Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680705605X/ez2106sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680705605X/ez2106Isup2.hkl |
CCDC reference: 674056
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.043
- wR factor = 0.123
- Data-to-parameter ratio = 14.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for O12 - N11 .. 13.24 su PLAT417_ALERT_2_B Short Inter D-H..H-D H12 .. H21 .. 1.69 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT230_ALERT_2_C Hirshfeld Test Diff for O11 - N11 .. 6.03 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N21 PLAT355_ALERT_3_C Long O-H Bond (0.82A) O3 - H31 ... 1.02 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (3) 3.68
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For an earlier structure refinement of the title compound, see: Reimann et al. (1971). For the crystal structure of [Co(bpy)3](CrO4)0.5NO3.7H2O, see: Wojciechowska et al. (2003). For geometrical studies of the coordination mode of the nitrate anion, see: Kleywegt et al. (1985); Dowling et al. (1996).
15 cm3 of a 0.50 M methanolic solution of 2,2'-bipyridine was added to 20 cm3 of an aqueous solution of K2CrO4 (0.25 M). After 15 min of mixing, 10 cm3 of an 0.25 M aqueous solution of cobalt nitrate was added dropwise. This mixture of [Co2+–2,2'-bipyridine–CrO42-] reagents in a 1:3:2 molar ratio was slowly evaporated at room temperature. After 14 days orange crystals of [Co(bpy)3](CrO4)0.5.NO3.7H2O were obtained. The crystals were filtered off and the filtrate was left to stand. After 30 days pink prismatic crystals of the title compound were isolated.
All the hydrogen atoms were visible on difference maps and were refined with isotropic displacement parameters correlated with the anisotropic displacement parameters of the atoms to which they were bonded [C—H 0.93 (2) Å and Uiso(H) = 1.2Ueq(C)]. The positions of hydrogen atoms in the hydroxide ion and water molecules were determined from difference maps and were not refined [Uiso(H) = 1.5Ueq(O)].
Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Westrip, 2007).
[Co(NO3)(C10H8N2)2](OH)(NO3)·4H2O | F(000) = 1208 |
Mr = 584.39 | Dx = 1.562 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2212 reflections |
a = 10.949 (2) Å | θ = 2.9–26.4° |
b = 16.047 (3) Å | µ = 0.76 mm−1 |
c = 14.456 (3) Å | T = 298 K |
β = 101.92 (3)° | Prism, pink |
V = 2485.1 (9) Å3 | 0.38 × 0.25 × 0.21 mm |
Z = 4 |
KUMA KM-4 with CCD area detector diffractometer | 2529 independent reflections |
Radiation source: fine-focus sealed tube | 2212 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1 | θmax = 26.4°, θmin = 2.9° |
ω–scan | h = −13→13 |
Absorption correction: numerical (CrysAlis RED; Oxford Diffraction, 2007) | k = −19→20 |
Tmin = 0.847, Tmax = 0.930 | l = −18→16 |
13043 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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0763P)2 + 1.6632P] where P = (Fo2 + 2Fc2)/3 |
2529 reflections | (Δ/σ)max < 0.001 |
175 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.54 e Å−3 |
[Co(NO3)(C10H8N2)2](OH)(NO3)·4H2O | V = 2485.1 (9) Å3 |
Mr = 584.39 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.949 (2) Å | µ = 0.76 mm−1 |
b = 16.047 (3) Å | T = 298 K |
c = 14.456 (3) Å | 0.38 × 0.25 × 0.21 mm |
β = 101.92 (3)° |
KUMA KM-4 with CCD area detector diffractometer | 2529 independent reflections |
Absorption correction: numerical (CrysAlis RED; Oxford Diffraction, 2007) | 2212 reflections with I > 2σ(I) |
Tmin = 0.847, Tmax = 0.930 | Rint = 0.035 |
13043 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.34 e Å−3 |
2529 reflections | Δρmin = −0.54 e Å−3 |
175 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 | ||
Co1 | 0.5000 | 0.50622 (2) | 0.2500 | 0.03378 (17) | |
N11 | 0.5000 | 0.6494 (2) | 0.2500 | 0.0744 (11) | |
O11 | 0.5000 | 0.72623 (19) | 0.2500 | 0.1021 (13) | |
O12 | 0.55680 (17) | 0.60295 (11) | 0.19693 (12) | 0.0486 (4) | |
N21 | 0.5000 | 0.1667 (3) | 0.2500 | 0.0739 (10) | |
O21 | 0.5000 | 0.2402 (3) | 0.2500 | 0.177 (3) | |
O22 | 0.5834 (4) | 0.1293 (3) | 0.3002 (3) | 0.1659 (18) | |
N1 | 0.56282 (17) | 0.42330 (12) | 0.17425 (12) | 0.0374 (4) | |
N2 | 0.35747 (19) | 0.50549 (11) | 0.14648 (13) | 0.0361 (4) | |
C1 | 0.6699 (2) | 0.38072 (17) | 0.19718 (18) | 0.0497 (6) | |
H1 | 0.7232 | 0.3913 | 0.2549 | 0.060* | |
C2 | 0.7033 (3) | 0.3220 (2) | 0.1382 (2) | 0.0639 (8) | |
H2 | 0.7784 | 0.2934 | 0.1557 | 0.077* | |
C3 | 0.6250 (3) | 0.30562 (19) | 0.0530 (2) | 0.0629 (7) | |
H3 | 0.6459 | 0.2652 | 0.0128 | 0.075* | |
C4 | 0.5152 (2) | 0.34973 (17) | 0.02769 (18) | 0.0508 (6) | |
H4 | 0.4615 | 0.3400 | −0.0301 | 0.061* | |
C5 | 0.2822 (2) | 0.45824 (17) | −0.01124 (16) | 0.0495 (6) | |
H5 | 0.2927 | 0.4256 | −0.0622 | 0.059* | |
C6 | 0.1773 (3) | 0.50778 (17) | −0.0174 (2) | 0.0571 (7) | |
H6 | 0.1169 | 0.5093 | −0.0730 | 0.068* | |
C7 | 0.1630 (2) | 0.55457 (18) | 0.0591 (2) | 0.0572 (7) | |
H7 | 0.0924 | 0.5874 | 0.0562 | 0.069* | |
C8 | 0.2546 (2) | 0.55237 (16) | 0.14060 (18) | 0.0486 (6) | |
H8 | 0.2448 | 0.5840 | 0.1925 | 0.058* | |
C9 | 0.4859 (2) | 0.40857 (14) | 0.08920 (14) | 0.0380 (5) | |
C10 | 0.3712 (2) | 0.45814 (14) | 0.07220 (14) | 0.0382 (5) | |
O1 | 0.2572 (3) | 0.2652 (2) | 0.0904 (3) | 0.1321 (12) | |
H11 | 0.3083 | 0.2320 | 0.1342 | 0.198* | |
H12 | 0.1874 | 0.2802 | 0.1126 | 0.198* | |
O2 | 0.0487 (4) | 0.33863 (18) | 0.1216 (2) | 0.1137 (10) | |
H21 | 0.0504 | 0.2873 | 0.1485 | 0.171* | |
H22 | 0.0588 | 0.3895 | 0.1520 | 0.171* | |
O3 | 0.0000 | 0.4538 (3) | 0.2500 | 0.1300 (18) | |
H31 | 0.0000 | 0.5172 | 0.2500 | 0.195* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0356 (3) | 0.0405 (3) | 0.0229 (2) | 0.000 | 0.00068 (16) | 0.000 |
N11 | 0.080 (3) | 0.055 (2) | 0.075 (2) | 0.000 | −0.014 (2) | 0.000 |
O11 | 0.129 (3) | 0.0345 (16) | 0.133 (3) | 0.000 | 0.004 (3) | 0.000 |
O12 | 0.0555 (10) | 0.0477 (9) | 0.0398 (9) | −0.0063 (8) | 0.0033 (7) | 0.0071 (7) |
N21 | 0.086 (3) | 0.063 (2) | 0.075 (3) | 0.000 | 0.022 (2) | 0.000 |
O21 | 0.257 (9) | 0.067 (3) | 0.218 (7) | 0.000 | 0.078 (7) | 0.000 |
O22 | 0.161 (4) | 0.161 (4) | 0.147 (4) | 0.060 (3) | −0.033 (3) | 0.016 (3) |
N1 | 0.0374 (9) | 0.0447 (10) | 0.0286 (8) | −0.0001 (7) | 0.0031 (7) | −0.0012 (7) |
N2 | 0.0364 (10) | 0.0425 (10) | 0.0274 (9) | 0.0009 (7) | 0.0020 (8) | 0.0033 (7) |
C1 | 0.0428 (13) | 0.0601 (15) | 0.0439 (13) | 0.0087 (11) | 0.0033 (10) | −0.0034 (11) |
C2 | 0.0544 (16) | 0.0712 (19) | 0.0656 (18) | 0.0173 (14) | 0.0112 (13) | −0.0103 (14) |
C3 | 0.0657 (18) | 0.0674 (18) | 0.0578 (16) | 0.0080 (14) | 0.0179 (14) | −0.0198 (14) |
C4 | 0.0560 (15) | 0.0588 (15) | 0.0371 (11) | −0.0078 (11) | 0.0089 (10) | −0.0112 (11) |
C5 | 0.0537 (15) | 0.0549 (15) | 0.0333 (12) | −0.0088 (11) | −0.0064 (10) | 0.0003 (10) |
C6 | 0.0502 (16) | 0.0656 (17) | 0.0439 (15) | −0.0060 (12) | −0.0168 (12) | 0.0080 (11) |
C7 | 0.0414 (13) | 0.0614 (16) | 0.0617 (16) | 0.0056 (11) | −0.0054 (12) | 0.0104 (13) |
C8 | 0.0435 (13) | 0.0547 (14) | 0.0452 (13) | 0.0056 (11) | 0.0035 (10) | 0.0020 (11) |
C9 | 0.0422 (12) | 0.0436 (12) | 0.0272 (10) | −0.0063 (9) | 0.0051 (9) | 0.0002 (8) |
C10 | 0.0438 (12) | 0.0398 (12) | 0.0278 (10) | −0.0068 (9) | 0.0003 (9) | 0.0033 (8) |
O1 | 0.101 (2) | 0.135 (3) | 0.147 (3) | 0.003 (2) | −0.004 (2) | 0.015 (2) |
O2 | 0.139 (3) | 0.094 (2) | 0.105 (2) | 0.0196 (19) | 0.017 (2) | 0.0046 (16) |
O3 | 0.191 (5) | 0.076 (3) | 0.106 (3) | 0.000 | −0.008 (3) | 0.000 |
Co1—O12i | 1.8924 (17) | C2—H2 | 0.9300 |
Co1—O12 | 1.8924 (17) | C3—C4 | 1.378 (4) |
Co1—N2i | 1.926 (2) | C3—H3 | 0.9300 |
Co1—N2 | 1.926 (2) | C4—C9 | 1.379 (3) |
Co1—N1i | 1.9374 (19) | C4—H4 | 0.9300 |
Co1—N1 | 1.9374 (19) | C5—C6 | 1.384 (4) |
Co1—N11 | 2.297 (4) | C5—C10 | 1.385 (3) |
N11—O11 | 1.233 (4) | C5—H5 | 0.9300 |
N11—O12 | 1.314 (3) | C6—C7 | 1.372 (4) |
N11—O12i | 1.314 (3) | C6—H6 | 0.9300 |
N21—O21 | 1.180 (6) | C7—C8 | 1.380 (4) |
N21—O22i | 1.202 (4) | C7—H7 | 0.9300 |
N21—O22 | 1.202 (4) | C8—H8 | 0.9300 |
N1—C1 | 1.338 (3) | C9—C10 | 1.464 (3) |
N1—C9 | 1.360 (3) | O1—H11 | 0.9218 |
N2—C8 | 1.342 (3) | O1—H12 | 0.9194 |
N2—C10 | 1.349 (3) | O2—H21 | 0.9100 |
C1—C2 | 1.371 (4) | O2—H22 | 0.9225 |
C1—H1 | 0.9300 | O3—H31 | 1.0180 |
C2—C3 | 1.372 (4) | ||
O12i—Co1—O12 | 69.80 (12) | C8—N2—Co1 | 125.47 (17) |
O12i—Co1—N2i | 88.36 (7) | C10—N2—Co1 | 114.60 (15) |
O12—Co1—N2i | 92.21 (8) | N1—C1—C2 | 122.0 (2) |
O12—Co1—N2 | 88.36 (7) | N1—C1—H1 | 119.0 |
O12i—Co1—N2 | 92.21 (7) | C2—C1—H1 | 119.0 |
O12—Co1—N1i | 167.72 (8) | C1—C2—C3 | 119.5 (3) |
O12—Co1—N1 | 98.59 (8) | C1—C2—H2 | 120.3 |
N2—Co1—N1 | 83.22 (8) | C3—C2—H2 | 120.3 |
N2—Co1—N1i | 96.30 (8) | C2—C3—C4 | 119.3 (2) |
N2i—Co1—N2 | 179.30 (10) | C2—C3—H3 | 120.4 |
O12i—Co1—N1i | 98.59 (8) | C4—C3—H3 | 120.4 |
N2i—Co1—N1i | 83.22 (8) | C3—C4—C9 | 119.1 (2) |
O12i—Co1—N1 | 167.72 (8) | C3—C4—H4 | 120.4 |
N2i—Co1—N1 | 96.30 (8) | C9—C4—H4 | 120.4 |
N1i—Co1—N1 | 93.25 (11) | C6—C5—C10 | 118.8 (2) |
O12i—Co1—N11 | 34.90 (6) | C6—C5—H5 | 120.6 |
O12—Co1—N11 | 34.90 (6) | C10—C5—H5 | 120.6 |
N2i—Co1—N11 | 90.35 (5) | C7—C6—C5 | 119.6 (2) |
N2—Co1—N11 | 90.35 (5) | C7—C6—H6 | 120.2 |
N1i—Co1—N11 | 133.38 (6) | C5—C6—H6 | 120.2 |
N1—Co1—N11 | 133.38 (6) | C6—C7—C8 | 119.3 (3) |
O11—N11—O12 | 124.54 (15) | C6—C7—H7 | 120.3 |
O11—N11—O12i | 124.54 (15) | C8—C7—H7 | 120.3 |
O12—N11—O12i | 110.9 (3) | N2—C8—C7 | 121.4 (2) |
O11—N11—Co1 | 180.0 | N2—C8—H8 | 119.3 |
O12—N11—Co1 | 55.46 (15) | C7—C8—H8 | 119.3 |
O12i—N11—Co1 | 55.46 (15) | N1—C9—C4 | 121.3 (2) |
N11—O12—Co1 | 89.64 (17) | N1—C9—C10 | 114.01 (19) |
O21—N21—O22i | 119.9 (3) | C4—C9—C10 | 124.7 (2) |
O21—N21—O22 | 119.9 (3) | N2—C10—C5 | 121.2 (2) |
O22i—N21—O22 | 120.2 (6) | N2—C10—C9 | 113.90 (18) |
C1—N1—C9 | 118.8 (2) | C5—C10—C9 | 124.9 (2) |
C1—N1—Co1 | 127.28 (16) | H11—O1—H12 | 110.0 |
C9—N1—Co1 | 113.87 (15) | H21—O2—H22 | 127.5 |
C8—N2—C10 | 119.7 (2) | ||
O12i—Co1—N11—O12 | 180.0 | N11—Co1—N2—C8 | −46.18 (19) |
N2i—Co1—N11—O12 | 93.37 (11) | O12i—Co1—N2—C10 | 162.94 (16) |
N2—Co1—N11—O12 | −86.63 (11) | O12—Co1—N2—C10 | 93.23 (16) |
N1i—Co1—N11—O12 | 174.35 (11) | N1i—Co1—N2—C10 | −98.16 (16) |
N1—Co1—N11—O12 | −5.65 (11) | N1—Co1—N2—C10 | −5.62 (15) |
O12—Co1—N11—O12i | 180.000 (1) | N11—Co1—N2—C10 | 128.08 (15) |
N2i—Co1—N11—O12i | −86.63 (11) | C9—N1—C1—C2 | −1.0 (4) |
N2—Co1—N11—O12i | 93.37 (11) | Co1—N1—C1—C2 | 178.6 (2) |
N1i—Co1—N11—O12i | −5.65 (11) | N1—C1—C2—C3 | −0.3 (5) |
N1—Co1—N11—O12i | 174.35 (11) | C1—C2—C3—C4 | 1.1 (5) |
O11—N11—O12—Co1 | 180.0 | C2—C3—C4—C9 | −0.8 (4) |
O12i—N11—O12—Co1 | 0.0 | C10—C5—C6—C7 | −0.8 (4) |
O12i—Co1—O12—N11 | 0.0 | C5—C6—C7—C8 | 1.0 (4) |
N2i—Co1—O12—N11 | −87.44 (9) | C10—N2—C8—C7 | −1.3 (4) |
N2—Co1—O12—N11 | 92.96 (9) | Co1—N2—C8—C7 | 172.68 (19) |
N1i—Co1—O12—N11 | −19.6 (4) | C6—C7—C8—N2 | 0.1 (4) |
N1—Co1—O12—N11 | 175.85 (8) | C1—N1—C9—C4 | 1.3 (3) |
O12i—Co1—N1—C1 | 114.8 (3) | Co1—N1—C9—C4 | −178.29 (18) |
O12—Co1—N1—C1 | 96.2 (2) | C1—N1—C9—C10 | 179.5 (2) |
N2i—Co1—N1—C1 | 2.9 (2) | Co1—N1—C9—C10 | −0.1 (2) |
N2—Co1—N1—C1 | −176.5 (2) | C3—C4—C9—N1 | −0.5 (4) |
N1i—Co1—N1—C1 | −80.6 (2) | C3—C4—C9—C10 | −178.4 (2) |
N11—Co1—N1—C1 | 99.4 (2) | C8—N2—C10—C5 | 1.4 (3) |
O12i—Co1—N1—C9 | −65.6 (4) | Co1—N2—C10—C5 | −173.18 (17) |
O12—Co1—N1—C9 | −84.26 (16) | C8—N2—C10—C9 | −178.4 (2) |
N2i—Co1—N1—C9 | −177.47 (15) | Co1—N2—C10—C9 | 7.0 (2) |
N2—Co1—N1—C9 | 3.04 (15) | C6—C5—C10—N2 | −0.4 (4) |
N1i—Co1—N1—C9 | 99.00 (16) | C6—C5—C10—C9 | 179.5 (2) |
N11—Co1—N1—C9 | −81.00 (16) | N1—C9—C10—N2 | −4.4 (3) |
O12i—Co1—N2—C8 | −11.3 (2) | C4—C9—C10—N2 | 173.6 (2) |
O12—Co1—N2—C8 | −81.0 (2) | N1—C9—C10—C5 | 175.7 (2) |
N1i—Co1—N2—C8 | 87.6 (2) | C4—C9—C10—C5 | −6.2 (4) |
N1—Co1—N2—C8 | −179.9 (2) |
Symmetry code: (i) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···O22i | 0.92 | 2.14 | 3.027 (6) | 162.4 |
O1—H11···O21 | 0.92 | 2.40 | 3.165 (4) | 139.9 |
O1—H12···O2 | 0.92 | 1.81 | 2.689 (5) | 158.4 |
O2—H21···O11ii | 0.91 | 1.94 | 2.718 (4) | 142.9 |
O2—H22···O3 | 0.92 | 1.97 | 2.748 (4) | 141.5 |
O3—H31···O22iii | 1.02 | 2.08 | 3.004 (6) | 150 |
O3—H31···O22iv | 1.02 | 2.08 | 3.004 (6) | 150 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(NO3)(C10H8N2)2](OH)(NO3)·4H2O |
Mr | 584.39 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 10.949 (2), 16.047 (3), 14.456 (3) |
β (°) | 101.92 (3) |
V (Å3) | 2485.1 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.76 |
Crystal size (mm) | 0.38 × 0.25 × 0.21 |
Data collection | |
Diffractometer | KUMA KM-4 with CCD area detector diffractometer |
Absorption correction | Numerical (CrysAlis RED; Oxford Diffraction, 2007) |
Tmin, Tmax | 0.847, 0.930 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13043, 2529, 2212 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.625 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.123, 1.06 |
No. of reflections | 2529 |
No. of parameters | 175 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.34, −0.54 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2005), publCIF (Westrip, 2007).
Co1—O12 | 1.8924 (17) | Co1—N1 | 1.9374 (19) |
Co1—N2 | 1.926 (2) | Co1—N11 | 2.297 (4) |
O12i—Co1—O12 | 69.80 (12) | N2—Co1—N1 | 83.22 (8) |
O12—Co1—N2 | 88.36 (7) | N2—Co1—N1i | 96.30 (8) |
O12i—Co1—N2 | 92.21 (7) | N2i—Co1—N2 | 179.30 (10) |
O12—Co1—N1i | 167.72 (8) | N1i—Co1—N1 | 93.25 (11) |
O12—Co1—N1 | 98.59 (8) |
Symmetry code: (i) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···O22i | 0.92 | 2.14 | 3.027 (6) | 162.4 |
O1—H11···O21 | 0.92 | 2.40 | 3.165 (4) | 139.9 |
O1—H12···O2 | 0.92 | 1.81 | 2.689 (5) | 158.4 |
O2—H21···O11ii | 0.91 | 1.94 | 2.718 (4) | 142.9 |
O2—H22···O3 | 0.92 | 1.97 | 2.748 (4) | 141.5 |
O3—H31···O22iii | 1.02 | 2.08 | 3.004 (6) | 149.9 |
O3—H31···O22iv | 1.02 | 2.08 | 3.004 (6) | 149.9 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x−1/2, y−1/2, z; (iii) x−1/2, y+1/2, z; (iv) −x+1/2, y+1/2, −z+1/2. |
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Bis(2,2'-bipyridine)(nitrato-O,O')cobalt(III) hydroxide nitrate tetrahydrate (I) was unintentionally obtained from a [Co2+–2,2'-bipyridine–CrO42-] mixture as the second product. The first product was identified as [Co(bpy)3](CrO4)0.5.NO3.7H2O (Wojciechowska et al., 2003). The present single-crystal study confirms the previous refinement (Reimann et al., 1971), but with all hydrogen atoms, which were visible in the difference maps, included in the refinement (Fig. 1). Two organic ligands and one nitrate ion form a distorted octahedral coordination sphere around the Co(III) ion. The differences between the Co—Onitrate bond lengths, and the Co—O—N and Co—N—Oterminal angles are 0 Å, 0° and 180° respectively, which correlate exactly with the bidentate mode of the nitrate group (Kleywegt et al., 1985; Dowling et al., 1996). The nitrate groups, hydroxide ions and water molecules form a rich hydrogen bonding network, which surrounds the [Co(bpy)2(NO3-O,O')]+ cation and links to it via an Owater—H···Onitrate hydrogen bond (Fig. 2).