Tris­(pyridine-2-carboxyl­ato-κ2O,N)­cobalt(III) monohydrate

Fu, A.-Y.; Wang, D.-Q.

doi:10.1107/S160053680500317X

Tris(pyridine-2-carboxylato-κ²O,N)cobalt(III) monohydrate

In the title complex, [Co(C₆H₄O₂N)₃]·H₂O, the cobalt(III) ion shows a distorted octahedral coordination, comprising three N-atom donors and three O-atom donors from three bidentate pyridine-2-carboxylate ligands. The uncoordinated water molecule interacts with nearby carboxyl groups of the pyridine-2-carboxylate ligands by way of O—H

O hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680500317X/hb6144sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680500317X/hb6144Isup2.hkl Contains datablock I

CCDC reference: 193852

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.006 Å
R factor = 0.050
wR factor = 0.066
Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct...         12
PLAT350_ALERT_3_C Short   C-H Bond (0.96A)   C9     -   H5     ...       0.84 Ang.

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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

Tris(pyridine-2-carboxylato-κ²0,N)cobalt(III) monohydrate top

Crystal data top

[Co(C₆H₄NO₂)₃]·H₂O	F(000) = 1808
M_r = 443.25	D_x = 1.696 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1193 reflections
a = 29.654 (18) Å	θ = 2.5–20.3°
b = 8.530 (5) Å	µ = 1.04 mm⁻¹
c = 13.801 (8) Å	T = 298 K
β = 95.829 (10)°	Prism, dark red
V = 3473 (4) Å³	0.28 × 0.25 × 0.18 mm
Z = 8

Data collection top

Bruker SMART CCD area-detector diffractometer	3589 independent reflections
Radiation source: fine-focus sealed tube	2020 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.059
φ and ω scans	θ_max = 26.5°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −25→37
T_min = 0.760, T_max = 0.835	k = −10→10
9671 measured reflections	l = −14→17

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.066	H atoms treated by a mixture of independent and constrained refinement
S = 0.95	w = 1/[σ²(F_o²)] where P = (F_o² + 2F_c²)/3
3589 reflections	(Δ/σ)_max = 0.001
315 parameters	Δρ_max = 0.75 e Å⁻³
3 restraints	Δρ_min = −0.49 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	0.387460 (17)	0.21873 (5)	0.87334 (3)	0.03472 (15)
N1	0.38357 (9)	0.2424 (3)	1.01036 (17)	0.0309 (7)
N2	0.33464 (9)	0.0897 (3)	0.8503 (2)	0.0329 (7)
N3	0.44347 (10)	0.3284 (3)	0.88006 (17)	0.0339 (7)
O1	0.34972 (8)	0.3952 (3)	0.86091 (15)	0.0385 (6)
O2	0.30261 (9)	0.5311 (3)	0.94475 (18)	0.0604 (8)
O3	0.38711 (8)	0.2182 (3)	0.73697 (15)	0.0405 (6)
O4	0.34080 (9)	0.1683 (3)	0.60350 (17)	0.0628 (9)
O5	0.42424 (8)	0.0394 (3)	0.88591 (15)	0.0402 (6)
O6	0.49517 (9)	−0.0402 (3)	0.87981 (19)	0.0582 (8)
O7	0.39030 (12)	0.2557 (3)	0.4458 (2)	0.0775 (9)
C1	0.33287 (13)	0.4382 (4)	0.9402 (3)	0.0420 (10)
C2	0.35444 (12)	0.3561 (4)	1.0286 (3)	0.0342 (9)
C3	0.34641 (15)	0.3915 (5)	1.1230 (3)	0.0491 (12)
C4	0.36846 (16)	0.3099 (5)	1.1984 (3)	0.0537 (12)
C5	0.39892 (15)	0.1985 (5)	1.1794 (3)	0.0476 (11)
C6	0.40585 (13)	0.1656 (5)	1.0840 (3)	0.0402 (10)
C7	0.35117 (14)	0.1619 (4)	0.6921 (3)	0.0398 (10)
C8	0.32015 (12)	0.0820 (4)	0.7549 (3)	0.0338 (9)
C9	0.28190 (15)	0.0059 (5)	0.7221 (3)	0.0514 (12)
C10	0.25745 (16)	−0.0690 (5)	0.7857 (4)	0.0600 (14)
C11	0.27208 (15)	−0.0663 (5)	0.8828 (4)	0.0550 (12)
C12	0.31034 (14)	0.0165 (5)	0.9128 (3)	0.0436 (11)
C13	0.46680 (14)	0.0627 (5)	0.8806 (2)	0.0386 (10)
C14	0.47919 (12)	0.2304 (4)	0.8786 (2)	0.0348 (9)
C15	0.52188 (14)	0.2874 (5)	0.8750 (3)	0.0444 (10)
C16	0.52897 (16)	0.4446 (6)	0.8730 (3)	0.0495 (12)
C17	0.49301 (17)	0.5447 (6)	0.8751 (3)	0.0471 (11)
C18	0.45050 (15)	0.4823 (5)	0.8784 (3)	0.0441 (11)
H1	0.3284 (10)	0.467 (3)	1.132 (2)	0.033 (11)*
H2	0.3611 (10)	0.330 (3)	1.262 (2)	0.036 (10)*
H3	0.4144 (10)	0.133 (3)	1.231 (2)	0.034 (10)*
H4	0.4270 (10)	0.087 (3)	1.0652 (19)	0.033 (10)*
H5	0.2744 (10)	−0.002 (3)	0.662 (2)	0.022 (10)*
H6	0.2311 (11)	−0.119 (4)	0.762 (2)	0.041 (11)*
H7	0.2579 (12)	−0.123 (4)	0.937 (2)	0.063 (12)*
H8	0.3233 (10)	0.022 (3)	0.980 (2)	0.035 (10)*
H9	0.5435 (10)	0.216 (3)	0.8729 (19)	0.029 (10)*
H10	0.5576 (11)	0.480 (4)	0.867 (2)	0.043 (11)*
H11	0.4935 (11)	0.651 (3)	0.873 (2)	0.044 (12)*
H12	0.4244 (11)	0.536 (4)	0.881 (2)	0.050*
H13	0.3733 (9)	0.239 (3)	0.4941 (17)	0.050*
H14	0.4062 (10)	0.170 (2)	0.437 (2)	0.050*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0297 (3)	0.0420 (3)	0.0324 (3)	−0.0001 (3)	0.0031 (2)	−0.0001 (2)
N1	0.0227 (17)	0.040 (2)	0.0297 (17)	−0.0024 (15)	0.0000 (14)	0.0025 (14)
N2	0.0283 (19)	0.0422 (19)	0.0282 (18)	−0.0012 (16)	0.0035 (15)	0.0036 (14)
N3	0.040 (2)	0.0359 (19)	0.0252 (16)	−0.0055 (17)	0.0005 (14)	−0.0001 (13)
O1	0.0356 (16)	0.0473 (16)	0.0327 (15)	0.0046 (13)	0.0036 (12)	0.0017 (12)
O2	0.0481 (19)	0.069 (2)	0.0633 (18)	0.0272 (17)	0.0013 (15)	−0.0047 (15)
O3	0.0334 (15)	0.0545 (17)	0.0345 (14)	−0.0113 (14)	0.0080 (12)	−0.0031 (12)
O4	0.067 (2)	0.090 (2)	0.0303 (15)	−0.0214 (17)	0.0028 (15)	−0.0026 (14)
O5	0.0312 (16)	0.0424 (16)	0.0472 (16)	0.0010 (14)	0.0045 (13)	−0.0016 (12)
O6	0.0414 (19)	0.0473 (18)	0.086 (2)	0.0145 (16)	0.0085 (16)	−0.0046 (15)
O7	0.087 (3)	0.060 (2)	0.093 (2)	0.0067 (19)	0.0449 (19)	0.0142 (18)
C1	0.030 (2)	0.044 (3)	0.051 (3)	0.003 (2)	−0.001 (2)	−0.002 (2)
C2	0.028 (2)	0.044 (2)	0.031 (2)	0.002 (2)	0.0024 (18)	0.0004 (18)
C3	0.038 (3)	0.054 (3)	0.055 (3)	0.008 (2)	0.006 (2)	−0.013 (2)
C4	0.057 (3)	0.075 (3)	0.029 (3)	−0.012 (3)	0.004 (2)	−0.006 (2)
C5	0.054 (3)	0.053 (3)	0.034 (3)	−0.009 (2)	−0.002 (2)	0.003 (2)
C6	0.034 (3)	0.042 (3)	0.043 (3)	0.000 (2)	−0.001 (2)	0.003 (2)
C7	0.040 (3)	0.043 (3)	0.037 (2)	0.004 (2)	0.010 (2)	−0.0032 (19)
C8	0.027 (2)	0.035 (2)	0.038 (2)	0.0005 (19)	−0.0003 (19)	−0.0043 (18)
C9	0.048 (3)	0.065 (3)	0.040 (3)	−0.007 (3)	0.000 (3)	−0.007 (2)
C10	0.038 (3)	0.069 (3)	0.073 (4)	−0.024 (3)	0.003 (3)	−0.014 (3)
C11	0.044 (3)	0.064 (3)	0.058 (3)	−0.015 (3)	0.012 (3)	0.003 (2)
C12	0.035 (3)	0.055 (3)	0.041 (3)	−0.001 (2)	0.005 (2)	0.004 (2)
C13	0.040 (3)	0.042 (3)	0.034 (2)	0.003 (2)	0.005 (2)	−0.0012 (18)
C14	0.027 (2)	0.048 (3)	0.029 (2)	−0.001 (2)	0.0010 (17)	−0.0040 (18)
C15	0.039 (3)	0.051 (3)	0.044 (2)	0.006 (3)	0.006 (2)	−0.001 (2)
C16	0.036 (3)	0.067 (4)	0.047 (3)	−0.017 (3)	0.007 (2)	−0.003 (2)
C17	0.053 (3)	0.051 (3)	0.037 (2)	−0.015 (3)	0.003 (2)	0.000 (2)
C18	0.047 (3)	0.048 (3)	0.037 (2)	0.003 (2)	0.003 (2)	0.000 (2)

Geometric parameters (Å, º) top

Co1—O1	1.873 (2)	C4—C5	1.355 (5)
Co1—O5	1.877 (2)	C4—H2	0.95 (3)
Co1—O3	1.881 (2)	C5—C6	1.381 (5)
Co1—N3	1.900 (3)	C5—H3	0.98 (3)
Co1—N2	1.914 (3)	C6—H4	0.97 (3)
Co1—N1	1.917 (3)	C7—C8	1.491 (5)
N1—C6	1.328 (4)	C8—C9	1.345 (5)
N1—C2	1.339 (4)	C9—C10	1.354 (5)
N2—C12	1.334 (4)	C9—H5	0.84 (3)
N2—C8	1.345 (4)	C10—C11	1.367 (5)
N3—C18	1.330 (4)	C10—H6	0.92 (3)
N3—C14	1.351 (4)	C11—C12	1.365 (5)
O1—C1	1.301 (4)	C11—H7	1.02 (3)
O2—C1	1.204 (4)	C12—H8	0.97 (3)
O3—C7	1.271 (4)	C13—C14	1.478 (5)
O4—C7	1.231 (4)	C14—C15	1.362 (5)
O5—C13	1.287 (4)	C15—C16	1.358 (5)
O6—C13	1.217 (4)	C15—H9	0.89 (3)
O7—H13	0.887 (10)	C16—C17	1.369 (5)
O7—H14	0.886 (10)	C16—H10	0.91 (3)
C1—C2	1.494 (5)	C17—C18	1.373 (5)
C2—C3	1.381 (5)	C17—H11	0.91 (3)
C3—C4	1.362 (5)	C18—H12	0.90 (3)
C3—H1	0.85 (3)

O1—Co1—O5	178.85 (11)	C4—C5—H3	122.2 (17)
O1—Co1—O3	88.14 (10)	C6—C5—H3	118.0 (17)
O5—Co1—O3	91.99 (10)	N1—C6—C5	121.2 (4)
O1—Co1—N3	96.90 (13)	N1—C6—H4	114.9 (16)
O5—Co1—N3	84.25 (13)	C5—C6—H4	123.9 (17)
O3—Co1—N3	88.04 (10)	O4—C7—O3	125.4 (4)
O1—Co1—N2	88.59 (12)	O4—C7—C8	119.4 (4)
O5—Co1—N2	90.28 (12)	O3—C7—C8	115.2 (3)
O3—Co1—N2	84.91 (11)	N2—C8—C9	121.9 (4)
N3—Co1—N2	170.93 (11)	N2—C8—C7	113.1 (3)
O1—Co1—N1	84.86 (11)	C9—C8—C7	125.0 (4)
O5—Co1—N1	95.01 (11)	C8—C9—C10	119.9 (4)
O3—Co1—N1	172.98 (12)	C8—C9—H5	120 (2)
N3—Co1—N1	92.28 (11)	C10—C9—H5	120 (2)
N2—Co1—N1	95.41 (11)	C9—C10—C11	119.4 (4)
C6—N1—C2	119.6 (3)	C9—C10—H6	118 (2)
C6—N1—Co1	128.9 (3)	C11—C10—H6	122 (2)
C2—N1—Co1	111.5 (2)	C12—C11—C10	118.5 (4)
C12—N2—C8	118.1 (3)	C12—C11—H7	114 (2)
C12—N2—Co1	130.4 (3)	C10—C11—H7	127 (2)
C8—N2—Co1	111.4 (2)	N2—C12—C11	122.2 (4)
C18—N3—C14	119.1 (3)	N2—C12—H8	114.0 (17)
C18—N3—Co1	128.5 (3)	C11—C12—H8	123.7 (17)
C14—N3—Co1	112.2 (2)	O6—C13—O5	124.8 (4)
C1—O1—Co1	115.3 (2)	O6—C13—C14	121.7 (4)
C7—O3—Co1	114.1 (2)	O5—C13—C14	113.4 (3)
C13—O5—Co1	115.6 (2)	N3—C14—C15	120.9 (4)
H13—O7—H14	109 (2)	N3—C14—C13	113.7 (3)
O2—C1—O1	125.6 (4)	C15—C14—C13	125.5 (4)
O2—C1—C2	121.7 (4)	C16—C15—C14	120.0 (4)
O1—C1—C2	112.7 (3)	C16—C15—H9	124 (2)
N1—C2—C3	120.8 (4)	C14—C15—H9	116 (2)
N1—C2—C1	114.6 (3)	C15—C16—C17	119.5 (4)
C3—C2—C1	124.6 (4)	C15—C16—H10	118 (2)
C4—C3—C2	119.5 (4)	C17—C16—H10	122 (2)
C4—C3—H1	123 (2)	C16—C17—C18	118.6 (4)
C2—C3—H1	118 (2)	C16—C17—H11	128 (2)
C5—C4—C3	119.2 (4)	C18—C17—H11	114 (2)
C5—C4—H2	122.1 (19)	N3—C18—C17	122.0 (4)
C3—C4—H2	118.7 (19)	N3—C18—H12	111 (2)
C4—C5—C6	119.6 (4)	C17—C18—H12	127 (2)

C8—N2—N3—C14	−91.7 (3)	O1—Co1—O3—C7	−77.9 (3)
O5—Co1—N1—C2	−173.3 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H14···O5ⁱ	0.89 (1)	2.01 (2)	2.864 (4)	161 (3)
O7—H13···O4	0.89 (1)	1.97 (1)	2.845 (4)	171 (3)

Symmetry code: (i) x, −y, z−1/2.

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Tris­(pyridine-2-carboxyl­ato-κ2O,N)­cobalt(III) monohydrate

Supporting information

Key indicators

checkCIF/PLATON results

Tris(pyridine-2-carboxylato-κ²O,N)cobalt(III) monohydrate