Polymeric dihydroxydiphthalatotricobalt(II)

In the crystal structure of di­hydroxy­diphthalatotricobalt(II), [Co₃(C₈H₄O₄)₂(OH)₂]_n, two of the four independent Co atoms lie at special positions of site symmetry 2. The hydroxy groups link three Co atoms to form a pyramidal Co₃O unit, and adjacent Co₃O units are linked through the Co base atoms into a honeycomb layer motif. Each of the phthalate dianions uses the O atoms of one carboxyl group to bind to three Co atoms, the bonding mode giving rise to six-coordinate Co atoms.

S1. Comment

Hydrothermally synthesized cobalt(II) derivatives of benzene polycarboxylic acids exist as hydroxides. The tetracarboxylate compound adopts a framework architecture that constitutes roughly only half the volume of the unit cell (Gutschke et al., 2001a). Cobalt hydroxide 1,4-dicarboxylate, on the other hand, packs in such a manner that the π systems of adjacent carboxylate anions interact magnetically (Huang et al., 2000). Other than a tricarboxylate derivative (Gutschke et al., 2001b), there are no further reports to date of such cobalt hydroxide derivatives of benzene polycarboxylic acids.

Unlike the reaction of cobalt(II) carbonate with phthalic acid in water, which affords hexaaquacobalt hydrogen phthalate (Karuiki & Jones, 1993), the reaction of cobalt(II) nitrate and potassium hydrogen phthalate under hydrothermal conditions yielded the title cobalt(II) hydroxide derivative, (I), and its structure is presented here. \sch

The crystal structure of (I) is built up of a layer motif consisting of corner-sharing pyramidal Co₃O units. These units are linked through the Co corners to form a hexagonal unit, which also shares its Co corners to give rise to a honeycomb motif (Fig. 1). The layers that make up the structure feature a Co₃O core, and the aromatic groups protrude from the top and bottom of each layer. Where the layers come together, aromatic-aromatic edge-face interactions exist. The Co₃O unit is also documented in the other compounds mentioned above Added text OK?. For example, in the terephthalate derivative, [Co₂(OH)₂(C₈H₄O₄)], the Co₃O units form layer structures by edge- and corner-sharing (Huang et al., 2000). This layer motif is not adopted by the tri- and tetracarboxylates.

The four independent Co atoms in (I) exist in an octahedral environment (Fig. 2), and each is coordinated by four O atoms from carboxyl groups and two O atoms from hydroxyl groups. Each hydroxyl group bridges three Co atoms. For both independent phthalate dianions, each carboxyl –CO₂ group is linked to three Co atoms.

S2. Experimental

Cobalt(II) nitrate hexahydrate (0.17 g, 0.6 mmol) and potassium hydrogen phthalate (0.37 g, 1.8 mmol) were dissolved in water (15 ml). The solution was placed in a Teflon-lined stainless-steel vessel, which was then heated to 473 K for 60 h. The vessel was then allowed to cool to room temperature and needle-shaped crystals of (I) deposited from the solution in about 10% yield. Analysis calculated for C₁₆H₁₀O₁₀Co₃: C 35.65, H 1.87%; found: C 35.51, H 1.86%. FT—IR (KBr, ν, cm⁻¹): 3596 s, 3422 br, 3070 w, 2930 w, 1625 s, 1599 versus, 1581 s, 1568 s, 1494, 1448, 1425, 1389 s, 1280 w, 1156, 1093, 1040, 947 w, 868, 842, 806, 788, 767, 738, 699, 658, 588 w, 469, 452.

S3. Refinement

The aromatic and hydroxyl H atoms were generated geometrically (C—H = 0.93 Å and O—H = 0.98 Å) and were allowed to ride on their parent atoms in riding model approximations, with U_iso(H) set to 1.2U_eq(parent). The final difference map had peaks of more than 1 e Å⁻³ near the four Co atoms.

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. A plot of the layer structure of (I), illustrating the honeycomb motif that is built from Co3O pyramids.
	Fig. 2. (a)-(d). Views of the coordination environments of the four independent Co atoms in (I). Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. [Symmetry codes: (i) 1/2 − x, 1/2 − y, z; (ii) x, 1/2 − y, z − 1/2; (iii) 3/2 − x, y, z − 1/2; (iv) 3/2 − x, 1/2 − y, z; (v) x, 1/2 − y, 1/2 + z; (vi) 1/2 − x, y, 1/2 + z.]

Dihydroxydiphthalatotricobalt(II)

Crystal data

[Co3(C8H4O4)2(OH)2]	Dx = 2.195 Mg m^−3
Mr = 539.03	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pccn	Cell parameters from 8115 reflections
a = 12.1121 (5) Å	θ = 1.8–28.3°
b = 22.6847 (9) Å	µ = 3.08 mm^−1
c = 11.8730 (5) Å	T = 298 K
V = 3262.2 (2) Å^3	Needle, pink
Z = 8	0.45 × 0.13 × 0.03 mm
F(000) = 2136

Data collection

Bruker Model CCD area-detector diffractometer	3904 independent reflections
Radiation source: fine-focus sealed tube	2518 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.057
ϕ and ω scans	θmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→15
Tmin = 0.692, Tmax = 0.912	k = −30→30
26490 measured reflections	l = −15→15

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.104	H-atom parameters constrained
S = 0.89	w = 1/[σ^2(Fo^2) + (0.0664P)^2] where P = (Fo^2 + 2Fc^2)/3
3904 reflections	(Δ/σ)max = 0.001
263 parameters	Δρmax = 1.71 e Å^−3
0 restraints	Δρmin = −0.82 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.50050 (3)	0.25133 (2)	0.38816 (3)	0.0155 (1)
Co2	0.50056 (3)	0.20705 (2)	0.63811 (3)	0.0146 (1)
Co3	0.2500	0.2500	0.76830 (5)	0.0169 (2)
Co4	0.7500	0.2500	0.50924 (5)	0.0177 (2)
O1	0.4047 (2)	0.14511 (1)	0.5490 (2)	0.0213 (5)
O2	0.3586 (2)	0.1968 (1)	0.3958 (2)	0.0220 (5)
O3	0.1953 (2)	0.1872 (1)	0.6556 (2)	0.0274 (6)
O4	0.0606 (2)	0.2204 (1)	0.5451 (2)	0.0207 (5)
O5	0.6963 (2)	0.3129 (1)	0.6212 (2)	0.0277 (6)
O6	0.5637 (2)	0.2779 (1)	0.7336 (2)	0.0191 (5)
O7	0.9045 (2)	0.3565 (1)	0.7254 (2)	0.0224 (5)
O8	0.8587 (2)	0.3064 (1)	0.8818 (2)	0.0233 (5)
O9	0.6057 (2)	0.2066 (1)	0.4989 (2)	0.0155 (5)
O10	0.3943 (2)	0.2057 (1)	0.7764 (2)	0.0152 (5)
C1	0.3439 (2)	0.1557 (1)	0.4670 (3)	0.0172 (7)
C2	0.2451 (2)	0.1173 (1)	0.4470 (2)	0.0158 (6)
C3	0.2518 (3)	0.0701 (2)	0.3725 (3)	0.0273 (8)
C4	0.1616 (3)	0.0350 (2)	0.3524 (3)	0.035 (1)
C5	0.0617 (3)	0.0471 (2)	0.4041 (3)	0.0320 (9)
C6	0.0521 (3)	0.0946 (1)	0.4754 (3)	0.0248 (8)
C7	0.1445 (2)	0.1296 (1)	0.4989 (2)	0.0159 (7)
C8	0.1341 (2)	0.1831 (1)	0.5729 (3)	0.0164 (7)
C9	0.6354 (2)	0.3167 (1)	0.7048 (3)	0.0172 (7)
C10	0.6433 (3)	0.3700 (1)	0.7780 (3)	0.0169 (7)
C11	0.5492 (3)	0.4036 (1)	0.8010 (3)	0.0223 (7)
C12	0.5561 (3)	0.4518 (2)	0.8692 (3)	0.0306 (9)
C13	0.6558 (3)	0.4665 (2)	0.9192 (3)	0.0350 (9)
C14	0.7484 (3)	0.4331 (2)	0.8983 (3)	0.0298 (9)
C15	0.7445 (3)	0.3850 (1)	0.8263 (3)	0.0184 (7)
C16	0.8443 (3)	0.3467 (1)	0.8083 (3)	0.0180 (7)
H9	0.6179	0.1661	0.4728	0.019*
H10	0.3816	0.1651	0.8010	0.018*
H3	0.3181	0.0622	0.3360	0.033*
H4	0.1676	0.0030	0.3038	0.041*
H5	0.0010	0.0230	0.3907	0.038*
H6	−0.0157	0.1034	0.5080	0.030*
H11	0.4816	0.3930	0.7696	0.027*
H12	0.4939	0.4749	0.8823	0.037*
H13	0.6601	0.4989	0.9669	0.042*
H14	0.8147	0.4429	0.9330	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0066 (2)	0.0281 (3)	0.0118 (2)	−0.0011 (2)	−0.0008 (2)	0.0011 (2)
Co2	0.0086 (2)	0.0245 (2)	0.0105 (2)	0.0000 (2)	0.0000 (2)	0.0000 (2)
Co3	0.0064 (3)	0.0280 (4)	0.0164 (3)	0.0023 (3)	0.000	0.000
Co4	0.0072 (3)	0.0292 (4)	0.0166 (3)	−0.0029 (2)	0.000	0.000
O1	0.016 (1)	0.029 (1)	0.018 (1)	−0.003 (1)	−0.004 (1)	0.000 (1)
O2	0.013 (1)	0.035 (1)	0.019 (1)	−0.007 (1)	−0.003 (1)	0.005 (1)
O3	0.018 (1)	0.040 (2)	0.025 (1)	0.006 (1)	−0.010 (1)	−0.011 (1)
O4	0.023 (1)	0.025 (1)	0.014 (1)	0.009 (1)	−0.001 (1)	−0.0017 (9)
O5	0.020 (1)	0.039 (2)	0.025 (1)	−0.007 (1)	0.010 (1)	−0.010 (1)
O6	0.016 (1)	0.028 (1)	0.014 (1)	−0.004 (1)	−0.002 (1)	0.0000 (9)
O7	0.017 (1)	0.031 (1)	0.019 (1)	0.003 (1)	0.003 (1)	0.000 (1)
O8	0.014 (1)	0.037 (1)	0.019 (1)	0.009 (1)	0.002 (1)	0.004 (1)
O9	0.009 (1)	0.025 (1)	0.013 (1)	0.001 (1)	−0.001 (1)	−0.0023 (9)
O10	0.008 (1)	0.022 (1)	0.015 (1)	0.000 (1)	0.000 (1)	−0.0003 (9)
C1	0.009 (2)	0.027 (2)	0.015 (2)	0.001 (1)	0.002 (1)	−0.005 (1)
C2	0.011 (2)	0.022 (2)	0.015 (1)	−0.001 (1)	−0.001 (1)	0.001 (1)
C3	0.016 (2)	0.035 (2)	0.031 (2)	0.002 (2)	0.003 (2)	−0.011 (2)
C4	0.029 (2)	0.035 (2)	0.040 (2)	−0.005 (2)	0.001 (2)	−0.019 (2)
C5	0.019 (2)	0.037 (2)	0.041 (2)	−0.010 (2)	−0.002 (2)	−0.008 (2)
C6	0.011 (2)	0.033 (2)	0.031 (2)	−0.003 (1)	−0.001 (2)	−0.003 (2)
C7	0.012 (2)	0.019 (2)	0.017 (2)	−0.001 (1)	−0.003 (1)	0.001 (1)
C8	0.010 (2)	0.024 (2)	0.015 (2)	−0.001 (1)	0.001 (1)	−0.001 (1)
C9	0.010 (2)	0.027 (2)	0.015 (2)	0.002 (1)	−0.002 (1)	0.003 (1)
C10	0.013 (2)	0.023 (2)	0.015 (2)	−0.001 (1)	0.003 (1)	0.001 (1)
C11	0.009 (2)	0.032 (2)	0.025 (2)	0.000 (1)	0.002 (1)	−0.001 (2)
C12	0.015 (2)	0.037 (2)	0.040 (2)	0.007 (2)	0.005 (2)	−0.007 (2)
C13	0.027 (2)	0.039 (2)	0.040 (2)	0.002 (2)	0.000 (2)	−0.021 (2)
C14	0.016 (2)	0.039 (2)	0.034 (2)	0.000 (2)	−0.004 (2)	−0.016 (2)
C15	0.015 (2)	0.026 (2)	0.015 (2)	0.002 (1)	0.000 (1)	0.000 (1)
C16	0.011 (2)	0.027 (2)	0.016 (2)	0.001 (1)	−0.006 (1)	−0.008 (1)

Geometric parameters (Å, º)

Co1—O2	2.119 (2)	O6—C9	1.282 (4)
Co1—O4^i	2.105 (2)	O7—C16	1.245 (4)
Co1—O6^ii	2.097 (2)	O8—C16	1.276 (4)
Co1—O8^iii	2.115 (2)	C1—C2	1.498 (4)
Co1—O9	2.094 (2)	C2—C3	1.392 (4)
Co1—O10^ii	2.089 (2)	C2—C7	1.393 (4)
Co2—O1	2.108 (2)	C3—C4	1.373 (5)
Co2—O4^i	2.116 (2)	C4—C5	1.384 (5)
Co2—O6	2.110 (2)	C5—C6	1.375 (5)
Co2—O7^iv	2.115 (2)	C6—C7	1.401 (4)
Co2—O9	2.087 (2)	C7—C8	1.504 (4)
Co2—O10	2.086 (2)	C9—C10	1.493 (4)
Co3—O2^v	2.340 (2)	C10—C15	1.395 (4)
Co3—O2^vi	2.340 (2)	C10—C11	1.398 (4)
Co3—O3	2.063 (2)	C11—C12	1.364 (5)
Co3—O3^i	2.063 (2)	C12—C13	1.386 (5)
Co3—O10	2.018 (2)	C13—C14	1.375 (5)
Co3—O10^i	2.018 (2)	C14—C15	1.386 (5)
Co4—O5	2.056 (2)	C15—C16	1.504 (4)
Co4—O5^iv	2.056 (2)	O9—H9	0.98
Co4—O8^ii	2.379 (2)	O10—H10	0.98
Co4—O8^iii	2.379 (2)	C3—H3	0.93
Co4—O9	2.010 (2)	C4—H4	0.93
Co4—O9^iv	2.010 (2)	C5—H5	0.93
O1—C1	1.244 (4)	C6—H6	0.93
O2—C1	1.272 (4)	C11—H11	0.93
O3—C8	1.234 (4)	C12—H12	0.93
O4—C8	1.272 (4)	C13—H13	0.93
O5—C9	1.239 (4)	C14—H14	0.93
O2—Co1—O4^i	81.7 (1)	C9—O5—Co4	139.0 (2)
O2—Co1—O6^ii	98.5 (1)	C9—O6—Co1^v	134.2 (2)
O2—Co1—O8^iii	179.4 (1)	C9—O6—Co2	128.7 (2)
O2—Co1—O9	100.6 (1)	Co1^v—O6—Co2	95.6 (1)
O2—Co1—O10^ii	78.5 (1)	C16—O8—Co1^vii	123.9 (2)
O4^i—Co1—O6^ii	178.8 (1)	C16—O8—Co4^v	138.1 (2)
O4^i—Co1—O8^iii	97.8 (1)	Co1^vii—O8—Co4^v	96.1 (1)
O4^i—Co1—O9	78.8 (1)	C16—O7—Co2^iv	125.8 (2)
O4^i—Co1—O10^ii	101.8 (1)	Co4—O9—Co2	118.6 (1)
O6^ii—Co1—O8^iii	82.0 (1)	Co4—O9—Co1	109.3 (1)
O6^ii—Co1—O9	100.0 (1)	Co2—O9—Co1	97.1 (1)
O6^ii—Co1—O10^ii	79.4 (1)	Co3—O10—Co2	119.3 (1)
O8^iii—Co1—O9	79.5 (1)	Co3—O10—Co1^v	109.4 (1)
O8^iii—Co1—O10^ii	101.4 (1)	Co2—O10—Co1^v	96.5 (1)
O9—Co1—O10^ii	178.8 (1)	O1—C1—O2	125.4 (3)
O1—Co2—O4^i	93.7 (1)	O1—C1—C2	119.0 (3)
O1—Co2—O6	167.7 (1)	O2—C1—C2	115.6 (3)
O1—Co2—O7^iv	95.2 (1)	C3—C2—C7	119.1 (3)
O1—Co2—O9	86.3 (1)	C3—C2—C1	120.1 (3)
O1—Co2—O10	92.6 (1)	C7—C2—C1	120.8 (3)
O4^i—Co2—O6	79.3 (1)	C4—C3—C2	120.7 (3)
O4^i—Co2—O7^iv	167.5 (1)	C3—C4—C5	120.3 (3)
O4^i—Co2—O9	78.7 (1)	C6—C5—C4	120.1 (3)
O4^i—Co2—O10	101.9 (1)	C5—C6—C7	120.0 (3)
O6—Co2—O7^iv	93.4 (1)	C2—C7—C6	119.8 (3)
O6—Co2—O9	102.0 (1)	C2—C7—C8	119.5 (3)
O6—Co2—O10	79.2 (1)	C6—C7—C8	120.5 (3)
O7^iv—Co2—O9	93.0 (1)	O3—C8—O4	125.2 (3)
O7^iv—Co2—O10	86.6 (1)	O3—C8—C7	118.4 (3)
O9—Co2—O10	178.8 (1)	O4—C8—C7	116.4 (3)
O2^v—Co3—O2^vi	99.4 (1)	O5—C9—O6	124.6 (3)
O2^v—Co3—O3	162.9 (1)	O5—C9—C10	119.0 (3)
O2^v—Co3—O3^i	83.3 (1)	O6—C9—C10	116.4 (3)
O2^v—Co3—O10	74.9 (1)	C15—C10—C11	120.3 (3)
O2^v—Co3—O10^i	101.5 (1)	C15—C10—C9	119.5 (3)
O2^vi—Co3—O3	83.3 (1)	C11—C10—C9	120.2 (3)
O2^vi—Co3—O3^i	162.9 (1)	C12—C11—C10	120.1 (3)
O2^vi—Co3—O10	101.5 (1)	C11—C12—C13	120.0 (3)
O2^vi—Co3—O10^i	74.9 (1)	C14—C13—C12	120.0 (3)
O3—Co3—O3^i	99.1 (1)	C13—C14—C15	121.1 (3)
O3—Co3—O10	88.0 (1)	C14—C15—C10	118.3 (3)
O3—Co3—O10^i	95.5 (1)	C14—C15—C16	121.0 (3)
O3^i—Co3—O10	95.5 (1)	C10—C15—C16	120.5 (3)
O3^i—Co3—O10^i	88.0 (1)	O7—C16—O8	126.0 (3)
O10—Co3—O10^i	174.6 (1)	O7—C16—C15	118.7 (3)
O5—Co4—O5^iv	99.4 (1)	O8—C16—C15	115.2 (3)
O5—Co4—O8^ii	163.7 (1)	Co4—O9—H9	110.3
O5—Co4—O8^iii	82.1 (1)	Co2—O9—H9	110.3
O5—Co4—O9	96.0 (1)	Co1—O9—H9	110.3
O5—Co4—O9^iv	88.5 (1)	Co3—O10—H10	110.2
O5^iv—Co4—O9^iv	96.0 (1)	Co2—O10—H10	110.2
O5^iv—Co4—O9	88.5 (1)	Co1^v—O10—H10	110.2
O5^iv—Co4—O8^ii	82.1 (1)	C4—C3—H3	119.6
O5^iv—Co4—O8^iii	163.7 (1)	C2—C3—H3	119.6
O8^ii—Co4—O8^iii	101.0 (1)	C3—C4—H4	119.9
O8^ii—Co4—O9^iv	75.1 (1)	C5—C4—H4	119.9
O8^ii—Co4—O9	100.3 (1)	C6—C5—H5	119.9
O8^iii—Co4—O9	75.1 (1)	C4—C5—H5	119.9
O8^iii—Co4—O9^iv	100.3 (1)	C5—C6—H6	120.0
O9—Co4—O9^iv	173.0 (1)	C7—C6—H6	120.0
C1—O1—Co2	126.1 (2)	C12—C11—H11	119.9
C1—O2—Co1	124.7 (2)	C10—C11—H11	119.9
C1—O2—Co3^ii	136.8 (2)	C11—C12—H12	120.0
Co1—O2—Co3^ii	97.3 (1)	C13—C12—H12	120.0
C8—O3—Co3	139.6 (2)	C14—C13—H13	120.0
C8—O4—Co1^i	132.7 (2)	C12—C13—H13	120.0
C8—O4—Co2^i	128.8 (2)	C13—C14—H14	119.4
Co1^i—O4—Co2^i	95.9 (1)	C15—C14—H14	119.4
O10—Co2—O1—C1	106.4 (3)	O4^i—Co2—O10—Co3	17.0 (1)
O9—Co2—O1—C1	−74.2 (3)	O1—Co2—O10—Co1^v	166.2 (1)
O6—Co2—O1—C1	58.9 (5)	O6—Co2—O10—Co1^v	−23.0 (1)
O7^iv—Co2—O1—C1	−166.9 (3)	O7^iv—Co2—O10—Co1^v	71.1 (1)
O4^i—Co2—O1—C1	4.3 (3)	O4^i—Co2—O10—Co1^v	−99.5 (1)
O10^ii—Co1—O2—C1	−169.8 (3)	Co2—O1—C1—O2	29.2 (5)
O9—Co1—O2—C1	11.0 (3)	Co2—O1—C1—C2	−151.5 (2)
O6^ii—Co1—O2—C1	112.9 (3)	Co1—O2—C1—O1	7.5 (5)
O4^i—Co1—O2—C1	−65.9 (3)	Co3^ii—O2—C1—O1	−157.7 (2)
O10^ii—Co1—O2—Co3^ii	0.0 (1)	Co1—O2—C1—C2	−171.8 (2)
O9—Co1—O2—Co3^ii	−179.2 (1)	Co3^ii—O2—C1—C2	23.0 (4)
O6^ii—Co1—O2—Co3^ii	−77.2 (1)	O1—C1—C2—C3	−95.4 (4)
O4^i—Co1—O2—Co3^ii	103.93 (9)	O2—C1—C2—C3	83.9 (4)
O10^i—Co3—O3—C8	36.7 (4)	O1—C1—C2—C7	87.1 (4)
O10—Co3—O3—C8	−147.5 (3)	O2—C1—C2—C7	−93.6 (4)
O3^i—Co3—O3—C8	−52.2 (3)	C7—C2—C3—C4	−1.7 (5)
O2^v—Co3—O3—C8	−149.1 (3)	C1—C2—C3—C4	−179.2 (3)
O2^vi—Co3—O3—C8	110.7 (3)	C2—C3—C4—C5	1.5 (6)
O9—Co4—O5—C9	38.2 (4)	C3—C4—C5—C6	0.5 (6)
O9^iv—Co4—O5—C9	−147.1 (3)	C4—C5—C6—C7	−2.3 (6)
O5^iv—Co4—O5—C9	−51.3 (3)	C3—C2—C7—C6	−0.1 (5)
O8^iii—Co4—O5—C9	112.3 (3)	C1—C2—C7—C6	177.4 (3)
O8^ii—Co4—O5—C9	−145.4 (3)	C3—C2—C7—C8	−175.5 (3)
O10—Co2—O6—C9	−169.9 (3)	C1—C2—C7—C8	2.0 (4)
O9—Co2—O6—C9	10.4 (3)	C5—C6—C7—C2	2.1 (5)
O1—Co2—O6—C9	−121.4 (4)	C5—C6—C7—C8	177.5 (3)
O7^iv—Co2—O6—C9	104.3 (3)	Co3—O3—C8—O4	−17.6 (6)
O4^i—Co2—O6—C9	−65.5 (3)	Co3—O3—C8—C7	163.5 (2)
O10—Co2—O6—Co1^v	22.9 (1)	Co1^i—O4—C8—O3	146.7 (3)
O9—Co2—O6—Co1^v	−156.8 (1)	Co2^i—O4—C8—O3	−10.5 (5)
O1—Co2—O6—Co1^v	71.5 (4)	Co1^i—O4—C8—C7	−34.4 (4)
O7^iv—Co2—O6—Co1^v	−62.9 (1)	Co2^i—O4—C8—C7	168.4 (2)
O4^i—Co2—O6—Co1^v	127.4 (1)	C2—C7—C8—O3	−59.2 (4)
O5—Co4—O9—Co2	−29.5 (1)	C6—C7—C8—O3	125.5 (3)
O5^iv—Co4—O9—Co2	69.8 (1)	C2—C7—C8—O4	121.9 (3)
O8^iii—Co4—O9—Co2	−109.7 (1)	C6—C7—C8—O4	−53.5 (4)
O8^ii—Co4—O9—Co2	151.5 (1)	Co4—O5—C9—O6	−16.5 (5)
O5—Co4—O9—Co1	80.3 (1)	Co4—O5—C9—C10	164.4 (2)
O5^iv—Co4—O9—Co1	179.6 (1)	Co1^v—O6—C9—O5	148.0 (3)
O8^iii—Co4—O9—Co1	0.1 (1)	Co2—O6—C9—O5	−14.1 (5)
O8^ii—Co4—O9—Co1	−98.7 (1)	Co1^v—O6—C9—C10	−32.9 (4)
O1—Co2—O9—Co4	−172.3 (1)	Co2—O6—C9—C10	165.0 (2)
O6—Co2—O9—Co4	16.9 (1)	O5—C9—C10—C15	−57.0 (4)
O7^iv—Co2—O9—Co4	−77.2 (1)	O6—C9—C10—C15	123.9 (3)
O4^i—Co2—O9—Co4	93.3 (1)	O5—C9—C10—C11	125.1 (3)
O1—Co2—O9—Co1	71.2 (1)	O6—C9—C10—C11	−54.1 (4)
O6—Co2—O9—Co1	−99.6 (1)	C15—C10—C11—C12	1.1 (5)
O7^iv—Co2—O9—Co1	166.3 (1)	C9—C10—C11—C12	179.0 (3)
O4^i—Co2—O9—Co1	−23.3 (1)	C10—C11—C12—C13	−2.2 (5)
O6^ii—Co1—O9—Co4	79.7 (1)	C11—C12—C13—C14	1.3 (6)
O4^i—Co1—O9—Co4	−100.3 (1)	C12—C13—C14—C15	0.9 (6)
O8^iii—Co1—O9—Co4	−0.2 (1)	C13—C14—C15—C10	−1.9 (6)
O2—Co1—O9—Co4	−179.5 (1)	C13—C14—C15—C16	−176.8 (4)
O6^ii—Co1—O9—Co2	−156.6 (1)	C11—C10—C15—C14	1.0 (5)
O4^i—Co1—O9—Co2	23.4 (1)	C9—C10—C15—C14	−176.9 (3)
O8^iii—Co1—O9—Co2	123.6 (1)	C11—C10—C15—C16	175.8 (3)
O2—Co1—O9—Co2	−55.8 (1)	C9—C10—C15—C16	−2.1 (5)
O3—Co3—O10—Co2	70.9 (1)	Co2^iv—O7—C16—O8	29.4 (5)
O3^i—Co3—O10—Co2	−28.1 (1)	Co2^iv—O7—C16—C15	−150.5 (2)
O2^v—Co3—O10—Co2	−109.6 (1)	Co1^vii—O8—C16—O7	6.4 (5)
O2^vi—Co3—O10—Co2	153.6 (1)	Co4^v—O8—C16—O7	−153.9 (2)
O3—Co3—O10—Co1^v	−179.5 (1)	Co1^vii—O8—C16—C15	−173.7 (2)
O3^i—Co3—O10—Co1^v	81.5 (1)	Co4^v—O8—C16—C15	26.0 (4)
O2^v—Co3—O10—Co1^v	0.0 (1)	C14—C15—C16—O7	−96.1 (4)
O2^vi—Co3—O10—Co1^v	−96.8 (1)	C10—C15—C16—O7	89.2 (4)
O1—Co2—O10—Co3	−77.3 (1)	C14—C15—C16—O8	84.0 (4)
O6—Co2—O10—Co3	93.5 (1)	C10—C15—C16—O8	−90.8 (4)
O7^iv—Co2—O10—Co3	−172.4 (1)

Symmetry codes: (i) −x+1/2, −y+1/2, z; (ii) x, −y+1/2, z−1/2; (iii) −x+3/2, y, z−1/2; (iv) −x+3/2, −y+1/2, z; (v) x, −y+1/2, z+1/2; (vi) −x+1/2, y, z+1/2; (vii) −x+3/2, y, z+1/2.