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The title compound, [Co(C4H13N3)2][Co(CN)6]·2H2O, comprises one [Co(dien)2]3+ cation (dien is diethylenetriamine), one [Co(CN)6]3- anion and two water molecules. The Co3+ atom of the [Co(dien)2]3+ cation is six-coordinated by six N atoms from two diethylenetriamine groups. The Co3+ atom of the [Co(CN)6]3- anion is six-coordinated by six C atoms from six cyanide ions. Neighboring cations and anions are connected by hydrogen bonds to each other and to the water molecules. The metal atoms lie on inversion sites.
Supporting information
CCDC reference: 633966
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.032
- wR factor = 0.095
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.13
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co2 - C3 .. 7.00 su
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5
N2 -CO1 -N2 -C6 -8.20 0.20 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6
N3 -CO1 -N3 -C4 2.00 0.00 3.555 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 -C5 14.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16
C2 -CO2 -C1 -N6 -29.00 7.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 17
C2 -CO2 -C1 -N6 151.00 7.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18
C3 -CO2 -C1 -N6 -118.00 7.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 19
C3 -CO2 -C1 -N6 62.00 7.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 20
C1 -CO2 -C1 -N6 14.00 0.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 23
N1 -CO1 -N1 -C7 5.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 26
C2 -CO2 -C2 -N4 1.00 0.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 27
C3 -CO2 -C2 -N4 127.00 6.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 28
C3 -CO2 -C2 -N4 -53.00 6.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 29
C1 -CO2 -C2 -N4 -142.00 6.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 30
C1 -CO2 -C2 -N4 38.00 6.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 31
C2 -CO2 -C3 -N5 2.00 0.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 32
C2 -CO2 -C3 -N5 17.00 0.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 33
C3 -CO2 -C3 -N5 10.00 0.00 3.656 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 34
C1 -CO2 -C3 -N5 10.00 0.00 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 35
C1 -CO2 -C3 -N5 8.00 0.00 3.656 1.555 1.555 1.555
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
24 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
20 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.
Bis(diethylenetriamine)cobalt(III) hexacyanocobaltate(III) monohydrate
top
Crystal data top
[Co(C4H13N3)2][Co(CN)6]·2H2O | F(000) = 536 |
Mr = 516.36 | Dx = 1.582 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.148 (3) Å | Cell parameters from 739 reflections |
b = 12.217 (4) Å | θ = 2.5–27.2° |
c = 10.935 (4) Å | µ = 1.57 mm−1 |
β = 94.973 (7)° | T = 293 K |
V = 1084.3 (6) Å3 | Block, yellow |
Z = 2 | 0.48 × 0.31 × 0.13 mm |
Data collection top
Bruker APEX area-detector diffractometer | 2375 independent reflections |
Radiation source: fine-focus sealed tube | 1473 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 27.2°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→10 |
Tmin = 0.520, Tmax = 0.822 | k = −15→15 |
6186 measured reflections | l = −8→14 |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0501P)2 + 0.0602P] where P = (Fo2 + 2Fc2)/3 |
2375 reflections | (Δ/σ)max < 0.001 |
139 parameters | Δρmax = 0.45 e Å−3 |
0 restraints | Δρmin = −0.21 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 | 0.02655 (14) | |
Co2 | 0.5000 | 0.0000 | 0.5000 | 0.03055 (15) | |
N2 | 0.0715 (3) | 0.11345 (17) | 0.12131 (19) | 0.0367 (5) | |
H2A | 0.1822 | 0.1162 | 0.1297 | 0.044* | |
H2B | 0.0341 | 0.1791 | 0.0939 | 0.044* | |
N5 | 0.4247 (3) | 0.06444 (19) | 0.2321 (2) | 0.0467 (6) | |
N3 | 0.1235 (3) | 0.06265 (17) | −0.12925 (19) | 0.0360 (5) | |
H3A | 0.2253 | 0.0819 | −0.0952 | 0.043* | |
C1 | 0.3830 (3) | 0.1246 (2) | 0.5507 (2) | 0.0377 (6) | |
N1 | 0.1847 (2) | −0.09322 (17) | 0.06332 (19) | 0.0368 (5) | |
H1A | 0.2057 | −0.1430 | 0.0061 | 0.044* | |
H1B | 0.2754 | −0.0518 | 0.0790 | 0.044* | |
C2 | 0.3061 (3) | −0.0870 (2) | 0.4933 (2) | 0.0379 (6) | |
C3 | 0.4522 (3) | 0.0401 (2) | 0.3325 (3) | 0.0356 (6) | |
C4 | 0.1435 (4) | −0.0223 (2) | −0.2228 (3) | 0.0509 (8) | |
H4A | 0.2362 | −0.0688 | −0.1961 | 0.061* | |
H4B | 0.1668 | 0.0123 | −0.2993 | 0.061* | |
N4 | 0.1920 (3) | −0.1426 (2) | 0.4907 (2) | 0.0582 (7) | |
N6 | 0.3179 (3) | 0.1998 (2) | 0.5828 (2) | 0.0549 (7) | |
C5 | 0.0369 (4) | 0.1642 (2) | −0.1764 (3) | 0.0474 (7) | |
H5A | 0.0662 | 0.1796 | −0.2587 | 0.057* | |
H5B | 0.0719 | 0.2257 | −0.1243 | 0.057* | |
C6 | 0.0090 (4) | 0.0908 (3) | 0.2439 (3) | 0.0496 (8) | |
H6A | 0.0919 | 0.0522 | 0.2962 | 0.060* | |
H6B | −0.0161 | 0.1590 | 0.2837 | 0.060* | |
C7 | 0.1460 (3) | −0.1508 (2) | 0.1782 (3) | 0.0478 (7) | |
H7A | 0.1869 | −0.1084 | 0.2494 | 0.057* | |
H7B | 0.1991 | −0.2219 | 0.1829 | 0.057* | |
O1W | 0.4440 (3) | 0.14114 (18) | −0.0152 (2) | 0.0616 (6) | |
H1C | 0.4445 | 0.1199 | 0.0600 | 0.074* | |
H1D | 0.4182 | 0.2086 | −0.0085 | 0.074* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0266 (2) | 0.0281 (3) | 0.0250 (3) | −0.00121 (19) | 0.00239 (19) | −0.0012 (2) |
Co2 | 0.0348 (3) | 0.0294 (3) | 0.0272 (3) | −0.0029 (2) | 0.0010 (2) | 0.0009 (2) |
N2 | 0.0343 (12) | 0.0381 (13) | 0.0376 (13) | −0.0030 (9) | 0.0022 (10) | −0.0069 (10) |
N5 | 0.0491 (14) | 0.0543 (17) | 0.0354 (14) | −0.0038 (12) | −0.0039 (11) | 0.0030 (12) |
N3 | 0.0370 (12) | 0.0409 (14) | 0.0306 (11) | −0.0061 (10) | 0.0050 (10) | −0.0001 (10) |
C1 | 0.0456 (16) | 0.0344 (16) | 0.0337 (15) | −0.0027 (13) | 0.0078 (13) | 0.0052 (13) |
N1 | 0.0348 (12) | 0.0351 (13) | 0.0400 (13) | 0.0023 (10) | −0.0007 (10) | −0.0015 (10) |
C2 | 0.0418 (16) | 0.0420 (17) | 0.0295 (14) | −0.0048 (13) | −0.0005 (12) | −0.0006 (12) |
C3 | 0.0336 (14) | 0.0368 (14) | 0.0366 (16) | −0.0018 (12) | 0.0041 (12) | −0.0010 (13) |
C4 | 0.0506 (18) | 0.059 (2) | 0.0455 (17) | 0.0006 (14) | 0.0196 (15) | −0.0047 (15) |
N4 | 0.0603 (17) | 0.0658 (19) | 0.0483 (16) | −0.0197 (14) | 0.0030 (13) | −0.0019 (13) |
N6 | 0.0690 (18) | 0.0362 (15) | 0.0621 (18) | 0.0001 (13) | 0.0208 (15) | 0.0034 (13) |
C5 | 0.062 (2) | 0.0379 (17) | 0.0423 (17) | −0.0068 (14) | 0.0061 (15) | 0.0076 (13) |
C6 | 0.0568 (19) | 0.0556 (19) | 0.0371 (17) | −0.0026 (15) | 0.0070 (14) | −0.0078 (14) |
C7 | 0.0543 (19) | 0.0442 (18) | 0.0427 (18) | 0.0029 (14) | −0.0074 (15) | 0.0047 (14) |
O1W | 0.0590 (13) | 0.0648 (15) | 0.0610 (14) | −0.0014 (11) | 0.0057 (11) | 0.0007 (11) |
Geometric parameters (Å, º) top
Co1—N3 | 1.960 (2) | C1—N6 | 1.132 (3) |
Co1—N3i | 1.960 (2) | N1—C7 | 1.496 (3) |
Co1—N1i | 1.965 (2) | N1—H1A | 0.9000 |
Co1—N1 | 1.965 (2) | N1—H1B | 0.9000 |
Co1—N2 | 1.971 (2) | C2—N4 | 1.150 (3) |
Co1—N2i | 1.971 (2) | C4—C6i | 1.499 (4) |
Co2—C2ii | 1.900 (3) | C4—H4A | 0.9700 |
Co2—C2 | 1.900 (3) | C4—H4B | 0.9700 |
Co2—C3 | 1.903 (3) | C5—C7i | 1.498 (4) |
Co2—C3ii | 1.903 (3) | C5—H5A | 0.9700 |
Co2—C1 | 1.903 (3) | C5—H5B | 0.9700 |
Co2—C1ii | 1.903 (3) | C6—C4i | 1.499 (4) |
N2—C6 | 1.500 (3) | C6—H6A | 0.9700 |
N2—H2A | 0.9000 | C6—H6B | 0.9700 |
N2—H2B | 0.9000 | C7—C5i | 1.498 (4) |
N5—C3 | 1.141 (3) | C7—H7A | 0.9700 |
N3—C4 | 1.476 (4) | C7—H7B | 0.9700 |
N3—C5 | 1.496 (3) | O1W—H1C | 0.8618 |
N3—H3A | 0.9100 | O1W—H1D | 0.8554 |
| | | |
N3—Co1—N3i | 180.00 (16) | C5—N3—Co1 | 108.42 (16) |
N3—Co1—N1i | 86.83 (9) | C4—N3—H3A | 108.2 |
N3i—Co1—N1i | 93.17 (9) | C5—N3—H3A | 108.2 |
N3—Co1—N1 | 93.17 (9) | Co1—N3—H3A | 108.2 |
N3i—Co1—N1 | 86.83 (9) | N6—C1—Co2 | 177.8 (3) |
N1i—Co1—N1 | 180.00 (15) | C7—N1—Co1 | 110.95 (16) |
N3—Co1—N2 | 94.05 (9) | C7—N1—H1A | 109.4 |
N3i—Co1—N2 | 85.95 (9) | Co1—N1—H1A | 109.4 |
N1i—Co1—N2 | 90.12 (9) | C7—N1—H1B | 109.4 |
N1—Co1—N2 | 89.88 (9) | Co1—N1—H1B | 109.4 |
N3—Co1—N2i | 85.95 (9) | H1A—N1—H1B | 108.0 |
N3i—Co1—N2i | 94.05 (9) | N4—C2—Co2 | 177.7 (3) |
N1i—Co1—N2i | 89.88 (9) | N5—C3—Co2 | 179.5 (3) |
N1—Co1—N2i | 90.12 (9) | N3—C4—C6i | 111.0 (2) |
N2—Co1—N2i | 180.00 (17) | N3—C4—H4A | 109.4 |
C2ii—Co2—C2 | 180.00 (13) | C6i—C4—H4A | 109.4 |
C2ii—Co2—C3 | 89.62 (11) | N3—C4—H4B | 109.4 |
C2—Co2—C3 | 90.38 (11) | C6i—C4—H4B | 109.4 |
C2ii—Co2—C3ii | 90.38 (11) | H4A—C4—H4B | 108.0 |
C2—Co2—C3ii | 89.62 (11) | N3—C5—C7i | 110.6 (2) |
C3—Co2—C3ii | 180.00 (6) | N3—C5—H5A | 109.5 |
C2ii—Co2—C1 | 88.69 (11) | C7i—C5—H5A | 109.5 |
C2—Co2—C1 | 91.31 (11) | N3—C5—H5B | 109.5 |
C3—Co2—C1 | 90.50 (11) | C7i—C5—H5B | 109.5 |
C3ii—Co2—C1 | 89.50 (11) | H5A—C5—H5B | 108.1 |
C2ii—Co2—C1ii | 91.31 (11) | C4i—C6—N2 | 107.9 (2) |
C2—Co2—C1ii | 88.69 (11) | C4i—C6—H6A | 110.1 |
C3—Co2—C1ii | 89.50 (11) | N2—C6—H6A | 110.1 |
C3ii—Co2—C1ii | 90.50 (11) | C4i—C6—H6B | 110.1 |
C1—Co2—C1ii | 180.00 (15) | N2—C6—H6B | 110.1 |
C6—N2—Co1 | 111.62 (16) | H6A—C6—H6B | 108.4 |
C6—N2—H2A | 109.3 | N1—C7—C5i | 108.8 (2) |
Co1—N2—H2A | 109.3 | N1—C7—H7A | 109.9 |
C6—N2—H2B | 109.3 | C5i—C7—H7A | 109.9 |
Co1—N2—H2B | 109.3 | N1—C7—H7B | 109.9 |
H2A—N2—H2B | 108.0 | C5i—C7—H7B | 109.9 |
C4—N3—C5 | 114.9 (2) | H7A—C7—H7B | 108.3 |
C4—N3—Co1 | 108.65 (16) | H1C—O1W—H1D | 101.0 |
| | | |
N3—Co1—N2—C6 | −176.25 (18) | N3i—Co1—N1—C7 | −5.96 (17) |
N3i—Co1—N2—C6 | 3.75 (18) | N1i—Co1—N1—C7 | −53 (51) |
N1i—Co1—N2—C6 | 96.92 (18) | N2—Co1—N1—C7 | 79.99 (18) |
N1—Co1—N2—C6 | −83.08 (18) | N2i—Co1—N1—C7 | −100.01 (18) |
N2i—Co1—N2—C6 | −8.2 (2) | C2ii—Co2—C2—N4 | 8 (68) |
N3i—Co1—N3—C4 | 15 (100) | C3—Co2—C2—N4 | 127 (6) |
N1i—Co1—N3—C4 | −109.02 (19) | C3ii—Co2—C2—N4 | −53 (6) |
N1—Co1—N3—C4 | 70.98 (19) | C1—Co2—C2—N4 | −142 (6) |
N2—Co1—N3—C4 | 161.08 (18) | C1ii—Co2—C2—N4 | 38 (6) |
N2i—Co1—N3—C4 | −18.92 (18) | C2ii—Co2—C3—N5 | 15 (33) |
N3i—Co1—N3—C5 | 140 (100) | C2—Co2—C3—N5 | −165 (100) |
N1i—Co1—N3—C5 | 16.51 (17) | C3ii—Co2—C3—N5 | −100 (100) |
N1—Co1—N3—C5 | −163.49 (17) | C1—Co2—C3—N5 | 104 (33) |
N2—Co1—N3—C5 | −73.38 (17) | C1ii—Co2—C3—N5 | −76 (33) |
N2i—Co1—N3—C5 | 106.62 (17) | C5—N3—C4—C6i | −83.2 (3) |
C2ii—Co2—C1—N6 | −29 (7) | Co1—N3—C4—C6i | 38.5 (3) |
C2—Co2—C1—N6 | 151 (7) | C4—N3—C5—C7i | 85.6 (3) |
C3—Co2—C1—N6 | −118 (7) | Co1—N3—C5—C7i | −36.1 (3) |
C3ii—Co2—C1—N6 | 62 (7) | Co1—N2—C6—C4i | −25.1 (3) |
C1ii—Co2—C1—N6 | 143 (33) | Co1—N1—C7—C5i | 27.1 (3) |
N3—Co1—N1—C7 | 174.04 (17) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···N5 | 0.90 | 2.27 | 3.083 (3) | 149 |
N2—H2B···N6iii | 0.90 | 2.30 | 3.082 (3) | 146 |
O1W—H1D···N4iv | 0.86 | 2.04 | 2.886 (3) | 168 |
N3—H3A···O1W | 0.91 | 2.05 | 2.955 (3) | 174 |
N1—H1A···N6v | 0.90 | 2.15 | 2.990 (3) | 154 |
N1—H1B···N5 | 0.90 | 2.44 | 3.212 (3) | 144 |
O1W—H1C···N5 | 0.86 | 2.02 | 2.879 (3) | 175 |
Symmetry codes: (iii) x−1/2, −y+1/2, z−1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) −x+1/2, y−1/2, −z+1/2. |
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