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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051051/ng2168sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051051/ng2168Isup2.hkl
Contains datablock I

CCDC reference: 633966

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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]·2H2OF(000) = 536
Mr = 516.36Dx = 1.582 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.148 (3) ÅCell parameters from 739 reflections
b = 12.217 (4) Åθ = 2.5–27.2°
c = 10.935 (4) ŵ = 1.57 mm1
β = 94.973 (7)°T = 293 K
V = 1084.3 (6) Å3Block, yellow
Z = 20.48 × 0.31 × 0.13 mm
Data collection top
Bruker APEX area-detector
diffractometer
2375 independent reflections
Radiation source: fine-focus sealed tube1473 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 27.2°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 910
Tmin = 0.520, Tmax = 0.822k = 1515
6186 measured reflectionsl = 814
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-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 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.21 e Å3
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*/Ueq
Co10.00000.00000.00000.02655 (14)
Co20.50000.00000.50000.03055 (15)
N20.0715 (3)0.11345 (17)0.12131 (19)0.0367 (5)
H2A0.18220.11620.12970.044*
H2B0.03410.17910.09390.044*
N50.4247 (3)0.06444 (19)0.2321 (2)0.0467 (6)
N30.1235 (3)0.06265 (17)0.12925 (19)0.0360 (5)
H3A0.22530.08190.09520.043*
C10.3830 (3)0.1246 (2)0.5507 (2)0.0377 (6)
N10.1847 (2)0.09322 (17)0.06332 (19)0.0368 (5)
H1A0.20570.14300.00610.044*
H1B0.27540.05180.07900.044*
C20.3061 (3)0.0870 (2)0.4933 (2)0.0379 (6)
C30.4522 (3)0.0401 (2)0.3325 (3)0.0356 (6)
C40.1435 (4)0.0223 (2)0.2228 (3)0.0509 (8)
H4A0.23620.06880.19610.061*
H4B0.16680.01230.29930.061*
N40.1920 (3)0.1426 (2)0.4907 (2)0.0582 (7)
N60.3179 (3)0.1998 (2)0.5828 (2)0.0549 (7)
C50.0369 (4)0.1642 (2)0.1764 (3)0.0474 (7)
H5A0.06620.17960.25870.057*
H5B0.07190.22570.12430.057*
C60.0090 (4)0.0908 (3)0.2439 (3)0.0496 (8)
H6A0.09190.05220.29620.060*
H6B0.01610.15900.28370.060*
C70.1460 (3)0.1508 (2)0.1782 (3)0.0478 (7)
H7A0.18690.10840.24940.057*
H7B0.19910.22190.18290.057*
O1W0.4440 (3)0.14114 (18)0.0152 (2)0.0616 (6)
H1C0.44450.11990.06000.074*
H1D0.41820.20860.00850.074*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0266 (2)0.0281 (3)0.0250 (3)0.00121 (19)0.00239 (19)0.0012 (2)
Co20.0348 (3)0.0294 (3)0.0272 (3)0.0029 (2)0.0010 (2)0.0009 (2)
N20.0343 (12)0.0381 (13)0.0376 (13)0.0030 (9)0.0022 (10)0.0069 (10)
N50.0491 (14)0.0543 (17)0.0354 (14)0.0038 (12)0.0039 (11)0.0030 (12)
N30.0370 (12)0.0409 (14)0.0306 (11)0.0061 (10)0.0050 (10)0.0001 (10)
C10.0456 (16)0.0344 (16)0.0337 (15)0.0027 (13)0.0078 (13)0.0052 (13)
N10.0348 (12)0.0351 (13)0.0400 (13)0.0023 (10)0.0007 (10)0.0015 (10)
C20.0418 (16)0.0420 (17)0.0295 (14)0.0048 (13)0.0005 (12)0.0006 (12)
C30.0336 (14)0.0368 (14)0.0366 (16)0.0018 (12)0.0041 (12)0.0010 (13)
C40.0506 (18)0.059 (2)0.0455 (17)0.0006 (14)0.0196 (15)0.0047 (15)
N40.0603 (17)0.0658 (19)0.0483 (16)0.0197 (14)0.0030 (13)0.0019 (13)
N60.0690 (18)0.0362 (15)0.0621 (18)0.0001 (13)0.0208 (15)0.0034 (13)
C50.062 (2)0.0379 (17)0.0423 (17)0.0068 (14)0.0061 (15)0.0076 (13)
C60.0568 (19)0.0556 (19)0.0371 (17)0.0026 (15)0.0070 (14)0.0078 (14)
C70.0543 (19)0.0442 (18)0.0427 (18)0.0029 (14)0.0074 (15)0.0047 (14)
O1W0.0590 (13)0.0648 (15)0.0610 (14)0.0014 (11)0.0057 (11)0.0007 (11)
Geometric parameters (Å, º) top
Co1—N31.960 (2)C1—N61.132 (3)
Co1—N3i1.960 (2)N1—C71.496 (3)
Co1—N1i1.965 (2)N1—H1A0.9000
Co1—N11.965 (2)N1—H1B0.9000
Co1—N21.971 (2)C2—N41.150 (3)
Co1—N2i1.971 (2)C4—C6i1.499 (4)
Co2—C2ii1.900 (3)C4—H4A0.9700
Co2—C21.900 (3)C4—H4B0.9700
Co2—C31.903 (3)C5—C7i1.498 (4)
Co2—C3ii1.903 (3)C5—H5A0.9700
Co2—C11.903 (3)C5—H5B0.9700
Co2—C1ii1.903 (3)C6—C4i1.499 (4)
N2—C61.500 (3)C6—H6A0.9700
N2—H2A0.9000C6—H6B0.9700
N2—H2B0.9000C7—C5i1.498 (4)
N5—C31.141 (3)C7—H7A0.9700
N3—C41.476 (4)C7—H7B0.9700
N3—C51.496 (3)O1W—H1C0.8618
N3—H3A0.9100O1W—H1D0.8554
N3—Co1—N3i180.00 (16)C5—N3—Co1108.42 (16)
N3—Co1—N1i86.83 (9)C4—N3—H3A108.2
N3i—Co1—N1i93.17 (9)C5—N3—H3A108.2
N3—Co1—N193.17 (9)Co1—N3—H3A108.2
N3i—Co1—N186.83 (9)N6—C1—Co2177.8 (3)
N1i—Co1—N1180.00 (15)C7—N1—Co1110.95 (16)
N3—Co1—N294.05 (9)C7—N1—H1A109.4
N3i—Co1—N285.95 (9)Co1—N1—H1A109.4
N1i—Co1—N290.12 (9)C7—N1—H1B109.4
N1—Co1—N289.88 (9)Co1—N1—H1B109.4
N3—Co1—N2i85.95 (9)H1A—N1—H1B108.0
N3i—Co1—N2i94.05 (9)N4—C2—Co2177.7 (3)
N1i—Co1—N2i89.88 (9)N5—C3—Co2179.5 (3)
N1—Co1—N2i90.12 (9)N3—C4—C6i111.0 (2)
N2—Co1—N2i180.00 (17)N3—C4—H4A109.4
C2ii—Co2—C2180.00 (13)C6i—C4—H4A109.4
C2ii—Co2—C389.62 (11)N3—C4—H4B109.4
C2—Co2—C390.38 (11)C6i—C4—H4B109.4
C2ii—Co2—C3ii90.38 (11)H4A—C4—H4B108.0
C2—Co2—C3ii89.62 (11)N3—C5—C7i110.6 (2)
C3—Co2—C3ii180.00 (6)N3—C5—H5A109.5
C2ii—Co2—C188.69 (11)C7i—C5—H5A109.5
C2—Co2—C191.31 (11)N3—C5—H5B109.5
C3—Co2—C190.50 (11)C7i—C5—H5B109.5
C3ii—Co2—C189.50 (11)H5A—C5—H5B108.1
C2ii—Co2—C1ii91.31 (11)C4i—C6—N2107.9 (2)
C2—Co2—C1ii88.69 (11)C4i—C6—H6A110.1
C3—Co2—C1ii89.50 (11)N2—C6—H6A110.1
C3ii—Co2—C1ii90.50 (11)C4i—C6—H6B110.1
C1—Co2—C1ii180.00 (15)N2—C6—H6B110.1
C6—N2—Co1111.62 (16)H6A—C6—H6B108.4
C6—N2—H2A109.3N1—C7—C5i108.8 (2)
Co1—N2—H2A109.3N1—C7—H7A109.9
C6—N2—H2B109.3C5i—C7—H7A109.9
Co1—N2—H2B109.3N1—C7—H7B109.9
H2A—N2—H2B108.0C5i—C7—H7B109.9
C4—N3—C5114.9 (2)H7A—C7—H7B108.3
C4—N3—Co1108.65 (16)H1C—O1W—H1D101.0
N3—Co1—N2—C6176.25 (18)N3i—Co1—N1—C75.96 (17)
N3i—Co1—N2—C63.75 (18)N1i—Co1—N1—C753 (51)
N1i—Co1—N2—C696.92 (18)N2—Co1—N1—C779.99 (18)
N1—Co1—N2—C683.08 (18)N2i—Co1—N1—C7100.01 (18)
N2i—Co1—N2—C68.2 (2)C2ii—Co2—C2—N48 (68)
N3i—Co1—N3—C415 (100)C3—Co2—C2—N4127 (6)
N1i—Co1—N3—C4109.02 (19)C3ii—Co2—C2—N453 (6)
N1—Co1—N3—C470.98 (19)C1—Co2—C2—N4142 (6)
N2—Co1—N3—C4161.08 (18)C1ii—Co2—C2—N438 (6)
N2i—Co1—N3—C418.92 (18)C2ii—Co2—C3—N515 (33)
N3i—Co1—N3—C5140 (100)C2—Co2—C3—N5165 (100)
N1i—Co1—N3—C516.51 (17)C3ii—Co2—C3—N5100 (100)
N1—Co1—N3—C5163.49 (17)C1—Co2—C3—N5104 (33)
N2—Co1—N3—C573.38 (17)C1ii—Co2—C3—N576 (33)
N2i—Co1—N3—C5106.62 (17)C5—N3—C4—C6i83.2 (3)
C2ii—Co2—C1—N629 (7)Co1—N3—C4—C6i38.5 (3)
C2—Co2—C1—N6151 (7)C4—N3—C5—C7i85.6 (3)
C3—Co2—C1—N6118 (7)Co1—N3—C5—C7i36.1 (3)
C3ii—Co2—C1—N662 (7)Co1—N2—C6—C4i25.1 (3)
C1ii—Co2—C1—N6143 (33)Co1—N1—C7—C5i27.1 (3)
N3—Co1—N1—C7174.04 (17)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···N50.902.273.083 (3)149
N2—H2B···N6iii0.902.303.082 (3)146
O1W—H1D···N4iv0.862.042.886 (3)168
N3—H3A···O1W0.912.052.955 (3)174
N1—H1A···N6v0.902.152.990 (3)154
N1—H1B···N50.902.443.212 (3)144
O1W—H1C···N50.862.022.879 (3)175
Symmetry codes: (iii) x1/2, y+1/2, z1/2; (iv) x+1/2, y+1/2, z+1/2; (v) x+1/2, y1/2, z+1/2.
 

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