In the title compound, [Co(C3H4N2)6]Cl2·4H2O, the CoII atom is situated on an inversion center. It is coordinated by six N atoms of six imidazole ligands and has a slightly distorted octahedral geometry. In the crystal structure, the Cl atoms, the water molecules of crystallization and the imidazole NH groups contribute to the formation of a three-dimensional hydrogen-bonded network.
Supporting information
CCDC reference: 227735
Key indicators
- Single-crystal X-ray study
- T = 298 K
- R factor = 0.044
- wR factor = 0.131
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT415_ALERT_2_B Short Inter D-H..H-X H2C .. H4A = 1.98 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H1C .. H1C = 1.86 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT417_ALERT_2_C Short Inter D-H..H-D H1B .. H2C = 2.14 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5
N1 -CO1 -N1 -C1 159.00100.00 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 10
N1 -CO1 -N1 -C3 -16.00100.00 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11
N3 -CO1 -N3 -C4 45.00100.00 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16
N3 -CO1 -N3 -C6 -137.00100.00 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 23
N5 -CO1 -N5 -C7 143.00 43.00 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 28
N5 -CO1 -N5 -C9 -40.00 43.00 2.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 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
6 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART'; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.
hexakis(1
H-imidazole-
κN3)cobalt(II) dichloride tetrahydrate
top
Crystal data top
[Co(C3H4N2)6]Cl2·4H2O | Z = 1 |
Mr = 610.39 | F(000) = 317 |
Triclinic, P1 | Dx = 1.412 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.783 (4) Å | Cell parameters from 2655 reflections |
b = 9.064 (4) Å | θ = 2.6–26.4° |
c = 10.575 (5) Å | µ = 0.83 mm−1 |
α = 75.156 (5)° | T = 298 K |
β = 83.105 (6)° | Prism, dark-purple |
γ = 61.848 (5)° | 0.42 × 0.35 × 0.21 mm |
V = 717.6 (5) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2494 independent reflections |
Radiation source: fine-focus sealed tube | 2186 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
φ and ω scans | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→9 |
Tmin = 0.715, Tmax = 0.843 | k = −10→6 |
3747 measured reflections | l = −12→12 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.23 | w = 1/[σ2(Fo2) + (0.0758P)2 + 0.1518P] where P = (Fo2 + 2Fc2)/3 |
2494 reflections | (Δ/σ)max = 0.001 |
169 parameters | Δρmax = 0.51 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
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 | Uiso*/Ueq | |
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.0304 (2) | |
Cl1 | 0.69765 (10) | 0.79337 (9) | 0.50424 (7) | 0.0466 (2) | |
N1 | −0.1962 (3) | 0.1467 (3) | 0.1260 (2) | 0.0363 (5) | |
N2 | −0.3865 (4) | 0.2055 (4) | 0.2831 (3) | 0.0565 (7) | |
H2B | −0.4485 | 0.1895 | 0.3547 | 0.080* | |
N3 | −0.0033 (3) | 0.2348 (3) | −0.1172 (2) | 0.0377 (5) | |
N4 | −0.0731 (4) | 0.4702 (3) | −0.2698 (3) | 0.0555 (7) | |
H4B | −0.1243 | 0.5541 | −0.3408 | 0.080* | |
N5 | 0.2020 (3) | −0.0356 (3) | 0.1216 (2) | 0.0375 (5) | |
N6 | 0.3305 (4) | −0.0234 (4) | 0.2801 (3) | 0.0593 (8) | |
H6B | 0.3456 | 0.0037 | 0.3522 | 0.080* | |
O1 | 0.0390 (4) | 0.8257 (4) | 0.5242 (3) | 0.0781 (8) | |
H1B | 0.1282 | 0.7943 | 0.5684 | 0.080* | |
H1C | −0.0471 | 0.9238 | 0.5223 | 0.080* | |
O2 | 0.6659 (4) | 0.4564 (4) | 0.5110 (4) | 0.1004 (11) | |
H2C | 0.7570 | 0.3846 | 0.5549 | 0.080* | |
H2D | 0.6258 | 0.5632 | 0.5064 | 0.080* | |
C1 | −0.2612 (4) | 0.0825 (4) | 0.2300 (3) | 0.0457 (7) | |
H1A | −0.2227 | −0.0384 | 0.2639 | 0.080* | |
C2 | −0.4038 (5) | 0.3578 (5) | 0.2085 (4) | 0.0617 (9) | |
H2A | −0.4829 | 0.4700 | 0.2221 | 0.080* | |
C3 | −0.2864 (4) | 0.3211 (4) | 0.1122 (3) | 0.0501 (8) | |
H3A | −0.2688 | 0.4045 | 0.0437 | 0.080* | |
C4 | −0.0997 (4) | 0.3337 (4) | −0.2212 (3) | 0.0461 (7) | |
H4A | −0.1790 | 0.3101 | −0.2573 | 0.080* | |
C5 | 0.0461 (5) | 0.4600 (5) | −0.1939 (4) | 0.0658 (10) | |
H5A | 0.0907 | 0.5408 | −0.2041 | 0.080* | |
C6 | 0.0888 (5) | 0.3155 (4) | −0.0999 (3) | 0.0519 (8) | |
H6A | 0.1715 | 0.2743 | −0.0315 | 0.080* | |
C7 | 0.1799 (4) | 0.0277 (4) | 0.2247 (3) | 0.0470 (7) | |
H7A | 0.0694 | 0.1017 | 0.2557 | 0.080* | |
C8 | 0.4568 (5) | −0.1253 (6) | 0.2100 (4) | 0.0677 (11) | |
H8A | 0.5787 | −0.1814 | 0.2264 | 0.080* | |
C9 | 0.3775 (4) | −0.1317 (5) | 0.1115 (3) | 0.0527 (8) | |
H9A | 0.4344 | −0.1932 | 0.0442 | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0316 (3) | 0.0325 (3) | 0.0252 (3) | −0.0142 (2) | −0.00077 (19) | −0.0042 (2) |
Cl1 | 0.0483 (4) | 0.0453 (4) | 0.0413 (4) | −0.0204 (3) | −0.0006 (3) | −0.0040 (3) |
N1 | 0.0359 (12) | 0.0417 (12) | 0.0307 (12) | −0.0169 (10) | 0.0013 (9) | −0.0095 (10) |
N2 | 0.0508 (16) | 0.075 (2) | 0.0481 (16) | −0.0309 (15) | 0.0207 (12) | −0.0261 (15) |
N3 | 0.0390 (12) | 0.0368 (12) | 0.0343 (12) | −0.0167 (10) | 0.0024 (10) | −0.0059 (10) |
N4 | 0.0624 (17) | 0.0408 (14) | 0.0498 (16) | −0.0210 (13) | −0.0070 (13) | 0.0091 (12) |
N5 | 0.0383 (12) | 0.0418 (13) | 0.0326 (12) | −0.0191 (11) | −0.0034 (9) | −0.0058 (10) |
N6 | 0.0655 (18) | 0.085 (2) | 0.0439 (15) | −0.0434 (17) | −0.0068 (13) | −0.0207 (15) |
O1 | 0.0591 (16) | 0.0806 (19) | 0.100 (2) | −0.0295 (14) | 0.0066 (14) | −0.0373 (17) |
O2 | 0.0719 (19) | 0.0640 (18) | 0.165 (3) | −0.0239 (15) | −0.028 (2) | −0.027 (2) |
C1 | 0.0478 (17) | 0.0558 (18) | 0.0359 (16) | −0.0264 (15) | 0.0072 (13) | −0.0125 (14) |
C2 | 0.054 (2) | 0.055 (2) | 0.065 (2) | −0.0136 (17) | 0.0149 (17) | −0.0262 (18) |
C3 | 0.0543 (18) | 0.0429 (17) | 0.0464 (18) | −0.0182 (15) | 0.0088 (14) | −0.0113 (14) |
C4 | 0.0475 (17) | 0.0416 (16) | 0.0418 (16) | −0.0191 (14) | −0.0054 (13) | 0.0021 (13) |
C5 | 0.086 (3) | 0.052 (2) | 0.067 (2) | −0.044 (2) | −0.009 (2) | 0.0014 (17) |
C6 | 0.063 (2) | 0.0493 (18) | 0.0479 (18) | −0.0329 (16) | −0.0088 (15) | −0.0003 (14) |
C7 | 0.0528 (18) | 0.0545 (18) | 0.0378 (16) | −0.0258 (15) | −0.0026 (13) | −0.0134 (14) |
C8 | 0.0461 (19) | 0.099 (3) | 0.065 (2) | −0.034 (2) | −0.0095 (17) | −0.025 (2) |
C9 | 0.0389 (16) | 0.067 (2) | 0.0508 (19) | −0.0193 (15) | −0.0047 (13) | −0.0187 (16) |
Geometric parameters (Å, º) top
Co1—N3i | 2.160 (2) | N6—C8 | 1.349 (5) |
Co1—N3 | 2.160 (2) | N6—H6B | 0.9000 |
Co1—N5 | 2.168 (2) | O1—H1B | 0.8500 |
Co1—N5i | 2.168 (2) | O1—H1C | 0.8500 |
Co1—N1i | 2.170 (2) | O2—H2C | 0.8500 |
Co1—N1 | 2.170 (2) | O2—H2D | 0.8500 |
N1—C1 | 1.307 (4) | C1—H1A | 0.9600 |
N1—C3 | 1.370 (4) | C2—C3 | 1.346 (5) |
N2—C1 | 1.336 (4) | C2—H2A | 0.9599 |
N2—C2 | 1.351 (5) | C3—H3A | 0.9600 |
N2—H2B | 0.9000 | C4—H4A | 0.9599 |
N3—C4 | 1.316 (4) | C5—C6 | 1.343 (5) |
N3—C6 | 1.373 (4) | C5—H5A | 0.9600 |
N4—C4 | 1.329 (4) | C6—H6A | 0.9600 |
N4—C5 | 1.350 (5) | C7—H7A | 0.9600 |
N4—H4B | 0.9000 | C8—C9 | 1.348 (5) |
N5—C7 | 1.312 (4) | C8—H8A | 0.9600 |
N5—C9 | 1.374 (4) | C9—H9A | 0.9600 |
N6—C7 | 1.332 (4) | | |
| | | |
N3i—Co1—N3 | 180.00 (17) | C7—N6—H6B | 126.3 |
N3i—Co1—N5 | 89.87 (9) | C8—N6—H6B | 125.8 |
N3—Co1—N5 | 90.13 (9) | H1B—O1—H1C | 120.0 |
N3i—Co1—N5i | 90.13 (9) | H2C—O2—H2D | 120.0 |
N3—Co1—N5i | 89.87 (9) | N1—C1—N2 | 111.7 (3) |
N5—Co1—N5i | 180.00 (9) | N1—C1—H1A | 123.9 |
N3i—Co1—N1i | 89.58 (9) | N2—C1—H1A | 124.5 |
N3—Co1—N1i | 90.42 (9) | C3—C2—N2 | 106.3 (3) |
N5—Co1—N1i | 89.39 (9) | C3—C2—H2A | 126.7 |
N5i—Co1—N1i | 90.61 (9) | N2—C2—H2A | 127.0 |
N3i—Co1—N1 | 90.42 (9) | C2—C3—N1 | 109.7 (3) |
N3—Co1—N1 | 89.58 (9) | C2—C3—H3A | 125.2 |
N5—Co1—N1 | 90.61 (9) | N1—C3—H3A | 125.0 |
N5i—Co1—N1 | 89.39 (9) | N3—C4—N4 | 111.3 (3) |
N1i—Co1—N1 | 180.00 (14) | N3—C4—H4A | 124.3 |
C1—N1—C3 | 105.0 (2) | N4—C4—H4A | 124.4 |
C1—N1—Co1 | 125.5 (2) | C6—C5—N4 | 106.5 (3) |
C3—N1—Co1 | 129.3 (2) | C6—C5—H5A | 126.6 |
C1—N2—C2 | 107.3 (3) | N4—C5—H5A | 126.9 |
C1—N2—H2B | 126.2 | C5—C6—N3 | 109.5 (3) |
C2—N2—H2B | 126.5 | C5—C6—H6A | 125.4 |
C4—N3—C6 | 105.1 (3) | N3—C6—H6A | 125.2 |
C4—N3—Co1 | 126.2 (2) | N5—C7—N6 | 111.2 (3) |
C6—N3—Co1 | 128.7 (2) | N5—C7—H7A | 124.2 |
C4—N4—C5 | 107.6 (3) | N6—C7—H7A | 124.6 |
C4—N4—H4B | 126.5 | C9—C8—N6 | 106.2 (3) |
C5—N4—H4B | 125.9 | C9—C8—H8A | 126.7 |
C7—N5—C9 | 105.2 (2) | N6—C8—H8A | 127.1 |
C7—N5—Co1 | 126.3 (2) | C8—C9—N5 | 109.5 (3) |
C9—N5—Co1 | 128.4 (2) | C8—C9—H9A | 125.5 |
C7—N6—C8 | 107.9 (3) | N5—C9—H9A | 125.0 |
| | | |
N3i—Co1—N1—C1 | 1.6 (2) | N3—Co1—N5—C9 | −95.3 (3) |
N3—Co1—N1—C1 | −178.4 (2) | N5i—Co1—N5—C9 | −40 (43) |
N5—Co1—N1—C1 | −88.3 (2) | N1i—Co1—N5—C9 | −4.8 (3) |
N5i—Co1—N1—C1 | 91.7 (2) | N1—Co1—N5—C9 | 175.2 (3) |
N1i—Co1—N1—C1 | 159 (100) | C3—N1—C1—N2 | −0.3 (3) |
N3i—Co1—N1—C3 | −173.6 (3) | Co1—N1—C1—N2 | −176.42 (19) |
N3—Co1—N1—C3 | 6.4 (3) | C2—N2—C1—N1 | 0.4 (4) |
N5—Co1—N1—C3 | 96.5 (3) | C1—N2—C2—C3 | −0.3 (4) |
N5i—Co1—N1—C3 | −83.5 (3) | N2—C2—C3—N1 | 0.2 (4) |
N1i—Co1—N1—C3 | −16 (100) | C1—N1—C3—C2 | 0.1 (4) |
N3i—Co1—N3—C4 | 45 (100) | Co1—N1—C3—C2 | 176.0 (2) |
N5—Co1—N3—C4 | 177.8 (2) | C6—N3—C4—N4 | 0.2 (4) |
N5i—Co1—N3—C4 | −2.2 (2) | Co1—N3—C4—N4 | 179.0 (2) |
N1i—Co1—N3—C4 | 88.4 (2) | C5—N4—C4—N3 | −0.1 (4) |
N1—Co1—N3—C4 | −91.6 (2) | C4—N4—C5—C6 | −0.1 (4) |
N3i—Co1—N3—C6 | −137 (100) | N4—C5—C6—N3 | 0.2 (4) |
N5—Co1—N3—C6 | −3.7 (3) | C4—N3—C6—C5 | −0.2 (4) |
N5i—Co1—N3—C6 | 176.3 (3) | Co1—N3—C6—C5 | −179.0 (2) |
N1i—Co1—N3—C6 | −93.1 (3) | C9—N5—C7—N6 | −0.3 (4) |
N1—Co1—N3—C6 | 86.9 (3) | Co1—N5—C7—N6 | 177.7 (2) |
N3i—Co1—N5—C7 | −92.8 (3) | C8—N6—C7—N5 | −0.2 (4) |
N3—Co1—N5—C7 | 87.2 (3) | C7—N6—C8—C9 | 0.5 (4) |
N5i—Co1—N5—C7 | 143 (43) | N6—C8—C9—N5 | −0.7 (4) |
N1i—Co1—N5—C7 | 177.6 (3) | C7—N5—C9—C8 | 0.6 (4) |
N1—Co1—N5—C7 | −2.4 (3) | Co1—N5—C9—C8 | −177.3 (2) |
N3i—Co1—N5—C9 | 84.7 (3) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2B···Cl1ii | 0.90 | 2.46 | 3.322 (3) | 161 |
N4—H4B···Cl1iii | 0.90 | 2.33 | 3.217 (3) | 169 |
N6—H6B···Cl1iv | 0.90 | 2.54 | 3.380 (3) | 155 |
O1—H1B···O2iv | 0.85 | 2.42 | 2.720 (4) | 101 |
O1—H1C···O1v | 0.85 | 2.23 | 2.815 (6) | 126 |
O2—H2C···O1iv | 0.85 | 2.19 | 2.720 (4) | 121 |
O2—H2D···Cl1 | 0.85 | 2.44 | 3.178 (3) | 145 |
Symmetry codes: (ii) −x, −y+1, −z+1; (iii) x−1, y, z−1; (iv) −x+1, −y+1, −z+1; (v) −x, −y+2, −z+1. |