Seven new metal–organic frameworks assembled from semi-rigid poly­car­box­yl­ate and auxiliary N-donor ligands: syntheses, structures and properties

Zhang, X.; Yang, Q.; Yun, M.; Si, C.; An, N.; Jia, M.; Liu, J.; Dong, X.

doi:10.1107/S2052520620012834

Seven new metal–organic frameworks assembled from semi-rigid polycarboxylate and auxiliary N-donor ligands: syntheses, structures and properties

X. Zhang, Q. Yang, M. Yun, C. Si, N. An, M. Jia, J. Liu and X. Dong

Seven new metal–organic frameworks (MOFs), namely, [Zn₂(L¹)(H₂O)₃]_n (1), [Zn₂(L¹)(dib)(H₂O)₂]_n (2), {[Zn₂(L¹)(4,4′-bipy)(H₂O)₂]·H₂O}_n (3), [Cd₂(L¹)(1,10-phen)]_n (4), [Ni₂(HL¹)(4,4′-bipy)(μ₃-OH)(μ₂-H₂O)]_n (5), {[Co₄(L¹)(4,4′-bibp)₃]·(4,4′-bibp)₃}_n (6), and [Co₂(L²)(4,4′-bibp)₂(H₂O)]_n (7), where H₄L¹ and H₄L² are semi-rigid 3-(3,5-dicarboxylphenoxy)phthalic acid and 4-(3,5-dicarboxylphenoxy)phthalic acid, respectively, and 4,4′-bipy is 4,4′-bipyridine, dib is 1,4-bis(1H-imidazol-1-yl)benzene, 1,10-phen is 1,10-phenanthroline and 4,4′-bipb is 1,4-bis(pyridin-4-yl)benzene, have been prepared under solvothermal conditions with Zn^II, Cd^II, Co^II and Ni^II ions in the presence of auxiliary N-donor ligands. The crystal structures and photoluminescence and magnetic properties of these compounds have been investigated. Compound 1 displays a 3,4,6-connected two-dimensional (2D) topology with a Schläfli symbol of (4².5)₂(4³.5².7)(4⁵.5⁶.6³)₂, and the 2D structure was further assembled to form a three-dimensional (3D) framework by intermolecular O—H

O hydrogen bonds. Compound 2 features a novel 3,3,4-connected structure and the point symbol is (4.10²)(4.6.8⁴)(6².8). Compound 3 exhibits a 3,4,6-connected 3-nodal net having a 3,4,6 T53 type topology, with the point symbol (4.6²)₂(4².6⁴)₂(4².6⁸.8².10³). Compound 4 shows a 2D→3D supramolecular structure formed by π–π stacking interactions. Compound 5 possesses a 3D framework with a tfz-d net topology. Compounds 6 and 7 are constructed from the same auxiliary ligand and metal salt at the same temperature, but with different main ligands and exhibiting different topologies. Compound 6 presents a 3D 4,6-connected topological network with a Schläfli symbol of (3.4⁴.6)(3².4⁴.5⁶.6³), while compound 7 has a 3D topological network with a Schläfli symbol of (4¹².6¹⁶). Magnetic analyses indicate that compounds 5 and 7 show weak antiferromagnetic interactions.

Keywords: MOF; topological analysis; crystal structure; semi-rigid polycarboxylate; auxiliary N-donor ligand; photoluminescence; magnetic properties.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520620012834/rm5037sup1.cif Contains datablocks global, 1, 2, 3, 4, 5, 6, 7
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50371sup2.hkl Contains datablock 1
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50372sup3.hkl Contains datablock 2
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50373sup4.hkl Contains datablock 3
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50374sup5.hkl Contains datablock 4
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50375sup6.hkl Contains datablock 5
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50376sup7.hkl Contains datablock 6
	Structure factor file (CIF format) https://doi.org/10.1107/S2052520620012834/rm50377sup8.hkl Contains datablock 7
	Portable Document Format (PDF) file https://doi.org/10.1107/S2052520620012834/rm5037sup9.pdf Tables with bond lengths and angles, the additional figures, the PXRD patterns, the FT-IR spectrum and TG curves

CCDC references: 1060395; 1973949; 1060388; 1973950; 1060398; 1060393; 1060391

Computing details top

Data collection: APEX2 (Bruker, 2015) for (1), (2), (4), (5); SMART (Bruker, 2008) for (3), (6), (7). Cell refinement: SAINT (Bruker, 2015) for (1), (2), (4), (5); SMART (Bruker, 2008) for (3), (6), (7). Data reduction: SAINT (Bruker, 2015) for (1), (2), (4), (5); SAINT (Bruker, 2008) for (3), (6), (7). Program(s) used to solve structure: SHELXS97 (Sheldrick, 2008) for (1), (2), (3), (4), (5), (7); SHELXT2018 (Sheldrick, 2015a) for (6). Program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) for (1), (2), (3), (4), (5), (7); SHELXL2018 (Sheldrick, 2015b) for (6). For all structures, molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Poly[triaqua[µ₆-3-(3,5-dicarboxylatophenoxy)phthalato]dizinc(II)] (1) top

Crystal data top

[Zn₂(C₁₆H₆O₉)(H₂O)₃]	F(000) = 2112
M_r = 527.00	D_x = 2.062 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.1681 (13) Å	Cell parameters from 4946 reflections
b = 16.2610 (13) Å	θ = 2.5–28.3°
c = 13.7893 (11) Å	µ = 2.90 mm⁻¹
β = 110.508 (1)°	T = 296 K
V = 3395.6 (5) Å³	Block, colorless
Z = 8	0.18 × 0.16 × 0.13 mm

Data collection top

Bruker APEXII CCD diffractometer	3008 independent reflections
Radiation source: fine-focus sealed tube	2723 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.021
φ and ω scans	θ_max = 25.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −19→19
T_min = 0.624, T_max = 0.704	k = −19→13
9404 measured reflections	l = −16→16

Refinement top

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.055	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.0296P)² + 2.6506P] where P = (F_o² + 2F_c²)/3
3008 reflections	(Δ/σ)_max = 0.001
272 parameters	Δρ_max = 0.30 e Å⁻³
0 restraints	Δρ_min = −0.35 e Å⁻³

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.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
O10	0.58441 (10)	0.29657 (11)	1.22096 (12)	0.0320 (4)
H10C	0.5774	0.3267	1.1621	0.038*
H10B	0.6030	0.3303	1.2678	0.048*
O1	0.26046 (10)	0.14504 (11)	1.01380 (12)	0.0281 (4)
Zn1	0.340549 (15)	0.327207 (15)	0.946954 (18)	0.01911 (8)
Zn2	0.5000	0.39842 (2)	0.7500	0.01795 (10)
Zn3	0.5000	0.22358 (2)	1.2500	0.02123 (10)
O8	0.39547 (10)	0.40647 (9)	0.60493 (12)	0.0252 (4)
O2	0.17212 (10)	0.09084 (9)	0.86662 (12)	0.0265 (4)
O4	0.41758 (10)	0.25077 (9)	1.04738 (12)	0.0239 (3)
O3	0.45759 (10)	0.13993 (9)	1.14143 (11)	0.0251 (4)
O7	0.29851 (10)	0.28180 (10)	0.80900 (12)	0.0265 (4)
O12	0.43473 (10)	0.49406 (10)	0.79590 (12)	0.0286 (4)
H12C	0.3916	0.5225	0.7424	0.034*
H12B	0.4173	0.4776	0.8416	0.043*
O6	0.42932 (9)	0.31166 (9)	0.80087 (11)	0.0208 (3)
O5	0.56518 (9)	0.12674 (10)	1.00049 (11)	0.0217 (3)
C7	0.62661 (13)	0.14745 (13)	0.95416 (16)	0.0172 (4)
O11	0.41916 (9)	0.42618 (9)	0.97909 (12)	0.0215 (3)
H11B	0.4168	0.4501	1.0345	0.026*
H11A	0.4709	0.4115	0.9983	0.032*
C1	0.32748 (14)	0.08868 (12)	0.90232 (16)	0.0164 (4)
C14	0.42687 (13)	0.17406 (13)	1.05497 (16)	0.0168 (4)
C2	0.31970 (14)	0.03552 (13)	0.82073 (17)	0.0216 (5)
H2	0.2643	0.0162	0.7798	0.026*
C10	0.75347 (13)	0.19540 (13)	0.87426 (16)	0.0179 (4)
H10A	0.7958	0.2103	0.8461	0.021*
C6	0.41058 (13)	0.11988 (12)	0.96204 (15)	0.0155 (4)
C11	0.66681 (13)	0.22199 (12)	0.82763 (16)	0.0160 (4)
C9	0.77723 (13)	0.14671 (13)	0.96251 (16)	0.0165 (4)
C5	0.48343 (13)	0.09695 (12)	0.93711 (16)	0.0168 (4)
C12	0.60267 (13)	0.19792 (13)	0.86789 (16)	0.0173 (4)
H12A	0.5446	0.2155	0.8372	0.021*
C15	0.35615 (13)	0.27609 (12)	0.76570 (16)	0.0167 (4)
O9	0.42392 (10)	0.36921 (10)	0.46452 (12)	0.0269 (4)
C16	0.37288 (13)	0.37798 (13)	0.51531 (16)	0.0173 (4)
C13	0.24719 (13)	0.10929 (12)	0.92786 (16)	0.0178 (4)
C8	0.71339 (13)	0.12228 (13)	1.00297 (16)	0.0183 (4)
H8	0.7287	0.0895	1.0619	0.022*
C4	0.47572 (15)	0.04183 (13)	0.85856 (17)	0.0221 (5)
H4	0.5256	0.0253	0.8449	0.027*
C3	0.39358 (15)	0.01123 (14)	0.80008 (18)	0.0244 (5)
H3	0.3881	−0.0258	0.7468	0.029*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O10	0.0293 (9)	0.0452 (10)	0.0212 (9)	−0.0114 (8)	0.0085 (7)	0.0009 (8)
O1	0.0157 (8)	0.0452 (10)	0.0246 (9)	−0.0039 (7)	0.0085 (7)	−0.0166 (8)
Zn1	0.01589 (14)	0.02411 (15)	0.01788 (14)	0.00064 (10)	0.00660 (11)	−0.00386 (10)
Zn2	0.01587 (18)	0.02016 (19)	0.01698 (19)	0.000	0.00470 (14)	0.000
Zn3	0.0241 (2)	0.0217 (2)	0.01691 (19)	0.000	0.00597 (15)	0.000
O8	0.0166 (8)	0.0355 (9)	0.0197 (9)	−0.0007 (6)	0.0019 (7)	−0.0105 (7)
O2	0.0141 (8)	0.0378 (9)	0.0257 (9)	−0.0025 (7)	0.0046 (7)	−0.0094 (7)
O4	0.0282 (9)	0.0175 (8)	0.0216 (8)	0.0001 (6)	0.0032 (7)	−0.0022 (6)
O3	0.0342 (9)	0.0242 (8)	0.0145 (8)	0.0015 (7)	0.0056 (7)	−0.0006 (6)
O7	0.0201 (8)	0.0404 (10)	0.0215 (8)	−0.0039 (7)	0.0105 (7)	−0.0121 (7)
O12	0.0359 (9)	0.0299 (9)	0.0208 (8)	0.0127 (7)	0.0112 (7)	0.0062 (7)
O6	0.0164 (8)	0.0261 (8)	0.0185 (8)	−0.0049 (6)	0.0045 (6)	−0.0052 (6)
O5	0.0134 (7)	0.0380 (9)	0.0151 (8)	−0.0028 (6)	0.0068 (6)	0.0032 (7)
C7	0.0138 (10)	0.0226 (11)	0.0168 (11)	−0.0020 (8)	0.0075 (9)	−0.0003 (9)
O11	0.0176 (8)	0.0226 (8)	0.0237 (8)	0.0005 (6)	0.0067 (6)	−0.0025 (6)
C1	0.0169 (11)	0.0179 (11)	0.0160 (11)	0.0000 (8)	0.0077 (9)	−0.0019 (8)
C14	0.0108 (10)	0.0231 (12)	0.0166 (11)	−0.0006 (8)	0.0050 (8)	−0.0007 (9)
C2	0.0202 (11)	0.0251 (12)	0.0203 (11)	−0.0058 (9)	0.0083 (9)	−0.0043 (9)
C10	0.0145 (10)	0.0230 (11)	0.0179 (11)	0.0000 (8)	0.0079 (9)	0.0002 (9)
C6	0.0184 (11)	0.0156 (10)	0.0137 (10)	0.0010 (8)	0.0071 (9)	0.0015 (8)
C11	0.0153 (10)	0.0194 (11)	0.0131 (10)	0.0005 (8)	0.0049 (8)	−0.0002 (8)
C9	0.0134 (10)	0.0192 (11)	0.0151 (11)	0.0010 (8)	0.0028 (9)	−0.0006 (8)
C5	0.0139 (10)	0.0214 (11)	0.0160 (11)	−0.0012 (8)	0.0062 (9)	0.0058 (8)
C12	0.0122 (10)	0.0224 (11)	0.0163 (11)	0.0018 (8)	0.0036 (8)	0.0008 (9)
C15	0.0140 (10)	0.0191 (11)	0.0157 (11)	0.0033 (8)	0.0034 (8)	0.0016 (8)
O9	0.0146 (8)	0.0425 (10)	0.0243 (9)	−0.0061 (7)	0.0076 (7)	−0.0099 (7)
C16	0.0133 (10)	0.0187 (11)	0.0178 (11)	0.0011 (8)	0.0029 (9)	−0.0004 (9)
C13	0.0162 (11)	0.0168 (11)	0.0200 (11)	0.0000 (8)	0.0058 (9)	−0.0008 (9)
C8	0.0182 (11)	0.0217 (11)	0.0144 (11)	0.0018 (8)	0.0050 (9)	0.0044 (9)
C4	0.0241 (12)	0.0245 (12)	0.0245 (12)	0.0040 (9)	0.0170 (10)	0.0009 (9)
C3	0.0324 (13)	0.0229 (12)	0.0235 (12)	−0.0035 (10)	0.0168 (11)	−0.0069 (9)

Geometric parameters (Å, º) top

O10—Zn3	1.9530 (16)	C7—C12	1.384 (3)
O10—H10C	0.9210	C7—C8	1.388 (3)
O10—H10B	0.8200	O11—H11B	0.8705
O1—C13	1.269 (3)	O11—H11A	0.8200
O1—Zn1ⁱ	1.9450 (15)	C1—C2	1.389 (3)
Zn1—O7	1.9288 (15)	C1—C6	1.402 (3)
Zn1—O1ⁱ	1.9451 (15)	C1—C13	1.497 (3)
Zn1—O4	1.9507 (15)	C14—C6	1.500 (3)
Zn1—O11	2.0019 (15)	C2—C3	1.379 (3)
Zn2—O6ⁱⁱ	2.0857 (15)	C2—H2	0.9300
Zn2—O6	2.0857 (15)	C10—C9	1.388 (3)
Zn2—O12ⁱⁱ	2.0978 (15)	C10—C11	1.390 (3)
Zn2—O12	2.0978 (15)	C10—H10A	0.9300
Zn2—O8	2.1227 (15)	C6—C5	1.389 (3)
Zn2—O8ⁱⁱ	2.1227 (15)	C11—C12	1.393 (3)
Zn3—O10ⁱⁱⁱ	1.9530 (16)	C11—C15ⁱⁱ	1.494 (3)
Zn3—O3	1.9602 (15)	C9—C8	1.392 (3)
Zn3—O3ⁱⁱⁱ	1.9603 (15)	C9—C16^iv	1.515 (3)
O8—C16	1.249 (3)	C5—C4	1.377 (3)
O2—C13	1.248 (3)	C12—H12A	0.9300
O4—C14	1.256 (2)	C15—C11ⁱⁱ	1.494 (3)
O3—C14	1.249 (3)	O9—C16	1.264 (2)
O7—C15	1.274 (2)	C16—C9^v	1.515 (3)
O12—H12C	0.9398	C8—H8	0.9300
O12—H12B	0.8200	C4—C3	1.383 (3)
O6—C15	1.252 (2)	C4—H4	0.9300
O5—C5	1.391 (2)	C3—H3	0.9300
O5—C7	1.397 (2)

Zn3—O10—H10C	128.7	C2—C1—C6	119.80 (19)
Zn3—O10—H10B	109.5	C2—C1—C13	119.33 (19)
H10C—O10—H10B	103.7	C6—C1—C13	120.82 (18)
C13—O1—Zn1ⁱ	118.84 (13)	O3—C14—O4	121.09 (19)
O7—Zn1—O1ⁱ	108.86 (6)	O3—C14—C6	116.51 (18)
O7—Zn1—O4	111.90 (7)	O4—C14—C6	122.13 (18)
O1ⁱ—Zn1—O4	109.86 (7)	C3—C2—C1	120.4 (2)
O7—Zn1—O11	120.21 (6)	C3—C2—H2	119.8
O1ⁱ—Zn1—O11	106.36 (6)	C1—C2—H2	119.8
O4—Zn1—O11	99.04 (6)	C9—C10—C11	120.48 (19)
O6ⁱⁱ—Zn2—O6	94.87 (8)	C9—C10—H10A	119.8
O6ⁱⁱ—Zn2—O12ⁱⁱ	90.41 (6)	C11—C10—H10A	119.8
O6—Zn2—O12ⁱⁱ	174.71 (6)	C5—C6—C1	118.61 (19)
O6ⁱⁱ—Zn2—O12	174.71 (6)	C5—C6—C14	117.31 (18)
O6—Zn2—O12	90.41 (6)	C1—C6—C14	124.02 (18)
O12ⁱⁱ—Zn2—O12	84.31 (9)	C10—C11—C12	119.92 (19)
O6ⁱⁱ—Zn2—O8	94.24 (6)	C10—C11—C15ⁱⁱ	119.17 (18)
O6—Zn2—O8	90.54 (6)	C12—C11—C15ⁱⁱ	120.91 (18)
O12ⁱⁱ—Zn2—O8	89.35 (6)	C10—C9—C8	119.85 (18)
O12—Zn2—O8	85.41 (6)	C10—C9—C16^iv	119.66 (18)
O6ⁱⁱ—Zn2—O8ⁱⁱ	90.54 (6)	C8—C9—C16^iv	120.48 (18)
O6—Zn2—O8ⁱⁱ	94.24 (6)	C4—C5—C6	121.23 (19)
O12ⁱⁱ—Zn2—O8ⁱⁱ	85.41 (6)	C4—C5—O5	121.66 (18)
O12—Zn2—O8ⁱⁱ	89.34 (6)	C6—C5—O5	116.89 (18)
O8—Zn2—O8ⁱⁱ	172.93 (8)	C7—C12—C11	119.08 (19)
O10ⁱⁱⁱ—Zn3—O10	105.16 (11)	C7—C12—H12A	120.5
O10ⁱⁱⁱ—Zn3—O3	119.71 (7)	C11—C12—H12A	120.5
O10—Zn3—O3	110.35 (7)	O6—C15—O7	122.13 (19)
O10ⁱⁱⁱ—Zn3—O3ⁱⁱⁱ	110.35 (7)	O6—C15—C11ⁱⁱ	121.44 (18)
O10—Zn3—O3ⁱⁱⁱ	119.71 (7)	O7—C15—C11ⁱⁱ	116.40 (18)
O3—Zn3—O3ⁱⁱⁱ	92.11 (9)	O8—C16—O9	124.68 (19)
C16—O8—Zn2	140.37 (14)	O8—C16—C9^v	118.00 (18)
C14—O4—Zn1	136.03 (14)	O9—C16—C9^v	117.31 (18)
C14—O3—Zn3	109.65 (13)	O2—C13—O1	123.24 (19)
C15—O7—Zn1	115.29 (13)	O2—C13—C1	120.31 (19)
Zn2—O12—H12C	116.2	O1—C13—C1	116.44 (18)
Zn2—O12—H12B	109.5	C7—C8—C9	119.13 (19)
H12C—O12—H12B	113.8	C7—C8—H8	120.4
C15—O6—Zn2	137.48 (14)	C9—C8—H8	120.4
C5—O5—C7	117.88 (15)	C5—C4—C3	119.78 (19)
C12—C7—C8	121.48 (18)	C5—C4—H4	120.1
C12—C7—O5	120.42 (18)	C3—C4—H4	120.1
C8—C7—O5	117.83 (18)	C2—C3—C4	120.1 (2)
Zn1—O11—H11B	109.6	C2—C3—H3	120.0
Zn1—O11—H11A	109.5	C4—C3—H3	120.0
H11B—O11—H11A	101.5

O6ⁱⁱ—Zn2—O8—C16	−1.4 (2)	C9—C10—C11—C12	−1.7 (3)
O6—Zn2—O8—C16	−96.3 (2)	C9—C10—C11—C15ⁱⁱ	178.46 (19)
O12ⁱⁱ—Zn2—O8—C16	89.0 (2)	C11—C10—C9—C8	1.9 (3)
O12—Zn2—O8—C16	173.3 (2)	C11—C10—C9—C16^iv	−176.87 (19)
O8ⁱⁱ—Zn2—O8—C16	131.1 (2)	C1—C6—C5—C4	−2.9 (3)
O7—Zn1—O4—C14	−26.6 (2)	C14—C6—C5—C4	174.45 (19)
O1ⁱ—Zn1—O4—C14	94.4 (2)	C1—C6—C5—O5	−177.70 (18)
O11—Zn1—O4—C14	−154.4 (2)	C14—C6—C5—O5	−0.3 (3)
O10ⁱⁱⁱ—Zn3—O3—C14	67.46 (15)	C7—O5—C5—C4	41.3 (3)
O10—Zn3—O3—C14	−54.74 (15)	C7—O5—C5—C6	−143.95 (19)
O3ⁱⁱⁱ—Zn3—O3—C14	−177.60 (17)	C8—C7—C12—C11	1.8 (3)
O1ⁱ—Zn1—O7—C15	166.65 (15)	O5—C7—C12—C11	175.70 (18)
O4—Zn1—O7—C15	−71.74 (16)	C10—C11—C12—C7	−0.1 (3)
O11—Zn1—O7—C15	43.74 (17)	C15ⁱⁱ—C11—C12—C7	179.70 (19)
O6ⁱⁱ—Zn2—O6—C15	−94.2 (2)	Zn2—O6—C15—O7	−120.8 (2)
O12ⁱⁱ—Zn2—O6—C15	88.9 (7)	Zn2—O6—C15—C11ⁱⁱ	61.4 (3)
O12—Zn2—O6—C15	85.5 (2)	Zn1—O7—C15—O6	−13.4 (3)
O8—Zn2—O6—C15	0.1 (2)	Zn1—O7—C15—C11ⁱⁱ	164.44 (14)
O8ⁱⁱ—Zn2—O6—C15	174.9 (2)	Zn2—O8—C16—O9	−43.3 (4)
C5—O5—C7—C12	50.2 (3)	Zn2—O8—C16—C9^v	137.73 (18)
C5—O5—C7—C8	−135.7 (2)	Zn1ⁱ—O1—C13—O2	0.0 (3)
Zn3—O3—C14—O4	−7.6 (2)	Zn1ⁱ—O1—C13—C1	−179.39 (14)
Zn3—O3—C14—C6	166.49 (14)	C2—C1—C13—O2	−12.3 (3)
Zn1—O4—C14—O3	−153.10 (16)	C6—C1—C13—O2	170.13 (19)
Zn1—O4—C14—C6	33.1 (3)	C2—C1—C13—O1	167.1 (2)
C6—C1—C2—C3	2.0 (3)	C6—C1—C13—O1	−10.4 (3)
C13—C1—C2—C3	−175.6 (2)	C12—C7—C8—C9	−1.7 (3)
C2—C1—C6—C5	0.5 (3)	O5—C7—C8—C9	−175.70 (18)
C13—C1—C6—C5	178.06 (18)	C10—C9—C8—C7	−0.2 (3)
C2—C1—C6—C14	−176.71 (19)	C16^iv—C9—C8—C7	178.54 (19)
C13—C1—C6—C14	0.9 (3)	C6—C5—C4—C3	2.9 (3)
O3—C14—C6—C5	−77.2 (2)	O5—C5—C4—C3	177.39 (19)
O4—C14—C6—C5	96.8 (2)	C1—C2—C3—C4	−2.1 (3)
O3—C14—C6—C1	100.0 (2)	C5—C4—C3—C2	−0.3 (3)
O4—C14—C6—C1	−86.0 (3)

Symmetry codes: (i) −x+1/2, −y+1/2, −z+2; (ii) −x+1, y, −z+3/2; (iii) −x+1, y, −z+5/2; (iv) x+1/2, −y+1/2, z+1/2; (v) x−1/2, −y+1/2, z−1/2.

Poly[diaqua[1,4-bis(1<it>H</it>-imidazol-1-yl)benzene][µ₄-3-(3,5-dicarboxylatophenoxy)phthalato]dizinc(II)] (2) top

Crystal data top

[Zn₂(C₁₆H₆O₉)(C₁₂H₁₄N₄O₂)(H₂O)₂]	Z = 2
M_r = 719.22	F(000) = 728
Triclinic, P1	D_x = 1.634 Mg m⁻³
a = 10.070 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.144 (3) Å	Cell parameters from 1707 reflections
c = 14.172 (4) Å	θ = 2.3–22.2°
α = 104.630 (5)°	µ = 1.71 mm⁻¹
β = 105.637 (5)°	T = 296 K
γ = 109.156 (5)°	Block, colorless
V = 1461.5 (7) Å³	0.27 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	5073 independent reflections
Radiation source: fine-focus sealed tube	3401 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
φ and ω scans	θ_max = 25.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −11→11
T_min = 0.655, T_max = 0.705	k = −14→14
10904 measured reflections	l = −16→16

Refinement top

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)] = 0.057	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.159	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ²(F_o²) + (0.0831P)²] where P = (F_o² + 2F_c²)/3
5073 reflections	(Δ/σ)_max < 0.001
406 parameters	Δρ_max = 0.61 e Å⁻³
1 restraint	Δρ_min = −0.72 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.4915 (6)	0.3987 (5)	0.1389 (4)	0.0263 (12)
C2	0.4181 (6)	0.4271 (4)	0.2163 (4)	0.0246 (12)
C3	0.3317 (6)	0.4964 (5)	0.2124 (4)	0.0287 (12)
C4	0.2764 (7)	0.5224 (6)	0.2905 (5)	0.0385 (14)
H4	0.2197	0.5693	0.2878	0.046*
C5	0.3033 (7)	0.4805 (6)	0.3723 (5)	0.0411 (15)
H5	0.2677	0.5014	0.4252	0.049*
C6	0.3828 (7)	0.4076 (5)	0.3757 (5)	0.0374 (14)
H6	0.4003	0.3777	0.4300	0.045*
C7	0.4366 (6)	0.3797 (5)	0.2958 (4)	0.0288 (12)
C8	0.4499 (6)	0.1837 (5)	0.2846 (4)	0.0274 (12)
C9	0.2994 (6)	0.1196 (5)	0.2666 (4)	0.0312 (13)
H9	0.2359	0.1607	0.2640	0.037*
C10	0.2423 (6)	−0.0065 (5)	0.2524 (5)	0.0321 (13)
C11	0.3354 (6)	−0.0688 (5)	0.2545 (5)	0.0349 (14)
H11	0.2963	−0.1536	0.2444	0.042*
C12	0.4855 (6)	−0.0055 (5)	0.2714 (5)	0.0347 (13)
C13	0.5427 (7)	0.1205 (6)	0.2871 (5)	0.0377 (14)
H13	0.6448	0.1637	0.2995	0.045*
C14	0.5842 (7)	−0.0747 (6)	0.2732 (5)	0.0408 (15)
C15	0.7092 (6)	0.4617 (5)	−0.1215 (5)	0.0302 (13)
C16	1.0811 (7)	−0.0774 (5)	0.2381 (5)	0.0370 (14)
C17	0.6929 (8)	0.2076 (6)	0.1082 (6)	0.057 (2)
H17	0.6275	0.2170	0.1418	0.068*
C18	0.7461 (8)	0.1191 (6)	0.1032 (6)	0.055 (2)
H18	0.7237	0.0562	0.1304	0.065*
C19	0.8377 (6)	0.2389 (5)	0.0241 (5)	0.0336 (14)
H19	0.8926	0.2730	−0.0127	0.040*
C20	1.0664 (7)	0.1284 (5)	0.0269 (5)	0.0349 (14)
H20	1.1110	0.2151	0.0452	0.042*
C21	0.9230 (6)	0.0691 (5)	0.0240 (4)	0.0291 (12)
C22	0.8565 (6)	−0.0574 (5)	−0.0020 (4)	0.0340 (14)
H22	0.7593	−0.0959	−0.0030	0.041*
C23	0.8674 (8)	−0.1469 (6)	0.4833 (5)	0.0461 (17)
H23	0.8478	−0.0788	0.5114	0.055*
C24	0.9040 (8)	−0.2181 (6)	0.5344 (5)	0.0473 (17)
H24	0.9149	−0.2082	0.6037	0.057*
C25	0.8972 (7)	−0.2863 (5)	0.3751 (5)	0.0380 (15)
H25	0.9030	−0.3334	0.3147	0.046*
C26	0.9618 (6)	−0.4063 (5)	0.4817 (4)	0.0296 (13)
C27	1.0523 (7)	−0.3881 (6)	0.5818 (5)	0.0391 (15)
H27	1.0864	−0.3125	0.6375	0.047*
C28	1.0927 (7)	−0.4810 (6)	0.6000 (5)	0.0412 (15)
H28	1.1563	−0.4675	0.6671	0.049*
N1	0.7477 (5)	0.2812 (4)	0.0574 (4)	0.0341 (11)
N2	0.8408 (5)	0.1415 (4)	0.0495 (4)	0.0327 (11)
N3	0.8634 (5)	−0.1898 (4)	0.3836 (4)	0.0350 (12)
N4	0.9225 (5)	−0.3084 (4)	0.4656 (4)	0.0341 (11)
O1	0.6303 (4)	0.4719 (3)	0.1672 (3)	0.0322 (9)
O2	0.4170 (4)	0.3043 (3)	0.0567 (3)	0.0386 (10)
O3	0.5201 (4)	0.3080 (3)	0.2968 (3)	0.0354 (10)
O4	0.5403 (5)	−0.1796 (4)	0.2769 (5)	0.0642 (15)
O5	0.7171 (5)	−0.0153 (4)	0.2749 (4)	0.0481 (12)
O6	0.6273 (4)	0.4584 (3)	−0.0673 (3)	0.0329 (9)
O7	0.8201 (4)	0.4367 (4)	−0.1011 (3)	0.0413 (10)
O8	0.9352 (4)	0.5673 (3)	0.1452 (3)	0.0407 (10)
H8A	0.9380	0.6398	0.1527	0.061*
H8C	0.9916	0.5542	0.1128	0.061*
O9	1.0066 (4)	−0.0153 (3)	0.2600 (3)	0.0357 (10)
O10	1.0283 (5)	−0.1915 (4)	0.2100 (5)	0.085 (2)
O11	0.6914 (4)	−0.2870 (4)	0.1399 (3)	0.0441 (11)
H11A	0.6657	−0.2699	0.0851	0.066*
H11C	0.6120	−0.3291	0.1478	0.066*
Zn1	0.72012 (7)	0.43640 (5)	0.06174 (5)	0.0278 (2)
Zn2	0.81860 (7)	−0.12623 (6)	0.26728 (5)	0.0309 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.032 (3)	0.027 (3)	0.033 (3)	0.020 (3)	0.018 (3)	0.016 (3)
C2	0.021 (3)	0.020 (2)	0.036 (3)	0.009 (2)	0.015 (2)	0.009 (2)
C3	0.025 (3)	0.031 (3)	0.036 (3)	0.014 (2)	0.015 (3)	0.015 (3)
C4	0.041 (4)	0.053 (4)	0.041 (4)	0.033 (3)	0.025 (3)	0.021 (3)
C5	0.050 (4)	0.052 (4)	0.031 (3)	0.023 (3)	0.025 (3)	0.017 (3)
C6	0.047 (4)	0.040 (3)	0.031 (3)	0.017 (3)	0.017 (3)	0.021 (3)
C7	0.027 (3)	0.032 (3)	0.035 (3)	0.015 (2)	0.014 (3)	0.020 (3)
C8	0.024 (3)	0.032 (3)	0.031 (3)	0.015 (2)	0.010 (2)	0.018 (2)
C9	0.031 (3)	0.036 (3)	0.035 (3)	0.020 (3)	0.012 (3)	0.018 (3)
C10	0.029 (3)	0.033 (3)	0.039 (3)	0.015 (2)	0.014 (3)	0.016 (3)
C11	0.030 (3)	0.033 (3)	0.054 (4)	0.017 (3)	0.023 (3)	0.023 (3)
C12	0.033 (3)	0.043 (3)	0.045 (4)	0.024 (3)	0.020 (3)	0.027 (3)
C13	0.030 (3)	0.051 (4)	0.048 (4)	0.020 (3)	0.022 (3)	0.030 (3)
C14	0.033 (3)	0.044 (3)	0.062 (4)	0.025 (3)	0.021 (3)	0.030 (3)
C15	0.026 (3)	0.029 (3)	0.038 (3)	0.010 (2)	0.018 (3)	0.013 (3)
C16	0.035 (3)	0.035 (3)	0.049 (4)	0.018 (3)	0.022 (3)	0.018 (3)
C17	0.078 (5)	0.062 (4)	0.096 (6)	0.055 (4)	0.070 (5)	0.059 (4)
C18	0.072 (5)	0.057 (4)	0.095 (6)	0.052 (4)	0.063 (5)	0.057 (4)
C19	0.039 (3)	0.032 (3)	0.051 (4)	0.024 (3)	0.028 (3)	0.025 (3)
C20	0.041 (3)	0.027 (3)	0.045 (4)	0.021 (3)	0.018 (3)	0.016 (3)
C21	0.032 (3)	0.029 (3)	0.034 (3)	0.019 (2)	0.014 (3)	0.014 (2)
C22	0.034 (3)	0.030 (3)	0.045 (4)	0.017 (3)	0.018 (3)	0.019 (3)
C23	0.067 (5)	0.042 (3)	0.046 (4)	0.037 (3)	0.025 (4)	0.020 (3)
C24	0.071 (5)	0.052 (4)	0.036 (4)	0.037 (4)	0.028 (3)	0.020 (3)
C25	0.046 (4)	0.036 (3)	0.034 (3)	0.022 (3)	0.013 (3)	0.011 (3)
C26	0.035 (3)	0.025 (3)	0.036 (3)	0.016 (2)	0.014 (3)	0.018 (3)
C27	0.047 (4)	0.039 (3)	0.030 (3)	0.021 (3)	0.008 (3)	0.014 (3)
C28	0.043 (4)	0.050 (4)	0.035 (4)	0.023 (3)	0.009 (3)	0.025 (3)
N1	0.040 (3)	0.032 (2)	0.047 (3)	0.020 (2)	0.027 (3)	0.022 (2)
N2	0.038 (3)	0.030 (2)	0.048 (3)	0.025 (2)	0.026 (2)	0.021 (2)
N3	0.039 (3)	0.035 (3)	0.044 (3)	0.024 (2)	0.019 (2)	0.021 (2)
N4	0.040 (3)	0.035 (3)	0.034 (3)	0.019 (2)	0.012 (2)	0.021 (2)
O1	0.022 (2)	0.035 (2)	0.047 (2)	0.0144 (17)	0.0169 (18)	0.0198 (19)
O2	0.040 (2)	0.029 (2)	0.043 (3)	0.0125 (19)	0.019 (2)	0.009 (2)
O3	0.030 (2)	0.036 (2)	0.055 (3)	0.0181 (18)	0.020 (2)	0.031 (2)
O4	0.054 (3)	0.053 (3)	0.127 (5)	0.039 (2)	0.055 (3)	0.055 (3)
O5	0.034 (2)	0.055 (3)	0.085 (4)	0.033 (2)	0.036 (2)	0.041 (3)
O6	0.030 (2)	0.045 (2)	0.041 (2)	0.0242 (18)	0.0204 (19)	0.026 (2)
O7	0.033 (2)	0.065 (3)	0.057 (3)	0.037 (2)	0.028 (2)	0.039 (2)
O8	0.032 (2)	0.029 (2)	0.064 (3)	0.0140 (17)	0.025 (2)	0.012 (2)
O9	0.022 (2)	0.037 (2)	0.051 (3)	0.0144 (17)	0.0156 (19)	0.0168 (19)
O10	0.043 (3)	0.029 (2)	0.177 (7)	0.017 (2)	0.047 (4)	0.026 (3)
O11	0.036 (2)	0.047 (2)	0.047 (3)	0.011 (2)	0.016 (2)	0.023 (2)
Zn1	0.0270 (4)	0.0284 (3)	0.0394 (4)	0.0175 (3)	0.0167 (3)	0.0184 (3)
Zn2	0.0268 (4)	0.0327 (4)	0.0430 (4)	0.0179 (3)	0.0144 (3)	0.0215 (3)

Geometric parameters (Å, º) top

C1—O2	1.235 (6)	C18—H18	0.9300
C1—O1	1.268 (6)	C19—N1	1.312 (7)
C1—C2	1.510 (8)	C19—N2	1.328 (6)
C2—C7	1.387 (7)	C19—H19	0.9300
C2—C3	1.395 (7)	C20—C21	1.370 (8)
C3—C4	1.381 (8)	C20—C22^iv	1.380 (7)
C3—C15ⁱ	1.506 (8)	C20—H20	0.9300
C4—C5	1.377 (8)	C21—C22	1.360 (7)
C4—H4	0.9300	C21—N2	1.438 (6)
C5—C6	1.375 (8)	C22—C20^iv	1.380 (7)
C5—H5	0.9300	C22—H22	0.9300
C6—C7	1.395 (8)	C23—C24	1.338 (8)
C6—H6	0.9300	C23—N3	1.361 (8)
C7—O3	1.395 (6)	C23—H23	0.9300
C8—C9	1.374 (7)	C24—N4	1.370 (8)
C8—O3	1.381 (6)	C24—H24	0.9300
C8—C13	1.389 (7)	C25—N3	1.309 (7)
C9—C10	1.386 (7)	C25—N4	1.351 (7)
C9—H9	0.9300	C25—H25	0.9300
C10—C11	1.383 (7)	C26—C28^v	1.371 (8)
C10—C16ⁱⁱ	1.494 (8)	C26—C27	1.381 (8)
C11—C12	1.372 (8)	C26—N4	1.420 (6)
C11—H11	0.9300	C27—C28	1.377 (8)
C12—C13	1.379 (8)	C27—H27	0.9300
C12—C14	1.497 (7)	C28—C26^v	1.371 (8)
C13—H13	0.9300	C28—H28	0.9300
C14—O4	1.223 (7)	N1—Zn1	1.982 (4)
C14—O5	1.285 (7)	N3—Zn2	1.997 (5)
C15—O7	1.231 (6)	O1—Zn1	1.974 (4)
C15—O6	1.268 (7)	O5—Zn2	1.939 (4)
C15—C3ⁱ	1.506 (8)	O6—Zn1	1.944 (4)
C16—O10	1.219 (7)	O8—Zn1	2.006 (4)
C16—O9	1.268 (6)	O8—H8A	0.8500
C16—C10ⁱⁱⁱ	1.494 (8)	O8—H8C	0.8500
C17—C18	1.345 (8)	O9—Zn2	1.978 (4)
C17—N1	1.355 (8)	O11—Zn2	2.011 (4)
C17—H17	0.9300	O11—H11A	0.8500
C18—N2	1.374 (8)	O11—H11C	0.8500

O2—C1—O1	124.7 (5)	C22—C21—C20	121.4 (5)
O2—C1—C2	119.0 (5)	C22—C21—N2	119.0 (5)
O1—C1—C2	116.2 (5)	C20—C21—N2	119.6 (5)
C7—C2—C3	117.9 (5)	C21—C22—C20^iv	119.8 (5)
C7—C2—C1	117.6 (4)	C21—C22—H22	120.1
C3—C2—C1	124.5 (5)	C20^iv—C22—H22	120.1
C4—C3—C2	119.7 (5)	C24—C23—N3	109.3 (5)
C4—C3—C15ⁱ	119.0 (5)	C24—C23—H23	125.4
C2—C3—C15ⁱ	121.2 (5)	N3—C23—H23	125.4
C5—C4—C3	121.5 (5)	C23—C24—N4	107.3 (6)
C5—C4—H4	119.3	C23—C24—H24	126.4
C3—C4—H4	119.3	N4—C24—H24	126.4
C6—C5—C4	120.1 (6)	N3—C25—N4	111.1 (5)
C6—C5—H5	120.0	N3—C25—H25	124.4
C4—C5—H5	120.0	N4—C25—H25	124.4
C5—C6—C7	118.4 (5)	C28^v—C26—C27	120.0 (5)
C5—C6—H6	120.8	C28^v—C26—N4	120.9 (5)
C7—C6—H6	120.8	C27—C26—N4	119.1 (5)
C2—C7—O3	117.1 (5)	C28—C27—C26	120.6 (5)
C2—C7—C6	122.2 (5)	C28—C27—H27	119.7
O3—C7—C6	120.6 (5)	C26—C27—H27	119.7
C9—C8—O3	125.8 (5)	C26^v—C28—C27	119.4 (5)
C9—C8—C13	119.3 (5)	C26^v—C28—H28	120.3
O3—C8—C13	114.9 (5)	C27—C28—H28	120.3
C8—C9—C10	119.8 (5)	C19—N1—C17	105.3 (5)
C8—C9—H9	120.1	C19—N1—Zn1	130.0 (4)
C10—C9—H9	120.1	C17—N1—Zn1	123.8 (4)
C11—C10—C9	120.4 (5)	C19—N2—C18	107.1 (4)
C11—C10—C16ⁱⁱ	118.4 (5)	C19—N2—C21	127.5 (5)
C9—C10—C16ⁱⁱ	121.2 (5)	C18—N2—C21	125.4 (5)
C12—C11—C10	120.0 (5)	C25—N3—C23	106.4 (5)
C12—C11—H11	120.0	C25—N3—Zn2	123.6 (4)
C10—C11—H11	120.0	C23—N3—Zn2	130.0 (4)
C11—C12—C13	119.5 (5)	C25—N4—C24	106.0 (5)
C11—C12—C14	119.1 (5)	C25—N4—C26	124.7 (5)
C13—C12—C14	121.3 (5)	C24—N4—C26	129.3 (5)
C12—C13—C8	120.9 (5)	C1—O1—Zn1	115.1 (3)
C12—C13—H13	119.5	C8—O3—C7	119.2 (4)
C8—C13—H13	119.5	C14—O5—Zn2	108.8 (4)
O4—C14—O5	123.3 (5)	C15—O6—Zn1	110.6 (3)
O4—C14—C12	120.7 (5)	Zn1—O8—H8A	109.5
O5—C14—C12	116.0 (5)	Zn1—O8—H8C	109.5
O7—C15—O6	123.4 (5)	H8A—O8—H8C	109.5
O7—C15—C3ⁱ	120.1 (5)	C16—O9—Zn2	109.5 (3)
O6—C15—C3ⁱ	116.5 (5)	Zn2—O11—H11A	109.4
O10—C16—O9	122.6 (5)	Zn2—O11—H11C	109.3
O10—C16—C10ⁱⁱⁱ	119.1 (5)	H11A—O11—H11C	109.5
O9—C16—C10ⁱⁱⁱ	118.2 (5)	O6—Zn1—O1	113.55 (16)
C18—C17—N1	110.6 (6)	O6—Zn1—N1	121.23 (18)
C18—C17—H17	124.7	O1—Zn1—N1	107.28 (17)
N1—C17—H17	124.7	O6—Zn1—O8	111.78 (17)
C17—C18—N2	105.3 (5)	O1—Zn1—O8	99.47 (16)
C17—C18—H18	127.4	N1—Zn1—O8	100.68 (17)
N2—C18—H18	127.4	O5—Zn2—O9	99.01 (16)
N1—C19—N2	111.7 (5)	O5—Zn2—N3	119.1 (2)
N1—C19—H19	124.1	O9—Zn2—N3	112.11 (18)
N2—C19—H19	124.1	O5—Zn2—O11	110.99 (18)
C21—C20—C22^iv	118.9 (5)	O9—Zn2—O11	114.37 (17)
C21—C20—H20	120.6	N3—Zn2—O11	101.94 (18)
C22^iv—C20—H20	120.6

O2—C1—C2—C7	91.6 (6)	C20—C21—N2—C19	38.7 (8)
O1—C1—C2—C7	−84.7 (6)	C22—C21—N2—C18	36.3 (9)
O2—C1—C2—C3	−87.6 (6)	C20—C21—N2—C18	−143.4 (7)
O1—C1—C2—C3	96.1 (6)	N4—C25—N3—C23	0.3 (7)
C7—C2—C3—C4	4.2 (8)	N4—C25—N3—Zn2	179.8 (4)
C1—C2—C3—C4	−176.6 (5)	C24—C23—N3—C25	0.1 (7)
C7—C2—C3—C15ⁱ	−172.8 (5)	C24—C23—N3—Zn2	−179.4 (4)
C1—C2—C3—C15ⁱ	6.4 (8)	N3—C25—N4—C24	−0.5 (7)
C2—C3—C4—C5	−0.6 (9)	N3—C25—N4—C26	−179.9 (5)
C15ⁱ—C3—C4—C5	176.4 (5)	C23—C24—N4—C25	0.6 (7)
C3—C4—C5—C6	−2.0 (9)	C23—C24—N4—C26	179.9 (5)
C4—C5—C6—C7	1.0 (9)	C28^v—C26—N4—C25	−32.7 (9)
C3—C2—C7—O3	178.4 (4)	C27—C26—N4—C25	149.2 (6)
C1—C2—C7—O3	−0.8 (7)	C28^v—C26—N4—C24	148.1 (7)
C3—C2—C7—C6	−5.4 (8)	C27—C26—N4—C24	−30.0 (9)
C1—C2—C7—C6	175.4 (5)	O2—C1—O1—Zn1	6.4 (7)
C5—C6—C7—C2	2.8 (8)	C2—C1—O1—Zn1	−177.5 (3)
C5—C6—C7—O3	178.9 (5)	C9—C8—O3—C7	2.9 (8)
O3—C8—C9—C10	177.9 (5)	C13—C8—O3—C7	−179.8 (5)
C13—C8—C9—C10	0.7 (8)	C2—C7—O3—C8	−118.2 (5)
C8—C9—C10—C11	−1.0 (9)	C6—C7—O3—C8	65.5 (7)
C8—C9—C10—C16ⁱⁱ	176.9 (5)	O4—C14—O5—Zn2	6.6 (8)
C9—C10—C11—C12	0.4 (9)	C12—C14—O5—Zn2	−176.2 (4)
C16ⁱⁱ—C10—C11—C12	−177.6 (6)	O7—C15—O6—Zn1	9.3 (6)
C10—C11—C12—C13	0.5 (9)	C3ⁱ—C15—O6—Zn1	−168.3 (4)
C10—C11—C12—C14	−179.9 (5)	O10—C16—O9—Zn2	10.7 (8)
C11—C12—C13—C8	−0.8 (9)	C10ⁱⁱⁱ—C16—O9—Zn2	−166.5 (4)
C14—C12—C13—C8	179.6 (5)	C15—O6—Zn1—O1	165.7 (3)
C9—C8—C13—C12	0.2 (8)	C15—O6—Zn1—N1	−64.3 (4)
O3—C8—C13—C12	−177.3 (5)	C15—O6—Zn1—O8	54.1 (4)
C11—C12—C14—O4	−11.9 (9)	C1—O1—Zn1—O6	64.0 (4)
C13—C12—C14—O4	167.7 (6)	C1—O1—Zn1—N1	−72.7 (4)
C11—C12—C14—O5	170.8 (6)	C1—O1—Zn1—O8	−177.1 (3)
C13—C12—C14—O5	−9.6 (9)	C19—N1—Zn1—O6	68.4 (6)
N1—C17—C18—N2	1.6 (9)	C17—N1—Zn1—O6	−124.4 (5)
C22^iv—C20—C21—C22	0.5 (10)	C19—N1—Zn1—O1	−158.9 (5)
C22^iv—C20—C21—N2	−179.9 (5)	C17—N1—Zn1—O1	8.3 (6)
C20—C21—C22—C20^iv	−0.5 (10)	C19—N1—Zn1—O8	−55.4 (6)
N2—C21—C22—C20^iv	179.9 (5)	C17—N1—Zn1—O8	111.8 (5)
N3—C23—C24—N4	−0.4 (8)	C14—O5—Zn2—O9	175.8 (4)
C28^v—C26—C27—C28	2.0 (10)	C14—O5—Zn2—N3	−62.6 (5)
N4—C26—C27—C28	−179.9 (5)	C14—O5—Zn2—O11	55.2 (5)
C26—C27—C28—C26^v	−2.0 (10)	C16—O9—Zn2—O5	−170.0 (4)
N2—C19—N1—C17	1.0 (7)	C16—O9—Zn2—N3	63.4 (4)
N2—C19—N1—Zn1	170.1 (4)	C16—O9—Zn2—O11	−52.0 (4)
C18—C17—N1—C19	−1.7 (8)	C25—N3—Zn2—O5	163.1 (4)
C18—C17—N1—Zn1	−171.6 (5)	C23—N3—Zn2—O5	−17.4 (6)
N1—C19—N2—C18	−0.1 (7)	C25—N3—Zn2—O9	−82.1 (5)
N1—C19—N2—C21	178.2 (5)	C23—N3—Zn2—O9	97.4 (6)
C17—C18—N2—C19	−0.9 (8)	C25—N3—Zn2—O11	40.7 (5)
C17—C18—N2—C21	−179.3 (5)	C23—N3—Zn2—O11	−139.9 (5)
C22—C21—N2—C19	−141.7 (6)

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

Poly[[diaqua(µ-4,4'-bipyridine)[µ₅-3-(3,5-dicarboxylatophenoxy)phthalato]dizinc(II)] monohydrate] (3) top

Crystal data top

[Zn₂(C₁₆H₆O₉)(C₁₀H₈N₂)(H₂O)₂]·H₂O	Z = 2
M_r = 683.18	F(000) = 692
Triclinic, P1	D_x = 1.833 Mg m⁻³
a = 7.8759 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 8.0318 (8) Å	Cell parameters from 3214 reflections
c = 20.590 (2) Å	θ = 2.7–28.2°
α = 86.441 (2)°	µ = 2.01 mm⁻¹
β = 88.986 (1)°	T = 293 K
γ = 72.182 (2)°	Block, colorless
V = 1237.6 (2) Å³	0.28 × 0.26 × 0.22 mm

Data collection top

Bruker SMART APEX CCD area detector diffractometer	4348 independent reflections
Radiation source: fine-focus sealed tube	3723 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
phi and ω scans	θ_max = 25.0°, θ_min = 1.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −9→8
T_min = 0.603, T_max = 0.666	k = −7→9
6953 measured reflections	l = −24→24

Refinement top

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0318P)² + 1.5428P] where P = (F_o² + 2F_c²)/3
4348 reflections	(Δ/σ)_max = 0.001
379 parameters	Δρ_max = 0.50 e Å⁻³
0 restraints	Δρ_min = −0.48 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Zn1	0.73589 (5)	0.23279 (5)	−0.075769 (16)	0.02473 (11)
Zn2	1.33829 (4)	−0.49606 (5)	0.443107 (16)	0.02216 (11)
C1	0.0244 (4)	0.4209 (4)	−0.39012 (14)	0.0245 (7)
H1	0.0536	0.3720	−0.4302	0.029*
C2	0.1592 (4)	0.4033 (4)	−0.34604 (14)	0.0248 (7)
H2	0.2768	0.3459	−0.3569	0.030*
C3	0.1194 (4)	0.4714 (4)	−0.28545 (14)	0.0220 (6)
C4	−0.0575 (4)	0.5649 (4)	−0.27336 (15)	0.0303 (7)
H4	−0.0896	0.6171	−0.2340	0.036*
C5	−0.1847 (4)	0.5793 (4)	−0.32039 (15)	0.0290 (7)
H5	−0.3021	0.6434	−0.3119	0.035*
C6	0.2594 (4)	0.4369 (4)	−0.23430 (15)	0.0245 (7)
C7	0.4359 (4)	0.4213 (5)	−0.24985 (15)	0.0302 (7)
H7	0.4668	0.4476	−0.2922	0.036*
C8	0.5648 (4)	0.3664 (5)	−0.20208 (15)	0.0305 (8)
H8	0.6821	0.3576	−0.2133	0.037*
C9	0.3584 (4)	0.3473 (5)	−0.12487 (15)	0.0311 (8)
H9	0.3305	0.3244	−0.0818	0.037*
C10	0.2210 (4)	0.4027 (5)	−0.16992 (15)	0.0314 (8)
H10C	0.1039	0.4167	−0.1570	0.038*
C11	0.6203 (4)	0.1776 (4)	0.04078 (15)	0.0264 (7)
C12	0.6068 (4)	0.1199 (4)	0.11071 (14)	0.0226 (6)
C13	0.4369 (4)	0.1340 (4)	0.13529 (16)	0.0292 (7)
H13	0.3373	0.1812	0.1087	0.035*
C14	0.4160 (4)	0.0779 (4)	0.19907 (16)	0.0304 (7)
H14	0.3028	0.0855	0.2150	0.037*
C15	0.5625 (4)	0.0111 (4)	0.23901 (15)	0.0284 (7)
H15	0.5491	−0.0263	0.2819	0.034*
C16	0.7297 (4)	0.0002 (4)	0.21449 (14)	0.0223 (6)
C17	0.7565 (4)	0.0505 (4)	0.15042 (14)	0.0211 (6)
C18	0.9208 (4)	−0.0121 (4)	0.30611 (13)	0.0220 (6)
C19	1.0937 (4)	−0.0892 (4)	0.32871 (14)	0.0228 (6)
H19	1.1724	−0.1773	0.3060	0.027*
C20	1.1489 (4)	−0.0354 (4)	0.38480 (14)	0.0221 (6)
C21	1.0306 (4)	0.0955 (4)	0.41910 (14)	0.0225 (6)
H21A	1.0675	0.1330	0.4567	0.027*
C22	0.8574 (4)	0.1693 (4)	0.39669 (14)	0.0203 (6)
C23	0.8022 (4)	0.1170 (4)	0.33918 (14)	0.0233 (7)
H23	0.6867	0.1690	0.3236	0.028*
C24	0.7243 (4)	0.3043 (4)	0.43387 (14)	0.0212 (6)
C25	1.3381 (4)	−0.1182 (4)	0.40713 (15)	0.0284 (7)
C26	0.9474 (4)	0.0263 (4)	0.12825 (14)	0.0268 (7)
N1	0.5295 (3)	0.3253 (3)	−0.14032 (12)	0.0250 (6)
N2	−0.1473 (3)	0.5053 (3)	−0.37787 (12)	0.0237 (6)
O1	0.5019 (3)	0.3014 (3)	0.01521 (11)	0.0418 (6)
O2	0.7567 (3)	0.0940 (3)	0.00872 (11)	0.0354 (6)
O3	1.0355 (3)	−0.1319 (3)	0.11834 (11)	0.0366 (6)
O4	1.0032 (3)	0.1531 (4)	0.12456 (13)	0.0466 (7)
O5	1.4097 (3)	−0.2797 (3)	0.39973 (11)	0.0295 (5)
O6	1.4182 (3)	−0.0249 (4)	0.42996 (15)	0.0560 (8)
O7	0.7759 (3)	0.3472 (3)	0.48585 (10)	0.0314 (5)
O8	0.5708 (3)	0.3636 (3)	0.41035 (11)	0.0299 (5)
O9	0.8842 (3)	−0.0801 (3)	0.25002 (10)	0.0300 (5)
O10	1.3170 (3)	−0.7246 (3)	0.49485 (11)	0.0324 (5)
H10A	1.3362	−0.8172	0.4724	0.039*
H10B	1.3730	−0.7625	0.5259	0.039*
O11	0.7834 (3)	0.4583 (3)	−0.06460 (12)	0.0388 (6)
H11A	0.6978	0.5504	−0.0522	0.047*
H11B	0.8838	0.4388	−0.0428	0.047*
O1W	0.0842 (3)	0.2850 (3)	0.00282 (13)	0.0447 (6)
H1WA	0.0508	0.2628	0.0431	0.054*
H1WB	0.1122	0.1720	−0.0116	0.054*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.02043 (19)	0.0304 (2)	0.01966 (19)	−0.00256 (15)	−0.00180 (14)	0.00037 (15)
Zn2	0.01411 (18)	0.0282 (2)	0.02026 (19)	0.00091 (14)	−0.00265 (13)	−0.00913 (15)
C1	0.0218 (16)	0.0315 (17)	0.0181 (15)	−0.0052 (13)	−0.0004 (12)	−0.0014 (13)
C2	0.0164 (15)	0.0327 (18)	0.0233 (16)	−0.0051 (13)	−0.0007 (12)	0.0011 (13)
C3	0.0201 (15)	0.0259 (16)	0.0212 (15)	−0.0092 (13)	−0.0051 (12)	0.0027 (13)
C4	0.0273 (17)	0.0377 (19)	0.0218 (16)	−0.0024 (15)	−0.0042 (13)	−0.0080 (14)
C5	0.0201 (16)	0.0342 (19)	0.0274 (17)	0.0002 (14)	−0.0023 (13)	−0.0055 (14)
C6	0.0229 (16)	0.0270 (17)	0.0234 (16)	−0.0073 (13)	−0.0061 (13)	0.0001 (13)
C7	0.0267 (17)	0.046 (2)	0.0189 (16)	−0.0131 (15)	−0.0025 (13)	0.0031 (14)
C8	0.0207 (16)	0.048 (2)	0.0238 (17)	−0.0122 (15)	0.0000 (13)	0.0007 (15)
C9	0.0260 (17)	0.049 (2)	0.0185 (16)	−0.0119 (15)	0.0001 (13)	0.0001 (15)
C10	0.0219 (16)	0.049 (2)	0.0234 (17)	−0.0110 (15)	−0.0004 (13)	−0.0008 (15)
C11	0.0256 (17)	0.0322 (18)	0.0215 (16)	−0.0086 (14)	−0.0035 (13)	−0.0009 (14)
C12	0.0220 (15)	0.0244 (16)	0.0197 (15)	−0.0046 (13)	−0.0005 (12)	−0.0012 (12)
C13	0.0205 (16)	0.0344 (18)	0.0297 (17)	−0.0040 (14)	−0.0062 (13)	0.0006 (14)
C14	0.0247 (17)	0.0346 (19)	0.0305 (18)	−0.0067 (14)	0.0067 (14)	−0.0048 (15)
C15	0.0314 (18)	0.0302 (18)	0.0206 (16)	−0.0052 (14)	0.0050 (13)	−0.0016 (14)
C16	0.0231 (16)	0.0227 (16)	0.0173 (15)	−0.0004 (12)	−0.0023 (12)	−0.0052 (12)
C17	0.0208 (15)	0.0222 (15)	0.0186 (15)	−0.0033 (12)	−0.0011 (12)	−0.0056 (12)
C18	0.0259 (16)	0.0232 (16)	0.0129 (14)	−0.0020 (13)	−0.0008 (12)	0.0000 (12)
C19	0.0227 (15)	0.0196 (15)	0.0218 (15)	0.0003 (12)	0.0024 (12)	−0.0029 (12)
C20	0.0190 (15)	0.0204 (15)	0.0228 (15)	−0.0003 (12)	−0.0001 (12)	0.0012 (12)
C21	0.0236 (16)	0.0241 (16)	0.0185 (15)	−0.0047 (13)	−0.0003 (12)	−0.0050 (12)
C22	0.0197 (15)	0.0182 (15)	0.0199 (15)	−0.0010 (12)	0.0020 (12)	−0.0018 (12)
C23	0.0177 (15)	0.0257 (16)	0.0208 (15)	0.0015 (12)	−0.0012 (12)	−0.0002 (13)
C24	0.0205 (16)	0.0182 (15)	0.0233 (16)	−0.0036 (12)	0.0065 (12)	−0.0023 (12)
C25	0.0231 (16)	0.0334 (19)	0.0229 (16)	0.0001 (14)	−0.0001 (13)	−0.0019 (14)
C26	0.0210 (16)	0.040 (2)	0.0170 (15)	−0.0052 (15)	−0.0029 (12)	−0.0019 (14)
N1	0.0224 (14)	0.0327 (15)	0.0195 (13)	−0.0078 (11)	−0.0031 (10)	−0.0010 (11)
N2	0.0207 (13)	0.0270 (14)	0.0211 (13)	−0.0038 (11)	−0.0040 (10)	0.0000 (11)
O1	0.0355 (14)	0.0494 (16)	0.0275 (13)	0.0043 (12)	−0.0048 (11)	0.0097 (12)
O2	0.0357 (13)	0.0402 (14)	0.0228 (12)	−0.0015 (11)	0.0034 (10)	0.0027 (10)
O3	0.0283 (13)	0.0384 (14)	0.0347 (13)	0.0018 (11)	0.0096 (10)	−0.0015 (11)
O4	0.0362 (14)	0.0543 (17)	0.0562 (17)	−0.0233 (13)	0.0053 (12)	−0.0094 (14)
O5	0.0209 (11)	0.0256 (12)	0.0346 (13)	0.0036 (9)	0.0042 (9)	−0.0011 (10)
O6	0.0307 (14)	0.0443 (16)	0.088 (2)	0.0014 (12)	−0.0231 (14)	−0.0251 (15)
O7	0.0323 (13)	0.0347 (13)	0.0239 (12)	−0.0032 (10)	0.0041 (10)	−0.0139 (10)
O8	0.0190 (11)	0.0307 (12)	0.0333 (13)	0.0033 (9)	0.0030 (9)	−0.0089 (10)
O9	0.0292 (12)	0.0338 (13)	0.0169 (11)	0.0068 (10)	−0.0063 (9)	−0.0071 (9)
O10	0.0279 (12)	0.0332 (13)	0.0297 (12)	−0.0004 (10)	−0.0064 (10)	0.0023 (10)
O11	0.0344 (13)	0.0347 (14)	0.0461 (15)	−0.0077 (11)	−0.0067 (11)	−0.0070 (11)
O1W	0.0453 (15)	0.0414 (15)	0.0493 (16)	−0.0164 (12)	−0.0073 (12)	0.0006 (12)

Geometric parameters (Å, º) top

Zn1—O3ⁱ	1.951 (2)	C13—H13	0.9300
Zn1—O11	1.986 (2)	C14—C15	1.377 (5)
Zn1—O2	1.988 (2)	C14—H14	0.9300
Zn1—N1	2.043 (2)	C15—C16	1.381 (4)
Zn2—O8ⁱⁱ	1.966 (2)	C15—H15	0.9300
Zn2—O7ⁱⁱⁱ	1.973 (2)	C16—O9	1.387 (3)
Zn2—N2^iv	2.055 (2)	C16—C17	1.387 (4)
Zn2—O10	2.115 (2)	C17—C26	1.521 (4)
Zn2—O5	2.126 (2)	C18—C23	1.373 (4)
C1—N2	1.341 (4)	C18—O9	1.379 (4)
C1—C2	1.378 (4)	C18—C19	1.387 (4)
C1—H1	0.9300	C19—C20	1.380 (4)
C2—C3	1.385 (4)	C19—H19	0.9300
C2—H2	0.9300	C20—C21	1.394 (4)
C3—C4	1.392 (4)	C20—C25	1.501 (4)
C3—C6	1.490 (4)	C21—C22	1.385 (4)
C4—C5	1.380 (4)	C21—H21A	0.9300
C4—H4	0.9300	C22—C23	1.400 (4)
C5—N2	1.345 (4)	C22—C24	1.497 (4)
C5—H5	0.9300	C23—H23	0.9300
C6—C10	1.384 (4)	C24—O8	1.250 (4)
C6—C7	1.391 (4)	C24—O7	1.256 (4)
C7—C8	1.378 (4)	C25—O6	1.235 (4)
C7—H7	0.9300	C25—O5	1.264 (4)
C8—N1	1.340 (4)	C26—O4	1.225 (4)
C8—H8	0.9300	C26—O3	1.274 (4)
C9—N1	1.340 (4)	N2—Zn2^iv	2.055 (2)
C9—C10	1.385 (4)	O3—Zn1ⁱ	1.951 (2)
C9—H9	0.9300	O7—Zn2ⁱⁱⁱ	1.972 (2)
C10—H10C	0.9300	O8—Zn2^v	1.967 (2)
C11—O1	1.233 (4)	O10—H10A	0.8719
C11—O2	1.276 (4)	O10—H10B	0.7748
C11—C12	1.497 (4)	O11—H11A	0.8826
C12—C17	1.395 (4)	O11—H11B	0.8832
C12—C13	1.396 (4)	O1W—H1WA	0.8888
C13—C14	1.385 (5)	O1W—H1WB	0.9330

O3ⁱ—Zn1—O11	92.95 (10)	C13—C14—H14	119.9
O3ⁱ—Zn1—O2	104.25 (10)	C14—C15—C16	119.1 (3)
O11—Zn1—O2	110.81 (10)	C14—C15—H15	120.4
O3ⁱ—Zn1—N1	112.76 (10)	C16—C15—H15	120.4
O11—Zn1—N1	97.63 (10)	C15—C16—O9	122.1 (3)
O2—Zn1—N1	131.59 (10)	C15—C16—C17	122.5 (3)
O8ⁱⁱ—Zn2—O7ⁱⁱⁱ	142.94 (9)	O9—C16—C17	115.0 (3)
O8ⁱⁱ—Zn2—N2^iv	107.52 (10)	C16—C17—C12	117.8 (3)
O7ⁱⁱⁱ—Zn2—N2^iv	109.52 (10)	C16—C17—C26	117.8 (3)
O8ⁱⁱ—Zn2—O10	88.46 (9)	C12—C17—C26	124.4 (3)
O7ⁱⁱⁱ—Zn2—O10	92.07 (9)	C23—C18—O9	125.6 (3)
N2^iv—Zn2—O10	90.93 (9)	C23—C18—C19	120.8 (3)
O8ⁱⁱ—Zn2—O5	84.41 (9)	O9—C18—C19	113.6 (3)
O7ⁱⁱⁱ—Zn2—O5	88.45 (9)	C20—C19—C18	120.1 (3)
N2^iv—Zn2—O5	99.45 (9)	C20—C19—H19	120.0
O10—Zn2—O5	168.79 (8)	C18—C19—H19	120.0
N2—C1—C2	122.9 (3)	C19—C20—C21	120.0 (3)
N2—C1—H1	118.5	C19—C20—C25	118.8 (3)
C2—C1—H1	118.5	C21—C20—C25	121.2 (3)
C1—C2—C3	119.9 (3)	C22—C21—C20	119.4 (3)
C1—C2—H2	120.0	C22—C21—H21A	120.3
C3—C2—H2	120.0	C20—C21—H21A	120.3
C2—C3—C4	117.4 (3)	C21—C22—C23	120.7 (3)
C2—C3—C6	120.9 (3)	C21—C22—C24	120.9 (3)
C4—C3—C6	121.6 (3)	C23—C22—C24	118.4 (3)
C5—C4—C3	119.2 (3)	C18—C23—C22	119.0 (3)
C5—C4—H4	120.4	C18—C23—H23	120.5
C3—C4—H4	120.4	C22—C23—H23	120.5
N2—C5—C4	123.3 (3)	O8—C24—O7	125.8 (3)
N2—C5—H5	118.4	O8—C24—C22	116.8 (3)
C4—C5—H5	118.4	O7—C24—C22	117.4 (3)
C10—C6—C7	117.4 (3)	O6—C25—O5	123.1 (3)
C10—C6—C3	120.6 (3)	O6—C25—C20	118.7 (3)
C7—C6—C3	121.7 (3)	O5—C25—C20	118.2 (3)
C8—C7—C6	119.5 (3)	O4—C26—O3	126.9 (3)
C8—C7—H7	120.2	O4—C26—C17	119.1 (3)
C6—C7—H7	120.2	O3—C26—C17	113.9 (3)
N1—C8—C7	123.2 (3)	C8—N1—C9	117.1 (3)
N1—C8—H8	118.4	C8—N1—Zn1	119.0 (2)
C7—C8—H8	118.4	C9—N1—Zn1	123.9 (2)
N1—C9—C10	123.1 (3)	C1—N2—C5	117.1 (3)
N1—C9—H9	118.4	C1—N2—Zn2^iv	118.9 (2)
C10—C9—H9	118.4	C5—N2—Zn2^iv	123.8 (2)
C6—C10—C9	119.5 (3)	C11—O2—Zn1	104.12 (19)
C6—C10—H10C	120.3	C26—O3—Zn1ⁱ	131.5 (2)
C9—C10—H10C	120.3	C25—O5—Zn2	128.7 (2)
O1—C11—O2	121.5 (3)	C24—O7—Zn2ⁱⁱⁱ	135.6 (2)
O1—C11—C12	120.5 (3)	C24—O8—Zn2^v	134.7 (2)
O2—C11—C12	118.0 (3)	C18—O9—C16	121.4 (2)
C17—C12—C13	120.2 (3)	Zn2—O10—H10A	116.0
C17—C12—C11	122.3 (3)	Zn2—O10—H10B	121.2
C13—C12—C11	117.5 (3)	H10A—O10—H10B	101.9
C14—C13—C12	120.3 (3)	Zn1—O11—H11A	120.7
C14—C13—H13	119.9	Zn1—O11—H11B	109.6
C12—C13—H13	119.9	H11A—O11—H11B	113.1
C15—C14—C13	120.1 (3)	H1WA—O1W—H1WB	98.3
C15—C14—H14	119.9

N2—C1—C2—C3	1.4 (5)	C23—C22—C24—O8	−0.8 (4)
C1—C2—C3—C4	−3.7 (5)	C21—C22—C24—O7	−0.1 (4)
C1—C2—C3—C6	173.1 (3)	C23—C22—C24—O7	178.9 (3)
C2—C3—C4—C5	2.7 (5)	C19—C20—C25—O6	140.7 (3)
C6—C3—C4—C5	−174.1 (3)	C21—C20—C25—O6	−38.4 (5)
C3—C4—C5—N2	0.8 (5)	C19—C20—C25—O5	−37.1 (4)
C2—C3—C6—C10	−139.8 (3)	C21—C20—C25—O5	143.8 (3)
C4—C3—C6—C10	36.8 (5)	C16—C17—C26—O4	−100.7 (4)
C2—C3—C6—C7	33.9 (5)	C12—C17—C26—O4	79.2 (4)
C4—C3—C6—C7	−149.5 (3)	C16—C17—C26—O3	76.0 (4)
C10—C6—C7—C8	2.6 (5)	C12—C17—C26—O3	−104.0 (4)
C3—C6—C7—C8	−171.4 (3)	C7—C8—N1—C9	−3.1 (5)
C6—C7—C8—N1	0.5 (6)	C7—C8—N1—Zn1	176.6 (3)
C7—C6—C10—C9	−2.9 (5)	C10—C9—N1—C8	2.8 (5)
C3—C6—C10—C9	171.1 (3)	C10—C9—N1—Zn1	−177.0 (3)
N1—C9—C10—C6	0.3 (6)	O3ⁱ—Zn1—N1—C8	−22.3 (3)
O1—C11—C12—C17	−147.5 (3)	O11—Zn1—N1—C8	74.2 (3)
O2—C11—C12—C17	33.1 (5)	O2—Zn1—N1—C8	−159.1 (2)
O1—C11—C12—C13	34.0 (5)	O3ⁱ—Zn1—N1—C9	157.5 (3)
O2—C11—C12—C13	−145.4 (3)	O11—Zn1—N1—C9	−106.1 (3)
C17—C12—C13—C14	−0.5 (5)	O2—Zn1—N1—C9	20.7 (3)
C11—C12—C13—C14	178.1 (3)	C2—C1—N2—C5	2.0 (5)
C12—C13—C14—C15	1.3 (5)	C2—C1—N2—Zn2^iv	−172.6 (2)
C13—C14—C15—C16	−0.3 (5)	C4—C5—N2—C1	−3.2 (5)
C14—C15—C16—O9	−174.1 (3)	C4—C5—N2—Zn2^iv	171.2 (3)
C14—C15—C16—C17	−1.5 (5)	O1—C11—O2—Zn1	8.1 (4)
C15—C16—C17—C12	2.2 (5)	C12—C11—O2—Zn1	−172.5 (2)
O9—C16—C17—C12	175.3 (3)	O3ⁱ—Zn1—O2—C11	169.7 (2)
C15—C16—C17—C26	−177.8 (3)	O11—Zn1—O2—C11	70.9 (2)
O9—C16—C17—C26	−4.8 (4)	N1—Zn1—O2—C11	−50.9 (3)
C13—C12—C17—C16	−1.2 (5)	O4—C26—O3—Zn1ⁱ	−16.1 (5)
C11—C12—C17—C16	−179.7 (3)	C17—C26—O3—Zn1ⁱ	167.5 (2)
C13—C12—C17—C26	178.9 (3)	O6—C25—O5—Zn2	118.2 (3)
C11—C12—C17—C26	0.3 (5)	C20—C25—O5—Zn2	−64.1 (4)
C23—C18—C19—C20	−0.5 (5)	O8ⁱⁱ—Zn2—O5—C25	−166.8 (3)
O9—C18—C19—C20	−179.4 (3)	O7ⁱⁱⁱ—Zn2—O5—C25	−23.3 (3)
C18—C19—C20—C21	0.5 (5)	N2^iv—Zn2—O5—C25	86.3 (3)
C18—C19—C20—C25	−178.5 (3)	O10—Zn2—O5—C25	−116.1 (4)
C19—C20—C21—C22	0.6 (5)	O8—C24—O7—Zn2ⁱⁱⁱ	5.9 (5)
C25—C20—C21—C22	179.6 (3)	C22—C24—O7—Zn2ⁱⁱⁱ	−173.7 (2)
C20—C21—C22—C23	−1.8 (5)	O7—C24—O8—Zn2^v	−12.9 (5)
C20—C21—C22—C24	177.2 (3)	C22—C24—O8—Zn2^v	166.8 (2)
O9—C18—C23—C22	178.2 (3)	C23—C18—O9—C16	12.3 (5)
C19—C18—C23—C22	−0.6 (5)	C19—C18—O9—C16	−168.8 (3)
C21—C22—C23—C18	1.8 (5)	C15—C16—O9—C18	−65.7 (4)
C24—C22—C23—C18	−177.2 (3)	C17—C16—O9—C18	121.2 (3)
C21—C22—C24—O8	−179.7 (3)

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

Poly[[µ₇-3-(3,5-dicarboxylatophenoxy)phthalato](1,10-phenanthroline)dicadmium(II)] (4) top

Crystal data top

[Cd₂(C₁₆H₆O₉)(C₁₂H₈N₂)]	Z = 2
M_r = 747.21	F(000) = 728
Triclinic, P1	D_x = 1.977 Mg m⁻³
a = 11.2042 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.2728 (5) Å	Cell parameters from 9186 reflections
c = 11.7208 (4) Å	θ = 3.2–28.4°
α = 109.537 (1)°	µ = 1.76 mm⁻¹
β = 97.561 (1)°	T = 296 K
γ = 110.368 (1)°	Block, colorless
V = 1255.33 (8) Å³	0.27 × 0.25 × 0.22 mm

Data collection top

Bruker APEXII CCD diffractometer	4376 independent reflections
Radiation source: fine-focus sealed tube	4188 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
φ and ω scans	θ_max = 25.0°, θ_min = 3.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −13→13
T_min = 0.649, T_max = 0.699	k = −11→13
8721 measured reflections	l = −13→13

Refinement top

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.060	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	w = 1/[σ²(F_o²) + (0.0224P)² + 1.4129P] where P = (F_o² + 2F_c²)/3
4376 reflections	(Δ/σ)_max = 0.002
364 parameters	Δρ_max = 0.55 e Å⁻³
0 restraints	Δρ_min = −0.99 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.2138 (3)	0.0051 (3)	−0.0691 (2)	0.0098 (5)
C2	0.2954 (2)	0.1506 (3)	0.0287 (2)	0.0091 (5)
C3	0.4281 (3)	0.2141 (3)	0.0348 (2)	0.0104 (5)
H3	0.4662	0.1648	−0.0168	0.012*
C4	0.5038 (2)	0.3517 (3)	0.1182 (2)	0.0083 (5)
C5	0.4490 (2)	0.4235 (3)	0.1990 (2)	0.0096 (5)
H5	0.5008	0.5144	0.2571	0.012*
C6	0.3155 (2)	0.3590 (3)	0.1930 (2)	0.0092 (5)
C7	0.2372 (2)	0.2224 (3)	0.1065 (2)	0.0086 (5)
H7	0.1477	0.1801	0.1009	0.010*
C8	0.2605 (2)	0.4435 (3)	0.2804 (2)	0.0096 (5)
C10	0.6959 (2)	0.6534 (3)	0.1663 (2)	0.0106 (5)
H10	0.6368	0.6331	0.0915	0.013*
C11	0.7726 (3)	0.7910 (3)	0.2521 (2)	0.0114 (5)
H11	0.7664	0.8633	0.2338	0.014*
C12	0.8578 (2)	0.8194 (3)	0.3644 (2)	0.0110 (5)
H12	0.9053	0.9106	0.4234	0.013*
C13	0.8727 (2)	0.7130 (3)	0.3896 (2)	0.0087 (5)
C14	0.7992 (2)	0.5746 (3)	0.3026 (2)	0.0081 (5)
C15	0.8173 (2)	0.4539 (3)	0.3189 (2)	0.0104 (5)
C16	0.9624 (2)	0.7429 (3)	0.5125 (2)	0.0101 (5)
C17	0.5957 (3)	0.0909 (3)	0.3453 (2)	0.0129 (5)
H17	0.5884	0.1467	0.3041	0.016*
C18	0.5114 (3)	−0.0509 (3)	0.2877 (3)	0.0163 (6)
H18	0.4485	−0.0875	0.2105	0.020*
C19	0.5225 (3)	−0.1345 (3)	0.3455 (3)	0.0158 (6)
H19	0.4677	−0.2290	0.3077	0.019*
C20	0.6175 (3)	−0.0772 (3)	0.4632 (3)	0.0138 (6)
C21	0.6354 (3)	−0.1590 (3)	0.5295 (3)	0.0177 (6)
H21	0.5829	−0.2540	0.4943	0.021*
C22	0.7271 (3)	−0.1003 (3)	0.6416 (3)	0.0190 (6)
H22	0.7393	−0.1559	0.6814	0.023*
C23	0.8065 (3)	0.0469 (3)	0.7010 (3)	0.0156 (6)
C24	0.8994 (3)	0.1134 (3)	0.8209 (3)	0.0200 (6)
H24	0.9152	0.0614	0.8631	0.024*
C25	0.9660 (3)	0.2542 (3)	0.8747 (3)	0.0210 (6)
H25	1.0258	0.2991	0.9546	0.025*
C26	0.9435 (3)	0.3309 (3)	0.8081 (3)	0.0167 (6)
H26	0.9894	0.4269	0.8457	0.020*
C27	0.7909 (3)	0.1309 (3)	0.6395 (3)	0.0127 (5)
C28	0.6966 (3)	0.0667 (3)	0.5162 (2)	0.0114 (5)
C29	0.7093 (2)	0.5485 (3)	0.1944 (2)	0.0087 (5)
Cd1	0.929284 (16)	0.235957 (18)	0.258125 (16)	0.00741 (7)
Cd2	0.827945 (18)	0.384786 (19)	0.564638 (17)	0.01061 (7)
N1	0.6856 (2)	0.1489 (2)	0.4566 (2)	0.0112 (4)
N2	0.8594 (2)	0.2718 (2)	0.6935 (2)	0.0128 (5)
O1	0.26922 (18)	−0.0521 (2)	−0.14289 (17)	0.0159 (4)
O2	0.09284 (17)	−0.05465 (19)	−0.07798 (17)	0.0135 (4)
O3	0.33651 (19)	0.5666 (2)	0.35345 (19)	0.0182 (4)
O4	0.13985 (18)	0.3928 (2)	0.28002 (18)	0.0155 (4)
O5	0.63232 (17)	0.40930 (19)	0.11172 (16)	0.0107 (4)
O6	0.89451 (19)	0.4165 (2)	0.26089 (18)	0.0163 (4)
O7	0.75461 (18)	0.3988 (2)	0.38144 (18)	0.0144 (4)
O8	1.00525 (17)	0.65264 (19)	0.51844 (16)	0.0107 (4)
O9	0.98876 (19)	0.8508 (2)	0.60685 (17)	0.017

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0111 (13)	0.0076 (13)	0.0076 (11)	0.0012 (11)	0.0004 (10)	0.0035 (10)
C2	0.0085 (12)	0.0066 (12)	0.0081 (11)	0.0004 (10)	−0.0007 (10)	0.0024 (10)
C3	0.0107 (13)	0.0098 (13)	0.0085 (11)	0.0031 (11)	0.0022 (10)	0.0025 (10)
C4	0.0053 (11)	0.0089 (13)	0.0085 (11)	0.0009 (10)	0.0003 (9)	0.0039 (10)
C5	0.0087 (12)	0.0063 (12)	0.0082 (11)	−0.0007 (10)	−0.0006 (10)	0.0017 (10)
C6	0.0090 (12)	0.0082 (12)	0.0090 (11)	0.0023 (10)	0.0013 (10)	0.0036 (10)
C7	0.0053 (11)	0.0090 (13)	0.0093 (12)	0.0004 (10)	0.0007 (9)	0.0046 (10)
C8	0.0090 (12)	0.0083 (13)	0.0090 (12)	0.0018 (11)	0.0012 (10)	0.0031 (10)
C10	0.0078 (12)	0.0115 (13)	0.0096 (12)	0.0016 (10)	0.0000 (10)	0.0043 (11)
C11	0.0101 (12)	0.0108 (13)	0.0149 (13)	0.0042 (11)	0.0033 (10)	0.0075 (11)
C12	0.0084 (12)	0.0065 (12)	0.0107 (12)	−0.0014 (10)	0.0010 (10)	0.0000 (10)
C13	0.0057 (12)	0.0101 (13)	0.0089 (12)	0.0024 (10)	0.0022 (10)	0.0033 (10)
C14	0.0060 (12)	0.0095 (13)	0.0097 (12)	0.0026 (10)	0.0047 (10)	0.0046 (10)
C15	0.0057 (12)	0.0076 (12)	0.0111 (12)	−0.0007 (10)	−0.0026 (10)	0.0016 (10)
C16	0.0039 (11)	0.0104 (13)	0.0107 (12)	−0.0017 (10)	0.0003 (10)	0.0039 (10)
C17	0.0113 (13)	0.0166 (14)	0.0124 (12)	0.0054 (11)	0.0064 (10)	0.0068 (11)
C18	0.0118 (13)	0.0206 (15)	0.0128 (13)	0.0048 (12)	0.0056 (11)	0.0037 (12)
C19	0.0123 (13)	0.0105 (14)	0.0187 (14)	0.0016 (11)	0.0087 (11)	0.0010 (11)
C20	0.0130 (13)	0.0130 (14)	0.0183 (13)	0.0064 (11)	0.0106 (11)	0.0065 (12)
C21	0.0191 (15)	0.0099 (14)	0.0283 (15)	0.0061 (12)	0.0137 (13)	0.0098 (12)
C22	0.0208 (15)	0.0197 (15)	0.0287 (16)	0.0117 (13)	0.0137 (13)	0.0183 (13)
C23	0.0138 (13)	0.0193 (15)	0.0210 (14)	0.0089 (12)	0.0111 (11)	0.0124 (12)
C24	0.0173 (14)	0.0292 (17)	0.0224 (15)	0.0111 (13)	0.0097 (12)	0.0180 (14)
C25	0.0146 (14)	0.0312 (18)	0.0166 (14)	0.0063 (13)	0.0046 (12)	0.0126 (13)
C26	0.0128 (13)	0.0190 (15)	0.0136 (13)	0.0020 (12)	0.0042 (11)	0.0059 (12)
C27	0.0092 (12)	0.0145 (14)	0.0163 (13)	0.0047 (11)	0.0076 (11)	0.0074 (11)
C28	0.0109 (13)	0.0113 (13)	0.0159 (13)	0.0052 (11)	0.0094 (11)	0.0073 (11)
C29	0.0046 (11)	0.0070 (12)	0.0093 (12)	−0.0001 (10)	0.0017 (9)	0.0001 (10)
Cd1	0.00602 (10)	0.00407 (10)	0.00688 (10)	−0.00046 (8)	−0.00085 (7)	−0.00016 (8)
Cd2	0.01248 (11)	0.00815 (11)	0.01252 (11)	0.00467 (8)	0.00653 (8)	0.00429 (8)
N1	0.0112 (11)	0.0125 (11)	0.0125 (10)	0.0058 (9)	0.0064 (9)	0.0058 (9)
N2	0.0106 (11)	0.0133 (12)	0.0149 (11)	0.0034 (9)	0.0063 (9)	0.0072 (10)
O1	0.0099 (9)	0.0095 (9)	0.0162 (9)	−0.0007 (8)	0.0044 (8)	−0.0041 (8)
O2	0.0068 (9)	0.0086 (9)	0.0135 (9)	−0.0030 (7)	0.0022 (7)	−0.0020 (8)
O3	0.0121 (10)	0.0077 (10)	0.0223 (10)	−0.0001 (8)	0.0063 (8)	−0.0045 (8)
O4	0.0078 (9)	0.0106 (10)	0.0190 (10)	−0.0007 (8)	0.0055 (8)	−0.0005 (8)
O5	0.0049 (8)	0.0072 (9)	0.0111 (8)	−0.0020 (7)	0.0012 (7)	−0.0014 (7)
O6	0.0189 (10)	0.0159 (10)	0.0212 (10)	0.0118 (9)	0.0093 (8)	0.0098 (9)
O7	0.0100 (9)	0.0141 (10)	0.0193 (10)	0.0011 (8)	0.0025 (8)	0.0119 (8)
O8	0.0074 (9)	0.0140 (10)	0.0107 (9)	0.0042 (8)	0.0015 (7)	0.0058 (8)
O9	0.018	0.011	0.011	0.003	−0.004	0.000

Geometric parameters (Å, º) top

C1—O2	1.258 (3)	C20—C28	1.408 (4)
C1—O1	1.263 (3)	C20—C21	1.435 (4)
C1—C2	1.504 (3)	C21—C22	1.346 (4)
C1—Cd1ⁱ	2.621 (3)	C21—H21	0.9300
C2—C3	1.387 (4)	C22—C23	1.437 (4)
C2—C7	1.394 (4)	C22—H22	0.9300
C3—C4	1.390 (4)	C23—C24	1.409 (4)
C3—H3	0.9300	C23—C27	1.410 (4)
C4—O5	1.383 (3)	C24—C25	1.362 (5)
C4—C5	1.384 (4)	C24—H24	0.9300
C5—C6	1.397 (4)	C25—C26	1.404 (4)
C5—H5	0.9300	C25—H25	0.9300
C6—C7	1.396 (4)	C26—N2	1.329 (4)
C6—C8	1.503 (4)	C26—H26	0.9300
C7—H7	0.9300	C27—N2	1.365 (4)
C8—O3	1.255 (3)	C27—C28	1.448 (4)
C8—O4	1.270 (3)	C28—N1	1.360 (3)
C8—Cd2ⁱⁱ	2.736 (3)	C29—O5	1.402 (3)
C10—C29	1.379 (4)	Cd1—O6	2.1927 (19)
C10—C11	1.399 (4)	Cd1—O1ⁱ	2.2791 (18)
C10—H10	0.9300	Cd1—O2ⁱ	2.3066 (18)
C11—C12	1.387 (4)	Cd1—O4^iv	2.3220 (18)
C11—H11	0.9300	Cd1—O9ⁱⁱⁱ	2.3628 (19)
C12—C13	1.384 (4)	Cd1—O8ⁱⁱⁱ	2.3721 (17)
C12—H12	0.9300	Cd1—C1ⁱ	2.621 (3)
C13—C14	1.404 (4)	Cd1—C16ⁱⁱⁱ	2.697 (2)
C13—C16	1.502 (3)	Cd2—O7	2.2721 (18)
C14—C29	1.385 (3)	Cd2—O8ⁱⁱⁱ	2.3178 (18)
C14—C15	1.511 (4)	Cd2—O3ⁱⁱ	2.3310 (19)
C15—O7	1.246 (3)	Cd2—N1	2.342 (2)
C15—O6	1.267 (3)	Cd2—N2	2.342 (2)
C16—O9	1.247 (3)	Cd2—O4ⁱⁱ	2.4240 (19)
C16—O8	1.285 (3)	Cd2—C8ⁱⁱ	2.736 (3)
C16—Cd1ⁱⁱⁱ	2.697 (2)	O1—Cd1ⁱ	2.2791 (18)
C17—N1	1.330 (3)	O2—Cd1ⁱ	2.3065 (18)
C17—C18	1.400 (4)	O3—Cd2ⁱⁱ	2.3310 (19)
C17—H17	0.9300	O4—Cd1^v	2.3220 (18)
C18—C19	1.360 (4)	O4—Cd2ⁱⁱ	2.4239 (19)
C18—H18	0.9300	O8—Cd2ⁱⁱⁱ	2.3179 (18)
C19—C20	1.412 (4)	O8—Cd1ⁱⁱⁱ	2.3721 (17)
C19—H19	0.9300	O9—Cd1ⁱⁱⁱ	2.3628 (19)

O2—C1—O1	121.8 (2)	N2—C26—C25	122.7 (3)
O2—C1—C2	119.9 (2)	N2—C26—H26	118.6
O1—C1—C2	118.3 (2)	C25—C26—H26	118.6
O2—C1—Cd1ⁱ	61.64 (13)	N2—C27—C23	122.3 (2)
O1—C1—Cd1ⁱ	60.40 (13)	N2—C27—C28	118.5 (2)
C2—C1—Cd1ⁱ	173.49 (18)	C23—C27—C28	119.2 (3)
C3—C2—C7	120.9 (2)	N1—C28—C20	122.2 (2)
C3—C2—C1	118.4 (2)	N1—C28—C27	118.4 (2)
C7—C2—C1	120.7 (2)	C20—C28—C27	119.3 (2)
C2—C3—C4	119.7 (2)	C10—C29—C14	122.3 (2)
C2—C3—H3	120.1	C10—C29—O5	120.5 (2)
C4—C3—H3	120.1	C14—C29—O5	117.2 (2)
O5—C4—C5	123.9 (2)	O6—Cd1—O1ⁱ	104.12 (7)
O5—C4—C3	115.8 (2)	O6—Cd1—O2ⁱ	124.73 (7)
C5—C4—C3	120.3 (2)	O1ⁱ—Cd1—O2ⁱ	57.44 (6)
C4—C5—C6	119.7 (2)	O6—Cd1—O4^iv	77.92 (7)
C4—C5—H5	120.1	O1ⁱ—Cd1—O4^iv	153.03 (7)
C6—C5—H5	120.1	O2ⁱ—Cd1—O4^iv	98.83 (6)
C7—C6—C5	120.5 (2)	O6—Cd1—O9ⁱⁱⁱ	141.78 (7)
C7—C6—C8	122.2 (2)	O1ⁱ—Cd1—O9ⁱⁱⁱ	100.34 (7)
C5—C6—C8	117.3 (2)	O2ⁱ—Cd1—O9ⁱⁱⁱ	93.19 (7)
C2—C7—C6	118.8 (2)	O4^iv—Cd1—O9ⁱⁱⁱ	93.06 (7)
C2—C7—H7	120.6	O6—Cd1—O8ⁱⁱⁱ	86.24 (7)
C6—C7—H7	120.6	O1ⁱ—Cd1—O8ⁱⁱⁱ	123.59 (6)
O3—C8—O4	120.4 (2)	O2ⁱ—Cd1—O8ⁱⁱⁱ	148.84 (7)
O3—C8—C6	118.4 (2)	O4^iv—Cd1—O8ⁱⁱⁱ	83.26 (6)
O4—C8—C6	121.2 (2)	O9ⁱⁱⁱ—Cd1—O8ⁱⁱⁱ	55.67 (6)
O3—C8—Cd2ⁱⁱ	58.13 (14)	O6—Cd1—C1ⁱ	118.92 (7)
O4—C8—Cd2ⁱⁱ	62.38 (14)	O1ⁱ—Cd1—C1ⁱ	28.82 (8)
C6—C8—Cd2ⁱⁱ	175.32 (18)	O2ⁱ—Cd1—C1ⁱ	28.68 (7)
C29—C10—C11	118.9 (2)	O4^iv—Cd1—C1ⁱ	126.88 (7)
C29—C10—H10	120.6	O9ⁱⁱⁱ—Cd1—C1ⁱ	96.34 (7)
C11—C10—H10	120.6	O8ⁱⁱⁱ—Cd1—C1ⁱ	142.32 (7)
C12—C11—C10	119.8 (2)	O6—Cd1—C16ⁱⁱⁱ	114.26 (8)
C12—C11—H11	120.1	O1ⁱ—Cd1—C16ⁱⁱⁱ	117.01 (7)
C10—C11—H11	120.1	O2ⁱ—Cd1—C16ⁱⁱⁱ	120.42 (8)
C13—C12—C11	120.5 (2)	O4^iv—Cd1—C16ⁱⁱⁱ	85.00 (7)
C13—C12—H12	119.7	O9ⁱⁱⁱ—Cd1—C16ⁱⁱⁱ	27.53 (8)
C11—C12—H12	119.7	O8ⁱⁱⁱ—Cd1—C16ⁱⁱⁱ	28.46 (7)
C12—C13—C14	120.2 (2)	C1ⁱ—Cd1—C16ⁱⁱⁱ	121.85 (8)
C12—C13—C16	120.7 (2)	O7—Cd2—O8ⁱⁱⁱ	85.24 (6)
C14—C13—C16	119.0 (2)	O7—Cd2—O3ⁱⁱ	93.00 (7)
C29—C14—C13	118.1 (2)	O8ⁱⁱⁱ—Cd2—O3ⁱⁱ	176.92 (7)
C29—C14—C15	118.6 (2)	O7—Cd2—N1	84.53 (7)
C13—C14—C15	123.3 (2)	O8ⁱⁱⁱ—Cd2—N1	90.71 (7)
O7—C15—O6	126.7 (2)	O3ⁱⁱ—Cd2—N1	91.63 (7)
O7—C15—C14	119.5 (2)	O7—Cd2—N2	155.64 (8)
O6—C15—C14	113.7 (2)	O8ⁱⁱⁱ—Cd2—N2	89.17 (7)
O9—C16—O8	121.7 (2)	O3ⁱⁱ—Cd2—N2	93.45 (8)
O9—C16—C13	119.7 (2)	N1—Cd2—N2	71.83 (8)
O8—C16—C13	118.5 (2)	O7—Cd2—O4ⁱⁱ	101.64 (7)
O9—C16—Cd1ⁱⁱⁱ	61.16 (13)	O8ⁱⁱⁱ—Cd2—O4ⁱⁱ	123.03 (6)
O8—C16—Cd1ⁱⁱⁱ	61.60 (12)	O3ⁱⁱ—Cd2—O4ⁱⁱ	54.84 (6)
C13—C16—Cd1ⁱⁱⁱ	166.79 (17)	N1—Cd2—O4ⁱⁱ	145.89 (7)
N1—C17—C18	122.7 (3)	N2—Cd2—O4ⁱⁱ	101.28 (7)
N1—C17—H17	118.7	O7—Cd2—C8ⁱⁱ	98.90 (7)
C18—C17—H17	118.7	O8ⁱⁱⁱ—Cd2—C8ⁱⁱ	150.68 (7)
C19—C18—C17	119.4 (2)	O3ⁱⁱ—Cd2—C8ⁱⁱ	27.20 (7)
C19—C18—H18	120.3	N1—Cd2—C8ⁱⁱ	118.52 (8)
C17—C18—H18	120.3	N2—Cd2—C8ⁱⁱ	97.53 (8)
C18—C19—C20	119.7 (3)	O4ⁱⁱ—Cd2—C8ⁱⁱ	27.66 (7)
C18—C19—H19	120.2	C17—N1—C28	118.5 (2)
C20—C19—H19	120.2	C17—N1—Cd2	125.84 (18)
C28—C20—C19	117.5 (3)	C28—N1—Cd2	115.63 (17)
C28—C20—C21	119.7 (3)	C26—N2—C27	118.4 (2)
C19—C20—C21	122.8 (3)	C26—N2—Cd2	126.13 (19)
C22—C21—C20	121.0 (3)	C27—N2—Cd2	115.27 (17)
C22—C21—H21	119.5	C1—O1—Cd1ⁱ	90.79 (15)
C20—C21—H21	119.5	C1—O2—Cd1ⁱ	89.67 (15)
C21—C22—C23	121.0 (3)	C8—O3—Cd2ⁱⁱ	94.67 (16)
C21—C22—H22	119.5	C8—O4—Cd1^v	161.78 (18)
C23—C22—H22	119.5	C8—O4—Cd2ⁱⁱ	89.96 (15)
C24—C23—C27	117.4 (3)	Cd1^v—O4—Cd2ⁱⁱ	106.53 (7)
C24—C23—C22	122.9 (3)	C4—O5—C29	116.34 (19)
C27—C23—C22	119.7 (3)	C15—O6—Cd1	121.64 (17)
C25—C24—C23	119.9 (3)	C15—O7—Cd2	130.47 (16)
C25—C24—H24	120.1	C16—O8—Cd2ⁱⁱⁱ	125.14 (16)
C23—C24—H24	120.1	C16—O8—Cd1ⁱⁱⁱ	89.94 (14)
C24—C25—C26	119.3 (3)	Cd2ⁱⁱⁱ—O8—Cd1ⁱⁱⁱ	113.47 (7)
C24—C25—H25	120.4	C16—O9—Cd1ⁱⁱⁱ	91.31 (16)
C26—C25—H25	120.4

O2—C1—C2—C3	−179.1 (2)	C18—C17—N1—Cd2	−178.36 (19)
O1—C1—C2—C3	−1.2 (4)	C20—C28—N1—C17	0.9 (4)
Cd1ⁱ—C1—C2—C3	−77.5 (17)	C27—C28—N1—C17	−177.6 (2)
O2—C1—C2—C7	−2.6 (4)	C20—C28—N1—Cd2	179.86 (19)
O1—C1—C2—C7	175.3 (2)	C27—C28—N1—Cd2	1.3 (3)
Cd1ⁱ—C1—C2—C7	99.0 (16)	O7—Cd2—N1—C17	−10.4 (2)
C7—C2—C3—C4	−0.8 (4)	O8ⁱⁱⁱ—Cd2—N1—C17	−95.6 (2)
C1—C2—C3—C4	175.6 (2)	O3ⁱⁱ—Cd2—N1—C17	82.4 (2)
C2—C3—C4—O5	−175.7 (2)	N2—Cd2—N1—C17	175.5 (2)
C2—C3—C4—C5	2.8 (4)	O4ⁱⁱ—Cd2—N1—C17	92.3 (2)
O5—C4—C5—C6	175.8 (2)	C8ⁱⁱ—Cd2—N1—C17	86.8 (2)
C3—C4—C5—C6	−2.6 (4)	O7—Cd2—N1—C28	170.73 (18)
C4—C5—C6—C7	0.3 (4)	O8ⁱⁱⁱ—Cd2—N1—C28	85.58 (18)
C4—C5—C6—C8	−178.3 (2)	O3ⁱⁱ—Cd2—N1—C28	−96.42 (18)
C3—C2—C7—C6	−1.4 (4)	N2—Cd2—N1—C28	−3.32 (17)
C1—C2—C7—C6	−177.7 (2)	O4ⁱⁱ—Cd2—N1—C28	−86.6 (2)
C5—C6—C7—C2	1.6 (4)	C8ⁱⁱ—Cd2—N1—C28	−92.10 (19)
C8—C6—C7—C2	−179.9 (2)	C25—C26—N2—C27	1.0 (4)
C7—C6—C8—O3	−178.4 (2)	C25—C26—N2—Cd2	−173.7 (2)
C5—C6—C8—O3	0.2 (4)	C23—C27—N2—C26	0.0 (4)
C7—C6—C8—O4	0.9 (4)	C28—C27—N2—C26	178.3 (2)
C5—C6—C8—O4	179.4 (2)	C23—C27—N2—Cd2	175.2 (2)
C7—C6—C8—Cd2ⁱⁱ	−138 (2)	C28—C27—N2—Cd2	−6.4 (3)
C5—C6—C8—Cd2ⁱⁱ	41 (2)	O7—Cd2—N2—C26	165.4 (2)
C29—C10—C11—C12	−1.5 (4)	O8ⁱⁱⁱ—Cd2—N2—C26	88.9 (2)
C10—C11—C12—C13	3.3 (4)	O3ⁱⁱ—Cd2—N2—C26	−89.5 (2)
C11—C12—C13—C14	−1.4 (4)	N1—Cd2—N2—C26	179.9 (2)
C11—C12—C13—C16	−178.5 (2)	O4ⁱⁱ—Cd2—N2—C26	−34.7 (2)
C12—C13—C14—C29	−2.2 (4)	C8ⁱⁱ—Cd2—N2—C26	−62.5 (2)
C16—C13—C14—C29	175.0 (2)	O7—Cd2—N2—C27	−9.4 (3)
C12—C13—C14—C15	175.4 (2)	O8ⁱⁱⁱ—Cd2—N2—C27	−85.93 (18)
C16—C13—C14—C15	−7.5 (4)	O3ⁱⁱ—Cd2—N2—C27	95.68 (18)
C29—C14—C15—O7	−95.8 (3)	N1—Cd2—N2—C27	5.09 (17)
C13—C14—C15—O7	86.6 (3)	O4ⁱⁱ—Cd2—N2—C27	150.49 (17)
C29—C14—C15—O6	81.7 (3)	C8ⁱⁱ—Cd2—N2—C27	122.70 (18)
C13—C14—C15—O6	−95.8 (3)	O2—C1—O1—Cd1ⁱ	5.1 (3)
C12—C13—C16—O9	23.9 (4)	C2—C1—O1—Cd1ⁱ	−172.7 (2)
C14—C13—C16—O9	−153.2 (2)	O1—C1—O2—Cd1ⁱ	−5.1 (3)
C12—C13—C16—O8	−159.2 (2)	C2—C1—O2—Cd1ⁱ	172.7 (2)
C14—C13—C16—O8	23.7 (3)	O4—C8—O3—Cd2ⁱⁱ	−2.9 (3)
C12—C13—C16—Cd1ⁱⁱⁱ	113.9 (8)	C6—C8—O3—Cd2ⁱⁱ	176.40 (19)
C14—C13—C16—Cd1ⁱⁱⁱ	−63.3 (9)	O3—C8—O4—Cd1^v	−152.5 (4)
N1—C17—C18—C19	−1.3 (4)	C6—C8—O4—Cd1^v	28.3 (7)
C17—C18—C19—C20	0.7 (4)	Cd2ⁱⁱ—C8—O4—Cd1^v	−155.2 (6)
C18—C19—C20—C28	0.6 (4)	O3—C8—O4—Cd2ⁱⁱ	2.7 (3)
C18—C19—C20—C21	−179.6 (3)	C6—C8—O4—Cd2ⁱⁱ	−176.5 (2)
C28—C20—C21—C22	−0.2 (4)	C5—C4—O5—C29	0.9 (3)
C19—C20—C21—C22	−179.9 (3)	C3—C4—O5—C29	179.3 (2)
C20—C21—C22—C23	2.4 (4)	C10—C29—O5—C4	−80.3 (3)
C21—C22—C23—C24	177.1 (3)	C14—C29—O5—C4	100.7 (3)
C21—C22—C23—C27	−1.7 (4)	O7—C15—O6—Cd1	1.2 (3)
C27—C23—C24—C25	2.5 (4)	C14—C15—O6—Cd1	−176.13 (15)
C22—C23—C24—C25	−176.3 (3)	O1ⁱ—Cd1—O6—C15	67.54 (19)
C23—C24—C25—C26	−1.7 (4)	O2ⁱ—Cd1—O6—C15	127.48 (18)
C24—C25—C26—N2	−0.1 (4)	O4^iv—Cd1—O6—C15	−140.1 (2)
C24—C23—C27—N2	−1.7 (4)	O9ⁱⁱⁱ—Cd1—O6—C15	−60.7 (2)
C22—C23—C27—N2	177.2 (2)	O8ⁱⁱⁱ—Cd1—O6—C15	−56.18 (19)
C24—C23—C27—C28	180.0 (2)	C1ⁱ—Cd1—O6—C15	94.3 (2)
C22—C23—C27—C28	−1.1 (4)	C16ⁱⁱⁱ—Cd1—O6—C15	−61.3 (2)
C19—C20—C28—N1	−1.4 (4)	O6—C15—O7—Cd2	66.6 (3)
C21—C20—C28—N1	178.8 (2)	C14—C15—O7—Cd2	−116.2 (2)
C19—C20—C28—C27	177.1 (2)	O8ⁱⁱⁱ—Cd2—O7—C15	−40.1 (2)
C21—C20—C28—C27	−2.7 (4)	O3ⁱⁱ—Cd2—O7—C15	137.4 (2)
N2—C27—C28—N1	3.5 (4)	N1—Cd2—O7—C15	−131.2 (2)
C23—C27—C28—N1	−178.1 (2)	N2—Cd2—O7—C15	−117.4 (3)
N2—C27—C28—C20	−175.1 (2)	O4ⁱⁱ—Cd2—O7—C15	82.7 (2)
C23—C27—C28—C20	3.3 (4)	C8ⁱⁱ—Cd2—O7—C15	110.7 (2)
C11—C10—C29—C14	−2.2 (4)	O9—C16—O8—Cd2ⁱⁱⁱ	−107.2 (3)
C11—C10—C29—O5	178.9 (2)	C13—C16—O8—Cd2ⁱⁱⁱ	75.9 (3)
C13—C14—C29—C10	4.0 (4)	Cd1ⁱⁱⁱ—C16—O8—Cd2ⁱⁱⁱ	−119.10 (15)
C15—C14—C29—C10	−173.7 (2)	O9—C16—O8—Cd1ⁱⁱⁱ	11.9 (2)
C13—C14—C29—O5	−177.0 (2)	C13—C16—O8—Cd1ⁱⁱⁱ	−165.0 (2)
C15—C14—C29—O5	5.3 (3)	O8—C16—O9—Cd1ⁱⁱⁱ	−12.0 (3)
C18—C17—N1—C28	0.5 (4)	C13—C16—O9—Cd1ⁱⁱⁱ	164.9 (2)

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

Poly[µ-aqua-(µ-4,4'-bipyridine)[µ₅-3-(3-carboxy-5-carboxylatophenoxy)phthalato]-µ₃-hydroxido-dinickel(II)] (5) top

Crystal data top

[Ni₂(C₁₆H₇O₉)(OH)(C₁₀H₈N₂)(H₂O)]	Z = 2
M_r = 651.84	F(000) = 664
Triclinic, P1	D_x = 1.716 Mg m⁻³
a = 9.2229 (8) Å	Cu Kα radiation, λ = 1.54178 Å
b = 12.2226 (10) Å	Cell parameters from 4552 reflections
c = 13.0730 (11) Å	θ = 4.1–67.2°
α = 112.261 (5)°	µ = 2.47 mm⁻¹
β = 106.134 (5)°	T = 293 K
γ = 97.765 (6)°	Block, green
V = 1261.34 (18) Å³	0.16 × 0.14 × 0.11 mm

Data collection top

Bruker APEXII CCD diffractometer	3886 independent reflections
Radiation source: fine-focus sealed tube	3421 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.028
φ and ω scans	θ_max = 63.0°, θ_min = 4.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −10→10
T_min = 0.694, T_max = 0.773	k = −14→14
7925 measured reflections	l = −15→14

Refinement top

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.146	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.1006P)² + 0.945P] where P = (F_o² + 2F_c²)/3
3886 reflections	(Δ/σ)_max = 0.001
370 parameters	Δρ_max = 1.06 e Å⁻³
0 restraints	Δρ_min = −0.37 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni1	0.44326 (6)	0.11611 (5)	0.99496 (4)	0.0211 (2)
Ni2	0.51874 (6)	−0.10978 (5)	0.76578 (4)	0.0233 (2)
C1	0.3857 (4)	0.3452 (3)	0.5192 (3)	0.0249 (7)
C2	0.3843 (4)	0.4635 (3)	0.5851 (3)	0.0259 (7)
H2A	0.3311	0.5055	0.5479	0.031*
C3	0.4626 (4)	0.5205 (3)	0.7076 (3)	0.0230 (7)
C4	0.5398 (4)	0.4571 (3)	0.7629 (3)	0.0256 (7)
H4	0.5889	0.4933	0.8449	0.031*
C5	0.5432 (4)	0.3398 (3)	0.6955 (3)	0.0239 (7)
C6	0.4680 (4)	0.2835 (3)	0.5747 (3)	0.0255 (7)
H6	0.4720	0.2047	0.5303	0.031*
C7	0.3068 (4)	0.2793 (3)	0.3875 (3)	0.0285 (7)
C8	0.4723 (4)	0.6541 (3)	0.7769 (3)	0.0242 (7)
C9	0.7696 (4)	0.3075 (3)	0.8141 (3)	0.0247 (7)
C10	0.8803 (4)	0.3904 (3)	0.8078 (3)	0.0304 (8)
H10	0.8511	0.4280	0.7584	0.037*
C11	1.0362 (4)	0.4161 (4)	0.8773 (3)	0.0334 (8)
H11	1.1129	0.4702	0.8729	0.040*
C12	1.0788 (4)	0.3621 (3)	0.9530 (3)	0.0302 (8)
H12	1.1835	0.3815	0.9999	0.036*
C13	0.9671 (4)	0.2796 (3)	0.9595 (3)	0.0246 (7)
C14	0.8092 (4)	0.2497 (3)	0.8878 (3)	0.0223 (7)
C15	1.0136 (4)	0.2221 (3)	1.0433 (3)	0.0296 (8)
C16	0.6799 (4)	0.1566 (3)	0.8818 (3)	0.0237 (7)
C17	0.2938 (4)	0.2038 (3)	0.8127 (3)	0.0296 (7)
H17	0.3935	0.2567	0.8424	0.036*
C18	0.1802 (4)	0.2057 (3)	0.7196 (3)	0.0317 (8)
H18	0.2048	0.2589	0.6877	0.038*
C19	0.0289 (4)	0.1287 (3)	0.6726 (3)	0.0261 (7)
C20	0.0012 (4)	0.0533 (3)	0.7260 (3)	0.0313 (8)
H20	−0.0983	0.0014	0.6997	0.038*
C21	0.1214 (4)	0.0550 (3)	0.8183 (3)	0.0299 (8)
H21	0.1000	0.0023	0.8514	0.036*
C22	−0.0974 (4)	0.1276 (3)	0.5719 (3)	0.0271 (7)
C23	−0.0833 (5)	0.2136 (4)	0.5281 (4)	0.0502 (12)
H23	0.0089	0.2764	0.5622	0.060*
C24	−0.2047 (5)	0.2068 (4)	0.4343 (4)	0.0483 (11)
H24	−0.1914	0.2669	0.4079	0.058*
C25	−0.3548 (5)	0.0379 (4)	0.4224 (4)	0.0405 (9)
H25	−0.4483	−0.0239	0.3870	0.049*
C26	−0.2391 (5)	0.0399 (4)	0.5167 (4)	0.0444 (10)
H26	−0.2572	−0.0192	0.5435	0.053*
N1	0.2663 (3)	0.1285 (3)	0.8624 (2)	0.0241 (6)
N2	−0.3393 (3)	0.1199 (3)	0.3796 (2)	0.0275 (6)
O1	0.3171 (3)	0.1775 (2)	0.3313 (2)	0.0366 (6)
O2	0.2273 (4)	0.3403 (3)	0.3416 (2)	0.0473 (8)
H2	0.1896	0.3024	0.2617	0.057*
O3	0.4375 (3)	0.7108 (2)	0.7145 (2)	0.0363 (6)
H3	0.4497	0.7954	0.7461	0.044*
O4	0.5200 (3)	0.6991 (2)	0.88749 (19)	0.0279 (5)
O5	0.6109 (3)	0.2686 (2)	0.7457 (2)	0.0339 (6)
O6	0.9239 (4)	0.1309 (3)	1.0330 (3)	0.0488 (8)
O7	1.1500 (3)	0.2703 (3)	1.1216 (2)	0.0394 (6)
O8	0.6375 (3)	0.0538 (2)	0.79461 (19)	0.0277 (5)
O9	0.6214 (3)	0.1902 (2)	0.9601 (2)	0.0317 (6)
O10	0.2902 (3)	0.0850 (2)	1.08058 (19)	0.0240 (5)
H10A	0.2155	0.0218	1.0576	0.029*
H10B	0.2461	0.1337	1.1008	0.029*
O11	0.5877 (3)	0.0663 (2)	1.11352 (18)	0.0241 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0261 (3)	0.0220 (3)	0.0126 (3)	0.0137 (2)	0.0009 (2)	0.0067 (2)
Ni2	0.0320 (3)	0.0196 (3)	0.0123 (3)	0.0122 (2)	−0.0012 (2)	0.0057 (2)
C1	0.0319 (17)	0.0222 (16)	0.0165 (16)	0.0117 (13)	0.0022 (13)	0.0073 (13)
C2	0.0337 (18)	0.0252 (17)	0.0186 (16)	0.0153 (14)	0.0025 (13)	0.0115 (14)
C3	0.0285 (16)	0.0203 (16)	0.0168 (15)	0.0103 (13)	0.0019 (13)	0.0079 (13)
C4	0.0291 (16)	0.0247 (16)	0.0165 (15)	0.0091 (13)	0.0000 (13)	0.0075 (13)
C5	0.0254 (16)	0.0231 (16)	0.0237 (16)	0.0111 (13)	0.0015 (13)	0.0142 (14)
C6	0.0297 (17)	0.0209 (15)	0.0222 (16)	0.0123 (13)	0.0036 (13)	0.0078 (13)
C7	0.0382 (19)	0.0277 (18)	0.0159 (16)	0.0131 (15)	0.0048 (14)	0.0079 (14)
C8	0.0274 (16)	0.0221 (16)	0.0185 (16)	0.0107 (13)	0.0010 (13)	0.0080 (13)
C9	0.0280 (16)	0.0247 (16)	0.0147 (14)	0.0153 (13)	−0.0015 (13)	0.0056 (13)
C10	0.042 (2)	0.0281 (17)	0.0264 (17)	0.0170 (15)	0.0129 (15)	0.0144 (15)
C11	0.036 (2)	0.0342 (19)	0.0317 (18)	0.0130 (15)	0.0139 (16)	0.0139 (16)
C12	0.0244 (16)	0.0315 (18)	0.0254 (17)	0.0119 (14)	0.0048 (14)	0.0044 (15)
C13	0.0259 (16)	0.0271 (16)	0.0140 (14)	0.0170 (13)	0.0002 (13)	0.0038 (13)
C14	0.0275 (16)	0.0190 (15)	0.0151 (14)	0.0129 (13)	0.0033 (12)	0.0030 (12)
C15	0.0301 (18)	0.0303 (18)	0.0209 (16)	0.0150 (15)	0.0005 (14)	0.0073 (14)
C16	0.0280 (16)	0.0241 (16)	0.0156 (15)	0.0165 (13)	−0.0022 (13)	0.0092 (13)
C17	0.0268 (17)	0.0355 (19)	0.0296 (18)	0.0136 (14)	0.0051 (14)	0.0191 (16)
C18	0.0322 (18)	0.039 (2)	0.0288 (18)	0.0133 (16)	0.0053 (15)	0.0228 (16)
C19	0.0318 (17)	0.0307 (17)	0.0143 (15)	0.0175 (14)	0.0025 (14)	0.0094 (13)
C20	0.0292 (18)	0.0314 (18)	0.0219 (17)	0.0060 (14)	−0.0049 (14)	0.0108 (15)
C21	0.0348 (19)	0.0307 (18)	0.0224 (17)	0.0119 (15)	0.0013 (14)	0.0152 (14)
C22	0.0327 (18)	0.0299 (18)	0.0162 (15)	0.0164 (15)	0.0026 (14)	0.0092 (14)
C23	0.042 (2)	0.049 (2)	0.044 (2)	−0.0042 (19)	−0.0147 (19)	0.032 (2)
C24	0.042 (2)	0.049 (2)	0.045 (2)	−0.0021 (19)	−0.0122 (19)	0.035 (2)
C25	0.035 (2)	0.040 (2)	0.035 (2)	0.0038 (16)	−0.0091 (17)	0.0230 (18)
C26	0.040 (2)	0.047 (2)	0.040 (2)	0.0051 (18)	−0.0089 (18)	0.032 (2)
N1	0.0289 (14)	0.0272 (14)	0.0153 (12)	0.0156 (12)	0.0035 (11)	0.0089 (11)
N2	0.0343 (15)	0.0260 (14)	0.0152 (13)	0.0127 (12)	−0.0007 (12)	0.0073 (11)
O1	0.0533 (16)	0.0269 (13)	0.0195 (12)	0.0162 (12)	0.0065 (11)	0.0028 (10)
O2	0.071 (2)	0.0457 (16)	0.0157 (12)	0.0343 (15)	−0.0008 (12)	0.0092 (11)
O3	0.0574 (16)	0.0199 (12)	0.0182 (11)	0.0152 (11)	−0.0041 (11)	0.0057 (10)
O4	0.0394 (13)	0.0247 (12)	0.0147 (11)	0.0153 (10)	0.0043 (10)	0.0052 (9)
O5	0.0312 (13)	0.0268 (12)	0.0354 (14)	0.0094 (10)	−0.0073 (11)	0.0185 (11)
O6	0.0494 (17)	0.0406 (16)	0.0418 (16)	0.0053 (13)	−0.0122 (13)	0.0256 (13)
O7	0.0322 (14)	0.0515 (17)	0.0234 (12)	0.0141 (12)	−0.0061 (11)	0.0155 (12)
O8	0.0397 (13)	0.0202 (11)	0.0177 (11)	0.0113 (10)	0.0029 (10)	0.0069 (10)
O9	0.0364 (13)	0.0277 (13)	0.0272 (13)	0.0120 (10)	0.0104 (11)	0.0079 (10)
O10	0.0289 (12)	0.0256 (11)	0.0163 (10)	0.0156 (9)	0.0032 (9)	0.0085 (9)
O11	0.0303 (12)	0.0230 (11)	0.0136 (10)	0.0151 (9)	−0.0003 (9)	0.0056 (9)

Geometric parameters (Å, º) top

Ni1—O9	2.013 (3)	C13—C15	1.510 (5)
Ni1—O11ⁱ	2.066 (2)	C14—C16	1.496 (5)
Ni1—O11	2.082 (2)	C15—O6	1.232 (5)
Ni1—N1	2.094 (3)	C15—O7	1.267 (4)
Ni1—O4ⁱⁱ	2.110 (2)	C16—O9	1.246 (4)
Ni1—O10	2.109 (2)	C16—O8	1.252 (4)
Ni2—O8	1.987 (2)	C17—N1	1.347 (5)
Ni2—O3ⁱⁱⁱ	1.995 (3)	C17—C18	1.378 (5)
Ni2—O11ⁱ	2.026 (2)	C17—H17	0.9300
Ni2—N2^iv	2.094 (3)	C18—C19	1.393 (5)
Ni2—O10ⁱ	2.159 (2)	C18—H18	0.9300
Ni2—O1^v	2.280 (3)	C19—C20	1.388 (5)
C1—C2	1.379 (5)	C19—C22	1.490 (5)
C1—C6	1.390 (5)	C20—C21	1.384 (5)
C1—C7	1.496 (4)	C20—H20	0.9300
C2—C3	1.395 (4)	C21—N1	1.335 (5)
C2—H2A	0.9300	C21—H21	0.9300
C3—C4	1.384 (4)	C22—C26	1.374 (6)
C3—C8	1.513 (4)	C22—C23	1.382 (6)
C4—C5	1.380 (5)	C23—C24	1.378 (6)
C4—H4	0.9300	C23—H23	0.9300
C5—C6	1.374 (5)	C24—N2	1.326 (5)
C5—O5	1.390 (4)	C24—H24	0.9300
C6—H6	0.9300	C25—N2	1.331 (5)
C7—O1	1.215 (4)	C25—C26	1.377 (5)
C7—O2	1.303 (4)	C25—H25	0.9300
C8—O4	1.251 (4)	C26—H26	0.9300
C8—O3	1.262 (4)	N2—Ni2^iv	2.094 (3)
C9—C10	1.380 (5)	O1—Ni2^v	2.280 (3)
C9—O5	1.389 (4)	O2—H2	0.9026
C9—C14	1.396 (5)	O3—Ni2^vi	1.995 (3)
C10—C11	1.388 (5)	O3—H3	0.9337
C10—H10	0.9300	O4—Ni1ⁱⁱ	2.110 (2)
C11—C12	1.385 (5)	O10—Ni2ⁱ	2.159 (2)
C11—H11	0.9300	O10—H10A	0.8522
C12—C13	1.386 (5)	O10—H10B	0.7716
C12—H12	0.9300	O11—Ni2ⁱ	2.026 (2)
C13—C14	1.404 (5)	O11—Ni1ⁱ	2.066 (2)

O9—Ni1—O11ⁱ	98.26 (10)	C12—C13—C14	119.5 (3)
O9—Ni1—O11	93.73 (10)	C12—C13—C15	120.7 (3)
O11ⁱ—Ni1—O11	79.46 (9)	C14—C13—C15	119.8 (3)
O9—Ni1—N1	95.20 (11)	C9—C14—C13	118.3 (3)
O11ⁱ—Ni1—N1	90.82 (9)	C9—C14—C16	117.2 (3)
O11—Ni1—N1	167.66 (11)	C13—C14—C16	124.4 (3)
O9—Ni1—O4ⁱⁱ	82.38 (10)	O6—C15—O7	122.4 (3)
O11ⁱ—Ni1—O4ⁱⁱ	177.36 (8)	O6—C15—C13	121.1 (3)
O11—Ni1—O4ⁱⁱ	97.95 (9)	O7—C15—C13	116.5 (3)
N1—Ni1—O4ⁱⁱ	91.67 (10)	O9—C16—O8	126.9 (3)
O9—Ni1—O10	162.84 (10)	O9—C16—C14	117.5 (3)
O11ⁱ—Ni1—O10	96.64 (9)	O8—C16—C14	115.5 (3)
O11—Ni1—O10	80.65 (9)	N1—C17—C18	122.7 (3)
N1—Ni1—O10	93.05 (10)	N1—C17—H17	118.6
O4ⁱⁱ—Ni1—O10	82.36 (9)	C18—C17—H17	118.6
O8—Ni2—O3ⁱⁱⁱ	164.87 (11)	C17—C18—C19	120.6 (3)
O8—Ni2—O11ⁱ	102.63 (10)	C17—C18—H18	119.7
O3ⁱⁱⁱ—Ni2—O11ⁱ	91.89 (11)	C19—C18—H18	119.7
O8—Ni2—N2^iv	91.40 (11)	C20—C19—C18	116.1 (3)
O3ⁱⁱⁱ—Ni2—N2^iv	90.46 (11)	C20—C19—C22	121.4 (3)
O11ⁱ—Ni2—N2^iv	99.14 (10)	C18—C19—C22	122.5 (3)
O8—Ni2—O10ⁱ	84.49 (9)	C21—C20—C19	120.1 (3)
O3ⁱⁱⁱ—Ni2—O10ⁱ	93.80 (9)	C21—C20—H20	119.9
O11ⁱ—Ni2—O10ⁱ	80.74 (8)	C19—C20—H20	119.9
N2^iv—Ni2—O10ⁱ	175.74 (10)	N1—C21—C20	123.4 (3)
O8—Ni2—O1^v	83.06 (10)	N1—C21—H21	118.3
O3ⁱⁱⁱ—Ni2—O1^v	81.81 (11)	C20—C21—H21	118.3
O11ⁱ—Ni2—O1^v	162.63 (9)	C26—C22—C23	115.1 (3)
N2^iv—Ni2—O1^v	97.09 (10)	C26—C22—C19	121.4 (3)
O10ⁱ—Ni2—O1^v	83.53 (9)	C23—C22—C19	123.5 (3)
C2—C1—C6	119.9 (3)	C24—C23—C22	120.5 (4)
C2—C1—C7	123.0 (3)	C24—C23—H23	119.7
C6—C1—C7	117.1 (3)	C22—C23—H23	119.7
C1—C2—C3	120.1 (3)	N2—C24—C23	123.9 (4)
C1—C2—H2A	120.0	N2—C24—H24	118.1
C3—C2—H2A	120.0	C23—C24—H24	118.1
C4—C3—C2	119.8 (3)	N2—C25—C26	123.2 (4)
C4—C3—C8	120.8 (3)	N2—C25—H25	118.4
C2—C3—C8	119.3 (3)	C26—C25—H25	118.4
C5—C4—C3	119.4 (3)	C22—C26—C25	121.3 (4)
C5—C4—H4	120.3	C22—C26—H26	119.3
C3—C4—H4	120.3	C25—C26—H26	119.3
C6—C5—C4	121.2 (3)	C21—N1—C17	116.9 (3)
C6—C5—O5	116.3 (3)	C21—N1—Ni1	120.3 (2)
C4—C5—O5	122.4 (3)	C17—N1—Ni1	122.6 (2)
C5—C6—C1	119.6 (3)	C24—N2—C25	116.0 (3)
C5—C6—H6	120.2	C24—N2—Ni2^iv	122.8 (2)
C1—C6—H6	120.2	C25—N2—Ni2^iv	121.2 (2)
O1—C7—O2	124.6 (3)	C7—O1—Ni2^v	132.9 (3)
O1—C7—C1	121.4 (3)	C7—O2—H2	112.2
O2—C7—C1	114.0 (3)	C8—O3—Ni2^vi	126.3 (2)
O4—C8—O3	126.4 (3)	C8—O3—H3	123.6
O4—C8—C3	118.9 (3)	Ni2^vi—O3—H3	17.4
O3—C8—C3	114.6 (3)	C8—O4—Ni1ⁱⁱ	126.6 (2)
C10—C9—O5	124.6 (3)	C9—O5—C5	120.3 (3)
C10—C9—C14	122.3 (3)	C16—O8—Ni2	131.5 (2)
O5—C9—C14	113.0 (3)	C16—O9—Ni1	136.5 (2)
C9—C10—C11	118.3 (3)	Ni1—O10—Ni2ⁱ	92.45 (9)
C9—C10—H10	120.8	Ni1—O10—H10A	128.8
C11—C10—H10	120.8	Ni2ⁱ—O10—H10A	111.9
C12—C11—C10	120.7 (4)	Ni1—O10—H10B	117.5
C12—C11—H11	119.7	Ni2ⁱ—O10—H10B	108.1
C10—C11—H11	119.7	H10A—O10—H10B	97.4
C11—C12—C13	120.8 (3)	Ni2ⁱ—O11—Ni1ⁱ	119.51 (12)
C11—C12—H12	119.6	Ni2ⁱ—O11—Ni1	97.19 (9)
C13—C12—H12	119.6	Ni1ⁱ—O11—Ni1	100.54 (9)

C6—C1—C2—C3	−1.3 (5)	C20—C21—N1—C17	0.0 (5)
C7—C1—C2—C3	−178.9 (3)	C20—C21—N1—Ni1	−176.1 (3)
C1—C2—C3—C4	−0.9 (5)	C18—C17—N1—C21	−0.9 (5)
C1—C2—C3—C8	174.4 (3)	C18—C17—N1—Ni1	175.1 (3)
C2—C3—C4—C5	2.4 (5)	O9—Ni1—N1—C21	156.9 (3)
C8—C3—C4—C5	−172.9 (3)	O11ⁱ—Ni1—N1—C21	58.6 (3)
C3—C4—C5—C6	−1.7 (5)	O11—Ni1—N1—C21	20.8 (6)
C3—C4—C5—O5	−176.3 (3)	O4ⁱⁱ—Ni1—N1—C21	−120.6 (3)
C4—C5—C6—C1	−0.5 (5)	O10—Ni1—N1—C21	−38.1 (3)
O5—C5—C6—C1	174.4 (3)	O9—Ni1—N1—C17	−18.9 (3)
C2—C1—C6—C5	2.0 (5)	O11ⁱ—Ni1—N1—C17	−117.3 (3)
C7—C1—C6—C5	179.8 (3)	O11—Ni1—N1—C17	−155.1 (4)
C2—C1—C7—O1	176.1 (4)	O4ⁱⁱ—Ni1—N1—C17	63.6 (3)
C6—C1—C7—O1	−1.6 (5)	O10—Ni1—N1—C17	146.0 (3)
C2—C1—C7—O2	−4.6 (5)	C23—C24—N2—C25	1.7 (7)
C6—C1—C7—O2	177.7 (3)	C23—C24—N2—Ni2^iv	−178.2 (4)
C4—C3—C8—O4	−16.0 (5)	C26—C25—N2—C24	−0.9 (7)
C2—C3—C8—O4	168.7 (3)	C26—C25—N2—Ni2^iv	179.0 (4)
C4—C3—C8—O3	160.6 (3)	O2—C7—O1—Ni2^v	86.4 (5)
C2—C3—C8—O3	−14.7 (5)	C1—C7—O1—Ni2^v	−94.4 (4)
O5—C9—C10—C11	−176.7 (3)	O4—C8—O3—Ni2^vi	24.7 (5)
C14—C9—C10—C11	0.3 (5)	C3—C8—O3—Ni2^vi	−151.6 (2)
C9—C10—C11—C12	−1.6 (5)	O3—C8—O4—Ni1ⁱⁱ	0.2 (5)
C10—C11—C12—C13	1.2 (5)	C3—C8—O4—Ni1ⁱⁱ	176.3 (2)
C11—C12—C13—C14	0.5 (5)	C10—C9—O5—C5	−22.1 (5)
C11—C12—C13—C15	−179.2 (3)	C14—C9—O5—C5	160.6 (3)
C10—C9—C14—C13	1.3 (5)	C6—C5—O5—C9	123.5 (3)
O5—C9—C14—C13	178.7 (3)	C4—C5—O5—C9	−61.6 (5)
C10—C9—C14—C16	−176.8 (3)	O9—C16—O8—Ni2	−22.0 (5)
O5—C9—C14—C16	0.6 (4)	C14—C16—O8—Ni2	161.2 (2)
C12—C13—C14—C9	−1.7 (5)	O3ⁱⁱⁱ—Ni2—O8—C16	−144.1 (3)
C15—C13—C14—C9	178.0 (3)	O11ⁱ—Ni2—O8—C16	19.2 (3)
C12—C13—C14—C16	176.2 (3)	N2^iv—Ni2—O8—C16	118.9 (3)
C15—C13—C14—C16	−4.0 (5)	O10ⁱ—Ni2—O8—C16	−60.0 (3)
C12—C13—C15—O6	−164.6 (4)	O1^v—Ni2—O8—C16	−144.1 (3)
C14—C13—C15—O6	15.7 (5)	O8—C16—O9—Ni1	−1.3 (5)
C12—C13—C15—O7	13.5 (5)	C14—C16—O9—Ni1	175.4 (2)
C14—C13—C15—O7	−166.3 (3)	O11ⁱ—Ni1—O9—C16	17.4 (3)
C9—C14—C16—O9	−99.4 (3)	O11—Ni1—O9—C16	97.3 (3)
C13—C14—C16—O9	82.6 (4)	N1—Ni1—O9—C16	−74.2 (3)
C9—C14—C16—O8	77.7 (4)	O4ⁱⁱ—Ni1—O9—C16	−165.2 (3)
C13—C14—C16—O8	−100.3 (4)	O10—Ni1—O9—C16	167.4 (3)
N1—C17—C18—C19	0.4 (6)	O9—Ni1—O10—Ni2ⁱ	−50.4 (3)
C17—C18—C19—C20	0.8 (5)	O11ⁱ—Ni1—O10—Ni2ⁱ	99.74 (8)
C17—C18—C19—C22	−179.9 (3)	O11—Ni1—O10—Ni2ⁱ	21.62 (8)
C18—C19—C20—C21	−1.6 (5)	N1—Ni1—O10—Ni2ⁱ	−169.07 (10)
C22—C19—C20—C21	179.1 (3)	O4ⁱⁱ—Ni1—O10—Ni2ⁱ	−77.80 (9)
C19—C20—C21—N1	1.3 (6)	O9—Ni1—O11—Ni2ⁱ	140.38 (10)
C20—C19—C22—C26	−9.7 (6)	O11ⁱ—Ni1—O11—Ni2ⁱ	−121.90 (14)
C18—C19—C22—C26	171.1 (4)	N1—Ni1—O11—Ni2ⁱ	−83.3 (5)
C20—C19—C22—C23	169.4 (4)	O4ⁱⁱ—Ni1—O11—Ni2ⁱ	57.56 (11)
C18—C19—C22—C23	−9.8 (6)	O10—Ni1—O11—Ni2ⁱ	−23.29 (9)
C26—C22—C23—C24	−1.1 (7)	O9—Ni1—O11—Ni1ⁱ	−97.72 (11)
C19—C22—C23—C24	179.7 (4)	O11ⁱ—Ni1—O11—Ni1ⁱ	0.0
C22—C23—C24—N2	−0.8 (8)	N1—Ni1—O11—Ni1ⁱ	38.6 (5)
C23—C22—C26—C25	1.8 (7)	O4ⁱⁱ—Ni1—O11—Ni1ⁱ	179.46 (10)
C19—C22—C26—C25	−179.0 (4)	O10—Ni1—O11—Ni1ⁱ	98.61 (10)
N2—C25—C26—C22	−0.9 (8)

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

Poly[[tetrakis[µ-1,4-bis(pyridin-4-yl)benzene]bis[µ₅-3-(3,5-dicarboxylatophenoxy)phthalato]tetracobalt(II)] bis[1,4-bis(pyridin-4-yl)benzene]] (6) top

Crystal data top

[Co₄(C₁₆H₆O₉)₂(C₁₆H₁₂N₂)₄]·2C₁₆H₁₂N₂	F(000) = 4756
M_r = 2314.79	D_x = 1.262 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 31.055 (9) Å	Cell parameters from 3076 reflections
b = 23.792 (6) Å	θ = 2.2–21.5°
c = 16.540 (4) Å	µ = 0.60 mm⁻¹
β = 94.255 (5)°	T = 296 K
V = 12187 (6) Å³	Block, purple
Z = 4	0.26 × 0.22 × 0.18 mm

Data collection top

Bruker SMART APEX CCD area detector diffractometer	11440 reflections with I > 2σ(I)
phi and ω scans	R_int = 0.073
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	θ_max = 25.0°, θ_min = 1.1°
T_min = 0.859, T_max = 0.899	h = −36→36
50457 measured reflections	k = −28→27
21028 independent reflections	l = −19→17

Refinement top

Refinement on F²	24 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.106	H-atom parameters constrained
wR(F²) = 0.280	w = 1/[σ²(F_o²) + (0.1P)² + 95.P] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max < 0.001
21028 reflections	Δρ_max = 0.91 e Å⁻³
1447 parameters	Δρ_min = −0.76 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.2867 (2)	0.6826 (3)	0.8688 (4)	0.0209 (15)
C2	0.2902 (2)	0.6527 (3)	0.7890 (4)	0.0212 (15)
C3	0.2865 (2)	0.6833 (3)	0.7160 (4)	0.0254 (16)
H3	0.281353	0.721729	0.717179	0.030*
C4	0.2905 (2)	0.6571 (3)	0.6435 (4)	0.0246 (16)
C5	0.2972 (2)	0.6001 (3)	0.6410 (4)	0.0290 (17)
H5	0.299233	0.582098	0.591525	0.035*
C6	0.3009 (2)	0.5696 (3)	0.7118 (4)	0.0281 (17)
C7	0.2972 (2)	0.5954 (3)	0.7849 (5)	0.0302 (17)
H7	0.299401	0.574208	0.832230	0.036*
C8	0.3121 (3)	0.4786 (3)	0.7712 (4)	0.0270 (17)
C9	0.3509 (3)	0.4757 (4)	0.8164 (5)	0.040 (2)
H9	0.374211	0.497417	0.802898	0.048*
C10	0.3548 (3)	0.4397 (4)	0.8826 (5)	0.044 (2)
H10	0.380769	0.437865	0.914320	0.053*
C11	0.3205 (3)	0.4066 (3)	0.9018 (5)	0.041 (2)
H11	0.323650	0.382480	0.946097	0.049*
C12	0.2804 (2)	0.4089 (3)	0.8547 (4)	0.0283 (17)
C13	0.2762 (2)	0.4442 (3)	0.7869 (4)	0.0255 (16)
C14	0.2349 (3)	0.4504 (3)	0.7330 (4)	0.0296 (17)
C15	0.2087 (3)	0.9827 (3)	0.8290 (5)	0.0345 (19)
C16	0.1656 (3)	0.9818 (3)	0.7949 (6)	0.046 (2)
H16	0.145305	1.005904	0.814627	0.055*
C17	0.1537 (3)	0.9461 (3)	0.7340 (5)	0.043 (2)
H17	0.125137	0.945006	0.712614	0.052*
C18	0.1844 (3)	0.9110 (4)	0.7031 (5)	0.042 (2)
H18	0.176679	0.888227	0.658689	0.050*
C19	0.2266 (2)	0.9095 (3)	0.7380 (5)	0.0288 (17)
C20	0.2388 (2)	0.9469 (3)	0.8024 (5)	0.0290 (17)
C21	0.2843 (3)	0.9500 (4)	0.8415 (5)	0.042 (2)
C22	0.2580 (2)	0.8675 (3)	0.7059 (5)	0.0283 (17)
C23	0.2200 (2)	1.0734 (3)	0.8842 (5)	0.0319 (18)
C24	0.2156 (2)	0.3000 (3)	0.5185 (4)	0.0276 (17)
C25	0.2177 (3)	0.3353 (3)	0.4440 (4)	0.0312 (18)
C26	0.2174 (2)	0.3115 (3)	0.3691 (4)	0.0239 (16)
H26	0.215332	0.272668	0.363871	0.029*
C27	0.2201 (2)	0.3443 (3)	0.3012 (4)	0.0241 (16)
C28	0.2202 (2)	0.4016 (3)	0.3073 (4)	0.0289 (17)
H28	0.220446	0.423852	0.261035	0.035*
C29	0.2208 (3)	0.3941 (3)	0.4526 (5)	0.0318 (18)
H29	0.223295	0.410473	0.503787	0.038*
C30	0.1322 (3)	0.1371 (4)	0.5924 (5)	0.041 (2)
H30	0.146528	0.127692	0.641905	0.050*
C31	0.0881 (3)	0.1361 (4)	0.5866 (6)	0.055 (3)
H31	0.073201	0.126222	0.631231	0.066*
C32	0.0657 (3)	0.1498 (3)	0.5139 (5)	0.039 (2)
C33	0.0902 (3)	0.1621 (4)	0.4490 (6)	0.054 (3)
H33	0.076573	0.169691	0.398176	0.064*
C34	0.1342 (3)	0.1629 (4)	0.4602 (6)	0.049 (2)
H34	0.149795	0.172161	0.416220	0.059*
C35	0.0169 (3)	0.1531 (4)	0.5065 (6)	0.047 (2)
C36	−0.0064 (3)	0.1386 (4)	0.5721 (6)	0.055 (3)
H36	0.007959	0.125069	0.619453	0.066*
C37	−0.0511 (3)	0.1443 (5)	0.5671 (7)	0.063 (3)
H37	−0.066190	0.133150	0.610940	0.076*
C38	−0.0737 (3)	0.1659 (4)	0.4995 (6)	0.049 (2)
C39	−0.0511 (3)	0.1769 (5)	0.4326 (6)	0.067 (3)
H39	−0.065652	0.187447	0.383815	0.080*
C40	−0.0062 (3)	0.1721 (5)	0.4385 (7)	0.066 (3)
H40	0.008698	0.182403	0.394006	0.080*
C41	−0.1214 (3)	0.1746 (4)	0.4977 (6)	0.045 (2)
C42	−0.1465 (3)	0.1438 (4)	0.5469 (6)	0.056 (3)
H42	−0.134006	0.117731	0.583438	0.067*
C43	−0.1420 (3)	0.2128 (4)	0.4475 (6)	0.059 (3)
H43	−0.126219	0.235242	0.414411	0.070*
C44	0.2209 (2)	0.1840 (3)	0.7191 (4)	0.0241 (16)
C45	0.2446 (2)	0.1299 (3)	0.3807 (4)	0.0258 (16)
C46	0.3165 (3)	0.1752 (4)	0.6150 (6)	0.052 (2)
H46	0.305580	0.149438	0.650577	0.062*
C47	0.3609 (3)	0.1870 (5)	0.6215 (6)	0.060 (3)
H47	0.378688	0.167553	0.659648	0.072*
C48	0.3788 (3)	0.2257 (4)	0.5744 (6)	0.048 (2)
C49	0.3498 (3)	0.2507 (4)	0.5163 (6)	0.050 (2)
H49	0.359629	0.277263	0.480797	0.060*
C50	0.3068 (3)	0.2361 (4)	0.5116 (5)	0.046 (2)
H50	0.288430	0.253028	0.471805	0.056*
C51	0.4250 (3)	0.2409 (5)	0.5825 (6)	0.053 (3)
C52	0.4565 (3)	0.2041 (5)	0.6188 (9)	0.093 (5)
H52	0.448323	0.169063	0.637461	0.112*
C53	0.3127 (3)	0.2783 (4)	0.7729 (5)	0.043 (2)
H53	0.296021	0.251771	0.797764	0.051*
C54	0.3564 (3)	0.2796 (4)	0.7933 (6)	0.053 (2)
H54	0.368133	0.253673	0.830827	0.063*
C55	0.3832 (2)	0.3176 (4)	0.7604 (5)	0.040 (2)
C56	0.3639 (3)	0.3513 (4)	0.6990 (5)	0.042 (2)
H56	0.380484	0.375551	0.669947	0.051*
C57	0.3189 (3)	0.3478 (4)	0.6818 (5)	0.041 (2)
H57	0.306384	0.371218	0.641582	0.049*
C58	0.4297 (3)	0.3231 (5)	0.7869 (7)	0.062 (3)
C59	0.4537 (4)	0.3680 (7)	0.7720 (10)	0.116 (6)
H59	0.440556	0.397945	0.743655	0.139*
C60	0.4971 (4)	0.3720 (6)	0.7966 (10)	0.100 (5)
H60	0.512508	0.403644	0.782962	0.120*
C61	0.5173 (3)	0.3307 (6)	0.8400 (7)	0.074 (3)
C62	0.4946 (4)	0.2803 (6)	0.8493 (9)	0.098
H62	0.508539	0.249525	0.873989	0.117*
C63	0.4500 (5)	0.2763 (7)	0.8208 (9)	0.108
H63	0.435039	0.242686	0.825014	0.130*
C64	0.1304 (3)	0.2899 (3)	0.6499 (6)	0.042 (2)
H64	0.144972	0.261822	0.623936	0.050*
C65	0.0864 (3)	0.2918 (4)	0.6363 (6)	0.053 (3)
H65	0.072096	0.267033	0.600032	0.063*
C66	0.0633 (3)	0.3313 (4)	0.6774 (5)	0.040 (2)
C67	0.0870 (3)	0.3690 (4)	0.7248 (6)	0.050 (2)
H67	0.072902	0.397216	0.751341	0.060*
C68	0.1315 (3)	0.3658 (4)	0.7341 (5)	0.041 (2)
H68	0.146485	0.392384	0.766403	0.050*
C69	0.0149 (3)	0.3324 (4)	0.6679 (6)	0.045 (2)
C70	−0.0084 (3)	0.3825 (4)	0.6604 (6)	0.051 (3)
H70	0.006004	0.416824	0.662696	0.062*
C71	−0.0541 (3)	0.3811 (4)	0.6491 (7)	0.054 (3)
H71	−0.069391	0.414717	0.645402	0.065*
C72	−0.0081 (3)	0.2818 (4)	0.6625 (9)	0.081 (4)
H72	0.006379	0.247600	0.666269	0.098*
C73	0.1874 (3)	0.7184 (4)	1.0544 (6)	0.055 (3)
H73	0.200704	0.744962	1.089113	0.066*
C74	0.1915 (3)	0.6525 (4)	0.9595 (5)	0.043 (2)
H74	0.208054	0.631716	0.925698	0.051*
C75	0.3758 (3)	0.7021 (6)	1.0454 (7)	0.078 (3)
H75	0.365840	0.726807	1.004617	0.094*
C76	0.4203 (4)	0.7018 (6)	1.0717 (8)	0.090 (4)
H76	0.438926	0.726577	1.048213	0.108*
C77	0.4363 (3)	0.6662 (5)	1.1300 (6)	0.062 (3)
C78	0.4065 (3)	0.6314 (5)	1.1634 (7)	0.062 (3)
H78	0.415634	0.606315	1.204239	0.074*
C79	0.3630 (3)	0.6337 (5)	1.1366 (6)	0.058 (3)
H79	0.343907	0.610297	1.161186	0.069*
C80	0.1931 (2)	0.8606 (3)	0.9236 (5)	0.0332 (18)
H80	0.209073	0.884967	0.958019	0.040*
C81	0.1490 (3)	0.8654 (4)	0.9178 (5)	0.041 (2)
H81	0.135720	0.892802	0.947302	0.049*
C82	0.1243 (2)	0.8292 (4)	0.8678 (5)	0.040 (2)
C83	0.1470 (3)	0.7894 (4)	0.8263 (6)	0.047 (2)
H83	0.132093	0.763881	0.791983	0.056*
C84	0.1913 (3)	0.7875 (3)	0.8358 (6)	0.042 (2)
H84	0.205554	0.760022	0.808109	0.051*
C85	0.0758 (3)	0.8320 (3)	0.8562 (5)	0.039 (2)
C86	0.0532 (3)	0.7837 (4)	0.8486 (8)	0.078 (4)
H86	0.068325	0.749895	0.850917	0.093*
C87	0.3696 (3)	0.7761 (4)	0.8216 (5)	0.046 (2)
H87	0.351782	0.758814	0.781237	0.056*
C88	0.4135 (3)	0.7643 (5)	0.8261 (6)	0.059 (3)
H88	0.424531	0.740870	0.787548	0.070*
C89	0.4407 (3)	0.7866 (4)	0.8860 (6)	0.047 (2)
C90	0.4236 (3)	0.8243 (5)	0.9389 (7)	0.063 (3)
H90	0.441082	0.841887	0.979331	0.075*
C91	0.3793 (3)	0.8353 (4)	0.9298 (6)	0.056 (3)
H91	0.368299	0.860976	0.965271	0.067*
C92	0.4871 (3)	0.7700 (4)	0.8971 (6)	0.052 (2)
C93	0.5179 (3)	0.8080 (5)	0.9295 (8)	0.068 (3)
H93	0.509246	0.843686	0.944631	0.082*
C94	0.5610 (3)	0.7938 (5)	0.9394 (8)	0.078 (4)
H94	0.580976	0.819884	0.961003	0.094*
C95	0.5006 (3)	0.7201 (6)	0.8732 (9)	0.094 (5)
H95	0.480352	0.694874	0.850097	0.112*
C96	0.0972 (5)	0.6649 (6)	0.6769 (10)	0.094 (5)
H96	0.075256	0.690594	0.683766	0.113*
C97	0.0877 (4)	0.6181 (5)	0.6350 (8)	0.070 (3)
H97	0.059408	0.612744	0.613857	0.084*
C98	0.1173 (3)	0.5779 (4)	0.6218 (6)	0.052 (2)
C99	0.1602 (4)	0.5910 (5)	0.6546 (7)	0.067 (3)
H99	0.182648	0.565922	0.648101	0.080*
C100	0.1679 (5)	0.6398 (6)	0.6949 (10)	0.109 (5)
H100	0.196082	0.648363	0.713696	0.131*
C101	0.1064 (3)	0.5256 (4)	0.5746 (6)	0.051 (2)
C102	0.0691 (4)	0.5234 (5)	0.5239 (7)	0.072 (3)
H102	0.051168	0.554702	0.518335	0.087*
C103	0.0581 (3)	0.4742 (5)	0.4807 (7)	0.069 (3)
H103	0.032022	0.472232	0.449530	0.083*
C104	0.0861 (3)	0.4277 (4)	0.4840 (6)	0.057 (3)
C105	0.1239 (3)	0.4307 (5)	0.5348 (6)	0.058 (3)
H105	0.142958	0.400477	0.538280	0.069*
C106	0.1332 (3)	0.4788 (4)	0.5799 (6)	0.053 (2)
H106	0.158004	0.479731	0.614946	0.064*
C107	0.0752 (3)	0.3785 (4)	0.4331 (7)	0.062 (3)
C108	0.0334 (4)	0.3536 (6)	0.4314 (11)	0.106 (5)
H108	0.012070	0.368134	0.462059	0.128*
C109	0.0258 (4)	0.3076 (6)	0.3833 (12)	0.117 (6)
H109	−0.001390	0.291174	0.382907	0.140*
C110	0.0930 (5)	0.3072 (7)	0.3399 (10)	0.116 (6)
H110	0.113801	0.291417	0.309192	0.140*
C111	0.1039 (4)	0.3523 (5)	0.3856 (8)	0.082 (4)
H111	0.131775	0.366413	0.385267	0.098*
C112	−0.0064 (6)	0.9658 (7)	0.2483 (10)	0.110 (5)
H112	−0.012536	0.944173	0.202033	0.132*
C113	0.0360 (5)	0.9659 (6)	0.2802 (7)	0.084 (4)
H113	0.057000	0.945653	0.255467	0.101*
C114	0.0468 (4)	0.9976 (5)	0.3517 (7)	0.071 (3)
C115	0.0127 (5)	1.0254 (6)	0.3825 (8)	0.089 (4)
H115	0.016964	1.046351	0.429905	0.107*
C116	−0.0294 (5)	1.0217 (6)	0.3410 (10)	0.094 (4)
H116	−0.051658	1.041723	0.362429	0.113*
C117	0.0910 (4)	0.9991 (4)	0.3946 (6)	0.064 (3)
C118	0.1275 (4)	0.9979 (4)	0.3494 (6)	0.067 (3)
H118	0.124207	0.996999	0.293079	0.080*
C119	0.1692 (4)	0.9980 (4)	0.3892 (6)	0.063 (3)
H119	0.193049	0.996472	0.358445	0.076*
C120	0.1757 (3)	1.0002 (4)	0.4735 (6)	0.051 (3)
C121	0.1376 (4)	1.0023 (4)	0.5150 (6)	0.061 (3)
H121	0.140289	1.003850	0.571306	0.073*
C122	0.0973 (4)	1.0022 (4)	0.4770 (6)	0.058 (3)
H122	0.073490	1.004214	0.507765	0.070*
C123	0.2186 (4)	1.0000 (4)	0.5130 (6)	0.056 (3)
C124	0.2279 (4)	1.0221 (4)	0.5892 (6)	0.057 (3)
H124	0.205846	1.037149	0.617551	0.068*
C125	0.2689 (4)	1.0223 (4)	0.6232 (7)	0.063 (3)
H125	0.273634	1.038429	0.674291	0.075*
C126	0.2941 (4)	0.9764 (4)	0.5143 (7)	0.064 (3)
H126	0.316307	0.959355	0.488521	0.077*
C127	0.2539 (4)	0.9759 (4)	0.4768 (7)	0.061 (3)
H127	0.249410	0.959243	0.425930	0.074*
C128	0.2882 (2)	0.8076 (3)	1.0686 (5)	0.0239 (16)
Co1	0.28072 (3)	0.67898 (4)	1.04253 (6)	0.0269 (3)
Co2	0.22418 (3)	0.32340 (4)	0.70777 (6)	0.0251 (2)
Co3	0.28385 (3)	0.82297 (4)	0.87846 (6)	0.0253 (2)
Co4	0.22361 (3)	0.17560 (4)	0.54531 (6)	0.0248 (2)
N1	0.1562 (2)	0.1509 (3)	0.5313 (4)	0.0354 (16)
N2	0.2901 (2)	0.1992 (3)	0.5605 (4)	0.0360 (16)
N3	0.29304 (19)	0.3132 (3)	0.7191 (4)	0.0300 (14)
N4	0.1542 (2)	0.3258 (3)	0.6982 (4)	0.0359 (16)
N5	0.2115 (2)	0.6879 (3)	1.0097 (4)	0.0374 (16)
N6	0.3475 (2)	0.6673 (4)	1.0783 (4)	0.053 (2)
N7	0.3513 (2)	0.8117 (3)	0.8738 (4)	0.0367 (16)
N8	0.21425 (19)	0.8224 (3)	0.8818 (4)	0.0312 (14)
N10	0.0543 (4)	0.2843 (5)	0.3365 (9)	0.119 (5)
N11	0.3037 (3)	1.0008 (4)	0.5889 (6)	0.068 (3)
N12	−0.0388 (4)	0.9930 (6)	0.2765 (8)	0.094 (4)
N13	0.1363 (5)	0.6763 (5)	0.7089 (8)	0.103 (4)
O1	0.22473 (19)	0.3229 (2)	0.5855 (3)	0.0380 (13)
O2	0.20370 (17)	0.2497 (2)	0.5073 (3)	0.0317 (12)
O3	0.22443 (17)	0.1506 (2)	0.6594 (3)	0.0340 (13)
O4	0.21805 (17)	0.2355 (2)	0.7133 (3)	0.0341 (13)
O5	0.23934 (18)	0.1270 (2)	0.4552 (3)	0.0360 (13)
O6	0.22251 (18)	0.4089 (2)	0.6919 (3)	0.0411 (14)
O7	0.2173 (2)	0.4971 (2)	0.7309 (3)	0.0466 (15)
O8	0.30808 (19)	0.5131 (2)	0.7031 (3)	0.0376 (14)
O9	0.29034 (17)	0.6512 (2)	0.9324 (3)	0.0318 (12)
O10	0.28029 (17)	0.7338 (2)	0.8700 (3)	0.0344 (13)
O11	0.29756 (19)	0.9086 (2)	0.8834 (4)	0.0473 (16)
O12	0.3050 (2)	0.9934 (3)	0.8312 (5)	0.070 (2)
O13	0.27646 (17)	0.8323 (2)	0.7506 (3)	0.0347 (13)
O14	0.2832 (3)	0.7573 (3)	1.0760 (4)	0.0608 (19)
O15	0.2915 (2)	0.8315 (2)	1.0020 (3)	0.0464 (15)
O16	0.25982 (17)	0.6292 (2)	1.1299 (3)	0.0370 (13)
O17	0.22460 (17)	0.3383 (2)	0.8320 (3)	0.0368 (13)
O73	0.2201 (2)	1.0165 (2)	0.8950 (3)	0.0424 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.012 (3)	0.026 (4)	0.026 (4)	−0.002 (3)	0.011 (3)	−0.005 (3)
C2	0.024 (4)	0.022 (4)	0.017 (4)	−0.006 (3)	0.005 (3)	−0.003 (3)
C3	0.027 (4)	0.021 (4)	0.029 (4)	−0.001 (3)	0.008 (3)	0.006 (3)
C4	0.024 (4)	0.033 (4)	0.017 (4)	−0.002 (3)	0.002 (3)	−0.003 (3)
C5	0.030 (4)	0.034 (4)	0.025 (4)	−0.010 (3)	0.014 (3)	−0.005 (3)
C6	0.026 (4)	0.027 (4)	0.033 (4)	−0.003 (3)	0.013 (3)	−0.005 (3)
C7	0.025 (4)	0.034 (5)	0.031 (4)	−0.005 (3)	0.004 (3)	0.003 (3)
C8	0.045 (5)	0.008 (3)	0.028 (4)	0.002 (3)	0.003 (3)	0.004 (3)
C9	0.040 (5)	0.043 (5)	0.036 (5)	−0.007 (4)	0.009 (4)	0.002 (4)
C10	0.029 (5)	0.052 (6)	0.049 (5)	−0.012 (4)	−0.009 (4)	0.000 (4)
C11	0.042 (5)	0.035 (5)	0.044 (5)	0.008 (4)	−0.001 (4)	0.005 (4)
C12	0.027 (4)	0.034 (4)	0.025 (4)	−0.002 (3)	0.011 (3)	−0.004 (3)
C13	0.037 (4)	0.023 (4)	0.017 (4)	0.005 (3)	0.004 (3)	0.000 (3)
C14	0.040 (5)	0.026 (4)	0.023 (4)	−0.007 (4)	0.011 (3)	−0.005 (3)
C15	0.044 (5)	0.025 (4)	0.035 (5)	0.006 (4)	0.001 (4)	0.006 (3)
C16	0.043 (5)	0.025 (5)	0.072 (7)	0.016 (4)	0.025 (5)	0.010 (4)
C17	0.047 (5)	0.032 (5)	0.051 (6)	0.005 (4)	−0.002 (4)	0.011 (4)
C18	0.043 (5)	0.041 (5)	0.041 (5)	0.003 (4)	−0.006 (4)	−0.005 (4)
C19	0.026 (4)	0.025 (4)	0.036 (4)	−0.003 (3)	0.004 (3)	0.000 (3)
C20	0.025 (4)	0.023 (4)	0.040 (5)	0.003 (3)	0.009 (3)	0.010 (3)
C21	0.063 (6)	0.031 (5)	0.032 (5)	−0.013 (4)	0.003 (4)	0.001 (4)
C22	0.025 (4)	0.033 (4)	0.028 (4)	0.003 (3)	0.005 (3)	0.005 (3)
C23	0.032 (4)	0.027 (4)	0.037 (5)	0.007 (3)	0.011 (4)	0.005 (3)
C24	0.034 (4)	0.037 (5)	0.013 (4)	0.001 (3)	0.006 (3)	0.004 (3)
C25	0.038 (5)	0.038 (5)	0.019 (4)	0.004 (3)	0.005 (3)	0.004 (3)
C26	0.019 (4)	0.022 (4)	0.031 (4)	0.006 (3)	0.010 (3)	0.007 (3)
C27	0.029 (4)	0.033 (4)	0.010 (3)	−0.005 (3)	0.005 (3)	−0.002 (3)
C28	0.037 (4)	0.031 (4)	0.018 (4)	−0.007 (3)	−0.001 (3)	0.000 (3)
C29	0.040 (5)	0.029 (4)	0.028 (4)	−0.004 (3)	0.011 (3)	−0.010 (3)
C30	0.031 (5)	0.053 (6)	0.040 (5)	−0.011 (4)	0.002 (4)	0.007 (4)
C31	0.032 (5)	0.065 (7)	0.071 (7)	0.007 (4)	0.027 (5)	0.021 (5)
C32	0.042 (5)	0.035 (5)	0.043 (5)	−0.007 (4)	0.011 (4)	−0.011 (4)
C33	0.032 (5)	0.090 (8)	0.038 (5)	−0.012 (5)	−0.004 (4)	0.004 (5)
C34	0.032 (5)	0.060 (6)	0.057 (6)	−0.009 (4)	0.014 (4)	0.005 (5)
C35	0.035 (5)	0.053 (6)	0.051 (6)	−0.002 (4)	0.004 (4)	−0.010 (4)
C36	0.040 (5)	0.066 (7)	0.061 (6)	−0.003 (5)	0.017 (5)	0.008 (5)
C37	0.032 (5)	0.077 (8)	0.081 (8)	0.002 (5)	0.013 (5)	0.018 (6)
C38	0.021 (4)	0.069 (7)	0.057 (6)	−0.008 (4)	0.004 (4)	0.002 (5)
C39	0.029 (5)	0.121 (10)	0.048 (6)	0.008 (6)	−0.001 (4)	0.016 (6)
C40	0.045 (6)	0.091 (9)	0.064 (7)	−0.008 (6)	0.009 (5)	0.024 (6)
C41	0.029 (4)	0.053 (6)	0.053 (6)	−0.003 (4)	0.006 (4)	0.002 (5)
C42	0.034 (5)	0.052 (6)	0.080 (7)	−0.004 (4)	−0.004 (5)	0.021 (5)
C43	0.042 (6)	0.072 (7)	0.064 (7)	−0.018 (5)	0.014 (5)	0.021 (5)
C44	0.028 (4)	0.021 (4)	0.024 (4)	−0.008 (3)	0.004 (3)	0.000 (3)
C45	0.028 (4)	0.026 (4)	0.024 (4)	−0.005 (3)	0.003 (3)	−0.001 (3)
C46	0.031 (5)	0.069 (7)	0.056 (6)	−0.010 (5)	0.005 (4)	0.015 (5)
C47	0.030 (5)	0.092 (8)	0.058 (6)	−0.010 (5)	−0.005 (4)	0.007 (6)
C48	0.030 (5)	0.057 (6)	0.056 (6)	−0.013 (4)	0.003 (4)	−0.014 (5)
C49	0.035 (5)	0.060 (6)	0.054 (6)	−0.011 (4)	0.003 (4)	0.022 (5)
C50	0.034 (5)	0.061 (6)	0.045 (5)	−0.005 (4)	0.011 (4)	0.005 (4)
C51	0.032 (5)	0.070 (7)	0.057 (6)	−0.006 (5)	−0.006 (4)	−0.013 (5)
C52	0.038 (6)	0.071 (8)	0.168 (14)	−0.016 (6)	−0.007 (7)	0.029 (9)
C53	0.037 (5)	0.039 (5)	0.051 (6)	−0.002 (4)	0.001 (4)	0.002 (4)
C54	0.044 (6)	0.060 (6)	0.055 (6)	0.007 (5)	0.005 (5)	0.005 (5)
C55	0.022 (4)	0.054 (6)	0.045 (5)	0.004 (4)	0.008 (4)	−0.004 (4)
C56	0.034 (5)	0.048 (5)	0.046 (5)	−0.014 (4)	0.018 (4)	0.004 (4)
C57	0.031 (5)	0.046 (5)	0.046 (5)	−0.004 (4)	0.010 (4)	0.006 (4)
C58	0.029 (5)	0.079 (8)	0.079 (8)	0.002 (5)	0.008 (5)	0.010 (6)
C59	0.032 (6)	0.129 (13)	0.183 (17)	−0.022 (7)	−0.019 (8)	0.058 (12)
C60	0.035 (6)	0.102 (11)	0.160 (14)	−0.014 (6)	−0.017 (7)	0.062 (10)
C61	0.035 (6)	0.109 (10)	0.078 (8)	−0.029 (6)	0.013 (5)	0.010 (7)
C62	0.060	0.104	0.126	−0.010	−0.015	0.033
C63	0.089	0.112	0.121	−0.016	−0.011	0.030
C64	0.028 (4)	0.035 (5)	0.062 (6)	0.002 (4)	−0.002 (4)	−0.014 (4)
C65	0.034 (5)	0.044 (6)	0.079 (7)	−0.002 (4)	−0.005 (5)	−0.018 (5)
C66	0.029 (4)	0.040 (5)	0.050 (5)	0.004 (4)	0.006 (4)	−0.003 (4)
C67	0.031 (5)	0.055 (6)	0.064 (6)	0.017 (4)	0.004 (4)	−0.015 (5)
C68	0.037 (5)	0.040 (5)	0.046 (5)	0.000 (4)	−0.005 (4)	−0.022 (4)
C69	0.033 (5)	0.043 (6)	0.058 (6)	0.005 (4)	−0.006 (4)	−0.001 (4)
C70	0.028 (5)	0.030 (5)	0.095 (8)	−0.001 (4)	0.003 (5)	0.001 (5)
C71	0.039 (5)	0.027 (5)	0.097 (8)	−0.003 (4)	0.010 (5)	−0.001 (5)
C72	0.030 (5)	0.039 (6)	0.174 (13)	0.015 (5)	−0.002 (7)	−0.009 (7)
C73	0.040 (5)	0.063 (7)	0.064 (7)	0.002 (5)	0.018 (5)	−0.020 (5)
C74	0.027 (4)	0.051 (6)	0.052 (6)	0.002 (4)	0.006 (4)	−0.010 (4)
C75	0.049 (6)	0.118 (8)	0.067 (6)	−0.018 (5)	0.007 (5)	0.038 (6)
C76	0.050 (6)	0.120 (8)	0.102 (8)	−0.028 (6)	0.017 (6)	0.029 (7)
C77	0.032 (5)	0.105 (9)	0.047 (6)	−0.013 (5)	−0.001 (4)	0.015 (6)
C78	0.031 (5)	0.077 (8)	0.076 (8)	−0.001 (5)	−0.006 (5)	0.012 (6)
C79	0.027 (5)	0.079 (8)	0.066 (7)	−0.009 (5)	−0.002 (5)	0.014 (6)
C80	0.023 (4)	0.037 (5)	0.041 (5)	−0.004 (3)	0.009 (3)	−0.009 (4)
C81	0.031 (5)	0.047 (5)	0.046 (5)	0.009 (4)	0.012 (4)	0.003 (4)
C82	0.021 (4)	0.044 (5)	0.056 (6)	−0.002 (4)	0.003 (4)	−0.006 (4)
C83	0.042 (5)	0.048 (6)	0.052 (6)	−0.009 (4)	0.003 (4)	−0.005 (4)
C84	0.035 (5)	0.025 (4)	0.068 (6)	−0.002 (4)	0.013 (4)	−0.005 (4)
C85	0.033 (5)	0.033 (5)	0.053 (5)	−0.003 (4)	0.008 (4)	0.003 (4)
C86	0.028 (5)	0.035 (6)	0.170 (13)	−0.006 (4)	0.001 (6)	0.009 (7)
C87	0.025 (4)	0.074 (7)	0.042 (5)	−0.002 (4)	0.016 (4)	−0.007 (5)
C88	0.019 (4)	0.099 (8)	0.059 (6)	0.009 (5)	0.013 (4)	−0.013 (6)
C89	0.040 (5)	0.047 (6)	0.052 (6)	−0.002 (4)	−0.007 (4)	0.005 (4)
C90	0.015 (4)	0.075 (7)	0.095 (8)	−0.007 (4)	−0.018 (5)	−0.016 (6)
C91	0.028 (5)	0.081 (8)	0.060 (6)	0.002 (5)	0.005 (4)	−0.026 (5)
C92	0.019 (4)	0.066 (7)	0.070 (7)	−0.001 (4)	−0.008 (4)	0.001 (5)
C93	0.022 (5)	0.066 (7)	0.117 (10)	0.008 (5)	0.005 (5)	−0.014 (6)
C94	0.046 (6)	0.071 (8)	0.114 (10)	0.008 (6)	−0.018 (6)	−0.008 (7)
C95	0.030 (6)	0.088 (9)	0.159 (14)	0.013 (6)	−0.020 (7)	−0.041 (9)
C96	0.064 (9)	0.067 (9)	0.152 (14)	0.013 (7)	0.015 (9)	−0.014 (9)
C97	0.055 (7)	0.061 (7)	0.097 (9)	0.009 (6)	0.016 (6)	−0.005 (6)
C98	0.057 (6)	0.052 (6)	0.047 (6)	−0.001 (5)	0.009 (5)	0.004 (5)
C99	0.063 (7)	0.062 (7)	0.071 (8)	0.013 (6)	−0.016 (6)	0.009 (6)
C100	0.087 (10)	0.056 (8)	0.179 (17)	−0.021 (8)	−0.020 (10)	−0.021 (9)
C101	0.048 (6)	0.049 (6)	0.055 (6)	0.007 (5)	0.006 (5)	0.005 (5)
C102	0.070 (8)	0.066 (8)	0.078 (8)	0.010 (6)	−0.021 (6)	−0.003 (6)
C103	0.052 (6)	0.062 (7)	0.088 (8)	0.018 (5)	−0.024 (6)	−0.008 (6)
C104	0.044 (6)	0.060 (7)	0.064 (7)	0.005 (5)	−0.018 (5)	−0.014 (5)
C105	0.035 (5)	0.068 (7)	0.067 (7)	0.000 (5)	−0.009 (5)	−0.003 (5)
C106	0.038 (5)	0.055 (6)	0.066 (7)	0.006 (4)	−0.006 (5)	0.001 (5)
C107	0.046 (6)	0.059 (7)	0.077 (8)	0.007 (5)	−0.011 (5)	0.003 (6)
C108	0.058 (8)	0.073 (9)	0.187 (17)	−0.011 (7)	0.003 (9)	−0.019 (10)
C109	0.045 (7)	0.073 (10)	0.23 (2)	−0.006 (7)	−0.013 (10)	−0.018 (11)
C110	0.078 (10)	0.118 (13)	0.151 (15)	−0.004 (9)	−0.009 (10)	−0.070 (11)
C111	0.046 (7)	0.088 (9)	0.111 (11)	−0.002 (6)	0.001 (7)	−0.031 (8)
C112	0.130 (15)	0.098 (12)	0.093 (11)	0.015 (11)	−0.044 (11)	−0.009 (9)
C113	0.114 (11)	0.099 (10)	0.042 (7)	0.006 (8)	0.016 (7)	−0.001 (6)
C114	0.095 (9)	0.050 (7)	0.072 (8)	0.017 (6)	0.023 (7)	0.025 (6)
C115	0.125 (12)	0.082 (9)	0.059 (8)	0.022 (9)	−0.001 (8)	−0.004 (6)
C116	0.076 (10)	0.099 (11)	0.109 (12)	0.011 (8)	0.018 (9)	0.014 (9)
C117	0.094 (9)	0.048 (6)	0.050 (6)	0.007 (6)	0.002 (6)	0.007 (5)
C118	0.120 (10)	0.050 (6)	0.034 (5)	0.002 (6)	0.029 (6)	0.008 (4)
C119	0.079 (8)	0.056 (7)	0.054 (7)	0.004 (6)	−0.002 (6)	0.005 (5)
C120	0.077 (7)	0.027 (5)	0.052 (6)	0.006 (5)	0.024 (5)	0.005 (4)
C121	0.083 (8)	0.062 (7)	0.038 (6)	−0.003 (6)	0.009 (6)	−0.003 (5)
C122	0.081 (8)	0.050 (6)	0.046 (6)	0.006 (5)	0.028 (6)	−0.007 (5)
C123	0.073 (7)	0.034 (5)	0.063 (7)	0.005 (5)	0.019 (6)	0.009 (5)
C124	0.077 (8)	0.046 (6)	0.048 (6)	0.007 (5)	0.016 (6)	−0.009 (5)
C125	0.086 (9)	0.051 (6)	0.053 (6)	0.006 (6)	0.020 (6)	−0.001 (5)
C126	0.066 (8)	0.055 (7)	0.076 (8)	−0.008 (5)	0.043 (6)	−0.014 (6)
C127	0.071 (8)	0.037 (6)	0.081 (8)	−0.005 (5)	0.034 (6)	−0.006 (5)
C128	0.016 (3)	0.017 (4)	0.039 (5)	−0.005 (3)	0.004 (3)	−0.003 (3)
Co1	0.0269 (5)	0.0317 (6)	0.0225 (5)	−0.0044 (4)	0.0040 (4)	−0.0018 (4)
Co2	0.0230 (5)	0.0290 (6)	0.0233 (5)	0.0003 (4)	0.0017 (4)	0.0009 (4)
Co3	0.0214 (5)	0.0317 (6)	0.0232 (5)	0.0036 (4)	0.0038 (4)	0.0004 (4)
Co4	0.0249 (5)	0.0295 (6)	0.0207 (5)	−0.0002 (4)	0.0061 (4)	0.0002 (4)
N1	0.033 (4)	0.037 (4)	0.036 (4)	−0.004 (3)	0.001 (3)	0.000 (3)
N2	0.024 (3)	0.052 (4)	0.032 (4)	0.002 (3)	0.002 (3)	−0.003 (3)
N3	0.027 (3)	0.030 (4)	0.033 (4)	−0.002 (3)	0.003 (3)	−0.003 (3)
N4	0.028 (3)	0.039 (4)	0.043 (4)	0.002 (3)	0.011 (3)	0.000 (3)
N5	0.025 (3)	0.047 (4)	0.042 (4)	−0.003 (3)	0.006 (3)	−0.001 (3)
N6	0.019 (4)	0.102 (7)	0.041 (4)	−0.018 (4)	0.013 (3)	0.004 (4)
N7	0.031 (4)	0.043 (4)	0.036 (4)	0.004 (3)	−0.001 (3)	0.000 (3)
N8	0.028 (3)	0.033 (4)	0.033 (4)	−0.005 (3)	0.008 (3)	0.002 (3)
N10	0.092 (9)	0.095 (9)	0.162 (13)	0.023 (8)	−0.049 (9)	−0.069 (9)
N11	0.061 (6)	0.063 (6)	0.083 (7)	−0.006 (5)	0.023 (5)	0.004 (5)
N12	0.092 (9)	0.112 (10)	0.075 (8)	0.005 (8)	−0.014 (7)	0.020 (7)
N13	0.130 (11)	0.058 (7)	0.124 (10)	0.014 (7)	0.019 (9)	−0.022 (7)
O1	0.057 (4)	0.038 (3)	0.018 (3)	−0.007 (3)	−0.006 (2)	0.005 (2)
O2	0.046 (3)	0.027 (3)	0.022 (3)	0.005 (2)	0.001 (2)	0.007 (2)
O3	0.040 (3)	0.037 (3)	0.026 (3)	0.000 (2)	0.007 (2)	0.003 (2)
O4	0.046 (3)	0.032 (3)	0.024 (3)	−0.003 (2)	−0.004 (2)	−0.003 (2)
O5	0.049 (4)	0.039 (3)	0.021 (3)	0.004 (3)	0.006 (2)	−0.007 (2)
O6	0.037 (3)	0.036 (3)	0.048 (4)	−0.001 (3)	−0.016 (3)	0.001 (3)
O7	0.057 (4)	0.039 (4)	0.043 (4)	0.022 (3)	−0.010 (3)	−0.001 (3)
O8	0.065 (4)	0.018 (3)	0.032 (3)	0.000 (3)	0.017 (3)	0.004 (2)
O9	0.038 (3)	0.034 (3)	0.023 (3)	0.006 (2)	0.002 (2)	−0.001 (2)
O10	0.045 (3)	0.023 (3)	0.036 (3)	0.003 (2)	0.012 (3)	−0.003 (2)
O11	0.044 (4)	0.030 (3)	0.065 (4)	0.000 (3)	−0.016 (3)	0.009 (3)
O12	0.066 (5)	0.060 (5)	0.081 (5)	−0.024 (4)	−0.014 (4)	0.015 (4)
O13	0.037 (3)	0.036 (3)	0.033 (3)	0.014 (3)	0.010 (2)	0.003 (2)
O14	0.111 (6)	0.041 (4)	0.032 (3)	−0.014 (4)	0.014 (4)	−0.004 (3)
O15	0.066 (4)	0.046 (4)	0.028 (3)	0.007 (3)	0.008 (3)	0.001 (3)
O16	0.038 (3)	0.042 (3)	0.031 (3)	−0.005 (3)	0.004 (2)	0.000 (2)
O17	0.038 (3)	0.049 (4)	0.024 (3)	−0.017 (3)	0.001 (2)	−0.014 (2)
O73	0.083 (5)	0.022 (3)	0.023 (3)	0.006 (3)	0.008 (3)	0.000 (2)

Geometric parameters (Å, º) top

C1—O10	1.233 (8)	C69—C72	1.398 (13)
C1—O9	1.289 (8)	C70—C71	1.417 (12)
C1—C2	1.510 (9)	C70—H70	0.9300
C2—C7	1.383 (10)	C71—C85^v	1.348 (11)
C2—C3	1.406 (9)	C71—H71	0.9300
C3—C4	1.364 (10)	C72—C86^v	1.401 (13)
C3—H3	0.9300	C72—H72	0.9300
C4—C5	1.375 (10)	C73—N5	1.310 (10)
C4—C128ⁱ	1.494 (10)	C73—H73	0.9300
C5—C6	1.374 (10)	C74—N5	1.308 (10)
C5—H5	0.9300	C74—H74	0.9300
C6—C7	1.368 (10)	C75—N6	1.349 (12)
C6—O8	1.372 (9)	C75—C76	1.420 (15)
C7—H7	0.9300	C75—H75	0.9300
C8—C9	1.373 (11)	C76—C77	1.350 (15)
C8—O8	1.392 (8)	C76—H76	0.9300
C8—C13	1.421 (10)	C77—C78	1.387 (14)
C9—C10	1.388 (12)	C78—C79	1.389 (12)
C9—H9	0.9300	C78—H78	0.9300
C10—C11	1.382 (11)	C79—N6	1.317 (12)
C10—H10	0.9300	C79—H79	0.9300
C11—C12	1.419 (11)	C80—N8	1.342 (9)
C11—H11	0.9300	C80—C81	1.369 (11)
C12—C13	1.401 (10)	C80—H80	0.9300
C12—C45ⁱⁱ	1.530 (10)	C81—C82	1.385 (12)
C13—C14	1.513 (11)	C81—H81	0.9300
C14—O7	1.236 (9)	C82—C83	1.393 (12)
C14—O6	1.243 (9)	C82—C85	1.506 (11)
C15—C20	1.364 (10)	C83—C84	1.373 (12)
C15—O73	1.380 (9)	C83—H83	0.9300
C15—C16	1.412 (12)	C84—N8	1.303 (10)
C16—C17	1.347 (12)	C84—H84	0.9300
C16—H16	0.9300	C85—C86	1.349 (12)
C17—C18	1.395 (12)	C86—H86	0.9300
C17—H17	0.9300	C87—N7	1.362 (10)
C18—C19	1.390 (11)	C87—C88	1.391 (11)
C18—H18	0.9300	C87—H87	0.9300
C19—C20	1.418 (11)	C88—C89	1.362 (13)
C19—C22	1.519 (10)	C88—H88	0.9300
C20—C21	1.511 (12)	C89—C90	1.387 (14)
C21—O12	1.236 (10)	C89—C92	1.492 (12)
C21—O11	1.256 (10)	C90—C91	1.396 (12)
C22—O13	1.232 (9)	C90—H90	0.9300
C22—O16ⁱ	1.265 (9)	C91—N7	1.345 (11)
C23—O73	1.367 (9)	C91—H91	0.9300
C23—C29ⁱⁱⁱ	1.369 (11)	C92—C95	1.329 (14)
C23—C28ⁱⁱⁱ	1.405 (10)	C92—C93	1.395 (13)
C24—O1	1.249 (9)	C93—C94	1.379 (13)
C24—O2	1.262 (9)	C93—H93	0.9300
C24—C25	1.498 (10)	C94—H94	0.9300
C25—C26	1.361 (10)	C95—H95	0.9300
C25—C29	1.407 (10)	C96—N13	1.317 (17)
C26—C27	1.376 (9)	C96—C97	1.332 (16)
C26—H26	0.9300	C96—H96	0.9300
C27—C28	1.367 (10)	C97—C98	1.355 (14)
C27—C44^iv	1.518 (9)	C97—H97	0.9300
C28—H28	0.9300	C98—C99	1.434 (14)
C29—H29	0.9300	C98—C101	1.494 (13)
C30—N1	1.339 (10)	C99—C100	1.352 (16)
C30—C31	1.368 (12)	C99—H99	0.9300
C30—H30	0.9300	C100—N13	1.343 (17)
C31—C32	1.381 (13)	C100—H100	0.9300
C31—H31	0.9300	C101—C102	1.380 (14)
C32—C33	1.391 (12)	C101—C106	1.389 (12)
C32—C35	1.514 (12)	C102—C103	1.399 (15)
C33—C34	1.366 (12)	C102—H102	0.9300
C33—H33	0.9300	C103—C104	1.405 (13)
C34—N1	1.347 (11)	C103—H103	0.9300
C34—H34	0.9300	C104—C105	1.393 (12)
C35—C40	1.366 (13)	C104—C107	1.469 (14)
C35—C36	1.392 (12)	C105—C106	1.384 (13)
C36—C37	1.391 (13)	C105—H105	0.9300
C36—H36	0.9300	C106—H106	0.9300
C37—C38	1.376 (13)	C107—C111	1.381 (15)
C37—H37	0.9300	C107—C108	1.425 (16)
C38—C39	1.379 (13)	C108—C109	1.362 (19)
C38—C41	1.492 (11)	C108—H108	0.9300
C39—C40	1.394 (13)	C109—N10	1.340 (19)
C39—H39	0.9300	C109—H109	0.9300
C40—H40	0.9300	C110—N10	1.318 (18)
C41—C43	1.359 (13)	C110—C111	1.340 (16)
C41—C42	1.379 (12)	C110—H110	0.9300
C42—C74^v	1.408 (12)	C111—H111	0.9300
C42—H42	0.9300	C112—N12	1.311 (19)
C43—C73^v	1.413 (13)	C112—C113	1.380 (19)
C43—H43	0.9300	C112—H112	0.9300
C44—O4	1.231 (8)	C113—C114	1.423 (16)
C44—O3	1.278 (8)	C113—H113	0.9300
C45—O17^iv	1.237 (9)	C114—C115	1.377 (16)
C45—O5	1.256 (8)	C114—C117	1.498 (16)
C46—N2	1.306 (11)	C115—C116	1.435 (19)
C46—C47	1.405 (12)	C115—H115	0.9300
C46—H46	0.9300	C116—N12	1.282 (17)
C47—C48	1.352 (13)	C116—H116	0.9300
C47—H47	0.9300	C117—C122	1.365 (13)
C48—C49	1.399 (13)	C117—C118	1.404 (15)
C48—C51	1.475 (12)	C118—C119	1.407 (16)
C49—C50	1.377 (12)	C118—H118	0.9300
C49—H49	0.9300	C119—C120	1.394 (13)
C50—N2	1.325 (11)	C119—H119	0.9300
C50—H50	0.9300	C120—C121	1.410 (14)
C51—C94^vi	1.388 (15)	C120—C123	1.440 (14)
C51—C52	1.413 (15)	C121—C122	1.359 (14)
C52—C95^vi	1.383 (14)	C121—H121	0.9300
C52—H52	0.9300	C122—H122	0.9300
C53—N3	1.332 (10)	C123—C124	1.377 (14)
C53—C54	1.374 (12)	C123—C127	1.410 (13)
C53—H53	0.9300	C124—C125	1.353 (15)
C54—C55	1.370 (12)	C124—H124	0.9300
C54—H54	0.9300	C125—N11	1.356 (13)
C55—C56	1.394 (12)	C125—H125	0.9300
C55—C58	1.482 (12)	C126—C127	1.353 (15)
C56—C57	1.409 (11)	C126—N11	1.376 (13)
C56—H56	0.9300	C126—H126	0.9300
C57—N3	1.334 (10)	C127—H127	0.9300
C57—H57	0.9300	C128—O14	1.212 (9)
C58—C59	1.335 (16)	C128—O15	1.251 (9)
C58—C63	1.380 (17)	Co1—O14	1.944 (6)
C59—C60	1.382 (15)	Co1—O9	1.981 (5)
C59—H59	0.9300	Co1—O16	2.013 (5)
C60—C61	1.344 (16)	Co1—N6	2.133 (7)
C60—H60	0.9300	Co1—N5	2.189 (7)
C61—C62	1.404 (16)	Co2—O1	2.024 (5)
C61—C77^vii	1.491 (14)	Co2—O6	2.052 (6)
C62—C63	1.432 (17)	Co2—O17	2.084 (5)
C62—H62	0.9300	Co2—O4	2.103 (5)
C63—H63	0.9300	Co2—N3	2.147 (6)
C64—N4	1.353 (10)	Co2—N4	2.167 (6)
C64—C65	1.370 (12)	Co3—O15	2.049 (6)
C64—H64	0.9300	Co3—O11	2.081 (6)
C65—C66	1.389 (12)	Co3—N7	2.119 (7)
C65—H65	0.9300	Co3—O13	2.122 (5)
C66—C67	1.369 (12)	Co3—O10	2.129 (5)
C66—C69	1.502 (12)	Co3—N8	2.167 (6)
C67—C68	1.382 (11)	Co4—O2	1.956 (5)
C67—H67	0.9300	Co4—O3	1.977 (5)
C68—N4	1.347 (10)	Co4—O5	1.977 (5)
C68—H68	0.9300	Co4—N2	2.136 (6)
C69—C70	1.395 (12)	Co4—N1	2.169 (7)

O10—C1—O9	124.3 (6)	C81—C80—H80	118.5
O10—C1—C2	120.1 (6)	C80—C81—C82	119.8 (8)
O9—C1—C2	115.6 (6)	C80—C81—H81	120.1
C7—C2—C3	118.0 (6)	C82—C81—H81	120.1
C7—C2—C1	122.0 (6)	C81—C82—C83	116.0 (7)
C3—C2—C1	120.0 (6)	C81—C82—C85	123.6 (8)
C4—C3—C2	120.9 (7)	C83—C82—C85	120.4 (8)
C4—C3—H3	119.6	C84—C83—C82	120.3 (8)
C2—C3—H3	119.6	C84—C83—H83	119.9
C3—C4—C5	120.0 (7)	C82—C83—H83	119.9
C3—C4—C128ⁱ	118.1 (7)	N8—C84—C83	123.2 (8)
C5—C4—C128ⁱ	121.9 (6)	N8—C84—H84	118.4
C4—C5—C6	119.9 (7)	C83—C84—H84	118.4
C4—C5—H5	120.0	C71^viii—C85—C86	118.6 (9)
C6—C5—H5	120.0	C71^viii—C85—C82	122.5 (8)
C7—C6—O8	123.8 (7)	C86—C85—C82	118.8 (8)
C7—C6—C5	120.6 (7)	C85—C86—C72^viii	123.1 (9)
O8—C6—C5	115.6 (6)	C85—C86—H86	118.4
C6—C7—C2	120.7 (7)	C72^viii—C86—H86	118.4
C6—C7—H7	119.7	N7—C87—C88	123.0 (9)
C2—C7—H7	119.7	N7—C87—H87	118.5
C9—C8—O8	119.4 (7)	C88—C87—H87	118.5
C9—C8—C13	122.8 (7)	C89—C88—C87	120.9 (9)
O8—C8—C13	117.6 (7)	C89—C88—H88	119.6
C8—C9—C10	118.8 (7)	C87—C88—H88	119.6
C8—C9—H9	120.6	C88—C89—C90	117.7 (8)
C10—C9—H9	120.6	C88—C89—C92	121.8 (9)
C11—C10—C9	120.6 (8)	C90—C89—C92	120.5 (8)
C11—C10—H10	119.7	C89—C90—C91	118.4 (9)
C9—C10—H10	119.7	C89—C90—H90	120.8
C10—C11—C12	120.8 (8)	C91—C90—H90	120.8
C10—C11—H11	119.6	N7—C91—C90	125.2 (9)
C12—C11—H11	119.6	N7—C91—H91	117.4
C13—C12—C11	119.2 (7)	C90—C91—H91	117.4
C13—C12—C45ⁱⁱ	124.1 (7)	C95—C92—C93	118.2 (9)
C11—C12—C45ⁱⁱ	116.7 (7)	C95—C92—C89	121.5 (9)
C12—C13—C8	117.6 (7)	C93—C92—C89	120.2 (9)
C12—C13—C14	123.7 (7)	C94—C93—C92	121.2 (10)
C8—C13—C14	118.6 (6)	C94—C93—H93	119.4
O7—C14—O6	125.4 (8)	C92—C93—H93	119.4
O7—C14—C13	117.2 (7)	C93—C94—C51^ix	120.8 (11)
O6—C14—C13	117.3 (7)	C93—C94—H94	119.6
C20—C15—O73	118.4 (7)	C51^ix—C94—H94	119.6
C20—C15—C16	120.9 (8)	C92—C95—C52^ix	122.7 (11)
O73—C15—C16	120.5 (7)	C92—C95—H95	118.7
C17—C16—C15	120.6 (8)	C52^ix—C95—H95	118.7
C17—C16—H16	119.7	N13—C96—C97	123.0 (12)
C15—C16—H16	119.7	N13—C96—H96	118.5
C16—C17—C18	119.6 (8)	C97—C96—H96	118.5
C16—C17—H17	120.2	C96—C97—C98	123.1 (12)
C18—C17—H17	120.2	C96—C97—H97	118.5
C19—C18—C17	120.8 (8)	C98—C97—H97	118.5
C19—C18—H18	119.6	C97—C98—C99	114.1 (10)
C17—C18—H18	119.6	C97—C98—C101	122.8 (10)
C18—C19—C20	119.2 (7)	C99—C98—C101	123.1 (9)
C18—C19—C22	118.7 (7)	C100—C99—C98	119.9 (11)
C20—C19—C22	122.1 (7)	C100—C99—H99	120.0
C15—C20—C19	118.8 (7)	C98—C99—H99	120.0
C15—C20—C21	118.2 (7)	N13—C100—C99	122.4 (13)
C19—C20—C21	122.9 (7)	N13—C100—H100	118.8
O12—C21—O11	125.4 (9)	C99—C100—H100	118.8
O12—C21—C20	117.5 (8)	C102—C101—C106	118.7 (10)
O11—C21—C20	117.2 (7)	C102—C101—C98	119.8 (9)
O13—C22—O16ⁱ	125.8 (7)	C106—C101—C98	121.5 (9)
O13—C22—C19	121.4 (7)	C101—C102—C103	120.2 (10)
O16ⁱ—C22—C19	112.6 (6)	C101—C102—H102	119.9
O73—C23—C29ⁱⁱⁱ	116.9 (7)	C103—C102—H102	119.9
O73—C23—C28ⁱⁱⁱ	122.5 (7)	C102—C103—C104	120.8 (10)
C29ⁱⁱⁱ—C23—C28ⁱⁱⁱ	120.6 (7)	C102—C103—H103	119.6
O1—C24—O2	126.2 (6)	C104—C103—H103	119.6
O1—C24—C25	117.6 (7)	C105—C104—C103	118.3 (9)
O2—C24—C25	116.2 (6)	C105—C104—C107	122.4 (9)
C26—C25—C29	120.1 (7)	C103—C104—C107	119.3 (9)
C26—C25—C24	121.1 (7)	C106—C105—C104	119.9 (9)
C29—C25—C24	118.8 (7)	C106—C105—H105	120.1
C25—C26—C27	120.6 (7)	C104—C105—H105	120.1
C25—C26—H26	119.7	C105—C106—C101	122.0 (9)
C27—C26—H26	119.7	C105—C106—H106	119.0
C28—C27—C26	120.4 (6)	C101—C106—H106	119.0
C28—C27—C44^iv	120.6 (6)	C111—C107—C108	115.2 (11)
C26—C27—C44^iv	119.0 (7)	C111—C107—C104	123.7 (10)
C27—C28—C23ⁱ	119.2 (7)	C108—C107—C104	121.1 (11)
C27—C28—H28	120.4	C109—C108—C107	117.6 (14)
C23ⁱ—C28—H28	120.4	C109—C108—H108	121.2
C23ⁱ—C29—C25	118.7 (7)	C107—C108—H108	121.2
C23ⁱ—C29—H29	120.7	N10—C109—C108	125.3 (13)
C25—C29—H29	120.7	N10—C109—H109	117.4
N1—C30—C31	124.2 (8)	C108—C109—H109	117.4
N1—C30—H30	117.9	N10—C110—C111	123.1 (14)
C31—C30—H30	117.9	N10—C110—H110	118.4
C30—C31—C32	119.5 (8)	C111—C110—H110	118.4
C30—C31—H31	120.2	C110—C111—C107	122.4 (12)
C32—C31—H31	120.2	C110—C111—H111	118.8
C31—C32—C33	117.0 (8)	C107—C111—H111	118.8
C31—C32—C35	121.2 (8)	N12—C112—C113	126.7 (15)
C33—C32—C35	121.8 (8)	N12—C112—H112	116.6
C34—C33—C32	119.7 (9)	C113—C112—H112	116.6
C34—C33—H33	120.1	C112—C113—C114	118.6 (13)
C32—C33—H33	120.1	C112—C113—H113	120.7
N1—C34—C33	123.6 (8)	C114—C113—H113	120.7
N1—C34—H34	118.2	C115—C114—C113	114.9 (13)
C33—C34—H34	118.2	C115—C114—C117	121.1 (12)
C40—C35—C36	116.9 (9)	C113—C114—C117	123.8 (11)
C40—C35—C32	123.1 (9)	C114—C115—C116	119.5 (13)
C36—C35—C32	120.0 (9)	C114—C115—H115	120.2
C37—C36—C35	120.3 (10)	C116—C115—H115	120.2
C37—C36—H36	119.8	N12—C116—C115	124.9 (14)
C35—C36—H36	119.8	N12—C116—H116	117.5
C38—C37—C36	122.1 (9)	C115—C116—H116	117.5
C38—C37—H37	119.0	C122—C117—C118	118.1 (11)
C36—C37—H37	119.0	C122—C117—C114	122.1 (11)
C37—C38—C39	117.6 (8)	C118—C117—C114	119.8 (10)
C37—C38—C41	120.8 (8)	C117—C118—C119	120.1 (10)
C39—C38—C41	121.5 (9)	C117—C118—H118	119.9
C38—C39—C40	119.7 (9)	C119—C118—H118	119.9
C38—C39—H39	120.2	C120—C119—C118	121.8 (11)
C40—C39—H39	120.2	C120—C119—H119	119.1
C35—C40—C39	123.1 (9)	C118—C119—H119	119.1
C35—C40—H40	118.5	C119—C120—C121	115.1 (10)
C39—C40—H40	118.5	C119—C120—C123	120.9 (9)
C43—C41—C42	117.0 (8)	C121—C120—C123	124.0 (9)
C43—C41—C38	121.7 (8)	C122—C121—C120	123.4 (10)
C42—C41—C38	121.3 (9)	C122—C121—H121	118.3
C41—C42—C74^v	118.6 (9)	C120—C121—H121	118.3
C41—C42—H42	120.7	C121—C122—C117	121.4 (10)
C74^v—C42—H42	120.7	C121—C122—H122	119.3
C41—C43—C73^v	120.1 (8)	C117—C122—H122	119.3
C41—C43—H43	120.0	C124—C123—C127	115.3 (11)
C73^v—C43—H43	120.0	C124—C123—C120	122.7 (9)
O4—C44—O3	124.5 (7)	C127—C123—C120	122.1 (10)
O4—C44—C27ⁱⁱ	120.4 (6)	C125—C124—C123	120.6 (10)
O3—C44—C27ⁱⁱ	115.1 (6)	C125—C124—H124	119.7
O17^iv—C45—O5	125.3 (7)	C123—C124—H124	119.7
O17^iv—C45—C12^iv	121.7 (6)	C124—C125—N11	125.3 (10)
O5—C45—C12^iv	113.0 (6)	C124—C125—H125	117.3
N2—C46—C47	121.9 (9)	N11—C125—H125	117.3
N2—C46—H46	119.1	C127—C126—N11	123.0 (9)
C47—C46—H46	119.1	C127—C126—H126	118.5
C48—C47—C46	122.4 (9)	N11—C126—H126	118.5
C48—C47—H47	118.8	C126—C127—C123	121.5 (11)
C46—C47—H47	118.8	C126—C127—H127	119.3
C47—C48—C49	114.5 (8)	C123—C127—H127	119.3
C47—C48—C51	123.5 (9)	O14—C128—O15	123.9 (7)
C49—C48—C51	122.0 (9)	O14—C128—C4ⁱⁱⁱ	118.0 (7)
C50—C49—C48	120.3 (8)	O15—C128—C4ⁱⁱⁱ	118.2 (6)
C50—C49—H49	119.9	O14—Co1—O9	125.1 (2)
C48—C49—H49	119.9	O14—Co1—O16	111.6 (2)
N2—C50—C49	123.7 (9)	O9—Co1—O16	122.9 (2)
N2—C50—H50	118.2	O14—Co1—N6	91.6 (3)
C49—C50—H50	118.2	O9—Co1—N6	90.1 (3)
C94^vi—C51—C52	116.9 (9)	O16—Co1—N6	94.8 (3)
C94^vi—C51—C48	121.2 (9)	O14—Co1—N5	89.7 (3)
C52—C51—C48	121.7 (10)	O9—Co1—N5	91.0 (2)
C95^vi—C52—C51	120.1 (11)	O16—Co1—N5	82.6 (2)
C95^vi—C52—H52	119.9	N6—Co1—N5	177.4 (3)
C51—C52—H52	119.9	O1—Co2—O6	83.1 (2)
N3—C53—C54	123.0 (8)	O1—Co2—O17	170.5 (2)
N3—C53—H53	118.5	O6—Co2—O17	87.4 (2)
C54—C53—H53	118.5	O1—Co2—O4	92.6 (2)
C55—C54—C53	122.4 (9)	O6—Co2—O4	172.1 (2)
C55—C54—H54	118.8	O17—Co2—O4	96.9 (2)
C53—C54—H54	118.8	O1—Co2—N3	90.3 (2)
C54—C55—C56	115.3 (8)	O6—Co2—N3	98.0 (2)
C54—C55—C58	123.3 (9)	O17—Co2—N3	90.0 (2)
C56—C55—C58	121.3 (8)	O4—Co2—N3	88.7 (2)
C55—C56—C57	118.7 (7)	O1—Co2—N4	90.6 (2)
C55—C56—H56	120.7	O6—Co2—N4	87.1 (2)
C57—C56—H56	120.7	O17—Co2—N4	90.0 (2)
N3—C57—C56	124.4 (8)	O4—Co2—N4	86.3 (2)
N3—C57—H57	117.8	N3—Co2—N4	175.0 (2)
C56—C57—H57	117.8	O15—Co3—O11	81.7 (2)
C59—C58—C63	118.4 (11)	O15—Co3—N7	90.4 (3)
C59—C58—C55	124.1 (10)	O11—Co3—N7	85.8 (2)
C63—C58—C55	117.0 (11)	O15—Co3—O13	168.3 (2)
C58—C59—C60	123.1 (13)	O11—Co3—O13	86.8 (2)
C58—C59—H59	118.5	N7—Co3—O13	90.6 (2)
C60—C59—H59	118.5	O15—Co3—O10	99.5 (2)
C61—C60—C59	120.9 (12)	O11—Co3—O10	171.0 (2)
C61—C60—H60	119.5	N7—Co3—O10	85.3 (2)
C59—C60—H60	119.5	O13—Co3—O10	92.1 (2)
C60—C61—C62	117.6 (11)	O15—Co3—N8	90.9 (2)
C60—C61—C77^vii	122.9 (10)	O11—Co3—N8	101.9 (2)
C62—C61—C77^vii	119.1 (12)	N7—Co3—N8	172.3 (3)
C61—C62—C63	120.1 (13)	O13—Co3—N8	89.5 (2)
C61—C62—H62	119.9	O10—Co3—N8	87.1 (2)
C63—C62—H62	119.9	O2—Co4—O3	124.0 (2)
C58—C63—C62	118.8 (13)	O2—Co4—O5	112.0 (2)
C58—C63—H63	120.6	O3—Co4—O5	123.9 (2)
C62—C63—H63	120.6	O2—Co4—N2	94.6 (3)
N4—C64—C65	124.9 (8)	O3—Co4—N2	91.3 (2)
N4—C64—H64	117.6	O5—Co4—N2	87.2 (2)
C65—C64—H64	117.6	O2—Co4—N1	86.0 (2)
C64—C65—C66	119.1 (8)	O3—Co4—N1	88.0 (2)
C64—C65—H65	120.4	O5—Co4—N1	93.0 (2)
C66—C65—H65	120.4	N2—Co4—N1	179.2 (3)
C67—C66—C65	116.6 (8)	C30—N1—C34	115.8 (7)
C67—C66—C69	122.7 (8)	C30—N1—Co4	124.9 (6)
C65—C66—C69	120.6 (8)	C34—N1—Co4	117.4 (5)
C66—C67—C68	121.3 (8)	C46—N2—C50	117.2 (7)
C66—C67—H67	119.4	C46—N2—Co4	121.2 (6)
C68—C67—H67	119.4	C50—N2—Co4	121.4 (6)
N4—C68—C67	122.8 (8)	C57—N3—C53	115.7 (7)
N4—C68—H68	118.6	C57—N3—Co2	121.4 (6)
C67—C68—H68	118.6	C53—N3—Co2	122.2 (5)
C70—C69—C72	118.2 (8)	C68—N4—C64	115.1 (7)
C70—C69—C66	122.2 (8)	C68—N4—Co2	122.8 (5)
C72—C69—C66	119.6 (8)	C64—N4—Co2	121.9 (5)
C69—C70—C71	119.9 (8)	C74—N5—C73	116.8 (8)
C69—C70—H70	120.1	C74—N5—Co1	120.4 (6)
C71—C70—H70	120.1	C73—N5—Co1	120.4 (6)
C85^v—C71—C70	121.3 (8)	C79—N6—C75	117.0 (8)
C85^v—C71—H71	119.3	C79—N6—Co1	125.3 (6)
C70—C71—H71	119.3	C75—N6—Co1	117.2 (7)
C69—C72—C86^v	118.8 (9)	C91—N7—C87	114.7 (7)
C69—C72—H72	120.6	C91—N7—Co3	120.8 (6)
C86^v—C72—H72	120.6	C87—N7—Co3	124.1 (6)
N5—C73—C43^viii	123.1 (9)	C84—N8—C80	117.7 (7)
N5—C73—H73	118.5	C84—N8—Co3	119.5 (5)
C43^viii—C73—H73	118.5	C80—N8—Co3	122.5 (5)
N5—C74—C42^viii	124.4 (8)	C110—N10—C109	116.3 (12)
N5—C74—H74	117.8	C125—N11—C126	114.1 (10)
C42^viii—C74—H74	117.8	C116—N12—C112	115.3 (13)
N6—C75—C76	121.5 (10)	C96—N13—C100	117.4 (12)
N6—C75—H75	119.3	C24—O1—Co2	150.5 (5)
C76—C75—H75	119.3	C24—O2—Co4	136.5 (5)
C77—C76—C75	121.3 (10)	C44—O3—Co4	123.8 (5)
C77—C76—H76	119.3	C44—O4—Co2	170.6 (5)
C75—C76—H76	119.3	C45—O5—Co4	139.8 (5)
C76—C77—C78	116.0 (9)	C14—O6—Co2	135.5 (5)
C76—C77—C61^vii	120.1 (10)	C6—O8—C8	120.0 (6)
C78—C77—C61^vii	123.7 (10)	C1—O9—Co1	123.2 (4)
C77—C78—C79	120.7 (10)	C1—O10—Co3	167.6 (5)
C77—C78—H78	119.6	C21—O11—Co3	133.4 (6)
C79—C78—H78	119.6	C22—O13—Co3	132.9 (5)
N6—C79—C78	123.5 (9)	C128—O14—Co1	156.8 (6)
N6—C79—H79	118.3	C128—O15—Co3	145.2 (5)
C78—C79—H79	118.3	C22ⁱⁱⁱ—O16—Co1	135.8 (5)
N8—C80—C81	123.0 (8)	C45ⁱⁱ—O17—Co2	135.4 (5)
N8—C80—H80	118.5	C23—O73—C15	118.4 (6)

O10—C1—C2—C7	−179.7 (6)	C85—C82—C83—C84	178.8 (8)
O9—C1—C2—C7	−0.3 (9)	C82—C83—C84—N8	−1.1 (14)
O10—C1—C2—C3	0.4 (10)	C81—C82—C85—C71^viii	39.2 (14)
O9—C1—C2—C3	179.8 (6)	C83—C82—C85—C71^viii	−139.7 (10)
C7—C2—C3—C4	−1.1 (10)	C81—C82—C85—C86	−142.6 (11)
C1—C2—C3—C4	178.7 (6)	C83—C82—C85—C86	38.5 (14)
C2—C3—C4—C5	1.5 (11)	C71^viii—C85—C86—C72^viii	−1.7 (19)
C2—C3—C4—C128ⁱ	−177.3 (6)	C82—C85—C86—C72^viii	−179.9 (12)
C3—C4—C5—C6	−1.5 (11)	N7—C87—C88—C89	2.7 (16)
C128ⁱ—C4—C5—C6	177.3 (7)	C87—C88—C89—C90	−4.3 (16)
C4—C5—C6—C7	1.1 (11)	C87—C88—C89—C92	173.5 (9)
C4—C5—C6—O8	−179.2 (6)	C88—C89—C90—C91	2.7 (16)
O8—C6—C7—C2	179.5 (7)	C92—C89—C90—C91	−175.1 (10)
C5—C6—C7—C2	−0.8 (11)	C89—C90—C91—N7	0.7 (17)
C3—C2—C7—C6	0.8 (10)	C88—C89—C92—C95	−26.4 (17)
C1—C2—C7—C6	−179.1 (6)	C90—C89—C92—C95	151.4 (12)
O8—C8—C9—C10	−178.0 (7)	C88—C89—C92—C93	150.3 (11)
C13—C8—C9—C10	−3.1 (12)	C90—C89—C92—C93	−31.9 (15)
C8—C9—C10—C11	1.2 (13)	C95—C92—C93—C94	−2.5 (19)
C9—C10—C11—C12	−0.5 (13)	C89—C92—C93—C94	−179.2 (11)
C10—C11—C12—C13	1.6 (12)	C92—C93—C94—C51^ix	0 (2)
C10—C11—C12—C45ⁱⁱ	179.4 (7)	C93—C92—C95—C52^ix	2 (2)
C11—C12—C13—C8	−3.2 (10)	C89—C92—C95—C52^ix	178.6 (13)
C45ⁱⁱ—C12—C13—C8	179.1 (6)	N13—C96—C97—C98	0 (2)
C11—C12—C13—C14	−179.4 (7)	C96—C97—C98—C99	−2.0 (18)
C45ⁱⁱ—C12—C13—C14	2.9 (11)	C96—C97—C98—C101	−179.7 (12)
C9—C8—C13—C12	4.1 (11)	C97—C98—C99—C100	0.5 (17)
O8—C8—C13—C12	179.1 (6)	C101—C98—C99—C100	178.2 (12)
C9—C8—C13—C14	−179.5 (7)	C98—C99—C100—N13	3 (2)
O8—C8—C13—C14	−4.5 (9)	C97—C98—C101—C102	18.1 (15)
C12—C13—C14—O7	115.9 (8)	C99—C98—C101—C102	−159.4 (11)
C8—C13—C14—O7	−60.2 (9)	C97—C98—C101—C106	−162.2 (10)
C12—C13—C14—O6	−67.1 (10)	C99—C98—C101—C106	20.3 (15)
C8—C13—C14—O6	116.8 (8)	C106—C101—C102—C103	1.7 (17)
C20—C15—C16—C17	−1.5 (12)	C98—C101—C102—C103	−178.6 (10)
O73—C15—C16—C17	−175.5 (7)	C101—C102—C103—C104	−4.2 (19)
C15—C16—C17—C18	−1.6 (13)	C102—C103—C104—C105	3.5 (18)
C16—C17—C18—C19	4.4 (13)	C102—C103—C104—C107	−175.3 (11)
C17—C18—C19—C20	−4.0 (12)	C103—C104—C105—C106	−0.3 (16)
C17—C18—C19—C22	175.7 (7)	C107—C104—C105—C106	178.4 (10)
O73—C15—C20—C19	176.0 (6)	C104—C105—C106—C101	−2.2 (16)
C16—C15—C20—C19	1.9 (11)	C102—C101—C106—C105	1.5 (16)
O73—C15—C20—C21	−5.7 (11)	C98—C101—C106—C105	−178.2 (9)
C16—C15—C20—C21	−179.8 (7)	C105—C104—C107—C111	−46.7 (18)
C18—C19—C20—C15	0.9 (11)	C103—C104—C107—C111	132.0 (13)
C22—C19—C20—C15	−178.9 (7)	C105—C104—C107—C108	131.8 (13)
C18—C19—C20—C21	−177.4 (7)	C103—C104—C107—C108	−49.5 (17)
C22—C19—C20—C21	2.9 (11)	C111—C107—C108—C109	−1 (2)
C15—C20—C21—O12	−65.9 (11)	C104—C107—C108—C109	−179.4 (13)
C19—C20—C21—O12	112.4 (9)	C107—C108—C109—N10	−1 (3)
C15—C20—C21—O11	112.7 (9)	N10—C110—C111—C107	0 (3)
C19—C20—C21—O11	−69.1 (11)	C108—C107—C111—C110	1 (2)
C18—C19—C22—O13	−122.2 (9)	C104—C107—C111—C110	179.7 (14)
C20—C19—C22—O13	57.5 (10)	N12—C112—C113—C114	1 (2)
C18—C19—C22—O16ⁱ	53.0 (10)	C112—C113—C114—C115	0.3 (18)
C20—C19—C22—O16ⁱ	−127.3 (8)	C112—C113—C114—C117	177.0 (12)
O1—C24—C25—C26	165.9 (7)	C113—C114—C115—C116	−1.5 (18)
O2—C24—C25—C26	−15.6 (11)	C117—C114—C115—C116	−178.3 (11)
O1—C24—C25—C29	−13.2 (11)	C114—C115—C116—N12	2 (2)
O2—C24—C25—C29	165.3 (7)	C115—C114—C117—C122	32.2 (16)
C29—C25—C26—C27	0.1 (11)	C113—C114—C117—C122	−144.2 (11)
C24—C25—C26—C27	−179.0 (7)	C115—C114—C117—C118	−147.0 (11)
C25—C26—C27—C28	−4.4 (11)	C113—C114—C117—C118	36.5 (16)
C25—C26—C27—C44^iv	178.2 (7)	C122—C117—C118—C119	2.1 (15)
C26—C27—C28—C23ⁱ	3.5 (11)	C114—C117—C118—C119	−178.6 (9)
C44^iv—C27—C28—C23ⁱ	−179.1 (7)	C117—C118—C119—C120	−1.1 (16)
C26—C25—C29—C23ⁱ	5.0 (11)	C118—C119—C120—C121	0.1 (14)
C24—C25—C29—C23ⁱ	−175.9 (7)	C118—C119—C120—C123	179.7 (9)
N1—C30—C31—C32	0.1 (15)	C119—C120—C121—C122	0.0 (15)
C30—C31—C32—C33	2.4 (14)	C123—C120—C121—C122	−179.6 (9)
C30—C31—C32—C35	−175.8 (8)	C120—C121—C122—C117	1.0 (16)
C31—C32—C33—C34	−3.2 (14)	C118—C117—C122—C121	−2.1 (15)
C35—C32—C33—C34	174.9 (9)	C114—C117—C122—C121	178.7 (10)
C32—C33—C34—N1	1.7 (15)	C119—C120—C123—C124	155.5 (10)
C31—C32—C35—C40	172.9 (10)	C121—C120—C123—C124	−24.9 (14)
C33—C32—C35—C40	−5.2 (15)	C119—C120—C123—C127	−25.8 (14)
C31—C32—C35—C36	−4.1 (13)	C121—C120—C123—C127	153.7 (10)
C33—C32—C35—C36	177.8 (9)	C127—C123—C124—C125	2.9 (14)
C40—C35—C36—C37	−0.6 (15)	C120—C123—C124—C125	−178.3 (9)
C32—C35—C36—C37	176.6 (9)	C123—C124—C125—N11	−1.3 (16)
C35—C36—C37—C38	−2.3 (17)	N11—C126—C127—C123	−1.1 (16)
C36—C37—C38—C39	6.3 (17)	C124—C123—C127—C126	−1.8 (14)
C36—C37—C38—C41	−176.5 (10)	C120—C123—C127—C126	179.4 (9)
C37—C38—C39—C40	−7.4 (17)	C31—C30—N1—C34	−1.7 (13)
C41—C38—C39—C40	175.5 (10)	C31—C30—N1—Co4	162.0 (7)
C36—C35—C40—C39	−0.6 (17)	C33—C34—N1—C30	0.8 (13)
C32—C35—C40—C39	−177.8 (10)	C33—C34—N1—Co4	−164.2 (8)
C38—C39—C40—C35	4.8 (19)	C47—C46—N2—C50	−0.7 (14)
C37—C38—C41—C43	155.8 (11)	C47—C46—N2—Co4	174.9 (8)
C39—C38—C41—C43	−27.1 (16)	C49—C50—N2—C46	−1.2 (14)
C37—C38—C41—C42	−24.5 (15)	C49—C50—N2—Co4	−176.8 (7)
C39—C38—C41—C42	152.6 (11)	C56—C57—N3—C53	−3.7 (12)
C43—C41—C42—C74^v	1.7 (15)	C56—C57—N3—Co2	166.4 (7)
C38—C41—C42—C74^v	−177.9 (9)	C54—C53—N3—C57	4.2 (12)
C42—C41—C43—C73^v	−1.8 (16)	C54—C53—N3—Co2	−165.8 (7)
C38—C41—C43—C73^v	177.8 (9)	C67—C68—N4—C64	2.2 (13)
N2—C46—C47—C48	3.0 (17)	C67—C68—N4—Co2	176.8 (7)
C46—C47—C48—C49	−3.0 (15)	C65—C64—N4—C68	−0.2 (13)
C46—C47—C48—C51	177.1 (10)	C65—C64—N4—Co2	−174.8 (8)
C47—C48—C49—C50	1.2 (14)	C42^viii—C74—N5—C73	−2.6 (14)
C51—C48—C49—C50	−178.9 (9)	C42^viii—C74—N5—Co1	160.0 (8)
C48—C49—C50—N2	0.9 (15)	C43^viii—C73—N5—C74	2.5 (15)
C47—C48—C51—C94^vi	−152.3 (11)	C43^viii—C73—N5—Co1	−160.1 (8)
C49—C48—C51—C94^vi	27.8 (15)	C78—C79—N6—C75	−2.0 (17)
C47—C48—C51—C52	22.4 (16)	C78—C79—N6—Co1	−173.4 (8)
C49—C48—C51—C52	−157.5 (11)	C76—C75—N6—C79	1.0 (18)
C94^vi—C51—C52—C95^vi	−4 (2)	C76—C75—N6—Co1	173.1 (10)
C48—C51—C52—C95^vi	−178.8 (12)	C90—C91—N7—C87	−2.4 (15)
N3—C53—C54—C55	0.8 (15)	C90—C91—N7—Co3	170.7 (9)
C53—C54—C55—C56	−6.1 (14)	C88—C87—N7—C91	0.7 (13)
C53—C54—C55—C58	174.3 (9)	C88—C87—N7—Co3	−172.1 (7)
C54—C55—C56—C57	6.3 (13)	C83—C84—N8—C80	2.2 (13)
C58—C55—C56—C57	−174.1 (9)	C83—C84—N8—Co3	−171.2 (7)
C55—C56—C57—N3	−1.7 (13)	C81—C80—N8—C84	−2.1 (12)
C54—C55—C58—C59	−162.0 (13)	C81—C80—N8—Co3	171.1 (6)
C56—C55—C58—C59	18.5 (18)	C111—C110—N10—C109	−2 (3)
C54—C55—C58—C63	25.7 (16)	C108—C109—N10—C110	2 (3)
C56—C55—C58—C63	−153.9 (11)	C124—C125—N11—C126	−1.6 (15)
C63—C58—C59—C60	−7 (3)	C127—C126—N11—C125	2.8 (15)
C55—C58—C59—C60	−179.4 (14)	C115—C116—N12—C112	0 (2)
C58—C59—C60—C61	−2 (3)	C113—C112—N12—C116	−1 (3)
C59—C60—C61—C62	9 (2)	C97—C96—N13—C100	3 (2)
C59—C60—C61—C77^vii	−178.1 (14)	C99—C100—N13—C96	−4 (2)
C60—C61—C62—C63	−7 (2)	O2—C24—O1—Co2	−13.8 (16)
C77^vii—C61—C62—C63	−179.9 (13)	C25—C24—O1—Co2	164.6 (8)
C59—C58—C63—C62	9 (2)	O1—C24—O2—Co4	−49.0 (11)
C55—C58—C63—C62	−178.2 (12)	C25—C24—O2—Co4	132.6 (6)
C61—C62—C63—C58	−2 (2)	O4—C44—O3—Co4	−2.5 (10)
N4—C64—C65—C66	−3.4 (15)	C27ⁱⁱ—C44—O3—Co4	177.0 (4)
C64—C65—C66—C67	4.8 (14)	O17^iv—C45—O5—Co4	−32.0 (13)
C64—C65—C66—C69	−176.3 (9)	C12^iv—C45—O5—Co4	145.8 (6)
C65—C66—C67—C68	−3.0 (14)	O7—C14—O6—Co2	−148.6 (6)
C69—C66—C67—C68	178.1 (9)	C13—C14—O6—Co2	34.7 (11)
C66—C67—C68—N4	−0.6 (15)	C7—C6—O8—C8	0.0 (11)
C67—C66—C69—C70	40.4 (14)	C5—C6—O8—C8	−179.7 (7)
C65—C66—C69—C70	−138.5 (10)	C9—C8—O8—C6	−81.6 (9)
C67—C66—C69—C72	−142.8 (11)	C13—C8—O8—C6	103.2 (8)
C65—C66—C69—C72	38.4 (14)	O10—C1—O9—Co1	6.0 (9)
C72—C69—C70—C71	1.2 (16)	C2—C1—O9—Co1	−173.3 (4)
C66—C69—C70—C71	178.1 (9)	O9—C1—O10—Co3	81 (2)
C69—C70—C71—C85^v	−1.4 (16)	C2—C1—O10—Co3	−99 (2)
C70—C69—C72—C86^v	−1.2 (18)	O12—C21—O11—Co3	−151.8 (7)
C66—C69—C72—C86^v	−178.2 (11)	C20—C21—O11—Co3	29.8 (12)
N6—C75—C76—C77	1 (2)	O16ⁱ—C22—O13—Co3	172.5 (5)
C75—C76—C77—C78	−1 (2)	C19—C22—O13—Co3	−13.0 (11)
C75—C76—C77—C61^vii	−176.1 (12)	O15—C128—O14—Co1	10 (2)
C76—C77—C78—C79	0.6 (18)	C4ⁱⁱⁱ—C128—O14—Co1	−169.5 (14)
C61^vii—C77—C78—C79	175.0 (11)	O14—C128—O15—Co3	13.1 (15)
C77—C78—C79—N6	1.2 (18)	C4ⁱⁱⁱ—C128—O15—Co3	−166.9 (6)
N8—C80—C81—C82	0.9 (13)	C29ⁱⁱⁱ—C23—O73—C15	164.1 (7)
C80—C81—C82—C83	0.3 (13)	C28ⁱⁱⁱ—C23—O73—C15	−17.5 (11)
C80—C81—C82—C85	−178.7 (8)	C20—C15—O73—C23	116.7 (8)
C81—C82—C83—C84	−0.2 (13)	C16—C15—O73—C23	−69.2 (10)

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

Poly[[µ-1,4-bis(pyridin-4-yl)benzene][µ-4-(3,5-dicarboxylatophenoxy)phthalato]dicobalt(II)] (7) top

Crystal data top

[Co₂(C₁₆H₆O₉)(C₁₆H₁₂N₄)₂(H₂O)]	Z = 2
M_r = 942.64	F(000) = 964
Triclinic, P1	D_x = 1.361 Mg m⁻³
a = 12.068 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.523 (3) Å	Cell parameters from 3563 reflections
c = 14.662 (3) Å	θ = 2.5–25.9°
α = 68.654 (3)°	µ = 0.78 mm⁻¹
β = 79.061 (3)°	T = 296 K
γ = 75.130 (3)°	Block, purple
V = 2300.1 (7) Å³	0.28 × 0.25 × 0.22 mm

Data collection top

Bruker SMART APEX CCD area detector diffractometer	8058 independent reflections
Radiation source: fine-focus sealed tube	5909 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.026
phi and ω scans	θ_max = 25.0°, θ_min = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −14→9
T_min = 0.811, T_max = 0.847	k = −17→17
12890 measured reflections	l = −17→17

Refinement top

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.151	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	w = 1/[σ²(F_o²) + (0.0973P)²] where P = (F_o² + 2F_c²)/3
8058 reflections	(Δ/σ)_max = 0.001
578 parameters	Δρ_max = 0.76 e Å⁻³
2 restraints	Δρ_min = −0.43 e Å⁻³

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.93445 (4)	0.07482 (3)	0.83730 (3)	0.02647 (15)
Co2	0.95248 (4)	0.26202 (3)	0.57353 (3)	0.02652 (15)
N1	0.8048 (3)	0.3645 (2)	0.6134 (2)	0.0353 (7)
N2	0.8156 (3)	0.2047 (2)	0.8595 (2)	0.0350 (7)
N3	1.0542 (3)	−0.0516 (2)	0.8042 (2)	0.0297 (7)
N4	0.9269 (3)	0.3337 (2)	0.4185 (2)	0.0323 (7)
O1	0.8231 (2)	0.0696 (2)	0.74955 (18)	0.0408 (7)
O2	0.8595 (2)	0.15569 (19)	0.59067 (19)	0.0373 (6)
O3	0.9118 (2)	−0.16394 (18)	0.47411 (17)	0.0310 (6)
O4	0.7763 (2)	−0.2557 (2)	0.5428 (2)	0.0480 (8)
O5	0.4554 (2)	0.0072 (3)	0.6329 (2)	0.0576 (9)
O6	0.0342 (2)	0.09175 (18)	0.92985 (17)	0.0297 (6)
O7	0.1618 (2)	0.0106 (2)	1.03886 (18)	0.0371 (6)
O8	1.0212 (2)	0.18163 (17)	0.72059 (17)	0.0282 (5)
O9	1.0624 (2)	0.36477 (17)	0.54785 (19)	0.0356 (6)
H9A	1.0774 (3)	0.3536 (2)	0.6119 (6)	0.043*
H9B	1.1103 (5)	0.3440 (2)	0.5142 (3)	0.043*
O10	1.1212 (2)	0.28424 (19)	0.7351 (2)	0.0422 (7)
C1	0.8171 (3)	0.0904 (3)	0.6606 (3)	0.0272 (8)
C2	0.7519 (3)	0.0305 (3)	0.6338 (3)	0.0289 (8)
C3	0.8107 (3)	−0.0395 (3)	0.5886 (2)	0.0284 (8)
H3	0.8898	−0.0453	0.5709	0.034*
C4	0.7544 (3)	−0.1005 (3)	0.5696 (3)	0.0331 (9)
C5	0.6347 (3)	−0.0848 (3)	0.5868 (3)	0.0396 (10)
H5	0.5952	−0.1236	0.5715	0.048*
C6	0.5757 (3)	−0.0118 (3)	0.6265 (3)	0.0411 (10)
C7	0.6315 (4)	0.0450 (3)	0.6538 (3)	0.0417 (10)
H7	0.5903	0.0913	0.6845	0.050*
C8	0.8183 (3)	−0.1803 (3)	0.5256 (3)	0.0323 (9)
C9	0.3903 (3)	0.0251 (3)	0.7129 (3)	0.0382 (10)
C10	0.2941 (3)	0.1019 (3)	0.6955 (3)	0.0337 (9)
H10	0.2847	0.1463	0.6319	0.040*
C11	0.2112 (3)	0.1132 (3)	0.7727 (3)	0.0276 (8)
C12	0.2291 (3)	0.0486 (3)	0.8684 (3)	0.0323 (8)
C13	0.3310 (3)	−0.0242 (3)	0.8844 (3)	0.0456 (10)
H13	0.3447	−0.0652	0.9485	0.055*
C14	0.4112 (3)	−0.0364 (3)	0.8078 (3)	0.0478 (11)
H14	0.4787	−0.0854	0.8194	0.057*
C15	0.1349 (3)	0.0511 (3)	0.9514 (3)	0.0291 (8)
C16	0.6968 (4)	0.3534 (4)	0.6171 (4)	0.0616 (14)
H16	0.6871	0.2977	0.6046	0.074*
C17	0.5993 (4)	0.4195 (4)	0.6383 (5)	0.0692 (16)
H17	0.5266	0.4067	0.6422	0.083*
C18	0.6103 (4)	0.5058 (3)	0.6539 (3)	0.0446 (10)
C19	0.7214 (4)	0.5179 (3)	0.6476 (3)	0.0496 (11)
H19	0.7338	0.5749	0.6559	0.060*
C20	0.8142 (4)	0.4465 (3)	0.6292 (3)	0.0460 (11)
H20	0.8878	0.4562	0.6277	0.055*
C21	0.5093 (4)	0.5807 (3)	0.6763 (3)	0.0476 (11)
C22	0.5046 (4)	0.6820 (3)	0.6309 (4)	0.0701 (16)
H22	0.5636	0.7042	0.5833	0.084*
C23	0.4128 (4)	0.7520 (3)	0.6552 (4)	0.0683 (16)
H23	0.4111	0.8204	0.6225	0.082*
C24	0.3282 (4)	0.6198 (3)	0.7706 (3)	0.0500 (11)
H24	0.2691	0.5978	0.8184	0.060*
C25	0.4181 (4)	0.5496 (3)	0.7450 (4)	0.0518 (12)
H25	0.4176	0.4811	0.7739	0.062*
C26	0.7022 (4)	0.2087 (3)	0.8730 (3)	0.0453 (11)
H26	0.6758	0.1600	0.8607	0.054*
C27	0.6224 (4)	0.2803 (3)	0.9039 (3)	0.0520 (12)
H27	0.5445	0.2784	0.9141	0.062*
C28	0.6592 (4)	0.3558 (3)	0.9200 (3)	0.0455 (11)
C29	0.7763 (4)	0.3553 (3)	0.9008 (3)	0.0453 (11)
H29	0.8041	0.4064	0.9075	0.054*
C30	0.8515 (4)	0.2795 (3)	0.8719 (3)	0.0421 (10)
H30	0.9299	0.2799	0.8606	0.051*
C31	0.5772 (4)	0.4302 (3)	0.9622 (3)	0.0543 (13)
C32	0.4828 (5)	0.4035 (4)	1.0262 (4)	0.0720 (17)
H32	0.4706	0.3382	1.0448	0.086*
C33	0.5939 (5)	0.5272 (4)	0.9368 (4)	0.0739 (17)
H33	0.6579	0.5461	0.8940	0.089*
C34	1.0982 (3)	−0.0399 (3)	0.7106 (3)	0.0341 (9)
H34	1.0682	0.0189	0.6620	0.041*
C35	1.1847 (3)	−0.1093 (3)	0.6819 (3)	0.0352 (9)
H35	1.2128	−0.0961	0.6158	0.042*
C36	1.2307 (3)	−0.1999 (3)	0.7524 (3)	0.0344 (9)
C37	1.1827 (4)	−0.2130 (3)	0.8488 (3)	0.0431 (10)
H37	1.2086	−0.2723	0.8987	0.052*
C38	1.0970 (4)	−0.1388 (3)	0.8714 (3)	0.0400 (10)
H38	1.0672	−0.1499	0.9369	0.048*
C39	0.9172 (4)	0.4327 (3)	0.3723 (3)	0.0426 (10)
H39	0.8973	0.4748	0.4103	0.051*
C40	0.9348 (4)	0.4758 (3)	0.2726 (3)	0.0479 (11)
H40	0.9267	0.5455	0.2449	0.057*
C41	0.9644 (4)	0.4172 (3)	0.2119 (3)	0.0395 (10)
C42	0.9743 (4)	0.3136 (3)	0.2598 (3)	0.0400 (10)
H42	0.9953	0.2696	0.2236	0.048*
C43	0.9528 (3)	0.2764 (3)	0.3613 (3)	0.0367 (9)
H43	0.9567	0.2073	0.3912	0.044*
C44	0.9840 (4)	0.4598 (3)	0.1036 (3)	0.0440 (10)
C45	0.9229 (5)	0.5535 (3)	0.0526 (3)	0.0603 (14)
H45	0.8702	0.5910	0.0875	0.072*
C46	0.9380 (5)	0.5926 (3)	−0.0485 (3)	0.0578 (14)
H46	0.8948	0.6556	−0.0805	0.069*
C47	0.3252 (3)	0.7235 (3)	0.7254 (3)	0.0391 (10)
C48	1.1090 (3)	0.1995 (3)	0.7437 (2)	0.0290 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0227 (3)	0.0266 (3)	0.0297 (3)	0.0004 (2)	0.0003 (2)	−0.0142 (2)
Co2	0.0256 (3)	0.0213 (3)	0.0305 (3)	−0.0018 (2)	0.0033 (2)	−0.0112 (2)
N1	0.0343 (18)	0.0266 (16)	0.0410 (18)	0.0011 (14)	−0.0013 (15)	−0.0129 (14)
N2	0.0316 (18)	0.0342 (17)	0.0347 (17)	0.0033 (15)	0.0013 (14)	−0.0155 (14)
N3	0.0264 (16)	0.0279 (15)	0.0355 (17)	−0.0005 (13)	0.0007 (13)	−0.0167 (14)
N4	0.0397 (19)	0.0275 (16)	0.0285 (16)	−0.0065 (14)	0.0010 (14)	−0.0105 (13)
O1	0.0386 (16)	0.0553 (17)	0.0313 (15)	−0.0131 (14)	−0.0043 (12)	−0.0151 (13)
O2	0.0380 (15)	0.0347 (14)	0.0401 (15)	−0.0134 (13)	−0.0023 (13)	−0.0105 (13)
O3	0.0313 (14)	0.0287 (13)	0.0323 (13)	−0.0047 (11)	0.0051 (11)	−0.0145 (11)
O4	0.0375 (16)	0.0417 (16)	0.076 (2)	−0.0152 (14)	0.0154 (15)	−0.0378 (16)
O5	0.0247 (15)	0.102 (3)	0.065 (2)	−0.0077 (16)	0.0059 (14)	−0.059 (2)
O6	0.0223 (13)	0.0346 (13)	0.0326 (13)	0.0004 (11)	−0.0006 (11)	−0.0171 (11)
O7	0.0290 (14)	0.0439 (15)	0.0333 (15)	−0.0045 (12)	−0.0027 (12)	−0.0093 (12)
O8	0.0225 (13)	0.0261 (12)	0.0341 (13)	0.0002 (10)	−0.0015 (11)	−0.0118 (11)
O9	0.0364 (15)	0.0277 (13)	0.0421 (15)	−0.0053 (12)	0.0062 (12)	−0.0169 (12)
O10	0.0430 (17)	0.0280 (14)	0.0621 (19)	−0.0051 (13)	−0.0108 (14)	−0.0216 (13)
C1	0.0212 (18)	0.0242 (18)	0.033 (2)	0.0042 (15)	0.0026 (15)	−0.0144 (16)
C2	0.0238 (18)	0.0276 (18)	0.036 (2)	−0.0042 (15)	0.0025 (15)	−0.0152 (16)
C3	0.0209 (18)	0.0310 (19)	0.0331 (19)	−0.0030 (16)	0.0023 (15)	−0.0144 (16)
C4	0.0227 (19)	0.035 (2)	0.048 (2)	−0.0063 (16)	0.0049 (17)	−0.0250 (18)
C5	0.035 (2)	0.050 (2)	0.043 (2)	−0.0141 (19)	0.0085 (18)	−0.029 (2)
C6	0.023 (2)	0.056 (3)	0.048 (2)	−0.0080 (19)	0.0005 (18)	−0.025 (2)
C7	0.035 (2)	0.048 (2)	0.049 (2)	−0.005 (2)	0.0045 (19)	−0.031 (2)
C8	0.027 (2)	0.031 (2)	0.043 (2)	−0.0006 (17)	−0.0076 (17)	−0.0185 (17)
C9	0.0199 (19)	0.053 (2)	0.052 (2)	−0.0051 (18)	0.0048 (17)	−0.035 (2)
C10	0.026 (2)	0.042 (2)	0.036 (2)	−0.0059 (18)	−0.0013 (16)	−0.0182 (18)
C11	0.0193 (17)	0.0316 (19)	0.036 (2)	−0.0056 (15)	0.0018 (15)	−0.0174 (16)
C12	0.0252 (19)	0.035 (2)	0.035 (2)	−0.0016 (17)	−0.0009 (16)	−0.0143 (17)
C13	0.030 (2)	0.047 (2)	0.045 (2)	0.0026 (19)	−0.0021 (19)	−0.006 (2)
C14	0.023 (2)	0.049 (3)	0.064 (3)	0.0033 (19)	0.002 (2)	−0.021 (2)
C15	0.027 (2)	0.0276 (18)	0.033 (2)	−0.0027 (16)	−0.0015 (16)	−0.0134 (16)
C16	0.033 (2)	0.049 (3)	0.118 (4)	0.004 (2)	−0.008 (3)	−0.053 (3)
C17	0.026 (2)	0.057 (3)	0.139 (5)	0.003 (2)	−0.002 (3)	−0.059 (3)
C18	0.037 (2)	0.033 (2)	0.057 (3)	−0.0007 (19)	0.006 (2)	−0.017 (2)
C19	0.043 (3)	0.034 (2)	0.073 (3)	−0.008 (2)	0.016 (2)	−0.030 (2)
C20	0.029 (2)	0.037 (2)	0.072 (3)	−0.0064 (19)	0.012 (2)	−0.028 (2)
C21	0.035 (2)	0.033 (2)	0.068 (3)	0.0038 (19)	0.006 (2)	−0.022 (2)
C22	0.050 (3)	0.043 (3)	0.094 (4)	−0.007 (2)	0.039 (3)	−0.022 (3)
C23	0.052 (3)	0.024 (2)	0.108 (4)	−0.004 (2)	0.028 (3)	−0.018 (2)
C24	0.036 (2)	0.040 (2)	0.063 (3)	−0.005 (2)	0.016 (2)	−0.017 (2)
C25	0.038 (2)	0.029 (2)	0.079 (3)	−0.0022 (19)	0.010 (2)	−0.019 (2)
C26	0.033 (2)	0.045 (2)	0.057 (3)	0.007 (2)	−0.003 (2)	−0.027 (2)
C27	0.033 (2)	0.051 (3)	0.061 (3)	0.011 (2)	0.002 (2)	−0.022 (2)
C28	0.046 (3)	0.039 (2)	0.039 (2)	0.012 (2)	0.0051 (19)	−0.0162 (19)
C29	0.050 (3)	0.034 (2)	0.047 (2)	0.003 (2)	0.005 (2)	−0.0203 (19)
C30	0.040 (2)	0.036 (2)	0.042 (2)	0.0030 (19)	0.0009 (19)	−0.0139 (18)
C31	0.052 (3)	0.037 (2)	0.057 (3)	0.015 (2)	0.008 (2)	−0.019 (2)
C32	0.065 (4)	0.043 (3)	0.089 (4)	0.002 (3)	0.029 (3)	−0.026 (3)
C33	0.058 (3)	0.046 (3)	0.098 (4)	0.003 (3)	0.028 (3)	−0.029 (3)
C34	0.034 (2)	0.0253 (18)	0.041 (2)	−0.0032 (17)	0.0018 (17)	−0.0143 (17)
C35	0.037 (2)	0.0310 (19)	0.035 (2)	−0.0066 (18)	0.0087 (17)	−0.0155 (17)
C36	0.026 (2)	0.031 (2)	0.049 (2)	−0.0018 (17)	−0.0024 (17)	−0.0207 (18)
C37	0.047 (3)	0.032 (2)	0.041 (2)	0.0098 (19)	−0.008 (2)	−0.0122 (18)
C38	0.047 (3)	0.038 (2)	0.032 (2)	0.0023 (19)	−0.0006 (18)	−0.0175 (18)
C39	0.059 (3)	0.030 (2)	0.038 (2)	−0.005 (2)	−0.001 (2)	−0.0162 (18)
C40	0.073 (3)	0.027 (2)	0.040 (2)	−0.008 (2)	−0.002 (2)	−0.0091 (18)
C41	0.048 (2)	0.038 (2)	0.030 (2)	−0.008 (2)	−0.0020 (18)	−0.0108 (17)
C42	0.053 (3)	0.035 (2)	0.036 (2)	−0.006 (2)	−0.0059 (19)	−0.0171 (18)
C43	0.044 (2)	0.0278 (19)	0.041 (2)	−0.0077 (18)	−0.0098 (19)	−0.0114 (17)
C44	0.057 (3)	0.042 (2)	0.030 (2)	−0.010 (2)	−0.0006 (19)	−0.0100 (18)
C45	0.081 (4)	0.048 (3)	0.039 (2)	0.005 (3)	0.002 (2)	−0.016 (2)
C46	0.079 (4)	0.042 (2)	0.032 (2)	0.010 (2)	−0.004 (2)	−0.0041 (19)
C47	0.033 (2)	0.033 (2)	0.050 (2)	0.0004 (18)	0.0042 (18)	−0.0205 (19)
C48	0.028 (2)	0.0295 (19)	0.0272 (19)	−0.0014 (16)	0.0013 (15)	−0.0114 (15)

Geometric parameters (Å, º) top

Co1—O1	2.061 (3)	C17—C18	1.394 (6)
Co1—O6ⁱ	2.089 (2)	C17—H17	0.9300
Co1—O7ⁱⁱ	2.117 (3)	C18—C19	1.378 (6)
Co1—N2	2.145 (3)	C18—C21	1.485 (5)
Co1—O8	2.157 (3)	C19—C20	1.377 (5)
Co1—N3	2.172 (3)	C19—H19	0.9300
Co2—O2	2.051 (3)	C20—H20	0.9300
Co2—O3ⁱⁱⁱ	2.072 (2)	C21—C22	1.367 (6)
Co2—O9	2.132 (3)	C21—C25	1.390 (6)
Co2—N1	2.147 (3)	C22—C23	1.386 (6)
Co2—N4	2.174 (3)	C22—H22	0.9300
Co2—O8	2.247 (2)	C23—C47	1.360 (6)
N1—C20	1.329 (5)	C23—H23	0.9300
N1—C16	1.342 (6)	C24—C25	1.384 (5)
N2—C26	1.334 (5)	C24—C47	1.402 (6)
N2—C30	1.348 (5)	C24—H24	0.9300
N3—C38	1.337 (5)	C25—H25	0.9300
N3—C34	1.340 (5)	C26—C27	1.371 (5)
N4—C43	1.330 (4)	C26—H26	0.9300
N4—C39	1.332 (5)	C27—C28	1.391 (6)
O1—C1	1.239 (4)	C27—H27	0.9300
O2—C1	1.246 (4)	C28—C29	1.386 (6)
O3—C8	1.258 (5)	C28—C31	1.494 (5)
O3—Co2ⁱⁱⁱ	2.072 (2)	C29—C30	1.377 (5)
O4—C8	1.247 (5)	C29—H29	0.9300
O5—C9	1.352 (4)	C30—H30	0.9300
O5—C6	1.398 (5)	C31—C32	1.373 (7)
O6—C15	1.252 (4)	C31—C33	1.379 (7)
O6—Co1^iv	2.089 (2)	C32—C33^v	1.375 (6)
O7—C15	1.267 (4)	C32—H32	0.9300
O7—Co1ⁱⁱ	2.117 (3)	C33—C32^v	1.375 (6)
O8—C48	1.282 (4)	C33—H33	0.9300
O9—H9A	0.9372	C34—C35	1.373 (5)
O9—H9B	0.7604	C34—H34	0.9300
O10—C48	1.235 (4)	C35—C36	1.401 (5)
C1—C2	1.499 (5)	C35—H35	0.9300
C2—C3	1.385 (4)	C36—C37	1.385 (5)
C2—C7	1.403 (5)	C36—C47^vi	1.481 (5)
C3—C4	1.373 (5)	C37—C38	1.379 (5)
C3—H3	0.9300	C37—H37	0.9300
C4—C5	1.392 (5)	C38—H38	0.9300
C4—C8	1.499 (5)	C39—C40	1.364 (6)
C5—C6	1.369 (5)	C39—H39	0.9300
C5—H5	0.9300	C40—C41	1.384 (5)
C6—C7	1.388 (6)	C40—H40	0.9300
C7—H7	0.9300	C41—C42	1.394 (5)
C9—C10	1.377 (5)	C41—C44	1.476 (5)
C9—C14	1.382 (6)	C42—C43	1.383 (5)
C10—C11	1.389 (5)	C42—H42	0.9300
C10—H10	0.9300	C43—H43	0.9300
C11—C12	1.396 (5)	C44—C46^vii	1.381 (6)
C11—C48^iv	1.514 (5)	C44—C45	1.382 (6)
C12—C13	1.395 (5)	C45—C46	1.376 (6)
C12—C15	1.504 (5)	C45—H45	0.9300
C13—C14	1.370 (6)	C46—C44^vii	1.381 (6)
C13—H13	0.9300	C46—H46	0.9300
C14—H14	0.9300	C47—C36^viii	1.481 (5)
C16—C17	1.379 (6)	C48—C11ⁱ	1.514 (5)
C16—H16	0.9300

O1—Co1—O6ⁱ	174.12 (10)	N1—C16—C17	123.9 (4)
O1—Co1—O7ⁱⁱ	88.42 (11)	N1—C16—H16	118.0
O6ⁱ—Co1—O7ⁱⁱ	90.37 (10)	C17—C16—H16	118.0
O1—Co1—N2	88.48 (12)	C16—C17—C18	119.7 (4)
O6ⁱ—Co1—N2	85.69 (11)	C16—C17—H17	120.2
O7ⁱⁱ—Co1—N2	85.64 (11)	C18—C17—H17	120.2
O1—Co1—O8	94.87 (10)	C19—C18—C17	116.1 (4)
O6ⁱ—Co1—O8	85.47 (10)	C19—C18—C21	121.3 (4)
O7ⁱⁱ—Co1—O8	170.70 (9)	C17—C18—C21	122.6 (4)
N2—Co1—O8	85.76 (11)	C20—C19—C18	120.6 (4)
O1—Co1—N3	89.09 (11)	C20—C19—H19	119.7
O6ⁱ—Co1—N3	96.77 (10)	C18—C19—H19	119.7
O7ⁱⁱ—Co1—N3	97.31 (11)	N1—C20—C19	123.9 (4)
N2—Co1—N3	176.13 (11)	N1—C20—H20	118.1
O8—Co1—N3	91.45 (10)	C19—C20—H20	118.1
O2—Co2—O3ⁱⁱⁱ	84.10 (10)	C22—C21—C25	118.4 (4)
O2—Co2—O9	174.30 (10)	C22—C21—C18	120.8 (4)
O3ⁱⁱⁱ—Co2—O9	90.31 (10)	C25—C21—C18	120.8 (4)
O2—Co2—N1	93.58 (12)	C21—C22—C23	120.8 (4)
O3ⁱⁱⁱ—Co2—N1	175.41 (11)	C21—C22—H22	119.6
O9—Co2—N1	91.91 (11)	C23—C22—H22	119.6
O2—Co2—N4	92.15 (11)	C47—C23—C22	122.0 (4)
O3ⁱⁱⁱ—Co2—N4	84.92 (10)	C47—C23—H23	119.0
O9—Co2—N4	86.20 (11)	C22—C23—H23	119.0
N1—Co2—N4	91.22 (11)	C25—C24—C47	120.7 (4)
O2—Co2—O8	93.94 (10)	C25—C24—H24	119.7
O3ⁱⁱⁱ—Co2—O8	84.32 (9)	C47—C24—H24	119.7
O9—Co2—O8	86.63 (10)	C24—C25—C21	120.5 (4)
N1—Co2—O8	99.81 (10)	C24—C25—H25	119.7
N4—Co2—O8	167.02 (11)	C21—C25—H25	119.7
C20—N1—C16	115.8 (3)	N2—C26—C27	123.8 (4)
C20—N1—Co2	122.1 (3)	N2—C26—H26	118.1
C16—N1—Co2	121.9 (3)	C27—C26—H26	118.1
C26—N2—C30	117.1 (3)	C26—C27—C28	119.3 (4)
C26—N2—Co1	120.6 (3)	C26—C27—H27	120.3
C30—N2—Co1	121.9 (3)	C28—C27—H27	120.3
C38—N3—C34	116.0 (3)	C29—C28—C27	117.1 (4)
C38—N3—Co1	125.1 (2)	C29—C28—C31	121.4 (4)
C34—N3—Co1	118.7 (2)	C27—C28—C31	121.4 (4)
C43—N4—C39	116.1 (3)	C30—C29—C28	120.2 (4)
C43—N4—Co2	118.5 (2)	C30—C29—H29	119.9
C39—N4—Co2	122.8 (2)	C28—C29—H29	119.9
C1—O1—Co1	137.9 (3)	N2—C30—C29	122.3 (4)
C1—O2—Co2	136.9 (2)	N2—C30—H30	118.8
C8—O3—Co2ⁱⁱⁱ	129.9 (2)	C29—C30—H30	118.8
C9—O5—C6	120.5 (3)	C32—C31—C33	118.6 (4)
C15—O6—Co1^iv	132.3 (2)	C32—C31—C28	120.6 (4)
C15—O7—Co1ⁱⁱ	127.0 (2)	C33—C31—C28	120.8 (4)
C48—O8—Co1	115.2 (2)	C31—C32—C33^v	120.5 (5)
C48—O8—Co2	123.5 (2)	C31—C32—H32	119.8
Co1—O8—Co2	121.23 (11)	C33^v—C32—H32	119.8
Co2—O9—H9A	102.0	C32^v—C33—C31	120.9 (5)
Co2—O9—H9B	98.2	C32^v—C33—H33	119.5
H9A—O9—H9B	118.0	C31—C33—H33	119.5
O1—C1—O2	127.2 (3)	N3—C34—C35	124.1 (3)
O1—C1—C2	116.6 (3)	N3—C34—H34	117.9
O2—C1—C2	116.2 (3)	C35—C34—H34	117.9
C3—C2—C7	119.6 (3)	C34—C35—C36	119.9 (3)
C3—C2—C1	119.9 (3)	C34—C35—H35	120.1
C7—C2—C1	120.5 (3)	C36—C35—H35	120.1
C4—C3—C2	121.2 (3)	C37—C36—C35	115.8 (3)
C4—C3—H3	119.4	C37—C36—C47^vi	122.2 (3)
C2—C3—H3	119.4	C35—C36—C47^vi	121.9 (3)
C3—C4—C5	119.4 (3)	C38—C37—C36	120.5 (4)
C3—C4—C8	121.5 (3)	C38—C37—H37	119.7
C5—C4—C8	119.1 (3)	C36—C37—H37	119.7
C6—C5—C4	119.4 (4)	N3—C38—C37	123.6 (4)
C6—C5—H5	120.3	N3—C38—H38	118.2
C4—C5—H5	120.3	C37—C38—H38	118.2
C5—C6—C7	122.2 (4)	N4—C39—C40	123.8 (3)
C5—C6—O5	116.7 (4)	N4—C39—H39	118.1
C7—C6—O5	121.0 (3)	C40—C39—H39	118.1
C6—C7—C2	117.9 (3)	C39—C40—C41	120.9 (4)
C6—C7—H7	121.1	C39—C40—H40	119.5
C2—C7—H7	121.1	C41—C40—H40	119.5
O4—C8—O3	125.9 (3)	C40—C41—C42	115.6 (4)
O4—C8—C4	118.7 (3)	C40—C41—C44	123.3 (4)
O3—C8—C4	115.4 (3)	C42—C41—C44	121.2 (3)
O5—C9—C10	116.5 (4)	C43—C42—C41	119.7 (3)
O5—C9—C14	122.2 (4)	C43—C42—H42	120.1
C10—C9—C14	120.9 (3)	C41—C42—H42	120.1
C9—C10—C11	120.3 (4)	N4—C43—C42	123.8 (4)
C9—C10—H10	119.9	N4—C43—H43	118.1
C11—C10—H10	119.9	C42—C43—H43	118.1
C10—C11—C12	119.1 (3)	C46^vii—C44—C45	117.0 (4)
C10—C11—C48^iv	115.1 (3)	C46^vii—C44—C41	121.9 (4)
C12—C11—C48^iv	125.7 (3)	C45—C44—C41	121.1 (4)
C13—C12—C11	119.2 (3)	C46—C45—C44	121.6 (4)
C13—C12—C15	120.4 (3)	C46—C45—H45	119.2
C11—C12—C15	120.2 (3)	C44—C45—H45	119.2
C14—C13—C12	121.3 (4)	C45—C46—C44^vii	121.4 (4)
C14—C13—H13	119.3	C45—C46—H46	119.3
C12—C13—H13	119.3	C44^vii—C46—H46	119.3
C13—C14—C9	118.9 (4)	C23—C47—C24	117.5 (4)
C13—C14—H14	120.5	C23—C47—C36^viii	120.7 (4)
C9—C14—H14	120.5	C24—C47—C36^viii	121.7 (4)
O6—C15—O7	123.9 (3)	O10—C48—O8	124.7 (3)
O6—C15—C12	117.8 (3)	O10—C48—C11ⁱ	116.7 (3)
O7—C15—C12	118.2 (3)	O8—C48—C11ⁱ	118.2 (3)

O2—Co2—N1—C20	170.4 (3)	C5—C4—C8—O3	150.5 (4)
O3ⁱⁱⁱ—Co2—N1—C20	−130.1 (13)	C6—O5—C9—C10	137.7 (4)
O9—Co2—N1—C20	−11.1 (3)	C6—O5—C9—C14	−49.0 (6)
N4—Co2—N1—C20	−97.4 (3)	O5—C9—C10—C11	167.8 (3)
O8—Co2—N1—C20	75.8 (3)	C14—C9—C10—C11	−5.6 (6)
O2—Co2—N1—C16	−14.4 (4)	C9—C10—C11—C12	2.7 (5)
O3ⁱⁱⁱ—Co2—N1—C16	45.2 (16)	C9—C10—C11—C48^iv	−179.2 (3)
O9—Co2—N1—C16	164.1 (4)	C10—C11—C12—C13	1.5 (6)
N4—Co2—N1—C16	77.8 (4)	C48^iv—C11—C12—C13	−176.4 (4)
O8—Co2—N1—C16	−109.0 (4)	C10—C11—C12—C15	−172.8 (3)
O1—Co1—N2—C26	40.4 (3)	C48^iv—C11—C12—C15	9.3 (6)
O6ⁱ—Co1—N2—C26	−138.8 (3)	C11—C12—C13—C14	−3.1 (6)
O7ⁱⁱ—Co1—N2—C26	−48.1 (3)	C15—C12—C13—C14	171.3 (4)
O8—Co1—N2—C26	135.4 (3)	C12—C13—C14—C9	0.3 (7)
N3—Co1—N2—C26	91.5 (19)	O5—C9—C14—C13	−169.0 (4)
O1—Co1—N2—C30	−147.5 (3)	C10—C9—C14—C13	4.1 (6)
O6ⁱ—Co1—N2—C30	33.3 (3)	Co1^iv—O6—C15—O7	−129.4 (3)
O7ⁱⁱ—Co1—N2—C30	124.0 (3)	Co1^iv—O6—C15—C12	49.5 (5)
O8—Co1—N2—C30	−52.5 (3)	Co1ⁱⁱ—O7—C15—O6	37.7 (5)
N3—Co1—N2—C30	−96.4 (18)	Co1ⁱⁱ—O7—C15—C12	−141.2 (3)
O1—Co1—N3—C38	−124.4 (3)	C13—C12—C15—O6	−156.4 (4)
O6ⁱ—Co1—N3—C38	55.2 (3)	C11—C12—C15—O6	17.9 (5)
O7ⁱⁱ—Co1—N3—C38	−36.1 (3)	C13—C12—C15—O7	22.5 (5)
N2—Co1—N3—C38	−175.4 (17)	C11—C12—C15—O7	−163.2 (3)
O8—Co1—N3—C38	140.8 (3)	C20—N1—C16—C17	−1.7 (8)
O1—Co1—N3—C34	62.2 (3)	Co2—N1—C16—C17	−177.2 (4)
O6ⁱ—Co1—N3—C34	−118.3 (3)	N1—C16—C17—C18	2.3 (9)
O7ⁱⁱ—Co1—N3—C34	150.5 (3)	C16—C17—C18—C19	−0.7 (8)
N2—Co1—N3—C34	11 (2)	C16—C17—C18—C21	179.5 (5)
O8—Co1—N3—C34	−32.7 (3)	C17—C18—C19—C20	−1.4 (7)
O2—Co2—N4—C43	−51.9 (3)	C21—C18—C19—C20	178.4 (4)
O3ⁱⁱⁱ—Co2—N4—C43	31.9 (3)	C16—N1—C20—C19	−0.5 (7)
O9—Co2—N4—C43	122.6 (3)	Co2—N1—C20—C19	175.0 (3)
N1—Co2—N4—C43	−145.6 (3)	C18—C19—C20—N1	2.1 (7)
O8—Co2—N4—C43	66.0 (6)	C19—C18—C21—C22	44.3 (7)
O2—Co2—N4—C39	146.8 (3)	C17—C18—C21—C22	−135.8 (6)
O3ⁱⁱⁱ—Co2—N4—C39	−129.3 (3)	C19—C18—C21—C25	−134.6 (5)
O9—Co2—N4—C39	−38.6 (3)	C17—C18—C21—C25	45.2 (7)
N1—Co2—N4—C39	53.2 (3)	C25—C21—C22—C23	2.0 (8)
O8—Co2—N4—C39	−95.2 (5)	C18—C21—C22—C23	−176.9 (5)
O6ⁱ—Co1—O1—C1	112.3 (10)	C21—C22—C23—C47	1.0 (9)
O7ⁱⁱ—Co1—O1—C1	−169.5 (4)	C47—C24—C25—C21	2.2 (7)
N2—Co1—O1—C1	104.9 (4)	C22—C21—C25—C24	−3.6 (8)
O8—Co1—O1—C1	19.3 (4)	C18—C21—C25—C24	175.3 (4)
N3—Co1—O1—C1	−72.1 (4)	C30—N2—C26—C27	−3.9 (6)
O3ⁱⁱⁱ—Co2—O2—C1	107.0 (3)	Co1—N2—C26—C27	168.5 (3)
O9—Co2—O2—C1	118.7 (10)	N2—C26—C27—C28	1.9 (7)
N1—Co2—O2—C1	−77.0 (3)	C26—C27—C28—C29	1.7 (6)
N4—Co2—O2—C1	−168.4 (3)	C26—C27—C28—C31	−174.5 (4)
O8—Co2—O2—C1	23.1 (3)	C27—C28—C29—C30	−3.1 (6)
O1—Co1—O8—C48	−173.7 (2)	C31—C28—C29—C30	173.1 (4)
O6ⁱ—Co1—O8—C48	12.2 (2)	C26—N2—C30—C29	2.3 (6)
O7ⁱⁱ—Co1—O8—C48	75.9 (6)	Co1—N2—C30—C29	−170.0 (3)
N2—Co1—O8—C48	98.2 (2)	C28—C29—C30—N2	1.2 (6)
N3—Co1—O8—C48	−84.5 (2)	C29—C28—C31—C32	−145.7 (5)
O1—Co1—O8—Co2	10.30 (13)	C27—C28—C31—C32	30.4 (7)
O6ⁱ—Co1—O8—Co2	−163.82 (12)	C29—C28—C31—C33	35.0 (7)
O7ⁱⁱ—Co1—O8—Co2	−100.1 (6)	C27—C28—C31—C33	−148.9 (5)
N2—Co1—O8—Co2	−77.81 (13)	C33—C31—C32—C33^v	0.7 (10)
N3—Co1—O8—Co2	99.51 (13)	C28—C31—C32—C33^v	−178.6 (5)
O2—Co2—O8—C48	162.5 (2)	C32—C31—C33—C32^v	−0.7 (10)
O3ⁱⁱⁱ—Co2—O8—C48	78.8 (2)	C28—C31—C33—C32^v	178.6 (5)
O9—Co2—O8—C48	−11.9 (2)	C38—N3—C34—C35	−2.3 (6)
N1—Co2—O8—C48	−103.2 (2)	Co1—N3—C34—C35	171.7 (3)
N4—Co2—O8—C48	44.7 (5)	N3—C34—C35—C36	1.4 (6)
O2—Co2—O8—Co1	−21.91 (13)	C34—C35—C36—C37	0.5 (6)
O3ⁱⁱⁱ—Co2—O8—Co1	−105.58 (13)	C34—C35—C36—C47^vi	−179.1 (4)
O9—Co2—O8—Co1	163.77 (12)	C35—C36—C37—C38	−1.3 (6)
N1—Co2—O8—Co1	72.41 (14)	C47^vi—C36—C37—C38	178.2 (4)
N4—Co2—O8—Co1	−139.7 (4)	C34—N3—C38—C37	1.3 (6)
Co1—O1—C1—O2	−28.3 (6)	Co1—N3—C38—C37	−172.3 (3)
Co1—O1—C1—C2	151.6 (3)	C36—C37—C38—N3	0.5 (7)
Co2—O2—C1—O1	−1.5 (6)	C43—N4—C39—C40	−1.5 (6)
Co2—O2—C1—C2	178.7 (2)	Co2—N4—C39—C40	160.1 (4)
O1—C1—C2—C3	−109.3 (4)	N4—C39—C40—C41	0.1 (8)
O2—C1—C2—C3	70.6 (4)	C39—C40—C41—C42	0.1 (7)
O1—C1—C2—C7	70.9 (5)	C39—C40—C41—C44	179.8 (4)
O2—C1—C2—C7	−109.2 (4)	C40—C41—C42—C43	1.1 (6)
C7—C2—C3—C4	−4.9 (6)	C44—C41—C42—C43	−178.6 (4)
C1—C2—C3—C4	175.3 (3)	C39—N4—C43—C42	2.9 (6)
C2—C3—C4—C5	6.5 (6)	Co2—N4—C43—C42	−159.6 (3)
C2—C3—C4—C8	−176.7 (3)	C41—C42—C43—N4	−2.8 (7)
C3—C4—C5—C6	−2.8 (6)	C40—C41—C44—C46^vii	148.3 (5)
C8—C4—C5—C6	−179.7 (4)	C42—C41—C44—C46^vii	−32.0 (7)
C4—C5—C6—C7	−2.5 (7)	C40—C41—C44—C45	−33.1 (7)
C4—C5—C6—O5	173.8 (4)	C42—C41—C44—C45	146.6 (5)
C9—O5—C6—C5	140.3 (4)	C46^vii—C44—C45—C46	0.6 (9)
C9—O5—C6—C7	−43.3 (6)	C41—C44—C45—C46	−178.1 (5)
C5—C6—C7—C2	4.1 (6)	C44—C45—C46—C44^vii	−0.7 (10)
O5—C6—C7—C2	−172.0 (4)	C22—C23—C47—C24	−2.4 (8)
C3—C2—C7—C6	−0.4 (6)	C22—C23—C47—C36^viii	177.6 (5)
C1—C2—C7—C6	179.4 (4)	C25—C24—C47—C23	0.8 (7)
Co2ⁱⁱⁱ—O3—C8—O4	−15.8 (6)	C25—C24—C47—C36^viii	−179.3 (4)
Co2ⁱⁱⁱ—O3—C8—C4	163.7 (2)	Co1—O8—C48—O10	−124.2 (3)
C3—C4—C8—O4	153.3 (4)	Co2—O8—C48—O10	51.7 (4)
C5—C4—C8—O4	−29.9 (6)	Co1—O8—C48—C11ⁱ	63.1 (3)
C3—C4—C8—O3	−26.2 (5)	Co2—O8—C48—C11ⁱ	−121.0 (3)

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

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Seven new metal–organic frameworks assembled from semi-rigid poly­car­box­yl­ate and auxiliary N-donor ligands: syntheses, structures and properties

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Seven new metal–organic frameworks assembled from semi-rigid polycarboxylate and auxiliary N-donor ligands: syntheses, structures and properties