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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

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

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 CoII 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[Tian, L., Yang, N. & Zhao, G.-Y. (2010). Inorg. Chem. Commun. 13, 1497-1500.]); Shi et al. (2010[Shi, X.-J., Wang, X., Li, L.-K., Hou, H.-W. & Fan, Y.-T. (2010). Cryst. Growth Des. 10, 2490-2500.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(SO4)(C9H8N6)(H2O)4]·2H2O

  • Mr = 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[Rigaku/MSC (2006). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.793, Tmax = 0.836

  • 10814 measured reflections

  • 4158 independent reflections

  • 3868 reflections with I > 2σ(I)

  • Rint = 0.019

Refinement
  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 0.069

  • S = 1.04

  • 4158 reflections

  • 272 parameters

  • H-atom parameters constrained

  • Δρmax = 0.37 e Å−3

  • Δρmin = −0.36 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA 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⋯O2iv 0.85 1.96 2.777 (4) 160
O7—H5W⋯O2v 0.85 1.94 2.771 (4) 167
O7—H5W⋯O2′v 0.85 2.15 2.961 (11) 159
O7—H6W⋯O9vi 0.85 1.89 2.728 (2) 168
O8—H8W⋯O3′vi 0.85 1.86 2.681 (7) 162
O8—H8W⋯O3vi 0.85 1.87 2.715 (3) 170
O8—H7W⋯O1v 0.85 1.99 2.8246 (18) 167
O9—H9W⋯O3vii 0.85 1.95 2.768 (6) 162
O9—H9W⋯O2′vii 0.85 2.19 2.911 (15) 142
O10—H11W⋯O4vii 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⋯O1viii 0.85 2.11 2.945 (2) 166
O10—H12W⋯N6ix 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[Rigaku/MSC (2006). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


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 CoII 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.

Refinement top

The disordered sulfate ligand was modeled by splitting the atoms into two components (O2, O3, O4 and O2', O3', O4'), the site occupation factors of which refined in a ratio of 0.662 (15):0.338 (15). H atoms are positioned geometrically and refined as riding atoms, with C-H = 0.93 (aromatic) and 0.97 (CH2) Å and O-H = 0.85 Å, and with Uiso(H) = 1.2 Ueq(C,O).

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
[Figure 1] 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.
[Figure 2] 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]·2H2OZ = 2
Mr = 463.30F(000) = 478
Triclinic, P1Dx = 1.749 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5471 (15) ÅCell parameters from 3052 reflections
b = 7.9415 (16) Åθ = 2.6–27.9°
c = 16.198 (3) ŵ = 1.16 mm1
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 tube3868 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 28.5714 pixels mm-1θmax = 27.9°, θmin = 2.6°
ω scansh = 99
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2006)
k = 1010
Tmin = 0.793, Tmax = 0.836l = 2119
10814 measured reflections
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0299P)2 + 0.4582P]
where P = (Fo2 + 2Fc2)/3
4158 reflections(Δ/σ)max = 0.001
272 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = 0.36 e Å3
Crystal data top
[Co(SO4)(C9H8N6)(H2O)4]·2H2Oγ = 112.22 (3)°
Mr = 463.30V = 879.8 (3) Å3
Triclinic, P1Z = 2
a = 7.5471 (15) ÅMo Kα radiation
b = 7.9415 (16) ŵ = 1.16 mm1
c = 16.198 (3) ÅT = 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)
Tmin = 0.793, Tmax = 0.836Rint = 0.019
10814 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.069H-atom parameters constrained
S = 1.04Δρmax = 0.37 e Å3
4158 reflectionsΔρmin = 0.36 e Å3
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
xyzUiso*/UeqOcc. (<1)
Co10.08883 (3)0.83076 (3)0.627602 (13)0.02224 (7)
N10.0089 (2)0.65836 (19)0.68655 (9)0.0277 (3)
N20.0484 (2)0.4200 (2)0.73017 (10)0.0328 (3)
N30.1979 (2)0.58276 (19)0.76299 (9)0.0267 (3)
N40.3108 (2)0.5942 (2)0.90460 (9)0.0305 (3)
N50.3118 (3)0.7536 (2)0.95135 (11)0.0401 (4)
N60.2705 (3)0.7243 (3)1.02609 (11)0.0426 (4)
O10.19941 (16)0.98544 (16)0.60342 (7)0.0298 (3)
O20.3506 (7)1.3182 (4)0.6265 (3)0.0383 (9)0.662 (15)
O30.5396 (3)1.1350 (6)0.6050 (3)0.0360 (11)0.662 (15)
O40.4014 (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)
O50.05411 (19)1.01086 (18)0.74101 (8)0.0364 (3)
H1W0.01621.12470.74370.044*
H2W0.15521.00650.76350.044*
O60.38083 (17)0.68003 (17)0.64472 (9)0.0357 (3)
H3W0.46640.69460.61440.043*
H4W0.43900.56350.64040.043*
O70.11655 (19)0.67039 (17)0.50698 (8)0.0334 (3)
H5W0.17830.69240.46800.040*
H6W0.17520.55330.49980.040*
O80.18197 (18)1.00403 (18)0.57005 (8)0.0324 (3)
H7W0.17371.02510.52030.039*
H8W0.26571.04540.58690.039*
O90.65865 (19)0.29975 (18)0.46850 (9)0.0384 (3)
H9W0.60030.25310.50810.046*
H10W0.71650.22800.45390.046*
O100.6405 (2)0.0290 (2)0.81395 (9)0.0430 (3)
H11W0.58410.08410.78910.052*
H12W0.66960.10110.86200.052*
C10.0606 (3)0.4727 (2)0.68424 (11)0.0320 (4)
H1A0.17580.38990.65280.038*
C20.1713 (3)0.7220 (2)0.73708 (11)0.0321 (4)
H2A0.25480.84620.75230.039*
C30.3579 (3)0.5914 (3)0.81927 (11)0.0311 (4)
H3A0.38930.48450.80020.037*
H3B0.47030.70220.81760.037*
C40.2692 (2)0.4584 (2)0.95100 (10)0.0279 (3)
C50.2429 (3)0.5440 (3)1.02937 (11)0.0345 (4)
C60.2012 (3)0.4478 (4)1.09590 (13)0.0476 (5)
H6A0.18380.50351.14860.057*
C70.1874 (3)0.2690 (4)1.07968 (15)0.0510 (6)
H7A0.15790.20061.12210.061*
C80.2164 (3)0.1848 (3)1.00044 (15)0.0458 (5)
H8A0.20770.06300.99260.055*
C90.2573 (3)0.2761 (3)0.93436 (12)0.0367 (4)
H9A0.27570.22010.88200.044*
S10.37497 (5)1.14888 (5)0.64536 (2)0.02329 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02054 (11)0.02314 (12)0.02269 (11)0.00744 (8)0.00097 (8)0.00663 (8)
N10.0270 (7)0.0262 (7)0.0292 (7)0.0083 (6)0.0018 (5)0.0096 (6)
N20.0346 (8)0.0230 (7)0.0377 (8)0.0087 (6)0.0027 (6)0.0059 (6)
N30.0260 (7)0.0268 (7)0.0258 (7)0.0081 (6)0.0012 (5)0.0077 (6)
N40.0361 (8)0.0314 (8)0.0263 (7)0.0165 (6)0.0014 (6)0.0048 (6)
N50.0495 (10)0.0360 (9)0.0374 (9)0.0231 (8)0.0025 (7)0.0007 (7)
N60.0487 (10)0.0470 (10)0.0352 (9)0.0268 (8)0.0002 (7)0.0022 (7)
O10.0213 (6)0.0294 (6)0.0287 (6)0.0002 (5)0.0023 (5)0.0026 (5)
O20.0438 (18)0.0245 (11)0.0470 (19)0.0144 (11)0.0031 (13)0.0072 (11)
O30.0199 (10)0.0397 (17)0.0452 (19)0.0098 (9)0.0083 (9)0.0035 (12)
O40.035 (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)
O50.0345 (7)0.0347 (7)0.0300 (6)0.0054 (5)0.0062 (5)0.0008 (5)
O60.0229 (6)0.0309 (6)0.0502 (8)0.0048 (5)0.0015 (5)0.0144 (6)
O70.0392 (7)0.0267 (6)0.0277 (6)0.0079 (5)0.0035 (5)0.0016 (5)
O80.0371 (7)0.0403 (7)0.0308 (6)0.0240 (6)0.0061 (5)0.0145 (5)
O90.0391 (7)0.0298 (7)0.0475 (8)0.0140 (6)0.0062 (6)0.0093 (6)
O100.0486 (8)0.0457 (8)0.0340 (7)0.0208 (7)0.0026 (6)0.0012 (6)
C10.0301 (8)0.0264 (8)0.0340 (9)0.0061 (7)0.0040 (7)0.0053 (7)
C20.0313 (9)0.0258 (8)0.0349 (9)0.0053 (7)0.0044 (7)0.0109 (7)
C30.0282 (8)0.0399 (10)0.0276 (8)0.0149 (7)0.0000 (7)0.0103 (7)
C40.0252 (8)0.0340 (9)0.0251 (8)0.0123 (7)0.0012 (6)0.0068 (7)
C50.0313 (9)0.0442 (10)0.0290 (9)0.0177 (8)0.0001 (7)0.0041 (8)
C60.0420 (11)0.0752 (16)0.0294 (9)0.0247 (11)0.0090 (8)0.0155 (10)
C70.0398 (11)0.0680 (15)0.0478 (12)0.0146 (10)0.0056 (9)0.0334 (12)
C80.0406 (11)0.0392 (11)0.0588 (13)0.0121 (9)0.0013 (10)0.0221 (10)
C90.0361 (10)0.0348 (10)0.0382 (10)0.0138 (8)0.0006 (8)0.0061 (8)
S10.01968 (18)0.02186 (19)0.02462 (19)0.00521 (14)0.00123 (14)0.00217 (15)
Geometric parameters (Å, º) top
Co1—O52.0672 (15)O5—H2W0.8500
Co1—O82.0907 (13)O6—H3W0.8500
Co1—O72.0982 (14)O6—H4W0.8500
Co1—N12.1169 (15)O7—H5W0.8501
Co1—O62.1292 (14)O7—H6W0.8500
Co1—O12.1462 (14)O8—H7W0.8498
N1—C21.318 (2)O8—H8W0.8500
N1—C11.358 (2)O9—H9W0.8500
N2—C11.312 (2)O9—H10W0.8500
N2—N31.357 (2)O10—H11W0.8500
N3—C21.326 (2)O10—H12W0.8500
N3—C31.456 (2)C1—H1A0.9300
N4—N51.357 (2)C2—H2A0.9300
N4—C41.365 (2)C3—H3A0.9700
N4—C31.440 (2)C3—H3B0.9700
N5—N61.300 (2)C4—C51.393 (2)
N6—C51.378 (3)C4—C91.394 (3)
O1—S11.4927 (14)C5—C61.403 (3)
O2—S11.503 (3)C6—C71.362 (4)
O3—S11.459 (2)C6—H6A0.9300
O4—S11.426 (7)C7—C81.409 (3)
O2'—S11.384 (6)C7—H7A0.9300
O3'—S11.512 (6)C8—C91.374 (3)
O4'—S11.480 (14)C8—H8A0.9300
O5—H1W0.8500C9—H9A0.9300
O5—Co1—O887.68 (6)N3—C2—H2A125.0
O5—Co1—O7174.46 (5)N4—C3—N3111.19 (14)
O8—Co1—O787.68 (5)N4—C3—H3A109.4
O5—Co1—N191.89 (6)N3—C3—H3A109.4
O8—Co1—N1179.24 (5)N4—C3—H3B109.4
O7—Co1—N192.72 (6)N3—C3—H3B109.4
O5—Co1—O690.03 (6)H3A—C3—H3B108.0
O8—Co1—O688.17 (6)N4—C4—C5103.75 (16)
O7—Co1—O692.85 (6)N4—C4—C9133.59 (17)
N1—Co1—O692.46 (6)C5—C4—C9122.63 (17)
O5—Co1—O191.77 (6)N6—C5—C4108.34 (16)
O8—Co1—O189.00 (6)N6—C5—C6130.85 (19)
O7—Co1—O185.13 (6)C4—C5—C6120.79 (19)
N1—Co1—O190.39 (6)C7—C6—C5116.8 (2)
O6—Co1—O1176.59 (5)C7—C6—H6A121.6
C2—N1—C1103.18 (14)C5—C6—H6A121.6
C2—N1—Co1123.09 (12)C6—C7—C8121.9 (2)
C1—N1—Co1133.72 (12)C6—C7—H7A119.1
C1—N2—N3102.41 (14)C8—C7—H7A119.1
C2—N3—N2110.20 (14)C9—C8—C7122.3 (2)
C2—N3—C3127.96 (15)C9—C8—H8A118.8
N2—N3—C3121.83 (14)C7—C8—H8A118.8
N5—N4—C4110.80 (15)C8—C9—C4115.56 (19)
N5—N4—C3119.16 (15)C8—C9—H9A122.2
C4—N4—C3129.99 (16)C4—C9—H9A122.2
N6—N5—N4108.13 (16)O2'—S1—O4124.5 (5)
N5—N6—C5108.98 (16)O2'—S1—O380.7 (5)
S1—O1—Co1139.41 (8)O4—S1—O3112.5 (2)
Co1—O5—H1W117.2O2'—S1—O4'117.9 (7)
Co1—O5—H2W117.5O4—S1—O4'18.4 (5)
H1W—O5—H2W107.3O3—S1—O4'130.4 (4)
Co1—O6—H3W116.6O2'—S1—O1112.5 (3)
Co1—O6—H4W128.0O4—S1—O1113.3 (3)
H3W—O6—H4W96.6O3—S1—O1107.70 (11)
Co1—O7—H5W115.8O4'—S1—O1105.7 (6)
Co1—O7—H6W118.4O2'—S1—O227.1 (5)
H5W—O7—H6W100.2O4—S1—O2108.7 (3)
Co1—O8—H7W130.1O3—S1—O2107.59 (16)
Co1—O8—H8W125.4O4'—S1—O296.4 (6)
H7W—O8—H8W102.5O1—S1—O2106.69 (14)
H9W—O9—H10W100.8O2'—S1—O3'110.4 (4)
H11W—O10—H12W98.1O4—S1—O3'86.7 (5)
N2—C1—N1114.30 (15)O3—S1—O3'31.4 (4)
N2—C1—H1A122.9O4'—S1—O3'104.9 (5)
N1—C1—H1A122.9O1—S1—O3'104.3 (3)
N1—C2—N3109.90 (15)O2—S1—O3'135.6 (4)
N1—C2—H2A125.0
O5—Co1—N1—C251.28 (15)N5—N4—C3—N376.3 (2)
O8—Co1—N1—C24 (4)C4—N4—C3—N3106.5 (2)
O7—Co1—N1—C2125.64 (15)C2—N3—C3—N496.6 (2)
O6—Co1—N1—C2141.39 (15)N2—N3—C3—N482.3 (2)
O1—Co1—N1—C240.50 (15)N5—N4—C4—C50.45 (19)
O5—Co1—N1—C1130.32 (17)C3—N4—C4—C5177.87 (17)
O8—Co1—N1—C1174 (100)N5—N4—C4—C9177.36 (19)
O7—Co1—N1—C152.76 (17)C3—N4—C4—C90.1 (3)
O6—Co1—N1—C140.21 (17)N5—N6—C5—C40.1 (2)
O1—Co1—N1—C1137.90 (17)N5—N6—C5—C6178.1 (2)
C1—N2—N3—C20.9 (2)N4—C4—C5—N60.20 (19)
C1—N2—N3—C3179.95 (16)C9—C4—C5—N6177.92 (17)
C4—N4—N5—N60.6 (2)N4—C4—C5—C6178.62 (17)
C3—N4—N5—N6178.29 (15)C9—C4—C5—C60.5 (3)
N4—N5—N6—C50.4 (2)N6—C5—C6—C7178.2 (2)
O5—Co1—O1—S13.70 (13)C4—C5—C6—C70.2 (3)
O8—Co1—O1—S191.36 (12)C5—C6—C7—C81.0 (3)
O7—Co1—O1—S1179.11 (13)C6—C7—C8—C91.1 (3)
N1—Co1—O1—S188.19 (13)C7—C8—C9—C40.3 (3)
O6—Co1—O1—S1125.4 (8)N4—C4—C9—C8177.90 (19)
N3—N2—C1—N10.7 (2)C5—C4—C9—C80.4 (3)
C2—N1—C1—N20.2 (2)Co1—O1—S1—O2'113.2 (8)
Co1—N1—C1—N2178.85 (13)Co1—O1—S1—O434.7 (3)
C1—N1—C2—N30.4 (2)Co1—O1—S1—O3159.7 (3)
Co1—N1—C2—N3178.43 (11)Co1—O1—S1—O4'16.9 (7)
N2—N3—C2—N10.9 (2)Co1—O1—S1—O285.0 (3)
C3—N3—C2—N1179.91 (16)Co1—O1—S1—O3'127.2 (7)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H1W···O40.852.382.823 (13)113
O5—H1W···N2i0.852.313.081 (2)150
O5—H2W···O10ii0.851.832.672 (2)173
O6—H3W···O9iii0.851.952.798 (2)171
O6—H4W···O2iv0.851.952.784 (7)167
O6—H4W···O2iv0.851.962.777 (4)160
O7—H5W···O2v0.851.942.771 (4)167
O7—H5W···O2v0.852.152.961 (11)159
O7—H6W···O9vi0.851.892.728 (2)168
O8—H8W···O3vi0.851.862.681 (7)162
O8—H8W···O3vi0.851.872.715 (3)170
O8—H7W···O1v0.851.992.8246 (18)167
O9—H9W···O3vii0.851.952.768 (6)162
O9—H9W···O2vii0.852.192.911 (15)142
O10—H11W···O4vii0.851.972.809 (7)168
O10—H11W···O4vii0.852.393.209 (16)163
O10—H11W···O3vii0.852.392.996 (17)129
O9—H10W···O1viii0.852.112.945 (2)166
O10—H12W···N6ix0.852.002.853 (2)177
Symmetry codes: (i) x, y+1, z; (ii) x1, y+1, z; (iii) x, y+1, z+1; (iv) x1, y1, z; (v) x, y+2, z+1; (vi) x1, y, z; (vii) x, y1, 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
Mr463.30
Crystal system, space groupTriclinic, 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)
V3)879.8 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.16
Crystal size (mm)0.21 × 0.19 × 0.16
Data collection
DiffractometerRigaku Saturn
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku/MSC, 2006)
Tmin, Tmax0.793, 0.836
No. of measured, independent and
observed [I > 2σ(I)] reflections
10814, 4158, 3868
Rint0.019
(sin θ/λ)max1)0.659
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.069, 1.04
No. of reflections4158
No. of parameters272
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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···AD—HH···AD···AD—H···A
O5—H1W···O4'0.852.382.823 (13)113.2
O5—H1W···N2i0.852.313.081 (2)150.2
O5—H2W···O10ii0.851.832.672 (2)172.8
O6—H3W···O9iii0.851.952.798 (2)171.4
O6—H4W···O2'iv0.851.952.784 (7)167.4
O6—H4W···O2iv0.851.962.777 (4)160.2
O7—H5W···O2v0.851.942.771 (4)166.9
O7—H5W···O2'v0.852.152.961 (11)159.2
O7—H6W···O9vi0.851.892.728 (2)168.3
O8—H8W···O3'vi0.851.862.681 (7)162.4
O8—H8W···O3vi0.851.872.715 (3)170.4
O8—H7W···O1v0.851.992.8246 (18)166.7
O9—H9W···O3vii0.851.952.768 (6)162.4
O9—H9W···O2'vii0.852.192.911 (15)142.0
O10—H11W···O4vii0.851.972.809 (7)167.5
O10—H11W···O4'vii0.852.393.209 (16)163.3
O10—H11W···O3'vii0.852.392.996 (17)128.9
O9—H10W···O1viii0.852.112.945 (2)166.2
O10—H12W···N6ix0.852.002.853 (2)177.4
Symmetry codes: (i) x, y+1, z; (ii) x1, y+1, z; (iii) x, y+1, z+1; (iv) x1, y1, z; (v) x, y+2, z+1; (vi) x1, y, z; (vii) x, y1, z; (viii) x+1, y+1, z+1; (ix) x+1, y+1, z+2.
 

References

First citationRigaku/MSC (2006). CrystalClear. Rigaku/MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationShi, 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
First citationTian, L., Yang, N. & Zhao, G.-Y. (2010). Inorg. Chem. Commun. 13, 1497–1500.  Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds