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The title compound, [Co(C18H23N10)](BF4)2·H2O, is the result of complexing a Co cation (initially in a CoII state) with tris­[2-(1H-imidazol-2-ylmethyl­eneamino)eth­yl]amine (L), obtained by a condensation process involving imidazole-2-carbaldehyde and tris­(2-amino­ethyl)amine. Both the Co cation and the ligand were modified in the synthesis process, the cation via oxidation to CoIII, and the ligand via deprotonation to convert it into the 2-(2-{bis­[2-(1H-imidazol-2-ylmethyl­eneamino)eth­yl]amino}ethyl­imino­meth­yl)imidazolide anion (L). The ligand chelates the metal centre in a hexa­dentate fashion, forming a slightly distorted octa­hedral CoN6 chromophore. Packing is governed by N—H...N hydrogen bonds defining zigzag chains. A similar structure in the literature is discussed, and the wrong assignment of the oxidation state, given therein to the Co cation, is corrected.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108033714/fg3063sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108033714/fg3063Isup2.hkl
Contains datablock I

CCDC reference: 718129

Comment top

It is well known (see e.g. Cotton & Wilkinson, 1988) that in the absence of complexing agents the CoIII species is usually not favoured in aqueous solutions containing the metal, while its stability is greatly increased when complexing agents containing nitrogen are present. Thus, it is not unusual to obtain CoIIIN6 chromophores via a synthesis procedure which starts with CoII as the initial cation, and which transforms into CoIII through an unwitting oxidation process. In such conditions, these tranformations do not require much energy and can be spontaneous and perfectly feasible, even at room temperature. We present herein the result of one such transformation, where an intended complexation of a CoII cation with tris[2-(1H-imidazol-2-ylmethyleneamino)ethyl]amine (L) obtained by condensation of imidazole-2-carbaldehyde and tris(2-aminoethyl)amine (see Experimental) resulted in the generation of the [CoIII(L-)]2+ cation through the oxidation of the metal and the simultaneous loss of an imidazole H atom. The resulting ionic species was [2-(2-{bis[2-(1H-imidazol-2-ylmethyleneamino)ethyl]amino}ethyliminomethyl) imidazolido]cobalt(III) bis(tetrafluoridoborate) monohydrate, (I), and the structure is reported herein.

Fig. 1 shows a view of (I). The CoIII centre is octahedrally surrounded by a chelating L- ligand acting in a µ1-κ6N,N',N'',N''',N'''',N''''' mode through three of its imidazolyl and three imine N atoms. The resulting coordination polyhedron is rather regular in spite of the restraints imposed by chelation, with trans angles spanning the range 173.27 (14)–176.19 (14)° and cis ones 82.49 (14)–94.80 (14)° (Table 1). Co—N distances are also in a tight range, 1.898 (3)–1.950 (3) Å, with a mean of 1.927 (24) Å, well within the expected values for CoIII—N distances reported in the literature [mean value in CoIIIN6 chromophores for 1220 cases in the 2008 version of the CSD (Allen, 2002): 1.955 (25) Å]. The cation has approximate non-crystallographic C3 symmetry, as assessed by the least-squares fit between one cation and its 120° rotated image, resulting in a mean deviation of 0.12 (1) Å (Fig. 2). The structure is completed by two well resolved, though strongly vibrating, BF4- counteranions, and a water molecule of crystallization.

From a crystallographic point of view, the most interesting feature of the structure is the formation of strong N—H···N hydrogen bonds between adjacent imidazole groups, which involves the deprotonated N22 as an acceptor and one of the protonated ones, N23, as a donor, and which appears as a distinctive feature for the CoIII presence (see discussion below). Fig. 3 shows the way in which this interaction threads a zigzag chain along [001]. The remaining imidazolyl nitrogen (N12), in turn, interacts with the pendant `water molecule + 2(BF4-) counteranions' hydrogen-bonded system shown in Fig. 1; the counterions stretch out at both sides of the [001] chains and their F atoms have weak C—H···F interactions (Table 2) between chains.

While searching in the literature for related structures, we came across a very similar Co compound (He, 2007) reported as a CoII complex with the fully protonated tris-(2-aminoethyl)amine (ligand L) in the scheme, but reported in the crystal-data text as [Co(C18H23N10)2](ClO4)2.0.5H2O, hereafter (II). This was described in the title, scheme and text as a CoII complex having two independent [CoIIL]2+ cationic groups in the asymmetric unit with charge balance provided by a four [ClO41-] counteranions; there was also one water molecule in the asymmetric unit. To our surprise, the reported Co—N distances and angles in this (He, 2007) structure were in complete agreement with those in (I) and in principle totally ascribable to a CoIII cationic centre instead of the reported CoII one. This misfit was also apparent in the reported formula, ORTEP plots and CIF coordinates, all of which confirmed that only two imidazole groups in the presumed L ligand were protonated, thus turning it into a L- anion and thus enforcing the need for a 3+ cation at the central core. All these facts support the contention that the composite cationic groups in both compounds are completely equivalent, and should have been reported as [CoIIIL-]2+ in the He (2007) paper.

While a table of hydrogen-bond data is provided in the He (2007) paper, there is no discussion or description of the hydrogen bonding in the structure of (II). Inspection of the CIF for (II) shows that the packing is defined by parallel chains extending along [100] [in this case of two different types, corresponding to the two independent cation moieties in (II)], organized through the characteristic N—H···N synthon, a fingerprint disclosing the presence of the L- ligand (and concomitantly, the CoIII cation) in these types of structures.

Related literature top

For related literature, see: Allen (2002); Cotton & Wilkinson (1988); He (2007); He et al. (2004).

Experimental top

Tris-(2-aminoethylamine) (0.0748 ml, 0.5 mmol) and imidazol-2-carbaldehyde (0.14135 g, 1.5 mmol) were dissolved in 10 ml of methanol and the solution kept at reflux while stirring for half an hour. A solution of CoCl2.6H2O, (0.11897 g, 0.5 mmol) in 10 ml of water was added to this mixture, and the composite became deep red. Finally, 0.15726 g (1.5 mmol) of NH4BF4 was added to the solution while kept at reflux for another 7 h. Slow evaporation at room temperature for 2 weeks yielded single crystals suitable for X-ray diffraction. For an alternative synthesis, see He et al. (2004).

Refinement top

All the H atoms were found in a difference Fourier, and positioned afterwards at their expected positions, while allowed to ride both in coordinates (C—H = 0.93–0.97 Å, N—H = 0.86 Å and O—H = 0.85 Å), as well as in their isotropic displacement parameters [Uiso(H) = 1.2 or 1.5Ueq(host)].

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008), PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with displacement ellipsoids at the 30% level. Hydrogen bonds are shown by broken lines.
[Figure 2] Fig. 2. A least-squares fit between one cation and its 120° rotated image, showing the non-crystallographic pseudo C3 symmetry, viewed down the pseudo C3 axis.
[Figure 3] Fig. 3. Packing view of (I) projected down [100]. Only the zigzag chains running along [001] are shown (without counterions and solvates), for clarity. N—H···H [N—H···N?] bonds are shown as dashed lines.
[2-(2-{Bis[2-(1H-imidazol-2- ylmethyleneamino)ethyl]amino}ethyliminomethyl)imidazolido]cobalt(III) bis(tetrafluoridoborate) monohydrate top
Crystal data top
[Co(C18H23N10)](BF4)2·H2OF(000) = 1280
Mr = 630.03Dx = 1.636 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9999 reflections
a = 9.1704 (9) Åθ = 2.1–26.2°
b = 18.2328 (19) ŵ = 0.76 mm1
c = 15.3594 (15) ÅT = 298 K
β = 93.843 (2)°Plate, red
V = 2562.3 (4) Å30.44 × 0.31 × 0.11 mm
Z = 4
Data collection top
Bruker SMART CCD area detector
diffractometer
5778 independent reflections
Radiation source: fine-focus sealed tube3528 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.076
CCD rotation images, thin slices scansθmax = 28.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS in SAINT-NT; Bruker, 2002)
h = 1111
Tmin = 0.70, Tmax = 0.92k = 2323
21379 measured reflectionsl = 2020
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.194H-atom parameters constrained
S = 0.93 w = 1/[σ2(Fo2) + (0.1166P)2 + 0.6005P]
where P = (Fo2 + 2Fc2)/3
5778 reflections(Δ/σ)max = 0.001
361 parametersΔρmax = 0.58 e Å3
0 restraintsΔρmin = 0.42 e Å3
Crystal data top
[Co(C18H23N10)](BF4)2·H2OV = 2562.3 (4) Å3
Mr = 630.03Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.1704 (9) ŵ = 0.76 mm1
b = 18.2328 (19) ÅT = 298 K
c = 15.3594 (15) Å0.44 × 0.31 × 0.11 mm
β = 93.843 (2)°
Data collection top
Bruker SMART CCD area detector
diffractometer
5778 independent reflections
Absorption correction: multi-scan
(SADABS in SAINT-NT; Bruker, 2002)
3528 reflections with I > 2σ(I)
Tmin = 0.70, Tmax = 0.92Rint = 0.076
21379 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0660 restraints
wR(F2) = 0.194H-atom parameters constrained
S = 0.93Δρmax = 0.58 e Å3
5778 reflectionsΔρmin = 0.42 e Å3
361 parameters
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
Co10.86211 (5)0.40146 (3)0.76323 (3)0.0392 (2)
N11.2341 (4)0.4155 (2)0.7710 (3)0.0643 (11)
N110.7339 (3)0.46309 (18)0.6917 (2)0.0432 (8)
N210.6739 (4)0.5723 (2)0.6461 (3)0.0594 (10)
H21N0.67590.61890.63780.071*
N310.9598 (4)0.49463 (19)0.7897 (2)0.0462 (8)
C110.6112 (5)0.4580 (3)0.6388 (3)0.0570 (12)
H110.56160.41490.62360.068*
C210.5724 (6)0.5253 (3)0.6117 (4)0.0696 (14)
H210.49040.53740.57570.084*
C310.7723 (5)0.5327 (2)0.6963 (3)0.0486 (10)
C410.8989 (5)0.5501 (2)0.7512 (3)0.0523 (11)
H410.93430.59760.75850.063*
C511.0876 (5)0.5046 (3)0.8506 (3)0.0606 (12)
H51A1.07890.47300.90080.073*
H51B1.09100.55500.87090.073*
C611.2281 (5)0.4868 (3)0.8083 (4)0.0686 (14)
H61A1.24180.52270.76300.082*
H61B1.30900.49190.85190.082*
N120.7513 (3)0.41238 (17)0.8624 (2)0.0426 (8)
N220.7126 (4)0.3694 (2)0.9951 (2)0.0515 (9)
N320.9849 (3)0.34084 (18)0.8425 (2)0.0418 (8)
C120.6230 (4)0.4403 (2)0.8854 (3)0.0487 (10)
H120.56160.47150.85210.058*
C220.6001 (5)0.4141 (2)0.9674 (3)0.0517 (11)
H220.51990.42520.99900.062*
C320.8005 (4)0.3704 (2)0.9299 (3)0.0431 (9)
C420.9340 (5)0.3319 (2)0.9168 (3)0.0484 (10)
H420.98010.30240.95970.058*
C521.1176 (4)0.3018 (2)0.8222 (3)0.0559 (12)
H52A1.10360.28040.76440.067*
H52B1.13560.26220.86360.067*
C621.2495 (5)0.3524 (3)0.8254 (4)0.0669 (14)
H62A1.27010.36830.88520.080*
H62B1.33330.32450.80870.080*
N130.7542 (3)0.31638 (17)0.7277 (2)0.0414 (8)
N230.7170 (4)0.22856 (19)0.6331 (2)0.0525 (9)
H23N0.72580.20060.58860.063*
N330.9679 (4)0.37837 (19)0.6608 (2)0.0460 (8)
C130.6387 (4)0.2769 (3)0.7513 (3)0.0517 (11)
H130.58430.28560.79920.062*
C230.6169 (5)0.2226 (2)0.6923 (3)0.0544 (11)
H230.54450.18690.69270.065*
C330.8004 (5)0.2863 (2)0.6565 (3)0.0445 (9)
C430.9209 (4)0.3221 (2)0.6188 (3)0.0497 (10)
H430.96080.30560.56830.060*
C531.0864 (5)0.4212 (3)0.6274 (3)0.0613 (13)
H53A1.06300.47300.63060.074*
H53B1.09560.40890.56650.074*
C631.2313 (5)0.4068 (3)0.6788 (4)0.0706 (15)
H63A1.26130.35700.66660.085*
H63B1.30400.43940.65690.085*
B10.7715 (8)0.8259 (5)0.3985 (5)0.087 (2)
F210.9170 (5)0.8209 (3)0.3895 (3)0.1396 (17)
F310.7555 (14)0.8841 (4)0.4361 (6)0.325 (7)
F410.7158 (5)0.8278 (5)0.3177 (4)0.226 (4)
F110.7348 (8)0.7692 (4)0.4460 (3)0.199 (3)
B20.1760 (11)0.6332 (4)0.5975 (6)0.100 (3)
F420.2207 (12)0.6219 (5)0.6738 (4)0.328 (7)
F120.2469 (4)0.6922 (2)0.5603 (2)0.1057 (12)
F220.0329 (6)0.6413 (3)0.5845 (3)0.1455 (17)
F320.2023 (6)0.5722 (3)0.5468 (4)0.162 (2)
O1W0.5670 (5)0.7015 (2)0.5700 (3)0.1080 (15)
H1WB0.47430.70460.56640.162*
H1WA0.59370.72630.52710.162*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0321 (3)0.0440 (3)0.0414 (3)0.0004 (2)0.0011 (2)0.0010 (2)
N10.043 (2)0.067 (3)0.082 (3)0.0013 (18)0.003 (2)0.003 (2)
N110.0355 (18)0.052 (2)0.0418 (19)0.0035 (15)0.0017 (14)0.0007 (15)
N210.058 (2)0.054 (2)0.066 (3)0.0107 (19)0.001 (2)0.0164 (19)
N310.0380 (18)0.048 (2)0.053 (2)0.0042 (15)0.0062 (16)0.0049 (16)
C110.043 (2)0.070 (3)0.056 (3)0.004 (2)0.009 (2)0.005 (2)
C210.052 (3)0.085 (4)0.070 (3)0.003 (3)0.015 (3)0.018 (3)
C310.046 (2)0.050 (3)0.051 (3)0.003 (2)0.007 (2)0.007 (2)
C410.053 (3)0.042 (2)0.061 (3)0.001 (2)0.005 (2)0.004 (2)
C510.052 (3)0.064 (3)0.064 (3)0.003 (2)0.014 (2)0.005 (2)
C610.037 (3)0.072 (3)0.096 (4)0.007 (2)0.007 (3)0.003 (3)
N120.0362 (18)0.049 (2)0.0429 (19)0.0067 (14)0.0038 (14)0.0036 (15)
N220.052 (2)0.058 (2)0.044 (2)0.0092 (17)0.0026 (17)0.0027 (17)
N320.0363 (17)0.0471 (19)0.0415 (19)0.0069 (14)0.0008 (14)0.0014 (15)
C120.041 (2)0.058 (3)0.048 (2)0.017 (2)0.0095 (19)0.003 (2)
C220.052 (3)0.054 (3)0.049 (3)0.013 (2)0.011 (2)0.005 (2)
C320.040 (2)0.052 (2)0.037 (2)0.0043 (18)0.0003 (18)0.0039 (18)
C420.045 (2)0.048 (2)0.051 (3)0.0018 (19)0.0090 (19)0.0039 (19)
C520.040 (2)0.060 (3)0.070 (3)0.020 (2)0.010 (2)0.011 (2)
C620.036 (2)0.073 (3)0.092 (4)0.013 (2)0.001 (2)0.005 (3)
N130.0382 (18)0.0433 (18)0.0427 (19)0.0054 (14)0.0021 (14)0.0040 (15)
N230.058 (2)0.056 (2)0.044 (2)0.0156 (18)0.0010 (17)0.0075 (16)
N330.0400 (19)0.050 (2)0.049 (2)0.0073 (15)0.0063 (15)0.0065 (16)
C130.037 (2)0.063 (3)0.055 (3)0.005 (2)0.010 (2)0.001 (2)
C230.052 (3)0.056 (3)0.056 (3)0.014 (2)0.001 (2)0.003 (2)
C330.046 (2)0.046 (2)0.041 (2)0.0057 (18)0.0019 (18)0.0010 (18)
C430.043 (2)0.058 (3)0.050 (2)0.001 (2)0.0173 (19)0.004 (2)
C530.052 (3)0.065 (3)0.069 (3)0.017 (2)0.018 (2)0.001 (2)
C630.051 (3)0.070 (3)0.094 (4)0.009 (2)0.032 (3)0.002 (3)
B10.065 (4)0.104 (6)0.091 (5)0.005 (4)0.002 (4)0.034 (5)
F210.114 (3)0.176 (5)0.127 (3)0.016 (3)0.004 (3)0.045 (3)
F310.603 (19)0.121 (5)0.284 (10)0.134 (8)0.269 (12)0.033 (5)
F410.115 (4)0.418 (11)0.139 (4)0.124 (5)0.050 (3)0.140 (6)
F110.259 (7)0.205 (6)0.135 (4)0.099 (5)0.022 (4)0.082 (4)
B20.127 (7)0.067 (5)0.096 (6)0.042 (5)0.060 (5)0.029 (4)
F420.530 (15)0.283 (8)0.145 (5)0.272 (10)0.178 (8)0.122 (6)
F120.115 (3)0.087 (2)0.113 (3)0.034 (2)0.011 (2)0.023 (2)
F220.121 (4)0.160 (4)0.159 (4)0.014 (3)0.030 (3)0.033 (3)
F320.169 (5)0.084 (3)0.236 (6)0.010 (3)0.038 (4)0.005 (4)
O1W0.102 (3)0.090 (3)0.132 (4)0.000 (2)0.007 (3)0.052 (3)
Geometric parameters (Å, º) top
Co1—N121.898 (3)C32—C421.438 (6)
Co1—N131.901 (3)C42—H420.9300
Co1—N111.918 (3)C52—C621.519 (6)
Co1—N321.946 (3)C52—H52A0.9700
Co1—N331.948 (3)C52—H52B0.9700
Co1—N311.950 (3)C62—H62A0.9700
N1—C611.422 (6)C62—H62B0.9700
N1—C631.424 (7)N13—C331.319 (5)
N1—C621.425 (6)N13—C131.350 (5)
N11—C311.318 (5)N23—C331.337 (5)
N11—C111.346 (5)N23—C231.339 (6)
N21—C211.347 (6)N23—H23N0.8600
N21—C311.354 (5)N33—C431.271 (5)
N21—H21N0.8600N33—C531.460 (5)
N31—C411.280 (5)C13—C231.348 (6)
N31—C511.461 (5)C13—H130.9300
C11—C211.335 (7)C23—H230.9300
C11—H110.9300C33—C431.438 (6)
C21—H210.9300C43—H430.9300
C31—C411.424 (6)C53—C631.523 (7)
C41—H410.9300C53—H53A0.9700
C51—C611.516 (7)C53—H53B0.9700
C51—H51A0.9700C63—H63A0.9700
C51—H51B0.9700C63—H63B0.9700
C61—H61A0.9700B1—F311.222 (11)
C61—H61B0.9700B1—F411.311 (9)
N12—C321.342 (5)B1—F111.320 (8)
N12—C121.350 (5)B1—F211.354 (8)
N22—C321.327 (5)B2—F421.233 (8)
N22—C221.360 (5)B2—F221.323 (10)
N32—C421.272 (5)B2—F321.388 (10)
N32—C521.461 (5)B2—F121.398 (8)
C12—C221.376 (6)O1W—H1WB0.8500
C12—H120.9300O1W—H1WA0.8497
C22—H220.9300
N12—Co1—N1391.13 (14)N22—C32—N12113.6 (4)
N12—Co1—N1193.33 (14)N22—C32—C42131.7 (4)
N13—Co1—N1191.50 (14)N12—C32—C42114.5 (4)
N12—Co1—N3282.88 (13)N32—C42—C32115.5 (4)
N13—Co1—N3289.10 (14)N32—C42—H42122.3
N11—Co1—N32176.18 (14)C32—C42—H42122.3
N12—Co1—N33173.26 (14)N32—C52—C62111.8 (4)
N13—Co1—N3382.49 (14)N32—C52—H52A109.3
N11—Co1—N3389.03 (14)C62—C52—H52A109.3
N32—Co1—N3394.79 (14)N32—C52—H52B109.3
N12—Co1—N3190.27 (14)C62—C52—H52B109.3
N13—Co1—N31173.63 (14)H52A—C52—H52B107.9
N11—Co1—N3182.21 (14)N1—C62—C52115.1 (4)
N32—Co1—N3197.24 (14)N1—C62—H62A108.5
N33—Co1—N3196.31 (14)C52—C62—H62A108.5
C61—N1—C63120.3 (5)N1—C62—H62B108.5
C61—N1—C62120.5 (5)C52—C62—H62B108.5
C63—N1—C62119.2 (4)H62A—C62—H62B107.5
C31—N11—C11107.9 (4)C33—N13—C13107.6 (3)
C31—N11—Co1112.5 (3)C33—N13—Co1112.8 (3)
C11—N11—Co1139.5 (3)C13—N13—Co1139.5 (3)
C21—N21—C31107.5 (4)C33—N23—C23106.7 (4)
C21—N21—H21N126.2C33—N23—H23N126.7
C31—N21—H21N126.2C23—N23—H23N126.7
C41—N31—C51120.3 (4)C43—N33—C53119.2 (4)
C41—N31—Co1114.3 (3)C43—N33—Co1114.5 (3)
C51—N31—Co1125.4 (3)C53—N33—Co1126.2 (3)
C21—C11—N11108.6 (4)C23—C13—N13107.1 (4)
C21—C11—H11125.7C23—C13—H13126.4
N11—C11—H11125.7N13—C13—H13126.4
C11—C21—N21107.4 (4)N23—C23—C13108.7 (4)
C11—C21—H21126.3N23—C23—H23125.7
N21—C21—H21126.3C13—C23—H23125.7
N11—C31—N21108.5 (4)N13—C33—N23109.9 (4)
N11—C31—C41116.7 (4)N13—C33—C43116.3 (4)
N21—C31—C41134.8 (4)N23—C33—C43133.7 (4)
N31—C41—C31114.3 (4)N33—C43—C33113.9 (4)
N31—C41—H41122.8N33—C43—H43123.0
C31—C41—H41122.8C33—C43—H43123.0
N31—C51—C61111.6 (4)N33—C53—C63111.7 (4)
N31—C51—H51A109.3N33—C53—H53A109.3
C61—C51—H51A109.3C63—C53—H53A109.3
N31—C51—H51B109.3N33—C53—H53B109.3
C61—C51—H51B109.3C63—C53—H53B109.3
H51A—C51—H51B108.0H53A—C53—H53B107.9
N1—C61—C51115.1 (4)N1—C63—C53117.0 (4)
N1—C61—H61A108.5N1—C63—H63A108.1
C51—C61—H61A108.5C53—C63—H63A108.1
N1—C61—H61B108.5N1—C63—H63B108.1
C51—C61—H61B108.5C53—C63—H63B108.1
H61A—C61—H61B107.5H63A—C63—H63B107.3
C32—N12—C12105.5 (3)F31—B1—F41111.8 (9)
C32—N12—Co1112.9 (3)F31—B1—F11112.1 (8)
C12—N12—Co1140.6 (3)F41—B1—F11116.5 (8)
C32—N22—C22104.0 (3)F31—B1—F21104.9 (9)
C42—N32—C52119.3 (3)F41—B1—F21103.2 (7)
C42—N32—Co1113.7 (3)F11—B1—F21107.1 (7)
C52—N32—Co1126.8 (3)F42—B2—F22115.2 (11)
N12—C12—C22107.3 (4)F42—B2—F32109.8 (9)
N12—C12—H12126.4F22—B2—F32102.3 (6)
C22—C12—H12126.4F42—B2—F12112.6 (6)
N22—C22—C12109.6 (4)F22—B2—F12109.7 (6)
N22—C22—H22125.2F32—B2—F12106.5 (8)
C12—C22—H22125.2H1WB—O1W—H1WA104.6
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···F110.852.012.814 (6)157
O1W—H1WB···F120.852.092.934 (6)170
N21—H21N···O1W0.862.052.779 (5)142
N23—H23N···N22i0.861.922.770 (5)170
C23—H23···F41ii0.932.403.181 (6)142
C41—H41···F21iii0.932.513.166 (6)127
C42—H42···F21iv0.932.473.197 (6)136
C43—H43···F22ii0.932.543.248 (7)133
C61—H61A···F42v0.972.273.213 (8)164
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x+1, y+1, z+1; (iii) x, y+3/2, z+1/2; (iv) x+2, y1/2, z+3/2; (v) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Co(C18H23N10)](BF4)2·H2O
Mr630.03
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)9.1704 (9), 18.2328 (19), 15.3594 (15)
β (°) 93.843 (2)
V3)2562.3 (4)
Z4
Radiation typeMo Kα
µ (mm1)0.76
Crystal size (mm)0.44 × 0.31 × 0.11
Data collection
DiffractometerBruker SMART CCD area detector
diffractometer
Absorption correctionMulti-scan
(SADABS in SAINT-NT; Bruker, 2002)
Tmin, Tmax0.70, 0.92
No. of measured, independent and
observed [I > 2σ(I)] reflections
21379, 5778, 3528
Rint0.076
(sin θ/λ)max1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.066, 0.194, 0.93
No. of reflections5778
No. of parameters361
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.58, 0.42

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), PLATON (Spek, 2003).

Selected geometric parameters (Å, º) top
Co1—N121.898 (3)Co1—N321.946 (3)
Co1—N131.901 (3)Co1—N331.948 (3)
Co1—N111.918 (3)Co1—N311.950 (3)
N12—Co1—N1391.13 (14)N11—Co1—N3389.03 (14)
N12—Co1—N1193.33 (14)N32—Co1—N3394.79 (14)
N13—Co1—N1191.50 (14)N12—Co1—N3190.27 (14)
N12—Co1—N3282.88 (13)N13—Co1—N31173.63 (14)
N13—Co1—N3289.10 (14)N11—Co1—N3182.21 (14)
N11—Co1—N32176.18 (14)N32—Co1—N3197.24 (14)
N12—Co1—N33173.26 (14)N33—Co1—N3196.31 (14)
N13—Co1—N3382.49 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···F110.852.012.814 (6)156.6
O1W—H1WB···F120.852.092.934 (6)169.9
N21—H21N···O1W0.862.052.779 (5)141.9
N23—H23N···N22i0.861.922.770 (5)169.5
C23—H23···F41ii0.932.403.181 (6)141.9
C41—H41···F21iii0.932.513.166 (6)127.4
C42—H42···F21iv0.932.473.197 (6)135.5
C43—H43···F22ii0.932.543.248 (7)133.0
C61—H61A···F42v0.972.273.213 (8)164.1
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x+1, y+1, z+1; (iii) x, y+3/2, z+1/2; (iv) x+2, y1/2, z+3/2; (v) x+1, y, z.
 

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