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The ions and water molecules of the title compound, [Co(C
4H
13N
3)
2]Cl
2·H
2O, are held together through both electrostatic interactions and N—H
O, N—H
Cl and O—H
Cl hydrogen bonds.
Supporting information
CCDC reference: 609327
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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·H2O | F(000) = 748 |
Mr = 354.19 | Dx = 1.453 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3117 reflections |
a = 13.459 (4) Å | θ = 2.8–26.5° |
b = 8.817 (3) Å | µ = 1.39 mm−1 |
c = 13.951 (4) Å | T = 298 K |
β = 102.097 (4)° | Block, amaranth |
V = 1618.8 (8) Å3 | 0.55 × 0.52 × 0.44 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX area-detector diffractometer | 2865 independent reflections |
Radiation source: fine-focus sealed tube | 2167 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
φ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −13→16 |
Tmin = 0.461, Tmax = 0.552 | k = −10→8 |
8122 measured reflections | l = −16→16 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H 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 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.35 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.23756 (3) | 0.38919 (5) | 0.43651 (3) | 0.02817 (15) | |
Cl1 | 0.46202 (6) | 0.72024 (11) | 0.35863 (6) | 0.0480 (2) | |
Cl2 | 0.09185 (6) | 0.45032 (11) | 0.70239 (6) | 0.0477 (3) | |
N1 | 0.29626 (19) | 0.4191 (3) | 0.59595 (18) | 0.0341 (6) | |
H1A | 0.2476 | 0.3964 | 0.6291 | 0.041* | |
H1B | 0.3497 | 0.3575 | 0.6168 | 0.041* | |
N2 | 0.25384 (19) | 0.6292 (3) | 0.44274 (17) | 0.0344 (6) | |
H2 | 0.3152 | 0.6526 | 0.4289 | 0.041* | |
N3 | 0.1674 (2) | 0.4476 (3) | 0.28461 (19) | 0.0502 (8) | |
H3A | 0.1987 | 0.3975 | 0.2431 | 0.060* | |
H3B | 0.1014 | 0.4207 | 0.2715 | 0.060* | |
N4 | 0.3884 (2) | 0.3349 (3) | 0.41557 (19) | 0.0399 (7) | |
H4A | 0.4042 | 0.3946 | 0.3686 | 0.048* | |
H4B | 0.4343 | 0.3514 | 0.4715 | 0.048* | |
N5 | 0.22410 (19) | 0.1488 (3) | 0.42213 (18) | 0.0331 (6) | |
H5 | 0.1923 | 0.1270 | 0.3595 | 0.040* | |
N6 | 0.08617 (19) | 0.3562 (3) | 0.46929 (18) | 0.0360 (6) | |
H6A | 0.0855 | 0.3915 | 0.5297 | 0.043* | |
H6B | 0.0394 | 0.4075 | 0.4258 | 0.043* | |
O1 | 0.6153 (3) | 0.9604 (5) | 0.2997 (3) | 0.0687 (9) | |
C1 | 0.3274 (3) | 0.5789 (4) | 0.6126 (2) | 0.0439 (9) | |
H1C | 0.3957 | 0.5921 | 0.6018 | 0.053* | |
H1D | 0.3273 | 0.6069 | 0.6798 | 0.053* | |
C2 | 0.2550 (3) | 0.6792 (4) | 0.5435 (2) | 0.0431 (8) | |
H2A | 0.1874 | 0.6718 | 0.5570 | 0.052* | |
H2B | 0.2770 | 0.7841 | 0.5519 | 0.052* | |
C3 | 0.1747 (3) | 0.6936 (4) | 0.3650 (2) | 0.0448 (9) | |
H3C | 0.1869 | 0.8009 | 0.3578 | 0.054* | |
H3D | 0.1087 | 0.6816 | 0.3816 | 0.054* | |
C4 | 0.1766 (3) | 0.6125 (4) | 0.2715 (2) | 0.0490 (9) | |
H4C | 0.1210 | 0.6479 | 0.2205 | 0.059* | |
H4D | 0.2398 | 0.6345 | 0.2513 | 0.059* | |
C5 | 0.3910 (3) | 0.1747 (4) | 0.3868 (3) | 0.0471 (9) | |
H5A | 0.4604 | 0.1378 | 0.4025 | 0.057* | |
H5B | 0.3660 | 0.1649 | 0.3166 | 0.057* | |
C6 | 0.3264 (2) | 0.0826 (4) | 0.4400 (3) | 0.0430 (9) | |
H6C | 0.3229 | −0.0214 | 0.4169 | 0.052* | |
H6D | 0.3558 | 0.0826 | 0.5097 | 0.052* | |
C7 | 0.1585 (3) | 0.1003 (4) | 0.4877 (3) | 0.0438 (8) | |
H7A | 0.1925 | 0.1160 | 0.5554 | 0.053* | |
H7B | 0.1426 | −0.0067 | 0.4782 | 0.053* | |
C8 | 0.0622 (3) | 0.1935 (4) | 0.4638 (3) | 0.0500 (9) | |
H8A | 0.0250 | 0.1686 | 0.3984 | 0.060* | |
H8B | 0.0195 | 0.1693 | 0.5098 | 0.060* | |
H1 | 0.587 (3) | 1.020 (5) | 0.267 (3) | 0.055 (15)* | |
H3 | 0.566 (5) | 0.909 (6) | 0.308 (4) | 0.12 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0247 (2) | 0.0307 (2) | 0.0285 (2) | 0.00202 (18) | 0.00431 (17) | 0.00033 (17) |
Cl1 | 0.0321 (5) | 0.0552 (6) | 0.0551 (5) | −0.0004 (4) | 0.0056 (4) | 0.0055 (4) |
Cl2 | 0.0332 (5) | 0.0733 (6) | 0.0352 (4) | 0.0048 (4) | 0.0043 (4) | 0.0060 (4) |
N1 | 0.0273 (14) | 0.0411 (17) | 0.0331 (13) | 0.0027 (12) | 0.0047 (11) | 0.0019 (12) |
N2 | 0.0240 (14) | 0.0356 (16) | 0.0434 (15) | −0.0003 (11) | 0.0066 (12) | 0.0059 (12) |
N3 | 0.061 (2) | 0.0523 (19) | 0.0332 (14) | 0.0064 (16) | 0.0018 (14) | 0.0008 (14) |
N4 | 0.0315 (15) | 0.0483 (17) | 0.0425 (15) | 0.0025 (13) | 0.0141 (13) | 0.0055 (13) |
N5 | 0.0288 (14) | 0.0345 (15) | 0.0342 (13) | 0.0008 (11) | 0.0025 (11) | −0.0050 (11) |
N6 | 0.0259 (14) | 0.0419 (17) | 0.0373 (14) | 0.0057 (12) | 0.0001 (12) | −0.0036 (12) |
O1 | 0.062 (2) | 0.082 (3) | 0.065 (2) | −0.002 (2) | 0.0209 (17) | 0.0169 (19) |
C1 | 0.038 (2) | 0.051 (2) | 0.0394 (18) | −0.0062 (17) | 0.0001 (15) | −0.0090 (16) |
C2 | 0.045 (2) | 0.0345 (19) | 0.050 (2) | −0.0019 (16) | 0.0107 (17) | −0.0094 (16) |
C3 | 0.0347 (19) | 0.039 (2) | 0.056 (2) | 0.0040 (16) | −0.0022 (16) | 0.0098 (17) |
C4 | 0.039 (2) | 0.061 (2) | 0.0427 (19) | 0.0067 (18) | 0.0009 (16) | 0.0217 (18) |
C5 | 0.039 (2) | 0.054 (2) | 0.049 (2) | 0.0104 (18) | 0.0130 (17) | −0.0080 (18) |
C6 | 0.037 (2) | 0.037 (2) | 0.054 (2) | 0.0097 (15) | 0.0064 (17) | −0.0044 (16) |
C7 | 0.041 (2) | 0.0324 (18) | 0.061 (2) | −0.0050 (16) | 0.0173 (17) | 0.0013 (16) |
C8 | 0.0275 (18) | 0.055 (2) | 0.069 (2) | −0.0083 (17) | 0.0114 (17) | −0.010 (2) |
Geometric parameters (Å, º) top
Co1—N2 | 2.128 (3) | N6—H6B | 0.9000 |
Co1—N5 | 2.133 (3) | O1—H1 | 0.74 (4) |
Co1—N4 | 2.164 (3) | O1—H3 | 0.84 (6) |
Co1—N3 | 2.193 (3) | C1—C2 | 1.505 (5) |
Co1—N6 | 2.199 (3) | C1—H1C | 0.9700 |
Co1—N1 | 2.215 (2) | C1—H1D | 0.9700 |
N1—C1 | 1.474 (4) | C2—H2A | 0.9700 |
N1—H1A | 0.9000 | C2—H2B | 0.9700 |
N1—H1B | 0.9000 | C3—C4 | 1.492 (5) |
N2—C3 | 1.466 (4) | C3—H3C | 0.9700 |
N2—C2 | 1.470 (4) | C3—H3D | 0.9700 |
N2—H2 | 0.9100 | C4—H4C | 0.9700 |
N3—C4 | 1.474 (4) | C4—H4D | 0.9700 |
N3—H3A | 0.9000 | C5—C6 | 1.496 (5) |
N3—H3B | 0.9000 | C5—H5A | 0.9700 |
N4—C5 | 1.471 (4) | C5—H5B | 0.9700 |
N4—H4A | 0.9000 | C6—H6C | 0.9700 |
N4—H4B | 0.9000 | C6—H6D | 0.9700 |
N5—C7 | 1.462 (4) | C7—C8 | 1.511 (5) |
N5—C6 | 1.469 (4) | C7—H7A | 0.9700 |
N5—H5 | 0.9100 | C7—H7B | 0.9700 |
N6—C8 | 1.469 (4) | C8—H8A | 0.9700 |
N6—H6A | 0.9000 | C8—H8B | 0.9700 |
| | | |
N2—Co1—N5 | 176.58 (10) | H6A—N6—H6B | 108.3 |
N2—Co1—N4 | 97.69 (10) | H1—O1—H3 | 99 (5) |
N5—Co1—N4 | 80.29 (10) | N1—C1—C2 | 109.7 (3) |
N2—Co1—N3 | 79.96 (10) | N1—C1—H1C | 109.7 |
N5—Co1—N3 | 97.57 (10) | C2—C1—H1C | 109.7 |
N4—Co1—N3 | 98.50 (11) | N1—C1—H1D | 109.7 |
N2—Co1—N6 | 102.41 (10) | C2—C1—H1D | 109.7 |
N5—Co1—N6 | 79.87 (10) | H1C—C1—H1D | 108.2 |
N4—Co1—N6 | 159.25 (11) | N2—C2—C1 | 108.2 (3) |
N3—Co1—N6 | 90.09 (11) | N2—C2—H2A | 110.1 |
N2—Co1—N1 | 80.11 (9) | C1—C2—H2A | 110.1 |
N5—Co1—N1 | 102.61 (9) | N2—C2—H2B | 110.1 |
N4—Co1—N1 | 90.84 (10) | C1—C2—H2B | 110.1 |
N3—Co1—N1 | 158.94 (11) | H2A—C2—H2B | 108.4 |
N6—Co1—N1 | 87.59 (10) | N2—C3—C4 | 108.6 (3) |
C1—N1—Co1 | 107.55 (19) | N2—C3—H3C | 110.0 |
C1—N1—H1A | 110.2 | C4—C3—H3C | 110.0 |
Co1—N1—H1A | 110.2 | N2—C3—H3D | 110.0 |
C1—N1—H1B | 110.2 | C4—C3—H3D | 110.0 |
Co1—N1—H1B | 110.2 | H3C—C3—H3D | 108.4 |
H1A—N1—H1B | 108.5 | N3—C4—C3 | 110.3 (3) |
C3—N2—C2 | 116.9 (3) | N3—C4—H4C | 109.6 |
C3—N2—Co1 | 107.58 (19) | C3—C4—H4C | 109.6 |
C2—N2—Co1 | 108.53 (19) | N3—C4—H4D | 109.6 |
C3—N2—H2 | 107.9 | C3—C4—H4D | 109.6 |
C2—N2—H2 | 107.9 | H4C—C4—H4D | 108.1 |
Co1—N2—H2 | 107.9 | N4—C5—C6 | 109.7 (3) |
C4—N3—Co1 | 108.7 (2) | N4—C5—H5A | 109.7 |
C4—N3—H3A | 109.9 | C6—C5—H5A | 109.7 |
Co1—N3—H3A | 109.9 | N4—C5—H5B | 109.7 |
C4—N3—H3B | 109.9 | C6—C5—H5B | 109.7 |
Co1—N3—H3B | 109.9 | H5A—C5—H5B | 108.2 |
H3A—N3—H3B | 108.3 | N5—C6—C5 | 108.8 (3) |
C5—N4—Co1 | 109.0 (2) | N5—C6—H6C | 109.9 |
C5—N4—H4A | 109.9 | C5—C6—H6C | 109.9 |
Co1—N4—H4A | 109.9 | N5—C6—H6D | 109.9 |
C5—N4—H4B | 109.9 | C5—C6—H6D | 109.9 |
Co1—N4—H4B | 109.9 | H6C—C6—H6D | 108.3 |
H4A—N4—H4B | 108.3 | N5—C7—C8 | 107.8 (3) |
C7—N5—C6 | 116.4 (3) | N5—C7—H7A | 110.1 |
C7—N5—Co1 | 106.42 (19) | C8—C7—H7A | 110.1 |
C6—N5—Co1 | 108.7 (2) | N5—C7—H7B | 110.1 |
C7—N5—H5 | 108.3 | C8—C7—H7B | 110.1 |
C6—N5—H5 | 108.3 | H7A—C7—H7B | 108.5 |
Co1—N5—H5 | 108.3 | N6—C8—C7 | 110.6 (3) |
C8—N6—Co1 | 108.7 (2) | N6—C8—H8A | 109.5 |
C8—N6—H6A | 109.9 | C7—C8—H8A | 109.5 |
Co1—N6—H6A | 109.9 | N6—C8—H8B | 109.5 |
C8—N6—H6B | 109.9 | C7—C8—H8B | 109.5 |
Co1—N6—H6B | 109.9 | H8A—C8—H8B | 108.1 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H3···Cl1 | 0.83 (6) | 2.38 (6) | 3.186 (3) | 164 (5) |
O1—H1···Cl1i | 0.75 (4) | 2.48 (4) | 3.201 (4) | 164 (4) |
N6—H6B···Cl2ii | 0.90 | 2.56 | 3.461 (3) | 178 |
N6—H6A···Cl2 | 0.90 | 2.45 | 3.341 (3) | 172 |
N5—H5···Cl2iii | 0.91 | 2.42 | 3.323 (3) | 172 |
N4—H4B···Cl1iv | 0.90 | 2.56 | 3.399 (3) | 155 |
N4—H4A···O1v | 0.90 | 2.38 | 3.189 (4) | 150 |
N2—H2···Cl1 | 0.91 | 2.46 | 3.354 (3) | 169 |
N1—H1B···Cl1iv | 0.90 | 2.58 | 3.411 (3) | 154 |
N1—H1A···Cl2 | 0.90 | 2.56 | 3.401 (3) | 155 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z−1/2; (iv) −x+1, −y+1, −z+1; (v) −x+1, y−1/2, −z+1/2. |
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