[4-Bromo-2-(pyridin-2-yl­methyl­imino­methyl)­phenolato-κ³O,N,N′]­methoxocobalt(III) perchlorate

The title Schiff base compound, [Co(C₁₃H₁₀BrN₂O)(CH₃O)]ClO₄, is a mononuclear cobalt(III) compound. The Co^III ion is coordinated by two N atoms and one O atom from a Schiff base ligand, and by another O atom from a coordinated methano­late ligand, giving an approximately square-planar geometry.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.007 Å
• Disorder in solvent or counterion
• R factor = 0.047
• wR factor = 0.134
• Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O6      ..       2.66 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O6     ..  O5'     ..       2.73 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  N1     ..  O2'     ..       2.85 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  O2     ..  C14     ..       2.91 Ang.

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl1
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      44.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7

   0 ALERT level A = In general: serious problem
   4 ALERT level B = Potentially serious problem
   4 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
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

[4-Bromo-2-(pyridin-2-ylmethyliminomethyl)phenolato- κ³O,N,N']methoxocobalt(III) perchlorate

Crystal data

[Co(C13H10BrN2O)(CH3O)]ClO4	F(000) = 952
Mr = 479.55	Dx = 1.834 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4575 reflections
a = 7.194 (2) Å	θ = 2.4–24.7°
b = 19.119 (2) Å	µ = 3.48 mm^−1
c = 12.694 (2) Å	T = 298 K
β = 95.846 (2)°	Block, brown
V = 1736.9 (6) Å^3	0.23 × 0.10 × 0.08 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	4190 independent reflections
Radiation source: fine-focus sealed tube	2962 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
ω scans	θmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
Tmin = 0.497, Tmax = 0.761	k = −25→25
20032 measured reflections	l = −16→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.134	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0602P)^2 + 1.7215P] where P = (Fo^2 + 2Fc^2)/3
4190 reflections	(Δ/σ)max = 0.001
263 parameters	Δρmax = 0.62 e Å^−3
42 restraints	Δρmin = −1.00 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.36110 (7)	0.12251 (2)	0.50987 (4)	0.03624 (15)
Br1	0.20441 (10)	0.06393 (4)	1.06605 (4)	0.0928 (3)
Cl1	0.84699 (15)	0.15842 (6)	0.45626 (9)	0.0582 (3)
O1	0.3860 (4)	0.05103 (14)	0.6141 (2)	0.0519 (7)
O2	1.0011 (14)	0.1120 (7)	0.4852 (11)	0.080 (4)	0.516 (19)
O3	0.788 (2)	0.1535 (8)	0.3481 (7)	0.100 (5)	0.516 (19)
O4	0.9158 (17)	0.2275 (4)	0.4866 (7)	0.075 (3)	0.516 (19)
O5	0.7042 (11)	0.1414 (7)	0.5215 (9)	0.078 (3)	0.516 (19)
O2'	1.0082 (16)	0.1334 (8)	0.5170 (13)	0.095 (5)	0.484 (19)
O3'	0.873 (2)	0.1587 (7)	0.3458 (6)	0.078 (4)	0.484 (19)
O4'	0.785 (3)	0.2270 (4)	0.4821 (8)	0.101 (6)	0.484 (19)
O5'	0.6936 (11)	0.1110 (6)	0.4685 (14)	0.085 (4)	0.484 (19)
O6	0.3617 (4)	0.05008 (14)	0.3966 (2)	0.0532 (7)
N1	0.3427 (5)	0.19660 (17)	0.6127 (3)	0.0500 (8)
N2	0.3395 (5)	0.20158 (18)	0.4077 (3)	0.0498 (8)
C1	0.3446 (6)	0.0567 (2)	0.7130 (3)	0.0472 (9)
C2	0.3289 (7)	−0.0037 (2)	0.7721 (4)	0.0631 (12)
H2	0.3457	−0.0469	0.7406	0.076*
C3	0.2889 (7)	−0.0016 (3)	0.8762 (4)	0.0665 (13)
H3	0.2794	−0.0429	0.9141	0.080*
C4	0.2634 (7)	0.0613 (3)	0.9231 (3)	0.0618 (12)
C5	0.2762 (7)	0.1218 (3)	0.8692 (4)	0.0588 (11)
H5	0.2586	0.1642	0.9026	0.071*
C6	0.3159 (6)	0.1213 (2)	0.7628 (3)	0.0486 (9)
C7	0.3194 (6)	0.1879 (2)	0.7100 (4)	0.0527 (10)
H7	0.3035	0.2277	0.7502	0.063*
C8	0.3350 (8)	0.2674 (2)	0.5694 (4)	0.0675 (13)
H8A	0.4450	0.2933	0.5975	0.081*
H8B	0.2258	0.2914	0.5903	0.081*
C9	0.3260 (6)	0.2649 (2)	0.4510 (4)	0.0534 (10)
C10	0.3080 (7)	0.3244 (3)	0.3901 (5)	0.0721 (14)
H10	0.2980	0.3681	0.4213	0.087*
C11	0.3051 (8)	0.3181 (3)	0.2820 (5)	0.0851 (17)
H11	0.2919	0.3576	0.2392	0.102*
C12	0.3217 (8)	0.2534 (3)	0.2377 (4)	0.0753 (15)
H12	0.3223	0.2485	0.1648	0.090*
C13	0.3374 (7)	0.1963 (2)	0.3023 (4)	0.0624 (12)
H13	0.3470	0.1522	0.2723	0.075*
C14	0.1874 (9)	0.0142 (3)	0.3546 (5)	0.0848 (17)
H14A	0.2144	−0.0186	0.3010	0.127*
H14B	0.0989	0.0481	0.3246	0.127*
H14C	0.1359	−0.0102	0.4110	0.127*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0441 (3)	0.0309 (2)	0.0346 (3)	0.0044 (2)	0.00835 (19)	0.0013 (2)
Br1	0.1131 (5)	0.1240 (6)	0.0446 (3)	0.0133 (4)	0.0252 (3)	−0.0001 (3)
Cl1	0.0576 (6)	0.0568 (6)	0.0614 (7)	−0.0003 (5)	0.0119 (5)	0.0035 (5)
O1	0.0718 (19)	0.0427 (15)	0.0434 (15)	0.0114 (13)	0.0163 (14)	0.0005 (12)
O2	0.044 (5)	0.073 (6)	0.124 (11)	0.006 (4)	0.010 (5)	0.007 (6)
O3	0.111 (11)	0.126 (9)	0.060 (6)	−0.038 (8)	−0.008 (5)	−0.012 (5)
O4	0.070 (6)	0.060 (4)	0.095 (6)	0.007 (4)	0.011 (5)	−0.004 (4)
O5	0.047 (4)	0.104 (8)	0.086 (7)	0.000 (4)	0.024 (4)	0.004 (6)
O2'	0.061 (6)	0.149 (14)	0.071 (7)	−0.028 (7)	−0.016 (5)	0.017 (8)
O3'	0.098 (10)	0.078 (6)	0.056 (5)	−0.007 (6)	−0.004 (5)	0.009 (4)
O4'	0.168 (16)	0.050 (5)	0.084 (6)	0.013 (7)	0.010 (8)	−0.011 (4)
O5'	0.046 (4)	0.066 (6)	0.143 (11)	−0.003 (4)	0.015 (5)	0.005 (6)
O6	0.0671 (19)	0.0486 (16)	0.0449 (16)	0.0073 (14)	0.0104 (14)	−0.0039 (12)
N1	0.054 (2)	0.0415 (18)	0.055 (2)	−0.0029 (15)	0.0055 (16)	−0.0026 (15)
N2	0.0445 (18)	0.0483 (19)	0.057 (2)	0.0030 (15)	0.0077 (15)	0.0067 (16)
C1	0.051 (2)	0.046 (2)	0.045 (2)	0.0050 (17)	0.0112 (18)	−0.0012 (17)
C2	0.088 (3)	0.050 (2)	0.055 (3)	0.013 (2)	0.022 (2)	0.002 (2)
C3	0.089 (3)	0.062 (3)	0.053 (3)	0.008 (2)	0.025 (2)	0.012 (2)
C4	0.065 (3)	0.084 (3)	0.038 (2)	0.005 (2)	0.010 (2)	−0.001 (2)
C5	0.064 (3)	0.064 (3)	0.049 (2)	0.002 (2)	0.010 (2)	−0.014 (2)
C6	0.051 (2)	0.055 (2)	0.041 (2)	0.0004 (18)	0.0096 (17)	−0.0049 (18)
C7	0.058 (2)	0.046 (2)	0.054 (2)	−0.0004 (19)	0.0076 (19)	−0.0130 (19)
C8	0.092 (4)	0.036 (2)	0.073 (3)	−0.003 (2)	0.005 (3)	0.000 (2)
C9	0.046 (2)	0.044 (2)	0.070 (3)	−0.0012 (17)	0.006 (2)	0.006 (2)
C10	0.080 (3)	0.048 (3)	0.087 (4)	−0.002 (2)	0.004 (3)	0.016 (3)
C11	0.094 (4)	0.066 (3)	0.093 (4)	−0.001 (3)	−0.001 (3)	0.040 (3)
C12	0.087 (4)	0.074 (4)	0.065 (3)	−0.002 (3)	0.005 (3)	0.025 (3)
C13	0.071 (3)	0.061 (3)	0.056 (3)	0.003 (2)	0.008 (2)	0.011 (2)
C14	0.106 (5)	0.072 (3)	0.075 (4)	0.016 (3)	0.004 (3)	−0.004 (3)

Geometric parameters (Å, º)

Co1—O1	1.898 (3)	C2—H2	0.93
Co1—N1	1.940 (3)	C3—C4	1.362 (7)
Co1—N2	1.987 (3)	C3—H3	0.93
Co1—O6	1.996 (3)	C4—C5	1.352 (7)
Br1—C4	1.906 (4)	C5—C6	1.408 (6)
Cl1—O3	1.397 (8)	C5—H5	0.93
Cl1—O2'	1.409 (9)	C6—C7	1.441 (6)
Cl1—O5	1.422 (7)	C7—H7	0.93
Cl1—O4'	1.433 (8)	C8—C9	1.499 (7)
Cl1—O3'	1.433 (8)	C8—H8A	0.97
Cl1—O2	1.438 (8)	C8—H8B	0.97
Cl1—O4	1.448 (7)	C9—C10	1.375 (6)
Cl1—O5'	1.448 (7)	C10—C11	1.376 (8)
O1—C1	1.324 (5)	C10—H10	0.93
O6—C14	1.480 (6)	C11—C12	1.369 (8)
N1—C7	1.274 (5)	C11—H11	0.93
N1—C8	1.461 (5)	C12—C13	1.364 (6)
N2—C9	1.337 (5)	C12—H12	0.93
N2—C13	1.341 (6)	C13—H13	0.93
C1—C2	1.388 (6)	C14—H14A	0.96
C1—C6	1.412 (5)	C14—H14B	0.96
C2—C3	1.382 (6)	C14—H14C	0.96
O1—Co1—N1	93.70 (13)	C1—C2—H2	119.0
O1—Co1—N2	176.48 (14)	C4—C3—C2	119.6 (4)
N1—Co1—N2	82.96 (15)	C4—C3—H3	120.2
O1—Co1—O6	89.75 (12)	C2—C3—H3	120.2
N1—Co1—O6	175.10 (13)	C5—C4—C3	121.0 (4)
N2—Co1—O6	93.65 (13)	C5—C4—Br1	119.5 (4)
O3—Cl1—O2'	131.6 (9)	C3—C4—Br1	119.5 (4)
O3—Cl1—O5	113.2 (6)	C4—C5—C6	120.7 (4)
O2'—Cl1—O5	101.9 (8)	C4—C5—H5	119.7
O3—Cl1—O4'	102.5 (8)	C6—C5—H5	119.7
O2'—Cl1—O4'	116.3 (6)	C5—C6—C1	119.3 (4)
O5—Cl1—O4'	79.4 (6)	C5—C6—C7	117.0 (4)
O2'—Cl1—O3'	110.7 (7)	C1—C6—C7	123.7 (4)
O5—Cl1—O3'	138.1 (6)	N1—C7—C6	125.2 (4)
O4'—Cl1—O3'	107.2 (6)	N1—C7—H7	117.4
O3—Cl1—O2	110.9 (7)	C6—C7—H7	117.4
O5—Cl1—O2	107.1 (6)	N1—C8—C9	110.1 (4)
O4'—Cl1—O2	139.1 (7)	N1—C8—H8A	109.6
O3'—Cl1—O2	94.4 (8)	C9—C8—H8A	109.6
O3—Cl1—O4	112.5 (6)	N1—C8—H8B	109.6
O2'—Cl1—O4	85.6 (6)	C9—C8—H8B	109.6
O5—Cl1—O4	107.6 (5)	H8A—C8—H8B	108.2
O3'—Cl1—O4	100.5 (7)	N2—C9—C10	121.7 (5)
O2—Cl1—O4	105.1 (5)	N2—C9—C8	116.3 (4)
O3—Cl1—O5'	84.7 (7)	C10—C9—C8	122.0 (4)
O2'—Cl1—O5'	108.8 (7)	C9—C10—C11	118.7 (5)
O4'—Cl1—O5'	106.8 (6)	C9—C10—H10	120.7
O3'—Cl1—O5'	106.5 (6)	C11—C10—H10	120.7
O2—Cl1—O5'	99.4 (7)	C12—C11—C10	119.7 (5)
O4—Cl1—O5'	141.7 (5)	C12—C11—H11	120.1
C1—O1—Co1	126.0 (2)	C10—C11—H11	120.1
C14—O6—Co1	121.1 (3)	C13—C12—C11	118.8 (5)
C7—N1—C8	118.8 (4)	C13—C12—H12	120.6
C7—N1—Co1	125.6 (3)	C11—C12—H12	120.6
C8—N1—Co1	115.2 (3)	N2—C13—C12	122.1 (5)
C9—N2—C13	119.0 (4)	N2—C13—H13	118.9
C9—N2—Co1	115.1 (3)	C12—C13—H13	118.9
C13—N2—Co1	125.9 (3)	O6—C14—H14A	109.5
O1—C1—C2	118.9 (4)	O6—C14—H14B	109.5
O1—C1—C6	123.6 (4)	H14A—C14—H14B	109.5
C2—C1—C6	117.5 (4)	O6—C14—H14C	109.5
C3—C2—C1	121.9 (4)	H14A—C14—H14C	109.5
C3—C2—H2	119.0	H14B—C14—H14C	109.5
N1—Co1—O1—C1	16.6 (3)	O1—C1—C6—C5	−178.7 (4)
O6—Co1—O1—C1	−159.9 (3)	C2—C1—C6—C5	1.1 (6)
O1—Co1—O6—C14	85.7 (3)	O1—C1—C6—C7	3.1 (7)
N2—Co1—O6—C14	−95.2 (3)	C2—C1—C6—C7	−177.1 (4)
O1—Co1—N1—C7	−11.6 (4)	C8—N1—C7—C6	177.5 (4)
N2—Co1—N1—C7	169.6 (4)	Co1—N1—C7—C6	4.7 (6)
O1—Co1—N1—C8	175.4 (3)	C5—C6—C7—N1	−175.9 (4)
N2—Co1—N1—C8	−3.5 (3)	C1—C6—C7—N1	2.3 (7)
N1—Co1—N2—C9	0.9 (3)	C7—N1—C8—C9	−168.4 (4)
O6—Co1—N2—C9	177.3 (3)	Co1—N1—C8—C9	5.1 (5)
N1—Co1—N2—C13	−179.0 (4)	C13—N2—C9—C10	0.7 (6)
O6—Co1—N2—C13	−2.6 (4)	Co1—N2—C9—C10	−179.2 (4)
Co1—O1—C1—C2	165.2 (3)	C13—N2—C9—C8	−178.2 (4)
Co1—O1—C1—C6	−15.0 (6)	Co1—N2—C9—C8	1.8 (5)
O1—C1—C2—C3	179.0 (5)	N1—C8—C9—N2	−4.5 (6)
C6—C1—C2—C3	−0.8 (7)	N1—C8—C9—C10	176.6 (4)
C1—C2—C3—C4	0.2 (8)	N2—C9—C10—C11	−0.4 (7)
C2—C3—C4—C5	0.2 (8)	C8—C9—C10—C11	178.5 (5)
C2—C3—C4—Br1	179.0 (4)	C9—C10—C11—C12	−0.6 (9)
C3—C4—C5—C6	0.1 (8)	C10—C11—C12—C13	1.2 (9)
Br1—C4—C5—C6	−178.7 (3)	C9—N2—C13—C12	−0.1 (7)
C4—C5—C6—C1	−0.8 (7)	Co1—N2—C13—C12	179.9 (4)
C4—C5—C6—C7	177.5 (4)	C11—C12—C13—N2	−0.9 (8)