Two novel Zn-MOFs: structures and characterization

Zheng, R.; Han, L.; Pan, Q.; Christensen, K.E.; Ren, T.

doi:10.1107/S0108768112007999

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Two novel Zn-MOFs: structures and characterization

R. Zheng, L. Han, Q. Pan, K. E. Christensen and T. Ren

Two novel three-dimensional Zn-MOFs (zinc metal-organic frameworks), Zn₅(μ₃-OH)(BTC)₃(Phen)₄·5H₂O (denoted as HUT-11) and Zn₄(μ₄-O)(BTC)₂(Phen)₂·4H₂O (denoted as HUT-12), have been synthesized by metal–ligand-directed assembly under hydrothermal conditions. Here, BTC and Phen are denoted as 1,3,5-benzenetricarboxylate and phenanthroline. HUT-11 contains two kinds of secondary building units (SBUs), Zn₃(μ₃-OH)(COO)₅ clusters and Zn₂(COO)₄ clusters. This material exhibits a new three-dimensional (3,4,5)-connected topology with the Schläfli symbol (4·6·8)₂(4·8²)(4·6⁴·8⁵)(4²·6²·8²). Two perpendicular planes cross at five coordinated Zn1—Zn3—Zn5 nodes, giving a new three-dimensional network. HUT-12 is composed of Zn₄(μ₄-O)(COO)₆ clusters as the secondary building units and displays a two-dimensional (3,6)-connected TiS₂ related net topology with the Schläfli symbol (4²·6)(4⁴·6²·8⁸·10). Both MOFs show blue light emission and a high thermal stability above 673 K.

Keywords: Zn metal-organic fragments; thermal stability; topology.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112007999/so5059sup1.cif Contains datablocks global, HUT-11, HUT-12
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768112007999/so5059HUT-11sup2.hkl Contains datablock HUT-11
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768112007999/so5059HUT-12sup3.hkl Contains datablock HUT-12

CCDC references: 879421; 879422

Computing details top

Data collection: CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) for HUT-11; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) for HUT-12. Cell refinement: CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) for HUT-11; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) for HUT-12. Data reduction: CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) for HUT-11; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) for HUT-12. For both compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 2008).

Figures top

(HUT-11) top

Crystal data top

C₇₅H₄₂N₈O₁₉Zn₅·H₂O·3.04(O)	F(000) = 7074.48
M_r = 1752.73	D_x = 1.672 Mg m⁻³
Monoclinic, C2/c	Synchrotron radiation, λ = 0.6889 Å
Hall symbol: -C 2yc	Cell parameters from 20652 reflections
a = 33.957 (3) Å	θ = 1.2–31.7°
b = 23.8834 (17) Å	µ = 1.64 mm⁻¹
c = 17.1688 (12) Å	T = 150 K
β = 90.079 (1)°	Prism, colorless
V = 13924.0 (19) Å³	0.04 × 0.03 × 0.03 mm
Z = 8

Data collection top

Rigaku Saturn724+ (2x2 bin mode) diffractometer	20944 independent reflections
Radiation source: Synchrotron	18223 reflections with I > 2σ(I)
Si-111 monochromator	R_int = 0.057
Detector resolution: 28.5714 pixels mm^-1	θ_max = 29.5°, θ_min = 1.5°
profile data from ω–scans	h = −48→48
Absorption correction: multi-scan ?	k = −33→33
T_min = 0.833, T_max = 1	l = −24→24
118881 measured reflections

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.092	All H-atom parameters refined
S = 1.06	w = 1/[σ²(F_o²) + (0.0374P)² + 26.1353P] where P = (F_o² + 2F_c²)/3
20944 reflections	(Δ/σ)_max = 0.004
1188 parameters	Δρ_max = 0.91 e Å⁻³
0 restraints	Δρ_min = −0.83 e Å⁻³

Crystal data top

C₇₅H₄₂N₈O₁₉Zn₅·H₂O·3.04(O)	V = 13924.0 (19) Å³
M_r = 1752.73	Z = 8
Monoclinic, C2/c	Synchrotron radiation, λ = 0.6889 Å
a = 33.957 (3) Å	µ = 1.64 mm⁻¹
b = 23.8834 (17) Å	T = 150 K
c = 17.1688 (12) Å	0.04 × 0.03 × 0.03 mm
β = 90.079 (1)°

Data collection top

Rigaku Saturn724+ (2x2 bin mode) diffractometer	20944 independent reflections
Absorption correction: multi-scan ?	18223 reflections with I > 2σ(I)
T_min = 0.833, T_max = 1	R_int = 0.057
118881 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	0 restraints
wR(F²) = 0.092	All H-atom parameters refined
S = 1.06	w = 1/[σ²(F_o²) + (0.0374P)² + 26.1353P] where P = (F_o² + 2F_c²)/3
20944 reflections	Δρ_max = 0.91 e Å⁻³
1188 parameters	Δρ_min = −0.83 e Å⁻³

Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 > 2σ(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	Occ. (<1)
Zn1	0.202889 (6)	0.152201 (10)	0.644086 (12)	0.01393 (5)
Zn2	0.276932 (6)	0.068840 (10)	0.702271 (13)	0.01462 (5)
Zn3	−0.030493 (6)	0.350710 (10)	0.842718 (13)	0.01556 (5)
Zn4	0.260426 (6)	0.191676 (10)	0.794078 (12)	0.01385 (5)
Zn5	0.027136 (6)	0.146031 (10)	1.161668 (12)	0.01509 (5)
N1	0.04369 (5)	0.06395 (8)	1.19615 (10)	0.0188 (3)
N2	−0.01645 (5)	0.09448 (9)	1.10316 (11)	0.0238 (4)
N3	−0.06900 (6)	0.40854 (9)	0.78714 (11)	0.0260 (4)
N4	−0.00342 (6)	0.42875 (9)	0.86913 (12)	0.0262 (4)
N5	0.21212 (5)	0.22575 (8)	0.86784 (10)	0.0177 (3)
N6	0.27194 (5)	0.15623 (7)	0.90443 (10)	0.0175 (3)
N7	0.18219 (5)	0.16329 (8)	0.52755 (9)	0.0173 (3)
N8	0.18818 (5)	0.06679 (7)	0.60723 (10)	0.0160 (3)
O1	0.31926 (4)	0.19006 (7)	0.76229 (9)	0.0207 (3)
O2	0.32927 (4)	0.10485 (6)	0.71066 (9)	0.0216 (3)
O3	−0.05452 (5)	0.32063 (7)	0.93871 (9)	0.0292 (4)
O4	−0.08798 (6)	0.39829 (8)	0.96712 (10)	0.0344 (4)
O5	0.43996 (4)	0.31768 (6)	0.75101 (8)	0.0191 (3)
O6	0.48692 (4)	0.29220 (7)	0.66657 (8)	0.0219 (3)
O7	0.05271 (5)	0.17974 (7)	1.07098 (9)	0.0238 (3)
O8	0.02282 (5)	0.31292 (7)	0.85588 (9)	0.0271 (3)
O9	0.04579 (5)	0.29211 (7)	0.73645 (9)	0.0259 (3)
O10	0.26365 (5)	0.14936 (7)	0.58995 (8)	0.0217 (3)
O11	0.15221 (4)	0.16115 (7)	0.70648 (8)	0.0215 (3)
O12	0.16784 (4)	0.10069 (7)	0.80184 (9)	0.0230 (3)
O13	0.28057 (5)	0.05933 (7)	0.58534 (9)	0.0228 (3)
O14	0.09730 (5)	0.11243 (7)	1.05293 (9)	0.0267 (3)
O15	0.25641 (4)	0.26584 (6)	0.73897 (8)	0.0209 (3)
O16	0.21230 (5)	0.23696 (6)	0.65008 (9)	0.0247 (3)
O17A	0.2731 (2)	0.03034 (12)	0.81639 (19)	0.0376 (12)	0.693 (15)
O17B	0.2989 (5)	0.0253 (3)	0.8240 (4)	0.043 (4)	0.307 (15)
O18	0.27309 (6)	−0.01963 (8)	0.71632 (11)	0.0415 (5)
O19	0.23747 (4)	0.12594 (6)	0.73774 (8)	0.0149 (3)
C1	0.37383 (5)	0.17645 (8)	0.67847 (11)	0.0149 (3)
C2	0.38375 (6)	0.15242 (9)	0.60689 (11)	0.0171 (4)
C3	0.41463 (6)	0.17406 (9)	0.56215 (11)	0.0183 (4)
C4	0.43673 (6)	0.21812 (9)	0.59222 (11)	0.0184 (4)
C5	0.42792 (5)	0.24103 (9)	0.66526 (11)	0.0166 (4)
C6	0.39571 (5)	0.22125 (9)	0.70745 (11)	0.0156 (3)
C7	0.33786 (5)	0.15564 (9)	0.72087 (11)	0.0161 (4)
C8	−0.07590 (6)	0.35107 (9)	0.98319 (12)	0.0203 (4)
C9	0.45345 (5)	0.28716 (9)	0.69698 (11)	0.0164 (4)
C10	0.02338 (6)	0.02238 (9)	1.15972 (12)	0.0209 (4)
C11	0.03288 (7)	−0.03469 (10)	1.16849 (14)	0.0294 (5)
C12	0.06526 (9)	−0.04797 (12)	1.21630 (16)	0.0357 (6)
C13	0.08545 (8)	−0.00632 (12)	1.25293 (15)	0.0329 (5)
C14	0.07371 (7)	0.04937 (10)	1.24203 (13)	0.0247 (4)
C15	−0.00925 (6)	0.03852 (10)	1.11120 (12)	0.0239 (4)
C16	−0.03236 (7)	−0.00284 (12)	1.07465 (14)	0.0309 (5)
C17	−0.02173 (9)	−0.06056 (13)	1.08491 (17)	0.0395 (7)
C18	0.00904 (9)	−0.07586 (12)	1.12914 (18)	0.0396 (6)
C19	−0.04664 (7)	0.11014 (13)	1.05939 (15)	0.0321 (5)
C20	−0.07171 (7)	0.07156 (15)	1.02210 (16)	0.0401 (7)
C21	−0.06463 (7)	0.01562 (14)	1.02967 (16)	0.0391 (7)
C22	0.21501 (6)	0.20840 (9)	0.94304 (11)	0.0170 (4)
C23	0.18910 (6)	0.22713 (9)	1.00204 (12)	0.0212 (4)
C24	0.16023 (6)	0.26640 (10)	0.98100 (14)	0.0269 (5)
C25	0.15790 (6)	0.28439 (10)	0.90531 (15)	0.0264 (5)
C26	0.18417 (6)	0.26254 (10)	0.84998 (13)	0.0225 (4)
C27	0.24579 (6)	0.16953 (9)	0.96162 (11)	0.0169 (4)
C28	0.24836 (7)	0.14730 (9)	1.03771 (12)	0.0221 (4)
C29	0.22133 (7)	0.16737 (11)	1.09611 (12)	0.0284 (5)
C30	0.19359 (7)	0.20557 (11)	1.07981 (12)	0.0275 (5)
C31	0.30006 (6)	0.11947 (10)	0.92025 (13)	0.0228 (4)
C32	0.30340 (8)	0.09269 (11)	0.99309 (14)	0.0294 (5)
C33	0.27745 (8)	0.10635 (11)	1.05171 (13)	0.0287 (5)
C34	0.17918 (5)	0.11500 (9)	0.48652 (11)	0.0170 (4)
C35	0.17351 (6)	0.11385 (10)	0.40494 (12)	0.0215 (4)
C36	0.17222 (7)	0.16576 (11)	0.36594 (13)	0.0264 (5)
C37	0.17527 (7)	0.21432 (11)	0.40806 (13)	0.0272 (5)
C38	0.17942 (6)	0.21117 (10)	0.48919 (13)	0.0221 (4)
C39	0.18169 (5)	0.06329 (9)	0.52930 (11)	0.0165 (4)
C40	0.17692 (6)	0.01168 (9)	0.48996 (13)	0.0210 (4)
C41	0.17183 (7)	0.01211 (11)	0.40660 (14)	0.0276 (5)
C42	0.17046 (7)	0.06067 (11)	0.36639 (13)	0.0277 (5)
C43	0.08368 (5)	0.17472 (9)	0.94813 (11)	0.0154 (3)
C44	0.06110 (5)	0.21857 (9)	0.91895 (11)	0.0171 (4)
C45	0.06589 (5)	0.23577 (9)	0.84184 (11)	0.0169 (4)
C46	0.09339 (6)	0.20913 (9)	0.79436 (11)	0.0172 (4)
C47	0.11618 (5)	0.16544 (8)	0.82338 (11)	0.0151 (3)
C48	0.11114 (5)	0.14814 (9)	0.90021 (11)	0.0154 (3)
C49	0.07831 (5)	0.15345 (9)	1.03035 (11)	0.0164 (4)
C50	0.04265 (6)	0.28398 (9)	0.80873 (12)	0.0195 (4)
C51	0.14782 (6)	0.13972 (9)	0.77385 (11)	0.0165 (4)
C52	0.27603 (8)	−0.01678 (11)	0.78762 (14)	0.0300 (5)
C53	0.27494 (6)	−0.06827 (9)	0.83759 (11)	0.0188 (4)
C54	0.27086 (6)	0.12133 (9)	0.30422 (11)	0.0181 (4)
C55	0.27701 (6)	0.06245 (9)	0.41857 (12)	0.0185 (4)
C56	0.27320 (6)	0.10615 (9)	0.55303 (11)	0.0177 (4)
C57	0.27483 (5)	0.10979 (9)	0.46558 (11)	0.0154 (3)
C58	0.27175 (6)	0.16243 (9)	0.43204 (11)	0.0165 (4)
C59	0.26987 (6)	0.16861 (9)	0.35136 (11)	0.0164 (4)
C60	−0.05924 (8)	0.46245 (11)	0.79908 (15)	0.0320 (5)
C61	−0.02418 (8)	0.47357 (11)	0.84319 (15)	0.0308 (5)
C62	−0.01273 (11)	0.52928 (13)	0.8581 (2)	0.0496 (8)
C63	0.02184 (13)	0.53675 (17)	0.9019 (3)	0.0637 (11)
C64	0.04286 (11)	0.49214 (17)	0.9271 (2)	0.0554 (9)
C65	0.02943 (8)	0.43775 (13)	0.90962 (17)	0.0379 (6)
C66	−0.10150 (8)	0.39717 (14)	0.74700 (17)	0.0388 (6)
C67	0.23350 (6)	0.27326 (9)	0.68182 (11)	0.0171 (4)
C68	0.18796 (6)	0.01995 (9)	0.64858 (12)	0.0198 (4)
C69	0.18214 (7)	−0.03306 (10)	0.61507 (15)	0.0259 (4)
C70	0.17728 (7)	−0.03700 (10)	0.53589 (15)	0.0266 (5)
C73	−0.08198 (11)	0.50748 (14)	0.7697 (2)	0.0536 (9)
C71	−0.12593 (10)	0.43849 (18)	0.7156 (2)	0.0593 (10)
C72	−0.11588 (12)	0.4932 (2)	0.7269 (3)	0.0691 (12)
C75	−0.03672 (17)	0.57380 (15)	0.8269 (3)	0.0734 (13)
C74	−0.06935 (17)	0.56317 (17)	0.7850 (3)	0.0778 (14)
H1	0.0962 (7)	0.2221 (11)	0.7418 (15)	0.020 (6)*
H2	0.4584 (8)	0.2318 (12)	0.5650 (16)	0.027 (7)*
H3	0.0420 (7)	0.2367 (11)	0.9504 (15)	0.018 (6)*
H4	0.0876 (8)	0.0791 (11)	1.2681 (15)	0.021 (6)*
H5	0.3702 (8)	0.1223 (12)	0.5881 (16)	0.026 (7)*
H6	0.1809 (8)	−0.0649 (12)	0.6493 (16)	0.025 (7)*
H7	0.1813 (8)	0.2437 (12)	0.5219 (16)	0.025 (7)*
H8	0.3883 (7)	0.2368 (11)	0.7561 (15)	0.019 (6)*
H9	0.1077 (10)	−0.0134 (13)	1.2870 (19)	0.043 (9)*
H10	0.0426 (9)	0.4039 (13)	0.9249 (18)	0.035 (8)*
H11	−0.0512 (8)	0.1502 (12)	1.0542 (16)	0.026 (7)*
H12	0.1262 (8)	0.1181 (12)	0.9180 (16)	0.027 (7)*
H13	−0.1074 (9)	0.3565 (13)	0.7391 (18)	0.034 (8)*
H14	0.1752 (7)	0.2204 (11)	1.1187 (15)	0.020 (6)*
H15	0.1677 (9)	0.0612 (13)	0.3127 (19)	0.039 (8)*
H16	0.2791 (8)	0.0267 (12)	0.4422 (16)	0.026 (7)*
H17	0.1695 (9)	0.1658 (13)	0.3117 (18)	0.035 (8)*
H18	0.2702 (7)	0.1951 (11)	0.4662 (15)	0.021 (6)*
H19	0.1730 (8)	−0.0714 (12)	0.5091 (17)	0.029 (7)*
H20	0.3176 (8)	0.1117 (11)	0.8810 (16)	0.022 (6)*
H21	0.1390 (8)	0.3126 (12)	0.8894 (17)	0.029 (7)*
H22	0.1701 (9)	−0.0217 (13)	0.3808 (18)	0.039 (8)*
H23	0.0166 (11)	−0.1130 (16)	1.136 (2)	0.056 (11)*
H24	0.0724 (10)	−0.0854 (14)	1.2192 (19)	0.044 (9)*
H25	0.1823 (8)	0.2751 (12)	0.7940 (17)	0.029 (7)*
H26	0.1909 (8)	0.0238 (11)	0.7075 (16)	0.025 (7)*
H27	−0.0384 (11)	−0.0855 (16)	1.059 (2)	0.061 (11)*
H28	0.3231 (9)	0.0651 (13)	0.9988 (18)	0.038 (8)*
H29	0.1752 (8)	0.2520 (12)	0.3843 (17)	0.030 (7)*
H30	0.1422 (9)	0.2804 (13)	1.0192 (19)	0.043 (9)*
H31	0.0305 (15)	0.576 (2)	0.913 (3)	0.109 (18)*
H32	−0.0800 (10)	−0.0109 (14)	1.005 (2)	0.048 (9)*
H33	0.2696 (8)	0.1254 (12)	0.2487 (17)	0.031 (7)*
H34	−0.1318 (12)	0.5213 (17)	0.706 (2)	0.071 (12)*
H36	−0.0289 (13)	0.609 (2)	0.839 (3)	0.081 (14)*
H37	0.0682 (12)	0.4952 (17)	0.955 (2)	0.067 (12)*
H38	−0.0928 (10)	0.0864 (14)	0.991 (2)	0.049 (9)*
H39	0.2787 (9)	0.0898 (13)	1.1024 (19)	0.038 (8)*
H40	−0.0860 (16)	0.594 (2)	0.765 (3)	0.114 (18)*
H41	0.2248 (9)	0.1526 (13)	1.1446 (19)	0.039 (8)*
H42	−0.1518 (13)	0.4274 (17)	0.686 (2)	0.076 (13)*
H50	0.2194 (9)	0.1142 (12)	0.7668 (18)	0.032 (8)*
OW1	0.36516 (5)	0.35554 (8)	0.80561 (10)	0.0301 (4)
H101	0.3865 (11)	0.3366 (15)	0.787 (2)	0.053 (10)*
H100	0.3755 (11)	0.3653 (15)	0.850 (2)	0.052 (10)*
OW2	0.08362 (9)	0.19245 (12)	0.58307 (18)	0.0711 (8)*
OW3	0.36037 (9)	0.01799 (13)	0.52534 (18)	0.0441 (10)*	0.710 (7)
OW4	0.37356 (18)	0.9937 (3)	0.4295 (4)	0.050 (2)*	0.373 (8)
OW5	0.6012 (2)	0.1210 (3)	0.5240 (4)	0.073 (3)*	0.429 (9)
OW6	0.4511 (3)	0.7957 (5)	0.3905 (7)	0.088 (5)*	0.310 (11)
OW7	0.4679 (4)	0.8150 (6)	0.4462 (8)	0.065 (5)*	0.215 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.02014 (10)	0.01147 (11)	0.01020 (9)	−0.00020 (8)	0.00209 (7)	−0.00041 (8)
Zn2	0.01870 (10)	0.01205 (11)	0.01311 (10)	−0.00033 (8)	0.00188 (7)	0.00153 (8)
Zn3	0.01826 (10)	0.01615 (12)	0.01228 (9)	0.00180 (8)	0.00227 (7)	−0.00008 (8)
Zn4	0.01782 (10)	0.01294 (11)	0.01081 (9)	−0.00090 (8)	0.00262 (7)	0.00049 (8)
Zn5	0.01558 (9)	0.01798 (12)	0.01170 (9)	0.00150 (8)	0.00263 (7)	−0.00008 (8)
N1	0.0213 (8)	0.0190 (9)	0.0162 (7)	−0.0021 (6)	0.0039 (6)	−0.0005 (6)
N2	0.0191 (8)	0.0319 (11)	0.0203 (8)	−0.0018 (7)	0.0020 (6)	−0.0056 (7)
N3	0.0270 (9)	0.0275 (11)	0.0235 (9)	0.0073 (8)	−0.0004 (7)	0.0009 (8)
N4	0.0260 (9)	0.0237 (10)	0.0290 (10)	−0.0005 (7)	0.0002 (7)	−0.0028 (8)
N5	0.0203 (7)	0.0166 (9)	0.0163 (7)	−0.0020 (6)	0.0028 (6)	−0.0008 (6)
N6	0.0212 (7)	0.0171 (9)	0.0142 (7)	−0.0021 (6)	−0.0001 (6)	−0.0008 (6)
N7	0.0201 (7)	0.0172 (9)	0.0145 (7)	0.0004 (6)	0.0004 (6)	0.0006 (6)
N8	0.0167 (7)	0.0149 (8)	0.0162 (7)	−0.0007 (6)	0.0015 (6)	−0.0009 (6)
O1	0.0187 (6)	0.0225 (8)	0.0210 (7)	−0.0035 (6)	0.0077 (5)	−0.0025 (6)
O2	0.0171 (6)	0.0150 (8)	0.0327 (8)	−0.0018 (5)	0.0014 (6)	0.0031 (6)
O3	0.0406 (9)	0.0281 (9)	0.0189 (7)	0.0083 (7)	0.0145 (6)	0.0040 (6)
O4	0.0461 (10)	0.0328 (10)	0.0243 (8)	0.0147 (8)	0.0129 (7)	0.0093 (7)
O5	0.0183 (6)	0.0212 (8)	0.0177 (6)	0.0000 (5)	0.0012 (5)	−0.0041 (6)
O6	0.0197 (6)	0.0273 (9)	0.0187 (7)	−0.0084 (6)	0.0063 (5)	−0.0021 (6)
O7	0.0265 (7)	0.0277 (9)	0.0172 (7)	0.0059 (6)	0.0098 (6)	0.0038 (6)
O8	0.0275 (8)	0.0288 (9)	0.0250 (8)	0.0143 (7)	−0.0009 (6)	−0.0044 (7)
O9	0.0291 (8)	0.0272 (9)	0.0213 (7)	0.0084 (6)	0.0049 (6)	0.0083 (6)
O10	0.0284 (7)	0.0228 (8)	0.0139 (6)	0.0002 (6)	0.0048 (5)	0.0004 (6)
O11	0.0271 (7)	0.0228 (8)	0.0147 (6)	0.0062 (6)	0.0080 (5)	0.0026 (6)
O12	0.0249 (7)	0.0191 (8)	0.0250 (7)	0.0076 (6)	0.0119 (6)	0.0079 (6)
O13	0.0315 (8)	0.0208 (8)	0.0160 (7)	−0.0023 (6)	0.0001 (6)	0.0055 (6)
O14	0.0363 (8)	0.0285 (9)	0.0154 (7)	0.0115 (7)	0.0038 (6)	0.0041 (6)
O15	0.0306 (7)	0.0173 (8)	0.0149 (6)	−0.0008 (6)	−0.0008 (5)	0.0046 (5)
O16	0.0395 (9)	0.0121 (8)	0.0225 (7)	−0.0030 (6)	−0.0025 (6)	0.0005 (6)
O17A	0.061 (3)	0.0111 (13)	0.0411 (16)	−0.0002 (13)	0.0006 (16)	0.0082 (11)
O17B	0.088 (11)	0.018 (3)	0.023 (3)	−0.018 (4)	0.008 (4)	0.002 (2)
O18	0.0560 (12)	0.0356 (11)	0.0327 (9)	−0.0114 (9)	−0.0123 (8)	0.0228 (8)
O19	0.0184 (6)	0.0144 (7)	0.0120 (6)	−0.0024 (5)	0.0044 (5)	−0.0009 (5)
C1	0.0151 (7)	0.0142 (9)	0.0154 (8)	0.0012 (6)	0.0031 (6)	0.0016 (7)
C2	0.0180 (8)	0.0162 (10)	0.0171 (8)	−0.0008 (7)	0.0013 (7)	0.0005 (7)
C3	0.0212 (8)	0.0202 (11)	0.0136 (8)	−0.0001 (7)	0.0049 (7)	−0.0002 (7)
C4	0.0197 (8)	0.0209 (11)	0.0147 (8)	−0.0015 (7)	0.0054 (7)	−0.0005 (7)
C5	0.0167 (8)	0.0181 (10)	0.0150 (8)	−0.0016 (7)	0.0026 (6)	0.0009 (7)
C6	0.0161 (8)	0.0178 (10)	0.0129 (8)	0.0011 (7)	0.0033 (6)	0.0015 (7)
C7	0.0153 (8)	0.0197 (10)	0.0134 (8)	−0.0010 (7)	0.0003 (6)	0.0047 (7)
C8	0.0238 (9)	0.0213 (11)	0.0158 (8)	0.0001 (8)	0.0040 (7)	0.0035 (8)
C9	0.0182 (8)	0.0176 (10)	0.0134 (8)	−0.0031 (7)	0.0019 (6)	0.0020 (7)
C10	0.0240 (9)	0.0211 (11)	0.0175 (9)	−0.0036 (8)	0.0072 (7)	−0.0029 (8)
C11	0.0381 (12)	0.0201 (12)	0.0299 (11)	−0.0047 (9)	0.0111 (9)	−0.0042 (9)
C12	0.0500 (15)	0.0195 (13)	0.0375 (14)	0.0050 (11)	0.0051 (11)	0.0050 (10)
C13	0.0376 (13)	0.0293 (14)	0.0316 (12)	0.0057 (10)	−0.0023 (10)	0.0063 (10)
C14	0.0263 (10)	0.0256 (12)	0.0223 (10)	−0.0011 (9)	0.0010 (8)	0.0033 (9)
C15	0.0215 (9)	0.0292 (13)	0.0210 (9)	−0.0066 (8)	0.0062 (7)	−0.0077 (9)
C16	0.0279 (10)	0.0377 (15)	0.0271 (11)	−0.0128 (10)	0.0079 (9)	−0.0132 (10)
C17	0.0430 (14)	0.0350 (16)	0.0407 (15)	−0.0192 (12)	0.0113 (12)	−0.0159 (12)
C18	0.0545 (17)	0.0232 (14)	0.0410 (15)	−0.0111 (12)	0.0118 (12)	−0.0087 (11)
C19	0.0240 (10)	0.0450 (17)	0.0274 (11)	0.0037 (10)	−0.0024 (8)	−0.0079 (11)
C20	0.0218 (11)	0.068 (2)	0.0302 (12)	−0.0014 (12)	−0.0025 (9)	−0.0122 (13)
C21	0.0268 (11)	0.057 (2)	0.0335 (13)	−0.0152 (12)	0.0012 (9)	−0.0201 (13)
C22	0.0199 (8)	0.0162 (10)	0.0149 (8)	−0.0060 (7)	0.0029 (6)	−0.0038 (7)
C23	0.0230 (9)	0.0216 (11)	0.0190 (9)	−0.0087 (8)	0.0075 (7)	−0.0075 (8)
C24	0.0214 (9)	0.0266 (13)	0.0327 (11)	−0.0045 (8)	0.0090 (8)	−0.0138 (10)
C25	0.0205 (9)	0.0223 (12)	0.0364 (12)	0.0012 (8)	0.0035 (8)	−0.0085 (9)
C26	0.0233 (9)	0.0206 (11)	0.0237 (10)	0.0010 (8)	0.0009 (7)	−0.0012 (8)
C27	0.0234 (9)	0.0149 (10)	0.0124 (8)	−0.0073 (7)	0.0017 (6)	−0.0007 (7)
C28	0.0321 (10)	0.0211 (11)	0.0130 (8)	−0.0104 (8)	−0.0009 (7)	0.0009 (7)
C29	0.0394 (12)	0.0341 (14)	0.0116 (8)	−0.0161 (10)	0.0033 (8)	0.0003 (9)
C30	0.0333 (11)	0.0336 (14)	0.0157 (9)	−0.0135 (10)	0.0094 (8)	−0.0070 (9)
C31	0.0255 (10)	0.0195 (11)	0.0233 (10)	0.0009 (8)	−0.0021 (8)	−0.0005 (8)
C32	0.0380 (12)	0.0220 (12)	0.0283 (11)	0.0014 (10)	−0.0091 (9)	0.0050 (9)
C33	0.0410 (13)	0.0265 (13)	0.0187 (10)	−0.0085 (10)	−0.0080 (9)	0.0059 (9)
C34	0.0155 (8)	0.0209 (11)	0.0147 (8)	−0.0007 (7)	0.0011 (6)	−0.0009 (7)
C35	0.0200 (9)	0.0296 (12)	0.0150 (8)	−0.0007 (8)	−0.0005 (7)	−0.0029 (8)
C36	0.0252 (10)	0.0390 (14)	0.0150 (9)	0.0023 (9)	−0.0030 (7)	0.0031 (9)
C37	0.0300 (11)	0.0294 (13)	0.0221 (10)	0.0047 (9)	−0.0023 (8)	0.0083 (9)
C38	0.0263 (10)	0.0188 (11)	0.0210 (9)	0.0018 (8)	−0.0022 (7)	0.0029 (8)
C39	0.0165 (8)	0.0163 (10)	0.0168 (8)	−0.0007 (7)	0.0022 (6)	−0.0033 (7)
C40	0.0196 (8)	0.0184 (11)	0.0251 (10)	−0.0017 (7)	−0.0007 (7)	−0.0080 (8)
C41	0.0258 (10)	0.0308 (13)	0.0262 (11)	−0.0024 (9)	−0.0013 (8)	−0.0153 (10)
C42	0.0274 (10)	0.0375 (14)	0.0184 (9)	−0.0036 (9)	−0.0022 (8)	−0.0104 (9)
C43	0.0155 (7)	0.0179 (10)	0.0129 (8)	0.0000 (7)	0.0031 (6)	−0.0005 (7)
C44	0.0154 (8)	0.0203 (11)	0.0156 (8)	0.0017 (7)	0.0041 (6)	−0.0007 (7)
C45	0.0174 (8)	0.0167 (10)	0.0165 (8)	0.0022 (7)	0.0029 (6)	0.0010 (7)
C46	0.0201 (8)	0.0185 (10)	0.0130 (8)	0.0023 (7)	0.0024 (6)	0.0010 (7)
C47	0.0179 (8)	0.0133 (9)	0.0142 (8)	0.0008 (7)	0.0052 (6)	−0.0008 (7)
C48	0.0157 (8)	0.0157 (10)	0.0149 (8)	0.0018 (7)	0.0017 (6)	0.0000 (7)
C49	0.0171 (8)	0.0207 (10)	0.0114 (7)	−0.0010 (7)	0.0033 (6)	−0.0012 (7)
C50	0.0182 (8)	0.0201 (11)	0.0203 (9)	0.0025 (7)	0.0004 (7)	0.0017 (8)
C51	0.0190 (8)	0.0142 (10)	0.0164 (8)	0.0013 (7)	0.0058 (6)	0.0013 (7)
C52	0.0384 (12)	0.0216 (12)	0.0301 (11)	0.0013 (9)	0.0118 (9)	0.0095 (9)
C53	0.0266 (9)	0.0141 (10)	0.0158 (8)	−0.0010 (7)	0.0039 (7)	0.0048 (7)
C54	0.0246 (9)	0.0174 (10)	0.0122 (8)	−0.0004 (7)	0.0019 (6)	−0.0021 (7)
C55	0.0242 (9)	0.0126 (10)	0.0187 (9)	0.0017 (7)	0.0040 (7)	0.0003 (7)
C56	0.0185 (8)	0.0207 (11)	0.0140 (8)	−0.0032 (7)	0.0012 (6)	0.0029 (7)
C57	0.0183 (8)	0.0165 (10)	0.0116 (7)	−0.0009 (7)	0.0022 (6)	0.0005 (7)
C58	0.0232 (9)	0.0147 (10)	0.0115 (8)	−0.0014 (7)	0.0026 (6)	−0.0030 (7)
C59	0.0220 (8)	0.0137 (10)	0.0136 (8)	−0.0007 (7)	0.0025 (6)	0.0015 (7)
C60	0.0382 (12)	0.0257 (13)	0.0321 (12)	0.0132 (10)	0.0046 (10)	0.0028 (10)
C61	0.0417 (13)	0.0190 (12)	0.0318 (12)	0.0021 (10)	0.0055 (10)	−0.0009 (9)
C62	0.074 (2)	0.0217 (15)	0.0532 (18)	−0.0044 (14)	0.0075 (16)	−0.0052 (13)
C63	0.082 (3)	0.038 (2)	0.071 (3)	−0.0235 (19)	−0.003 (2)	−0.0074 (18)
C64	0.0536 (19)	0.059 (2)	0.0536 (19)	−0.0277 (17)	−0.0028 (15)	−0.0112 (17)
C65	0.0345 (13)	0.0406 (17)	0.0387 (14)	−0.0055 (11)	−0.0053 (11)	−0.0062 (12)
C66	0.0288 (12)	0.0499 (19)	0.0375 (14)	0.0095 (12)	−0.0067 (10)	−0.0040 (13)
C67	0.0254 (9)	0.0129 (9)	0.0130 (8)	0.0005 (7)	0.0068 (7)	0.0004 (7)
C68	0.0212 (9)	0.0160 (10)	0.0221 (9)	−0.0010 (7)	0.0019 (7)	0.0008 (8)
C69	0.0276 (10)	0.0150 (11)	0.0353 (12)	−0.0028 (8)	0.0002 (9)	0.0030 (9)
C70	0.0258 (10)	0.0145 (11)	0.0397 (13)	−0.0026 (8)	−0.0040 (9)	−0.0083 (9)
C73	0.064 (2)	0.0385 (18)	0.058 (2)	0.0292 (16)	−0.0029 (16)	0.0037 (15)
C71	0.0452 (17)	0.076 (3)	0.057 (2)	0.0287 (17)	−0.0189 (15)	−0.0067 (19)
C72	0.063 (2)	0.074 (3)	0.070 (2)	0.045 (2)	−0.0176 (19)	0.005 (2)
C75	0.119 (4)	0.0151 (17)	0.086 (3)	0.0084 (19)	0.006 (3)	−0.0025 (17)
C74	0.111 (4)	0.034 (2)	0.088 (3)	0.035 (2)	−0.006 (3)	0.006 (2)
OW1	0.0222 (7)	0.0452 (12)	0.0228 (8)	0.0008 (7)	0.0019 (6)	−0.0034 (7)

Geometric parameters (Å, º) top

Zn1—O11	2.0395 (14)	C19—H11	0.97 (3)
Zn1—O16	2.0519 (16)	C20—C21	1.364 (5)
Zn1—O19	2.0862 (14)	C20—H38	0.96 (3)
Zn1—N7	2.1362 (17)	C21—H32	0.92 (3)
Zn1—N8	2.1933 (17)	C22—C23	1.415 (3)
Zn1—O10	2.2650 (15)	C22—C27	1.434 (3)
Zn2—O2	1.9794 (14)	C23—C24	1.403 (3)
Zn2—O19	2.0072 (14)	C23—C30	1.439 (3)
Zn2—O13	2.0243 (15)	C24—C25	1.371 (4)
Zn2—O18	2.131 (2)	C24—H30	0.96 (3)
Zn2—O17A	2.168 (3)	C25—C26	1.405 (3)
Zn2—O17B	2.450 (11)	C25—H21	0.97 (3)
Zn2—C52	2.516 (2)	C26—H25	1.01 (3)
Zn3—O3	1.9752 (15)	C27—C28	1.413 (3)
Zn3—O9ⁱ	2.0186 (16)	C28—C33	1.411 (3)
Zn3—O8	2.0353 (15)	C28—C29	1.442 (3)
Zn3—N4	2.127 (2)	C29—C30	1.341 (4)
Zn3—N3	2.1272 (19)	C29—H41	0.91 (3)
Zn4—O19	2.0016 (14)	C30—H14	0.98 (3)
Zn4—O15	2.0127 (15)	C31—C32	1.409 (3)
Zn4—O1	2.0721 (14)	C31—H20	0.92 (3)
Zn4—N6	2.1112 (17)	C32—C33	1.378 (4)
Zn4—N5	2.2276 (17)	C32—H28	0.94 (3)
Zn5—O7	1.9572 (15)	C33—H39	0.96 (3)
Zn5—O6ⁱⁱ	2.0122 (15)	C34—C35	1.414 (3)
Zn5—O5ⁱⁱⁱ	2.0597 (14)	C34—C39	1.439 (3)
Zn5—N1	2.1234 (18)	C35—C36	1.410 (3)
Zn5—N2	2.1706 (19)	C35—C42	1.436 (3)
N1—C14	1.334 (3)	C36—C37	1.371 (4)
N1—C10	1.361 (3)	C36—H17	0.94 (3)
N2—C19	1.324 (3)	C37—C38	1.402 (3)
N2—C15	1.366 (3)	C37—H29	0.99 (3)
N3—C66	1.329 (3)	C38—H7	0.96 (3)
N3—C60	1.345 (3)	C39—C40	1.415 (3)
N4—C65	1.331 (3)	C40—C70	1.405 (3)
N4—C61	1.357 (3)	C40—C41	1.441 (3)
N5—C26	1.329 (3)	C41—C42	1.351 (4)
N5—C22	1.359 (2)	C41—H22	0.92 (3)
N6—C31	1.325 (3)	C42—H15	0.93 (3)
N6—C27	1.362 (2)	C43—C44	1.391 (3)
N7—C38	1.323 (3)	C43—C48	1.397 (3)
N7—C34	1.355 (3)	C43—C49	1.511 (3)
N8—C68	1.325 (3)	C44—C45	1.396 (3)
N8—C39	1.358 (2)	C44—H3	0.95 (3)
O1—C7	1.258 (2)	C45—C46	1.394 (3)
O2—C7	1.260 (3)	C45—C50	1.507 (3)
O3—C8	1.281 (3)	C46—C47	1.391 (3)
O4—C8	1.231 (3)	C46—H1	0.96 (3)
O5—C9	1.266 (2)	C47—C48	1.393 (3)
O5—Zn5ⁱⁱⁱ	2.0597 (14)	C47—C51	1.503 (3)
O6—C9	1.257 (2)	C48—H12	0.93 (3)
O6—Zn5^iv	2.0122 (15)	C52—C53	1.500 (3)
O7—C49	1.280 (2)	C53—C54^v	1.398 (3)
O8—C50	1.260 (2)	C53—C55^v	1.399 (3)
O9—C50	1.261 (2)	C54—C59	1.390 (3)
O9—Zn3ⁱ	2.0186 (16)	C54—C53^vi	1.398 (3)
O10—C56	1.254 (3)	C54—H33	0.96 (3)
O11—C51	1.274 (2)	C55—C57	1.391 (3)
O12—C51	1.249 (2)	C55—C53^vi	1.399 (3)
O13—C56	1.273 (3)	C55—H16	0.95 (3)
O14—C49	1.235 (3)	C56—C57	1.505 (3)
O15—C67	1.264 (2)	C57—C58	1.387 (3)
O16—C67	1.251 (3)	C58—C59	1.394 (3)
O17A—O17B	0.897 (14)	C58—H18	0.98 (3)
O17A—C52	1.233 (4)	C59—C67^vii	1.505 (3)
O17B—C52	1.415 (10)	C60—C73	1.417 (4)
O18—C52	1.230 (3)	C60—C61	1.435 (4)
O19—H50	0.84 (3)	C61—C62	1.409 (4)
C1—C6	1.394 (3)	C62—C63	1.405 (5)
C1—C2	1.398 (3)	C62—C75	1.441 (6)
C1—C7	1.507 (3)	C63—C64	1.354 (6)
C2—C3	1.400 (3)	C63—H31	1.00 (5)
C2—H5	0.91 (3)	C64—C65	1.409 (4)
C3—C4	1.391 (3)	C64—H37	0.99 (4)
C3—C8^iv	1.517 (3)	C65—H10	0.96 (3)
C4—C5	1.401 (3)	C66—C71	1.397 (4)
C4—H2	0.93 (3)	C66—H13	1.00 (3)
C5—C6	1.395 (2)	C67—C59^vii	1.505 (3)
C5—C9	1.504 (3)	C68—C69	1.404 (3)
C6—H8	0.95 (3)	C68—H26	1.02 (3)
C8—C3ⁱⁱ	1.517 (3)	C69—C70	1.372 (3)
C10—C11	1.409 (3)	C69—H6	0.96 (3)
C10—C15	1.438 (3)	C70—H19	0.95 (3)
C11—C12	1.407 (4)	C73—C72	1.407 (6)
C11—C18	1.441 (4)	C73—C74	1.422 (6)
C12—C13	1.362 (4)	C71—C72	1.364 (6)
C12—H24	0.93 (3)	C71—H42	1.05 (4)
C13—C14	1.401 (4)	C72—H34	0.93 (4)
C13—H9	0.97 (3)	C75—C74	1.345 (7)
C14—H4	0.96 (3)	C75—H36	0.91 (5)
C15—C16	1.409 (3)	C74—H40	0.99 (5)
C16—C21	1.410 (4)	OW1—H101	0.91 (4)
C16—C17	1.436 (4)	OW1—H100	0.87 (4)
C17—C18	1.342 (5)	OW3—OW4^viii	1.801 (7)
C17—H27	0.94 (4)	OW4—OW3^ix	1.801 (7)
C18—H23	0.93 (4)	OW6—OW7	1.205 (16)
C19—C20	1.408 (4)

O11—Zn1—O16	90.10 (7)	C21—C20—H38	123 (2)
O11—Zn1—O19	95.80 (6)	C19—C20—H38	117 (2)
O16—Zn1—O19	99.82 (6)	C20—C21—C16	119.7 (2)
O11—Zn1—N7	101.67 (6)	C20—C21—H32	122 (2)
O16—Zn1—N7	88.61 (7)	C16—C21—H32	118 (2)
O19—Zn1—N7	160.61 (6)	N5—C22—C23	122.6 (2)
O11—Zn1—N8	93.27 (6)	N5—C22—C27	117.40 (17)
O16—Zn1—N8	165.34 (6)	C23—C22—C27	119.95 (18)
O19—Zn1—N8	94.03 (6)	C24—C23—C22	117.5 (2)
N7—Zn1—N8	76.74 (7)	C24—C23—C30	123.4 (2)
O11—Zn1—O10	171.24 (6)	C22—C23—C30	119.1 (2)
O16—Zn1—O10	84.73 (6)	C25—C24—C23	119.5 (2)
O19—Zn1—O10	78.19 (5)	C25—C24—H30	120 (2)
N7—Zn1—O10	85.30 (6)	C23—C24—H30	120 (2)
N8—Zn1—O10	93.50 (6)	C24—C25—C26	119.3 (2)
O2—Zn2—O19	106.41 (6)	C24—C25—H21	121.5 (17)
O2—Zn2—O13	93.72 (7)	C26—C25—H21	119.2 (17)
O19—Zn2—O13	114.76 (6)	N5—C26—C25	122.9 (2)
O2—Zn2—O18	118.53 (7)	N5—C26—H25	117.4 (16)
O19—Zn2—O18	126.76 (7)	C25—C26—H25	119.7 (16)
O13—Zn2—O18	90.28 (7)	N6—C27—C28	122.6 (2)
O2—Zn2—O17A	100.03 (18)	N6—C27—C22	117.81 (17)
O19—Zn2—O17A	88.42 (14)	C28—C27—C22	119.54 (18)
O13—Zn2—O17A	148.47 (9)	C33—C28—C27	117.4 (2)
O18—Zn2—O17A	58.23 (10)	C33—C28—C29	123.9 (2)
O2—Zn2—O17B	81.4 (3)	C27—C28—C29	118.7 (2)
O19—Zn2—O17B	103.5 (3)	C30—C29—C28	121.9 (2)
O13—Zn2—O17B	141.2 (3)	C30—C29—H41	123 (2)
O18—Zn2—O17B	60.06 (16)	C28—C29—H41	115 (2)
O17A—Zn2—O17B	21.3 (3)	C29—C30—C23	120.7 (2)
O2—Zn2—C52	108.81 (8)	C29—C30—H14	123.5 (15)
O19—Zn2—C52	111.52 (7)	C23—C30—H14	115.8 (15)
O13—Zn2—C52	119.16 (8)	N6—C31—C32	122.7 (2)
O18—Zn2—C52	29.22 (8)	N6—C31—H20	116.8 (17)
O17A—Zn2—C52	29.35 (10)	C32—C31—H20	120.5 (17)
O17B—Zn2—C52	33.1 (2)	C33—C32—C31	119.4 (2)
O3—Zn3—O9ⁱ	101.74 (7)	C33—C32—H28	122.9 (19)
O3—Zn3—O8	96.57 (7)	C31—C32—H28	117.7 (19)
O9ⁱ—Zn3—O8	89.73 (7)	C32—C33—C28	119.2 (2)
O3—Zn3—N4	108.65 (8)	C32—C33—H39	122.6 (18)
O9ⁱ—Zn3—N4	149.54 (7)	C28—C33—H39	118.2 (18)
O8—Zn3—N4	88.90 (7)	N7—C34—C35	122.79 (19)
O3—Zn3—N3	110.86 (7)	N7—C34—C39	117.43 (17)
O9ⁱ—Zn3—N3	89.47 (8)	C35—C34—C39	119.79 (19)
O8—Zn3—N3	152.12 (7)	C36—C35—C34	117.2 (2)
N4—Zn3—N3	77.99 (8)	C36—C35—C42	123.8 (2)
O19—Zn4—O15	115.92 (6)	C34—C35—C42	118.9 (2)
O19—Zn4—O1	103.49 (6)	C37—C36—C35	119.4 (2)
O15—Zn4—O1	87.55 (6)	C37—C36—H17	122.2 (19)
O19—Zn4—N6	100.99 (6)	C35—C36—H17	118.4 (19)
O15—Zn4—N6	141.92 (6)	C36—C37—C38	119.1 (2)
O1—Zn4—N6	92.95 (6)	C36—C37—H29	123.6 (17)
O19—Zn4—N5	105.94 (6)	C38—C37—H29	117.3 (17)
O15—Zn4—N5	84.04 (6)	N7—C38—C37	123.2 (2)
O1—Zn4—N5	150.17 (6)	N7—C38—H7	113.8 (17)
N6—Zn4—N5	76.82 (6)	C37—C38—H7	123.0 (17)
O7—Zn5—O6ⁱⁱ	91.93 (6)	N8—C39—C40	122.82 (19)
O7—Zn5—O5ⁱⁱⁱ	99.50 (7)	N8—C39—C34	117.35 (18)
O6ⁱⁱ—Zn5—O5ⁱⁱⁱ	91.64 (6)	C40—C39—C34	119.82 (18)
O7—Zn5—N1	118.95 (6)	C70—C40—C39	116.9 (2)
O6ⁱⁱ—Zn5—N1	147.64 (6)	C70—C40—C41	124.3 (2)
O5ⁱⁱⁱ—Zn5—N1	92.43 (6)	C39—C40—C41	118.8 (2)
O7—Zn5—N2	99.69 (7)	C42—C41—C40	121.2 (2)
O6ⁱⁱ—Zn5—N2	88.45 (7)	C42—C41—H22	120 (2)
O5ⁱⁱⁱ—Zn5—N2	160.80 (7)	C40—C41—H22	119 (2)
N1—Zn5—N2	77.61 (7)	C41—C42—C35	121.4 (2)
C14—N1—C10	117.9 (2)	C41—C42—H15	121.6 (19)
C14—N1—Zn5	127.41 (16)	C35—C42—H15	116.9 (19)
C10—N1—Zn5	114.31 (14)	C44—C43—C48	119.88 (17)
C19—N2—C15	118.2 (2)	C44—C43—C49	121.50 (17)
C19—N2—Zn5	128.99 (19)	C48—C43—C49	118.59 (18)
C15—N2—Zn5	112.74 (14)	C43—C44—C45	119.89 (17)
C66—N3—C60	118.6 (2)	C43—C44—H3	121.1 (15)
C66—N3—Zn3	127.6 (2)	C45—C44—H3	119.0 (15)
C60—N3—Zn3	113.69 (16)	C46—C45—C44	119.95 (18)
C65—N4—C61	118.6 (2)	C46—C45—C50	118.63 (17)
C65—N4—Zn3	127.93 (19)	C44—C45—C50	121.40 (17)
C61—N4—Zn3	113.40 (16)	C47—C46—C45	120.38 (17)
C26—N5—C22	118.11 (18)	C47—C46—H1	121.6 (15)
C26—N5—Zn4	129.54 (14)	C45—C46—H1	118.0 (15)
C22—N5—Zn4	112.11 (13)	C46—C47—C48	119.52 (17)
C31—N6—C27	118.50 (18)	C46—C47—C51	120.13 (17)
C31—N6—Zn4	125.60 (14)	C48—C47—C51	120.23 (17)
C27—N6—Zn4	115.67 (14)	C47—C48—C43	120.38 (18)
C38—N7—C34	118.14 (18)	C47—C48—H12	118.1 (17)
C38—N7—Zn1	126.62 (15)	C43—C48—H12	121.5 (17)
C34—N7—Zn1	113.94 (13)	O14—C49—O7	124.95 (18)
C68—N8—C39	118.35 (18)	O14—C49—C43	119.76 (17)
C68—N8—Zn1	129.22 (14)	O7—C49—C43	115.26 (18)
C39—N8—Zn1	112.20 (13)	O8—C50—O9	126.4 (2)
C7—O1—Zn4	130.26 (13)	O8—C50—C45	117.19 (18)
C7—O2—Zn2	129.51 (13)	O9—C50—C45	116.36 (18)
C8—O3—Zn3	121.75 (15)	O12—C51—O11	125.78 (18)
C9—O5—Zn5ⁱⁱⁱ	125.39 (13)	O12—C51—C47	118.46 (17)
C9—O6—Zn5^iv	134.55 (15)	O11—C51—C47	115.74 (17)
C49—O7—Zn5	122.29 (14)	O18—C52—O17A	116.3 (3)
C50—O8—Zn3	130.39 (14)	O18—C52—O17B	121.5 (3)
C50—O9—Zn3ⁱ	138.38 (15)	O18—C52—C53	121.5 (2)
C56—O10—Zn1	117.93 (13)	O17A—C52—C53	121.1 (2)
C51—O11—Zn1	122.33 (13)	O17B—C52—C53	110.1 (4)
C56—O13—Zn2	108.75 (13)	O18—C52—Zn2	57.74 (13)
C67—O15—Zn4	121.98 (14)	O17A—C52—Zn2	59.51 (17)
C67—O16—Zn1	142.65 (15)	O17B—C52—Zn2	70.9 (4)
O17B—O17A—C52	81.6 (5)	C53—C52—Zn2	179.0 (2)
O17B—O17A—Zn2	97.3 (6)	C54^v—C53—C55^v	120.15 (18)
C52—O17A—Zn2	91.1 (2)	C54^v—C53—C52	120.75 (19)
O17A—O17B—C52	59.6 (7)	C55^v—C53—C52	119.1 (2)
O17A—O17B—Zn2	61.4 (6)	C59—C54—C53^vi	120.03 (18)
C52—O17B—Zn2	76.0 (5)	C59—C54—H33	119.7 (18)
C52—O18—Zn2	93.04 (17)	C53^vi—C54—H33	120.2 (18)
Zn4—O19—Zn2	114.82 (7)	C57—C55—C53^vi	119.55 (19)
Zn4—O19—Zn1	110.80 (7)	C57—C55—H16	119.2 (17)
Zn2—O19—Zn1	110.23 (6)	C53^vi—C55—H16	121.2 (17)
Zn4—O19—H50	105 (2)	O10—C56—O13	123.60 (18)
Zn2—O19—H50	116 (2)	O10—C56—C57	117.82 (18)
Zn1—O19—H50	98 (2)	O13—C56—C57	118.55 (18)
C6—C1—C2	119.99 (17)	C58—C57—C55	120.00 (17)
C6—C1—C7	120.84 (17)	C58—C57—C56	117.63 (17)
C2—C1—C7	119.05 (18)	C55—C57—C56	122.27 (18)
C1—C2—C3	120.83 (19)	C57—C58—C59	120.78 (18)
C1—C2—H5	120.7 (17)	C57—C58—H18	118.6 (15)
C3—C2—H5	118.4 (17)	C59—C58—H18	120.6 (15)
C4—C3—C2	118.66 (18)	C54—C59—C58	119.43 (19)
C4—C3—C8^iv	121.05 (17)	C54—C59—C67^vii	122.08 (17)
C2—C3—C8^iv	120.27 (19)	C58—C59—C67^vii	118.49 (18)
C3—C4—C5	120.78 (18)	N3—C60—C73	122.6 (3)
C3—C4—H2	120.3 (17)	N3—C60—C61	117.5 (2)
C5—C4—H2	118.8 (17)	C73—C60—C61	119.9 (3)
C6—C5—C4	120.08 (19)	N4—C61—C62	122.8 (3)
C6—C5—C9	120.80 (17)	N4—C61—C60	117.2 (2)
C4—C5—C9	119.12 (17)	C62—C61—C60	119.9 (3)
C1—C6—C5	119.49 (18)	C63—C62—C61	116.5 (3)
C1—C6—H8	118.2 (15)	C63—C62—C75	125.2 (4)
C5—C6—H8	122.3 (15)	C61—C62—C75	118.3 (4)
O1—C7—O2	126.27 (18)	C64—C63—C62	120.8 (3)
O1—C7—C1	117.73 (18)	C64—C63—H31	121 (3)
O2—C7—C1	115.99 (17)	C62—C63—H31	118 (3)
O4—C8—O3	125.11 (19)	C63—C64—C65	119.2 (3)
O4—C8—C3ⁱⁱ	119.45 (19)	C63—C64—H37	124 (2)
O3—C8—C3ⁱⁱ	115.42 (19)	C65—C64—H37	117 (2)
O6—C9—O5	125.27 (19)	N4—C65—C64	122.1 (3)
O6—C9—C5	116.15 (17)	N4—C65—H10	113.4 (19)
O5—C9—C5	118.58 (16)	C64—C65—H10	124.5 (19)
N1—C10—C11	122.8 (2)	N3—C66—C71	123.2 (3)
N1—C10—C15	117.4 (2)	N3—C66—H13	115.8 (18)
C11—C10—C15	119.8 (2)	C71—C66—H13	120.9 (18)
C12—C11—C10	117.3 (2)	O16—C67—O15	126.44 (19)
C12—C11—C18	123.9 (3)	O16—C67—C59^vii	115.53 (18)
C10—C11—C18	118.8 (3)	O15—C67—C59^vii	118.02 (18)
C13—C12—C11	119.8 (2)	N8—C68—C69	122.9 (2)
C13—C12—H24	123 (2)	N8—C68—H26	117.0 (15)
C11—C12—H24	117 (2)	C69—C68—H26	120.1 (15)
C12—C13—C14	119.3 (2)	C70—C69—C68	119.0 (2)
C12—C13—H9	122.9 (19)	C70—C69—H6	123.1 (17)
C14—C13—H9	117.8 (19)	C68—C69—H6	118.0 (17)
N1—C14—C13	122.9 (2)	C69—C70—C40	120.0 (2)
N1—C14—H4	117.2 (16)	C69—C70—H19	123.7 (17)
C13—C14—H4	119.9 (16)	C40—C70—H19	116.2 (17)
N2—C15—C16	122.8 (2)	C72—C73—C60	116.6 (3)
N2—C15—C10	117.30 (19)	C72—C73—C74	124.7 (3)
C16—C15—C10	119.9 (2)	C60—C73—C74	118.7 (4)
C15—C16—C21	117.2 (3)	C72—C71—C66	118.3 (3)
C15—C16—C17	118.6 (2)	C72—C71—H42	121 (2)
C21—C16—C17	124.2 (2)	C66—C71—H42	120 (2)
C18—C17—C16	121.8 (2)	C71—C72—C73	120.7 (3)
C18—C17—H27	125 (2)	C71—C72—H34	119 (3)
C16—C17—H27	114 (2)	C73—C72—H34	120 (3)
C17—C18—C11	121.1 (3)	C74—C75—C62	121.6 (4)
C17—C18—H23	123 (2)	C74—C75—H36	123 (3)
C11—C18—H23	116 (2)	C62—C75—H36	116 (3)
N2—C19—C20	122.7 (3)	C75—C74—C73	121.6 (4)
N2—C19—H11	116.9 (17)	C75—C74—H40	121 (3)
C20—C19—H11	120.4 (17)	C73—C74—H40	118 (3)
C21—C20—C19	119.4 (3)	H101—OW1—H100	97 (3)

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

(HUT-12) top

Crystal data top

C₄₂H₂₂N₄O₁₃Zn₄·4(O)	F(000) = 2232
M_r = 1116.12	D_x = 1.793 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2830 reflections
a = 15.4925 (4) Å	θ = 3.7–32.3°
b = 15.6741 (6) Å	µ = 2.38 mm⁻¹
c = 17.0388 (5) Å	T = 298 K
β = 92.353 (3)°	Prism, colorless
V = 4134.1 (2) Å³	0.24 × 0.2 × 0.2 mm
Z = 4

Data collection top

Xcalibur diffractometer	4185 independent reflections
Graphite monochromator	2285 reflections with I > 2σ(I)
Detector resolution: 16.5467 pixels mm^-1	R_int = 0.079
profile data from ω–scans	θ_max = 26.4°, θ_min = 3.9°
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −18→19
T_min = 0.971, T_max = 1	k = −19→11
13337 measured reflections	l = −21→21

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) = 0.076	H-atom parameters constrained
S = 0.82	w = 1/[σ²(F_o²) + (0.0252P)²] where P = (F_o² + 2F_c²)/3
4185 reflections	(Δ/σ)_max = 0.001
308 parameters	Δρ_max = 0.63 e Å⁻³
0 restraints	Δρ_min = −0.66 e Å⁻³

Crystal data top

C₄₂H₂₂N₄O₁₃Zn₄·4(O)	V = 4134.1 (2) Å³
M_r = 1116.12	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 15.4925 (4) Å	µ = 2.38 mm⁻¹
b = 15.6741 (6) Å	T = 298 K
c = 17.0388 (5) Å	0.24 × 0.2 × 0.2 mm
β = 92.353 (3)°

Data collection top

Xcalibur diffractometer	4185 independent reflections
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	2285 reflections with I > 2σ(I)
T_min = 0.971, T_max = 1	R_int = 0.079
13337 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.046	0 restraints
wR(F²) = 0.076	H-atom parameters constrained
S = 0.82	Δρ_max = 0.63 e Å⁻³
4185 reflections	Δρ_min = −0.66 e Å⁻³
308 parameters

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Zn1	0.44033 (3)	0.09669 (4)	0.68257 (3)	0.02220 (16)
Zn2	0.55900 (3)	0.25651 (4)	0.67482 (3)	0.02268 (16)
N1	0.6873 (3)	0.2055 (3)	0.6644 (3)	0.0333 (11)
N2	0.5635 (3)	0.2198 (2)	0.5516 (2)	0.0281 (11)
O1	0.3808 (2)	0.1188 (2)	0.58669 (18)	0.0362 (9)
O2	0.2422 (2)	0.1412 (3)	0.6093 (2)	0.0617 (13)
O3	0.4509 (2)	0.3255 (2)	0.63914 (18)	0.0312 (9)
O4	0.6109 (2)	0.3468 (2)	0.74704 (18)	0.0294 (9)
O5	0.5418 (2)	0.0303 (2)	0.64645 (19)	0.0341 (9)
O6	0.3758 (2)	0.0150 (2)	0.74336 (19)	0.0338 (9)
O7	0.5	0.1803 (3)	0.75	0.0216 (11)
C1	0.3099 (3)	0.3829 (3)	0.6372 (3)	0.0213 (12)
C2	0.3425 (3)	0.0633 (3)	0.4381 (3)	0.0218 (12)
H2A	0.394	0.0457	0.4629	0.026*
C3	0.3884 (3)	0.3493 (3)	0.6787 (3)	0.0245 (12)
C4	0.2822 (3)	0.1061 (3)	0.4804 (3)	0.0216 (11)
C5	0.2488 (3)	0.4256 (3)	0.6784 (3)	0.0250 (12)
H5A	0.2587	0.4357	0.7318	0.03*
C6	0.3002 (4)	0.1240 (3)	0.5668 (3)	0.0315 (15)
C7	0.6731 (3)	−0.0461 (3)	0.6417 (3)	0.0214 (11)
C8	0.2948 (3)	0.3685 (3)	0.5578 (3)	0.0243 (13)
H8A	0.3368	0.3414	0.5294	0.029*
C9	0.6072 (3)	0.0036 (3)	0.6843 (3)	0.0259 (12)
C10	0.8461 (4)	0.1319 (4)	0.6364 (4)	0.059 (2)
H10A	0.8996	0.1076	0.6277	0.071*
C11	0.7932 (4)	0.1035 (4)	0.4967 (4)	0.0578 (19)
H11A	0.845	0.0777	0.4845	0.069*
C12	0.5100 (4)	0.1986 (4)	0.4201 (3)	0.0466 (16)
H12A	0.4657	0.2067	0.3823	0.056*
C13	0.5836 (4)	0.1577 (4)	0.4022 (3)	0.0502 (17)
H13A	0.5892	0.1357	0.3519	0.06*
C14	0.7306 (5)	0.1096 (4)	0.4417 (4)	0.0594 (19)
H14A	0.7397	0.0882	0.3919	0.071*
C15	0.8295 (4)	0.1633 (4)	0.7074 (4)	0.0583 (19)
H15A	0.871	0.1603	0.7482	0.07*
C16	0.6498 (4)	0.1482 (3)	0.4568 (3)	0.0387 (15)
C17	0.7828 (4)	0.1358 (3)	0.5748 (4)	0.0414 (16)
C18	0.5026 (3)	0.2277 (3)	0.4950 (3)	0.0384 (15)
H18A	0.4514	0.2548	0.5072	0.046*
C19	0.7036 (3)	0.1731 (3)	0.5921 (3)	0.0309 (13)
C20	0.7491 (4)	0.2004 (4)	0.7195 (3)	0.0440 (16)
H20A	0.7389	0.2226	0.7689	0.053*
C21	0.6371 (3)	0.1804 (3)	0.5326 (3)	0.0281 (13)
O9W	0.5	0.5172 (4)	0.75	0.0710 (19)
O10W	0.0736 (3)	0.0837 (4)	0.6158 (3)	0.1050 (18)
O11W	0.4954 (5)	0.4644 (5)	0.5259 (5)	0.063 (3)	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0195 (3)	0.0342 (4)	0.0125 (3)	−0.0002 (3)	−0.0043 (2)	−0.0002 (3)
Zn2	0.0188 (3)	0.0341 (4)	0.0150 (3)	0.0007 (3)	−0.0012 (2)	0.0012 (3)
N1	0.028 (3)	0.043 (3)	0.028 (3)	0.001 (2)	0.001 (2)	0.014 (2)
N2	0.028 (2)	0.035 (3)	0.022 (2)	−0.001 (2)	0.006 (2)	0.000 (2)
O1	0.025 (2)	0.067 (3)	0.0162 (18)	0.0010 (19)	−0.0089 (17)	0.0023 (18)
O2	0.034 (2)	0.127 (4)	0.024 (2)	0.018 (2)	0.000 (2)	−0.020 (2)
O3	0.0205 (19)	0.051 (2)	0.022 (2)	0.0142 (18)	−0.0014 (16)	−0.0040 (18)
O4	0.031 (2)	0.044 (2)	0.0126 (19)	−0.0123 (17)	−0.0107 (16)	0.0010 (16)
O5	0.024 (2)	0.050 (2)	0.027 (2)	0.0115 (18)	−0.0092 (17)	−0.0040 (18)
O6	0.033 (2)	0.049 (2)	0.019 (2)	−0.0192 (18)	−0.0028 (17)	0.0060 (18)
O7	0.018 (3)	0.027 (3)	0.019 (3)	0	−0.001 (2)	0
C1	0.017 (3)	0.030 (3)	0.016 (3)	0.005 (2)	−0.009 (2)	−0.005 (2)
C2	0.014 (3)	0.027 (3)	0.024 (3)	0.003 (2)	−0.010 (2)	−0.001 (2)
C3	0.020 (3)	0.025 (3)	0.028 (3)	−0.001 (2)	−0.016 (3)	0.004 (3)
C4	0.017 (3)	0.030 (3)	0.017 (3)	0.002 (2)	−0.006 (2)	−0.004 (2)
C5	0.026 (3)	0.032 (3)	0.015 (2)	0.004 (2)	−0.009 (2)	−0.001 (2)
C6	0.030 (3)	0.039 (4)	0.024 (3)	0.004 (3)	−0.010 (3)	−0.002 (3)
C7	0.019 (3)	0.027 (3)	0.017 (3)	0.003 (2)	−0.003 (2)	−0.002 (2)
C8	0.016 (3)	0.040 (3)	0.017 (3)	0.007 (2)	−0.003 (2)	−0.007 (2)
C9	0.019 (3)	0.032 (3)	0.026 (3)	−0.001 (3)	−0.003 (3)	0.003 (3)
C10	0.035 (4)	0.069 (5)	0.076 (5)	0.016 (3)	0.023 (4)	0.024 (4)
C11	0.056 (5)	0.044 (4)	0.077 (5)	0.018 (4)	0.047 (4)	0.008 (4)
C12	0.058 (4)	0.064 (4)	0.018 (3)	−0.013 (4)	−0.003 (3)	0.001 (3)
C13	0.080 (5)	0.052 (4)	0.020 (3)	−0.014 (4)	0.015 (4)	−0.009 (3)
C14	0.078 (5)	0.048 (5)	0.055 (5)	0.001 (4)	0.034 (4)	−0.002 (4)
C15	0.033 (4)	0.073 (5)	0.068 (5)	0.009 (4)	−0.006 (4)	0.038 (4)
C16	0.060 (4)	0.028 (3)	0.029 (4)	−0.002 (3)	0.019 (3)	−0.004 (3)
C17	0.029 (3)	0.034 (4)	0.062 (5)	0.004 (3)	0.017 (3)	0.016 (3)
C18	0.036 (3)	0.053 (4)	0.026 (3)	0.002 (3)	−0.001 (3)	0.005 (3)
C19	0.028 (3)	0.031 (3)	0.034 (4)	0.001 (3)	0.012 (3)	0.005 (3)
C20	0.038 (4)	0.058 (4)	0.036 (4)	0.003 (3)	−0.002 (3)	0.022 (3)
C21	0.028 (3)	0.024 (3)	0.033 (3)	−0.004 (3)	0.010 (3)	−0.002 (3)
O9W	0.070 (4)	0.064 (4)	0.077 (5)	0	−0.010 (4)	0
O10W	0.073 (3)	0.178 (5)	0.065 (3)	−0.032 (4)	0.011 (3)	−0.021 (3)
O11W	0.050 (5)	0.080 (7)	0.060 (7)	0.002 (6)	0.008 (5)	−0.008 (5)

Geometric parameters (Å, º) top

Zn1—O1	1.875 (3)	C4—C6	1.513 (6)
Zn1—O6	1.948 (3)	C5—C7^iv	1.379 (6)
Zn1—O7	1.951 (3)	C5—H5A	0.93
Zn1—O5	2.004 (3)	C7—C5^v	1.379 (6)
Zn1—Zn1ⁱ	2.8896 (11)	C7—C2ⁱⁱ	1.397 (6)
Zn1—Zn2	3.1133 (8)	C7—C9	1.495 (6)
Zn2—O7	2.000 (3)	C8—C4ⁱⁱⁱ	1.393 (6)
Zn2—O4	2.021 (3)	C8—H8A	0.93
Zn2—O3	2.063 (3)	C9—O6ⁱ	1.263 (5)
Zn2—N1	2.156 (4)	C10—C15	1.341 (8)
Zn2—N2	2.180 (4)	C10—C17	1.408 (8)
N1—C20	1.317 (6)	C10—H10A	0.93
N1—C19	1.365 (6)	C11—C14	1.323 (8)
N2—C18	1.328 (6)	C11—C17	1.439 (8)
N2—C21	1.348 (6)	C11—H11A	0.93
O1—C6	1.282 (6)	C12—C13	1.355 (7)
O2—C6	1.208 (6)	C12—C18	1.365 (7)
O3—C3	1.259 (5)	C12—H12A	0.93
O4—C3ⁱ	1.266 (5)	C13—C16	1.364 (7)
O5—C9	1.250 (5)	C13—H13A	0.93
O6—C9ⁱ	1.263 (5)	C14—C16	1.423 (8)
O7—Zn1ⁱ	1.951 (3)	C14—H14A	0.93
O7—Zn2ⁱ	2.000 (3)	C15—C20	1.397 (7)
C1—C5	1.375 (6)	C15—H15A	0.93
C1—C8	1.382 (6)	C16—C21	1.408 (7)
C1—C3	1.479 (6)	C17—C19	1.402 (7)
C2—C4	1.377 (6)	C18—H18A	0.93
C2—C7ⁱⁱ	1.397 (6)	C19—C21	1.420 (7)
C2—H2A	0.93	C20—H20A	0.93
C3—O4ⁱ	1.266 (5)	O11W—O11W^vi	1.434 (15)
C4—C8ⁱⁱⁱ	1.393 (6)

O1—Zn1—O6	109.84 (14)	O4ⁱ—C3—C1	117.4 (5)
O1—Zn1—O7	126.40 (14)	C2—C4—C8ⁱⁱⁱ	118.6 (4)
O6—Zn1—O7	111.69 (11)	C2—C4—C6	119.8 (4)
O1—Zn1—O5	101.10 (14)	C8ⁱⁱⁱ—C4—C6	121.5 (4)
O6—Zn1—O5	104.39 (14)	C1—C5—C7^iv	121.1 (4)
O7—Zn1—O5	99.85 (11)	C1—C5—H5A	119.5
O1—Zn1—Zn1ⁱ	165.62 (11)	C7^iv—C5—H5A	119.5
O6—Zn1—Zn1ⁱ	84.43 (10)	O2—C6—O1	126.6 (5)
O7—Zn1—Zn1ⁱ	42.22 (9)	O2—C6—C4	120.8 (4)
O5—Zn1—Zn1ⁱ	76.09 (9)	O1—C6—C4	112.6 (5)
O1—Zn1—Zn2	94.87 (11)	C5^v—C7—C2ⁱⁱ	119.2 (4)
O6—Zn1—Zn2	150.23 (10)	C5^v—C7—C9	122.2 (4)
O7—Zn1—Zn2	38.55 (6)	C2ⁱⁱ—C7—C9	118.6 (4)
O5—Zn1—Zn2	86.14 (10)	C1—C8—C4ⁱⁱⁱ	121.3 (4)
Zn1ⁱ—Zn1—Zn2	70.976 (17)	C1—C8—H8A	119.4
O7—Zn2—O4	102.08 (12)	C4ⁱⁱⁱ—C8—H8A	119.4
O7—Zn2—O3	96.59 (11)	O5—C9—O6ⁱ	126.0 (5)
O4—Zn2—O3	96.35 (13)	O5—C9—C7	118.6 (4)
O7—Zn2—N1	106.18 (12)	O6ⁱ—C9—C7	115.3 (4)
O4—Zn2—N1	87.98 (15)	C15—C10—C17	120.2 (6)
O3—Zn2—N1	155.42 (14)	C15—C10—H10A	119.9
O7—Zn2—N2	119.51 (12)	C17—C10—H10A	119.9
O4—Zn2—N2	138.02 (14)	C14—C11—C17	121.5 (6)
O3—Zn2—N2	84.97 (14)	C14—C11—H11A	119.3
N1—Zn2—N2	75.90 (16)	C17—C11—H11A	119.3
O7—Zn2—Zn1	37.45 (7)	C13—C12—C18	118.2 (6)
O4—Zn2—Zn1	139.36 (9)	C13—C12—H12A	120.9
O3—Zn2—Zn1	87.73 (10)	C18—C12—H12A	120.9
N1—Zn2—Zn1	104.66 (11)	C12—C13—C16	120.9 (6)
N2—Zn2—Zn1	82.57 (10)	C12—C13—H13A	119.5
C20—N1—C19	117.7 (5)	C16—C13—H13A	119.5
C20—N1—Zn2	127.6 (4)	C11—C14—C16	121.8 (6)
C19—N1—Zn2	114.7 (3)	C11—C14—H14A	119.1
C18—N2—C21	116.8 (4)	C16—C14—H14A	119.1
C18—N2—Zn2	128.7 (3)	C10—C15—C20	119.5 (6)
C21—N2—Zn2	114.4 (3)	C10—C15—H15A	120.3
C6—O1—Zn1	132.9 (3)	C20—C15—H15A	120.3
C3—O3—Zn2	129.1 (3)	C13—C16—C21	117.2 (6)
C3ⁱ—O4—Zn2	128.1 (3)	C13—C16—C14	124.4 (6)
C9—O5—Zn1	130.2 (3)	C21—C16—C14	118.4 (6)
C9ⁱ—O6—Zn1	121.4 (3)	C19—C17—C10	116.8 (6)
Zn1—O7—Zn1ⁱ	95.56 (18)	C19—C17—C11	118.3 (6)
Zn1—O7—Zn2	104.01 (2)	C10—C17—C11	125.0 (6)
Zn1ⁱ—O7—Zn2	124.09 (3)	N2—C18—C12	124.3 (5)
Zn1—O7—Zn2ⁱ	124.09 (3)	N2—C18—H18A	117.8
Zn1ⁱ—O7—Zn2ⁱ	104.01 (2)	C12—C18—H18A	117.8
Zn2—O7—Zn2ⁱ	106.67 (19)	N1—C19—C17	122.8 (5)
C5—C1—C8	119.1 (4)	N1—C19—C21	117.3 (5)
C5—C1—C3	120.0 (4)	C17—C19—C21	119.9 (5)
C8—C1—C3	120.8 (4)	N1—C20—C15	123.1 (6)
C4—C2—C7ⁱⁱ	120.7 (4)	N1—C20—H20A	118.4
C4—C2—H2A	119.7	C15—C20—H20A	118.4
C7ⁱⁱ—C2—H2A	119.7	N2—C21—C16	122.4 (5)
O3—C3—O4ⁱ	123.5 (4)	N2—C21—C19	117.5 (5)
O3—C3—C1	119.1 (4)	C16—C21—C19	120.1 (5)

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

Experimental details

	(HUT-11)	(HUT-12)
Crystal data
Chemical formula	C₇₅H₄₂N₈O₁₉Zn₅·H₂O·3.04(O)	C₄₂H₂₂N₄O₁₃Zn₄·4(O)
M_r	1752.73	1116.12
Crystal system, space group	Monoclinic, C2/c	Monoclinic, C2/c
Temperature (K)	150	298
a, b, c (Å)	33.957 (3), 23.8834 (17), 17.1688 (12)	15.4925 (4), 15.6741 (6), 17.0388 (5)
β (°)	90.079 (1)	92.353 (3)
V (Å³)	13924.0 (19)	4134.1 (2)
Z	8	4
Radiation type	Synchrotron, λ = 0.6889 Å	Mo Kα
µ (mm⁻¹)	1.64	2.38
Crystal size (mm)	0.04 × 0.03 × 0.03	0.24 × 0.2 × 0.2

Data collection
Diffractometer	Rigaku Saturn724+ (2x2 bin mode) diffractometer	Xcalibur diffractometer
Absorption correction	Multi-scan	Multi-scan CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
T_min, T_max	0.833, 1	0.971, 1
No. of measured, independent and observed [I > 2σ(I)] reflections	118881, 20944, 18223	13337, 4185, 2285
R_int	0.057	0.079
(sin θ/λ)_max (Å⁻¹)	0.714	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.092, 1.06	0.046, 0.076, 0.82
No. of reflections	20944	4185
No. of parameters	1188	308
H-atom treatment	All H-atom parameters refined	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0374P)² + 26.1353P] where P = (F_o² + 2F_c²)/3	w = 1/[σ²(F_o²) + (0.0252P)²] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.91, −0.83	0.63, −0.66

Computer programs: CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010), CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10), CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10), SHELXL97 (Sheldrick, 2008).

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