)	C4—C5	1.390 (4)
O1—S1	1.4865 (19)	C5—C6	1.369 (4)
O2—S1	1.425 (11)	C5—H5A	0.9300
O3—S1	1.510 (3)	C6—C7	1.405 (5)
O4—S1	1.442 (3)	C6—H6A	0.9300
O2'—S1	1.45 (2)	C7—C8	1.362 (5)
O3'—S1	1.386 (7)	C7—H7A	0.9300
O4'—S1	1.535 (8)	C8—C9	1.401 (4)
O5—H1W	0.8500	C8—H8A	0.9300

O6—Cd1—O5	86.64 (7)	N3—C2—H2A	125.0
O6—Cd1—N1	92.34 (8)	N4—C3—N3	110.7 (2)
O5—Cd1—N1	178.69 (7)	N4—C3—H3A	109.5
O6—Cd1—O8	171.79 (7)	N3—C3—H3A	109.5
O5—Cd1—O8	86.05 (7)	N4—C3—H3B	109.5
N1—Cd1—O8	94.91 (8)	N3—C3—H3B	109.5
O6—Cd1—O7	90.40 (8)	H3A—C3—H3B	108.1
O5—Cd1—O7	86.24 (7)	N4—C4—C9	103.5 (2)
N1—Cd1—O7	94.59 (7)	N4—C4—C5	133.5 (2)
O8—Cd1—O7	92.85 (8)	C9—C4—C5	123.0 (3)
O6—Cd1—O1	92.83 (8)	C6—C5—C4	115.7 (3)
O5—Cd1—O1	90.09 (7)	C6—C5—H5A	122.2
N1—Cd1—O1	89.14 (7)	C4—C5—H5A	122.2
O8—Cd1—O1	83.45 (8)	C5—C6—C7	122.2 (3)
O7—Cd1—O1	174.97 (7)	C5—C6—H6A	118.9
C2—N1—C1	103.1 (2)	C7—C6—H6A	118.9
C2—N1—Cd1	122.73 (17)	C8—C7—C6	121.7 (3)
C1—N1—Cd1	134.18 (17)	C8—C7—H7A	119.2
C1—N2—N3	102.4 (2)	C6—C7—H7A	119.2
C2—N3—N2	110.2 (2)	C7—C8—C9	117.1 (3)
C2—N3—C3	128.2 (2)	C7—C8—H8A	121.5
N2—N3—C3	121.6 (2)	C9—C8—H8A	121.5
N5—N4—C4	111.0 (2)	N6—C9—C4	108.7 (2)
N5—N4—C3	118.8 (2)	N6—C9—C8	130.9 (3)
C4—N4—C3	130.2 (2)	C4—C9—C8	120.4 (3)
N6—N5—N4	107.9 (2)	O3'—S1—O2	128.0 (6)
N5—N6—C9	109.0 (2)	O3'—S1—O4	72.3 (6)
S1—O1—Cd1	135.01 (11)	O2—S1—O4	112.9 (3)
Cd1—O5—H1W	118.7	O3'—S1—O2'	118.7 (9)
Cd1—O5—H2W	124.1	O2—S1—O2'	20.7 (6)
H1W—O5—H2W	108.5	O4—S1—O2'	131.2 (6)
Cd1—O6—H3W	116.9	O3'—S1—O1	113.4 (4)
Cd1—O6—H4W	109.1	O2—S1—O1	112.7 (5)
H3W—O6—H4W	111.7	O4—S1—O1	109.03 (15)
Cd1—O7—H5W	126.0	O2'—S1—O1	108.1 (8)
Cd1—O7—H6W	109.7	O3'—S1—O3	35.5 (6)
H5W—O7—H6W	112.3	O2—S1—O3	108.7 (4)
Cd1—O8—H7W	112.7	O4—S1—O3	107.5 (2)
Cd1—O8—H8W	111.9	O2'—S1—O3	91.6 (7)
H7W—O8—H8W	109.5	O1—S1—O3	105.62 (16)
H9W—O9—H10W	105.1	O3'—S1—O4'	108.7 (6)
H11W—O10—H12W	109.9	O2—S1—O4'	83.7 (4)
N2—C1—N1	114.3 (2)	O4—S1—O4'	37.4 (4)
N2—C1—H1A	122.9	O2'—S1—O4'	104.4 (6)
N1—C1—H1A	122.9	O1—S1—O4'	101.8 (4)
N1—C2—N3	110.0 (2)	O3—S1—O4'	142.0 (5)
N1—C2—H2A	125.0

O6—Cd1—N1—C2	−52.6 (2)	N5—N4—C3—N3	−76.9 (3)
O5—Cd1—N1—C2	−14 (3)	C4—N4—C3—N3	104.2 (3)
O8—Cd1—N1—C2	123.5 (2)	C2—N3—C3—N4	99.9 (3)
O7—Cd1—N1—C2	−143.2 (2)	N2—N3—C3—N4	−78.5 (3)
O1—Cd1—N1—C2	40.2 (2)	N5—N4—C4—C9	−0.1 (3)
O6—Cd1—N1—C1	126.7 (2)	C3—N4—C4—C9	178.9 (2)
O5—Cd1—N1—C1	166 (3)	N5—N4—C4—C5	−177.7 (3)
O8—Cd1—N1—C1	−57.2 (2)	C3—N4—C4—C5	1.2 (5)
O7—Cd1—N1—C1	36.1 (2)	N4—C4—C5—C6	178.0 (3)
O1—Cd1—N1—C1	−140.6 (2)	C9—C4—C5—C6	0.7 (4)
C1—N2—N3—C2	0.9 (3)	C4—C5—C6—C7	0.2 (4)
C1—N2—N3—C3	179.5 (2)	C5—C6—C7—C8	−0.9 (5)
C4—N4—N5—N6	0.0 (3)	C6—C7—C8—C9	0.8 (5)
C3—N4—N5—N6	−179.1 (2)	N5—N6—C9—C4	−0.1 (3)
N4—N5—N6—C9	0.0 (3)	N5—N6—C9—C8	178.7 (3)
O6—Cd1—O1—S1	3.69 (17)	N4—C4—C9—N6	0.1 (3)
O5—Cd1—O1—S1	90.33 (17)	C5—C4—C9—N6	178.1 (2)
N1—Cd1—O1—S1	−88.62 (17)	N4—C4—C9—C8	−178.8 (2)
O8—Cd1—O1—S1	176.35 (17)	C5—C4—C9—C8	−0.8 (4)
O7—Cd1—O1—S1	133.4 (7)	C7—C8—C9—N6	−178.6 (3)
N3—N2—C1—N1	−0.7 (3)	C7—C8—C9—C4	0.1 (4)
C2—N1—C1—N2	0.3 (3)	Cd1—O1—S1—O3'	−118.8 (8)
Cd1—N1—C1—N2	−179.11 (17)	Cd1—O1—S1—O2	36.6 (4)
C1—N1—C2—N3	0.3 (3)	Cd1—O1—S1—O4	162.8 (3)
Cd1—N1—C2—N3	179.79 (15)	Cd1—O1—S1—O2'	15.0 (7)
N2—N3—C2—N1	−0.8 (3)	Cd1—O1—S1—O3	−82.0 (3)
C3—N3—C2—N1	−179.3 (2)	Cd1—O1—S1—O4'	124.6 (6)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8W···O9	0.85	1.89	2.732 (3)	170
O6—H4W···O2′	0.85	2.39	2.905 (19)	119
O5—H1W···O4ⁱ	0.85	1.91	2.719 (4)	157
O5—H1W···O4′ⁱ	0.85	1.84	2.672 (7)	166
O5—H2W···O1ⁱⁱ	0.85	1.97	2.817 (3)	172
O5—H2W···S1ⁱⁱ	0.85	2.89	3.616 (2)	145
O8—H7W···O3ⁱⁱ	0.85	2.00	2.795 (4)	156
O8—H7W···O3′ⁱⁱ	0.85	2.38	3.127 (15)	147
O6—H3W···O10ⁱⁱⁱ	0.85	1.83	2.680 (3)	178
O6—H4W···N2^iv	0.85	2.27	3.025 (3)	148
O7—H5W···O3^v	0.85	1.93	2.730 (4)	157
O7—H5W···S1^v	0.85	3.01	3.856 (2)	178
O9—H9W···O4^v	0.85	2.00	2.795 (6)	155
O9—H9W···S1^v	0.85	2.92	3.770 (2)	177
O7—H5W···O3′^v	0.85	1.91	2.720 (8)	159
O9—H9W···O3′^v	0.85	2.06	2.844 (14)	155
O7—H6W···O9^vi	0.85	1.97	2.791 (3)	161
O9—H10W···O1^vii	0.85	2.06	2.906 (3)	175
O9—H10W···S1^vii	0.85	2.88	3.667 (2)	155
O9—H10W···O4′^vii	0.85	2.48	3.030 (11)	123
O10—H11W···N6^viii	0.85	2.01	2.861 (3)	177
O10—H12W···O2^ix	0.85	2.02	2.809 (8)	155
O10—H12W···S1^ix	0.85	2.95	3.796 (2)	173
O10—H12W···O4′^ix	0.85	2.19	2.944 (14)	148
O10—H12W···O2′^ix	0.85	2.51	3.280 (16)	151

Symmetry codes: (i) x−1, y, z; (ii) −x, −y+2, −z+1; (iii) x−1, y+1, z; (iv) x, y+1, z; (v) x−1, y−1, z; (vi) −x−1, −y+1, −z+1; (vii) −x, −y+1, −z+1; (viii) −x+1, −y+1, −z+2; (ix) x, y−1, z.

Experimental details

Crystal data
Chemical formula	[Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M_r	516.77
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	7.7154 (15), 8.0667 (16), 16.369 (3)
α, β, γ (°)	100.12 (3), 91.64 (3), 112.38 (3)
V (Å³)	922.3 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.36
Crystal size (mm)	0.19 × 0.17 × 0.14

Data collection
Diffractometer	Rigaku Saturn CCD diffractometer
Absorption correction	Multi-scan (REQAB; Jacobson, 1998)
T_min, T_max	0.782, 0.832
No. of measured, independent and observed [I > 2σ(I)] reflections	8812, 3608, 3361
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.057, 1.05
No. of reflections	3608
No. of parameters	272
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.56, −0.32

Computer programs: CrystalClear (Rigaku/MSC, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8W···O9	0.85	1.89	2.732 (3)	170.4
O6—H4W···O2'	0.85	2.39	2.905 (19)	119.1
O5—H1W···O4ⁱ	0.85	1.91	2.719 (4)	157.4
O5—H1W···O4'ⁱ	0.85	1.84	2.672 (7)	165.6
O5—H2W···O1ⁱⁱ	0.85	1.97	2.817 (3)	172.1
O5—H2W···S1ⁱⁱ	0.85	2.89	3.616 (2)	144.8
O8—H7W···O3ⁱⁱ	0.85	2.00	2.795 (4)	155.9
O8—H7W···O3'ⁱⁱ	0.85	2.38	3.127 (15)	146.7
O6—H3W···O10ⁱⁱⁱ	0.85	1.83	2.680 (3)	178.1
O6—H4W···N2^iv	0.85	2.27	3.025 (3)	147.5
O7—H5W···O3^v	0.85	1.93	2.730 (4)	156.6
O7—H5W···S1^v	0.85	3.01	3.856 (2)	177.7
O9—H9W···O4^v	0.85	2.00	2.795 (6)	155.0
O9—H9W···S1^v	0.85	2.92	3.770 (2)	177.2
O7—H5W···O3'^v	0.85	1.91	2.720 (8)	158.9
O9—H9W···O3'^v	0.85	2.06	2.844 (14)	154.7
O7—H6W···O9^vi	0.85	1.97	2.791 (3)	161.3
O9—H10W···O1^vii	0.85	2.06	2.906 (3)	174.7
O9—H10W···S1^vii	0.85	2.88	3.667 (2)	155.2
O9—H10W···O4'^vii	0.85	2.48	3.030 (11)	123.1
O10—H11W···N6^viii	0.85	2.01	2.861 (3)	176.7
O10—H12W···O2^ix	0.85	2.02	2.809 (8)	154.9
O10—H12W···S1^ix	0.85	2.95	3.796 (2)	172.6
O10—H12W···O4'^ix	0.85	2.19	2.944 (14)	147.6
O10—H12W···O2'^ix	0.85	2.51	3.280 (16)	151.2

References

Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. Google Scholar
Meng, X.-R., Jin, S.-Z., Hou, H.-W., Du, C.-X. & Ng, S. W. (2009). Inorg. Chim. Acta, 362, 1519–1527. CrossRef CAS Google Scholar
Rigaku/MSC (2006). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yang, H., Zhang, J. & Zhao, D. (2011). Acta Cryst. E67, m602. Google Scholar

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Volume 67| Part 9| September 2011| Page m1251

doi:10.1107/S1600536811032442

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Tetra­aqua­{1-[(1H-1,2,3-benzotriazol-1-yl)meth­yl]-1H-1,2,4-triazole}sulfato­cadmium dihydrate

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Experimental

Crystal data

Data collection

Refinement

Supporting information

References

metal-organic compounds

Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole}sulfatocadmium dihydrate