Bis(2,2'-bipyridyl-κN,N')(carbonato-κO,O')cobalt(III) bromide trihydrate.

The title complex, [Co(CO(3))(C(10)H(8)N(2))(2)]Br·3H(2)O, is isostructural with the chloride analogue. The six-coordinated octahedral [Co(2,2'-bipy)(2)CO(3)](+) cation (2,2'-bipy is 2,2'-bipyrid-yl), bromide ion and water mol-ecules are linked together via O-H⋯Br and O-H⋯O hydrogen bonds, generating a one-dimensional chain.

Related literature

For related literature, see: Das et al. (1993 ▶); Thirumurugan & Natarajan (2004 ▶).

Experimental

Crystal data

[Co(CO3)(C10H8N2)2]Br·3H2O

M = 565.27

Triclinic,

a = 9.1281 (1) Å

b = 9.6652 (2) Å

c = 13.0732 (2) Å

α = 92.054 (1)°

β = 102.315 (1)°

γ = 91.448 (1)°

V = 1125.48 (3) Å3

Z = 2

Mo Kα radiation

μ = 2.58 mm−1

T = 296 (2) K

0.18 × 0.12 × 0.09 mm

Data collection

Bruker SMART APEX CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.654, T max = 0.801

14734 measured reflections

4411 independent reflections

4000 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.084

S = 1.08

4411 reflections

323 parameters

9 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.31 e Å−3

Δρmin = −0.56 e Å−3

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 2001 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807062551/at2506sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807062551/at2506Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(CO3)(C10H8N2)2]Br·3H2O	Z = 2
Mr = 565.27	F000 = 572
Triclinic, P1	Dx = 1.668 Mg m−3
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 9.1281 (1) Å	Cell parameters from 9295 reflections
b = 9.6652 (2) Å	θ = 2.6–26.7º
c = 13.0732 (2) Å	µ = 2.58 mm−1
α = 92.054 (1)º	T = 296 (2) K
β = 102.315 (1)º	Block, red
γ = 91.448 (1)º	0.18 × 0.12 × 0.09 mm
V = 1125.48 (3) Å3

Bruker SMART APEX CCD area-detector diffractometer	4411 independent reflections
Radiation source: fine-focus sealed tube	4000 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.020
T = 296(2) K	θmax = 26.0º
φ and ω scans	θmin = 2.1º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −10→11
Tmin = 0.654, Tmax = 0.801	k = −11→11
14734 measured reflections	l = −16→16

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.084	w = 1/[σ2(Fo2) + (0.0499P)2 + 0.4188P] where P = (Fo2 + 2Fc2)/3
S = 1.08	(Δ/σ)max = 0.001
4411 reflections	Δρmax = 0.31 e Å−3
323 parameters	Δρmin = −0.56 e Å−3
9 restraints	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0160 (12)

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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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 andgoodness of fit S are based on F2, conventional R-factors R are basedon F, with F set to zero for negative F2. The threshold expression ofF2 > σ(F2) is used only for calculating R-factors(gt) etc. and isnot relevant to the choice of reflections for refinement. R-factors basedon F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
Co1	0.26787 (3)	0.01455 (3)	0.244258 (18)	0.02444 (10)
Br1	0.68362 (3)	0.61581 (3)	0.14986 (2)	0.06088 (12)
C1	0.3267 (2)	−0.2651 (2)	0.31331 (18)	0.0361 (5)
H1	0.2315	−0.2896	0.2742	0.043*
C2	0.4099 (3)	−0.3639 (2)	0.37077 (19)	0.0421 (5)
H2	0.3717	−0.4542	0.3702	0.051*
C3	0.5510 (3)	−0.3268 (2)	0.42920 (18)	0.0422 (5)
H3	0.6083	−0.3917	0.4694	0.051*
C4	0.6063 (2)	−0.1933 (2)	0.42761 (17)	0.0369 (5)
H4	0.7016	−0.1672	0.4660	0.044*
C5	0.5184 (2)	−0.0982 (2)	0.36814 (14)	0.0278 (4)
C6	0.5627 (2)	0.0465 (2)	0.35739 (14)	0.0278 (4)
C7	0.7009 (2)	0.1073 (2)	0.40451 (17)	0.0366 (5)
H7	0.7727	0.0569	0.4478	0.044*
C8	0.7303 (3)	0.2439 (3)	0.38614 (19)	0.0436 (5)
H8	0.8224	0.2865	0.4169	0.052*
C9	0.6221 (3)	0.3167 (2)	0.3219 (2)	0.0430 (5)
H9	0.6406	0.4087	0.3086	0.052*
C10	0.4857 (2)	0.2511 (2)	0.27730 (17)	0.0354 (5)
H10	0.4126	0.3004	0.2342	0.042*
C11	0.3835 (2)	−0.1361 (2)	0.07871 (17)	0.0331 (4)
H11	0.4386	−0.1880	0.1312	0.040*
C12	0.3882 (3)	−0.1675 (2)	−0.02410 (18)	0.0390 (5)
H12	0.4445	−0.2404	−0.0409	0.047*
C13	0.3086 (3)	−0.0894 (3)	−0.10162 (17)	0.0399 (5)
H13	0.3101	−0.1097	−0.1715	0.048*
C14	0.2262 (2)	0.0193 (2)	−0.07523 (15)	0.0341 (5)
H14	0.1740	0.0744	−0.1266	0.041*
C15	0.2232 (2)	0.0443 (2)	0.02917 (15)	0.0263 (4)
C16	0.1368 (2)	0.1543 (2)	0.06733 (15)	0.0265 (4)
C17	0.0429 (2)	0.2405 (2)	0.00477 (17)	0.0338 (4)
H17	0.0303	0.2332	−0.0677	0.041*
C18	−0.0327 (2)	0.3386 (2)	0.0514 (2)	0.0413 (5)
H18	−0.0990	0.3964	0.0106	0.050*
C19	−0.0085 (3)	0.3493 (2)	0.1585 (2)	0.0447 (6)
H19	−0.0560	0.4167	0.1910	0.054*
C20	0.0864 (3)	0.2598 (2)	0.21795 (18)	0.0395 (5)
H20	0.1021	0.2673	0.2906	0.047*
O3	−0.0230 (2)	−0.0747 (2)	0.37222 (16)	0.0604 (5)
C21	0.0755 (2)	−0.0408 (2)	0.32724 (17)	0.0368 (5)
N1	0.45605 (18)	0.11867 (17)	0.29456 (13)	0.0282 (3)
N2	0.37927 (18)	−0.13463 (17)	0.31232 (12)	0.0281 (3)
N3	0.30138 (17)	−0.03247 (17)	0.10536 (12)	0.0265 (3)
N4	0.15670 (18)	0.16221 (17)	0.17294 (13)	0.0292 (4)
O1	0.08496 (15)	−0.08699 (15)	0.23240 (11)	0.0321 (3)
O2	0.18851 (16)	0.04514 (16)	0.36505 (11)	0.0341 (3)
O4	0.1357 (3)	0.4381 (3)	0.43419 (18)	0.0666 (6)
O5	0.9249 (3)	0.6454 (3)	0.37190 (19)	0.0676 (6)
O6	0.3364 (3)	0.4743 (3)	0.1049 (2)	0.0754 (7)
H4A	0.109 (4)	0.409 (3)	0.4873 (19)	0.084 (12)*
H4B	0.075 (3)	0.498 (3)	0.410 (2)	0.061 (9)*
H6A	0.331 (3)	0.445 (4)	0.0429 (13)	0.074 (12)*
H5A	0.939 (3)	0.7312 (12)	0.379 (2)	0.055 (9)*
H6B	0.423 (2)	0.510 (4)	0.125 (2)	0.082 (12)*
H5B	0.856 (3)	0.630 (3)	0.3190 (19)	0.086 (12)*

	U11	U22	U33	U12	U13	U23
Co1	0.02552 (15)	0.02518 (16)	0.02032 (14)	0.00563 (10)	−0.00088 (10)	0.00176 (10)
Br1	0.05214 (18)	0.0591 (2)	0.0695 (2)	0.00644 (13)	0.00614 (14)	0.01561 (15)
C1	0.0349 (11)	0.0304 (11)	0.0403 (12)	0.0004 (8)	0.0015 (9)	0.0057 (9)
C2	0.0496 (13)	0.0294 (11)	0.0486 (13)	0.0054 (9)	0.0114 (11)	0.0107 (10)
C3	0.0474 (13)	0.0386 (13)	0.0398 (12)	0.0159 (10)	0.0036 (10)	0.0143 (10)
C4	0.0358 (11)	0.0412 (13)	0.0302 (10)	0.0108 (9)	−0.0025 (8)	0.0049 (9)
C5	0.0287 (9)	0.0325 (11)	0.0212 (9)	0.0064 (8)	0.0022 (7)	0.0016 (8)
C6	0.0295 (9)	0.0318 (11)	0.0210 (9)	0.0051 (8)	0.0027 (7)	0.0001 (8)
C7	0.0312 (10)	0.0439 (13)	0.0311 (10)	0.0020 (9)	−0.0008 (8)	−0.0013 (9)
C8	0.0387 (12)	0.0451 (14)	0.0438 (13)	−0.0090 (10)	0.0043 (10)	−0.0082 (10)
C9	0.0501 (13)	0.0308 (12)	0.0478 (13)	−0.0054 (10)	0.0111 (11)	−0.0022 (10)
C10	0.0403 (11)	0.0289 (11)	0.0361 (11)	0.0032 (9)	0.0054 (9)	0.0035 (9)
C11	0.0323 (10)	0.0320 (11)	0.0349 (11)	0.0084 (8)	0.0064 (8)	0.0028 (8)
C12	0.0407 (12)	0.0376 (12)	0.0410 (12)	0.0079 (9)	0.0142 (10)	−0.0039 (10)
C13	0.0415 (12)	0.0504 (14)	0.0286 (10)	0.0009 (10)	0.0109 (9)	−0.0057 (9)
C14	0.0323 (10)	0.0435 (12)	0.0245 (10)	0.0009 (9)	0.0010 (8)	0.0048 (9)
C15	0.0230 (9)	0.0283 (10)	0.0261 (9)	0.0007 (7)	0.0017 (7)	0.0027 (8)
C16	0.0235 (9)	0.0263 (10)	0.0279 (9)	0.0004 (7)	0.0009 (7)	0.0034 (8)
C17	0.0303 (10)	0.0341 (11)	0.0351 (11)	0.0037 (8)	0.0008 (8)	0.0110 (9)
C18	0.0345 (11)	0.0324 (12)	0.0550 (14)	0.0109 (9)	0.0016 (10)	0.0155 (10)
C19	0.0439 (12)	0.0327 (12)	0.0583 (15)	0.0143 (10)	0.0116 (11)	0.0008 (11)
C20	0.0456 (12)	0.0354 (12)	0.0377 (11)	0.0143 (10)	0.0082 (9)	−0.0017 (9)
O3	0.0540 (11)	0.0702 (13)	0.0655 (12)	−0.0069 (9)	0.0345 (10)	−0.0080 (10)
C21	0.0353 (11)	0.0412 (12)	0.0339 (11)	0.0074 (9)	0.0065 (9)	0.0011 (9)
N1	0.0304 (8)	0.0269 (9)	0.0257 (8)	0.0042 (7)	0.0023 (6)	0.0010 (6)
N2	0.0292 (8)	0.0282 (9)	0.0251 (8)	0.0036 (6)	0.0012 (6)	0.0031 (6)
N3	0.0264 (8)	0.0259 (8)	0.0256 (8)	0.0043 (6)	0.0015 (6)	0.0015 (6)
N4	0.0295 (8)	0.0291 (9)	0.0274 (8)	0.0063 (7)	0.0019 (6)	0.0005 (7)
O1	0.0260 (7)	0.0374 (8)	0.0298 (7)	0.0018 (6)	−0.0003 (5)	−0.0014 (6)
O2	0.0387 (8)	0.0394 (8)	0.0229 (7)	0.0030 (6)	0.0040 (6)	−0.0022 (6)
O4	0.0692 (14)	0.0753 (16)	0.0579 (13)	0.0224 (12)	0.0159 (11)	0.0070 (11)
O5	0.0678 (14)	0.0646 (15)	0.0665 (14)	0.0084 (11)	0.0022 (11)	0.0222 (11)
O6	0.0618 (14)	0.0878 (18)	0.0730 (17)	−0.0079 (12)	0.0045 (11)	0.0232 (14)

Co1—O1	1.8896 (14)	C11—C12	1.377 (3)
Co1—O2	1.8897 (14)	C11—H11	0.9300
Co1—N2	1.9195 (16)	C12—C13	1.376 (3)
Co1—N4	1.9238 (16)	C12—H12	0.9300
Co1—N1	1.9440 (17)	C13—C14	1.383 (3)
Co1—N3	1.9447 (16)	C13—H13	0.9300
Co1—C21	2.314 (2)	C14—C15	1.384 (3)
C1—N2	1.339 (3)	C14—H14	0.9300
C1—C2	1.378 (3)	C15—N3	1.352 (2)
C1—H1	0.9300	C15—C16	1.474 (3)
C2—C3	1.381 (3)	C16—N4	1.353 (3)
C2—H2	0.9300	C16—C17	1.373 (3)
C3—C4	1.377 (3)	C17—C18	1.385 (3)
C3—H3	0.9300	C17—H17	0.9300
C4—C5	1.384 (3)	C18—C19	1.370 (4)
C4—H4	0.9300	C18—H18	0.9300
C5—N2	1.353 (2)	C19—C20	1.379 (3)
C5—C6	1.467 (3)	C19—H19	0.9300
C6—N1	1.357 (2)	C20—N4	1.342 (3)
C6—C7	1.387 (3)	C20—H20	0.9300
C7—C8	1.380 (3)	O3—C21	1.219 (3)
C7—H7	0.9300	C21—O2	1.307 (3)
C8—C9	1.378 (4)	C21—O1	1.324 (3)
C8—H8	0.9300	O4—H4A	0.839 (10)
C9—C10	1.384 (3)	O4—H4B	0.841 (10)
C9—H9	0.9300	O5—H5A	0.835 (10)
C10—N1	1.339 (3)	O5—H5B	0.837 (10)
C10—H10	0.9300	O6—H6A	0.841 (10)
C11—N3	1.346 (3)	O6—H6B	0.840 (10)
O1—Co1—O2	69.26 (6)	N3—C11—H11	119.1
O1—Co1—N2	91.31 (7)	C12—C11—H11	119.1
O2—Co1—N2	88.81 (7)	C13—C12—C11	119.1 (2)
O1—Co1—N4	88.69 (7)	C13—C12—H12	120.4
O2—Co1—N4	92.44 (7)	C11—C12—H12	120.4
N2—Co1—N4	178.66 (7)	C12—C13—C14	119.7 (2)
O1—Co1—N1	165.27 (7)	C12—C13—H13	120.2
O2—Co1—N1	96.93 (7)	C14—C13—H13	120.2
N2—Co1—N1	83.06 (7)	C13—C14—C15	118.66 (19)
N4—Co1—N1	97.25 (7)	C13—C14—H14	120.7
O1—Co1—N3	97.79 (6)	C15—C14—H14	120.7
O2—Co1—N3	166.44 (7)	N3—C15—C14	121.61 (18)
N2—Co1—N3	95.69 (7)	N3—C15—C16	114.35 (16)
N4—Co1—N3	82.99 (7)	C14—C15—C16	124.04 (18)
N1—Co1—N3	96.31 (7)	N4—C16—C17	121.78 (18)
O1—Co1—C21	34.90 (7)	N4—C16—C15	113.11 (16)
O2—Co1—C21	34.39 (7)	C17—C16—C15	125.10 (18)
N2—Co1—C21	89.09 (7)	C16—C17—C18	118.9 (2)
N4—Co1—C21	91.68 (7)	C16—C17—H17	120.6
N1—Co1—C21	131.00 (7)	C18—C17—H17	120.6
N3—Co1—C21	132.64 (7)	C19—C18—C17	119.2 (2)
N2—C1—C2	121.8 (2)	C19—C18—H18	120.4
N2—C1—H1	119.1	C17—C18—H18	120.4
C2—C1—H1	119.1	C18—C19—C20	119.7 (2)
C1—C2—C3	118.9 (2)	C18—C19—H19	120.1
C1—C2—H2	120.5	C20—C19—H19	120.1
C3—C2—H2	120.5	N4—C20—C19	121.3 (2)
C4—C3—C2	119.6 (2)	N4—C20—H20	119.4
C4—C3—H3	120.2	C19—C20—H20	119.4
C2—C3—H3	120.2	O3—C21—O2	125.6 (2)
C3—C4—C5	119.1 (2)	O3—C21—O1	124.9 (2)
C3—C4—H4	120.4	O2—C21—O1	109.44 (18)
C5—C4—H4	120.4	O3—C21—Co1	177.39 (19)
N2—C5—C4	121.01 (19)	O2—C21—Co1	54.74 (10)
N2—C5—C6	113.60 (16)	O1—C21—Co1	54.75 (10)
C4—C5—C6	125.38 (18)	C10—N1—C6	119.14 (17)
N1—C6—C7	121.44 (19)	C10—N1—Co1	126.97 (14)
N1—C6—C5	114.04 (17)	C6—N1—Co1	113.81 (14)
C7—C6—C5	124.51 (18)	C1—N2—C5	119.56 (17)
C8—C7—C6	118.9 (2)	C1—N2—Co1	125.30 (14)
C8—C7—H7	120.5	C5—N2—Co1	115.00 (14)
C6—C7—H7	120.5	C11—N3—C15	119.05 (17)
C9—C8—C7	119.6 (2)	C11—N3—Co1	127.02 (14)
C9—C8—H8	120.2	C15—N3—Co1	113.76 (12)
C7—C8—H8	120.2	C20—N4—C16	119.12 (17)
C8—C9—C10	119.1 (2)	C20—N4—Co1	125.47 (14)
C8—C9—H9	120.4	C16—N4—Co1	115.00 (13)
C10—C9—H9	120.4	C21—O1—Co1	90.36 (12)
N1—C10—C9	121.8 (2)	C21—O2—Co1	90.87 (12)
N1—C10—H10	119.1	H4A—O4—H4B	106.4 (16)
C9—C10—H10	119.1	H5A—O5—H5B	106.9 (16)
N3—C11—C12	121.83 (19)	H6A—O6—H6B	105.4 (16)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4B···O5i	0.841 (10)	1.997 (11)	2.832 (3)	172 (3)
O4—H4A···O5ii	0.839 (10)	2.016 (12)	2.847 (3)	171 (4)
O5—H5A···O3iii	0.835 (10)	1.907 (12)	2.735 (3)	171 (3)
O5—H5B···Br1	0.837 (10)	2.422 (13)	3.247 (2)	169 (3)
O6—H6B···Br1	0.840 (10)	2.514 (12)	3.345 (2)	170 (3)
O6—H6A···Br1iv	0.841 (10)	2.541 (12)	3.378 (3)	173 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H4B⋯O5i	0.841 (10)	1.997 (11)	2.832 (3)	172 (3)
O4—H4A⋯O5ii	0.839 (10)	2.016 (12)	2.847 (3)	171 (4)
O5—H5A⋯O3iii	0.835 (10)	1.907 (12)	2.735 (3)	171 (3)
O5—H5B⋯Br1	0.837 (10)	2.422 (13)	3.247 (2)	169 (3)
O6—H6B⋯Br1	0.840 (10)	2.514 (12)	3.345 (2)	170 (3)
O6—H6A⋯Br1iv	0.841 (10)	2.541 (12)	3.378 (3)	173 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .