Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806021210/sj2075sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806021210/sj2075Isup2.hkl |
CCDC reference: 613817
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.035
- wR factor = 0.093
- Data-to-parameter ratio = 12.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact N3 .. O9 .. 2.81 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.72 mm PLAT221_ALERT_4_C Large Solvent/Anion O Ueq(max)/Ueq(min) ... 3.19 Ratio PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C28 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C29 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.26 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 21.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact O5 .. C9 .. 2.97 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C15 .. F8 .. 2.94 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.60 Deg. O9 -S1 -O6 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.20 Deg. O5 -S1 -O8 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 35.10 Deg. C31 -S1 -C28 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.40 Deg. C28 -F3 -C31 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 34.00 Deg. F3 -C28 -F8 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 41.10 Deg. C31 -F8 -C28 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 32.30 Deg. F8 -C31 -F3 1.555 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C27 H27 N3 O4 Zn PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C F3 O3 S PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C F3 O3 S PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C H2 Cl2
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.85 From the CIF: _reflns_number_total 6882 Count of symmetry unique reflns 3905 Completeness (_total/calc) 176.24% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2977 Fraction of Friedel pairs measured 0.762 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 24 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 13 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SIR97 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Mercury (version 1.4; Macrae et al., 2006); software used to prepare material for publication: SHELXL97.
[Zn(C27H27N3O4)](CF3O3S)2·CH2Cl2 | Cell parameters were determined by indexing 7997 reflections with I/sigma limit 6.0. |
Mr = 905.99 | Dx = 1.683 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 7997 reflections |
a = 8.7347 (6) Å | θ = 2.5–25.9° |
b = 15.2145 (10) Å | µ = 1.04 mm−1 |
c = 26.9055 (19) Å | T = 173 K |
V = 3575.6 (4) Å3 | Rectangular plate, colourless |
Z = 4 | 0.72 × 0.24 × 0.18 mm |
F(000) = 1840 |
Stoe IPDS diffractometer | 6882 independent reflections |
Radiation source: fine-focus sealed tube | 6405 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
rotation scans | θmax = 25.9°, θmin = 2.5° |
Absorption correction: numerical [FACEIT in X-RED (Stoe & Cie, 1996)] | h = −10→10 |
Tmin = 0.592, Tmax = 0.816 | k = −18→18 |
30057 measured reflections | l = −32→32 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters constrained |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0601P)2 + 1.1443P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
6882 reflections | Δρmax = 0.60 e Å−3 |
533 parameters | Δρmin = −0.35 e Å−3 |
0 restraints | Absolute structure: Flack (1983), with 3002 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.001 (10) |
Experimental. Data were collected applying an imaging plate system (Stoe) with the following measurement parameters: Detector distance [mm] 70 Phi movement mode Oscillation Phi incr. [degrees] 0.8 Number of exposures 270 Irradiation / exposure [min] 2.00 For a detailed description of the method see: Sheldrick, G. M., Paulus, E., Vertesy, L. & Hahn, F. (1995). Acta Cryst. B51, 89–98. |
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) | |
Zn1 | −0.68881 (4) | −0.48377 (2) | −0.107272 (11) | 0.03480 (9) | |
O1 | −0.6621 (2) | −0.49245 (14) | −0.02381 (7) | 0.0382 (4) | |
O2 | −1.0055 (3) | −0.28828 (15) | −0.07237 (8) | 0.0456 (5) | |
O3 | −0.7633 (3) | −0.53720 (16) | −0.18148 (8) | 0.0445 (5) | |
O4 | −0.2548 (3) | −0.5435 (2) | −0.15954 (10) | 0.0610 (7) | |
N1 | −0.7805 (3) | −0.60277 (17) | −0.09017 (9) | 0.0367 (5) | |
N2 | −0.8184 (3) | −0.38360 (16) | −0.08697 (8) | 0.0346 (5) | |
N3 | −0.4872 (3) | −0.49401 (19) | −0.13949 (9) | 0.0421 (6) | |
C1 | −0.7570 (4) | −0.6372 (2) | −0.04500 (12) | 0.0391 (6) | |
C2 | −0.8127 (5) | −0.7201 (2) | −0.03300 (13) | 0.0518 (8) | |
H2 | −0.7983 | −0.7431 | −0.0013 | 0.062* | |
C3 | −0.8894 (5) | −0.7674 (2) | −0.06858 (16) | 0.0609 (10) | |
H3 | −0.9255 | −0.8235 | −0.0614 | 0.073* | |
C4 | −0.9129 (4) | −0.7316 (3) | −0.11508 (15) | 0.0548 (9) | |
H4 | −0.9653 | −0.7629 | −0.1394 | 0.066* | |
C5 | −0.8575 (3) | −0.6485 (2) | −0.12495 (13) | 0.0424 (7) | |
C6 | −0.6613 (4) | −0.5834 (2) | −0.01007 (11) | 0.0428 (7) | |
H6A | −0.7007 | −0.5895 | 0.0235 | 0.051* | |
H6B | −0.5569 | −0.6051 | −0.0104 | 0.051* | |
C7 | −0.7898 (4) | −0.4439 (2) | −0.00374 (10) | 0.0407 (6) | |
H7A | −0.7730 | −0.4307 | 0.0311 | 0.049* | |
H7B | −0.8836 | −0.4776 | −0.0068 | 0.049* | |
C8 | −0.7997 (4) | −0.3604 (2) | −0.03373 (10) | 0.0386 (6) | |
H8 | −0.7067 | −0.3253 | −0.0291 | 0.046* | |
C9 | −0.9422 (4) | −0.3039 (2) | −0.02341 (12) | 0.0482 (8) | |
H9A | −1.0146 | −0.3351 | −0.0025 | 0.058* | |
H9B | −0.9145 | −0.2491 | −0.0074 | 0.058* | |
C10 | −0.9311 (3) | −0.33929 (19) | −0.10471 (12) | 0.0373 (6) | |
C11 | −0.9880 (4) | −0.3390 (2) | −0.15587 (12) | 0.0397 (6) | |
C12 | −0.8892 (4) | −0.3506 (2) | −0.19581 (12) | 0.0423 (7) | |
H12 | −0.7848 | −0.3576 | −0.1903 | 0.051* | |
C13 | −0.9461 (4) | −0.3518 (3) | −0.24373 (13) | 0.0520 (8) | |
H13 | −0.8805 | −0.3597 | −0.2706 | 0.062* | |
C14 | −1.1026 (5) | −0.3411 (3) | −0.25139 (14) | 0.0575 (9) | |
H14 | −1.1418 | −0.3432 | −0.2835 | 0.069* | |
C15 | −1.2000 (4) | −0.3274 (3) | −0.21192 (14) | 0.0590 (9) | |
H15 | −1.3040 | −0.3191 | −0.2177 | 0.071* | |
C16 | −1.1446 (4) | −0.3259 (2) | −0.16400 (13) | 0.0474 (8) | |
H16 | −1.2104 | −0.3163 | −0.1374 | 0.057* | |
C17 | −0.8807 (4) | −0.6006 (3) | −0.17348 (13) | 0.0498 (8) | |
H17A | −0.8807 | −0.6426 | −0.2006 | 0.060* | |
H17B | −0.9795 | −0.5714 | −0.1731 | 0.060* | |
C18 | −0.6260 (4) | −0.5753 (3) | −0.20282 (12) | 0.0531 (9) | |
H18A | −0.6397 | −0.5853 | −0.2381 | 0.064* | |
H18B | −0.6029 | −0.6311 | −0.1870 | 0.064* | |
C19 | −0.4976 (4) | −0.5104 (3) | −0.19401 (11) | 0.0556 (9) | |
H19 | −0.5153 | −0.4556 | −0.2123 | 0.067* | |
C20 | −0.3396 (4) | −0.5492 (4) | −0.20629 (14) | 0.0681 (11) | |
H20A | −0.3486 | −0.6098 | −0.2171 | 0.082* | |
H20B | −0.2894 | −0.5154 | −0.2322 | 0.082* | |
C21 | −0.3517 (3) | −0.5152 (2) | −0.12493 (12) | 0.0434 (7) | |
C22 | −0.2933 (3) | −0.5115 (2) | −0.07367 (11) | 0.0405 (6) | |
C23 | −0.3340 (4) | −0.4422 (2) | −0.04257 (12) | 0.0435 (7) | |
H23 | −0.3931 | −0.3960 | −0.0546 | 0.052* | |
C24 | −0.2854 (4) | −0.4428 (2) | 0.00630 (13) | 0.0492 (8) | |
H24 | −0.3122 | −0.3967 | 0.0273 | 0.059* | |
C25 | −0.1976 (4) | −0.5110 (2) | 0.02418 (12) | 0.0490 (7) | |
H25 | −0.1668 | −0.5112 | 0.0573 | 0.059* | |
C26 | −0.1551 (4) | −0.5794 (2) | −0.00709 (14) | 0.0486 (8) | |
H26 | −0.0950 | −0.6251 | 0.0051 | 0.058* | |
C27 | −0.2014 (4) | −0.5799 (2) | −0.05600 (13) | 0.0463 (7) | |
H27 | −0.1720 | −0.6253 | −0.0771 | 0.056* | |
S1 | −0.53928 (10) | −0.21992 (5) | −0.11801 (3) | 0.0494 (2) | |
F1 | −0.5727 (3) | −0.0866 (2) | −0.17971 (11) | 0.0818 (8) | |
F2 | −0.4571 (4) | −0.05580 (19) | −0.11350 (12) | 0.0652 (9) | 0.760 (6) |
F3 | −0.3421 (4) | −0.1293 (3) | −0.17057 (15) | 0.0620 (10) | 0.760 (6) |
O5 | −0.4214 (7) | −0.2387 (4) | −0.08407 (18) | 0.0820 (19) | 0.760 (6) |
O6 | −0.5490 (5) | −0.2799 (3) | −0.1602 (2) | 0.0745 (15) | 0.760 (6) |
O7 | −0.6846 (3) | −0.19502 (16) | −0.09692 (11) | 0.0643 (7) | |
C28 | −0.4758 (5) | −0.1181 (4) | −0.14763 (17) | 0.0472 (11) | 0.760 (6) |
F7 | −0.617 (2) | −0.1990 (13) | −0.2058 (6) | 0.126 (7) | 0.240 (6) |
F8 | −0.3841 (19) | −0.1691 (12) | −0.1920 (6) | 0.091 (5) | 0.240 (6) |
C31 | −0.528 (3) | −0.1628 (14) | −0.1738 (8) | 0.079 (7) | 0.240 (6) |
S2 | −0.38322 (11) | −0.78061 (8) | −0.12088 (4) | 0.0670 (3) | |
F4 | −0.5329 (7) | −0.7968 (3) | −0.20303 (15) | 0.163 (2) | |
F5 | −0.6098 (4) | −0.8776 (3) | −0.1474 (2) | 0.150 (2) | |
F6 | −0.4025 (4) | −0.90989 (19) | −0.18426 (10) | 0.0804 (8) | |
O10 | −0.3513 (11) | −0.8364 (4) | −0.08423 (17) | 0.222 (5) | |
O11 | −0.2518 (5) | −0.7563 (5) | −0.1488 (3) | 0.192 (4) | |
O12 | −0.4786 (3) | −0.7078 (2) | −0.11082 (13) | 0.0695 (8) | |
C29 | −0.4826 (6) | −0.8430 (3) | −0.16651 (18) | 0.0706 (11) | |
Cl1 | −0.97777 (15) | −0.09529 (9) | −0.20480 (4) | 0.0767 (3) | |
Cl2 | −1.05442 (17) | 0.01539 (8) | −0.12060 (5) | 0.0830 (3) | |
C30 | −0.9904 (7) | −0.0879 (3) | −0.14030 (16) | 0.0762 (13) | |
H30A | −0.8905 | −0.0993 | −0.1260 | 0.091* | |
H30B | −1.0602 | −0.1326 | −0.1282 | 0.091* | |
O9 | −0.5163 (14) | −0.3111 (7) | −0.1291 (7) | 0.061 (3) | 0.240 (6) |
O8 | −0.4090 (18) | −0.1888 (13) | −0.0883 (5) | 0.072 (5) | 0.240 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.03172 (15) | 0.04608 (16) | 0.02660 (14) | 0.00491 (14) | 0.00110 (13) | 0.00149 (13) |
O1 | 0.0365 (10) | 0.0481 (11) | 0.0301 (9) | −0.0032 (9) | 0.0000 (8) | 0.0038 (8) |
O2 | 0.0465 (12) | 0.0469 (11) | 0.0433 (12) | 0.0073 (10) | 0.0105 (10) | −0.0031 (9) |
O3 | 0.0398 (11) | 0.0632 (14) | 0.0305 (10) | 0.0130 (10) | −0.0030 (9) | −0.0009 (9) |
O4 | 0.0375 (11) | 0.102 (2) | 0.0432 (13) | 0.0114 (13) | 0.0101 (10) | 0.0017 (13) |
N1 | 0.0291 (12) | 0.0471 (13) | 0.0340 (12) | 0.0042 (10) | 0.0016 (9) | −0.0011 (10) |
N2 | 0.0328 (11) | 0.0429 (12) | 0.0282 (10) | −0.0014 (11) | 0.0055 (10) | −0.0006 (9) |
N3 | 0.0357 (12) | 0.0594 (16) | 0.0312 (12) | 0.0042 (11) | 0.0046 (10) | 0.0038 (11) |
C1 | 0.0368 (14) | 0.0424 (15) | 0.0382 (16) | 0.0078 (12) | 0.0074 (12) | 0.0033 (12) |
C2 | 0.062 (2) | 0.0480 (17) | 0.0457 (17) | 0.0030 (17) | 0.0171 (18) | 0.0015 (13) |
C3 | 0.069 (2) | 0.0478 (19) | 0.066 (2) | −0.0142 (18) | 0.028 (2) | −0.0110 (17) |
C4 | 0.0418 (17) | 0.065 (2) | 0.057 (2) | −0.0104 (15) | 0.0111 (16) | −0.0235 (17) |
C5 | 0.0304 (14) | 0.0509 (17) | 0.0458 (16) | 0.0043 (12) | 0.0049 (12) | −0.0110 (14) |
C6 | 0.0412 (17) | 0.0527 (17) | 0.0345 (15) | 0.0019 (13) | −0.0053 (13) | 0.0107 (12) |
C7 | 0.0395 (16) | 0.0559 (17) | 0.0268 (13) | −0.0041 (14) | 0.0043 (12) | −0.0017 (12) |
C8 | 0.0419 (16) | 0.0464 (15) | 0.0276 (13) | −0.0064 (13) | 0.0039 (13) | −0.0066 (11) |
C9 | 0.0523 (19) | 0.0524 (18) | 0.0399 (16) | −0.0040 (15) | 0.0093 (15) | −0.0083 (14) |
C10 | 0.0324 (13) | 0.0395 (13) | 0.0400 (14) | 0.0013 (11) | 0.0082 (13) | 0.0004 (13) |
C11 | 0.0381 (15) | 0.0417 (15) | 0.0391 (15) | 0.0066 (12) | 0.0056 (13) | 0.0076 (12) |
C12 | 0.0387 (16) | 0.0507 (17) | 0.0377 (16) | 0.0082 (14) | 0.0050 (13) | 0.0066 (13) |
C13 | 0.0492 (19) | 0.066 (2) | 0.0408 (17) | 0.0086 (16) | 0.0058 (15) | 0.0091 (15) |
C14 | 0.055 (2) | 0.079 (2) | 0.0384 (17) | 0.0040 (19) | −0.0044 (15) | 0.0122 (17) |
C15 | 0.0402 (17) | 0.083 (3) | 0.054 (2) | 0.0045 (18) | −0.0049 (17) | 0.0128 (18) |
C16 | 0.0393 (16) | 0.061 (2) | 0.0416 (17) | 0.0092 (14) | 0.0043 (13) | 0.0069 (14) |
C17 | 0.0408 (17) | 0.069 (2) | 0.0396 (17) | 0.0083 (16) | −0.0082 (14) | −0.0126 (15) |
C18 | 0.0440 (17) | 0.087 (3) | 0.0286 (15) | 0.0178 (17) | 0.0034 (13) | −0.0088 (16) |
C19 | 0.0478 (17) | 0.091 (3) | 0.0284 (14) | 0.0115 (19) | 0.0071 (13) | 0.0057 (16) |
C20 | 0.044 (2) | 0.121 (3) | 0.0393 (17) | 0.008 (2) | 0.0126 (16) | 0.002 (2) |
C21 | 0.0335 (14) | 0.0573 (17) | 0.0395 (15) | 0.0009 (13) | 0.0069 (12) | 0.0026 (14) |
C22 | 0.0279 (13) | 0.0497 (15) | 0.0438 (15) | −0.0021 (13) | 0.0038 (11) | 0.0045 (13) |
C23 | 0.0356 (16) | 0.0457 (16) | 0.0493 (17) | 0.0003 (13) | −0.0018 (13) | 0.0047 (13) |
C24 | 0.0441 (19) | 0.0532 (18) | 0.0502 (18) | −0.0065 (15) | −0.0038 (15) | −0.0031 (14) |
C25 | 0.0410 (15) | 0.0601 (18) | 0.0460 (16) | −0.0032 (16) | −0.0098 (14) | 0.0080 (14) |
C26 | 0.0331 (16) | 0.0516 (17) | 0.061 (2) | −0.0001 (13) | −0.0095 (14) | 0.0131 (15) |
C27 | 0.0314 (14) | 0.0500 (16) | 0.0575 (19) | 0.0013 (13) | 0.0016 (15) | 0.0020 (14) |
S1 | 0.0530 (5) | 0.0448 (4) | 0.0503 (5) | 0.0022 (3) | 0.0212 (4) | 0.0045 (3) |
F1 | 0.0768 (17) | 0.0924 (19) | 0.0763 (17) | 0.0049 (15) | −0.0129 (14) | 0.0372 (15) |
F2 | 0.0703 (19) | 0.0574 (16) | 0.0679 (19) | −0.0108 (14) | 0.0101 (16) | −0.0100 (14) |
F3 | 0.0476 (18) | 0.083 (2) | 0.056 (2) | −0.0092 (15) | 0.0202 (15) | 0.0042 (17) |
O5 | 0.107 (4) | 0.091 (4) | 0.048 (2) | 0.057 (3) | 0.018 (2) | 0.030 (3) |
O6 | 0.063 (3) | 0.067 (3) | 0.094 (3) | −0.013 (2) | 0.034 (3) | −0.031 (3) |
O7 | 0.0637 (15) | 0.0479 (12) | 0.0814 (19) | −0.0003 (12) | 0.0417 (16) | 0.0012 (12) |
C28 | 0.040 (2) | 0.071 (3) | 0.031 (2) | 0.001 (2) | 0.0062 (18) | 0.005 (2) |
F7 | 0.147 (15) | 0.156 (14) | 0.075 (8) | −0.008 (11) | −0.054 (10) | 0.030 (9) |
F8 | 0.090 (10) | 0.107 (12) | 0.075 (10) | 0.026 (9) | 0.039 (8) | 0.058 (9) |
C31 | 0.110 (18) | 0.071 (12) | 0.055 (11) | 0.022 (12) | 0.041 (13) | 0.018 (10) |
S2 | 0.0494 (5) | 0.0916 (7) | 0.0600 (6) | 0.0250 (5) | −0.0214 (4) | −0.0318 (5) |
F4 | 0.281 (7) | 0.094 (2) | 0.113 (3) | 0.002 (3) | −0.128 (4) | −0.001 (2) |
F5 | 0.070 (2) | 0.093 (2) | 0.288 (7) | −0.0142 (18) | 0.022 (3) | −0.021 (3) |
F6 | 0.095 (2) | 0.0757 (16) | 0.0705 (16) | −0.0132 (15) | 0.0114 (15) | −0.0217 (13) |
O10 | 0.408 (12) | 0.182 (5) | 0.076 (3) | 0.196 (7) | −0.121 (5) | −0.057 (3) |
O11 | 0.061 (2) | 0.219 (6) | 0.297 (9) | −0.055 (3) | 0.060 (4) | −0.182 (7) |
O12 | 0.0565 (15) | 0.0716 (17) | 0.0804 (19) | 0.0175 (13) | 0.0008 (16) | −0.0126 (16) |
C29 | 0.072 (3) | 0.071 (3) | 0.069 (3) | −0.005 (2) | −0.016 (2) | 0.009 (2) |
Cl1 | 0.0806 (7) | 0.1009 (8) | 0.0485 (5) | −0.0053 (6) | 0.0099 (5) | −0.0128 (5) |
Cl2 | 0.1009 (8) | 0.0733 (6) | 0.0749 (7) | 0.0047 (6) | 0.0083 (6) | −0.0220 (6) |
C30 | 0.094 (3) | 0.085 (3) | 0.049 (2) | 0.036 (3) | 0.005 (2) | 0.008 (2) |
O9 | 0.047 (6) | 0.042 (6) | 0.094 (10) | 0.006 (4) | 0.013 (6) | 0.011 (6) |
O8 | 0.067 (8) | 0.109 (13) | 0.039 (6) | −0.023 (9) | −0.028 (6) | 0.000 (8) |
Zn1—N3 | 1.969 (2) | C18—C19 | 1.513 (6) |
Zn1—N2 | 1.976 (2) | C18—H18A | 0.9700 |
Zn1—N1 | 2.033 (3) | C18—H18B | 0.9700 |
Zn1—O3 | 2.252 (2) | C19—C20 | 1.538 (5) |
Zn1—O1 | 2.2614 (19) | C19—H19 | 0.9800 |
O1—C6 | 1.432 (4) | C20—H20A | 0.9700 |
O1—C7 | 1.443 (4) | C20—H20B | 0.9700 |
O2—C10 | 1.335 (4) | C21—C22 | 1.471 (4) |
O2—C9 | 1.448 (4) | C22—C23 | 1.392 (5) |
O3—C17 | 1.424 (5) | C22—C27 | 1.398 (5) |
O3—C18 | 1.451 (4) | C23—C24 | 1.382 (5) |
O4—C21 | 1.330 (4) | C23—H23 | 0.9300 |
O4—C20 | 1.462 (5) | C24—C25 | 1.377 (5) |
N1—C1 | 1.339 (4) | C24—H24 | 0.9300 |
N1—C5 | 1.346 (4) | C25—C26 | 1.389 (5) |
N2—C10 | 1.285 (4) | C25—H25 | 0.9300 |
N2—C8 | 1.484 (3) | C26—C27 | 1.377 (5) |
N3—C21 | 1.288 (4) | C26—H26 | 0.9300 |
N3—C19 | 1.491 (4) | C27—H27 | 0.9300 |
C1—C2 | 1.390 (5) | S1—O5 | 1.406 (6) |
C1—C6 | 1.501 (5) | S1—O9 | 1.432 (11) |
C2—C3 | 1.373 (6) | S1—O7 | 1.441 (3) |
C2—H2 | 0.9300 | S1—O6 | 1.459 (4) |
C3—C4 | 1.380 (6) | S1—O8 | 1.470 (12) |
C3—H3 | 0.9300 | S1—C31 | 1.738 (18) |
C4—C5 | 1.380 (5) | S1—C28 | 1.829 (5) |
C4—H4 | 0.9300 | F1—C31 | 1.23 (2) |
C5—C17 | 1.509 (5) | F1—C28 | 1.300 (5) |
C6—H6A | 0.9700 | F2—C28 | 1.329 (6) |
C6—H6B | 0.9700 | F3—F8 | 0.91 (2) |
C7—C8 | 1.508 (4) | F3—C28 | 1.332 (6) |
C7—H7A | 0.9700 | F3—C31 | 1.70 (3) |
C7—H7B | 0.9700 | O5—O8 | 0.775 (17) |
C8—C9 | 1.538 (5) | O6—O9 | 1.003 (14) |
C8—H8 | 0.9800 | O6—C31 | 1.83 (2) |
C9—H9A | 0.9700 | C28—C31 | 1.08 (3) |
C9—H9B | 0.9700 | C28—F8 | 1.634 (17) |
C10—C11 | 1.464 (5) | F7—C31 | 1.29 (3) |
C11—C12 | 1.390 (4) | F8—C31 | 1.35 (3) |
C11—C16 | 1.399 (5) | S2—O10 | 1.330 (5) |
C12—C13 | 1.382 (5) | S2—O12 | 1.413 (3) |
C12—H12 | 0.9300 | S2—O11 | 1.421 (5) |
C13—C14 | 1.392 (5) | S2—C29 | 1.778 (5) |
C13—H13 | 0.9300 | F4—C29 | 1.285 (6) |
C14—C15 | 1.377 (6) | F5—C29 | 1.332 (6) |
C14—H14 | 0.9300 | F6—C29 | 1.324 (6) |
C15—C16 | 1.378 (5) | Cl1—C30 | 1.742 (4) |
C15—H15 | 0.9300 | Cl2—C30 | 1.750 (5) |
C16—H16 | 0.9300 | C30—H30A | 0.9700 |
C17—H17A | 0.9700 | C30—H30B | 0.9700 |
C17—H17B | 0.9700 | ||
N3—Zn1—N2 | 134.06 (11) | H20A—C20—H20B | 108.9 |
N3—Zn1—N1 | 112.42 (11) | N3—C21—O4 | 116.9 (3) |
N2—Zn1—N1 | 113.50 (10) | N3—C21—C22 | 126.4 (3) |
N3—Zn1—O3 | 80.76 (9) | O4—C21—C22 | 116.6 (3) |
N2—Zn1—O3 | 110.98 (9) | C23—C22—C27 | 120.4 (3) |
N1—Zn1—O3 | 76.43 (9) | C23—C22—C21 | 120.3 (3) |
N3—Zn1—O1 | 109.89 (9) | C27—C22—C21 | 119.2 (3) |
N2—Zn1—O1 | 80.19 (9) | C24—C23—C22 | 119.3 (3) |
N1—Zn1—O1 | 76.34 (9) | C24—C23—H23 | 120.4 |
O3—Zn1—O1 | 152.77 (8) | C22—C23—H23 | 120.4 |
C6—O1—C7 | 113.7 (2) | C25—C24—C23 | 120.6 (3) |
C6—O1—Zn1 | 108.26 (17) | C25—C24—H24 | 119.7 |
C7—O1—Zn1 | 105.18 (15) | C23—C24—H24 | 119.7 |
C10—O2—C9 | 108.2 (2) | C24—C25—C26 | 120.1 (3) |
C17—O3—C18 | 112.6 (3) | C24—C25—H25 | 119.9 |
C17—O3—Zn1 | 108.57 (18) | C26—C25—H25 | 119.9 |
C18—O3—Zn1 | 104.86 (18) | C27—C26—C25 | 120.3 (3) |
C21—O4—C20 | 107.4 (3) | C27—C26—H26 | 119.9 |
C1—N1—C5 | 120.4 (3) | C25—C26—H26 | 119.9 |
C1—N1—Zn1 | 119.6 (2) | C26—C27—C22 | 119.3 (3) |
C5—N1—Zn1 | 120.0 (2) | C26—C27—H27 | 120.3 |
C10—N2—C8 | 108.5 (3) | C22—C27—H27 | 120.3 |
C10—N2—Zn1 | 137.8 (2) | O5—S1—O9 | 80.6 (7) |
C8—N2—Zn1 | 112.79 (19) | O5—S1—O7 | 116.3 (2) |
C21—N3—C19 | 108.3 (3) | O9—S1—O7 | 117.4 (5) |
C21—N3—Zn1 | 135.1 (2) | O5—S1—O6 | 114.9 (3) |
C19—N3—Zn1 | 113.1 (2) | O9—S1—O6 | 40.6 (6) |
N1—C1—C2 | 120.8 (3) | O7—S1—O6 | 114.8 (2) |
N1—C1—C6 | 116.1 (3) | O5—S1—O8 | 31.2 (7) |
C2—C1—C6 | 123.0 (3) | O9—S1—O8 | 108.5 (10) |
C3—C2—C1 | 119.0 (3) | O7—S1—O8 | 112.5 (7) |
C3—C2—H2 | 120.5 | O6—S1—O8 | 132.1 (8) |
C1—C2—H2 | 120.5 | O5—S1—C31 | 128.3 (10) |
C2—C3—C4 | 119.8 (3) | O9—S1—C31 | 107.2 (10) |
C2—C3—H3 | 120.1 | O7—S1—C31 | 105.0 (7) |
C4—C3—H3 | 120.1 | O6—S1—C31 | 69.2 (9) |
C5—C4—C3 | 119.0 (3) | O8—S1—C31 | 105.3 (12) |
C5—C4—H4 | 120.5 | O5—S1—C28 | 103.5 (3) |
C3—C4—H4 | 120.5 | O9—S1—C28 | 133.4 (6) |
N1—C5—C4 | 121.0 (3) | O7—S1—C28 | 102.46 (18) |
N1—C5—C17 | 114.8 (3) | O6—S1—C28 | 102.1 (3) |
C4—C5—C17 | 124.2 (3) | O8—S1—C28 | 74.3 (7) |
O1—C6—C1 | 111.3 (2) | C31—S1—C28 | 35.1 (10) |
O1—C6—H6A | 109.4 | C31—F1—C28 | 50.4 (14) |
C1—C6—H6A | 109.4 | F8—F3—C28 | 91.4 (10) |
O1—C6—H6B | 109.4 | F8—F3—C31 | 52.1 (11) |
C1—C6—H6B | 109.4 | C28—F3—C31 | 39.4 (7) |
H6A—C6—H6B | 108.0 | O8—O5—S1 | 79.0 (11) |
O1—C7—C8 | 106.0 (2) | O9—O6—S1 | 68.3 (8) |
O1—C7—H7A | 110.5 | O9—O6—C31 | 126.8 (12) |
C8—C7—H7A | 110.5 | S1—O6—C31 | 62.6 (7) |
O1—C7—H7B | 110.5 | C31—C28—F1 | 61.6 (11) |
C8—C7—H7B | 110.5 | C31—C28—F2 | 162.1 (13) |
H7A—C7—H7B | 108.7 | F1—C28—F2 | 106.0 (4) |
N2—C8—C7 | 108.8 (2) | C31—C28—F3 | 89.2 (12) |
N2—C8—C9 | 102.6 (3) | F1—C28—F3 | 108.1 (4) |
C7—C8—C9 | 114.9 (3) | F2—C28—F3 | 107.7 (4) |
N2—C8—H8 | 110.1 | C31—C28—F8 | 55.2 (14) |
C7—C8—H8 | 110.1 | F1—C28—F8 | 90.5 (6) |
C9—C8—H8 | 110.1 | F2—C28—F8 | 141.6 (8) |
O2—C9—C8 | 103.7 (2) | F3—C28—F8 | 34.0 (7) |
O2—C9—H9A | 111.0 | C31—C28—S1 | 67.8 (10) |
C8—C9—H9A | 111.0 | F1—C28—S1 | 113.8 (4) |
O2—C9—H9B | 111.0 | F2—C28—S1 | 109.9 (3) |
C8—C9—H9B | 111.0 | F3—C28—S1 | 111.0 (4) |
H9A—C9—H9B | 109.0 | F8—C28—S1 | 93.7 (6) |
N2—C10—O2 | 115.8 (3) | F3—F8—C31 | 95.6 (17) |
N2—C10—C11 | 127.7 (3) | F3—F8—C28 | 54.6 (9) |
O2—C10—C11 | 116.5 (3) | C31—F8—C28 | 41.1 (13) |
C12—C11—C16 | 120.3 (3) | C28—C31—F1 | 68.0 (13) |
C12—C11—C10 | 121.1 (3) | C28—C31—F7 | 164 (2) |
C16—C11—C10 | 118.7 (3) | F1—C31—F7 | 97 (2) |
C13—C12—C11 | 120.0 (3) | C28—C31—F8 | 84 (2) |
C13—C12—H12 | 120.0 | F1—C31—F8 | 108.4 (17) |
C11—C12—H12 | 120.0 | F7—C31—F8 | 106.9 (19) |
C12—C13—C14 | 119.3 (3) | C28—C31—F3 | 51.5 (13) |
C12—C13—H13 | 120.3 | F1—C31—F3 | 91.6 (16) |
C14—C13—H13 | 120.3 | F7—C31—F3 | 137.8 (16) |
C15—C14—C13 | 120.7 (3) | F8—C31—F3 | 32.3 (11) |
C15—C14—H14 | 119.6 | C28—C31—S1 | 77.0 (13) |
C13—C14—H14 | 119.6 | F1—C31—S1 | 124.2 (14) |
C14—C15—C16 | 120.5 (3) | F7—C31—S1 | 109.2 (17) |
C14—C15—H15 | 119.8 | F8—C31—S1 | 109.4 (16) |
C16—C15—H15 | 119.8 | F3—C31—S1 | 99.2 (14) |
C15—C16—C11 | 119.2 (3) | C28—C31—O6 | 121.7 (16) |
C15—C16—H16 | 120.4 | F1—C31—O6 | 155 (2) |
C11—C16—H16 | 120.4 | F7—C31—O6 | 69.8 (14) |
O3—C17—C5 | 111.2 (3) | F8—C31—O6 | 95.6 (13) |
O3—C17—H17A | 109.4 | F3—C31—O6 | 112.2 (12) |
C5—C17—H17A | 109.4 | S1—C31—O6 | 48.2 (5) |
O3—C17—H17B | 109.4 | O10—S2—O12 | 118.8 (3) |
C5—C17—H17B | 109.4 | O10—S2—O11 | 112.9 (5) |
H17A—C17—H17B | 108.0 | O12—S2—O11 | 111.9 (3) |
O3—C18—C19 | 106.8 (3) | O10—S2—C29 | 105.9 (4) |
O3—C18—H18A | 110.4 | O12—S2—C29 | 105.2 (2) |
C19—C18—H18A | 110.4 | O11—S2—C29 | 99.7 (3) |
O3—C18—H18B | 110.4 | F4—C29—F6 | 109.0 (5) |
C19—C18—H18B | 110.4 | F4—C29—F5 | 103.1 (5) |
H18A—C18—H18B | 108.6 | F6—C29—F5 | 106.0 (4) |
N3—C19—C18 | 108.0 (3) | F4—C29—S2 | 113.8 (3) |
N3—C19—C20 | 102.8 (3) | F6—C29—S2 | 113.7 (3) |
C18—C19—C20 | 112.4 (4) | F5—C29—S2 | 110.6 (4) |
N3—C19—H19 | 111.1 | Cl1—C30—Cl2 | 112.3 (3) |
C18—C19—H19 | 111.1 | Cl1—C30—H30A | 109.1 |
C20—C19—H19 | 111.1 | Cl2—C30—H30A | 109.1 |
O4—C20—C19 | 104.3 (3) | Cl1—C30—H30B | 109.1 |
O4—C20—H20A | 110.9 | Cl2—C30—H30B | 109.1 |
C19—C20—H20A | 110.9 | H30A—C30—H30B | 107.9 |
O4—C20—H20B | 110.9 | O6—O9—S1 | 71.1 (7) |
C19—C20—H20B | 110.9 | O5—O8—S1 | 69.9 (11) |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register