Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807042018/hb2516sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807042018/hb2516Isup2.hkl |
CCDC reference: 663541
Key indicators
- Single-crystal X-ray study
- T = 220 K
- Mean (C-C) = 0.013 Å
- Disorder in main residue
- R factor = 0.061
- wR factor = 0.169
- Data-to-parameter ratio = 19.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 6
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C11 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C50 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C60 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C80 PLAT301_ALERT_3_C Main Residue Disorder ......................... 16.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 14 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C11 - C12 ... 1.38 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 21
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A solution of diethyl zinc in toluene (1 ml, 15 wt%) was added to dry t-butanol (10 ml) at 303 K. After several minutes, colourless needles of (I) started to form, and the reaction appeared complete after 30 minutes. The crystal was mounted for X-ray data collection immersed in the reaction solvent.
The atoms of the ethyl groups bound to three of the four Zn atoms are disordered over two positions. The C atoms of these disordered groups were refined with common isotropic displacement parameters. The occupancy factor of the major disorder component refined to 0.559 (9). All H-atoms were positioned geometrically and refined using a riding model with C—H = 0.98Å and Uiso(H) = 1.2Ueq(C) for CH2 groups and C—H = 0.97 Å, Uiso(H) = 1.5Ueq(C) for CH3groups.
Zinc oxide films show promise in a wide variety of optoelectronic devices such as photovoltaics (Delahoy & Cherny, 1996) and sensors (Dimova-Malinovska 2005) due to their electrical conductivity and transparency. While purely inorganic sol-gel, electrochemical or CVD techniques are often employed to make zinc oxide films, another technique is to use organozinc compounds that hydrolyse before or after film deposition. For instance, composite films of zinc oxide have been produced by the spincoating and subsequent hydrolysis of THF solutions of diethyl zinc (Beek et al., 2005). The THF solvent was apparently able to stabilize the otherwise reactive organozinc in order to form good films. In an attempt to use t-butanol as a solvent for zinc oxide thin film deposition with diethyl zinc, we found that large needles of the partially alcoholyzed zinc title compound, (I), crystallized out after a few minutes.
In the structure of (I) (Fig 1) each Zn atom carries an ethyl substituent and binds to three t-butoxo O atoms. The resulting tetrameric unit is a distorted cube with the Zn and O atoms in distorted tetrahedral arrangements and Zn—O distances in the range 2.084 (4)Å to 2.055 (4)Å [mean 2.073 (6) Å]. This compares with a mean value of 2.07 (2)Å for the 11 other cubic tetrakis(µ3-alkyloxo)tetra-alkyl-tetrazinc complexes reported previously (Bond et al., 2001; Herman et al., 1992; Polarz et al., 2005 and Shearer & Spencer, 1980; Boyle et al., 2004). In the crystal structure of (I) there are no significant close contacts with the shortest intermolecular C62···H32Di (i = x, y - 1, z) distance being 3.02 Å.
For background on zinc oxide films see Delahoy & Cherny (1996); Dimova-Malinovska (2005); Beek et al. (2005). Structures of a number of related tetrakis(µ3-alkyloxo)tetra-alkyl-tetrazinc complexes have been reported previously: Bond et al. (2001); Herman et al. (1992); Polarz et al. (2005); Shearer & Spencer (1980); Boyle et al. (2004).
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), enCIFer (Allen et al., 2004) and PLATON (Spek, 2003).
[Zn4(C2H5)4(C4H9O)4] | Z = 2 |
Mr = 670.17 | F(000) = 704 |
Triclinic, P1 | Dx = 1.387 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.0097 (3) Å | Cell parameters from 13011 reflections |
b = 10.1372 (3) Å | θ = 1.0–25.0° |
c = 17.7908 (7) Å | µ = 2.98 mm−1 |
α = 94.740 (2)° | T = 220 K |
β = 101.120 (2)° | Needle, colourless |
γ = 113.086 (2)° | 0.23 × 0.07 × 0.02 mm |
V = 1604.25 (9) Å3 |
Nonius KappaCCD diffractometer | 4047 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.068 |
Thin–slice ω and φ scans | θmax = 25.1°, θmin = 3.5° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −11→11 |
Tmin = 0.808, Tmax = 0.985 | k = −12→12 |
13938 measured reflections | l = −19→21 |
5615 independent reflections |
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)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.169 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0757P)2 + 2.8014P] where P = (Fo2 + 2Fc2)/3 |
5615 reflections | (Δ/σ)max = 0.001 |
293 parameters | Δρmax = 0.63 e Å−3 |
21 restraints | Δρmin = −0.70 e Å−3 |
[Zn4(C2H5)4(C4H9O)4] | γ = 113.086 (2)° |
Mr = 670.17 | V = 1604.25 (9) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.0097 (3) Å | Mo Kα radiation |
b = 10.1372 (3) Å | µ = 2.98 mm−1 |
c = 17.7908 (7) Å | T = 220 K |
α = 94.740 (2)° | 0.23 × 0.07 × 0.02 mm |
β = 101.120 (2)° |
Nonius KappaCCD diffractometer | 5615 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | 4047 reflections with I > 2σ(I) |
Tmin = 0.808, Tmax = 0.985 | Rint = 0.068 |
13938 measured reflections |
R[F2 > 2σ(F2)] = 0.061 | 21 restraints |
wR(F2) = 0.169 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.63 e Å−3 |
5615 reflections | Δρmin = −0.70 e Å−3 |
293 parameters |
Experimental. Three of the four ethyl groups are disordered, each over two sites. Common, isotropic displacement parameters were applied to the carbon atoms in all four of these groups. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'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 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn10 | 0.35356 (8) | 0.28721 (8) | 0.66335 (4) | 0.0558 (2) | |
Zn20 | 0.33809 (8) | 0.13653 (8) | 0.80705 (5) | 0.0581 (2) | |
Zn30 | 0.54499 (9) | 0.11431 (9) | 0.70330 (5) | 0.0634 (3) | |
Zn40 | 0.62433 (8) | 0.40687 (8) | 0.80647 (4) | 0.0569 (2) | |
C11 | 0.2445 (12) | 0.3324 (13) | 0.5710 (5) | 0.111 (4) | |
H11A | 0.3213 | 0.3880 | 0.5452 | 0.133* | |
H11B | 0.1839 | 0.2387 | 0.5362 | 0.133* | |
C12 | 0.1518 (14) | 0.4034 (14) | 0.5699 (6) | 0.134 (5) | |
H12A | 0.1141 | 0.4110 | 0.5167 | 0.200* | |
H12B | 0.2076 | 0.5002 | 0.6008 | 0.200* | |
H12C | 0.0684 | 0.3491 | 0.5912 | 0.200* | |
C21 | 0.203 (3) | −0.003 (3) | 0.8655 (17) | 0.095 (2)* | 0.441 (9) |
H21A | 0.1783 | −0.1023 | 0.8405 | 0.114* | 0.441 (9) |
H21B | 0.2636 | 0.0109 | 0.9183 | 0.114* | 0.441 (9) |
C22 | 0.068 (3) | 0.003 (3) | 0.8727 (19) | 0.140 (4)* | 0.441 (9) |
H22A | 0.0062 | −0.0852 | 0.8889 | 0.209* | 0.441 (9) |
H22B | 0.0147 | 0.0115 | 0.8229 | 0.209* | 0.441 (9) |
H22C | 0.0892 | 0.0867 | 0.9112 | 0.209* | 0.441 (9) |
C21' | 0.216 (2) | 0.039 (2) | 0.8726 (13) | 0.095 (2)* | 0.559 (9) |
H21C | 0.1217 | −0.0274 | 0.8358 | 0.114* | 0.559 (9) |
H21D | 0.2624 | −0.0228 | 0.8936 | 0.114* | 0.559 (9) |
C22' | 0.168 (3) | 0.084 (3) | 0.9346 (13) | 0.140 (4)* | 0.559 (9) |
H22D | 0.1186 | 0.0008 | 0.9580 | 0.209* | 0.559 (9) |
H22E | 0.0988 | 0.1261 | 0.9159 | 0.209* | 0.559 (9) |
H22F | 0.2541 | 0.1562 | 0.9731 | 0.209* | 0.559 (9) |
C31 | 0.583 (2) | −0.043 (3) | 0.6554 (14) | 0.095 (2)* | 0.441 (9) |
H31A | 0.5468 | −0.1255 | 0.6824 | 0.114* | 0.441 (9) |
H31B | 0.5233 | −0.0744 | 0.6015 | 0.114* | 0.441 (9) |
C32 | 0.733 (3) | −0.014 (4) | 0.6544 (18) | 0.140 (4)* | 0.441 (9) |
H32A | 0.7652 | 0.0538 | 0.6192 | 0.209* | 0.441 (9) |
H32B | 0.7392 | −0.1039 | 0.6368 | 0.209* | 0.441 (9) |
H32C | 0.7968 | 0.0285 | 0.7064 | 0.209* | 0.441 (9) |
C31' | 0.656 (2) | 0.0269 (19) | 0.6527 (11) | 0.095 (2)* | 0.559 (9) |
H31C | 0.6278 | 0.0264 | 0.5968 | 0.114* | 0.559 (9) |
H31D | 0.7630 | 0.0925 | 0.6711 | 0.114* | 0.559 (9) |
C32' | 0.642 (3) | −0.116 (2) | 0.6621 (14) | 0.140 (4)* | 0.559 (9) |
H32D | 0.6983 | −0.1450 | 0.6310 | 0.209* | 0.559 (9) |
H32E | 0.5367 | −0.1834 | 0.6451 | 0.209* | 0.559 (9) |
H32F | 0.6794 | −0.1165 | 0.7164 | 0.209* | 0.559 (9) |
C41 | 0.764 (3) | 0.586 (3) | 0.8822 (14) | 0.095 (2)* | 0.441 (9) |
H41A | 0.7842 | 0.6631 | 0.8508 | 0.142* | 0.441 (9) |
H41B | 0.7025 | 0.6025 | 0.9150 | 0.142* | 0.441 (9) |
C42 | 0.901 (3) | 0.622 (3) | 0.9333 (17) | 0.140 (4)* | 0.441 (9) |
H42A | 0.9554 | 0.7267 | 0.9454 | 0.209* | 0.441 (9) |
H42B | 0.9578 | 0.5794 | 0.9098 | 0.209* | 0.441 (9) |
H42C | 0.8845 | 0.5841 | 0.9808 | 0.209* | 0.441 (9) |
C41' | 0.794 (2) | 0.591 (2) | 0.8590 (11) | 0.095 (2)* | 0.559 (9) |
H41C | 0.7961 | 0.6592 | 0.8228 | 0.142* | 0.559 (9) |
H41D | 0.7630 | 0.6249 | 0.9032 | 0.142* | 0.559 (9) |
C42' | 0.942 (2) | 0.616 (3) | 0.8881 (15) | 0.140 (4)* | 0.559 (9) |
H42D | 0.9985 | 0.7166 | 0.9142 | 0.209* | 0.559 (9) |
H42E | 0.9839 | 0.5980 | 0.8456 | 0.209* | 0.559 (9) |
H42F | 0.9476 | 0.5517 | 0.9247 | 0.209* | 0.559 (9) |
O50 | 0.3256 (5) | 0.0832 (4) | 0.6901 (2) | 0.0569 (10) | |
C50 | 0.2051 (10) | −0.0496 (8) | 0.6407 (5) | 0.087 (2) | |
C51 | 0.2095 (14) | −0.1776 (10) | 0.6775 (7) | 0.133 (4) | |
H51A | 0.1862 | −0.1714 | 0.7278 | 0.199* | |
H51B | 0.3087 | −0.1758 | 0.6842 | 0.199* | |
H51C | 0.1363 | −0.2676 | 0.6441 | 0.199* | |
C52 | 0.2303 (13) | −0.0573 (11) | 0.5584 (5) | 0.123 (4) | |
H52A | 0.2310 | 0.0289 | 0.5382 | 0.184* | |
H52B | 0.1502 | −0.1433 | 0.5248 | 0.184* | |
H52C | 0.3255 | −0.0624 | 0.5601 | 0.184* | |
C53 | 0.0588 (10) | −0.0402 (12) | 0.6401 (7) | 0.117 (3) | |
H53A | 0.0449 | −0.0355 | 0.6926 | 0.176* | |
H53B | −0.0227 | −0.1255 | 0.6068 | 0.176* | |
H53C | 0.0596 | 0.0467 | 0.6206 | 0.176* | |
O60 | 0.5792 (5) | 0.3255 (5) | 0.6893 (2) | 0.0554 (10) | |
C60 | 0.6733 (9) | 0.4022 (10) | 0.6402 (5) | 0.083 (2) | |
C61 | 0.8320 (10) | 0.4144 (14) | 0.6760 (7) | 0.133 (4) | |
H61A | 0.8591 | 0.4503 | 0.7315 | 0.200* | |
H61B | 0.9033 | 0.4813 | 0.6518 | 0.200* | |
H61C | 0.8333 | 0.3193 | 0.6671 | 0.200* | |
C62 | 0.6752 (12) | 0.5518 (10) | 0.6416 (6) | 0.109 (3) | |
H62A | 0.5743 | 0.5429 | 0.6214 | 0.164* | |
H62B | 0.7393 | 0.6042 | 0.6096 | 0.164* | |
H62C | 0.7133 | 0.6046 | 0.6947 | 0.164* | |
C63 | 0.6096 (12) | 0.3108 (12) | 0.5580 (5) | 0.107 (3) | |
H63A | 0.5051 | 0.2925 | 0.5401 | 0.160* | |
H63B | 0.6181 | 0.2188 | 0.5590 | 0.160* | |
H63C | 0.6655 | 0.3632 | 0.5229 | 0.160* | |
O70 | 0.3941 (4) | 0.3452 (4) | 0.7825 (2) | 0.0483 (9) | |
C70 | 0.3316 (8) | 0.4399 (8) | 0.8144 (4) | 0.0668 (18) | |
C71 | 0.3813 (12) | 0.4622 (11) | 0.9020 (5) | 0.100 (3) | |
H71A | 0.4896 | 0.5124 | 0.9184 | 0.149* | |
H71B | 0.3488 | 0.3684 | 0.9188 | 0.149* | |
H71C | 0.3373 | 0.5202 | 0.9251 | 0.149* | |
C72 | 0.3888 (11) | 0.5799 (9) | 0.7851 (5) | 0.091 (3) | |
H72A | 0.3690 | 0.5603 | 0.7288 | 0.137* | |
H72B | 0.4959 | 0.6318 | 0.8072 | 0.137* | |
H72C | 0.3388 | 0.6389 | 0.8002 | 0.137* | |
C73 | 0.1627 (9) | 0.3624 (10) | 0.7861 (5) | 0.086 (2) | |
H73A | 0.1342 | 0.3499 | 0.7298 | 0.129* | |
H73B | 0.1175 | 0.4199 | 0.8084 | 0.129* | |
H73C | 0.1282 | 0.2678 | 0.8019 | 0.129* | |
O80 | 0.5643 (5) | 0.1904 (4) | 0.8183 (2) | 0.0527 (10) | |
C80 | 0.6518 (9) | 0.1508 (8) | 0.8808 (4) | 0.0694 (19) | |
C81 | 0.8102 (9) | 0.2040 (11) | 0.8726 (5) | 0.098 (3) | |
H81A | 0.8113 | 0.1578 | 0.8229 | 0.147* | |
H81B | 0.8698 | 0.1798 | 0.9144 | 0.147* | |
H81C | 0.8519 | 0.3088 | 0.8754 | 0.147* | |
C82 | 0.6450 (11) | 0.2222 (11) | 0.9572 (4) | 0.091 (3) | |
H82A | 0.6920 | 0.3272 | 0.9614 | 0.136* | |
H82B | 0.6974 | 0.1933 | 0.9999 | 0.136* | |
H82C | 0.5412 | 0.1917 | 0.9592 | 0.136* | |
C83 | 0.5779 (12) | −0.0139 (10) | 0.8734 (6) | 0.099 (3) | |
H83A | 0.5809 | −0.0589 | 0.8238 | 0.148* | |
H83B | 0.4745 | −0.0443 | 0.8762 | 0.148* | |
H83C | 0.6311 | −0.0436 | 0.9153 | 0.148* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn10 | 0.0630 (5) | 0.0626 (5) | 0.0470 (4) | 0.0363 (4) | 0.0053 (3) | 0.0042 (3) |
Zn20 | 0.0594 (5) | 0.0578 (5) | 0.0626 (5) | 0.0271 (4) | 0.0198 (4) | 0.0144 (4) |
Zn30 | 0.0773 (6) | 0.0697 (5) | 0.0595 (5) | 0.0495 (4) | 0.0165 (4) | 0.0029 (4) |
Zn40 | 0.0526 (4) | 0.0529 (4) | 0.0584 (5) | 0.0211 (3) | 0.0034 (3) | 0.0019 (3) |
C11 | 0.148 (9) | 0.158 (10) | 0.062 (5) | 0.115 (8) | −0.001 (5) | 0.010 (6) |
C12 | 0.170 (11) | 0.211 (13) | 0.078 (6) | 0.149 (11) | 0.008 (7) | 0.032 (7) |
O50 | 0.066 (3) | 0.042 (2) | 0.056 (3) | 0.023 (2) | 0.004 (2) | −0.0074 (19) |
C50 | 0.083 (6) | 0.053 (4) | 0.095 (6) | 0.016 (4) | −0.003 (4) | −0.015 (4) |
C51 | 0.152 (10) | 0.052 (5) | 0.155 (11) | 0.018 (6) | 0.013 (8) | −0.001 (6) |
C52 | 0.153 (10) | 0.100 (7) | 0.078 (6) | 0.044 (7) | −0.012 (6) | −0.039 (6) |
C53 | 0.065 (5) | 0.115 (8) | 0.130 (9) | 0.015 (5) | −0.004 (5) | −0.012 (7) |
O60 | 0.060 (3) | 0.063 (3) | 0.053 (2) | 0.031 (2) | 0.022 (2) | 0.018 (2) |
C60 | 0.078 (5) | 0.101 (6) | 0.089 (6) | 0.041 (5) | 0.043 (4) | 0.041 (5) |
C61 | 0.068 (6) | 0.189 (12) | 0.152 (10) | 0.042 (7) | 0.058 (6) | 0.063 (9) |
C62 | 0.129 (8) | 0.087 (7) | 0.123 (8) | 0.038 (6) | 0.055 (7) | 0.062 (6) |
C63 | 0.130 (8) | 0.148 (9) | 0.069 (6) | 0.072 (7) | 0.050 (6) | 0.032 (6) |
O70 | 0.056 (2) | 0.050 (2) | 0.046 (2) | 0.0334 (19) | 0.0097 (18) | −0.0023 (18) |
C70 | 0.081 (5) | 0.070 (5) | 0.071 (5) | 0.053 (4) | 0.023 (4) | 0.006 (4) |
C71 | 0.135 (8) | 0.123 (8) | 0.068 (5) | 0.089 (7) | 0.021 (5) | −0.007 (5) |
C72 | 0.116 (7) | 0.068 (5) | 0.103 (7) | 0.057 (5) | 0.023 (5) | 0.001 (5) |
C73 | 0.086 (6) | 0.112 (7) | 0.099 (6) | 0.074 (5) | 0.036 (5) | 0.025 (5) |
O80 | 0.060 (2) | 0.058 (3) | 0.049 (2) | 0.036 (2) | 0.0082 (19) | 0.009 (2) |
C80 | 0.087 (5) | 0.078 (5) | 0.060 (4) | 0.055 (4) | 0.011 (4) | 0.013 (4) |
C81 | 0.084 (6) | 0.132 (8) | 0.098 (6) | 0.073 (6) | 0.003 (5) | 0.026 (6) |
C82 | 0.110 (7) | 0.123 (7) | 0.054 (5) | 0.066 (6) | 0.013 (4) | 0.019 (5) |
C83 | 0.137 (8) | 0.087 (6) | 0.101 (7) | 0.072 (6) | 0.029 (6) | 0.043 (5) |
Zn10—C11 | 1.981 (7) | C42—H42C | 0.9700 |
Zn10—O70 | 2.069 (4) | C41'—C42' | 1.387 (14) |
Zn10—O50 | 2.084 (4) | C41'—H41C | 0.9800 |
Zn10—O60 | 2.084 (4) | C41'—H41D | 0.9800 |
Zn10—Zn20 | 3.0831 (10) | C42'—H42D | 0.9700 |
Zn10—Zn40 | 3.0903 (10) | C42'—H42E | 0.9700 |
Zn10—Zn30 | 3.0925 (10) | C42'—H42F | 0.9700 |
Zn20—C21' | 1.90 (2) | O50—C50 | 1.470 (9) |
Zn20—C21 | 2.05 (3) | C50—C53 | 1.503 (12) |
Zn20—O50 | 2.072 (4) | C50—C51 | 1.512 (13) |
Zn20—O70 | 2.072 (4) | C50—C52 | 1.535 (13) |
Zn20—O80 | 2.074 (4) | C51—H51A | 0.9700 |
Zn20—Zn30 | 3.0852 (10) | C51—H51B | 0.9700 |
Zn20—Zn40 | 3.0949 (11) | C51—H51C | 0.9700 |
Zn30—C31 | 1.95 (2) | C52—H52A | 0.9700 |
Zn30—C31' | 1.967 (18) | C52—H52B | 0.9700 |
Zn30—O50 | 2.055 (4) | C52—H52C | 0.9700 |
Zn30—O80 | 2.070 (4) | C53—H53A | 0.9700 |
Zn30—O60 | 2.075 (4) | C53—H53B | 0.9700 |
Zn30—Zn40 | 3.0799 (11) | C53—H53C | 0.9700 |
Zn40—C41' | 1.96 (2) | O60—C60 | 1.454 (8) |
Zn40—C41 | 1.98 (3) | C60—C62 | 1.507 (12) |
Zn40—O60 | 2.071 (4) | C60—C63 | 1.535 (13) |
Zn40—O80 | 2.077 (4) | C60—C61 | 1.545 (13) |
Zn40—O70 | 2.081 (4) | C61—H61A | 0.9700 |
C11—C12 | 1.378 (10) | C61—H61B | 0.9700 |
C11—H11A | 0.9800 | C61—H61C | 0.9700 |
C11—H11B | 0.9800 | C62—H62A | 0.9700 |
C12—H12A | 0.9700 | C62—H62B | 0.9700 |
C12—H12B | 0.9700 | C62—H62C | 0.9700 |
C12—H12C | 0.9700 | C63—H63A | 0.9700 |
C21—C22 | 1.409 (16) | C63—H63B | 0.9700 |
C21—H21A | 0.9800 | C63—H63C | 0.9700 |
C21—H21B | 0.9800 | O70—C70 | 1.467 (7) |
C22—H22A | 0.9700 | C70—C72 | 1.488 (11) |
C22—H22B | 0.9700 | C70—C71 | 1.511 (11) |
C22—H22C | 0.9700 | C70—C73 | 1.515 (11) |
C21'—C22' | 1.390 (15) | C71—H71A | 0.9700 |
C21'—H21C | 0.9800 | C71—H71B | 0.9700 |
C21'—H21D | 0.9800 | C71—H71C | 0.9700 |
C22'—H22D | 0.9700 | C72—H72A | 0.9700 |
C22'—H22E | 0.9700 | C72—H72B | 0.9700 |
C22'—H22F | 0.9700 | C72—H72C | 0.9700 |
C31—C32 | 1.410 (15) | C73—H73A | 0.9700 |
C31—H31A | 0.9800 | C73—H73B | 0.9700 |
C31—H31B | 0.9800 | C73—H73C | 0.9700 |
C32—H32A | 0.9700 | O80—C80 | 1.462 (8) |
C32—H32B | 0.9700 | C80—C81 | 1.502 (11) |
C32—H32C | 0.9700 | C80—C82 | 1.513 (10) |
C31'—C32' | 1.424 (14) | C80—C83 | 1.519 (11) |
C31'—H31C | 0.9800 | C81—H81A | 0.9700 |
C31'—H31D | 0.9800 | C81—H81B | 0.9700 |
C32'—H32D | 0.9700 | C81—H81C | 0.9700 |
C32'—H32E | 0.9700 | C82—H82A | 0.9700 |
C32'—H32F | 0.9700 | C82—H82B | 0.9700 |
C41—C42 | 1.378 (16) | C82—H82C | 0.9700 |
C41—H41A | 0.9800 | C83—H83A | 0.9700 |
C41—H41B | 0.9800 | C83—H83B | 0.9700 |
C42—H42A | 0.9700 | C83—H83C | 0.9700 |
C42—H42B | 0.9700 | ||
C11—Zn10—O70 | 135.1 (3) | H31C—C31'—H31D | 106.9 |
C11—Zn10—O50 | 128.1 (4) | C31'—C32'—H32D | 109.5 |
O70—Zn10—O50 | 83.44 (16) | C31'—C32'—H32E | 109.5 |
C11—Zn10—O60 | 126.2 (4) | H32D—C32'—H32E | 109.5 |
O70—Zn10—O60 | 83.43 (15) | C31'—C32'—H32F | 109.5 |
O50—Zn10—O60 | 82.85 (17) | H32D—C32'—H32F | 109.5 |
C11—Zn10—Zn20 | 147.8 (4) | H32E—C32'—H32F | 109.5 |
O70—Zn10—Zn20 | 41.93 (11) | C42—C41—Zn40 | 133 (2) |
O50—Zn10—Zn20 | 41.96 (11) | C42—C41—H41A | 104.1 |
O60—Zn10—Zn20 | 85.60 (11) | Zn40—C41—H41A | 104.1 |
C11—Zn10—Zn40 | 146.2 (4) | C42—C41—H41B | 104.1 |
O70—Zn10—Zn40 | 42.01 (11) | Zn40—C41—H41B | 104.1 |
O50—Zn10—Zn40 | 85.08 (12) | H41A—C41—H41B | 105.5 |
O60—Zn10—Zn40 | 41.78 (11) | C42'—C41'—Zn40 | 128.3 (17) |
Zn20—Zn10—Zn40 | 60.17 (2) | C42'—C41'—H41C | 105.2 |
C11—Zn10—Zn30 | 139.6 (3) | Zn40—C41'—H41C | 105.2 |
O70—Zn10—Zn30 | 85.28 (10) | C42'—C41'—H41D | 105.2 |
O50—Zn10—Zn30 | 41.31 (12) | Zn40—C41'—H41D | 105.2 |
O60—Zn10—Zn30 | 41.86 (12) | H41C—C41'—H41D | 105.9 |
Zn20—Zn10—Zn30 | 59.94 (2) | C41'—C42'—H42D | 109.5 |
Zn40—Zn10—Zn30 | 59.76 (2) | C41'—C42'—H42E | 109.5 |
C21'—Zn20—C21 | 10.8 (11) | H42D—C42'—H42E | 109.5 |
C21'—Zn20—O50 | 131.8 (7) | C41'—C42'—H42F | 109.5 |
C21—Zn20—O50 | 122.8 (8) | H42D—C42'—H42F | 109.5 |
C21'—Zn20—O70 | 129.5 (6) | H42E—C42'—H42F | 109.5 |
C21—Zn20—O70 | 139.6 (7) | C50—O50—Zn30 | 119.6 (4) |
O50—Zn20—O70 | 83.65 (15) | C50—O50—Zn20 | 121.9 (5) |
C21'—Zn20—O80 | 128.2 (7) | Zn30—O50—Zn20 | 96.74 (18) |
C21—Zn20—O80 | 126.1 (7) | C50—O50—Zn10 | 120.3 (4) |
O50—Zn20—O80 | 82.95 (16) | Zn30—O50—Zn10 | 96.68 (18) |
O70—Zn20—O80 | 83.41 (15) | Zn20—O50—Zn10 | 95.78 (16) |
C21'—Zn20—Zn10 | 146.1 (7) | O50—C50—C53 | 107.7 (7) |
C21—Zn20—Zn10 | 146.4 (8) | O50—C50—C51 | 107.5 (7) |
O50—Zn20—Zn10 | 42.26 (11) | C53—C50—C51 | 109.6 (9) |
O70—Zn20—Zn10 | 41.85 (10) | O50—C50—C52 | 108.6 (7) |
O80—Zn20—Zn10 | 85.65 (11) | C53—C50—C52 | 110.7 (9) |
C21'—Zn20—Zn30 | 145.0 (6) | C51—C50—C52 | 112.5 (8) |
C21—Zn20—Zn30 | 134.9 (7) | C50—C51—H51A | 109.5 |
O50—Zn20—Zn30 | 41.43 (12) | C50—C51—H51B | 109.5 |
O70—Zn20—Zn30 | 85.42 (10) | H51A—C51—H51B | 109.5 |
O80—Zn20—Zn30 | 41.85 (11) | C50—C51—H51C | 109.5 |
Zn10—Zn20—Zn30 | 60.18 (2) | H51A—C51—H51C | 109.5 |
C21'—Zn20—Zn40 | 143.1 (7) | H51B—C51—H51C | 109.5 |
C21—Zn20—Zn40 | 150.8 (8) | C50—C52—H52A | 109.5 |
O50—Zn20—Zn40 | 85.15 (12) | C50—C52—H52B | 109.5 |
O70—Zn20—Zn40 | 41.92 (11) | H52A—C52—H52B | 109.5 |
O80—Zn20—Zn40 | 41.82 (11) | C50—C52—H52C | 109.5 |
Zn10—Zn20—Zn40 | 60.03 (2) | H52A—C52—H52C | 109.5 |
Zn30—Zn20—Zn40 | 59.78 (3) | H52B—C52—H52C | 109.5 |
C31—Zn30—C31' | 23.8 (7) | C50—C53—H53A | 109.5 |
C31—Zn30—O50 | 117.8 (7) | C50—C53—H53B | 109.5 |
C31'—Zn30—O50 | 137.0 (6) | H53A—C53—H53B | 109.5 |
C31—Zn30—O80 | 131.8 (7) | C50—C53—H53C | 109.5 |
C31'—Zn30—O80 | 133.0 (6) | H53A—C53—H53C | 109.5 |
O50—Zn30—O80 | 83.45 (16) | H53B—C53—H53C | 109.5 |
C31—Zn30—O60 | 137.6 (8) | C60—O60—Zn40 | 121.5 (5) |
C31'—Zn30—O60 | 117.0 (5) | C60—O60—Zn30 | 121.6 (4) |
O50—Zn30—O60 | 83.77 (16) | Zn40—O60—Zn30 | 95.96 (16) |
O80—Zn30—O60 | 83.70 (16) | C60—O60—Zn10 | 119.4 (4) |
C31—Zn30—Zn40 | 156.2 (7) | Zn40—O60—Zn10 | 96.10 (16) |
C31'—Zn30—Zn40 | 135.4 (6) | Zn30—O60—Zn10 | 96.05 (17) |
O50—Zn30—Zn40 | 85.81 (11) | O60—C60—C62 | 109.1 (7) |
O80—Zn30—Zn40 | 42.12 (11) | O60—C60—C63 | 107.7 (7) |
O60—Zn30—Zn40 | 41.96 (11) | C62—C60—C63 | 112.2 (8) |
C31—Zn30—Zn20 | 135.3 (7) | O60—C60—C61 | 106.2 (7) |
C31'—Zn30—Zn20 | 157.2 (5) | C62—C60—C61 | 110.1 (9) |
O50—Zn30—Zn20 | 41.84 (12) | C63—C60—C61 | 111.2 (8) |
O80—Zn30—Zn20 | 41.95 (11) | C60—C61—H61A | 109.5 |
O60—Zn30—Zn20 | 85.69 (11) | C60—C61—H61B | 109.5 |
Zn40—Zn30—Zn20 | 60.26 (2) | H61A—C61—H61B | 109.5 |
C31—Zn30—Zn10 | 140.0 (7) | C60—C61—H61C | 109.5 |
C31'—Zn30—Zn10 | 138.9 (5) | H61A—C61—H61C | 109.5 |
O50—Zn30—Zn10 | 42.01 (12) | H61B—C61—H61C | 109.5 |
O80—Zn30—Zn10 | 85.47 (11) | C60—C62—H62A | 109.5 |
O60—Zn30—Zn10 | 42.09 (11) | C60—C62—H62B | 109.5 |
Zn40—Zn30—Zn10 | 60.09 (2) | H62A—C62—H62B | 109.5 |
Zn20—Zn30—Zn10 | 59.88 (2) | C60—C62—H62C | 109.5 |
C41'—Zn40—C41 | 15.8 (8) | H62A—C62—H62C | 109.5 |
C41'—Zn40—O60 | 123.3 (6) | H62B—C62—H62C | 109.5 |
C41—Zn40—O60 | 138.5 (7) | C60—C63—H63A | 109.5 |
C41'—Zn40—O80 | 134.2 (6) | C60—C63—H63B | 109.5 |
C41—Zn40—O80 | 128.9 (7) | H63A—C63—H63B | 109.5 |
O60—Zn40—O80 | 83.66 (16) | C60—C63—H63C | 109.5 |
C41'—Zn40—O70 | 131.4 (6) | H63A—C63—H63C | 109.5 |
C41—Zn40—O70 | 120.7 (7) | H63B—C63—H63C | 109.5 |
O60—Zn40—O70 | 83.49 (15) | C70—O70—Zn10 | 120.0 (4) |
O80—Zn40—O70 | 83.15 (16) | C70—O70—Zn20 | 120.9 (4) |
C41'—Zn40—Zn30 | 142.4 (6) | Zn10—O70—Zn20 | 96.22 (16) |
C41—Zn40—Zn30 | 153.2 (7) | C70—O70—Zn40 | 121.1 (4) |
O60—Zn40—Zn30 | 42.08 (12) | Zn10—O70—Zn40 | 96.26 (15) |
O80—Zn40—Zn30 | 41.96 (11) | Zn20—O70—Zn40 | 96.35 (15) |
O70—Zn40—Zn30 | 85.42 (10) | O70—C70—C72 | 108.5 (6) |
C41'—Zn40—Zn10 | 140.0 (6) | O70—C70—C71 | 107.2 (5) |
C41—Zn40—Zn10 | 143.4 (7) | C72—C70—C71 | 111.7 (7) |
O60—Zn40—Zn10 | 42.12 (11) | O70—C70—C73 | 107.4 (6) |
O80—Zn40—Zn10 | 85.43 (11) | C72—C70—C73 | 110.6 (7) |
O70—Zn40—Zn10 | 41.73 (10) | C71—C70—C73 | 111.3 (7) |
Zn30—Zn40—Zn10 | 60.16 (2) | C70—C71—H71A | 109.5 |
C41'—Zn40—Zn20 | 151.1 (5) | C70—C71—H71B | 109.5 |
C41—Zn40—Zn20 | 135.5 (7) | H71A—C71—H71B | 109.5 |
O60—Zn40—Zn20 | 85.52 (12) | C70—C71—H71C | 109.5 |
O80—Zn40—Zn20 | 41.76 (11) | H71A—C71—H71C | 109.5 |
O70—Zn40—Zn20 | 41.72 (11) | H71B—C71—H71C | 109.5 |
Zn30—Zn40—Zn20 | 59.95 (3) | C70—C72—H72A | 109.5 |
Zn10—Zn40—Zn20 | 59.80 (2) | C70—C72—H72B | 109.5 |
C12—C11—Zn10 | 127.3 (7) | H72A—C72—H72B | 109.5 |
C12—C11—H11A | 105.5 | C70—C72—H72C | 109.5 |
Zn10—C11—H11A | 105.5 | H72A—C72—H72C | 109.5 |
C12—C11—H11B | 105.5 | H72B—C72—H72C | 109.5 |
Zn10—C11—H11B | 105.5 | C70—C73—H73A | 109.5 |
H11A—C11—H11B | 106.1 | C70—C73—H73B | 109.5 |
C11—C12—H12A | 109.5 | H73A—C73—H73B | 109.5 |
C11—C12—H12B | 109.5 | C70—C73—H73C | 109.5 |
H12A—C12—H12B | 109.5 | H73A—C73—H73C | 109.5 |
C11—C12—H12C | 109.5 | H73B—C73—H73C | 109.5 |
H12A—C12—H12C | 109.5 | C80—O80—Zn30 | 119.9 (4) |
H12B—C12—H12C | 109.5 | C80—O80—Zn20 | 121.7 (4) |
C22—C21—Zn20 | 121 (2) | Zn30—O80—Zn20 | 96.21 (17) |
C22—C21—H21A | 107.2 | C80—O80—Zn40 | 120.7 (4) |
Zn20—C21—H21A | 107.2 | Zn30—O80—Zn40 | 95.92 (16) |
C22—C21—H21B | 107.2 | Zn20—O80—Zn40 | 96.42 (16) |
Zn20—C21—H21B | 107.2 | O80—C80—C81 | 108.7 (6) |
H21A—C21—H21B | 106.8 | O80—C80—C82 | 107.5 (5) |
C22'—C21'—Zn20 | 134.9 (17) | C81—C80—C82 | 111.1 (7) |
C22'—C21'—H21C | 103.4 | O80—C80—C83 | 107.3 (6) |
Zn20—C21'—H21C | 103.4 | C81—C80—C83 | 112.0 (7) |
C22'—C21'—H21D | 103.4 | C82—C80—C83 | 109.9 (7) |
Zn20—C21'—H21D | 103.4 | C80—C81—H81A | 109.5 |
H21C—C21'—H21D | 105.3 | C80—C81—H81B | 109.5 |
C21'—C22'—H22D | 109.5 | H81A—C81—H81B | 109.5 |
C21'—C22'—H22E | 109.5 | C80—C81—H81C | 109.5 |
H22D—C22'—H22E | 109.5 | H81A—C81—H81C | 109.5 |
C21'—C22'—H22F | 109.5 | H81B—C81—H81C | 109.5 |
H22D—C22'—H22F | 109.5 | C80—C82—H82A | 109.5 |
H22E—C22'—H22F | 109.5 | C80—C82—H82B | 109.5 |
C32—C31—Zn30 | 118 (2) | H82A—C82—H82B | 109.5 |
C32—C31—H31A | 107.9 | C80—C82—H82C | 109.5 |
Zn30—C31—H31A | 107.9 | H82A—C82—H82C | 109.5 |
C32—C31—H31B | 107.9 | H82B—C82—H82C | 109.5 |
Zn30—C31—H31B | 107.9 | C80—C83—H83A | 109.5 |
H31A—C31—H31B | 107.2 | C80—C83—H83B | 109.5 |
C32'—C31'—Zn30 | 119.8 (17) | H83A—C83—H83B | 109.5 |
C32'—C31'—H31C | 107.4 | C80—C83—H83C | 109.5 |
Zn30—C31'—H31C | 107.4 | H83A—C83—H83C | 109.5 |
C32'—C31'—H31D | 107.4 | H83B—C83—H83C | 109.5 |
Zn30—C31'—H31D | 107.4 | ||
C11—Zn10—Zn20—C21' | −9.9 (12) | C31—Zn30—C31'—C32' | −28 (2) |
O70—Zn10—Zn20—C21' | 92.8 (11) | O50—Zn30—C31'—C32' | −70 (2) |
O50—Zn10—Zn20—C21' | −97.9 (11) | O80—Zn30—C31'—C32' | 70 (2) |
O60—Zn10—Zn20—C21' | 177.9 (11) | O60—Zn30—C31'—C32' | 178.0 (16) |
Zn40—Zn10—Zn20—C21' | 142.8 (11) | Zn40—Zn30—C31'—C32' | 130.2 (17) |
Zn30—Zn10—Zn20—C21' | −147.0 (11) | Zn20—Zn30—C31'—C32' | 4 (3) |
C11—Zn10—Zn20—C21 | 9.6 (14) | Zn10—Zn30—C31'—C32' | −135.0 (15) |
O70—Zn10—Zn20—C21 | 112.4 (13) | C41'—Zn40—C41—C42 | −76 (4) |
O50—Zn10—Zn20—C21 | −78.4 (13) | O60—Zn40—C41—C42 | −94 (3) |
O60—Zn10—Zn20—C21 | −162.6 (13) | O80—Zn40—C41—C42 | 40 (3) |
Zn40—Zn10—Zn20—C21 | 162.3 (13) | O70—Zn40—C41—C42 | 147 (3) |
Zn30—Zn10—Zn20—C21 | −127.5 (13) | Zn30—Zn40—C41—C42 | −19 (4) |
C11—Zn10—Zn20—O50 | 88.0 (6) | Zn10—Zn40—C41—C42 | −164 (2) |
O70—Zn10—Zn20—O50 | −169.3 (2) | Zn20—Zn40—C41—C42 | 97 (3) |
O60—Zn10—Zn20—O50 | −84.2 (2) | C41—Zn40—C41'—C42' | 113 (5) |
Zn40—Zn10—Zn20—O50 | −119.31 (18) | O60—Zn40—C41'—C42' | −82 (2) |
Zn30—Zn10—Zn20—O50 | −49.13 (18) | O80—Zn40—C41'—C42' | 35 (2) |
C11—Zn10—Zn20—O70 | −102.8 (5) | O70—Zn40—C41'—C42' | 164.6 (16) |
O50—Zn10—Zn20—O70 | 169.3 (2) | Zn30—Zn40—C41'—C42' | −29 (2) |
O60—Zn10—Zn20—O70 | 85.1 (2) | Zn10—Zn40—C41'—C42' | −135.2 (17) |
Zn40—Zn10—Zn20—O70 | 49.95 (16) | Zn20—Zn40—C41'—C42' | 102 (2) |
Zn30—Zn10—Zn20—O70 | 120.13 (16) | C31—Zn30—O50—C50 | −4.7 (10) |
C11—Zn10—Zn20—O80 | 172.3 (5) | C31'—Zn30—O50—C50 | 13.2 (9) |
O70—Zn10—Zn20—O80 | −84.97 (19) | O80—Zn30—O50—C50 | −138.9 (5) |
O50—Zn10—Zn20—O80 | 84.3 (2) | O60—Zn30—O50—C50 | 136.7 (5) |
O60—Zn10—Zn20—O80 | 0.09 (16) | Zn40—Zn30—O50—C50 | 178.8 (5) |
Zn40—Zn10—Zn20—O80 | −35.02 (11) | Zn20—Zn30—O50—C50 | −132.8 (6) |
Zn30—Zn10—Zn20—O80 | 35.16 (11) | Zn10—Zn30—O50—C50 | 130.6 (6) |
C11—Zn10—Zn20—Zn30 | 137.1 (5) | C31—Zn30—O50—Zn20 | 128.1 (8) |
O70—Zn10—Zn20—Zn30 | −120.13 (16) | C31'—Zn30—O50—Zn20 | 145.9 (7) |
O50—Zn10—Zn20—Zn30 | 49.13 (18) | O80—Zn30—O50—Zn20 | −6.16 (16) |
O60—Zn10—Zn20—Zn30 | −35.07 (12) | O60—Zn30—O50—Zn20 | −90.50 (17) |
Zn40—Zn10—Zn20—Zn30 | −70.18 (3) | Zn40—Zn30—O50—Zn20 | −48.41 (12) |
C11—Zn10—Zn20—Zn40 | −152.7 (5) | Zn10—Zn30—O50—Zn20 | −96.66 (18) |
O70—Zn10—Zn20—Zn40 | −49.95 (16) | C31—Zn30—O50—Zn10 | −135.2 (8) |
O50—Zn10—Zn20—Zn40 | 119.31 (18) | C31'—Zn30—O50—Zn10 | −117.4 (7) |
O60—Zn10—Zn20—Zn40 | 35.11 (12) | O80—Zn30—O50—Zn10 | 90.50 (17) |
Zn30—Zn10—Zn20—Zn40 | 70.18 (3) | O60—Zn30—O50—Zn10 | 6.16 (16) |
C21'—Zn20—Zn30—C31 | 15.8 (15) | Zn40—Zn30—O50—Zn10 | 48.25 (12) |
C21—Zn20—Zn30—C31 | 9.4 (15) | Zn20—Zn30—O50—Zn10 | 96.66 (18) |
O50—Zn20—Zn30—C31 | −82.1 (10) | C21'—Zn20—O50—C50 | 1.0 (10) |
O70—Zn20—Zn30—C31 | −167.7 (10) | C21—Zn20—O50—C50 | 8.6 (10) |
O80—Zn20—Zn30—C31 | 107.1 (10) | O70—Zn20—O50—C50 | −138.5 (5) |
Zn10—Zn20—Zn30—C31 | −132.3 (9) | O80—Zn20—O50—C50 | 137.4 (5) |
Zn40—Zn20—Zn30—C31 | 157.1 (9) | Zn10—Zn20—O50—C50 | −131.3 (6) |
C21'—Zn20—Zn30—C31' | −2 (2) | Zn30—Zn20—O50—C50 | 131.3 (6) |
C21—Zn20—Zn30—C31' | −8.4 (19) | Zn40—Zn20—O50—C50 | 179.4 (5) |
O50—Zn20—Zn30—C31' | −99.9 (16) | C21'—Zn20—O50—Zn30 | −130.3 (9) |
O70—Zn20—Zn30—C31' | 174.5 (16) | C21—Zn20—O50—Zn30 | −122.7 (8) |
O80—Zn20—Zn30—C31' | 89.3 (16) | O70—Zn20—O50—Zn30 | 90.27 (17) |
Zn10—Zn20—Zn30—C31' | −150.1 (16) | O80—Zn20—O50—Zn30 | 6.15 (16) |
Zn40—Zn20—Zn30—C31' | 139.3 (16) | Zn10—Zn20—O50—Zn30 | 97.4 (2) |
C21'—Zn20—Zn30—O50 | 97.9 (12) | Zn40—Zn20—O50—Zn30 | 48.15 (12) |
C21—Zn20—Zn30—O50 | 91.5 (12) | C21'—Zn20—O50—Zn10 | 132.2 (8) |
O70—Zn20—Zn30—O50 | −85.6 (2) | C21—Zn20—O50—Zn10 | 139.9 (8) |
O80—Zn20—Zn30—O50 | −170.8 (2) | O70—Zn20—O50—Zn10 | −7.18 (16) |
Zn10—Zn20—Zn30—O50 | −50.22 (17) | O80—Zn20—O50—Zn10 | −91.30 (17) |
Zn40—Zn20—Zn30—O50 | −120.80 (17) | Zn30—Zn20—O50—Zn10 | −97.4 (2) |
C21'—Zn20—Zn30—O80 | −91.3 (12) | Zn40—Zn20—O50—Zn10 | −49.29 (13) |
C21—Zn20—Zn30—O80 | −97.7 (12) | C11—Zn10—O50—C50 | −5.1 (7) |
O50—Zn20—Zn30—O80 | 170.8 (2) | O70—Zn10—O50—C50 | 139.6 (5) |
O70—Zn20—Zn30—O80 | 85.2 (2) | O60—Zn10—O50—C50 | −136.3 (5) |
Zn10—Zn20—Zn30—O80 | 120.60 (17) | Zn20—Zn10—O50—C50 | 132.4 (6) |
Zn40—Zn20—Zn30—O80 | 50.03 (17) | Zn40—Zn10—O50—C50 | −178.2 (5) |
C21'—Zn20—Zn30—O60 | −176.6 (12) | Zn30—Zn10—O50—C50 | −130.1 (6) |
C21—Zn20—Zn30—O60 | 177.0 (11) | C11—Zn10—O50—Zn30 | 125.0 (4) |
O50—Zn20—Zn30—O60 | 85.5 (2) | O70—Zn10—O50—Zn30 | −90.31 (17) |
O70—Zn20—Zn30—O60 | −0.13 (16) | O60—Zn10—O50—Zn30 | −6.14 (16) |
O80—Zn20—Zn30—O60 | −85.4 (2) | Zn20—Zn10—O50—Zn30 | −97.5 (2) |
Zn10—Zn20—Zn30—O60 | 35.24 (12) | Zn40—Zn10—O50—Zn30 | −48.10 (12) |
Zn40—Zn20—Zn30—O60 | −35.33 (12) | C11—Zn10—O50—Zn20 | −137.5 (4) |
C21'—Zn20—Zn30—Zn40 | −141.3 (12) | O70—Zn10—O50—Zn20 | 7.20 (17) |
C21—Zn20—Zn30—Zn40 | −147.7 (11) | O60—Zn10—O50—Zn20 | 91.36 (17) |
O50—Zn20—Zn30—Zn40 | 120.80 (17) | Zn40—Zn10—O50—Zn20 | 49.40 (13) |
O70—Zn20—Zn30—Zn40 | 35.20 (11) | Zn30—Zn10—O50—Zn20 | 97.5 (2) |
O80—Zn20—Zn30—Zn40 | −50.03 (16) | Zn30—O50—C50—C53 | −178.2 (6) |
Zn10—Zn20—Zn30—Zn40 | 70.58 (3) | Zn20—O50—C50—C53 | 60.9 (8) |
C21'—Zn20—Zn30—Zn10 | 148.1 (12) | Zn10—O50—C50—C53 | −59.1 (9) |
C21—Zn20—Zn30—Zn10 | 141.7 (11) | Zn30—O50—C50—C51 | 63.7 (9) |
O50—Zn20—Zn30—Zn10 | 50.22 (17) | Zn20—O50—C50—C51 | −57.1 (9) |
O70—Zn20—Zn30—Zn10 | −35.37 (11) | Zn10—O50—C50—C51 | −177.2 (6) |
O80—Zn20—Zn30—Zn10 | −120.60 (17) | Zn30—O50—C50—C52 | −58.3 (8) |
Zn40—Zn20—Zn30—Zn10 | −70.58 (3) | Zn20—O50—C50—C52 | −179.1 (6) |
C11—Zn10—Zn30—C31 | −20.0 (13) | Zn10—O50—C50—C52 | 60.9 (8) |
O70—Zn10—Zn30—C31 | 161.4 (11) | C41'—Zn40—O60—C60 | 0.4 (9) |
O50—Zn10—Zn30—C31 | 76.0 (11) | C41—Zn40—O60—C60 | 6.3 (12) |
O60—Zn10—Zn30—C31 | −113.1 (11) | O80—Zn40—O60—C60 | −139.7 (5) |
Zn20—Zn10—Zn30—C31 | 126.0 (11) | O70—Zn40—O60—C60 | 136.5 (5) |
Zn40—Zn10—Zn30—C31 | −163.1 (11) | Zn30—Zn40—O60—C60 | −133.1 (5) |
C11—Zn10—Zn30—C31' | 16.9 (11) | Zn10—Zn40—O60—C60 | 130.2 (5) |
O70—Zn10—Zn30—C31' | −161.7 (9) | Zn20—Zn40—O60—C60 | 178.4 (5) |
O50—Zn10—Zn30—C31' | 112.9 (9) | C41'—Zn40—O60—Zn30 | 133.5 (7) |
O60—Zn10—Zn30—C31' | −76.2 (9) | C41—Zn40—O60—Zn30 | 139.4 (10) |
Zn20—Zn10—Zn30—C31' | 162.9 (9) | O80—Zn40—O60—Zn30 | −6.58 (16) |
Zn40—Zn10—Zn30—C31' | −126.2 (9) | O70—Zn40—O60—Zn30 | −90.37 (17) |
C11—Zn10—Zn30—O50 | −96.0 (6) | Zn10—Zn40—O60—Zn30 | −96.77 (19) |
O70—Zn10—Zn30—O50 | 85.4 (2) | Zn20—Zn40—O60—Zn30 | −48.50 (12) |
O60—Zn10—Zn30—O50 | 170.8 (2) | C41'—Zn40—O60—Zn10 | −129.8 (7) |
Zn20—Zn10—Zn30—O50 | 49.99 (17) | C41—Zn40—O60—Zn10 | −123.9 (10) |
Zn40—Zn10—Zn30—O50 | 120.86 (17) | O80—Zn40—O60—Zn10 | 90.19 (17) |
C11—Zn10—Zn30—O80 | 178.7 (6) | O70—Zn40—O60—Zn10 | 6.39 (16) |
O70—Zn10—Zn30—O80 | 0.19 (17) | Zn30—Zn40—O60—Zn10 | 96.77 (19) |
O50—Zn10—Zn30—O80 | −85.2 (2) | Zn20—Zn40—O60—Zn10 | 48.27 (12) |
O60—Zn10—Zn30—O80 | 85.6 (2) | C31—Zn30—O60—C60 | −11.2 (11) |
Zn20—Zn10—Zn30—O80 | −35.25 (12) | C31'—Zn30—O60—C60 | 4.0 (8) |
Zn40—Zn10—Zn30—O80 | 35.62 (12) | O50—Zn30—O60—C60 | −136.3 (5) |
C11—Zn10—Zn30—O60 | 93.1 (6) | O80—Zn30—O60—C60 | 139.6 (5) |
O70—Zn10—Zn30—O60 | −85.4 (2) | Zn40—Zn30—O60—C60 | 133.0 (6) |
O50—Zn10—Zn30—O60 | −170.8 (2) | Zn20—Zn30—O60—C60 | −178.3 (5) |
Zn20—Zn10—Zn30—O60 | −120.86 (17) | Zn10—Zn30—O60—C60 | −130.2 (6) |
Zn40—Zn10—Zn30—O60 | −49.99 (17) | C31—Zn30—O60—Zn40 | −144.3 (10) |
C11—Zn10—Zn30—Zn40 | 143.1 (6) | C31'—Zn30—O60—Zn40 | −129.0 (7) |
O70—Zn10—Zn30—Zn40 | −35.42 (11) | O50—Zn30—O60—Zn40 | 90.66 (17) |
O50—Zn10—Zn30—Zn40 | −120.86 (17) | O80—Zn30—O60—Zn40 | 6.60 (16) |
O60—Zn10—Zn30—Zn40 | 49.99 (17) | Zn20—Zn30—O60—Zn40 | 48.69 (12) |
Zn20—Zn10—Zn30—Zn40 | −70.87 (3) | Zn10—Zn30—O60—Zn40 | 96.81 (18) |
C11—Zn10—Zn30—Zn20 | −146.0 (6) | C31—Zn30—O60—Zn10 | 118.9 (10) |
O70—Zn10—Zn30—Zn20 | 35.44 (11) | C31'—Zn30—O60—Zn10 | 134.2 (7) |
O50—Zn10—Zn30—Zn20 | −49.99 (17) | O50—Zn30—O60—Zn10 | −6.15 (16) |
O60—Zn10—Zn30—Zn20 | 120.86 (17) | O80—Zn30—O60—Zn10 | −90.22 (17) |
Zn40—Zn10—Zn30—Zn20 | 70.87 (3) | Zn40—Zn30—O60—Zn10 | −96.81 (18) |
C31—Zn30—Zn40—C41' | 18 (2) | Zn20—Zn30—O60—Zn10 | −48.13 (12) |
C31'—Zn30—Zn40—C41' | −3.7 (12) | C11—Zn10—O60—C60 | 5.0 (7) |
O50—Zn30—Zn40—C41' | −169.7 (9) | O70—Zn10—O60—C60 | −138.0 (5) |
O80—Zn30—Zn40—C41' | 105.4 (9) | O50—Zn10—O60—C60 | 137.8 (5) |
O60—Zn30—Zn40—C41' | −84.4 (9) | Zn20—Zn10—O60—C60 | 179.9 (5) |
Zn20—Zn30—Zn40—C41' | 155.2 (9) | Zn40—Zn10—O60—C60 | −131.6 (6) |
Zn10—Zn30—Zn40—C41' | −134.6 (9) | Zn30—Zn10—O60—C60 | 131.7 (6) |
C31—Zn30—Zn40—C41 | −4 (2) | C11—Zn10—O60—Zn40 | 136.6 (4) |
C31'—Zn30—Zn40—C41 | −25.8 (17) | O70—Zn10—O60—Zn40 | −6.43 (16) |
O50—Zn30—Zn40—C41 | 168.1 (16) | O50—Zn10—O60—Zn40 | −90.61 (17) |
O80—Zn30—Zn40—C41 | 83.2 (16) | Zn20—Zn10—O60—Zn40 | −48.51 (12) |
O60—Zn30—Zn40—C41 | −106.6 (16) | Zn30—Zn10—O60—Zn40 | −96.68 (18) |
Zn20—Zn30—Zn40—C41 | 133.0 (16) | C11—Zn10—O60—Zn30 | −126.7 (4) |
Zn10—Zn30—Zn40—C41 | −156.7 (16) | O70—Zn10—O60—Zn30 | 90.25 (17) |
C31—Zn30—Zn40—O60 | 102.3 (18) | O50—Zn10—O60—Zn30 | 6.07 (16) |
C31'—Zn30—Zn40—O60 | 80.7 (7) | Zn20—Zn10—O60—Zn30 | 48.18 (12) |
O50—Zn30—Zn40—O60 | −85.3 (2) | Zn40—Zn10—O60—Zn30 | 96.68 (18) |
O80—Zn30—Zn40—O60 | −170.2 (2) | Zn40—O60—C60—C62 | −58.9 (8) |
Zn20—Zn30—Zn40—O60 | −120.40 (17) | Zn30—O60—C60—C62 | 179.7 (6) |
Zn10—Zn30—Zn40—O60 | −50.16 (17) | Zn10—O60—C60—C62 | 60.4 (8) |
C31—Zn30—Zn40—O80 | −87.5 (18) | Zn40—O60—C60—C63 | 179.0 (5) |
C31'—Zn30—Zn40—O80 | −109.1 (7) | Zn30—O60—C60—C63 | 57.6 (7) |
O50—Zn30—Zn40—O80 | 84.9 (2) | Zn10—O60—C60—C63 | −61.7 (7) |
O60—Zn30—Zn40—O80 | 170.2 (2) | Zn40—O60—C60—C61 | 59.8 (9) |
Zn20—Zn30—Zn40—O80 | 49.80 (16) | Zn30—O60—C60—C61 | −61.7 (9) |
Zn10—Zn30—Zn40—O80 | 120.04 (17) | Zn10—O60—C60—C61 | 179.0 (6) |
C31—Zn30—Zn40—O70 | −172.3 (18) | C11—Zn10—O70—C70 | 1.3 (7) |
C31'—Zn30—Zn40—O70 | 166.1 (7) | O50—Zn10—O70—C70 | −138.5 (5) |
O50—Zn30—Zn40—O70 | 0.02 (16) | O60—Zn10—O70—C70 | 138.0 (5) |
O80—Zn30—Zn40—O70 | −84.8 (2) | Zn20—Zn10—O70—C70 | −131.3 (5) |
O60—Zn30—Zn40—O70 | 85.4 (2) | Zn40—Zn10—O70—C70 | 131.6 (5) |
Zn20—Zn30—Zn40—O70 | −35.04 (11) | Zn30—Zn10—O70—C70 | −180.0 (4) |
Zn10—Zn30—Zn40—O70 | 35.19 (11) | C11—Zn10—O70—Zn20 | 132.6 (5) |
C31—Zn30—Zn40—Zn10 | 152.5 (18) | O50—Zn10—O70—Zn20 | −7.20 (16) |
C31'—Zn30—Zn40—Zn10 | 130.9 (7) | O60—Zn10—O70—Zn20 | −90.72 (17) |
O50—Zn30—Zn40—Zn10 | −35.17 (12) | Zn40—Zn10—O70—Zn20 | −97.12 (17) |
O80—Zn30—Zn40—Zn10 | −120.04 (17) | Zn30—Zn10—O70—Zn20 | −48.69 (11) |
O60—Zn30—Zn40—Zn10 | 50.16 (17) | C11—Zn10—O70—Zn40 | −130.2 (5) |
Zn20—Zn30—Zn40—Zn10 | −70.24 (3) | O50—Zn10—O70—Zn40 | 89.92 (17) |
C31—Zn30—Zn40—Zn20 | −137.3 (18) | O60—Zn10—O70—Zn40 | 6.40 (16) |
C31'—Zn30—Zn40—Zn20 | −158.9 (7) | Zn20—Zn10—O70—Zn40 | 97.12 (17) |
O50—Zn30—Zn40—Zn20 | 35.06 (12) | Zn30—Zn10—O70—Zn40 | 48.43 (11) |
O80—Zn30—Zn40—Zn20 | −49.80 (16) | C21'—Zn20—O70—C70 | −3.1 (10) |
O60—Zn30—Zn40—Zn20 | 120.40 (17) | C21—Zn20—O70—C70 | 2.7 (14) |
Zn10—Zn30—Zn40—Zn20 | 70.24 (3) | O50—Zn20—O70—C70 | 137.9 (4) |
C11—Zn10—Zn40—C41' | 2.0 (10) | O80—Zn20—O70—C70 | −138.5 (4) |
O70—Zn10—Zn40—C41' | −102.1 (9) | Zn10—Zn20—O70—C70 | 130.7 (5) |
O50—Zn10—Zn40—C41' | 172.2 (9) | Zn30—Zn20—O70—C70 | 179.5 (4) |
O60—Zn10—Zn40—C41' | 87.5 (9) | Zn40—Zn20—O70—C70 | −132.3 (5) |
Zn20—Zn10—Zn40—C41' | −152.0 (8) | C21'—Zn20—O70—Zn10 | −133.8 (9) |
Zn30—Zn10—Zn40—C41' | 137.6 (8) | C21—Zn20—O70—Zn10 | −128.0 (13) |
C11—Zn10—Zn40—C41 | 27.1 (12) | O50—Zn20—O70—Zn10 | 7.24 (17) |
O70—Zn10—Zn40—C41 | −77.0 (11) | O80—Zn20—O70—Zn10 | 90.84 (16) |
O50—Zn10—Zn40—C41 | −162.7 (11) | Zn30—Zn20—O70—Zn10 | 48.83 (11) |
O60—Zn10—Zn40—C41 | 112.5 (11) | Zn40—Zn20—O70—Zn10 | 97.04 (17) |
Zn20—Zn10—Zn40—C41 | −126.9 (11) | C21'—Zn20—O70—Zn40 | 129.2 (9) |
Zn30—Zn10—Zn40—C41 | 162.6 (11) | C21—Zn20—O70—Zn40 | 135.0 (13) |
C11—Zn10—Zn40—O60 | −85.5 (5) | O50—Zn20—O70—Zn40 | −89.79 (17) |
O70—Zn10—Zn40—O60 | 170.4 (2) | O80—Zn20—O70—Zn40 | −6.20 (15) |
O50—Zn10—Zn40—O60 | 84.8 (2) | Zn10—Zn20—O70—Zn40 | −97.04 (17) |
Zn20—Zn10—Zn40—O60 | 120.59 (17) | Zn30—Zn20—O70—Zn40 | −48.21 (11) |
Zn30—Zn10—Zn40—O60 | 50.10 (17) | C41'—Zn40—O70—C70 | −7.8 (9) |
C11—Zn10—Zn40—O80 | −171.1 (5) | C41—Zn40—O70—C70 | 6.7 (9) |
O70—Zn10—Zn40—O80 | 84.83 (19) | O60—Zn40—O70—C70 | −137.3 (4) |
O50—Zn10—Zn40—O80 | −0.83 (16) | O80—Zn40—O70—C70 | 138.4 (4) |
O60—Zn10—Zn40—O80 | −85.6 (2) | Zn30—Zn40—O70—C70 | −179.5 (4) |
Zn20—Zn10—Zn40—O80 | 34.99 (11) | Zn10—Zn40—O70—C70 | −130.8 (5) |
Zn30—Zn10—Zn40—O80 | −35.50 (11) | Zn20—Zn40—O70—C70 | 132.2 (5) |
C11—Zn10—Zn40—O70 | 104.1 (5) | C41'—Zn40—O70—Zn10 | 123.0 (7) |
O50—Zn10—Zn40—O70 | −85.7 (2) | C41—Zn40—O70—Zn10 | 137.5 (8) |
O60—Zn10—Zn40—O70 | −170.4 (2) | O60—Zn40—O70—Zn10 | −6.44 (16) |
Zn20—Zn10—Zn40—O70 | −49.84 (16) | O80—Zn40—O70—Zn10 | −90.80 (16) |
Zn30—Zn10—Zn40—O70 | −120.33 (16) | Zn30—Zn40—O70—Zn10 | −48.68 (12) |
C11—Zn10—Zn40—Zn30 | −135.6 (5) | Zn20—Zn40—O70—Zn10 | −97.00 (17) |
O70—Zn10—Zn40—Zn30 | 120.33 (16) | C41'—Zn40—O70—Zn20 | −140.0 (7) |
O50—Zn10—Zn40—Zn30 | 34.67 (12) | C41—Zn40—O70—Zn20 | −125.5 (8) |
O60—Zn10—Zn40—Zn30 | −50.10 (17) | O60—Zn40—O70—Zn20 | 90.56 (16) |
Zn20—Zn10—Zn40—Zn30 | 70.49 (3) | O80—Zn40—O70—Zn20 | 6.20 (15) |
C11—Zn10—Zn40—Zn20 | 153.9 (5) | Zn30—Zn40—O70—Zn20 | 48.32 (11) |
O70—Zn10—Zn40—Zn20 | 49.84 (16) | Zn10—Zn40—O70—Zn20 | 97.00 (17) |
O50—Zn10—Zn40—Zn20 | −35.82 (12) | Zn10—O70—C70—C72 | −59.0 (7) |
O60—Zn10—Zn40—Zn20 | −120.59 (17) | Zn20—O70—C70—C72 | −178.5 (5) |
Zn30—Zn10—Zn40—Zn20 | −70.49 (3) | Zn40—O70—C70—C72 | 60.7 (7) |
C21'—Zn20—Zn40—C41' | −4.7 (16) | Zn10—O70—C70—C71 | −179.8 (5) |
C21—Zn20—Zn40—C41' | −18.7 (18) | Zn20—O70—C70—C71 | 60.8 (7) |
O50—Zn20—Zn40—C41' | 177.2 (12) | Zn40—O70—C70—C71 | −60.0 (7) |
O70—Zn20—Zn40—C41' | 91.3 (12) | Zn10—O70—C70—C73 | 60.5 (7) |
O80—Zn20—Zn40—C41' | −97.9 (12) | Zn20—O70—C70—C73 | −59.0 (6) |
Zn10—Zn20—Zn40—C41' | 141.2 (12) | Zn40—O70—C70—C73 | −179.8 (4) |
Zn30—Zn20—Zn40—C41' | −148.0 (12) | C31—Zn30—O80—C80 | 16.6 (10) |
C21'—Zn20—Zn40—C41 | −8.7 (14) | C31'—Zn30—O80—C80 | −15.7 (9) |
C21—Zn20—Zn40—C41 | −22.7 (17) | O50—Zn30—O80—C80 | 138.4 (5) |
O50—Zn20—Zn40—C41 | 173.2 (10) | O60—Zn30—O80—C80 | −137.2 (5) |
O70—Zn20—Zn40—C41 | 87.3 (10) | Zn40—Zn30—O80—C80 | −130.6 (5) |
O80—Zn20—Zn40—C41 | −101.9 (10) | Zn20—Zn30—O80—C80 | 132.2 (5) |
Zn10—Zn20—Zn40—C41 | 137.2 (10) | Zn10—Zn30—O80—C80 | −179.5 (5) |
Zn30—Zn20—Zn40—C41 | −152.0 (10) | C31—Zn30—O80—Zn20 | −115.6 (9) |
C21'—Zn20—Zn40—O60 | 178.7 (10) | C31'—Zn30—O80—Zn20 | −148.0 (8) |
C21—Zn20—Zn40—O60 | 164.7 (14) | O50—Zn30—O80—Zn20 | 6.15 (16) |
O50—Zn20—Zn40—O60 | 0.66 (16) | O60—Zn30—O80—Zn20 | 90.56 (17) |
O70—Zn20—Zn40—O60 | −85.24 (19) | Zn40—Zn30—O80—Zn20 | 97.14 (17) |
O80—Zn20—Zn40—O60 | 85.5 (2) | Zn10—Zn30—O80—Zn20 | 48.32 (12) |
Zn10—Zn20—Zn40—O60 | −35.39 (11) | C31—Zn30—O80—Zn40 | 147.3 (9) |
Zn30—Zn20—Zn40—O60 | 35.44 (11) | C31'—Zn30—O80—Zn40 | 114.9 (8) |
C21'—Zn20—Zn40—O80 | 93.3 (11) | O50—Zn30—O80—Zn40 | −90.99 (17) |
C21—Zn20—Zn40—O80 | 79.2 (14) | O60—Zn30—O80—Zn40 | −6.58 (16) |
O50—Zn20—Zn40—O80 | −84.8 (2) | Zn20—Zn30—O80—Zn40 | −97.14 (17) |
O70—Zn20—Zn40—O80 | −170.7 (2) | Zn10—Zn30—O80—Zn40 | −48.82 (12) |
Zn10—Zn20—Zn40—O80 | −120.89 (17) | C21'—Zn20—O80—C80 | 2.0 (9) |
Zn30—Zn20—Zn40—O80 | −50.06 (17) | C21—Zn20—O80—C80 | −11.3 (11) |
C21'—Zn20—Zn40—O70 | −96.0 (11) | O50—Zn20—O80—C80 | −137.1 (5) |
C21—Zn20—Zn40—O70 | −110.1 (14) | O70—Zn20—O80—C80 | 138.5 (5) |
O50—Zn20—Zn40—O70 | 85.90 (19) | Zn10—Zn20—O80—C80 | −179.5 (4) |
O80—Zn20—Zn40—O70 | 170.7 (2) | Zn30—Zn20—O80—C80 | −131.0 (5) |
Zn10—Zn20—Zn40—O70 | 49.86 (15) | Zn40—Zn20—O80—C80 | 132.3 (5) |
Zn30—Zn20—Zn40—O70 | 120.68 (15) | C21'—Zn20—O80—Zn30 | 133.1 (8) |
C21'—Zn20—Zn40—Zn30 | 143.3 (10) | C21—Zn20—O80—Zn30 | 119.7 (10) |
C21—Zn20—Zn40—Zn30 | 129.3 (13) | O50—Zn20—O80—Zn30 | −6.10 (16) |
O50—Zn20—Zn40—Zn30 | −34.78 (12) | O70—Zn20—O80—Zn30 | −90.49 (16) |
O70—Zn20—Zn40—Zn30 | −120.68 (15) | Zn10—Zn20—O80—Zn30 | −48.50 (12) |
O80—Zn20—Zn40—Zn30 | 50.06 (17) | Zn40—Zn20—O80—Zn30 | −96.70 (18) |
Zn10—Zn20—Zn40—Zn30 | −70.82 (3) | C21'—Zn20—O80—Zn40 | −130.2 (8) |
C21'—Zn20—Zn40—Zn10 | −145.9 (10) | C21—Zn20—O80—Zn40 | −143.6 (9) |
C21—Zn20—Zn40—Zn10 | −159.9 (13) | O50—Zn20—O80—Zn40 | 90.60 (17) |
O50—Zn20—Zn40—Zn10 | 36.05 (12) | O70—Zn20—O80—Zn40 | 6.21 (15) |
O70—Zn20—Zn40—Zn10 | −49.86 (15) | Zn10—Zn20—O80—Zn40 | 48.21 (12) |
O80—Zn20—Zn40—Zn10 | 120.89 (17) | Zn30—Zn20—O80—Zn40 | 96.70 (18) |
Zn30—Zn20—Zn40—Zn10 | 70.82 (3) | C41'—Zn40—O80—C80 | 5.2 (9) |
O70—Zn10—C11—C12 | −9.6 (16) | C41—Zn40—O80—C80 | −14.8 (10) |
O50—Zn10—C11—C12 | 116.0 (12) | O60—Zn40—O80—C80 | 136.7 (4) |
O60—Zn10—C11—C12 | −131.8 (12) | O70—Zn40—O80—C80 | −139.1 (4) |
Zn20—Zn10—C11—C12 | 57.9 (16) | Zn30—Zn40—O80—C80 | 130.1 (5) |
Zn40—Zn10—C11—C12 | −76.4 (15) | Zn10—Zn40—O80—C80 | 179.0 (4) |
Zn30—Zn10—C11—C12 | 172.5 (10) | Zn20—Zn40—O80—C80 | −132.9 (5) |
C21'—Zn20—C21—C22 | 55 (6) | C41'—Zn40—O80—Zn30 | −124.9 (8) |
O50—Zn20—C21—C22 | −93 (2) | C41—Zn40—O80—Zn30 | −144.9 (9) |
O70—Zn20—C21—C22 | 30 (3) | O60—Zn40—O80—Zn30 | 6.59 (16) |
O80—Zn20—C21—C22 | 160 (2) | O70—Zn40—O80—Zn30 | 90.76 (16) |
Zn10—Zn20—C21—C22 | −42 (3) | Zn10—Zn40—O80—Zn30 | 48.88 (12) |
Zn30—Zn20—C21—C22 | −145 (2) | Zn20—Zn40—O80—Zn30 | 96.95 (19) |
Zn40—Zn20—C21—C22 | 106 (3) | C41'—Zn40—O80—Zn20 | 138.2 (8) |
C21—Zn20—C21'—C22' | 179 (9) | C41—Zn40—O80—Zn20 | 118.1 (9) |
O50—Zn20—C21'—C22' | −144 (2) | O60—Zn40—O80—Zn20 | −90.36 (17) |
O70—Zn20—C21'—C22' | −21 (3) | O70—Zn40—O80—Zn20 | −6.19 (15) |
O80—Zn20—C21'—C22' | 96 (3) | Zn30—Zn40—O80—Zn20 | −96.95 (19) |
Zn10—Zn20—C21'—C22' | −81 (3) | Zn10—Zn40—O80—Zn20 | −48.08 (12) |
Zn30—Zn20—C21'—C22' | 154 (2) | Zn30—O80—C80—C81 | 59.5 (7) |
Zn40—Zn20—C21'—C22' | 38 (3) | Zn20—O80—C80—C81 | 179.6 (5) |
C31'—Zn30—C31—C32 | 22 (2) | Zn40—O80—C80—C81 | −59.1 (7) |
O50—Zn30—C31—C32 | 170.8 (19) | Zn30—O80—C80—C82 | 180.0 (5) |
O80—Zn30—C31—C32 | −82 (2) | Zn20—O80—C80—C82 | −59.9 (7) |
O60—Zn30—C31—C32 | 58 (3) | Zn40—O80—C80—C82 | 61.3 (7) |
Zn40—Zn30—C31—C32 | −18 (4) | Zn30—O80—C80—C83 | −61.8 (7) |
Zn20—Zn30—C31—C32 | −140.9 (19) | Zn20—O80—C80—C83 | 58.3 (7) |
Zn10—Zn30—C31—C32 | 123.6 (19) | Zn40—O80—C80—C83 | 179.5 (5) |
Experimental details
Crystal data | |
Chemical formula | [Zn4(C2H5)4(C4H9O)4] |
Mr | 670.17 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 220 |
a, b, c (Å) | 10.0097 (3), 10.1372 (3), 17.7908 (7) |
α, β, γ (°) | 94.740 (2), 101.120 (2), 113.086 (2) |
V (Å3) | 1604.25 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.98 |
Crystal size (mm) | 0.23 × 0.07 × 0.02 |
Data collection | |
Diffractometer | Nonius KappaCCD |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995) |
Tmin, Tmax | 0.808, 0.985 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13938, 5615, 4047 |
Rint | 0.068 |
(sin θ/λ)max (Å−1) | 0.598 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.061, 0.169, 1.06 |
No. of reflections | 5615 |
No. of parameters | 293 |
No. of restraints | 21 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.63, −0.70 |
Computer programs: COLLECT (Nonius, 1998), SCALEPACK (Otwinowski & Minor, 1997), SCALEPACK and DENZO (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1993), ORTEP-3 (Farrugia, 1997), SHELXL97 (Sheldrick, 1997), enCIFer (Allen et al., 2004) and PLATON (Spek, 2003).
Zinc oxide films show promise in a wide variety of optoelectronic devices such as photovoltaics (Delahoy & Cherny, 1996) and sensors (Dimova-Malinovska 2005) due to their electrical conductivity and transparency. While purely inorganic sol-gel, electrochemical or CVD techniques are often employed to make zinc oxide films, another technique is to use organozinc compounds that hydrolyse before or after film deposition. For instance, composite films of zinc oxide have been produced by the spincoating and subsequent hydrolysis of THF solutions of diethyl zinc (Beek et al., 2005). The THF solvent was apparently able to stabilize the otherwise reactive organozinc in order to form good films. In an attempt to use t-butanol as a solvent for zinc oxide thin film deposition with diethyl zinc, we found that large needles of the partially alcoholyzed zinc title compound, (I), crystallized out after a few minutes.
In the structure of (I) (Fig 1) each Zn atom carries an ethyl substituent and binds to three t-butoxo O atoms. The resulting tetrameric unit is a distorted cube with the Zn and O atoms in distorted tetrahedral arrangements and Zn—O distances in the range 2.084 (4)Å to 2.055 (4)Å [mean 2.073 (6) Å]. This compares with a mean value of 2.07 (2)Å for the 11 other cubic tetrakis(µ3-alkyloxo)tetra-alkyl-tetrazinc complexes reported previously (Bond et al., 2001; Herman et al., 1992; Polarz et al., 2005 and Shearer & Spencer, 1980; Boyle et al., 2004). In the crystal structure of (I) there are no significant close contacts with the shortest intermolecular C62···H32Di (i = x, y - 1, z) distance being 3.02 Å.