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The crystal structure of the title compound consists of dinuclear complexes, in which the CoII cations are fivefold coordinated and linked by centrosymmetric pairs of μ-1,1(O,O)-bridging 2-methyl­pyridine N-oxide coligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989023008228/pk2697sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989023008228/pk2697Isup2.hkl
Contains datablock I

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Portable Network Graphics (PNG) image https://doi.org/10.1107/S2056989023008228/pk2697sup3.png
DTG, TG and DTA curve of the title compound measured with 4C/min in a nitrogen atmosphere.

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Portable Network Graphics (PNG) image https://doi.org/10.1107/S2056989023008228/pk2697sup4.png
Experimental powder pattern of the residue obtained after the first mass loss in a DTA-TG measurement of the title compound.

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Portable Network Graphics (PNG) image https://doi.org/10.1107/S2056989023008228/pk2697sup5.png
IR spectrum of the residue obtained after the first mass loss in a DTA-TG measurement of the title compound. The wavenumbers of the most prominent vibrations are given.

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Portable Network Graphics (PNG) image https://doi.org/10.1107/S2056989023008228/pk2697sup6.png
IR spectrum of the title compound. The wavenumbers of the most prominent vibrations are given.

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Portable Network Graphics (PNG) image https://doi.org/10.1107/S2056989023008228/pk2697sup7.png
Experimental powder pattern of the residue obtained after storage of the title compound for 60 h at room-temperature.

CCDC reference: 2295983

Computing details top

Data collection: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); cell refinement: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); data reduction: CrysAlis PRO 1.171.42.67a (Rigaku OD, 2022); program(s) used to solve structure: SHELXT2014/4 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis(µ-2-methylpyridine N-oxide-κ2O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvate top
Crystal data top
[Co2Br4(C6H7NO)4]·C4H10OZ = 1
Mr = 948.12F(000) = 468
Triclinic, P1Dx = 1.819 Mg m3
a = 8.0900 (1) ÅCu Kα radiation, λ = 1.54184 Å
b = 9.5772 (1) ÅCell parameters from 14929 reflections
c = 12.2400 (1) Åθ = 3.9–79.9°
α = 70.242 (1)°µ = 13.26 mm1
β = 76.004 (1)°T = 100 K
γ = 83.860 (1)°Block, dark blue
V = 865.69 (2) Å30.15 × 0.03 × 0.03 mm
Data collection top
XtaLAB Synergy, Dualflex, HyPix
diffractometer
3705 independent reflections
Mirror monochromator3686 reflections with I > 2σ(I)
Detector resolution: 10.0000 pixels mm-1Rint = 0.021
ω scansθmax = 80.2°, θmin = 3.9°
Absorption correction: multi-scan
(CrysAlisPro; Rigaku OD, 2022)
h = 1010
Tmin = 0.721, Tmax = 1.000k = 1212
18480 measured reflectionsl = 1215
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.0306P)2 + 1.2686P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.065(Δ/σ)max < 0.001
S = 1.09Δρmax = 0.50 e Å3
3705 reflectionsΔρmin = 0.59 e Å3
204 parametersExtinction correction: SHELXL2016/6 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.00106 (14)
Primary atom site location: dual
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.52210 (5)0.46947 (4)0.36734 (3)0.01558 (10)
Br10.24435 (3)0.41656 (3)0.34944 (2)0.02233 (8)
Br20.71203 (4)0.28893 (3)0.28069 (2)0.02820 (9)
O10.5761 (2)0.38106 (17)0.52800 (14)0.0163 (3)
N10.6713 (2)0.2555 (2)0.56405 (17)0.0161 (4)
C10.5945 (3)0.1227 (3)0.60505 (19)0.0183 (4)
C20.6944 (3)0.0046 (3)0.6432 (2)0.0238 (5)
H20.6443480.0992750.6737350.029*
C30.8660 (4)0.0060 (3)0.6368 (2)0.0279 (5)
H30.9333820.0810320.6632420.033*
C40.9388 (3)0.1438 (3)0.5918 (2)0.0264 (5)
H41.0567080.1523770.5862520.032*
C50.8382 (3)0.2689 (3)0.5550 (2)0.0212 (5)
H50.8867590.3642570.5232580.025*
C60.4125 (3)0.1211 (3)0.6032 (2)0.0211 (5)
H6A0.3454950.1834620.6479980.032*
H6B0.3725680.0191300.6395420.032*
H6C0.3989960.1596510.5206710.032*
O110.6147 (2)0.65388 (19)0.24397 (14)0.0243 (4)
N110.6946 (3)0.6523 (2)0.13423 (17)0.0234 (4)
C110.8634 (3)0.6742 (3)0.0986 (2)0.0254 (5)
C120.9411 (4)0.6781 (3)0.0169 (2)0.0318 (6)
H121.0598120.6949100.0450900.038*
C130.8485 (4)0.6581 (3)0.0914 (2)0.0346 (7)
H130.9030940.6602510.1699090.041*
C140.6774 (4)0.6351 (3)0.0508 (2)0.0369 (7)
H140.6119360.6213420.1010290.044*
C150.6004 (4)0.6320 (3)0.0638 (2)0.0320 (6)
H150.4816430.6157370.0928730.038*
C160.9546 (4)0.6917 (4)0.1847 (3)0.0347 (6)
H16A0.9114100.7814150.2049570.052*
H16B1.0768710.7001570.1489680.052*
H16C0.9356410.6049830.2569560.052*
O210.6568 (6)0.1984 (4)0.0597 (4)0.0427 (10)0.5
H210.6735830.2004770.1242000.064*0.5
C210.6912 (6)0.0492 (4)0.0530 (3)0.0562 (10)
H21A0.6584750.0234330.1337640.067*0.5
H21B0.8149410.0357050.0231280.067*0.5
H21C0.6659430.0270680.1314020.067*0.5
H21D0.6561020.1470240.0611530.067*0.5
H21E0.8138230.0474380.0187540.067*0.5
C220.5932 (5)0.0184 (4)0.0294 (3)0.0485 (9)
H22A0.5981400.1066390.1014450.058*
H22B0.6503540.0656630.0549820.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02026 (19)0.01482 (18)0.01137 (18)0.00042 (13)0.00241 (14)0.00463 (13)
Br10.02518 (13)0.02280 (13)0.02382 (14)0.00051 (9)0.01136 (10)0.00991 (10)
Br20.03810 (16)0.01941 (13)0.02232 (14)0.00291 (10)0.00953 (10)0.01123 (10)
O10.0195 (7)0.0143 (7)0.0161 (7)0.0058 (6)0.0053 (6)0.0070 (6)
N10.0196 (9)0.0134 (8)0.0159 (9)0.0051 (7)0.0058 (7)0.0061 (7)
C10.0250 (11)0.0177 (10)0.0122 (10)0.0007 (8)0.0029 (8)0.0057 (8)
C20.0314 (13)0.0187 (11)0.0200 (11)0.0045 (9)0.0055 (10)0.0064 (9)
C30.0334 (13)0.0264 (12)0.0235 (12)0.0117 (10)0.0107 (10)0.0085 (10)
C40.0224 (11)0.0291 (13)0.0305 (13)0.0070 (10)0.0087 (10)0.0136 (11)
C50.0201 (11)0.0223 (11)0.0235 (12)0.0013 (9)0.0034 (9)0.0119 (9)
C60.0247 (11)0.0173 (11)0.0215 (11)0.0026 (9)0.0048 (9)0.0062 (9)
O110.0383 (10)0.0193 (8)0.0119 (7)0.0059 (7)0.0046 (7)0.0063 (6)
N110.0373 (12)0.0158 (9)0.0139 (9)0.0049 (8)0.0030 (8)0.0054 (7)
C110.0348 (13)0.0173 (11)0.0199 (12)0.0049 (9)0.0010 (10)0.0056 (9)
C120.0414 (15)0.0250 (13)0.0210 (12)0.0047 (11)0.0042 (11)0.0067 (10)
C130.0589 (19)0.0239 (12)0.0161 (11)0.0058 (12)0.0055 (12)0.0085 (10)
C140.063 (2)0.0294 (14)0.0200 (13)0.0174 (13)0.0001 (13)0.0112 (11)
C150.0461 (16)0.0282 (13)0.0240 (13)0.0153 (12)0.0010 (12)0.0119 (11)
C160.0295 (13)0.0441 (16)0.0257 (13)0.0102 (12)0.0078 (11)0.0072 (12)
O210.053 (3)0.044 (2)0.044 (3)0.006 (2)0.027 (2)0.022 (2)
C210.079 (3)0.053 (2)0.0378 (18)0.035 (2)0.0255 (18)0.0177 (16)
C220.081 (3)0.0339 (16)0.0270 (15)0.0242 (17)0.0127 (15)0.0121 (13)
Geometric parameters (Å, º) top
Co1—Br12.4312 (4)C11—C121.391 (3)
Co1—Br22.5217 (4)C11—C161.485 (4)
Co1—O11.9964 (16)C12—H120.9500
Co1—O1i2.1968 (15)C12—C131.381 (4)
Co1—O111.9732 (17)C13—H130.9500
O1—N11.357 (2)C13—C141.368 (5)
N1—C11.357 (3)C14—H140.9500
N1—C51.344 (3)C14—C151.382 (4)
C1—C21.394 (3)C15—H150.9500
C1—C61.480 (3)C16—H16A0.9800
C2—H20.9500C16—H16B0.9800
C2—C31.384 (4)C16—H16C0.9800
C3—H30.9500O21—H210.8400
C3—C41.382 (4)O21—C211.4524 (10)
C4—H40.9500C21—H21A0.9900
C4—C51.380 (3)C21—H21B0.9900
C5—H50.9500C21—H21C0.9800
C6—H6A0.9800C21—H21D0.9800
C6—H6B0.9800C21—H21E0.9800
C6—H6C0.9800C21—C221.539 (5)
O11—N111.347 (2)C22—C22ii1.528 (8)
N11—C111.346 (4)C22—H22A0.9900
N11—C151.351 (4)C22—H22B0.9900
Br1—Co1—Br2101.355 (16)N11—C11—C12117.5 (3)
O1—Co1—Br1116.56 (5)N11—C11—C16118.2 (2)
O1i—Co1—Br195.39 (4)C12—C11—C16124.3 (3)
O1—Co1—Br294.52 (4)C11—C12—H12119.5
O1i—Co1—Br2161.54 (4)C13—C12—C11121.1 (3)
O1—Co1—O1i70.82 (7)C13—C12—H12119.5
O11—Co1—Br1112.08 (6)C12—C13—H13120.4
O11—Co1—Br297.54 (5)C14—C13—C12119.3 (2)
O11—Co1—O1i83.12 (6)C14—C13—H13120.4
O11—Co1—O1126.08 (7)C13—C14—H14120.2
Co1—O1—Co1i109.18 (7)C13—C14—C15119.5 (3)
N1—O1—Co1125.78 (12)C15—C14—H14120.2
N1—O1—Co1i124.80 (12)N11—C15—C14119.7 (3)
O1—N1—C1118.60 (18)N11—C15—H15120.1
C5—N1—O1118.18 (19)C14—C15—H15120.1
C5—N1—C1123.2 (2)C11—C16—H16A109.5
N1—C1—C2117.5 (2)C11—C16—H16B109.5
N1—C1—C6118.4 (2)C11—C16—H16C109.5
C2—C1—C6124.0 (2)H16A—C16—H16B109.5
C1—C2—H2119.8H16A—C16—H16C109.5
C3—C2—C1120.5 (2)H16B—C16—H16C109.5
C3—C2—H2119.8C21—O21—H21109.5
C2—C3—H3120.2O21—C21—H21A109.2
C4—C3—C2119.7 (2)O21—C21—H21B109.2
C4—C3—H3120.2O21—C21—C22112.1 (3)
C3—C4—H4120.4H21A—C21—H21B107.9
C5—C4—C3119.2 (2)H21C—C21—H21D109.5
C5—C4—H4120.4H21C—C21—H21E109.5
N1—C5—C4119.9 (2)H21D—C21—H21E109.5
N1—C5—H5120.1C22—C21—H21A109.2
C4—C5—H5120.1C22—C21—H21B109.2
C1—C6—H6A109.5C22—C21—H21C109.5
C1—C6—H6B109.5C22—C21—H21D109.5
C1—C6—H6C109.5C22—C21—H21E109.5
H6A—C6—H6B109.5C21—C22—H22A108.9
H6A—C6—H6C109.5C21—C22—H22B108.9
H6B—C6—H6C109.5C22ii—C22—C21113.3 (3)
N11—O11—Co1120.09 (13)C22ii—C22—H22A108.9
O11—N11—C15118.3 (2)C22ii—C22—H22B108.9
C11—N11—O11118.8 (2)H22A—C22—H22B107.7
C11—N11—C15122.9 (2)
Co1i—O1—N1—C1102.20 (19)C5—N1—C1—C6175.8 (2)
Co1—O1—N1—C184.0 (2)C6—C1—C2—C3176.9 (2)
Co1i—O1—N1—C579.2 (2)O11—N11—C11—C12177.4 (2)
Co1—O1—N1—C594.6 (2)O11—N11—C11—C163.0 (3)
Co1—O11—N11—C11111.6 (2)O11—N11—C15—C14177.7 (2)
Co1—O11—N11—C1569.9 (3)N11—C11—C12—C130.9 (4)
O1—N1—C1—C2179.10 (19)C11—N11—C15—C140.7 (4)
O1—N1—C1—C62.8 (3)C11—C12—C13—C140.5 (4)
O1—N1—C5—C4179.4 (2)C12—C13—C14—C150.1 (4)
N1—C1—C2—C31.1 (3)C13—C14—C15—N110.2 (4)
C1—N1—C5—C42.1 (4)C15—N11—C11—C121.1 (4)
C1—C2—C3—C40.3 (4)C15—N11—C11—C16178.6 (2)
C2—C3—C4—C50.6 (4)C16—C11—C12—C13178.7 (3)
C3—C4—C5—N10.5 (4)O21—C21—C22—C22ii79.5 (5)
C5—N1—C1—C22.3 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···Br1iii0.953.123.704 (2)121
C5—H5···Br1i0.952.983.531 (2)118
C6—H6A···O11i0.982.453.259 (3)140
C6—H6B···Br2iv0.982.883.852 (2)172
C6—H6C···Br10.983.023.845 (2)142
C12—H12···Br2v0.952.993.676 (3)130
C12—H12···O21v0.952.553.441 (6)156
C14—H14···Br1vi0.953.113.747 (3)126
C16—H16C···Br1iii0.983.133.725 (3)121
O21—H21···Br20.842.433.244 (4)162
Symmetry codes: (i) x+1, y+1, z+1; (iii) x+1, y, z; (iv) x+1, y, z+1; (v) x+2, y+1, z; (vi) x+1, y+1, z.
 

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