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The ions and water molecules of the title compound, [Co(C4H13N3)2]Cl2·H2O, are held together through both electrostatic inter­actions and N—H...O, N—H...Cl and O—H...Cl hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806035896/hy2011sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806035896/hy2011Isup2.hkl
Contains datablock I

CCDC reference: 609327

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.035
  • wR factor = 0.098
  • Data-to-parameter ratio = 16.7

checkCIF/PLATON results

No syntax errors found



Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. amaranth CRYSC01_ALERT_1_C No recognised colour has been given for crystal colour. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N6 .. 5.13 su PLAT245_ALERT_2_C U(iso) H1 Smaller than U(eq) O1 by ... 0.01 AngSq PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3B ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

bis(diethylenetriamine-κ3N)cobalt(II) dichloride monohydrate top
Crystal data top
[Co(C4H13N3)2]Cl2·H2OF(000) = 748
Mr = 354.19Dx = 1.453 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3117 reflections
a = 13.459 (4) Åθ = 2.8–26.5°
b = 8.817 (3) ŵ = 1.39 mm1
c = 13.951 (4) ÅT = 298 K
β = 102.097 (4)°Block, amaranth
V = 1618.8 (8) Å30.55 × 0.52 × 0.44 mm
Z = 4
Data collection top
Bruker SMART APEX area-detector
diffractometer
2865 independent reflections
Radiation source: fine-focus sealed tube2167 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
φ and ω scansθmax = 25.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 1316
Tmin = 0.461, Tmax = 0.552k = 108
8122 measured reflectionsl = 1616
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0425P)2 + 0.5627P]
where P = (Fo2 + 2Fc2)/3
2863 reflections(Δ/σ)max = 0.002
171 parametersΔρmax = 0.48 e Å3
0 restraintsΔρmin = 0.35 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.23756 (3)0.38919 (5)0.43651 (3)0.02817 (15)
Cl10.46202 (6)0.72024 (11)0.35863 (6)0.0480 (2)
Cl20.09185 (6)0.45032 (11)0.70239 (6)0.0477 (3)
N10.29626 (19)0.4191 (3)0.59595 (18)0.0341 (6)
H1A0.24760.39640.62910.041*
H1B0.34970.35750.61680.041*
N20.25384 (19)0.6292 (3)0.44274 (17)0.0344 (6)
H20.31520.65260.42890.041*
N30.1674 (2)0.4476 (3)0.28461 (19)0.0502 (8)
H3A0.19870.39750.24310.060*
H3B0.10140.42070.27150.060*
N40.3884 (2)0.3349 (3)0.41557 (19)0.0399 (7)
H4A0.40420.39460.36860.048*
H4B0.43430.35140.47150.048*
N50.22410 (19)0.1488 (3)0.42213 (18)0.0331 (6)
H50.19230.12700.35950.040*
N60.08617 (19)0.3562 (3)0.46929 (18)0.0360 (6)
H6A0.08550.39150.52970.043*
H6B0.03940.40750.42580.043*
O10.6153 (3)0.9604 (5)0.2997 (3)0.0687 (9)
C10.3274 (3)0.5789 (4)0.6126 (2)0.0439 (9)
H1C0.39570.59210.60180.053*
H1D0.32730.60690.67980.053*
C20.2550 (3)0.6792 (4)0.5435 (2)0.0431 (8)
H2A0.18740.67180.55700.052*
H2B0.27700.78410.55190.052*
C30.1747 (3)0.6936 (4)0.3650 (2)0.0448 (9)
H3C0.18690.80090.35780.054*
H3D0.10870.68160.38160.054*
C40.1766 (3)0.6125 (4)0.2715 (2)0.0490 (9)
H4C0.12100.64790.22050.059*
H4D0.23980.63450.25130.059*
C50.3910 (3)0.1747 (4)0.3868 (3)0.0471 (9)
H5A0.46040.13780.40250.057*
H5B0.36600.16490.31660.057*
C60.3264 (2)0.0826 (4)0.4400 (3)0.0430 (9)
H6C0.32290.02140.41690.052*
H6D0.35580.08260.50970.052*
C70.1585 (3)0.1003 (4)0.4877 (3)0.0438 (8)
H7A0.19250.11600.55540.053*
H7B0.14260.00670.47820.053*
C80.0622 (3)0.1935 (4)0.4638 (3)0.0500 (9)
H8A0.02500.16860.39840.060*
H8B0.01950.16930.50980.060*
H10.587 (3)1.020 (5)0.267 (3)0.055 (15)*
H30.566 (5)0.909 (6)0.308 (4)0.12 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0247 (2)0.0307 (2)0.0285 (2)0.00202 (18)0.00431 (17)0.00033 (17)
Cl10.0321 (5)0.0552 (6)0.0551 (5)0.0004 (4)0.0056 (4)0.0055 (4)
Cl20.0332 (5)0.0733 (6)0.0352 (4)0.0048 (4)0.0043 (4)0.0060 (4)
N10.0273 (14)0.0411 (17)0.0331 (13)0.0027 (12)0.0047 (11)0.0019 (12)
N20.0240 (14)0.0356 (16)0.0434 (15)0.0003 (11)0.0066 (12)0.0059 (12)
N30.061 (2)0.0523 (19)0.0332 (14)0.0064 (16)0.0018 (14)0.0008 (14)
N40.0315 (15)0.0483 (17)0.0425 (15)0.0025 (13)0.0141 (13)0.0055 (13)
N50.0288 (14)0.0345 (15)0.0342 (13)0.0008 (11)0.0025 (11)0.0050 (11)
N60.0259 (14)0.0419 (17)0.0373 (14)0.0057 (12)0.0001 (12)0.0036 (12)
O10.062 (2)0.082 (3)0.065 (2)0.002 (2)0.0209 (17)0.0169 (19)
C10.038 (2)0.051 (2)0.0394 (18)0.0062 (17)0.0001 (15)0.0090 (16)
C20.045 (2)0.0345 (19)0.050 (2)0.0019 (16)0.0107 (17)0.0094 (16)
C30.0347 (19)0.039 (2)0.056 (2)0.0040 (16)0.0022 (16)0.0098 (17)
C40.039 (2)0.061 (2)0.0427 (19)0.0067 (18)0.0009 (16)0.0217 (18)
C50.039 (2)0.054 (2)0.049 (2)0.0104 (18)0.0130 (17)0.0080 (18)
C60.037 (2)0.037 (2)0.054 (2)0.0097 (15)0.0064 (17)0.0044 (16)
C70.041 (2)0.0324 (18)0.061 (2)0.0050 (16)0.0173 (17)0.0013 (16)
C80.0275 (18)0.055 (2)0.069 (2)0.0083 (17)0.0114 (17)0.010 (2)
Geometric parameters (Å, º) top
Co1—N22.128 (3)N6—H6B0.9000
Co1—N52.133 (3)O1—H10.74 (4)
Co1—N42.164 (3)O1—H30.84 (6)
Co1—N32.193 (3)C1—C21.505 (5)
Co1—N62.199 (3)C1—H1C0.9700
Co1—N12.215 (2)C1—H1D0.9700
N1—C11.474 (4)C2—H2A0.9700
N1—H1A0.9000C2—H2B0.9700
N1—H1B0.9000C3—C41.492 (5)
N2—C31.466 (4)C3—H3C0.9700
N2—C21.470 (4)C3—H3D0.9700
N2—H20.9100C4—H4C0.9700
N3—C41.474 (4)C4—H4D0.9700
N3—H3A0.9000C5—C61.496 (5)
N3—H3B0.9000C5—H5A0.9700
N4—C51.471 (4)C5—H5B0.9700
N4—H4A0.9000C6—H6C0.9700
N4—H4B0.9000C6—H6D0.9700
N5—C71.462 (4)C7—C81.511 (5)
N5—C61.469 (4)C7—H7A0.9700
N5—H50.9100C7—H7B0.9700
N6—C81.469 (4)C8—H8A0.9700
N6—H6A0.9000C8—H8B0.9700
N2—Co1—N5176.58 (10)H6A—N6—H6B108.3
N2—Co1—N497.69 (10)H1—O1—H399 (5)
N5—Co1—N480.29 (10)N1—C1—C2109.7 (3)
N2—Co1—N379.96 (10)N1—C1—H1C109.7
N5—Co1—N397.57 (10)C2—C1—H1C109.7
N4—Co1—N398.50 (11)N1—C1—H1D109.7
N2—Co1—N6102.41 (10)C2—C1—H1D109.7
N5—Co1—N679.87 (10)H1C—C1—H1D108.2
N4—Co1—N6159.25 (11)N2—C2—C1108.2 (3)
N3—Co1—N690.09 (11)N2—C2—H2A110.1
N2—Co1—N180.11 (9)C1—C2—H2A110.1
N5—Co1—N1102.61 (9)N2—C2—H2B110.1
N4—Co1—N190.84 (10)C1—C2—H2B110.1
N3—Co1—N1158.94 (11)H2A—C2—H2B108.4
N6—Co1—N187.59 (10)N2—C3—C4108.6 (3)
C1—N1—Co1107.55 (19)N2—C3—H3C110.0
C1—N1—H1A110.2C4—C3—H3C110.0
Co1—N1—H1A110.2N2—C3—H3D110.0
C1—N1—H1B110.2C4—C3—H3D110.0
Co1—N1—H1B110.2H3C—C3—H3D108.4
H1A—N1—H1B108.5N3—C4—C3110.3 (3)
C3—N2—C2116.9 (3)N3—C4—H4C109.6
C3—N2—Co1107.58 (19)C3—C4—H4C109.6
C2—N2—Co1108.53 (19)N3—C4—H4D109.6
C3—N2—H2107.9C3—C4—H4D109.6
C2—N2—H2107.9H4C—C4—H4D108.1
Co1—N2—H2107.9N4—C5—C6109.7 (3)
C4—N3—Co1108.7 (2)N4—C5—H5A109.7
C4—N3—H3A109.9C6—C5—H5A109.7
Co1—N3—H3A109.9N4—C5—H5B109.7
C4—N3—H3B109.9C6—C5—H5B109.7
Co1—N3—H3B109.9H5A—C5—H5B108.2
H3A—N3—H3B108.3N5—C6—C5108.8 (3)
C5—N4—Co1109.0 (2)N5—C6—H6C109.9
C5—N4—H4A109.9C5—C6—H6C109.9
Co1—N4—H4A109.9N5—C6—H6D109.9
C5—N4—H4B109.9C5—C6—H6D109.9
Co1—N4—H4B109.9H6C—C6—H6D108.3
H4A—N4—H4B108.3N5—C7—C8107.8 (3)
C7—N5—C6116.4 (3)N5—C7—H7A110.1
C7—N5—Co1106.42 (19)C8—C7—H7A110.1
C6—N5—Co1108.7 (2)N5—C7—H7B110.1
C7—N5—H5108.3C8—C7—H7B110.1
C6—N5—H5108.3H7A—C7—H7B108.5
Co1—N5—H5108.3N6—C8—C7110.6 (3)
C8—N6—Co1108.7 (2)N6—C8—H8A109.5
C8—N6—H6A109.9C7—C8—H8A109.5
Co1—N6—H6A109.9N6—C8—H8B109.5
C8—N6—H6B109.9C7—C8—H8B109.5
Co1—N6—H6B109.9H8A—C8—H8B108.1
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H3···Cl10.83 (6)2.38 (6)3.186 (3)164 (5)
O1—H1···Cl1i0.75 (4)2.48 (4)3.201 (4)164 (4)
N6—H6B···Cl2ii0.902.563.461 (3)178
N6—H6A···Cl20.902.453.341 (3)172
N5—H5···Cl2iii0.912.423.323 (3)172
N4—H4B···Cl1iv0.902.563.399 (3)155
N4—H4A···O1v0.902.383.189 (4)150
N2—H2···Cl10.912.463.354 (3)169
N1—H1B···Cl1iv0.902.583.411 (3)154
N1—H1A···Cl20.902.563.401 (3)155
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y+1, z+1; (iii) x, y+1/2, z1/2; (iv) x+1, y+1, z+1; (v) x+1, y1/2, z+1/2.
 

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