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Two novel three-dimensional Zn-MOFs (zinc metal-organic frameworks), Zn53-OH)(BTC)3(Phen)4·5H2O (denoted as HUT-11) and Zn44-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), Zn33-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 Zn44-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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112007999/so5059sup1.cif
Contains datablocks global, HUT-11, HUT-12

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112007999/so5059HUT-11sup2.hkl
Contains datablock HUT-11

hkl

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
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
(HUT-11) top
Crystal data top
C75H42N8O19Zn5·H2O·3.04(O)F(000) = 7074.48
Mr = 1752.73Dx = 1.672 Mg m3
Monoclinic, C2/cSynchrotron radiation, λ = 0.6889 Å
Hall symbol: -C 2ycCell parameters from 20652 reflections
a = 33.957 (3) Åθ = 1.2–31.7°
b = 23.8834 (17) ŵ = 1.64 mm1
c = 17.1688 (12) ÅT = 150 K
β = 90.079 (1)°Prism, colorless
V = 13924.0 (19) Å30.04 × 0.03 × 0.03 mm
Z = 8
Data collection top
Rigaku Saturn724+ (2x2 bin mode)
diffractometer
20944 independent reflections
Radiation source: Synchrotron18223 reflections with I > 2σ(I)
Si-111 monochromatorRint = 0.057
Detector resolution: 28.5714 pixels mm-1θmax = 29.5°, θmin = 1.5°
profile data from ω–scansh = 4848
Absorption correction: multi-scan
?
k = 3333
Tmin = 0.833, Tmax = 1l = 2424
118881 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092All H-atom parameters refined
S = 1.06 w = 1/[σ2(Fo2) + (0.0374P)2 + 26.1353P]
where P = (Fo2 + 2Fc2)/3
20944 reflections(Δ/σ)max = 0.004
1188 parametersΔρmax = 0.91 e Å3
0 restraintsΔρmin = 0.83 e Å3
Crystal data top
C75H42N8O19Zn5·H2O·3.04(O)V = 13924.0 (19) Å3
Mr = 1752.73Z = 8
Monoclinic, C2/cSynchrotron radiation, λ = 0.6889 Å
a = 33.957 (3) ŵ = 1.64 mm1
b = 23.8834 (17) ÅT = 150 K
c = 17.1688 (12) Å0.04 × 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)
Tmin = 0.833, Tmax = 1Rint = 0.057
118881 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0390 restraints
wR(F2) = 0.092All H-atom parameters refined
S = 1.06 w = 1/[σ2(Fo2) + (0.0374P)2 + 26.1353P]
where P = (Fo2 + 2Fc2)/3
20944 reflectionsΔρmax = 0.91 e Å3
1188 parametersΔρmin = 0.83 e Å3
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
xyzUiso*/UeqOcc. (<1)
Zn10.202889 (6)0.152201 (10)0.644086 (12)0.01393 (5)
Zn20.276932 (6)0.068840 (10)0.702271 (13)0.01462 (5)
Zn30.030493 (6)0.350710 (10)0.842718 (13)0.01556 (5)
Zn40.260426 (6)0.191676 (10)0.794078 (12)0.01385 (5)
Zn50.027136 (6)0.146031 (10)1.161668 (12)0.01509 (5)
N10.04369 (5)0.06395 (8)1.19615 (10)0.0188 (3)
N20.01645 (5)0.09448 (9)1.10316 (11)0.0238 (4)
N30.06900 (6)0.40854 (9)0.78714 (11)0.0260 (4)
N40.00342 (6)0.42875 (9)0.86913 (12)0.0262 (4)
N50.21212 (5)0.22575 (8)0.86784 (10)0.0177 (3)
N60.27194 (5)0.15623 (7)0.90443 (10)0.0175 (3)
N70.18219 (5)0.16329 (8)0.52755 (9)0.0173 (3)
N80.18818 (5)0.06679 (7)0.60723 (10)0.0160 (3)
O10.31926 (4)0.19006 (7)0.76229 (9)0.0207 (3)
O20.32927 (4)0.10485 (6)0.71066 (9)0.0216 (3)
O30.05452 (5)0.32063 (7)0.93871 (9)0.0292 (4)
O40.08798 (6)0.39829 (8)0.96712 (10)0.0344 (4)
O50.43996 (4)0.31768 (6)0.75101 (8)0.0191 (3)
O60.48692 (4)0.29220 (7)0.66657 (8)0.0219 (3)
O70.05271 (5)0.17974 (7)1.07098 (9)0.0238 (3)
O80.02282 (5)0.31292 (7)0.85588 (9)0.0271 (3)
O90.04579 (5)0.29211 (7)0.73645 (9)0.0259 (3)
O100.26365 (5)0.14936 (7)0.58995 (8)0.0217 (3)
O110.15221 (4)0.16115 (7)0.70648 (8)0.0215 (3)
O120.16784 (4)0.10069 (7)0.80184 (9)0.0230 (3)
O130.28057 (5)0.05933 (7)0.58534 (9)0.0228 (3)
O140.09730 (5)0.11243 (7)1.05293 (9)0.0267 (3)
O150.25641 (4)0.26584 (6)0.73897 (8)0.0209 (3)
O160.21230 (5)0.23696 (6)0.65008 (9)0.0247 (3)
O17A0.2731 (2)0.03034 (12)0.81639 (19)0.0376 (12)0.693 (15)
O17B0.2989 (5)0.0253 (3)0.8240 (4)0.043 (4)0.307 (15)
O180.27309 (6)0.01963 (8)0.71632 (11)0.0415 (5)
O190.23747 (4)0.12594 (6)0.73774 (8)0.0149 (3)
C10.37383 (5)0.17645 (8)0.67847 (11)0.0149 (3)
C20.38375 (6)0.15242 (9)0.60689 (11)0.0171 (4)
C30.41463 (6)0.17406 (9)0.56215 (11)0.0183 (4)
C40.43673 (6)0.21812 (9)0.59222 (11)0.0184 (4)
C50.42792 (5)0.24103 (9)0.66526 (11)0.0166 (4)
C60.39571 (5)0.22125 (9)0.70745 (11)0.0156 (3)
C70.33786 (5)0.15564 (9)0.72087 (11)0.0161 (4)
C80.07590 (6)0.35107 (9)0.98319 (12)0.0203 (4)
C90.45345 (5)0.28716 (9)0.69698 (11)0.0164 (4)
C100.02338 (6)0.02238 (9)1.15972 (12)0.0209 (4)
C110.03288 (7)0.03469 (10)1.16849 (14)0.0294 (5)
C120.06526 (9)0.04797 (12)1.21630 (16)0.0357 (6)
C130.08545 (8)0.00632 (12)1.25293 (15)0.0329 (5)
C140.07371 (7)0.04937 (10)1.24203 (13)0.0247 (4)
C150.00925 (6)0.03852 (10)1.11120 (12)0.0239 (4)
C160.03236 (7)0.00284 (12)1.07465 (14)0.0309 (5)
C170.02173 (9)0.06056 (13)1.08491 (17)0.0395 (7)
C180.00904 (9)0.07586 (12)1.12914 (18)0.0396 (6)
C190.04664 (7)0.11014 (13)1.05939 (15)0.0321 (5)
C200.07171 (7)0.07156 (15)1.02210 (16)0.0401 (7)
C210.06463 (7)0.01562 (14)1.02967 (16)0.0391 (7)
C220.21501 (6)0.20840 (9)0.94304 (11)0.0170 (4)
C230.18910 (6)0.22713 (9)1.00204 (12)0.0212 (4)
C240.16023 (6)0.26640 (10)0.98100 (14)0.0269 (5)
C250.15790 (6)0.28439 (10)0.90531 (15)0.0264 (5)
C260.18417 (6)0.26254 (10)0.84998 (13)0.0225 (4)
C270.24579 (6)0.16953 (9)0.96162 (11)0.0169 (4)
C280.24836 (7)0.14730 (9)1.03771 (12)0.0221 (4)
C290.22133 (7)0.16737 (11)1.09611 (12)0.0284 (5)
C300.19359 (7)0.20557 (11)1.07981 (12)0.0275 (5)
C310.30006 (6)0.11947 (10)0.92025 (13)0.0228 (4)
C320.30340 (8)0.09269 (11)0.99309 (14)0.0294 (5)
C330.27745 (8)0.10635 (11)1.05171 (13)0.0287 (5)
C340.17918 (5)0.11500 (9)0.48652 (11)0.0170 (4)
C350.17351 (6)0.11385 (10)0.40494 (12)0.0215 (4)
C360.17222 (7)0.16576 (11)0.36594 (13)0.0264 (5)
C370.17527 (7)0.21432 (11)0.40806 (13)0.0272 (5)
C380.17942 (6)0.21117 (10)0.48919 (13)0.0221 (4)
C390.18169 (5)0.06329 (9)0.52930 (11)0.0165 (4)
C400.17692 (6)0.01168 (9)0.48996 (13)0.0210 (4)
C410.17183 (7)0.01211 (11)0.40660 (14)0.0276 (5)
C420.17046 (7)0.06067 (11)0.36639 (13)0.0277 (5)
C430.08368 (5)0.17472 (9)0.94813 (11)0.0154 (3)
C440.06110 (5)0.21857 (9)0.91895 (11)0.0171 (4)
C450.06589 (5)0.23577 (9)0.84184 (11)0.0169 (4)
C460.09339 (6)0.20913 (9)0.79436 (11)0.0172 (4)
C470.11618 (5)0.16544 (8)0.82338 (11)0.0151 (3)
C480.11114 (5)0.14814 (9)0.90021 (11)0.0154 (3)
C490.07831 (5)0.15345 (9)1.03035 (11)0.0164 (4)
C500.04265 (6)0.28398 (9)0.80873 (12)0.0195 (4)
C510.14782 (6)0.13972 (9)0.77385 (11)0.0165 (4)
C520.27603 (8)0.01678 (11)0.78762 (14)0.0300 (5)
C530.27494 (6)0.06827 (9)0.83759 (11)0.0188 (4)
C540.27086 (6)0.12133 (9)0.30422 (11)0.0181 (4)
C550.27701 (6)0.06245 (9)0.41857 (12)0.0185 (4)
C560.27320 (6)0.10615 (9)0.55303 (11)0.0177 (4)
C570.27483 (5)0.10979 (9)0.46558 (11)0.0154 (3)
C580.27175 (6)0.16243 (9)0.43204 (11)0.0165 (4)
C590.26987 (6)0.16861 (9)0.35136 (11)0.0164 (4)
C600.05924 (8)0.46245 (11)0.79908 (15)0.0320 (5)
C610.02418 (8)0.47357 (11)0.84319 (15)0.0308 (5)
C620.01273 (11)0.52928 (13)0.8581 (2)0.0496 (8)
C630.02184 (13)0.53675 (17)0.9019 (3)0.0637 (11)
C640.04286 (11)0.49214 (17)0.9271 (2)0.0554 (9)
C650.02943 (8)0.43775 (13)0.90962 (17)0.0379 (6)
C660.10150 (8)0.39717 (14)0.74700 (17)0.0388 (6)
C670.23350 (6)0.27326 (9)0.68182 (11)0.0171 (4)
C680.18796 (6)0.01995 (9)0.64858 (12)0.0198 (4)
C690.18214 (7)0.03306 (10)0.61507 (15)0.0259 (4)
C700.17728 (7)0.03700 (10)0.53589 (15)0.0266 (5)
C730.08198 (11)0.50748 (14)0.7697 (2)0.0536 (9)
C710.12593 (10)0.43849 (18)0.7156 (2)0.0593 (10)
C720.11588 (12)0.4932 (2)0.7269 (3)0.0691 (12)
C750.03672 (17)0.57380 (15)0.8269 (3)0.0734 (13)
C740.06935 (17)0.56317 (17)0.7850 (3)0.0778 (14)
H10.0962 (7)0.2221 (11)0.7418 (15)0.020 (6)*
H20.4584 (8)0.2318 (12)0.5650 (16)0.027 (7)*
H30.0420 (7)0.2367 (11)0.9504 (15)0.018 (6)*
H40.0876 (8)0.0791 (11)1.2681 (15)0.021 (6)*
H50.3702 (8)0.1223 (12)0.5881 (16)0.026 (7)*
H60.1809 (8)0.0649 (12)0.6493 (16)0.025 (7)*
H70.1813 (8)0.2437 (12)0.5219 (16)0.025 (7)*
H80.3883 (7)0.2368 (11)0.7561 (15)0.019 (6)*
H90.1077 (10)0.0134 (13)1.2870 (19)0.043 (9)*
H100.0426 (9)0.4039 (13)0.9249 (18)0.035 (8)*
H110.0512 (8)0.1502 (12)1.0542 (16)0.026 (7)*
H120.1262 (8)0.1181 (12)0.9180 (16)0.027 (7)*
H130.1074 (9)0.3565 (13)0.7391 (18)0.034 (8)*
H140.1752 (7)0.2204 (11)1.1187 (15)0.020 (6)*
H150.1677 (9)0.0612 (13)0.3127 (19)0.039 (8)*
H160.2791 (8)0.0267 (12)0.4422 (16)0.026 (7)*
H170.1695 (9)0.1658 (13)0.3117 (18)0.035 (8)*
H180.2702 (7)0.1951 (11)0.4662 (15)0.021 (6)*
H190.1730 (8)0.0714 (12)0.5091 (17)0.029 (7)*
H200.3176 (8)0.1117 (11)0.8810 (16)0.022 (6)*
H210.1390 (8)0.3126 (12)0.8894 (17)0.029 (7)*
H220.1701 (9)0.0217 (13)0.3808 (18)0.039 (8)*
H230.0166 (11)0.1130 (16)1.136 (2)0.056 (11)*
H240.0724 (10)0.0854 (14)1.2192 (19)0.044 (9)*
H250.1823 (8)0.2751 (12)0.7940 (17)0.029 (7)*
H260.1909 (8)0.0238 (11)0.7075 (16)0.025 (7)*
H270.0384 (11)0.0855 (16)1.059 (2)0.061 (11)*
H280.3231 (9)0.0651 (13)0.9988 (18)0.038 (8)*
H290.1752 (8)0.2520 (12)0.3843 (17)0.030 (7)*
H300.1422 (9)0.2804 (13)1.0192 (19)0.043 (9)*
H310.0305 (15)0.576 (2)0.913 (3)0.109 (18)*
H320.0800 (10)0.0109 (14)1.005 (2)0.048 (9)*
H330.2696 (8)0.1254 (12)0.2487 (17)0.031 (7)*
H340.1318 (12)0.5213 (17)0.706 (2)0.071 (12)*
H360.0289 (13)0.609 (2)0.839 (3)0.081 (14)*
H370.0682 (12)0.4952 (17)0.955 (2)0.067 (12)*
H380.0928 (10)0.0864 (14)0.991 (2)0.049 (9)*
H390.2787 (9)0.0898 (13)1.1024 (19)0.038 (8)*
H400.0860 (16)0.594 (2)0.765 (3)0.114 (18)*
H410.2248 (9)0.1526 (13)1.1446 (19)0.039 (8)*
H420.1518 (13)0.4274 (17)0.686 (2)0.076 (13)*
H500.2194 (9)0.1142 (12)0.7668 (18)0.032 (8)*
OW10.36516 (5)0.35554 (8)0.80561 (10)0.0301 (4)
H1010.3865 (11)0.3366 (15)0.787 (2)0.053 (10)*
H1000.3755 (11)0.3653 (15)0.850 (2)0.052 (10)*
OW20.08362 (9)0.19245 (12)0.58307 (18)0.0711 (8)*
OW30.36037 (9)0.01799 (13)0.52534 (18)0.0441 (10)*0.710 (7)
OW40.37356 (18)0.9937 (3)0.4295 (4)0.050 (2)*0.373 (8)
OW50.6012 (2)0.1210 (3)0.5240 (4)0.073 (3)*0.429 (9)
OW60.4511 (3)0.7957 (5)0.3905 (7)0.088 (5)*0.310 (11)
OW70.4679 (4)0.8150 (6)0.4462 (8)0.065 (5)*0.215 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.02014 (10)0.01147 (11)0.01020 (9)0.00020 (8)0.00209 (7)0.00041 (8)
Zn20.01870 (10)0.01205 (11)0.01311 (10)0.00033 (8)0.00188 (7)0.00153 (8)
Zn30.01826 (10)0.01615 (12)0.01228 (9)0.00180 (8)0.00227 (7)0.00008 (8)
Zn40.01782 (10)0.01294 (11)0.01081 (9)0.00090 (8)0.00262 (7)0.00049 (8)
Zn50.01558 (9)0.01798 (12)0.01170 (9)0.00150 (8)0.00263 (7)0.00008 (8)
N10.0213 (8)0.0190 (9)0.0162 (7)0.0021 (6)0.0039 (6)0.0005 (6)
N20.0191 (8)0.0319 (11)0.0203 (8)0.0018 (7)0.0020 (6)0.0056 (7)
N30.0270 (9)0.0275 (11)0.0235 (9)0.0073 (8)0.0004 (7)0.0009 (8)
N40.0260 (9)0.0237 (10)0.0290 (10)0.0005 (7)0.0002 (7)0.0028 (8)
N50.0203 (7)0.0166 (9)0.0163 (7)0.0020 (6)0.0028 (6)0.0008 (6)
N60.0212 (7)0.0171 (9)0.0142 (7)0.0021 (6)0.0001 (6)0.0008 (6)
N70.0201 (7)0.0172 (9)0.0145 (7)0.0004 (6)0.0004 (6)0.0006 (6)
N80.0167 (7)0.0149 (8)0.0162 (7)0.0007 (6)0.0015 (6)0.0009 (6)
O10.0187 (6)0.0225 (8)0.0210 (7)0.0035 (6)0.0077 (5)0.0025 (6)
O20.0171 (6)0.0150 (8)0.0327 (8)0.0018 (5)0.0014 (6)0.0031 (6)
O30.0406 (9)0.0281 (9)0.0189 (7)0.0083 (7)0.0145 (6)0.0040 (6)
O40.0461 (10)0.0328 (10)0.0243 (8)0.0147 (8)0.0129 (7)0.0093 (7)
O50.0183 (6)0.0212 (8)0.0177 (6)0.0000 (5)0.0012 (5)0.0041 (6)
O60.0197 (6)0.0273 (9)0.0187 (7)0.0084 (6)0.0063 (5)0.0021 (6)
O70.0265 (7)0.0277 (9)0.0172 (7)0.0059 (6)0.0098 (6)0.0038 (6)
O80.0275 (8)0.0288 (9)0.0250 (8)0.0143 (7)0.0009 (6)0.0044 (7)
O90.0291 (8)0.0272 (9)0.0213 (7)0.0084 (6)0.0049 (6)0.0083 (6)
O100.0284 (7)0.0228 (8)0.0139 (6)0.0002 (6)0.0048 (5)0.0004 (6)
O110.0271 (7)0.0228 (8)0.0147 (6)0.0062 (6)0.0080 (5)0.0026 (6)
O120.0249 (7)0.0191 (8)0.0250 (7)0.0076 (6)0.0119 (6)0.0079 (6)
O130.0315 (8)0.0208 (8)0.0160 (7)0.0023 (6)0.0001 (6)0.0055 (6)
O140.0363 (8)0.0285 (9)0.0154 (7)0.0115 (7)0.0038 (6)0.0041 (6)
O150.0306 (7)0.0173 (8)0.0149 (6)0.0008 (6)0.0008 (5)0.0046 (5)
O160.0395 (9)0.0121 (8)0.0225 (7)0.0030 (6)0.0025 (6)0.0005 (6)
O17A0.061 (3)0.0111 (13)0.0411 (16)0.0002 (13)0.0006 (16)0.0082 (11)
O17B0.088 (11)0.018 (3)0.023 (3)0.018 (4)0.008 (4)0.002 (2)
O180.0560 (12)0.0356 (11)0.0327 (9)0.0114 (9)0.0123 (8)0.0228 (8)
O190.0184 (6)0.0144 (7)0.0120 (6)0.0024 (5)0.0044 (5)0.0009 (5)
C10.0151 (7)0.0142 (9)0.0154 (8)0.0012 (6)0.0031 (6)0.0016 (7)
C20.0180 (8)0.0162 (10)0.0171 (8)0.0008 (7)0.0013 (7)0.0005 (7)
C30.0212 (8)0.0202 (11)0.0136 (8)0.0001 (7)0.0049 (7)0.0002 (7)
C40.0197 (8)0.0209 (11)0.0147 (8)0.0015 (7)0.0054 (7)0.0005 (7)
C50.0167 (8)0.0181 (10)0.0150 (8)0.0016 (7)0.0026 (6)0.0009 (7)
C60.0161 (8)0.0178 (10)0.0129 (8)0.0011 (7)0.0033 (6)0.0015 (7)
C70.0153 (8)0.0197 (10)0.0134 (8)0.0010 (7)0.0003 (6)0.0047 (7)
C80.0238 (9)0.0213 (11)0.0158 (8)0.0001 (8)0.0040 (7)0.0035 (8)
C90.0182 (8)0.0176 (10)0.0134 (8)0.0031 (7)0.0019 (6)0.0020 (7)
C100.0240 (9)0.0211 (11)0.0175 (9)0.0036 (8)0.0072 (7)0.0029 (8)
C110.0381 (12)0.0201 (12)0.0299 (11)0.0047 (9)0.0111 (9)0.0042 (9)
C120.0500 (15)0.0195 (13)0.0375 (14)0.0050 (11)0.0051 (11)0.0050 (10)
C130.0376 (13)0.0293 (14)0.0316 (12)0.0057 (10)0.0023 (10)0.0063 (10)
C140.0263 (10)0.0256 (12)0.0223 (10)0.0011 (9)0.0010 (8)0.0033 (9)
C150.0215 (9)0.0292 (13)0.0210 (9)0.0066 (8)0.0062 (7)0.0077 (9)
C160.0279 (10)0.0377 (15)0.0271 (11)0.0128 (10)0.0079 (9)0.0132 (10)
C170.0430 (14)0.0350 (16)0.0407 (15)0.0192 (12)0.0113 (12)0.0159 (12)
C180.0545 (17)0.0232 (14)0.0410 (15)0.0111 (12)0.0118 (12)0.0087 (11)
C190.0240 (10)0.0450 (17)0.0274 (11)0.0037 (10)0.0024 (8)0.0079 (11)
C200.0218 (11)0.068 (2)0.0302 (12)0.0014 (12)0.0025 (9)0.0122 (13)
C210.0268 (11)0.057 (2)0.0335 (13)0.0152 (12)0.0012 (9)0.0201 (13)
C220.0199 (8)0.0162 (10)0.0149 (8)0.0060 (7)0.0029 (6)0.0038 (7)
C230.0230 (9)0.0216 (11)0.0190 (9)0.0087 (8)0.0075 (7)0.0075 (8)
C240.0214 (9)0.0266 (13)0.0327 (11)0.0045 (8)0.0090 (8)0.0138 (10)
C250.0205 (9)0.0223 (12)0.0364 (12)0.0012 (8)0.0035 (8)0.0085 (9)
C260.0233 (9)0.0206 (11)0.0237 (10)0.0010 (8)0.0009 (7)0.0012 (8)
C270.0234 (9)0.0149 (10)0.0124 (8)0.0073 (7)0.0017 (6)0.0007 (7)
C280.0321 (10)0.0211 (11)0.0130 (8)0.0104 (8)0.0009 (7)0.0009 (7)
C290.0394 (12)0.0341 (14)0.0116 (8)0.0161 (10)0.0033 (8)0.0003 (9)
C300.0333 (11)0.0336 (14)0.0157 (9)0.0135 (10)0.0094 (8)0.0070 (9)
C310.0255 (10)0.0195 (11)0.0233 (10)0.0009 (8)0.0021 (8)0.0005 (8)
C320.0380 (12)0.0220 (12)0.0283 (11)0.0014 (10)0.0091 (9)0.0050 (9)
C330.0410 (13)0.0265 (13)0.0187 (10)0.0085 (10)0.0080 (9)0.0059 (9)
C340.0155 (8)0.0209 (11)0.0147 (8)0.0007 (7)0.0011 (6)0.0009 (7)
C350.0200 (9)0.0296 (12)0.0150 (8)0.0007 (8)0.0005 (7)0.0029 (8)
C360.0252 (10)0.0390 (14)0.0150 (9)0.0023 (9)0.0030 (7)0.0031 (9)
C370.0300 (11)0.0294 (13)0.0221 (10)0.0047 (9)0.0023 (8)0.0083 (9)
C380.0263 (10)0.0188 (11)0.0210 (9)0.0018 (8)0.0022 (7)0.0029 (8)
C390.0165 (8)0.0163 (10)0.0168 (8)0.0007 (7)0.0022 (6)0.0033 (7)
C400.0196 (8)0.0184 (11)0.0251 (10)0.0017 (7)0.0007 (7)0.0080 (8)
C410.0258 (10)0.0308 (13)0.0262 (11)0.0024 (9)0.0013 (8)0.0153 (10)
C420.0274 (10)0.0375 (14)0.0184 (9)0.0036 (9)0.0022 (8)0.0104 (9)
C430.0155 (7)0.0179 (10)0.0129 (8)0.0000 (7)0.0031 (6)0.0005 (7)
C440.0154 (8)0.0203 (11)0.0156 (8)0.0017 (7)0.0041 (6)0.0007 (7)
C450.0174 (8)0.0167 (10)0.0165 (8)0.0022 (7)0.0029 (6)0.0010 (7)
C460.0201 (8)0.0185 (10)0.0130 (8)0.0023 (7)0.0024 (6)0.0010 (7)
C470.0179 (8)0.0133 (9)0.0142 (8)0.0008 (7)0.0052 (6)0.0008 (7)
C480.0157 (8)0.0157 (10)0.0149 (8)0.0018 (7)0.0017 (6)0.0000 (7)
C490.0171 (8)0.0207 (10)0.0114 (7)0.0010 (7)0.0033 (6)0.0012 (7)
C500.0182 (8)0.0201 (11)0.0203 (9)0.0025 (7)0.0004 (7)0.0017 (8)
C510.0190 (8)0.0142 (10)0.0164 (8)0.0013 (7)0.0058 (6)0.0013 (7)
C520.0384 (12)0.0216 (12)0.0301 (11)0.0013 (9)0.0118 (9)0.0095 (9)
C530.0266 (9)0.0141 (10)0.0158 (8)0.0010 (7)0.0039 (7)0.0048 (7)
C540.0246 (9)0.0174 (10)0.0122 (8)0.0004 (7)0.0019 (6)0.0021 (7)
C550.0242 (9)0.0126 (10)0.0187 (9)0.0017 (7)0.0040 (7)0.0003 (7)
C560.0185 (8)0.0207 (11)0.0140 (8)0.0032 (7)0.0012 (6)0.0029 (7)
C570.0183 (8)0.0165 (10)0.0116 (7)0.0009 (7)0.0022 (6)0.0005 (7)
C580.0232 (9)0.0147 (10)0.0115 (8)0.0014 (7)0.0026 (6)0.0030 (7)
C590.0220 (8)0.0137 (10)0.0136 (8)0.0007 (7)0.0025 (6)0.0015 (7)
C600.0382 (12)0.0257 (13)0.0321 (12)0.0132 (10)0.0046 (10)0.0028 (10)
C610.0417 (13)0.0190 (12)0.0318 (12)0.0021 (10)0.0055 (10)0.0009 (9)
C620.074 (2)0.0217 (15)0.0532 (18)0.0044 (14)0.0075 (16)0.0052 (13)
C630.082 (3)0.038 (2)0.071 (3)0.0235 (19)0.003 (2)0.0074 (18)
C640.0536 (19)0.059 (2)0.0536 (19)0.0277 (17)0.0028 (15)0.0112 (17)
C650.0345 (13)0.0406 (17)0.0387 (14)0.0055 (11)0.0053 (11)0.0062 (12)
C660.0288 (12)0.0499 (19)0.0375 (14)0.0095 (12)0.0067 (10)0.0040 (13)
C670.0254 (9)0.0129 (9)0.0130 (8)0.0005 (7)0.0068 (7)0.0004 (7)
C680.0212 (9)0.0160 (10)0.0221 (9)0.0010 (7)0.0019 (7)0.0008 (8)
C690.0276 (10)0.0150 (11)0.0353 (12)0.0028 (8)0.0002 (9)0.0030 (9)
C700.0258 (10)0.0145 (11)0.0397 (13)0.0026 (8)0.0040 (9)0.0083 (9)
C730.064 (2)0.0385 (18)0.058 (2)0.0292 (16)0.0029 (16)0.0037 (15)
C710.0452 (17)0.076 (3)0.057 (2)0.0287 (17)0.0189 (15)0.0067 (19)
C720.063 (2)0.074 (3)0.070 (2)0.045 (2)0.0176 (19)0.005 (2)
C750.119 (4)0.0151 (17)0.086 (3)0.0084 (19)0.006 (3)0.0025 (17)
C740.111 (4)0.034 (2)0.088 (3)0.035 (2)0.006 (3)0.006 (2)
OW10.0222 (7)0.0452 (12)0.0228 (8)0.0008 (7)0.0019 (6)0.0034 (7)
Geometric parameters (Å, º) top
Zn1—O112.0395 (14)C19—H110.97 (3)
Zn1—O162.0519 (16)C20—C211.364 (5)
Zn1—O192.0862 (14)C20—H380.96 (3)
Zn1—N72.1362 (17)C21—H320.92 (3)
Zn1—N82.1933 (17)C22—C231.415 (3)
Zn1—O102.2650 (15)C22—C271.434 (3)
Zn2—O21.9794 (14)C23—C241.403 (3)
Zn2—O192.0072 (14)C23—C301.439 (3)
Zn2—O132.0243 (15)C24—C251.371 (4)
Zn2—O182.131 (2)C24—H300.96 (3)
Zn2—O17A2.168 (3)C25—C261.405 (3)
Zn2—O17B2.450 (11)C25—H210.97 (3)
Zn2—C522.516 (2)C26—H251.01 (3)
Zn3—O31.9752 (15)C27—C281.413 (3)
Zn3—O9i2.0186 (16)C28—C331.411 (3)
Zn3—O82.0353 (15)C28—C291.442 (3)
Zn3—N42.127 (2)C29—C301.341 (4)
Zn3—N32.1272 (19)C29—H410.91 (3)
Zn4—O192.0016 (14)C30—H140.98 (3)
Zn4—O152.0127 (15)C31—C321.409 (3)
Zn4—O12.0721 (14)C31—H200.92 (3)
Zn4—N62.1112 (17)C32—C331.378 (4)
Zn4—N52.2276 (17)C32—H280.94 (3)
Zn5—O71.9572 (15)C33—H390.96 (3)
Zn5—O6ii2.0122 (15)C34—C351.414 (3)
Zn5—O5iii2.0597 (14)C34—C391.439 (3)
Zn5—N12.1234 (18)C35—C361.410 (3)
Zn5—N22.1706 (19)C35—C421.436 (3)
N1—C141.334 (3)C36—C371.371 (4)
N1—C101.361 (3)C36—H170.94 (3)
N2—C191.324 (3)C37—C381.402 (3)
N2—C151.366 (3)C37—H290.99 (3)
N3—C661.329 (3)C38—H70.96 (3)
N3—C601.345 (3)C39—C401.415 (3)
N4—C651.331 (3)C40—C701.405 (3)
N4—C611.357 (3)C40—C411.441 (3)
N5—C261.329 (3)C41—C421.351 (4)
N5—C221.359 (2)C41—H220.92 (3)
N6—C311.325 (3)C42—H150.93 (3)
N6—C271.362 (2)C43—C441.391 (3)
N7—C381.323 (3)C43—C481.397 (3)
N7—C341.355 (3)C43—C491.511 (3)
N8—C681.325 (3)C44—C451.396 (3)
N8—C391.358 (2)C44—H30.95 (3)
O1—C71.258 (2)C45—C461.394 (3)
O2—C71.260 (3)C45—C501.507 (3)
O3—C81.281 (3)C46—C471.391 (3)
O4—C81.231 (3)C46—H10.96 (3)
O5—C91.266 (2)C47—C481.393 (3)
O5—Zn5iii2.0597 (14)C47—C511.503 (3)
O6—C91.257 (2)C48—H120.93 (3)
O6—Zn5iv2.0122 (15)C52—C531.500 (3)
O7—C491.280 (2)C53—C54v1.398 (3)
O8—C501.260 (2)C53—C55v1.399 (3)
O9—C501.261 (2)C54—C591.390 (3)
O9—Zn3i2.0186 (16)C54—C53vi1.398 (3)
O10—C561.254 (3)C54—H330.96 (3)
O11—C511.274 (2)C55—C571.391 (3)
O12—C511.249 (2)C55—C53vi1.399 (3)
O13—C561.273 (3)C55—H160.95 (3)
O14—C491.235 (3)C56—C571.505 (3)
O15—C671.264 (2)C57—C581.387 (3)
O16—C671.251 (3)C58—C591.394 (3)
O17A—O17B0.897 (14)C58—H180.98 (3)
O17A—C521.233 (4)C59—C67vii1.505 (3)
O17B—C521.415 (10)C60—C731.417 (4)
O18—C521.230 (3)C60—C611.435 (4)
O19—H500.84 (3)C61—C621.409 (4)
C1—C61.394 (3)C62—C631.405 (5)
C1—C21.398 (3)C62—C751.441 (6)
C1—C71.507 (3)C63—C641.354 (6)
C2—C31.400 (3)C63—H311.00 (5)
C2—H50.91 (3)C64—C651.409 (4)
C3—C41.391 (3)C64—H370.99 (4)
C3—C8iv1.517 (3)C65—H100.96 (3)
C4—C51.401 (3)C66—C711.397 (4)
C4—H20.93 (3)C66—H131.00 (3)
C5—C61.395 (2)C67—C59vii1.505 (3)
C5—C91.504 (3)C68—C691.404 (3)
C6—H80.95 (3)C68—H261.02 (3)
C8—C3ii1.517 (3)C69—C701.372 (3)
C10—C111.409 (3)C69—H60.96 (3)
C10—C151.438 (3)C70—H190.95 (3)
C11—C121.407 (4)C73—C721.407 (6)
C11—C181.441 (4)C73—C741.422 (6)
C12—C131.362 (4)C71—C721.364 (6)
C12—H240.93 (3)C71—H421.05 (4)
C13—C141.401 (4)C72—H340.93 (4)
C13—H90.97 (3)C75—C741.345 (7)
C14—H40.96 (3)C75—H360.91 (5)
C15—C161.409 (3)C74—H400.99 (5)
C16—C211.410 (4)OW1—H1010.91 (4)
C16—C171.436 (4)OW1—H1000.87 (4)
C17—C181.342 (5)OW3—OW4viii1.801 (7)
C17—H270.94 (4)OW4—OW3ix1.801 (7)
C18—H230.93 (4)OW6—OW71.205 (16)
C19—C201.408 (4)
O11—Zn1—O1690.10 (7)C21—C20—H38123 (2)
O11—Zn1—O1995.80 (6)C19—C20—H38117 (2)
O16—Zn1—O1999.82 (6)C20—C21—C16119.7 (2)
O11—Zn1—N7101.67 (6)C20—C21—H32122 (2)
O16—Zn1—N788.61 (7)C16—C21—H32118 (2)
O19—Zn1—N7160.61 (6)N5—C22—C23122.6 (2)
O11—Zn1—N893.27 (6)N5—C22—C27117.40 (17)
O16—Zn1—N8165.34 (6)C23—C22—C27119.95 (18)
O19—Zn1—N894.03 (6)C24—C23—C22117.5 (2)
N7—Zn1—N876.74 (7)C24—C23—C30123.4 (2)
O11—Zn1—O10171.24 (6)C22—C23—C30119.1 (2)
O16—Zn1—O1084.73 (6)C25—C24—C23119.5 (2)
O19—Zn1—O1078.19 (5)C25—C24—H30120 (2)
N7—Zn1—O1085.30 (6)C23—C24—H30120 (2)
N8—Zn1—O1093.50 (6)C24—C25—C26119.3 (2)
O2—Zn2—O19106.41 (6)C24—C25—H21121.5 (17)
O2—Zn2—O1393.72 (7)C26—C25—H21119.2 (17)
O19—Zn2—O13114.76 (6)N5—C26—C25122.9 (2)
O2—Zn2—O18118.53 (7)N5—C26—H25117.4 (16)
O19—Zn2—O18126.76 (7)C25—C26—H25119.7 (16)
O13—Zn2—O1890.28 (7)N6—C27—C28122.6 (2)
O2—Zn2—O17A100.03 (18)N6—C27—C22117.81 (17)
O19—Zn2—O17A88.42 (14)C28—C27—C22119.54 (18)
O13—Zn2—O17A148.47 (9)C33—C28—C27117.4 (2)
O18—Zn2—O17A58.23 (10)C33—C28—C29123.9 (2)
O2—Zn2—O17B81.4 (3)C27—C28—C29118.7 (2)
O19—Zn2—O17B103.5 (3)C30—C29—C28121.9 (2)
O13—Zn2—O17B141.2 (3)C30—C29—H41123 (2)
O18—Zn2—O17B60.06 (16)C28—C29—H41115 (2)
O17A—Zn2—O17B21.3 (3)C29—C30—C23120.7 (2)
O2—Zn2—C52108.81 (8)C29—C30—H14123.5 (15)
O19—Zn2—C52111.52 (7)C23—C30—H14115.8 (15)
O13—Zn2—C52119.16 (8)N6—C31—C32122.7 (2)
O18—Zn2—C5229.22 (8)N6—C31—H20116.8 (17)
O17A—Zn2—C5229.35 (10)C32—C31—H20120.5 (17)
O17B—Zn2—C5233.1 (2)C33—C32—C31119.4 (2)
O3—Zn3—O9i101.74 (7)C33—C32—H28122.9 (19)
O3—Zn3—O896.57 (7)C31—C32—H28117.7 (19)
O9i—Zn3—O889.73 (7)C32—C33—C28119.2 (2)
O3—Zn3—N4108.65 (8)C32—C33—H39122.6 (18)
O9i—Zn3—N4149.54 (7)C28—C33—H39118.2 (18)
O8—Zn3—N488.90 (7)N7—C34—C35122.79 (19)
O3—Zn3—N3110.86 (7)N7—C34—C39117.43 (17)
O9i—Zn3—N389.47 (8)C35—C34—C39119.79 (19)
O8—Zn3—N3152.12 (7)C36—C35—C34117.2 (2)
N4—Zn3—N377.99 (8)C36—C35—C42123.8 (2)
O19—Zn4—O15115.92 (6)C34—C35—C42118.9 (2)
O19—Zn4—O1103.49 (6)C37—C36—C35119.4 (2)
O15—Zn4—O187.55 (6)C37—C36—H17122.2 (19)
O19—Zn4—N6100.99 (6)C35—C36—H17118.4 (19)
O15—Zn4—N6141.92 (6)C36—C37—C38119.1 (2)
O1—Zn4—N692.95 (6)C36—C37—H29123.6 (17)
O19—Zn4—N5105.94 (6)C38—C37—H29117.3 (17)
O15—Zn4—N584.04 (6)N7—C38—C37123.2 (2)
O1—Zn4—N5150.17 (6)N7—C38—H7113.8 (17)
N6—Zn4—N576.82 (6)C37—C38—H7123.0 (17)
O7—Zn5—O6ii91.93 (6)N8—C39—C40122.82 (19)
O7—Zn5—O5iii99.50 (7)N8—C39—C34117.35 (18)
O6ii—Zn5—O5iii91.64 (6)C40—C39—C34119.82 (18)
O7—Zn5—N1118.95 (6)C70—C40—C39116.9 (2)
O6ii—Zn5—N1147.64 (6)C70—C40—C41124.3 (2)
O5iii—Zn5—N192.43 (6)C39—C40—C41118.8 (2)
O7—Zn5—N299.69 (7)C42—C41—C40121.2 (2)
O6ii—Zn5—N288.45 (7)C42—C41—H22120 (2)
O5iii—Zn5—N2160.80 (7)C40—C41—H22119 (2)
N1—Zn5—N277.61 (7)C41—C42—C35121.4 (2)
C14—N1—C10117.9 (2)C41—C42—H15121.6 (19)
C14—N1—Zn5127.41 (16)C35—C42—H15116.9 (19)
C10—N1—Zn5114.31 (14)C44—C43—C48119.88 (17)
C19—N2—C15118.2 (2)C44—C43—C49121.50 (17)
C19—N2—Zn5128.99 (19)C48—C43—C49118.59 (18)
C15—N2—Zn5112.74 (14)C43—C44—C45119.89 (17)
C66—N3—C60118.6 (2)C43—C44—H3121.1 (15)
C66—N3—Zn3127.6 (2)C45—C44—H3119.0 (15)
C60—N3—Zn3113.69 (16)C46—C45—C44119.95 (18)
C65—N4—C61118.6 (2)C46—C45—C50118.63 (17)
C65—N4—Zn3127.93 (19)C44—C45—C50121.40 (17)
C61—N4—Zn3113.40 (16)C47—C46—C45120.38 (17)
C26—N5—C22118.11 (18)C47—C46—H1121.6 (15)
C26—N5—Zn4129.54 (14)C45—C46—H1118.0 (15)
C22—N5—Zn4112.11 (13)C46—C47—C48119.52 (17)
C31—N6—C27118.50 (18)C46—C47—C51120.13 (17)
C31—N6—Zn4125.60 (14)C48—C47—C51120.23 (17)
C27—N6—Zn4115.67 (14)C47—C48—C43120.38 (18)
C38—N7—C34118.14 (18)C47—C48—H12118.1 (17)
C38—N7—Zn1126.62 (15)C43—C48—H12121.5 (17)
C34—N7—Zn1113.94 (13)O14—C49—O7124.95 (18)
C68—N8—C39118.35 (18)O14—C49—C43119.76 (17)
C68—N8—Zn1129.22 (14)O7—C49—C43115.26 (18)
C39—N8—Zn1112.20 (13)O8—C50—O9126.4 (2)
C7—O1—Zn4130.26 (13)O8—C50—C45117.19 (18)
C7—O2—Zn2129.51 (13)O9—C50—C45116.36 (18)
C8—O3—Zn3121.75 (15)O12—C51—O11125.78 (18)
C9—O5—Zn5iii125.39 (13)O12—C51—C47118.46 (17)
C9—O6—Zn5iv134.55 (15)O11—C51—C47115.74 (17)
C49—O7—Zn5122.29 (14)O18—C52—O17A116.3 (3)
C50—O8—Zn3130.39 (14)O18—C52—O17B121.5 (3)
C50—O9—Zn3i138.38 (15)O18—C52—C53121.5 (2)
C56—O10—Zn1117.93 (13)O17A—C52—C53121.1 (2)
C51—O11—Zn1122.33 (13)O17B—C52—C53110.1 (4)
C56—O13—Zn2108.75 (13)O18—C52—Zn257.74 (13)
C67—O15—Zn4121.98 (14)O17A—C52—Zn259.51 (17)
C67—O16—Zn1142.65 (15)O17B—C52—Zn270.9 (4)
O17B—O17A—C5281.6 (5)C53—C52—Zn2179.0 (2)
O17B—O17A—Zn297.3 (6)C54v—C53—C55v120.15 (18)
C52—O17A—Zn291.1 (2)C54v—C53—C52120.75 (19)
O17A—O17B—C5259.6 (7)C55v—C53—C52119.1 (2)
O17A—O17B—Zn261.4 (6)C59—C54—C53vi120.03 (18)
C52—O17B—Zn276.0 (5)C59—C54—H33119.7 (18)
C52—O18—Zn293.04 (17)C53vi—C54—H33120.2 (18)
Zn4—O19—Zn2114.82 (7)C57—C55—C53vi119.55 (19)
Zn4—O19—Zn1110.80 (7)C57—C55—H16119.2 (17)
Zn2—O19—Zn1110.23 (6)C53vi—C55—H16121.2 (17)
Zn4—O19—H50105 (2)O10—C56—O13123.60 (18)
Zn2—O19—H50116 (2)O10—C56—C57117.82 (18)
Zn1—O19—H5098 (2)O13—C56—C57118.55 (18)
C6—C1—C2119.99 (17)C58—C57—C55120.00 (17)
C6—C1—C7120.84 (17)C58—C57—C56117.63 (17)
C2—C1—C7119.05 (18)C55—C57—C56122.27 (18)
C1—C2—C3120.83 (19)C57—C58—C59120.78 (18)
C1—C2—H5120.7 (17)C57—C58—H18118.6 (15)
C3—C2—H5118.4 (17)C59—C58—H18120.6 (15)
C4—C3—C2118.66 (18)C54—C59—C58119.43 (19)
C4—C3—C8iv121.05 (17)C54—C59—C67vii122.08 (17)
C2—C3—C8iv120.27 (19)C58—C59—C67vii118.49 (18)
C3—C4—C5120.78 (18)N3—C60—C73122.6 (3)
C3—C4—H2120.3 (17)N3—C60—C61117.5 (2)
C5—C4—H2118.8 (17)C73—C60—C61119.9 (3)
C6—C5—C4120.08 (19)N4—C61—C62122.8 (3)
C6—C5—C9120.80 (17)N4—C61—C60117.2 (2)
C4—C5—C9119.12 (17)C62—C61—C60119.9 (3)
C1—C6—C5119.49 (18)C63—C62—C61116.5 (3)
C1—C6—H8118.2 (15)C63—C62—C75125.2 (4)
C5—C6—H8122.3 (15)C61—C62—C75118.3 (4)
O1—C7—O2126.27 (18)C64—C63—C62120.8 (3)
O1—C7—C1117.73 (18)C64—C63—H31121 (3)
O2—C7—C1115.99 (17)C62—C63—H31118 (3)
O4—C8—O3125.11 (19)C63—C64—C65119.2 (3)
O4—C8—C3ii119.45 (19)C63—C64—H37124 (2)
O3—C8—C3ii115.42 (19)C65—C64—H37117 (2)
O6—C9—O5125.27 (19)N4—C65—C64122.1 (3)
O6—C9—C5116.15 (17)N4—C65—H10113.4 (19)
O5—C9—C5118.58 (16)C64—C65—H10124.5 (19)
N1—C10—C11122.8 (2)N3—C66—C71123.2 (3)
N1—C10—C15117.4 (2)N3—C66—H13115.8 (18)
C11—C10—C15119.8 (2)C71—C66—H13120.9 (18)
C12—C11—C10117.3 (2)O16—C67—O15126.44 (19)
C12—C11—C18123.9 (3)O16—C67—C59vii115.53 (18)
C10—C11—C18118.8 (3)O15—C67—C59vii118.02 (18)
C13—C12—C11119.8 (2)N8—C68—C69122.9 (2)
C13—C12—H24123 (2)N8—C68—H26117.0 (15)
C11—C12—H24117 (2)C69—C68—H26120.1 (15)
C12—C13—C14119.3 (2)C70—C69—C68119.0 (2)
C12—C13—H9122.9 (19)C70—C69—H6123.1 (17)
C14—C13—H9117.8 (19)C68—C69—H6118.0 (17)
N1—C14—C13122.9 (2)C69—C70—C40120.0 (2)
N1—C14—H4117.2 (16)C69—C70—H19123.7 (17)
C13—C14—H4119.9 (16)C40—C70—H19116.2 (17)
N2—C15—C16122.8 (2)C72—C73—C60116.6 (3)
N2—C15—C10117.30 (19)C72—C73—C74124.7 (3)
C16—C15—C10119.9 (2)C60—C73—C74118.7 (4)
C15—C16—C21117.2 (3)C72—C71—C66118.3 (3)
C15—C16—C17118.6 (2)C72—C71—H42121 (2)
C21—C16—C17124.2 (2)C66—C71—H42120 (2)
C18—C17—C16121.8 (2)C71—C72—C73120.7 (3)
C18—C17—H27125 (2)C71—C72—H34119 (3)
C16—C17—H27114 (2)C73—C72—H34120 (3)
C17—C18—C11121.1 (3)C74—C75—C62121.6 (4)
C17—C18—H23123 (2)C74—C75—H36123 (3)
C11—C18—H23116 (2)C62—C75—H36116 (3)
N2—C19—C20122.7 (3)C75—C74—C73121.6 (4)
N2—C19—H11116.9 (17)C75—C74—H40121 (3)
C20—C19—H11120.4 (17)C73—C74—H40118 (3)
C21—C20—C19119.4 (3)H101—OW1—H10097 (3)
Symmetry codes: (i) x, y, z+3/2; (ii) x1/2, y+1/2, z+1/2; (iii) x+1/2, y+1/2, z+2; (iv) x+1/2, y+1/2, z1/2; (v) x, y, z+1/2; (vi) x, y, z1/2; (vii) x+1/2, y+1/2, z+1; (viii) x, y1, z; (ix) x, y+1, z.
(HUT-12) top
Crystal data top
C42H22N4O13Zn4·4(O)F(000) = 2232
Mr = 1116.12Dx = 1.793 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2830 reflections
a = 15.4925 (4) Åθ = 3.7–32.3°
b = 15.6741 (6) ŵ = 2.38 mm1
c = 17.0388 (5) ÅT = 298 K
β = 92.353 (3)°Prism, colorless
V = 4134.1 (2) Å30.24 × 0.2 × 0.2 mm
Z = 4
Data collection top
Xcalibur
diffractometer
4185 independent reflections
Graphite monochromator2285 reflections with I > 2σ(I)
Detector resolution: 16.5467 pixels mm-1Rint = 0.079
profile data from ω–scansθmax = 26.4°, θmin = 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 = 1819
Tmin = 0.971, Tmax = 1k = 1911
13337 measured reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 0.82 w = 1/[σ2(Fo2) + (0.0252P)2]
where P = (Fo2 + 2Fc2)/3
4185 reflections(Δ/σ)max = 0.001
308 parametersΔρmax = 0.63 e Å3
0 restraintsΔρmin = 0.66 e Å3
Crystal data top
C42H22N4O13Zn4·4(O)V = 4134.1 (2) Å3
Mr = 1116.12Z = 4
Monoclinic, C2/cMo Kα radiation
a = 15.4925 (4) ŵ = 2.38 mm1
b = 15.6741 (6) ÅT = 298 K
c = 17.0388 (5) Å0.24 × 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)
Tmin = 0.971, Tmax = 1Rint = 0.079
13337 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.076H-atom parameters constrained
S = 0.82Δρmax = 0.63 e Å3
4185 reflectionsΔρmin = 0.66 e Å3
308 parameters
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
xyzUiso*/UeqOcc. (<1)
Zn10.44033 (3)0.09669 (4)0.68257 (3)0.02220 (16)
Zn20.55900 (3)0.25651 (4)0.67482 (3)0.02268 (16)
N10.6873 (3)0.2055 (3)0.6644 (3)0.0333 (11)
N20.5635 (3)0.2198 (2)0.5516 (2)0.0281 (11)
O10.3808 (2)0.1188 (2)0.58669 (18)0.0362 (9)
O20.2422 (2)0.1412 (3)0.6093 (2)0.0617 (13)
O30.4509 (2)0.3255 (2)0.63914 (18)0.0312 (9)
O40.6109 (2)0.3468 (2)0.74704 (18)0.0294 (9)
O50.5418 (2)0.0303 (2)0.64645 (19)0.0341 (9)
O60.3758 (2)0.0150 (2)0.74336 (19)0.0338 (9)
O70.50.1803 (3)0.750.0216 (11)
C10.3099 (3)0.3829 (3)0.6372 (3)0.0213 (12)
C20.3425 (3)0.0633 (3)0.4381 (3)0.0218 (12)
H2A0.3940.04570.46290.026*
C30.3884 (3)0.3493 (3)0.6787 (3)0.0245 (12)
C40.2822 (3)0.1061 (3)0.4804 (3)0.0216 (11)
C50.2488 (3)0.4256 (3)0.6784 (3)0.0250 (12)
H5A0.25870.43570.73180.03*
C60.3002 (4)0.1240 (3)0.5668 (3)0.0315 (15)
C70.6731 (3)0.0461 (3)0.6417 (3)0.0214 (11)
C80.2948 (3)0.3685 (3)0.5578 (3)0.0243 (13)
H8A0.33680.34140.52940.029*
C90.6072 (3)0.0036 (3)0.6843 (3)0.0259 (12)
C100.8461 (4)0.1319 (4)0.6364 (4)0.059 (2)
H10A0.89960.10760.62770.071*
C110.7932 (4)0.1035 (4)0.4967 (4)0.0578 (19)
H11A0.8450.07770.48450.069*
C120.5100 (4)0.1986 (4)0.4201 (3)0.0466 (16)
H12A0.46570.20670.38230.056*
C130.5836 (4)0.1577 (4)0.4022 (3)0.0502 (17)
H13A0.58920.13570.35190.06*
C140.7306 (5)0.1096 (4)0.4417 (4)0.0594 (19)
H14A0.73970.08820.39190.071*
C150.8295 (4)0.1633 (4)0.7074 (4)0.0583 (19)
H15A0.8710.16030.74820.07*
C160.6498 (4)0.1482 (3)0.4568 (3)0.0387 (15)
C170.7828 (4)0.1358 (3)0.5748 (4)0.0414 (16)
C180.5026 (3)0.2277 (3)0.4950 (3)0.0384 (15)
H18A0.45140.25480.50720.046*
C190.7036 (3)0.1731 (3)0.5921 (3)0.0309 (13)
C200.7491 (4)0.2004 (4)0.7195 (3)0.0440 (16)
H20A0.73890.22260.76890.053*
C210.6371 (3)0.1804 (3)0.5326 (3)0.0281 (13)
O9W0.50.5172 (4)0.750.0710 (19)
O10W0.0736 (3)0.0837 (4)0.6158 (3)0.1050 (18)
O11W0.4954 (5)0.4644 (5)0.5259 (5)0.063 (3)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0195 (3)0.0342 (4)0.0125 (3)0.0002 (3)0.0043 (2)0.0002 (3)
Zn20.0188 (3)0.0341 (4)0.0150 (3)0.0007 (3)0.0012 (2)0.0012 (3)
N10.028 (3)0.043 (3)0.028 (3)0.001 (2)0.001 (2)0.014 (2)
N20.028 (2)0.035 (3)0.022 (2)0.001 (2)0.006 (2)0.000 (2)
O10.025 (2)0.067 (3)0.0162 (18)0.0010 (19)0.0089 (17)0.0023 (18)
O20.034 (2)0.127 (4)0.024 (2)0.018 (2)0.000 (2)0.020 (2)
O30.0205 (19)0.051 (2)0.022 (2)0.0142 (18)0.0014 (16)0.0040 (18)
O40.031 (2)0.044 (2)0.0126 (19)0.0123 (17)0.0107 (16)0.0010 (16)
O50.024 (2)0.050 (2)0.027 (2)0.0115 (18)0.0092 (17)0.0040 (18)
O60.033 (2)0.049 (2)0.019 (2)0.0192 (18)0.0028 (17)0.0060 (18)
O70.018 (3)0.027 (3)0.019 (3)00.001 (2)0
C10.017 (3)0.030 (3)0.016 (3)0.005 (2)0.009 (2)0.005 (2)
C20.014 (3)0.027 (3)0.024 (3)0.003 (2)0.010 (2)0.001 (2)
C30.020 (3)0.025 (3)0.028 (3)0.001 (2)0.016 (3)0.004 (3)
C40.017 (3)0.030 (3)0.017 (3)0.002 (2)0.006 (2)0.004 (2)
C50.026 (3)0.032 (3)0.015 (2)0.004 (2)0.009 (2)0.001 (2)
C60.030 (3)0.039 (4)0.024 (3)0.004 (3)0.010 (3)0.002 (3)
C70.019 (3)0.027 (3)0.017 (3)0.003 (2)0.003 (2)0.002 (2)
C80.016 (3)0.040 (3)0.017 (3)0.007 (2)0.003 (2)0.007 (2)
C90.019 (3)0.032 (3)0.026 (3)0.001 (3)0.003 (3)0.003 (3)
C100.035 (4)0.069 (5)0.076 (5)0.016 (3)0.023 (4)0.024 (4)
C110.056 (5)0.044 (4)0.077 (5)0.018 (4)0.047 (4)0.008 (4)
C120.058 (4)0.064 (4)0.018 (3)0.013 (4)0.003 (3)0.001 (3)
C130.080 (5)0.052 (4)0.020 (3)0.014 (4)0.015 (4)0.009 (3)
C140.078 (5)0.048 (5)0.055 (5)0.001 (4)0.034 (4)0.002 (4)
C150.033 (4)0.073 (5)0.068 (5)0.009 (4)0.006 (4)0.038 (4)
C160.060 (4)0.028 (3)0.029 (4)0.002 (3)0.019 (3)0.004 (3)
C170.029 (3)0.034 (4)0.062 (5)0.004 (3)0.017 (3)0.016 (3)
C180.036 (3)0.053 (4)0.026 (3)0.002 (3)0.001 (3)0.005 (3)
C190.028 (3)0.031 (3)0.034 (4)0.001 (3)0.012 (3)0.005 (3)
C200.038 (4)0.058 (4)0.036 (4)0.003 (3)0.002 (3)0.022 (3)
C210.028 (3)0.024 (3)0.033 (3)0.004 (3)0.010 (3)0.002 (3)
O9W0.070 (4)0.064 (4)0.077 (5)00.010 (4)0
O10W0.073 (3)0.178 (5)0.065 (3)0.032 (4)0.011 (3)0.021 (3)
O11W0.050 (5)0.080 (7)0.060 (7)0.002 (6)0.008 (5)0.008 (5)
Geometric parameters (Å, º) top
Zn1—O11.875 (3)C4—C61.513 (6)
Zn1—O61.948 (3)C5—C7iv1.379 (6)
Zn1—O71.951 (3)C5—H5A0.93
Zn1—O52.004 (3)C7—C5v1.379 (6)
Zn1—Zn1i2.8896 (11)C7—C2ii1.397 (6)
Zn1—Zn23.1133 (8)C7—C91.495 (6)
Zn2—O72.000 (3)C8—C4iii1.393 (6)
Zn2—O42.021 (3)C8—H8A0.93
Zn2—O32.063 (3)C9—O6i1.263 (5)
Zn2—N12.156 (4)C10—C151.341 (8)
Zn2—N22.180 (4)C10—C171.408 (8)
N1—C201.317 (6)C10—H10A0.93
N1—C191.365 (6)C11—C141.323 (8)
N2—C181.328 (6)C11—C171.439 (8)
N2—C211.348 (6)C11—H11A0.93
O1—C61.282 (6)C12—C131.355 (7)
O2—C61.208 (6)C12—C181.365 (7)
O3—C31.259 (5)C12—H12A0.93
O4—C3i1.266 (5)C13—C161.364 (7)
O5—C91.250 (5)C13—H13A0.93
O6—C9i1.263 (5)C14—C161.423 (8)
O7—Zn1i1.951 (3)C14—H14A0.93
O7—Zn2i2.000 (3)C15—C201.397 (7)
C1—C51.375 (6)C15—H15A0.93
C1—C81.382 (6)C16—C211.408 (7)
C1—C31.479 (6)C17—C191.402 (7)
C2—C41.377 (6)C18—H18A0.93
C2—C7ii1.397 (6)C19—C211.420 (7)
C2—H2A0.93C20—H20A0.93
C3—O4i1.266 (5)O11W—O11Wvi1.434 (15)
C4—C8iii1.393 (6)
O1—Zn1—O6109.84 (14)O4i—C3—C1117.4 (5)
O1—Zn1—O7126.40 (14)C2—C4—C8iii118.6 (4)
O6—Zn1—O7111.69 (11)C2—C4—C6119.8 (4)
O1—Zn1—O5101.10 (14)C8iii—C4—C6121.5 (4)
O6—Zn1—O5104.39 (14)C1—C5—C7iv121.1 (4)
O7—Zn1—O599.85 (11)C1—C5—H5A119.5
O1—Zn1—Zn1i165.62 (11)C7iv—C5—H5A119.5
O6—Zn1—Zn1i84.43 (10)O2—C6—O1126.6 (5)
O7—Zn1—Zn1i42.22 (9)O2—C6—C4120.8 (4)
O5—Zn1—Zn1i76.09 (9)O1—C6—C4112.6 (5)
O1—Zn1—Zn294.87 (11)C5v—C7—C2ii119.2 (4)
O6—Zn1—Zn2150.23 (10)C5v—C7—C9122.2 (4)
O7—Zn1—Zn238.55 (6)C2ii—C7—C9118.6 (4)
O5—Zn1—Zn286.14 (10)C1—C8—C4iii121.3 (4)
Zn1i—Zn1—Zn270.976 (17)C1—C8—H8A119.4
O7—Zn2—O4102.08 (12)C4iii—C8—H8A119.4
O7—Zn2—O396.59 (11)O5—C9—O6i126.0 (5)
O4—Zn2—O396.35 (13)O5—C9—C7118.6 (4)
O7—Zn2—N1106.18 (12)O6i—C9—C7115.3 (4)
O4—Zn2—N187.98 (15)C15—C10—C17120.2 (6)
O3—Zn2—N1155.42 (14)C15—C10—H10A119.9
O7—Zn2—N2119.51 (12)C17—C10—H10A119.9
O4—Zn2—N2138.02 (14)C14—C11—C17121.5 (6)
O3—Zn2—N284.97 (14)C14—C11—H11A119.3
N1—Zn2—N275.90 (16)C17—C11—H11A119.3
O7—Zn2—Zn137.45 (7)C13—C12—C18118.2 (6)
O4—Zn2—Zn1139.36 (9)C13—C12—H12A120.9
O3—Zn2—Zn187.73 (10)C18—C12—H12A120.9
N1—Zn2—Zn1104.66 (11)C12—C13—C16120.9 (6)
N2—Zn2—Zn182.57 (10)C12—C13—H13A119.5
C20—N1—C19117.7 (5)C16—C13—H13A119.5
C20—N1—Zn2127.6 (4)C11—C14—C16121.8 (6)
C19—N1—Zn2114.7 (3)C11—C14—H14A119.1
C18—N2—C21116.8 (4)C16—C14—H14A119.1
C18—N2—Zn2128.7 (3)C10—C15—C20119.5 (6)
C21—N2—Zn2114.4 (3)C10—C15—H15A120.3
C6—O1—Zn1132.9 (3)C20—C15—H15A120.3
C3—O3—Zn2129.1 (3)C13—C16—C21117.2 (6)
C3i—O4—Zn2128.1 (3)C13—C16—C14124.4 (6)
C9—O5—Zn1130.2 (3)C21—C16—C14118.4 (6)
C9i—O6—Zn1121.4 (3)C19—C17—C10116.8 (6)
Zn1—O7—Zn1i95.56 (18)C19—C17—C11118.3 (6)
Zn1—O7—Zn2104.01 (2)C10—C17—C11125.0 (6)
Zn1i—O7—Zn2124.09 (3)N2—C18—C12124.3 (5)
Zn1—O7—Zn2i124.09 (3)N2—C18—H18A117.8
Zn1i—O7—Zn2i104.01 (2)C12—C18—H18A117.8
Zn2—O7—Zn2i106.67 (19)N1—C19—C17122.8 (5)
C5—C1—C8119.1 (4)N1—C19—C21117.3 (5)
C5—C1—C3120.0 (4)C17—C19—C21119.9 (5)
C8—C1—C3120.8 (4)N1—C20—C15123.1 (6)
C4—C2—C7ii120.7 (4)N1—C20—H20A118.4
C4—C2—H2A119.7C15—C20—H20A118.4
C7ii—C2—H2A119.7N2—C21—C16122.4 (5)
O3—C3—O4i123.5 (4)N2—C21—C19117.5 (5)
O3—C3—C1119.1 (4)C16—C21—C19120.1 (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) x1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y+1, z+1.

Experimental details

(HUT-11)(HUT-12)
Crystal data
Chemical formulaC75H42N8O19Zn5·H2O·3.04(O)C42H22N4O13Zn4·4(O)
Mr1752.731116.12
Crystal system, space groupMonoclinic, C2/cMonoclinic, C2/c
Temperature (K)150298
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)
V3)13924.0 (19)4134.1 (2)
Z84
Radiation typeSynchrotron, λ = 0.6889 ÅMo Kα
µ (mm1)1.642.38
Crystal size (mm)0.04 × 0.03 × 0.030.24 × 0.2 × 0.2
Data collection
DiffractometerRigaku Saturn724+ (2x2 bin mode)
diffractometer
Xcalibur
diffractometer
Absorption correctionMulti-scanMulti-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.
Tmin, Tmax0.833, 10.971, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
118881, 20944, 18223 13337, 4185, 2285
Rint0.0570.079
(sin θ/λ)max1)0.7140.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.092, 1.06 0.046, 0.076, 0.82
No. of reflections209444185
No. of parameters1188308
H-atom treatmentAll H-atom parameters refinedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0374P)2 + 26.1353P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0252P)2]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.91, 0.830.63, 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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