Poly[di-μ(2)-acetato-diaquabis(2,2'-bi-pyridine)bis(μ(3)-5-nitroisophthalato)tricobalt(II)].

The title complex, [Co(3)(C(8)H(3)NO(6))(2)(C(2)H(3)O(2))(2)(C(10)H(8)N(2))(2)(H(2)O)(2)], was synthesized under hydro-thermal conditions. The structure features a centrosymmetric complex with three Co(II) centres, one of which is located on a centre of inversion. The Co centres are coordinated in a distorted octa-hedral geometry. The bipyridine ligands are bonded to just one Co centre in a chelating mode, whereas the 5-nitro-isophthalate and acetate ions are bonded to two different Co atoms. The crystal structure is stabilized by O-H⋯O hydrogen bonds.

Related literature

For related structures, see: He et al. (2004 ▶, 2005 ▶); Zhang et al. (2006 ▶).

Experimental

Crystal data

[Co3(C8H3NO6)2(C2H3O2)2(C10H8N2)2(H2O)2]

M = 1061.51

Triclinic,

a = 10.0084 (1) Å

b = 10.0781 (1) Å

c = 11.3941 (1) Å

α = 81.196 (1)°

β = 67.685 (1)°

γ = 69.472 (1)°

V = 995.43 (2) Å3

Z = 1

Mo Kα radiation

μ = 1.33 mm−1

T = 296 K

0.26 × 0.13 × 0.10 mm

Data collection

Bruker SMART 1K CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T min = 0.724, T max = 0.883

10424 measured reflections

3679 independent reflections

3296 reflections with I > 2σ(I)

R int = 0.020

Refinement

R[F 2 > 2σ(F 2)] = 0.030

wR(F 2) = 0.077

S = 1.03

3679 reflections

310 parameters

3 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.53 e Å−3

Δρmin = −0.45 e Å−3

Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶).

Crystal structure: contains datablocks I, added_by_encifer. DOI: 10.1107/S1600536809012562/bt2923sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809012562/bt2923Isup2.hkl

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

[Co3(C8H3NO6)2(C2H3O2)2(C10H8N2)2(H2O)2]	Z = 1
Mr = 1061.51	F(000) = 539
Triclinic, P1	Dx = 1.771 Mg m−3
a = 10.0084 (1) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.0781 (1) Å	Cell parameters from 10424 reflections
c = 11.3941 (1) Å	θ = 1.9–25.5°
α = 81.196 (1)°	µ = 1.33 mm−1
β = 67.685 (1)°	T = 296 K
γ = 69.472 (1)°	Plate, red
V = 995.43 (2) Å3	0.26 × 0.13 × 0.10 mm

Bruker SMART 1K CCD diffractometer	3679 independent reflections
Radiation source: fine-focus sealed tube	3296 reflections with I > 2σ(I)
graphite	Rint = 0.020
phi/ω scans	θmax = 25.5°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −12→12
Tmin = 0.724, Tmax = 0.883	k = −12→12
10424 measured reflections	l = −13→13

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ2(Fo2) + (0.0358P)2 + 1.058P] where P = (Fo2 + 2Fc2)/3
3679 reflections	(Δ/σ)max < 0.001
310 parameters	Δρmax = 0.53 e Å−3
3 restraints	Δρmin = −0.45 e Å−3

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.

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 > 2sigma(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.

	x	y	z	Uiso*/Ueq
Co1	0.0000	1.0000	0.5000	0.02056 (11)
Co2	0.29863 (3)	0.66172 (3)	0.34001 (3)	0.02348 (10)
N1	0.5014 (2)	0.4947 (2)	0.26205 (19)	0.0264 (4)
N2	0.2395 (2)	0.5533 (2)	0.23098 (19)	0.0271 (4)
C6	0.3533 (3)	0.4463 (2)	0.1610 (2)	0.0259 (5)
O1	0.38924 (18)	0.74188 (17)	0.43457 (16)	0.0283 (4)
O9	0.10814 (18)	0.86327 (17)	0.34394 (15)	0.0263 (4)
C11	0.5544 (3)	0.8074 (2)	0.5603 (2)	0.0218 (5)
H11A	0.6088	0.7353	0.5017	0.026*
C17	0.3124 (3)	0.8272 (2)	0.5243 (2)	0.0233 (5)
C16	0.3980 (3)	0.8686 (2)	0.5891 (2)	0.0219 (5)
C19	0.8024 (3)	0.7950 (3)	0.5801 (2)	0.0269 (5)
C12	0.6310 (3)	0.8526 (2)	0.6180 (2)	0.0233 (5)
O3	0.8695 (2)	0.67757 (19)	0.5289 (2)	0.0414 (5)
C5	0.5033 (3)	0.4180 (2)	0.1738 (2)	0.0256 (5)
C4	0.6363 (3)	0.3199 (3)	0.1018 (2)	0.0337 (6)
H4A	0.6361	0.2703	0.0395	0.040*
C14	0.3935 (3)	1.0141 (2)	0.7364 (2)	0.0273 (5)
C13	0.5491 (3)	0.9578 (3)	0.7079 (2)	0.0272 (5)
H13A	0.5977	0.9894	0.7478	0.033*
C15	0.3160 (3)	0.9740 (2)	0.6786 (2)	0.0262 (5)
H15A	0.2114	1.0163	0.6989	0.031*
C9	0.0689 (3)	0.5133 (3)	0.1519 (3)	0.0382 (6)
H9A	−0.0288	0.5389	0.1495	0.046*
C7	0.3293 (3)	0.3687 (3)	0.0849 (3)	0.0352 (6)
H7A	0.4092	0.2951	0.0369	0.042*
C10	0.1008 (3)	0.5858 (3)	0.2260 (3)	0.0328 (6)
H10A	0.0225	0.6601	0.2742	0.039*
C1	0.6309 (3)	0.4698 (3)	0.2832 (3)	0.0327 (6)
H1A	0.6295	0.5217	0.3447	0.039*
C8	0.1844 (3)	0.4028 (3)	0.0818 (3)	0.0406 (7)
H8A	0.1652	0.3512	0.0324	0.049*
C2	0.7661 (3)	0.3707 (3)	0.2180 (3)	0.0379 (6)
H2A	0.8533	0.3539	0.2369	0.046*
N3	0.3069 (3)	1.1250 (3)	0.8321 (2)	0.0462 (6)
C3	0.7690 (3)	0.2970 (3)	0.1241 (3)	0.0392 (6)
H3A	0.8598	0.2323	0.0761	0.047*
O6	0.1710 (3)	1.1769 (3)	0.8577 (3)	0.0776 (9)
O2	0.17072 (18)	0.88101 (19)	0.56665 (16)	0.0318 (4)
O4	0.8652 (2)	0.8704 (2)	0.60355 (17)	0.0369 (4)
O5	0.3732 (3)	1.1514 (4)	0.8890 (3)	0.1161 (15)
O1W	0.17349 (19)	0.56964 (19)	0.50084 (18)	0.0318 (4)
H1WA	0.0831 (15)	0.620 (2)	0.523 (3)	0.048*
H1WB	0.180 (3)	0.4895 (15)	0.486 (3)	0.048*
O8	0.31763 (19)	0.80788 (18)	0.17845 (16)	0.0334 (4)
C32	0.1871 (3)	0.8911 (2)	0.2305 (2)	0.0263 (5)
C33	0.1213 (4)	1.0190 (3)	0.1602 (3)	0.0468 (7)
H33A	0.1949	1.0239	0.0772	0.070*
H33B	0.0952	1.1025	0.2056	0.070*
H33C	0.0314	1.0129	0.1524	0.070*

	U11	U22	U33	U12	U13	U23
Co1	0.0155 (2)	0.0220 (2)	0.0263 (2)	−0.00532 (16)	−0.00810 (17)	−0.00619 (17)
Co2	0.02330 (17)	0.02240 (17)	0.02775 (18)	−0.00702 (13)	−0.01024 (13)	−0.00655 (13)
N1	0.0258 (10)	0.0226 (10)	0.0315 (11)	−0.0068 (8)	−0.0108 (8)	−0.0030 (8)
N2	0.0270 (10)	0.0274 (10)	0.0295 (11)	−0.0090 (8)	−0.0106 (9)	−0.0057 (8)
C6	0.0327 (13)	0.0215 (11)	0.0249 (12)	−0.0087 (10)	−0.0114 (10)	−0.0010 (9)
O1	0.0230 (8)	0.0311 (9)	0.0350 (9)	−0.0075 (7)	−0.0115 (7)	−0.0123 (7)
O9	0.0279 (9)	0.0240 (8)	0.0270 (9)	−0.0078 (7)	−0.0085 (7)	−0.0052 (7)
C11	0.0251 (11)	0.0195 (11)	0.0236 (11)	−0.0089 (9)	−0.0092 (9)	−0.0022 (9)
C17	0.0251 (12)	0.0214 (11)	0.0255 (12)	−0.0074 (9)	−0.0121 (9)	0.0016 (9)
C16	0.0243 (11)	0.0212 (11)	0.0221 (11)	−0.0085 (9)	−0.0093 (9)	−0.0001 (9)
C19	0.0258 (12)	0.0310 (13)	0.0279 (12)	−0.0145 (10)	−0.0099 (10)	0.0027 (10)
C12	0.0256 (12)	0.0219 (11)	0.0256 (11)	−0.0115 (9)	−0.0099 (9)	0.0020 (9)
O3	0.0261 (9)	0.0334 (10)	0.0636 (13)	−0.0083 (8)	−0.0114 (9)	−0.0124 (9)
C5	0.0301 (12)	0.0213 (11)	0.0248 (12)	−0.0083 (10)	−0.0093 (10)	0.0005 (9)
C4	0.0369 (14)	0.0273 (13)	0.0303 (13)	−0.0046 (11)	−0.0087 (11)	−0.0040 (10)
C14	0.0327 (13)	0.0255 (12)	0.0241 (12)	−0.0113 (10)	−0.0063 (10)	−0.0070 (10)
C13	0.0337 (13)	0.0317 (13)	0.0246 (12)	−0.0182 (11)	−0.0113 (10)	−0.0029 (10)
C15	0.0239 (12)	0.0250 (12)	0.0274 (12)	−0.0058 (9)	−0.0073 (9)	−0.0040 (10)
C9	0.0380 (15)	0.0400 (15)	0.0478 (16)	−0.0155 (12)	−0.0235 (13)	−0.0031 (13)
C7	0.0434 (15)	0.0287 (13)	0.0365 (14)	−0.0074 (11)	−0.0180 (12)	−0.0090 (11)
C10	0.0288 (13)	0.0325 (13)	0.0387 (14)	−0.0082 (11)	−0.0117 (11)	−0.0098 (11)
C1	0.0318 (13)	0.0284 (13)	0.0433 (15)	−0.0104 (11)	−0.0180 (11)	−0.0015 (11)
C8	0.0552 (18)	0.0359 (15)	0.0451 (16)	−0.0165 (13)	−0.0280 (14)	−0.0090 (12)
C2	0.0274 (13)	0.0329 (14)	0.0530 (17)	−0.0102 (11)	−0.0160 (12)	0.0063 (13)
N3	0.0444 (15)	0.0481 (14)	0.0441 (14)	−0.0132 (12)	−0.0057 (11)	−0.0256 (12)
C3	0.0300 (14)	0.0309 (14)	0.0419 (15)	−0.0007 (11)	−0.0053 (12)	−0.0006 (12)
O6	0.0595 (16)	0.0778 (18)	0.0809 (18)	0.0265 (13)	−0.0342 (14)	−0.0527 (15)
O2	0.0200 (8)	0.0421 (10)	0.0341 (9)	−0.0035 (7)	−0.0137 (7)	−0.0073 (8)
O4	0.0339 (10)	0.0497 (11)	0.0392 (10)	−0.0286 (9)	−0.0109 (8)	−0.0037 (9)
O5	0.0539 (16)	0.176 (3)	0.130 (3)	−0.0378 (19)	0.0024 (16)	−0.128 (3)
O1W	0.0276 (9)	0.0288 (9)	0.0382 (10)	−0.0091 (7)	−0.0093 (8)	−0.0044 (8)
O8	0.0297 (9)	0.0333 (9)	0.0322 (9)	−0.0078 (8)	−0.0055 (8)	−0.0059 (8)
C32	0.0309 (13)	0.0255 (12)	0.0277 (12)	−0.0107 (10)	−0.0125 (10)	−0.0058 (10)
C33	0.0542 (18)	0.0416 (16)	0.0379 (16)	−0.0079 (14)	−0.0182 (14)	0.0054 (13)

Co1—O2	2.0503 (16)	C5—C4	1.384 (3)
Co1—O2i	2.0503 (16)	C4—C3	1.381 (4)
Co1—O9i	2.1153 (15)	C4—H4A	0.9300
Co1—O9	2.1153 (15)	C14—C15	1.375 (3)
Co1—O4ii	2.1154 (17)	C14—C13	1.380 (4)
Co1—O4iii	2.1154 (17)	C14—N3	1.471 (3)
Co2—O1	2.0392 (15)	C13—H13A	0.9300
Co2—O1W	2.0831 (18)	C15—H15A	0.9300
Co2—N1	2.1053 (19)	C9—C8	1.372 (4)
Co2—N2	2.1249 (19)	C9—C10	1.380 (4)
Co2—O8	2.1668 (18)	C9—H9A	0.9300
Co2—O9	2.2382 (16)	C7—C8	1.382 (4)
N1—C1	1.338 (3)	C7—H7A	0.9300
N1—C5	1.350 (3)	C10—H10A	0.9300
N2—C10	1.331 (3)	C1—C2	1.377 (4)
N2—C6	1.345 (3)	C1—H1A	0.9300
C6—C7	1.385 (3)	C8—H8A	0.9300
C6—C5	1.487 (3)	C2—C3	1.380 (4)
O1—C17	1.259 (3)	C2—H2A	0.9300
O9—C32	1.281 (3)	N3—O5	1.199 (3)
C11—C16	1.391 (3)	N3—O6	1.206 (3)
C11—C12	1.395 (3)	C3—H3A	0.9300
C11—H11A	0.9300	O4—Co1iv	2.1154 (17)
C17—O2	1.248 (3)	O1W—H1WA	0.826 (10)
C17—C16	1.508 (3)	O1W—H1WB	0.824 (10)
C16—C15	1.388 (3)	O8—C32	1.248 (3)
C19—O3	1.244 (3)	C32—C33	1.493 (4)
C19—O4	1.252 (3)	C33—H33A	0.9600
C19—C12	1.510 (3)	C33—H33B	0.9600
C12—C13	1.390 (3)	C33—H33C	0.9600
O2—Co1—O2i	180.0	C13—C12—C19	119.0 (2)
O2—Co1—O9i	92.58 (6)	C11—C12—C19	121.4 (2)
O2i—Co1—O9i	87.42 (6)	N1—C5—C4	121.7 (2)
O2—Co1—O9	87.42 (6)	N1—C5—C6	115.1 (2)
O2i—Co1—O9	92.58 (6)	C4—C5—C6	123.2 (2)
O9i—Co1—O9	180.000 (1)	C3—C4—C5	119.0 (2)
O2—Co1—O4ii	90.67 (7)	C3—C4—H4A	120.5
O2i—Co1—O4ii	89.33 (7)	C5—C4—H4A	120.5
O9i—Co1—O4ii	88.72 (7)	C15—C14—C13	123.5 (2)
O9—Co1—O4ii	91.28 (7)	C15—C14—N3	118.4 (2)
O2—Co1—O4iii	89.33 (7)	C13—C14—N3	118.1 (2)
O2i—Co1—O4iii	90.67 (7)	C14—C13—C12	118.1 (2)
O9i—Co1—O4iii	91.28 (7)	C14—C13—H13A	120.9
O9—Co1—O4iii	88.72 (7)	C12—C13—H13A	120.9
O4ii—Co1—O4iii	180.0	C14—C15—C16	118.3 (2)
O1—Co2—O1W	94.98 (7)	C14—C15—H15A	120.9
O1—Co2—N1	94.01 (7)	C16—C15—H15A	120.9
O1W—Co2—N1	103.72 (7)	C8—C9—C10	118.6 (2)
O1—Co2—N2	170.78 (7)	C8—C9—H9A	120.7
O1W—Co2—N2	87.41 (7)	C10—C9—H9A	120.7
N1—Co2—N2	76.77 (7)	C8—C7—C6	118.7 (2)
O1—Co2—O8	98.32 (7)	C8—C7—H7A	120.7
O1W—Co2—O8	152.53 (7)	C6—C7—H7A	120.7
N1—Co2—O8	99.22 (7)	N2—C10—C9	122.5 (2)
N2—Co2—O8	83.29 (7)	N2—C10—H10A	118.8
O1—Co2—O9	94.50 (6)	C9—C10—H10A	118.8
O1W—Co2—O9	95.80 (7)	N1—C1—C2	123.0 (2)
N1—Co2—O9	157.91 (7)	N1—C1—H1A	118.5
N2—Co2—O9	94.12 (7)	C2—C1—H1A	118.5
O8—Co2—O9	59.37 (6)	C9—C8—C7	119.6 (2)
C1—N1—C5	118.4 (2)	C9—C8—H8A	120.2
C1—N1—Co2	124.99 (16)	C7—C8—H8A	120.2
C5—N1—Co2	116.21 (15)	C1—C2—C3	118.4 (2)
C10—N2—C6	119.0 (2)	C1—C2—H2A	120.8
C10—N2—Co2	124.78 (16)	C3—C2—H2A	120.8
C6—N2—Co2	116.22 (15)	O5—N3—O6	122.5 (3)
N2—C6—C7	121.6 (2)	O5—N3—C14	117.9 (3)
N2—C6—C5	114.8 (2)	O6—N3—C14	119.3 (2)
C7—C6—C5	123.6 (2)	C2—C3—C4	119.5 (2)
C17—O1—Co2	124.66 (14)	C2—C3—H3A	120.3
C32—O9—Co1	126.76 (14)	C4—C3—H3A	120.3
C32—O9—Co2	88.61 (13)	C17—O2—Co1	138.15 (16)
Co1—O9—Co2	121.97 (8)	C19—O4—Co1iv	137.23 (17)
C16—C11—C12	121.0 (2)	Co2—O1W—H1WA	109 (2)
C16—C11—H11A	119.5	Co2—O1W—H1WB	111 (2)
C12—C11—H11A	119.5	H1WA—O1W—H1WB	109 (2)
O2—C17—O1	126.4 (2)	C32—O8—Co2	92.74 (15)
O2—C17—C16	116.0 (2)	O8—C32—O9	119.2 (2)
O1—C17—C16	117.6 (2)	O8—C32—C33	120.5 (2)
C15—C16—C11	119.6 (2)	O9—C32—C33	120.2 (2)
C15—C16—C17	117.9 (2)	C32—C33—H33A	109.5
C11—C16—C17	122.5 (2)	C32—C33—H33B	109.5
O3—C19—O4	125.4 (2)	H33A—C33—H33B	109.5
O3—C19—C12	118.0 (2)	C32—C33—H33C	109.5
O4—C19—C12	116.6 (2)	H33A—C33—H33C	109.5
C13—C12—C11	119.5 (2)	H33B—C33—H33C	109.5

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O3ii	0.83 (2)	1.99 (2)	2.755 (3)	154 (2)
O1W—H1WB···O3v	0.83 (2)	1.96 (2)	2.762 (3)	163 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯O3i	0.83 (2)	1.99 (2)	2.755 (3)	154 (2)
O1W—H1WB⋯O3ii	0.826 (18)	1.96 (2)	2.762 (3)	163 (3)

Symmetry codes: (i) ; (ii) .