



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536811027231/lh5272sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536811027231/lh5272Isup2.hkl |
CCDC reference: 841025
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean
(C-C) = 0.003 Å
- Disorder in main residue
- R factor = 0.030
- wR factor = 0.069
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 20 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 30 PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT154_ALERT_1_G The su's on the Cell Angles are Equal .......... 0.03000 Deg. PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K PLAT301_ALERT_3_G Note: Main Residue Disorder ................... 12 Perc. PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 2 O8 -CO1 -N1 -C2 4.00 4.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 O8 -CO1 -N1 -C1 17.00 0.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 20 O6 -CO1 -O1 -S1 125.40 0.80 1.555 1.555 1.555 1.555 PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 77 O4 -S1 -O4' 1.555 1.555 1.555 18.40 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 83 O2' -S1 -O2 1.555 1.555 1.555 27.10 Deg. PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 90 O3 -S1 -O3' 1.555 1.555 1.555 31.40 Deg.
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 5 ALERT level C = Check. Ensure it is not caused by an omission or oversight 11 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
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.
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).
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).
[Co(SO4)(C9H8N6)(H2O)4]·2H2O | Z = 2 |
Mr = 463.30 | F(000) = 478 |
Triclinic, P1 | Dx = 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 |
Rigaku Saturn diffractometer | 4158 independent reflections |
Radiation source: fine-focus sealed tube | 3868 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
Detector resolution: 28.5714 pixels mm-1 | θmax = 27.9°, θmin = 2.6° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006) | k = −10→10 |
Tmin = 0.793, Tmax = 0.836 | l = −21→19 |
10814 measured reflections |
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(Fo2) + (0.0299P)2 + 0.4582P] where P = (Fo2 + 2Fc2)/3 |
4158 reflections | (Δ/σ)max = 0.001 |
272 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.36 e Å−3 |
[Co(SO4)(C9H8N6)(H2O)4]·2H2O | γ = 112.22 (3)° |
Mr = 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)° |
Rigaku Saturn diffractometer | 4158 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006) | 3868 reflections with I > 2σ(I) |
Tmin = 0.793, Tmax = 0.836 | Rint = 0.019 |
10814 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 0 restraints |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.37 e Å−3 |
4158 reflections | Δρmin = −0.36 e Å−3 |
272 parameters |
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. |
x | y | z | Uiso*/Ueq | 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) |
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) |
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) |
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···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. |
Experimental details
Crystal data | |
Chemical formula | [Co(SO4)(C9H8N6)(H2O)4]·2H2O |
Mr | 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) |
Tmin, Tmax | 0.793, 0.836 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10814, 4158, 3868 |
Rint | 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 |
Δρmax, Δρmin (e Å−3) | 0.37, −0.36 |
Computer programs: CrystalClear (Rigaku/MSC, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
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···O2iv | 0.85 | 1.96 | 2.777 (4) | 160.2 |
O7—H5W···O2v | 0.85 | 1.94 | 2.771 (4) | 166.9 |
O7—H5W···O2'v | 0.85 | 2.15 | 2.961 (11) | 159.2 |
O7—H6W···O9vi | 0.85 | 1.89 | 2.728 (2) | 168.3 |
O8—H8W···O3'vi | 0.85 | 1.86 | 2.681 (7) | 162.4 |
O8—H8W···O3vi | 0.85 | 1.87 | 2.715 (3) | 170.4 |
O8—H7W···O1v | 0.85 | 1.99 | 2.8246 (18) | 166.7 |
O9—H9W···O3vii | 0.85 | 1.95 | 2.768 (6) | 162.4 |
O9—H9W···O2'vii | 0.85 | 2.19 | 2.911 (15) | 142.0 |
O10—H11W···O4vii | 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···O1viii | 0.85 | 2.11 | 2.945 (2) | 166.2 |
O10—H12W···N6ix | 0.85 | 2.00 | 2.853 (2) | 177.4 |
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. |
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).