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

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

doi:10.1107/S1600536811027231

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 8| August 2011| Page m1078

doi:10.1107/S1600536811027231

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Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole}sulfatocobalt(II) 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 27 June 2011; accepted 7 July 2011; online 13 July 2011)

In the title complex, [Co(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O, the Co^II ion is six-coordinated by one N atom from a 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand, one O atom from a monodentate sulfate ligand and four water molecules in a slightly distorted octahedral geometry. The sulfate ligand is rotationally disordered over two sets of sites with refined occupancies of 0.662 (15) and 0.338 (15). In the crystal, complex molecules and solvent water molecules are linked through intermolecular O—H⋯O and O—H⋯N hydrogen bonds into a three-dimensional network.

Related literature

For background to complexes constructed from N-heterocyclic ligands, see: Tian et al. (2010 ); Shi et al. (2010 ).

Experimental

Crystal data

[Co(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M_r = 463.30
Triclinic, $[P \overline 1]$
a = 7.5471 (15) Å
b = 7.9415 (16) Å
c = 16.198 (3) Å
α = 99.79 (3)°
β = 92.32 (3)°
γ = 112.22 (3)°
V = 879.8 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 293 K
0.21 × 0.19 × 0.16 mm

Data collection

Rigaku Saturn diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006 ) T_min = 0.793, T_max = 0.836
10814 measured reflections
4158 independent reflections
3868 reflections with I > 2σ(I)
R_int = 0.019

Refinement

R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.069
S = 1.04
4158 reflections
272 parameters
H-atom parameters constrained
Δρ_max = 0.37 e Å⁻³
Δρ_min = −0.36 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H1W⋯O4′	0.85	2.38	2.823 (13)	113
O5—H1W⋯N2ⁱ	0.85	2.31	3.081 (2)	150
O5—H2W⋯O10ⁱⁱ	0.85	1.83	2.672 (2)	173
O6—H3W⋯O9ⁱⁱⁱ	0.85	1.95	2.798 (2)	171
O6—H4W⋯O2′^iv	0.85	1.95	2.784 (7)	167
O6—H4W⋯O2^iv	0.85	1.96	2.777 (4)	160
O7—H5W⋯O2^v	0.85	1.94	2.771 (4)	167
O7—H5W⋯O2′^v	0.85	2.15	2.961 (11)	159
O7—H6W⋯O9^vi	0.85	1.89	2.728 (2)	168
O8—H8W⋯O3′^vi	0.85	1.86	2.681 (7)	162
O8—H8W⋯O3^vi	0.85	1.87	2.715 (3)	170
O8—H7W⋯O1^v	0.85	1.99	2.8246 (18)	167
O9—H9W⋯O3^vii	0.85	1.95	2.768 (6)	162
O9—H9W⋯O2′^vii	0.85	2.19	2.911 (15)	142
O10—H11W⋯O4^vii	0.85	1.97	2.809 (7)	168
O10—H11W⋯O4′^vii	0.85	2.39	3.209 (16)	163
O10—H11W⋯O3′^vii	0.85	2.39	2.996 (17)	129
O9—H10W⋯O1^viii	0.85	2.11	2.945 (2)	166
O10—H12W⋯N6^ix	0.85	2.00	2.853 (2)	177
Symmetry codes: (i) x, y+1, z; (ii) x-1, y+1, z; (iii) -x, -y+1, -z+1; (iv) x-1, y-1, z; (v) -x, -y+2, -z+1; (vi) x-1, y, z; (vii) x, y-1, z; (viii) -x+1, -y+1, -z+1; (ix) -x+1, -y+1, -z+2.

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/S1600536811027231/lh5272sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811027231/lh5272Isup2.hkl

checkCIF report

Comment top

Numerous one-, two- and three dimensional complexes constructed from N-heterocyclic ligands have been synthesized (Tian et al., 2010; Shi et al., 2010). To further explore frameworks with new structures, we used 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole which has abundant N-donor sites to self-assembly with CoSO₄ and obtained the title complex of which the crystal structure is reported herein. As shown in Figure 1, the Co^II ion is in a slightly distorted octahedral coordination environment defined by five oxygen atoms, four from water molecules and one from monodentate sulfate ligand and one nitrogen atom from a 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand. Atoms O1, O5, O6, O7 and Co1 are essentially co-planar (the mean deviation from the plane is 0.0238 Å). Atom O8 and N1 atoms are located in the apical sites. The SO₄ ligand is rotationally disordered about an S—O bond passing though atoms O1 and S1. In the crystal, complex molecules and solvent water molecules linked through intermolecular O—H···O and O—H···N hydrogen bonds into a three-dimensional network (Figure 2).

Related literature top

For background to complexes constructed from N-heterocyclic ligands, see: Tian et al. (2010); Shi et al. (2010).

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 (2 ml) of cobalt sulfate (0.1 mmol). The resulting solution was allowed to stand at room temperature. After three weeks good quality red crystals 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 asymmetric unit of the title complex with displacement ellipsoids displayed at the 30% probability level. H atoms are omitted for clarity. Only one component of the disordered SO₄ ligand is shown.
	Fig. 2. Part of the crystal structure with hydrogen bonds indicated by dashed lines.

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

Crystal data top

[Co(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O	Z = 2
M_r = 463.30	F(000) = 478
Triclinic, P1	D_x = 1.749 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.5471 (15) Å	Cell parameters from 3052 reflections
b = 7.9415 (16) Å	θ = 2.6–27.9°
c = 16.198 (3) Å	µ = 1.16 mm⁻¹
α = 99.79 (3)°	T = 293 K
β = 92.32 (3)°	Prism, red
γ = 112.22 (3)°	0.21 × 0.19 × 0.16 mm
V = 879.8 (3) Å³

Data collection top

Rigaku Saturn diffractometer	4158 independent reflections
Radiation source: fine-focus sealed tube	3868 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.019
Detector resolution: 28.5714 pixels mm^-1	θ_max = 27.9°, θ_min = 2.6°
ω scans	h = −9→9
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006)	k = −10→10
T_min = 0.793, T_max = 0.836	l = −21→19
10814 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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.069	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0299P)² + 0.4582P] where P = (F_o² + 2F_c²)/3
4158 reflections	(Δ/σ)_max = 0.001
272 parameters	Δρ_max = 0.37 e Å⁻³
0 restraints	Δρ_min = −0.36 e Å⁻³

Crystal data top

[Co(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O	γ = 112.22 (3)°
M_r = 463.30	V = 879.8 (3) Å³
Triclinic, P1	Z = 2
a = 7.5471 (15) Å	Mo Kα radiation
b = 7.9415 (16) Å	µ = 1.16 mm⁻¹
c = 16.198 (3) Å	T = 293 K
α = 99.79 (3)°	0.21 × 0.19 × 0.16 mm
β = 92.32 (3)°

Data collection top

Rigaku Saturn diffractometer	4158 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006)	3868 reflections with I > 2σ(I)
T_min = 0.793, T_max = 0.836	R_int = 0.019
10814 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	0 restraints
wR(F²) = 0.069	H-atom parameters constrained
S = 1.04	Δρ_max = 0.37 e Å⁻³
4158 reflections	Δρ_min = −0.36 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)
Co1	−0.08883 (3)	0.83076 (3)	0.627602 (13)	0.02224 (7)
N1	0.0089 (2)	0.65836 (19)	0.68655 (9)	0.0277 (3)
N2	0.0484 (2)	0.4200 (2)	0.73017 (10)	0.0328 (3)
N3	0.1979 (2)	0.58276 (19)	0.76299 (9)	0.0267 (3)
N4	0.3108 (2)	0.5942 (2)	0.90460 (9)	0.0305 (3)
N5	0.3118 (3)	0.7536 (2)	0.95135 (11)	0.0401 (4)
N6	0.2705 (3)	0.7243 (3)	1.02609 (11)	0.0426 (4)
O1	0.19941 (16)	0.98544 (16)	0.60342 (7)	0.0298 (3)
O2	0.3506 (7)	1.3182 (4)	0.6265 (3)	0.0383 (9)	0.662 (15)
O3	0.5396 (3)	1.1350 (6)	0.6050 (3)	0.0360 (11)	0.662 (15)
O4	0.4014 (9)	1.1668 (11)	0.7346 (4)	0.0379 (10)	0.662 (15)
O2'	0.4176 (19)	1.2967 (10)	0.6045 (5)	0.047 (2)	0.338 (15)
O3'	0.5343 (8)	1.0771 (14)	0.6418 (9)	0.060 (3)	0.338 (15)
O4'	0.3471 (18)	1.181 (2)	0.7357 (9)	0.045 (3)	0.338 (15)
O5	−0.05411 (19)	1.01086 (18)	0.74101 (8)	0.0364 (3)
H1W	0.0162	1.1247	0.7437	0.044*
H2W	−0.1552	1.0065	0.7635	0.044*
O6	−0.38083 (17)	0.68003 (17)	0.64472 (9)	0.0357 (3)
H3W	−0.4664	0.6946	0.6144	0.043*
H4W	−0.4390	0.5635	0.6404	0.043*
O7	−0.11655 (19)	0.67039 (17)	0.50698 (8)	0.0334 (3)
H5W	−0.1783	0.6924	0.4680	0.040*
H6W	−0.1752	0.5533	0.4998	0.040*
O8	−0.18197 (18)	1.00403 (18)	0.57005 (8)	0.0324 (3)
H7W	−0.1737	1.0251	0.5203	0.039*
H8W	−0.2657	1.0454	0.5869	0.039*
O9	0.65865 (19)	0.29975 (18)	0.46850 (9)	0.0384 (3)
H9W	0.6003	0.2531	0.5081	0.046*
H10W	0.7165	0.2280	0.4539	0.046*
O10	0.6405 (2)	0.0290 (2)	0.81395 (9)	0.0430 (3)
H11W	0.5841	0.0841	0.7891	0.052*
H12W	0.6696	0.1011	0.8620	0.052*
C1	−0.0606 (3)	0.4727 (2)	0.68424 (11)	0.0320 (4)
H1A	−0.1758	0.3899	0.6528	0.038*
C2	0.1713 (3)	0.7220 (2)	0.73708 (11)	0.0321 (4)
H2A	0.2548	0.8462	0.7523	0.039*
C3	0.3579 (3)	0.5914 (3)	0.81927 (11)	0.0311 (4)
H3A	0.3893	0.4845	0.8002	0.037*
H3B	0.4703	0.7022	0.8176	0.037*
C4	0.2692 (2)	0.4584 (2)	0.95100 (10)	0.0279 (3)
C5	0.2429 (3)	0.5440 (3)	1.02937 (11)	0.0345 (4)
C6	0.2012 (3)	0.4478 (4)	1.09590 (13)	0.0476 (5)
H6A	0.1838	0.5035	1.1486	0.057*
C7	0.1874 (3)	0.2690 (4)	1.07968 (15)	0.0510 (6)
H7A	0.1579	0.2006	1.1221	0.061*
C8	0.2164 (3)	0.1848 (3)	1.00044 (15)	0.0458 (5)
H8A	0.2077	0.0630	0.9926	0.055*
C9	0.2573 (3)	0.2761 (3)	0.93436 (12)	0.0367 (4)
H9A	0.2757	0.2201	0.8820	0.044*
S1	0.37497 (5)	1.14888 (5)	0.64536 (2)	0.02329 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.02054 (11)	0.02314 (12)	0.02269 (11)	0.00744 (8)	0.00097 (8)	0.00663 (8)
N1	0.0270 (7)	0.0262 (7)	0.0292 (7)	0.0083 (6)	−0.0018 (5)	0.0096 (6)
N2	0.0346 (8)	0.0230 (7)	0.0377 (8)	0.0087 (6)	−0.0027 (6)	0.0059 (6)
N3	0.0260 (7)	0.0268 (7)	0.0258 (7)	0.0081 (6)	−0.0012 (5)	0.0077 (6)
N4	0.0361 (8)	0.0314 (8)	0.0263 (7)	0.0165 (6)	−0.0014 (6)	0.0048 (6)
N5	0.0495 (10)	0.0360 (9)	0.0374 (9)	0.0231 (8)	−0.0025 (7)	0.0007 (7)
N6	0.0487 (10)	0.0470 (10)	0.0352 (9)	0.0268 (8)	0.0002 (7)	−0.0022 (7)
O1	0.0213 (6)	0.0294 (6)	0.0287 (6)	0.0002 (5)	0.0023 (5)	0.0026 (5)
O2	0.0438 (18)	0.0245 (11)	0.0470 (19)	0.0144 (11)	−0.0031 (13)	0.0072 (11)
O3	0.0199 (10)	0.0397 (17)	0.0452 (19)	0.0098 (9)	0.0083 (9)	0.0035 (12)
O4	0.035 (3)	0.0462 (16)	0.0235 (14)	0.007 (2)	−0.0014 (18)	0.0060 (11)
O2'	0.065 (5)	0.024 (3)	0.042 (3)	0.004 (3)	−0.002 (3)	0.014 (2)
O3'	0.033 (3)	0.069 (4)	0.092 (7)	0.032 (3)	0.017 (3)	0.020 (5)
O4'	0.032 (5)	0.054 (5)	0.027 (3)	−0.001 (4)	0.001 (4)	−0.007 (3)
O5	0.0345 (7)	0.0347 (7)	0.0300 (6)	0.0054 (5)	0.0062 (5)	−0.0008 (5)
O6	0.0229 (6)	0.0309 (6)	0.0502 (8)	0.0048 (5)	0.0015 (5)	0.0144 (6)
O7	0.0392 (7)	0.0267 (6)	0.0277 (6)	0.0079 (5)	−0.0035 (5)	0.0016 (5)
O8	0.0371 (7)	0.0403 (7)	0.0308 (6)	0.0240 (6)	0.0061 (5)	0.0145 (5)
O9	0.0391 (7)	0.0298 (7)	0.0475 (8)	0.0140 (6)	0.0062 (6)	0.0093 (6)
O10	0.0486 (8)	0.0457 (8)	0.0340 (7)	0.0208 (7)	0.0026 (6)	0.0012 (6)
C1	0.0301 (8)	0.0264 (8)	0.0340 (9)	0.0061 (7)	−0.0040 (7)	0.0053 (7)
C2	0.0313 (9)	0.0258 (8)	0.0349 (9)	0.0053 (7)	−0.0044 (7)	0.0109 (7)
C3	0.0282 (8)	0.0399 (10)	0.0276 (8)	0.0149 (7)	0.0000 (7)	0.0103 (7)
C4	0.0252 (8)	0.0340 (9)	0.0251 (8)	0.0123 (7)	−0.0012 (6)	0.0068 (7)
C5	0.0313 (9)	0.0442 (10)	0.0290 (9)	0.0177 (8)	0.0001 (7)	0.0041 (8)
C6	0.0420 (11)	0.0752 (16)	0.0294 (9)	0.0247 (11)	0.0090 (8)	0.0155 (10)
C7	0.0398 (11)	0.0680 (15)	0.0478 (12)	0.0146 (10)	0.0056 (9)	0.0334 (12)
C8	0.0406 (11)	0.0392 (11)	0.0588 (13)	0.0121 (9)	0.0013 (10)	0.0221 (10)
C9	0.0361 (10)	0.0348 (10)	0.0382 (10)	0.0138 (8)	−0.0006 (8)	0.0061 (8)
S1	0.01968 (18)	0.02186 (19)	0.02462 (19)	0.00521 (14)	0.00123 (14)	0.00217 (15)

Geometric parameters (Å, º) top

Co1—O5	2.0672 (15)	O5—H2W	0.8500
Co1—O8	2.0907 (13)	O6—H3W	0.8500
Co1—O7	2.0982 (14)	O6—H4W	0.8500
Co1—N1	2.1169 (15)	O7—H5W	0.8501
Co1—O6	2.1292 (14)	O7—H6W	0.8500
Co1—O1	2.1462 (14)	O8—H7W	0.8498
N1—C2	1.318 (2)	O8—H8W	0.8500
N1—C1	1.358 (2)	O9—H9W	0.8500
N2—C1	1.312 (2)	O9—H10W	0.8500
N2—N3	1.357 (2)	O10—H11W	0.8500
N3—C2	1.326 (2)	O10—H12W	0.8500
N3—C3	1.456 (2)	C1—H1A	0.9300
N4—N5	1.357 (2)	C2—H2A	0.9300
N4—C4	1.365 (2)	C3—H3A	0.9700
N4—C3	1.440 (2)	C3—H3B	0.9700
N5—N6	1.300 (2)	C4—C5	1.393 (2)
N6—C5	1.378 (3)	C4—C9	1.394 (3)
O1—S1	1.4927 (14)	C5—C6	1.403 (3)
O2—S1	1.503 (3)	C6—C7	1.362 (4)
O3—S1	1.459 (2)	C6—H6A	0.9300
O4—S1	1.426 (7)	C7—C8	1.409 (3)
O2'—S1	1.384 (6)	C7—H7A	0.9300
O3'—S1	1.512 (6)	C8—C9	1.374 (3)
O4'—S1	1.480 (14)	C8—H8A	0.9300
O5—H1W	0.8500	C9—H9A	0.9300

O5—Co1—O8	87.68 (6)	N3—C2—H2A	125.0
O5—Co1—O7	174.46 (5)	N4—C3—N3	111.19 (14)
O8—Co1—O7	87.68 (5)	N4—C3—H3A	109.4
O5—Co1—N1	91.89 (6)	N3—C3—H3A	109.4
O8—Co1—N1	179.24 (5)	N4—C3—H3B	109.4
O7—Co1—N1	92.72 (6)	N3—C3—H3B	109.4
O5—Co1—O6	90.03 (6)	H3A—C3—H3B	108.0
O8—Co1—O6	88.17 (6)	N4—C4—C5	103.75 (16)
O7—Co1—O6	92.85 (6)	N4—C4—C9	133.59 (17)
N1—Co1—O6	92.46 (6)	C5—C4—C9	122.63 (17)
O5—Co1—O1	91.77 (6)	N6—C5—C4	108.34 (16)
O8—Co1—O1	89.00 (6)	N6—C5—C6	130.85 (19)
O7—Co1—O1	85.13 (6)	C4—C5—C6	120.79 (19)
N1—Co1—O1	90.39 (6)	C7—C6—C5	116.8 (2)
O6—Co1—O1	176.59 (5)	C7—C6—H6A	121.6
C2—N1—C1	103.18 (14)	C5—C6—H6A	121.6
C2—N1—Co1	123.09 (12)	C6—C7—C8	121.9 (2)
C1—N1—Co1	133.72 (12)	C6—C7—H7A	119.1
C1—N2—N3	102.41 (14)	C8—C7—H7A	119.1
C2—N3—N2	110.20 (14)	C9—C8—C7	122.3 (2)
C2—N3—C3	127.96 (15)	C9—C8—H8A	118.8
N2—N3—C3	121.83 (14)	C7—C8—H8A	118.8
N5—N4—C4	110.80 (15)	C8—C9—C4	115.56 (19)
N5—N4—C3	119.16 (15)	C8—C9—H9A	122.2
C4—N4—C3	129.99 (16)	C4—C9—H9A	122.2
N6—N5—N4	108.13 (16)	O2'—S1—O4	124.5 (5)
N5—N6—C5	108.98 (16)	O2'—S1—O3	80.7 (5)
S1—O1—Co1	139.41 (8)	O4—S1—O3	112.5 (2)
Co1—O5—H1W	117.2	O2'—S1—O4'	117.9 (7)
Co1—O5—H2W	117.5	O4—S1—O4'	18.4 (5)
H1W—O5—H2W	107.3	O3—S1—O4'	130.4 (4)
Co1—O6—H3W	116.6	O2'—S1—O1	112.5 (3)
Co1—O6—H4W	128.0	O4—S1—O1	113.3 (3)
H3W—O6—H4W	96.6	O3—S1—O1	107.70 (11)
Co1—O7—H5W	115.8	O4'—S1—O1	105.7 (6)
Co1—O7—H6W	118.4	O2'—S1—O2	27.1 (5)
H5W—O7—H6W	100.2	O4—S1—O2	108.7 (3)
Co1—O8—H7W	130.1	O3—S1—O2	107.59 (16)
Co1—O8—H8W	125.4	O4'—S1—O2	96.4 (6)
H7W—O8—H8W	102.5	O1—S1—O2	106.69 (14)
H9W—O9—H10W	100.8	O2'—S1—O3'	110.4 (4)
H11W—O10—H12W	98.1	O4—S1—O3'	86.7 (5)
N2—C1—N1	114.30 (15)	O3—S1—O3'	31.4 (4)
N2—C1—H1A	122.9	O4'—S1—O3'	104.9 (5)
N1—C1—H1A	122.9	O1—S1—O3'	104.3 (3)
N1—C2—N3	109.90 (15)	O2—S1—O3'	135.6 (4)
N1—C2—H2A	125.0

O5—Co1—N1—C2	−51.28 (15)	N5—N4—C3—N3	−76.3 (2)
O8—Co1—N1—C2	4 (4)	C4—N4—C3—N3	106.5 (2)
O7—Co1—N1—C2	125.64 (15)	C2—N3—C3—N4	96.6 (2)
O6—Co1—N1—C2	−141.39 (15)	N2—N3—C3—N4	−82.3 (2)
O1—Co1—N1—C2	40.50 (15)	N5—N4—C4—C5	0.45 (19)
O5—Co1—N1—C1	130.32 (17)	C3—N4—C4—C5	177.87 (17)
O8—Co1—N1—C1	−174 (100)	N5—N4—C4—C9	−177.36 (19)
O7—Co1—N1—C1	−52.76 (17)	C3—N4—C4—C9	0.1 (3)
O6—Co1—N1—C1	40.21 (17)	N5—N6—C5—C4	−0.1 (2)
O1—Co1—N1—C1	−137.90 (17)	N5—N6—C5—C6	178.1 (2)
C1—N2—N3—C2	0.9 (2)	N4—C4—C5—N6	−0.20 (19)
C1—N2—N3—C3	−179.95 (16)	C9—C4—C5—N6	177.92 (17)
C4—N4—N5—N6	−0.6 (2)	N4—C4—C5—C6	−178.62 (17)
C3—N4—N5—N6	−178.29 (15)	C9—C4—C5—C6	−0.5 (3)
N4—N5—N6—C5	0.4 (2)	N6—C5—C6—C7	−178.2 (2)
O5—Co1—O1—S1	3.70 (13)	C4—C5—C6—C7	−0.2 (3)
O8—Co1—O1—S1	91.36 (12)	C5—C6—C7—C8	1.0 (3)
O7—Co1—O1—S1	179.11 (13)	C6—C7—C8—C9	−1.1 (3)
N1—Co1—O1—S1	−88.19 (13)	C7—C8—C9—C4	0.3 (3)
O6—Co1—O1—S1	125.4 (8)	N4—C4—C9—C8	177.90 (19)
N3—N2—C1—N1	−0.7 (2)	C5—C4—C9—C8	0.4 (3)
C2—N1—C1—N2	0.2 (2)	Co1—O1—S1—O2'	−113.2 (8)
Co1—N1—C1—N2	178.85 (13)	Co1—O1—S1—O4	34.7 (3)
C1—N1—C2—N3	0.4 (2)	Co1—O1—S1—O3	159.7 (3)
Co1—N1—C2—N3	−178.43 (11)	Co1—O1—S1—O4'	16.9 (7)
N2—N3—C2—N1	−0.9 (2)	Co1—O1—S1—O2	−85.0 (3)
C3—N3—C2—N1	−179.91 (16)	Co1—O1—S1—O3'	127.2 (7)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H1W···O4′	0.85	2.38	2.823 (13)	113
O5—H1W···N2ⁱ	0.85	2.31	3.081 (2)	150
O5—H2W···O10ⁱⁱ	0.85	1.83	2.672 (2)	173
O6—H3W···O9ⁱⁱⁱ	0.85	1.95	2.798 (2)	171
O6—H4W···O2′^iv	0.85	1.95	2.784 (7)	167
O6—H4W···O2^iv	0.85	1.96	2.777 (4)	160
O7—H5W···O2^v	0.85	1.94	2.771 (4)	167
O7—H5W···O2′^v	0.85	2.15	2.961 (11)	159
O7—H6W···O9^vi	0.85	1.89	2.728 (2)	168
O8—H8W···O3′^vi	0.85	1.86	2.681 (7)	162
O8—H8W···O3^vi	0.85	1.87	2.715 (3)	170
O8—H7W···O1^v	0.85	1.99	2.8246 (18)	167
O9—H9W···O3^vii	0.85	1.95	2.768 (6)	162
O9—H9W···O2′^vii	0.85	2.19	2.911 (15)	142
O10—H11W···O4^vii	0.85	1.97	2.809 (7)	168
O10—H11W···O4′^vii	0.85	2.39	3.209 (16)	163
O10—H11W···O3′^vii	0.85	2.39	2.996 (17)	129
O9—H10W···O1^viii	0.85	2.11	2.945 (2)	166
O10—H12W···N6^ix	0.85	2.00	2.853 (2)	177

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

Experimental details

Crystal data
Chemical formula	[Co(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M_r	463.30
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	7.5471 (15), 7.9415 (16), 16.198 (3)
α, β, γ (°)	99.79 (3), 92.32 (3), 112.22 (3)
V (Å³)	879.8 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.16
Crystal size (mm)	0.21 × 0.19 × 0.16

Data collection
Diffractometer	Rigaku Saturn diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku/MSC, 2006)
T_min, T_max	0.793, 0.836
No. of measured, independent and observed [I > 2σ(I)] reflections	10814, 4158, 3868
R_int	0.019
(sin θ/λ)_max (Å⁻¹)	0.659

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.069, 1.04
No. of reflections	4158
No. of parameters	272
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.37, −0.36

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
O5—H1W···O4'	0.85	2.38	2.823 (13)	113.2
O5—H1W···N2ⁱ	0.85	2.31	3.081 (2)	150.2
O5—H2W···O10ⁱⁱ	0.85	1.83	2.672 (2)	172.8
O6—H3W···O9ⁱⁱⁱ	0.85	1.95	2.798 (2)	171.4
O6—H4W···O2'^iv	0.85	1.95	2.784 (7)	167.4
O6—H4W···O2^iv	0.85	1.96	2.777 (4)	160.2
O7—H5W···O2^v	0.85	1.94	2.771 (4)	166.9
O7—H5W···O2'^v	0.85	2.15	2.961 (11)	159.2
O7—H6W···O9^vi	0.85	1.89	2.728 (2)	168.3
O8—H8W···O3'^vi	0.85	1.86	2.681 (7)	162.4
O8—H8W···O3^vi	0.85	1.87	2.715 (3)	170.4
O8—H7W···O1^v	0.85	1.99	2.8246 (18)	166.7
O9—H9W···O3^vii	0.85	1.95	2.768 (6)	162.4
O9—H9W···O2'^vii	0.85	2.19	2.911 (15)	142.0
O10—H11W···O4^vii	0.85	1.97	2.809 (7)	167.5
O10—H11W···O4'^vii	0.85	2.39	3.209 (16)	163.3
O10—H11W···O3'^vii	0.85	2.39	2.996 (17)	128.9
O9—H10W···O1^viii	0.85	2.11	2.945 (2)	166.2
O10—H12W···N6^ix	0.85	2.00	2.853 (2)	177.4

References

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
Shi, X.-J., Wang, X., Li, L.-K., Hou, H.-W. & Fan, Y.-T. (2010). Cryst. Growth Des. 10, 2490–2500. Web of Science CSD CrossRef CAS Google Scholar
Tian, L., Yang, N. & Zhao, G.-Y. (2010). Inorg. Chem. Commun. 13, 1497–1500. Web of Science CSD CrossRef CAS Google Scholar

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Volume 67| Part 8| August 2011| Page m1078

doi:10.1107/S1600536811027231

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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}sulfato­cobalt(II) 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}sulfatocobalt(II) dihydrate