Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804008591/cv6295sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804008591/cv6295Isup2.hkl |
CCDC reference: 239057
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.043
- wR factor = 0.112
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 27.00 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 8203 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 8808 Completeness (_total/calc) 93.13% SHFSU01_ALERT_2_C The absolute value of parameter shift to su ratio > 0.05 Absolute value of the parameter shift to su ratio given 0.094 Additional refinement cycles may be required. PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.93 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT080_ALERT_2_C Maximum Shift/Error ............................ 0.09 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.62 Ratio PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... S53 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact C42 .. Cl58 .. 3.23 Ang.
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1999); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SIR97 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and Mercury (Bruno et al., 2002); software used to prepare material for publication: SHELXL97.
[Zn(C44H28N4)]·1.79C2H6OS·0.21CHCl3 | Z = 2 |
Mr = 842.99 | F(000) = 875 |
Triclinic, P1 | Dx = 1.387 Mg m−3 |
a = 10.9118 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.0998 (2) Å | Cell parameters from 6359 reflections |
c = 17.4255 (4) Å | θ = 2.2–27.0° |
α = 87.9607 (9)° | µ = 0.79 mm−1 |
β = 81.5984 (9)° | T = 110 K |
γ = 75.2901 (10)° | Rod, red |
V = 2019.60 (8) Å3 | 0.30 × 0.15 × 0.15 mm |
Nonius KappaCCD diffractometer | 8203 independent reflections |
Radiation source: fine-focus sealed tube | 6359 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
Detector resolution: 56 microns pixels mm-1 | θmax = 27.0°, θmin = 2.2° |
1° φ and ω scans | h = −12→13 |
Absorption correction: multi-scan (Blessing, 1995) | k = −13→14 |
Tmin = 0.798, Tmax = 0.891 | l = −22→22 |
16161 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full with fixed elements per cycle | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0562P)2 + 0.8349P] where P = (Fo2 + 2Fc2)/3 |
8203 reflections | (Δ/σ)max = 0.094 |
555 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.59 e Å−3 |
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 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains a 79:21% mixture of DMSO and chloroform as crystallization solvent. Due to technical problems with the instrument, only 93% of all data could be collected out to 2*theta=54 deg., and 96% of all data to 2*theta=50 deg. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn | 0.13460 (2) | 0.20473 (2) | 0.227315 (16) | 0.01888 (9) | |
C1 | −0.0100 (2) | 0.0215 (2) | 0.31276 (14) | 0.0201 (5) | |
C2 | −0.1330 (2) | 0.0166 (2) | 0.35424 (14) | 0.0225 (5) | |
H2 | −0.1531 | −0.0520 | 0.3828 | 0.027* | |
C3 | −0.2144 (2) | 0.1288 (2) | 0.34454 (15) | 0.0231 (5) | |
H3 | −0.3027 | 0.1533 | 0.3648 | 0.028* | |
C4 | −0.1424 (2) | 0.2042 (2) | 0.29775 (14) | 0.0196 (5) | |
C5 | −0.1934 (2) | 0.3254 (2) | 0.27172 (14) | 0.0198 (5) | |
C6 | −0.1241 (2) | 0.3980 (2) | 0.22436 (14) | 0.0198 (5) | |
C7 | −0.1763 (2) | 0.5238 (2) | 0.19919 (14) | 0.0228 (5) | |
H7 | −0.2629 | 0.5704 | 0.2102 | 0.027* | |
C8 | −0.0799 (2) | 0.5627 (2) | 0.15726 (15) | 0.0232 (5) | |
H8 | −0.0855 | 0.6420 | 0.1336 | 0.028* | |
C9 | 0.0340 (2) | 0.4609 (2) | 0.15492 (14) | 0.0197 (5) | |
C10 | 0.1548 (2) | 0.4642 (2) | 0.11569 (14) | 0.0201 (5) | |
C11 | 0.2656 (2) | 0.3657 (2) | 0.11184 (14) | 0.0203 (5) | |
C12 | 0.3885 (2) | 0.3687 (2) | 0.06822 (14) | 0.0234 (5) | |
H12 | 0.4080 | 0.4359 | 0.0378 | 0.028* | |
C13 | 0.4703 (2) | 0.2569 (2) | 0.07920 (14) | 0.0231 (5) | |
H13 | 0.5583 | 0.2313 | 0.0582 | 0.028* | |
C14 | 0.3985 (2) | 0.1845 (2) | 0.12870 (14) | 0.0197 (5) | |
C15 | 0.4476 (2) | 0.0609 (2) | 0.15096 (13) | 0.0188 (5) | |
C16 | 0.3767 (2) | −0.0142 (2) | 0.19454 (13) | 0.0183 (5) | |
C17 | 0.4268 (2) | −0.1430 (2) | 0.21407 (14) | 0.0218 (5) | |
H17 | 0.5119 | −0.1916 | 0.1997 | 0.026* | |
C18 | 0.3304 (2) | −0.1816 (2) | 0.25658 (14) | 0.0221 (5) | |
H18 | 0.3348 | −0.2625 | 0.2776 | 0.027* | |
C19 | 0.2192 (2) | −0.0774 (2) | 0.26415 (14) | 0.0201 (5) | |
C20 | 0.0991 (2) | −0.0790 (2) | 0.30596 (14) | 0.0208 (5) | |
N21 | −0.01710 (18) | 0.13659 (17) | 0.27972 (12) | 0.0205 (4) | |
N22 | 0.00418 (18) | 0.36198 (17) | 0.19644 (11) | 0.0200 (4) | |
N23 | 0.27382 (18) | 0.25292 (17) | 0.14785 (12) | 0.0202 (4) | |
N24 | 0.24939 (18) | 0.02413 (17) | 0.22570 (11) | 0.0191 (4) | |
C25 | −0.3337 (2) | 0.3803 (2) | 0.29319 (14) | 0.0208 (5) | |
C26 | −0.3878 (2) | 0.4126 (2) | 0.36934 (15) | 0.0248 (5) | |
H26 | −0.3347 | 0.3984 | 0.4091 | 0.030* | |
C27 | −0.5181 (2) | 0.4654 (2) | 0.38816 (16) | 0.0289 (6) | |
H27 | −0.5533 | 0.4870 | 0.4405 | 0.035* | |
C28 | −0.5967 (2) | 0.4868 (2) | 0.33112 (17) | 0.0308 (6) | |
H28 | −0.6856 | 0.5245 | 0.3438 | 0.037* | |
C29 | −0.5449 (2) | 0.4528 (3) | 0.25520 (17) | 0.0334 (6) | |
H29 | −0.5987 | 0.4652 | 0.2159 | 0.040* | |
C30 | −0.4141 (2) | 0.4007 (2) | 0.23643 (15) | 0.0272 (6) | |
H30 | −0.3792 | 0.3786 | 0.1841 | 0.033* | |
C31 | 0.1673 (2) | 0.5835 (2) | 0.07543 (14) | 0.0204 (5) | |
C32 | 0.2180 (2) | 0.6672 (2) | 0.11007 (16) | 0.0268 (6) | |
H32 | 0.2461 | 0.6482 | 0.1592 | 0.032* | |
C33 | 0.2281 (3) | 0.7783 (2) | 0.07356 (16) | 0.0289 (6) | |
H33 | 0.2619 | 0.8353 | 0.0981 | 0.035* | |
C34 | 0.1890 (2) | 0.8062 (2) | 0.00154 (15) | 0.0272 (6) | |
H34 | 0.1962 | 0.8820 | −0.0235 | 0.033* | |
C35 | 0.1397 (3) | 0.7234 (2) | −0.03369 (15) | 0.0288 (6) | |
H35 | 0.1134 | 0.7419 | −0.0833 | 0.035* | |
C36 | 0.1282 (3) | 0.6128 (2) | 0.00312 (15) | 0.0281 (6) | |
H36 | 0.0932 | 0.5567 | −0.0214 | 0.034* | |
C37 | 0.5886 (2) | 0.0036 (2) | 0.12930 (14) | 0.0195 (5) | |
C38 | 0.6340 (2) | −0.0785 (2) | 0.06737 (16) | 0.0286 (6) | |
H38 | 0.5759 | −0.0965 | 0.0366 | 0.034* | |
C39 | 0.7640 (3) | −0.1346 (2) | 0.05004 (17) | 0.0320 (6) | |
H39 | 0.7942 | −0.1906 | 0.0075 | 0.038* | |
C40 | 0.8496 (2) | −0.1093 (2) | 0.09436 (16) | 0.0294 (6) | |
H40 | 0.9384 | −0.1478 | 0.0825 | 0.035* | |
C41 | 0.8052 (2) | −0.0275 (3) | 0.15608 (16) | 0.0318 (6) | |
H41 | 0.8636 | −0.0100 | 0.1869 | 0.038* | |
C42 | 0.6750 (2) | 0.0293 (2) | 0.17307 (15) | 0.0262 (6) | |
H42 | 0.6451 | 0.0864 | 0.2151 | 0.031* | |
C43 | 0.0864 (2) | −0.1985 (2) | 0.34527 (15) | 0.0239 (5) | |
C44 | 0.1130 (3) | −0.2234 (2) | 0.42043 (16) | 0.0323 (6) | |
H44 | 0.1394 | −0.1640 | 0.4477 | 0.039* | |
C45 | 0.1013 (3) | −0.3356 (3) | 0.45643 (17) | 0.0357 (7) | |
H45 | 0.1182 | −0.3516 | 0.5083 | 0.043* | |
C46 | 0.0651 (3) | −0.4230 (2) | 0.41615 (18) | 0.0355 (7) | |
H46 | 0.0591 | −0.4998 | 0.4402 | 0.043* | |
C47 | 0.0377 (3) | −0.3996 (2) | 0.34204 (18) | 0.0350 (7) | |
H47 | 0.0123 | −0.4598 | 0.3149 | 0.042* | |
C48 | 0.0474 (3) | −0.2871 (2) | 0.30656 (17) | 0.0300 (6) | |
H48 | 0.0272 | −0.2706 | 0.2554 | 0.036* | |
S49 | 0.23927 (7) | 0.24791 (6) | 0.39412 (4) | 0.03066 (17) | |
O50 | 0.17015 (17) | 0.29085 (15) | 0.32552 (10) | 0.0290 (4) | |
C51 | 0.3986 (3) | 0.1664 (3) | 0.35689 (18) | 0.0381 (7) | |
H51A | 0.3963 | 0.1007 | 0.3215 | 0.057* | |
H51B | 0.4440 | 0.1292 | 0.3999 | 0.057* | |
H51C | 0.4432 | 0.2247 | 0.3288 | 0.057* | |
C52 | 0.1834 (3) | 0.1167 (3) | 0.43337 (18) | 0.0481 (8) | |
H52A | 0.0905 | 0.1423 | 0.4487 | 0.072* | |
H52B | 0.2250 | 0.0852 | 0.4788 | 0.072* | |
H52C | 0.2043 | 0.0509 | 0.3940 | 0.072* | |
S53 | 0.43730 (9) | 0.13359 (8) | 0.60560 (5) | 0.0334 (2) | 0.79 |
O54 | 0.3719 (3) | 0.0800 (3) | 0.55174 (16) | 0.0534 (8) | 0.79 |
C55 | 0.5477 (4) | 0.2053 (4) | 0.5461 (2) | 0.0463 (10) | 0.79 |
H55A | 0.6111 | 0.1418 | 0.5137 | 0.069* | 0.79 |
H55B | 0.5912 | 0.2452 | 0.5792 | 0.069* | 0.79 |
H55C | 0.5009 | 0.2681 | 0.5127 | 0.069* | 0.79 |
C56 | 0.3284 (5) | 0.2712 (4) | 0.6438 (3) | 0.0738 (16) | 0.79 |
H56A | 0.2868 | 0.3184 | 0.6019 | 0.111* | 0.79 |
H56B | 0.3744 | 0.3219 | 0.6675 | 0.111* | 0.79 |
H56C | 0.2634 | 0.2498 | 0.6831 | 0.111* | 0.79 |
C57 | 0.3916 (13) | 0.2614 (12) | 0.6256 (9) | 0.042 (4) | 0.21 |
H57 | 0.4224 | 0.3152 | 0.6594 | 0.050* | 0.21 |
Cl58 | 0.3341 (4) | 0.1600 (4) | 0.6821 (2) | 0.0535 (10) | 0.21 |
Cl59 | 0.2705 (4) | 0.3614 (4) | 0.5757 (2) | 0.0477 (9) | 0.21 |
Cl60 | 0.5222 (4) | 0.1928 (4) | 0.5536 (2) | 0.0592 (11) | 0.21 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.01465 (14) | 0.01548 (15) | 0.02500 (16) | −0.00249 (11) | −0.00051 (11) | 0.00135 (11) |
C1 | 0.0163 (11) | 0.0178 (11) | 0.0258 (13) | −0.0050 (10) | −0.0012 (10) | 0.0019 (10) |
C2 | 0.0200 (12) | 0.0214 (12) | 0.0247 (13) | −0.0062 (10) | 0.0022 (10) | 0.0038 (10) |
C3 | 0.0165 (12) | 0.0205 (12) | 0.0292 (13) | −0.0028 (10) | 0.0028 (10) | 0.0022 (10) |
C4 | 0.0141 (11) | 0.0182 (11) | 0.0255 (12) | −0.0039 (9) | 0.0003 (10) | 0.0003 (10) |
C5 | 0.0160 (11) | 0.0195 (12) | 0.0234 (12) | −0.0039 (10) | −0.0015 (9) | −0.0015 (10) |
C6 | 0.0156 (11) | 0.0165 (11) | 0.0257 (12) | −0.0016 (9) | −0.0023 (10) | −0.0008 (10) |
C7 | 0.0175 (12) | 0.0176 (12) | 0.0289 (13) | 0.0012 (10) | 0.0008 (10) | 0.0007 (10) |
C8 | 0.0208 (12) | 0.0166 (11) | 0.0308 (14) | −0.0028 (10) | −0.0036 (11) | 0.0049 (10) |
C9 | 0.0165 (11) | 0.0157 (11) | 0.0264 (13) | −0.0034 (9) | −0.0029 (10) | 0.0015 (10) |
C10 | 0.0188 (12) | 0.0186 (12) | 0.0230 (12) | −0.0050 (10) | −0.0028 (10) | 0.0028 (10) |
C11 | 0.0180 (12) | 0.0163 (11) | 0.0255 (13) | −0.0040 (10) | 0.0003 (10) | −0.0003 (10) |
C12 | 0.0201 (12) | 0.0202 (12) | 0.0289 (13) | −0.0060 (10) | 0.0010 (10) | 0.0030 (10) |
C13 | 0.0181 (12) | 0.0216 (12) | 0.0280 (13) | −0.0045 (10) | 0.0004 (10) | 0.0016 (10) |
C14 | 0.0150 (11) | 0.0187 (12) | 0.0239 (12) | −0.0031 (10) | 0.0007 (10) | −0.0013 (10) |
C15 | 0.0168 (11) | 0.0180 (11) | 0.0211 (12) | −0.0037 (9) | −0.0015 (9) | −0.0037 (10) |
C16 | 0.0137 (11) | 0.0184 (11) | 0.0223 (12) | −0.0030 (9) | −0.0023 (9) | −0.0005 (10) |
C17 | 0.0185 (12) | 0.0176 (11) | 0.0271 (13) | −0.0008 (10) | −0.0019 (10) | −0.0013 (10) |
C18 | 0.0210 (12) | 0.0148 (11) | 0.0295 (13) | −0.0027 (10) | −0.0037 (10) | 0.0016 (10) |
C19 | 0.0174 (11) | 0.0170 (11) | 0.0251 (12) | −0.0040 (10) | −0.0013 (10) | 0.0009 (10) |
C20 | 0.0199 (12) | 0.0148 (11) | 0.0272 (13) | −0.0036 (10) | −0.0038 (10) | 0.0028 (10) |
N21 | 0.0142 (9) | 0.0165 (10) | 0.0294 (11) | −0.0019 (8) | −0.0021 (8) | 0.0027 (9) |
N22 | 0.0153 (9) | 0.0172 (10) | 0.0250 (11) | −0.0018 (8) | −0.0001 (8) | 0.0034 (8) |
N23 | 0.0158 (10) | 0.0167 (10) | 0.0261 (11) | −0.0019 (8) | −0.0009 (8) | 0.0024 (8) |
N24 | 0.0152 (9) | 0.0180 (10) | 0.0237 (10) | −0.0050 (8) | 0.0005 (8) | −0.0001 (8) |
C25 | 0.0173 (12) | 0.0150 (11) | 0.0279 (13) | −0.0019 (10) | −0.0003 (10) | 0.0012 (10) |
C26 | 0.0198 (12) | 0.0228 (13) | 0.0299 (14) | −0.0042 (10) | 0.0003 (11) | 0.0002 (11) |
C27 | 0.0280 (14) | 0.0227 (13) | 0.0324 (14) | −0.0054 (11) | 0.0062 (12) | −0.0029 (11) |
C28 | 0.0167 (12) | 0.0227 (13) | 0.0467 (17) | 0.0000 (11) | 0.0057 (12) | 0.0039 (12) |
C29 | 0.0203 (13) | 0.0359 (15) | 0.0407 (16) | −0.0003 (12) | −0.0066 (12) | 0.0040 (13) |
C30 | 0.0212 (13) | 0.0290 (14) | 0.0290 (14) | −0.0033 (11) | −0.0014 (11) | 0.0012 (11) |
C31 | 0.0129 (11) | 0.0173 (11) | 0.0277 (13) | −0.0006 (9) | 0.0018 (10) | 0.0011 (10) |
C32 | 0.0272 (13) | 0.0254 (13) | 0.0295 (14) | −0.0073 (11) | −0.0093 (11) | 0.0065 (11) |
C33 | 0.0293 (14) | 0.0220 (13) | 0.0375 (15) | −0.0094 (11) | −0.0070 (12) | 0.0051 (11) |
C34 | 0.0212 (12) | 0.0204 (12) | 0.0338 (15) | −0.0005 (10) | 0.0059 (11) | 0.0096 (11) |
C35 | 0.0316 (14) | 0.0304 (14) | 0.0220 (13) | −0.0050 (12) | −0.0027 (11) | 0.0067 (11) |
C36 | 0.0315 (14) | 0.0263 (13) | 0.0261 (14) | −0.0082 (11) | −0.0021 (11) | 0.0025 (11) |
C37 | 0.0158 (11) | 0.0157 (11) | 0.0241 (12) | −0.0014 (9) | 0.0012 (10) | 0.0044 (10) |
C38 | 0.0236 (13) | 0.0263 (13) | 0.0341 (15) | −0.0033 (11) | −0.0023 (11) | −0.0055 (12) |
C39 | 0.0276 (14) | 0.0229 (13) | 0.0385 (16) | 0.0004 (11) | 0.0074 (12) | −0.0062 (12) |
C40 | 0.0188 (12) | 0.0235 (13) | 0.0386 (15) | 0.0017 (11) | 0.0045 (11) | 0.0119 (12) |
C41 | 0.0192 (13) | 0.0405 (16) | 0.0328 (15) | −0.0030 (12) | −0.0035 (11) | 0.0059 (13) |
C42 | 0.0190 (12) | 0.0331 (14) | 0.0234 (13) | −0.0022 (11) | 0.0000 (10) | −0.0016 (11) |
C43 | 0.0172 (12) | 0.0163 (12) | 0.0328 (14) | 0.0011 (10) | 0.0034 (10) | 0.0040 (11) |
C44 | 0.0332 (15) | 0.0280 (14) | 0.0349 (15) | −0.0076 (12) | −0.0037 (12) | 0.0074 (12) |
C45 | 0.0345 (15) | 0.0328 (15) | 0.0336 (15) | −0.0025 (13) | 0.0026 (13) | 0.0103 (13) |
C46 | 0.0311 (15) | 0.0199 (13) | 0.0472 (18) | −0.0013 (12) | 0.0107 (13) | 0.0062 (12) |
C47 | 0.0349 (15) | 0.0201 (13) | 0.0476 (18) | −0.0095 (12) | 0.0065 (13) | 0.0010 (12) |
C48 | 0.0287 (14) | 0.0216 (13) | 0.0378 (15) | −0.0063 (11) | 0.0005 (12) | 0.0024 (12) |
S49 | 0.0368 (4) | 0.0266 (3) | 0.0269 (3) | −0.0030 (3) | −0.0064 (3) | −0.0054 (3) |
O50 | 0.0315 (10) | 0.0225 (9) | 0.0325 (10) | −0.0035 (8) | −0.0085 (8) | −0.0024 (8) |
C51 | 0.0323 (15) | 0.0401 (16) | 0.0429 (17) | −0.0058 (13) | −0.0140 (13) | −0.0048 (14) |
C52 | 0.066 (2) | 0.0419 (18) | 0.0337 (17) | −0.0160 (17) | 0.0036 (16) | 0.0071 (14) |
S53 | 0.0415 (5) | 0.0297 (5) | 0.0306 (5) | −0.0114 (4) | −0.0052 (4) | −0.0009 (4) |
O54 | 0.065 (2) | 0.070 (2) | 0.0406 (16) | −0.0454 (17) | −0.0017 (14) | −0.0137 (14) |
C55 | 0.045 (2) | 0.049 (2) | 0.052 (3) | −0.029 (2) | 0.002 (2) | −0.004 (2) |
C56 | 0.058 (3) | 0.050 (3) | 0.098 (4) | −0.001 (2) | 0.022 (3) | −0.030 (3) |
C57 | 0.041 (8) | 0.034 (7) | 0.055 (9) | −0.001 (6) | −0.033 (7) | −0.001 (7) |
Cl58 | 0.057 (2) | 0.054 (2) | 0.063 (3) | −0.0330 (19) | −0.023 (2) | 0.0221 (19) |
Cl59 | 0.051 (2) | 0.053 (2) | 0.046 (2) | −0.0176 (18) | −0.0210 (17) | 0.0090 (17) |
Cl60 | 0.063 (3) | 0.059 (2) | 0.042 (2) | 0.006 (2) | 0.0003 (19) | −0.0060 (19) |
Zn—N23 | 2.063 (2) | C31—C32 | 1.390 (3) |
Zn—N22 | 2.0632 (19) | C31—C36 | 1.391 (4) |
Zn—N21 | 2.072 (2) | C32—C33 | 1.390 (4) |
Zn—N24 | 2.0753 (19) | C32—H32 | 0.9500 |
Zn—O50 | 2.1193 (17) | C33—C34 | 1.384 (4) |
C1—N21 | 1.371 (3) | C33—H33 | 0.9500 |
C1—C20 | 1.403 (3) | C34—C35 | 1.379 (4) |
C1—C2 | 1.442 (3) | C34—H34 | 0.9500 |
C2—C3 | 1.355 (3) | C35—C36 | 1.390 (4) |
C2—H2 | 0.9500 | C35—H35 | 0.9500 |
C3—C4 | 1.443 (3) | C36—H36 | 0.9500 |
C3—H3 | 0.9500 | C37—C42 | 1.384 (3) |
C4—N21 | 1.379 (3) | C37—C38 | 1.387 (3) |
C4—C5 | 1.405 (3) | C38—C39 | 1.389 (4) |
C5—C6 | 1.408 (3) | C38—H38 | 0.9500 |
C5—C25 | 1.494 (3) | C39—C40 | 1.381 (4) |
C6—N22 | 1.373 (3) | C39—H39 | 0.9500 |
C6—C7 | 1.447 (3) | C40—C41 | 1.382 (4) |
C7—C8 | 1.346 (3) | C40—H40 | 0.9500 |
C7—H7 | 0.9500 | C41—C42 | 1.393 (3) |
C8—C9 | 1.449 (3) | C41—H41 | 0.9500 |
C8—H8 | 0.9500 | C42—H42 | 0.9500 |
C9—N22 | 1.375 (3) | C43—C44 | 1.386 (4) |
C9—C10 | 1.403 (3) | C43—C48 | 1.395 (4) |
C10—C11 | 1.404 (3) | C44—C45 | 1.401 (4) |
C10—C31 | 1.504 (3) | C44—H44 | 0.9500 |
C11—N23 | 1.368 (3) | C45—C46 | 1.384 (4) |
C11—C12 | 1.449 (3) | C45—H45 | 0.9500 |
C12—C13 | 1.358 (3) | C46—C47 | 1.369 (4) |
C12—H12 | 0.9500 | C46—H46 | 0.9500 |
C13—C14 | 1.441 (3) | C47—C48 | 1.395 (4) |
C13—H13 | 0.9500 | C47—H47 | 0.9500 |
C14—N23 | 1.378 (3) | C48—H48 | 0.9500 |
C14—C15 | 1.403 (3) | S49—O50 | 1.5051 (19) |
C15—C16 | 1.408 (3) | S49—C51 | 1.782 (3) |
C15—C37 | 1.505 (3) | S49—C52 | 1.794 (3) |
C16—N24 | 1.379 (3) | C51—H51A | 0.9800 |
C16—C17 | 1.443 (3) | C51—H51B | 0.9800 |
C17—C18 | 1.349 (3) | C51—H51C | 0.9800 |
C17—H17 | 0.9500 | C52—H52A | 0.9800 |
C18—C19 | 1.441 (3) | C52—H52B | 0.9800 |
C18—H18 | 0.9500 | C52—H52C | 0.9800 |
C19—N24 | 1.378 (3) | S53—O54 | 1.482 (3) |
C19—C20 | 1.407 (3) | S53—C56 | 1.763 (4) |
C20—C43 | 1.500 (3) | S53—C55 | 1.796 (4) |
C25—C26 | 1.391 (3) | C55—H55A | 0.9800 |
C25—C30 | 1.391 (4) | C55—H55B | 0.9800 |
C26—C27 | 1.388 (3) | C55—H55C | 0.9800 |
C26—H26 | 0.9500 | C56—H56A | 0.9800 |
C27—C28 | 1.382 (4) | C56—H56B | 0.9800 |
C27—H27 | 0.9500 | C56—H56C | 0.9800 |
C28—C29 | 1.386 (4) | C57—Cl58 | 1.651 (16) |
C28—H28 | 0.9500 | C57—Cl60 | 1.783 (16) |
C29—C30 | 1.392 (3) | C57—Cl59 | 1.805 (13) |
C29—H29 | 0.9500 | C57—H57 | 1.0000 |
C30—H30 | 0.9500 | ||
N23—Zn—N22 | 89.07 (8) | C26—C27—H27 | 119.9 |
N23—Zn—N21 | 163.99 (8) | C27—C28—C29 | 119.5 (2) |
N22—Zn—N21 | 88.72 (8) | C27—C28—H28 | 120.3 |
N23—Zn—N24 | 88.60 (7) | C29—C28—H28 | 120.3 |
N22—Zn—N24 | 160.77 (8) | C28—C29—C30 | 120.1 (3) |
N21—Zn—N24 | 88.28 (7) | C28—C29—H29 | 120.0 |
N23—Zn—O50 | 97.37 (7) | C30—C29—H29 | 120.0 |
N22—Zn—O50 | 93.62 (7) | C29—C30—C25 | 120.9 (2) |
N21—Zn—O50 | 98.59 (8) | C29—C30—H30 | 119.5 |
N24—Zn—O50 | 105.61 (7) | C25—C30—H30 | 119.5 |
N21—C1—C20 | 125.7 (2) | C32—C31—C36 | 118.5 (2) |
N21—C1—C2 | 110.0 (2) | C32—C31—C10 | 120.5 (2) |
C20—C1—C2 | 124.3 (2) | C36—C31—C10 | 121.0 (2) |
C3—C2—C1 | 106.7 (2) | C33—C32—C31 | 120.7 (2) |
C3—C2—H2 | 126.6 | C33—C32—H32 | 119.7 |
C1—C2—H2 | 126.6 | C31—C32—H32 | 119.7 |
C2—C3—C4 | 107.5 (2) | C34—C33—C32 | 120.2 (2) |
C2—C3—H3 | 126.3 | C34—C33—H33 | 119.9 |
C4—C3—H3 | 126.3 | C32—C33—H33 | 119.9 |
N21—C4—C5 | 125.4 (2) | C35—C34—C33 | 119.7 (2) |
N21—C4—C3 | 109.25 (19) | C35—C34—H34 | 120.2 |
C5—C4—C3 | 125.3 (2) | C33—C34—H34 | 120.2 |
C4—C5—C6 | 125.4 (2) | C34—C35—C36 | 120.3 (2) |
C4—C5—C25 | 117.6 (2) | C34—C35—H35 | 119.9 |
C6—C5—C25 | 117.0 (2) | C36—C35—H35 | 119.9 |
N22—C6—C5 | 125.5 (2) | C35—C36—C31 | 120.7 (2) |
N22—C6—C7 | 109.3 (2) | C35—C36—H36 | 119.7 |
C5—C6—C7 | 125.2 (2) | C31—C36—H36 | 119.7 |
C8—C7—C6 | 107.5 (2) | C42—C37—C38 | 118.9 (2) |
C8—C7—H7 | 126.3 | C42—C37—C15 | 119.9 (2) |
C6—C7—H7 | 126.3 | C38—C37—C15 | 121.2 (2) |
C7—C8—C9 | 107.1 (2) | C37—C38—C39 | 120.5 (2) |
C7—C8—H8 | 126.4 | C37—C38—H38 | 119.7 |
C9—C8—H8 | 126.4 | C39—C38—H38 | 119.7 |
N22—C9—C10 | 126.1 (2) | C40—C39—C38 | 120.3 (2) |
N22—C9—C8 | 109.4 (2) | C40—C39—H39 | 119.8 |
C10—C9—C8 | 124.6 (2) | C38—C39—H39 | 119.8 |
C9—C10—C11 | 125.3 (2) | C39—C40—C41 | 119.6 (2) |
C9—C10—C31 | 117.4 (2) | C39—C40—H40 | 120.2 |
C11—C10—C31 | 117.3 (2) | C41—C40—H40 | 120.2 |
N23—C11—C10 | 125.5 (2) | C40—C41—C42 | 120.0 (3) |
N23—C11—C12 | 109.9 (2) | C40—C41—H41 | 120.0 |
C10—C11—C12 | 124.6 (2) | C42—C41—H41 | 120.0 |
C13—C12—C11 | 106.8 (2) | C37—C42—C41 | 120.7 (2) |
C13—C12—H12 | 126.6 | C37—C42—H42 | 119.7 |
C11—C12—H12 | 126.6 | C41—C42—H42 | 119.7 |
C12—C13—C14 | 107.1 (2) | C44—C43—C48 | 118.6 (2) |
C12—C13—H13 | 126.5 | C44—C43—C20 | 121.0 (2) |
C14—C13—H13 | 126.5 | C48—C43—C20 | 120.4 (2) |
N23—C14—C15 | 125.4 (2) | C43—C44—C45 | 120.5 (3) |
N23—C14—C13 | 109.8 (2) | C43—C44—H44 | 119.8 |
C15—C14—C13 | 124.7 (2) | C45—C44—H44 | 119.8 |
C14—C15—C16 | 125.5 (2) | C46—C45—C44 | 119.7 (3) |
C14—C15—C37 | 118.1 (2) | C46—C45—H45 | 120.1 |
C16—C15—C37 | 116.3 (2) | C44—C45—H45 | 120.1 |
N24—C16—C15 | 125.3 (2) | C47—C46—C45 | 120.6 (3) |
N24—C16—C17 | 109.6 (2) | C47—C46—H46 | 119.7 |
C15—C16—C17 | 125.0 (2) | C45—C46—H46 | 119.7 |
C18—C17—C16 | 107.2 (2) | C46—C47—C48 | 119.7 (3) |
C18—C17—H17 | 126.4 | C46—C47—H47 | 120.1 |
C16—C17—H17 | 126.4 | C48—C47—H47 | 120.1 |
C17—C18—C19 | 107.3 (2) | C43—C48—C47 | 120.8 (3) |
C17—C18—H18 | 126.3 | C43—C48—H48 | 119.6 |
C19—C18—H18 | 126.3 | C47—C48—H48 | 119.6 |
N24—C19—C20 | 125.4 (2) | O50—S49—C51 | 107.09 (12) |
N24—C19—C18 | 109.7 (2) | O50—S49—C52 | 105.97 (14) |
C20—C19—C18 | 124.9 (2) | C51—S49—C52 | 98.02 (15) |
C1—C20—C19 | 125.3 (2) | S49—O50—Zn | 135.80 (10) |
C1—C20—C43 | 117.5 (2) | S49—C51—H51A | 109.5 |
C19—C20—C43 | 117.2 (2) | S49—C51—H51B | 109.5 |
C1—N21—C4 | 106.51 (19) | H51A—C51—H51B | 109.5 |
C1—N21—Zn | 126.74 (15) | S49—C51—H51C | 109.5 |
C4—N21—Zn | 126.18 (15) | H51A—C51—H51C | 109.5 |
C6—N22—C9 | 106.79 (18) | H51B—C51—H51C | 109.5 |
C6—N22—Zn | 126.73 (16) | S49—C52—H52A | 109.5 |
C9—N22—Zn | 125.55 (15) | S49—C52—H52B | 109.5 |
C11—N23—C14 | 106.38 (19) | H52A—C52—H52B | 109.5 |
C11—N23—Zn | 126.47 (15) | S49—C52—H52C | 109.5 |
C14—N23—Zn | 126.62 (15) | H52A—C52—H52C | 109.5 |
C19—N24—C16 | 106.19 (18) | H52B—C52—H52C | 109.5 |
C19—N24—Zn | 126.86 (15) | O54—S53—C56 | 106.7 (2) |
C16—N24—Zn | 126.44 (15) | O54—S53—C55 | 106.30 (18) |
C26—C25—C30 | 118.2 (2) | C56—S53—C55 | 97.6 (2) |
C26—C25—C5 | 121.7 (2) | Cl58—C57—Cl60 | 114.3 (8) |
C30—C25—C5 | 120.1 (2) | Cl58—C57—Cl59 | 111.9 (8) |
C27—C26—C25 | 121.0 (2) | Cl60—C57—Cl59 | 107.1 (8) |
C27—C26—H26 | 119.5 | Cl58—C57—H57 | 107.8 |
C25—C26—H26 | 119.5 | Cl60—C57—H57 | 107.7 |
C28—C27—C26 | 120.3 (2) | Cl59—C57—H57 | 107.8 |
C28—C27—H27 | 119.9 |
D—H···A | D—H | H···A | D···A | D—H···A |
C34—H34···Cg1i | 0.95 | 2.66 | 3.582 (3) | 163 |
C28—H28···Cg2ii | 0.95 | 2.78 | 3.705 (3) | 165 |
C40—H40···Cg3iii | 0.95 | 2.77 | 3.702 (3) | 167 |
Symmetry codes: (i) −x+1, −y, −z; (ii) x−1, y+1, z; (iii) x+1, y−1, z. |