Hexakis(1H-imidazole-κN3)­cobalt(II) dichloride tetrahydrate

Zhu, H.-L.; Yang, S.; Qiu, X.-Y.; Xiong, Z.-D.; You, Z.-L.; Wang, D.-Q.

doi:10.1107/S1600536803024747

Hexakis(1H-imidazole-κN³)cobalt(II) dichloride tetrahydrate

H.-L. Zhu, S. Yang, X.-Y. Qiu, Z.-D. Xiong, Z.-L. You and D.-Q. Wang

In the title compound, [Co(C₃H₄N₂)₆]Cl₂·4H₂O, the Co^II atom is situated on an inversion center. It is coordinated by six N atoms of six imidazole ligands and has a slightly distorted octahedral geometry. In the crystal structure, the Cl atoms, the water molecules of crystallization and the imidazole NH groups contribute to the formation of a three-dimensional hydrogen-bonded network.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024747/su6044sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024747/su6044Isup2.hkl Contains datablock I

CCDC reference: 227735

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
R factor = 0.044
wR factor = 0.131
Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT415_ALERT_2_B Short Inter D-H..H-X       H2C    ..  H4A      =       1.98 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H1C    ..  H1C      =       1.86 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT417_ALERT_2_C Short Inter D-H..H-D       H1B    ..  H2C      =       2.14 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          5
            N1  -CO1 -N1  -C1    159.00100.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            N1  -CO1 -N1  -C3    -16.00100.00   2.555   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  -C4     45.00100.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16
            N3  -CO1 -N3  -C6   -137.00100.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         23
            N5  -CO1 -N5  -C7    143.00 43.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         28
            N5  -CO1 -N5  -C9    -40.00 43.00   2.555   1.555   1.555   1.555

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART'; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.

hexakis(1H-imidazole-κN³)cobalt(II) dichloride tetrahydrate top

Crystal data top

[Co(C₃H₄N₂)₆]Cl₂·4H₂O	Z = 1
M_r = 610.39	F(000) = 317
Triclinic, P1	D_x = 1.412 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.783 (4) Å	Cell parameters from 2655 reflections
b = 9.064 (4) Å	θ = 2.6–26.4°
c = 10.575 (5) Å	µ = 0.83 mm⁻¹
α = 75.156 (5)°	T = 298 K
β = 83.105 (6)°	Prism, dark-purple
γ = 61.848 (5)°	0.42 × 0.35 × 0.21 mm
V = 717.6 (5) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	2494 independent reflections
Radiation source: fine-focus sealed tube	2186 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
φ and ω scans	θ_max = 25.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→9
T_min = 0.715, T_max = 0.843	k = −10→6
3747 measured reflections	l = −12→12

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.131	H-atom parameters constrained
S = 1.23	w = 1/[σ²(F_o²) + (0.0758P)² + 0.1518P] where P = (F_o² + 2F_c²)/3
2494 reflections	(Δ/σ)_max = 0.001
169 parameters	Δρ_max = 0.51 e Å⁻³
0 restraints	Δρ_min = −0.62 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	U_iso*/U_eq
Co1	0.0000	0.0000	0.0000	0.0304 (2)
Cl1	0.69765 (10)	0.79337 (9)	0.50424 (7)	0.0466 (2)
N1	−0.1962 (3)	0.1467 (3)	0.1260 (2)	0.0363 (5)
N2	−0.3865 (4)	0.2055 (4)	0.2831 (3)	0.0565 (7)
H2B	−0.4485	0.1895	0.3547	0.080*
N3	−0.0033 (3)	0.2348 (3)	−0.1172 (2)	0.0377 (5)
N4	−0.0731 (4)	0.4702 (3)	−0.2698 (3)	0.0555 (7)
H4B	−0.1243	0.5541	−0.3408	0.080*
N5	0.2020 (3)	−0.0356 (3)	0.1216 (2)	0.0375 (5)
N6	0.3305 (4)	−0.0234 (4)	0.2801 (3)	0.0593 (8)
H6B	0.3456	0.0037	0.3522	0.080*
O1	0.0390 (4)	0.8257 (4)	0.5242 (3)	0.0781 (8)
H1B	0.1282	0.7943	0.5684	0.080*
H1C	−0.0471	0.9238	0.5223	0.080*
O2	0.6659 (4)	0.4564 (4)	0.5110 (4)	0.1004 (11)
H2C	0.7570	0.3846	0.5549	0.080*
H2D	0.6258	0.5632	0.5064	0.080*
C1	−0.2612 (4)	0.0825 (4)	0.2300 (3)	0.0457 (7)
H1A	−0.2227	−0.0384	0.2639	0.080*
C2	−0.4038 (5)	0.3578 (5)	0.2085 (4)	0.0617 (9)
H2A	−0.4829	0.4700	0.2221	0.080*
C3	−0.2864 (4)	0.3211 (4)	0.1122 (3)	0.0501 (8)
H3A	−0.2688	0.4045	0.0437	0.080*
C4	−0.0997 (4)	0.3337 (4)	−0.2212 (3)	0.0461 (7)
H4A	−0.1790	0.3101	−0.2573	0.080*
C5	0.0461 (5)	0.4600 (5)	−0.1939 (4)	0.0658 (10)
H5A	0.0907	0.5408	−0.2041	0.080*
C6	0.0888 (5)	0.3155 (4)	−0.0999 (3)	0.0519 (8)
H6A	0.1715	0.2743	−0.0315	0.080*
C7	0.1799 (4)	0.0277 (4)	0.2247 (3)	0.0470 (7)
H7A	0.0694	0.1017	0.2557	0.080*
C8	0.4568 (5)	−0.1253 (6)	0.2100 (4)	0.0677 (11)
H8A	0.5787	−0.1814	0.2264	0.080*
C9	0.3775 (4)	−0.1317 (5)	0.1115 (3)	0.0527 (8)
H9A	0.4344	−0.1932	0.0442	0.080*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0316 (3)	0.0325 (3)	0.0252 (3)	−0.0142 (2)	−0.00077 (19)	−0.0042 (2)
Cl1	0.0483 (4)	0.0453 (4)	0.0413 (4)	−0.0204 (3)	−0.0006 (3)	−0.0040 (3)
N1	0.0359 (12)	0.0417 (12)	0.0307 (12)	−0.0169 (10)	0.0013 (9)	−0.0095 (10)
N2	0.0508 (16)	0.075 (2)	0.0481 (16)	−0.0309 (15)	0.0207 (12)	−0.0261 (15)
N3	0.0390 (12)	0.0368 (12)	0.0343 (12)	−0.0167 (10)	0.0024 (10)	−0.0059 (10)
N4	0.0624 (17)	0.0408 (14)	0.0498 (16)	−0.0210 (13)	−0.0070 (13)	0.0091 (12)
N5	0.0383 (12)	0.0418 (13)	0.0326 (12)	−0.0191 (11)	−0.0034 (9)	−0.0058 (10)
N6	0.0655 (18)	0.085 (2)	0.0439 (15)	−0.0434 (17)	−0.0068 (13)	−0.0207 (15)
O1	0.0591 (16)	0.0806 (19)	0.100 (2)	−0.0295 (14)	0.0066 (14)	−0.0373 (17)
O2	0.0719 (19)	0.0640 (18)	0.165 (3)	−0.0239 (15)	−0.028 (2)	−0.027 (2)
C1	0.0478 (17)	0.0558 (18)	0.0359 (16)	−0.0264 (15)	0.0072 (13)	−0.0125 (14)
C2	0.054 (2)	0.055 (2)	0.065 (2)	−0.0136 (17)	0.0149 (17)	−0.0262 (18)
C3	0.0543 (18)	0.0429 (17)	0.0464 (18)	−0.0182 (15)	0.0088 (14)	−0.0113 (14)
C4	0.0475 (17)	0.0416 (16)	0.0418 (16)	−0.0191 (14)	−0.0054 (13)	0.0021 (13)
C5	0.086 (3)	0.052 (2)	0.067 (2)	−0.044 (2)	−0.009 (2)	0.0014 (17)
C6	0.063 (2)	0.0493 (18)	0.0479 (18)	−0.0329 (16)	−0.0088 (15)	−0.0003 (14)
C7	0.0528 (18)	0.0545 (18)	0.0378 (16)	−0.0258 (15)	−0.0026 (13)	−0.0134 (14)
C8	0.0461 (19)	0.099 (3)	0.065 (2)	−0.034 (2)	−0.0095 (17)	−0.025 (2)
C9	0.0389 (16)	0.067 (2)	0.0508 (19)	−0.0193 (15)	−0.0047 (13)	−0.0187 (16)

Geometric parameters (Å, º) top

Co1—N3ⁱ	2.160 (2)	N6—C8	1.349 (5)
Co1—N3	2.160 (2)	N6—H6B	0.9000
Co1—N5	2.168 (2)	O1—H1B	0.8500
Co1—N5ⁱ	2.168 (2)	O1—H1C	0.8500
Co1—N1ⁱ	2.170 (2)	O2—H2C	0.8500
Co1—N1	2.170 (2)	O2—H2D	0.8500
N1—C1	1.307 (4)	C1—H1A	0.9600
N1—C3	1.370 (4)	C2—C3	1.346 (5)
N2—C1	1.336 (4)	C2—H2A	0.9599
N2—C2	1.351 (5)	C3—H3A	0.9600
N2—H2B	0.9000	C4—H4A	0.9599
N3—C4	1.316 (4)	C5—C6	1.343 (5)
N3—C6	1.373 (4)	C5—H5A	0.9600
N4—C4	1.329 (4)	C6—H6A	0.9600
N4—C5	1.350 (5)	C7—H7A	0.9600
N4—H4B	0.9000	C8—C9	1.348 (5)
N5—C7	1.312 (4)	C8—H8A	0.9600
N5—C9	1.374 (4)	C9—H9A	0.9600
N6—C7	1.332 (4)

N3ⁱ—Co1—N3	180.00 (17)	C7—N6—H6B	126.3
N3ⁱ—Co1—N5	89.87 (9)	C8—N6—H6B	125.8
N3—Co1—N5	90.13 (9)	H1B—O1—H1C	120.0
N3ⁱ—Co1—N5ⁱ	90.13 (9)	H2C—O2—H2D	120.0
N3—Co1—N5ⁱ	89.87 (9)	N1—C1—N2	111.7 (3)
N5—Co1—N5ⁱ	180.00 (9)	N1—C1—H1A	123.9
N3ⁱ—Co1—N1ⁱ	89.58 (9)	N2—C1—H1A	124.5
N3—Co1—N1ⁱ	90.42 (9)	C3—C2—N2	106.3 (3)
N5—Co1—N1ⁱ	89.39 (9)	C3—C2—H2A	126.7
N5ⁱ—Co1—N1ⁱ	90.61 (9)	N2—C2—H2A	127.0
N3ⁱ—Co1—N1	90.42 (9)	C2—C3—N1	109.7 (3)
N3—Co1—N1	89.58 (9)	C2—C3—H3A	125.2
N5—Co1—N1	90.61 (9)	N1—C3—H3A	125.0
N5ⁱ—Co1—N1	89.39 (9)	N3—C4—N4	111.3 (3)
N1ⁱ—Co1—N1	180.00 (14)	N3—C4—H4A	124.3
C1—N1—C3	105.0 (2)	N4—C4—H4A	124.4
C1—N1—Co1	125.5 (2)	C6—C5—N4	106.5 (3)
C3—N1—Co1	129.3 (2)	C6—C5—H5A	126.6
C1—N2—C2	107.3 (3)	N4—C5—H5A	126.9
C1—N2—H2B	126.2	C5—C6—N3	109.5 (3)
C2—N2—H2B	126.5	C5—C6—H6A	125.4
C4—N3—C6	105.1 (3)	N3—C6—H6A	125.2
C4—N3—Co1	126.2 (2)	N5—C7—N6	111.2 (3)
C6—N3—Co1	128.7 (2)	N5—C7—H7A	124.2
C4—N4—C5	107.6 (3)	N6—C7—H7A	124.6
C4—N4—H4B	126.5	C9—C8—N6	106.2 (3)
C5—N4—H4B	125.9	C9—C8—H8A	126.7
C7—N5—C9	105.2 (2)	N6—C8—H8A	127.1
C7—N5—Co1	126.3 (2)	C8—C9—N5	109.5 (3)
C9—N5—Co1	128.4 (2)	C8—C9—H9A	125.5
C7—N6—C8	107.9 (3)	N5—C9—H9A	125.0

N3ⁱ—Co1—N1—C1	1.6 (2)	N3—Co1—N5—C9	−95.3 (3)
N3—Co1—N1—C1	−178.4 (2)	N5ⁱ—Co1—N5—C9	−40 (43)
N5—Co1—N1—C1	−88.3 (2)	N1ⁱ—Co1—N5—C9	−4.8 (3)
N5ⁱ—Co1—N1—C1	91.7 (2)	N1—Co1—N5—C9	175.2 (3)
N1ⁱ—Co1—N1—C1	159 (100)	C3—N1—C1—N2	−0.3 (3)
N3ⁱ—Co1—N1—C3	−173.6 (3)	Co1—N1—C1—N2	−176.42 (19)
N3—Co1—N1—C3	6.4 (3)	C2—N2—C1—N1	0.4 (4)
N5—Co1—N1—C3	96.5 (3)	C1—N2—C2—C3	−0.3 (4)
N5ⁱ—Co1—N1—C3	−83.5 (3)	N2—C2—C3—N1	0.2 (4)
N1ⁱ—Co1—N1—C3	−16 (100)	C1—N1—C3—C2	0.1 (4)
N3ⁱ—Co1—N3—C4	45 (100)	Co1—N1—C3—C2	176.0 (2)
N5—Co1—N3—C4	177.8 (2)	C6—N3—C4—N4	0.2 (4)
N5ⁱ—Co1—N3—C4	−2.2 (2)	Co1—N3—C4—N4	179.0 (2)
N1ⁱ—Co1—N3—C4	88.4 (2)	C5—N4—C4—N3	−0.1 (4)
N1—Co1—N3—C4	−91.6 (2)	C4—N4—C5—C6	−0.1 (4)
N3ⁱ—Co1—N3—C6	−137 (100)	N4—C5—C6—N3	0.2 (4)
N5—Co1—N3—C6	−3.7 (3)	C4—N3—C6—C5	−0.2 (4)
N5ⁱ—Co1—N3—C6	176.3 (3)	Co1—N3—C6—C5	−179.0 (2)
N1ⁱ—Co1—N3—C6	−93.1 (3)	C9—N5—C7—N6	−0.3 (4)
N1—Co1—N3—C6	86.9 (3)	Co1—N5—C7—N6	177.7 (2)
N3ⁱ—Co1—N5—C7	−92.8 (3)	C8—N6—C7—N5	−0.2 (4)
N3—Co1—N5—C7	87.2 (3)	C7—N6—C8—C9	0.5 (4)
N5ⁱ—Co1—N5—C7	143 (43)	N6—C8—C9—N5	−0.7 (4)
N1ⁱ—Co1—N5—C7	177.6 (3)	C7—N5—C9—C8	0.6 (4)
N1—Co1—N5—C7	−2.4 (3)	Co1—N5—C9—C8	−177.3 (2)
N3ⁱ—Co1—N5—C9	84.7 (3)

Symmetry code: (i) −x, −y, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2B···Cl1ⁱⁱ	0.90	2.46	3.322 (3)	161
N4—H4B···Cl1ⁱⁱⁱ	0.90	2.33	3.217 (3)	169
N6—H6B···Cl1^iv	0.90	2.54	3.380 (3)	155
O1—H1B···O2^iv	0.85	2.42	2.720 (4)	101
O1—H1C···O1^v	0.85	2.23	2.815 (6)	126
O2—H2C···O1^iv	0.85	2.19	2.720 (4)	121
O2—H2D···Cl1	0.85	2.44	3.178 (3)	145

Symmetry codes: (ii) −x, −y+1, −z+1; (iii) x−1, y, z−1; (iv) −x+1, −y+1, −z+1; (v) −x, −y+2, −z+1.

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Hexakis(1H-imidazole-κN3)­cobalt(II) dichloride tetrahydrate

Supporting information

Key indicators

checkCIF/PLATON results

Hexakis(1H-imidazole-κN³)cobalt(II) dichloride tetrahydrate