


Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808010003/sj2481sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536808010003/sj2481Isup2.hkl |
CCDC reference: 688832
Key indicators
- Single-crystal X-ray study
- T = 98 K
- Mean
(C-C) = 0.003 Å
- R factor = 0.041
- wR factor = 0.090
- Data-to-parameter ratio = 20.8
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.757 1.000 Tmin(prime) and Tmax expected: 0.818 0.866 RR(prime) = 0.801 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.80 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.87 PLAT150_ALERT_1_C Volume as Calculated Differs from that Given ... 5064.00 Ang-3 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.70 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for S4 - C8 .. 5.62 su PLAT230_ALERT_2_C Hirshfeld Test Diff for S6 - C27 .. 5.16 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - S6 .. 8.96 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - S8 .. 8.53 su
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.866 Tmax scaled 0.866 Tmin scaled 0.655
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 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 5 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The title compound was prepared by refluxing the parent zinc dithiocarbamate with 1,2-bis(4-pyridyl)ethane using a literature procedure (Lai et al., 2004). Colourless crystals of (I) were isolated by the slow evaporation of an ethanol/methanol (1/1) solution; m.p. 451 - 453 K.
The H atoms were geometrically placed (C—H = 0.95–0.99 Å) and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C).
Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
[Zn2(C7H14NS2)4(C12H12N2)] | F(000) = 2152 |
Mr = 1020.22 | Dx = 1.338 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 17064 reflections |
a = 18.645 (5) Å | θ = 2.1–30.5° |
b = 15.464 (5) Å | µ = 1.31 mm−1 |
c = 17.567 (4) Å | T = 98 K |
β = 90.756 (11)° | Block, colourless |
V = 5064 (3) Å3 | 0.15 × 0.11 × 0.11 mm |
Z = 4 |
Rigaku AFC12K/SATURN724 diffractometer | 10501 independent reflections |
Radiation source: fine-focus sealed tube | 9945 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
ω scans | θmax = 26.5°, θmin = 1.8° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −20→23 |
Tmin = 0.757, Tmax = 1 | k = −19→19 |
52873 measured reflections | l = −22→22 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.089 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0347P)2 + 4.0808P] where P = (Fo2 + 2Fc2)/3 |
10501 reflections | (Δ/σ)max = 0.001 |
505 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Zn2(C7H14NS2)4(C12H12N2)] | V = 5064 (3) Å3 |
Mr = 1020.22 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 18.645 (5) Å | µ = 1.31 mm−1 |
b = 15.464 (5) Å | T = 98 K |
c = 17.567 (4) Å | 0.15 × 0.11 × 0.11 mm |
β = 90.756 (11)° |
Rigaku AFC12K/SATURN724 diffractometer | 10501 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 9945 reflections with I > 2σ(I) |
Tmin = 0.757, Tmax = 1 | Rint = 0.040 |
52873 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.089 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.47 e Å−3 |
10501 reflections | Δρmin = −0.41 e Å−3 |
505 parameters |
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 | ||
Zn1 | 0.276298 (14) | 0.197149 (17) | 0.666864 (15) | 0.01860 (7) | |
Zn2 | 0.233401 (14) | 0.792692 (17) | 0.113503 (15) | 0.01919 (7) | |
S1 | 0.17394 (3) | 0.17012 (4) | 0.74108 (3) | 0.02267 (13) | |
S2 | 0.19934 (3) | 0.08862 (4) | 0.59234 (3) | 0.02227 (13) | |
S3 | 0.38566 (3) | 0.12770 (4) | 0.69274 (3) | 0.02016 (12) | |
S4 | 0.33916 (3) | 0.28608 (4) | 0.77400 (3) | 0.01942 (12) | |
S5 | 0.14013 (3) | 0.88860 (4) | 0.08654 (3) | 0.02158 (13) | |
S6 | 0.25034 (3) | 0.92616 (4) | 0.20351 (3) | 0.02157 (13) | |
S7 | 0.34319 (3) | 0.79323 (4) | 0.05134 (3) | 0.02127 (13) | |
S8 | 0.22111 (3) | 0.68586 (4) | 0.00107 (3) | 0.02082 (13) | |
N1 | 0.07846 (11) | 0.06823 (13) | 0.67052 (11) | 0.0228 (4) | |
N2 | 0.46332 (10) | 0.20599 (12) | 0.80062 (11) | 0.0192 (4) | |
N3 | 0.28479 (10) | 0.29088 (12) | 0.58188 (11) | 0.0182 (4) | |
N4 | 0.23109 (10) | 0.70372 (12) | 0.20140 (11) | 0.0185 (4) | |
N5 | 0.14157 (10) | 1.03193 (12) | 0.17162 (11) | 0.0203 (4) | |
N6 | 0.35081 (10) | 0.68252 (12) | −0.06437 (11) | 0.0202 (4) | |
C1 | 0.14307 (12) | 0.10457 (14) | 0.66783 (13) | 0.0197 (5) | |
C2 | 0.02924 (14) | 0.07935 (17) | 0.73493 (15) | 0.0290 (6) | |
H2A | 0.0570 | 0.1002 | 0.7797 | 0.035* | |
H2B | 0.0086 | 0.0224 | 0.7481 | 0.035* | |
C3 | −0.03145 (15) | 0.14235 (18) | 0.71824 (18) | 0.0370 (7) | |
H3A | −0.0579 | 0.1227 | 0.6722 | 0.044* | |
H3B | −0.0652 | 0.1414 | 0.7612 | 0.044* | |
C4 | −0.00637 (16) | 0.23467 (19) | 0.7060 (2) | 0.0501 (9) | |
H4A | −0.0478 | 0.2715 | 0.6940 | 0.075* | |
H4B | 0.0273 | 0.2363 | 0.6636 | 0.075* | |
H4C | 0.0176 | 0.2558 | 0.7523 | 0.075* | |
C5 | 0.05257 (13) | 0.00974 (15) | 0.60992 (14) | 0.0247 (5) | |
H5A | 0.0719 | 0.0292 | 0.5606 | 0.030* | |
H5B | −0.0004 | 0.0132 | 0.6066 | 0.030* | |
C6 | 0.07454 (14) | −0.08379 (16) | 0.62354 (16) | 0.0308 (6) | |
H6A | 0.0580 | −0.1022 | 0.6744 | 0.037* | |
H6B | 0.1275 | −0.0881 | 0.6232 | 0.037* | |
C7 | 0.04309 (15) | −0.14398 (19) | 0.56328 (19) | 0.0418 (7) | |
H7A | 0.0579 | −0.2035 | 0.5742 | 0.063* | |
H7B | 0.0605 | −0.1270 | 0.5130 | 0.063* | |
H7C | −0.0094 | −0.1402 | 0.5637 | 0.063* | |
C8 | 0.40247 (12) | 0.20721 (14) | 0.76077 (13) | 0.0186 (5) | |
C9 | 0.47860 (13) | 0.27132 (15) | 0.85971 (13) | 0.0209 (5) | |
H9A | 0.5103 | 0.2455 | 0.8992 | 0.025* | |
H9B | 0.4331 | 0.2878 | 0.8843 | 0.025* | |
C10 | 0.51413 (15) | 0.35234 (16) | 0.82855 (14) | 0.0281 (6) | |
H10A | 0.5567 | 0.3357 | 0.7988 | 0.034* | |
H10B | 0.4801 | 0.3825 | 0.7939 | 0.034* | |
C11 | 0.53706 (15) | 0.41336 (16) | 0.89228 (15) | 0.0302 (6) | |
H11A | 0.5593 | 0.4650 | 0.8704 | 0.045* | |
H11B | 0.5717 | 0.3841 | 0.9259 | 0.045* | |
H11C | 0.4950 | 0.4304 | 0.9215 | 0.045* | |
C12 | 0.52046 (12) | 0.14240 (15) | 0.78581 (13) | 0.0213 (5) | |
H12A | 0.5668 | 0.1663 | 0.8043 | 0.026* | |
H12B | 0.5241 | 0.1338 | 0.7301 | 0.026* | |
C13 | 0.50823 (13) | 0.05467 (15) | 0.82364 (13) | 0.0237 (5) | |
H13A | 0.4664 | 0.0264 | 0.7988 | 0.028* | |
H13B | 0.5507 | 0.0177 | 0.8149 | 0.028* | |
C14 | 0.49519 (14) | 0.05979 (16) | 0.90901 (14) | 0.0270 (5) | |
H14A | 0.4868 | 0.0016 | 0.9290 | 0.041* | |
H14B | 0.4531 | 0.0960 | 0.9184 | 0.041* | |
H14C | 0.5373 | 0.0851 | 0.9345 | 0.041* | |
C15 | 0.30356 (12) | 0.37329 (15) | 0.59697 (13) | 0.0204 (5) | |
H15 | 0.3127 | 0.3895 | 0.6484 | 0.025* | |
C16 | 0.31004 (12) | 0.43544 (15) | 0.54064 (13) | 0.0207 (5) | |
H16 | 0.3226 | 0.4931 | 0.5539 | 0.025* | |
C17 | 0.29832 (12) | 0.41359 (15) | 0.46541 (13) | 0.0215 (5) | |
C18 | 0.27989 (14) | 0.32803 (16) | 0.44944 (14) | 0.0246 (5) | |
H18 | 0.2717 | 0.3101 | 0.3983 | 0.029* | |
C19 | 0.27354 (13) | 0.26952 (15) | 0.50843 (13) | 0.0231 (5) | |
H19 | 0.2606 | 0.2116 | 0.4966 | 0.028* | |
C20 | 0.30233 (13) | 0.47978 (16) | 0.40236 (14) | 0.0251 (5) | |
H20A | 0.3227 | 0.4526 | 0.3564 | 0.030* | |
H20B | 0.3346 | 0.5275 | 0.4183 | 0.030* | |
C21 | 0.22824 (13) | 0.51607 (15) | 0.38322 (13) | 0.0232 (5) | |
H21A | 0.1961 | 0.4680 | 0.3679 | 0.028* | |
H21B | 0.2082 | 0.5432 | 0.4293 | 0.028* | |
C22 | 0.22989 (12) | 0.58203 (15) | 0.32004 (13) | 0.0205 (5) | |
C23 | 0.20409 (13) | 0.66545 (15) | 0.33017 (13) | 0.0225 (5) | |
H23 | 0.1854 | 0.6825 | 0.3780 | 0.027* | |
C24 | 0.20565 (13) | 0.72358 (15) | 0.27055 (13) | 0.0224 (5) | |
H24 | 0.1879 | 0.7804 | 0.2788 | 0.027* | |
C25 | 0.25688 (13) | 0.62323 (15) | 0.19170 (13) | 0.0227 (5) | |
H25 | 0.2756 | 0.6081 | 0.1435 | 0.027* | |
C26 | 0.25737 (13) | 0.56184 (15) | 0.24854 (13) | 0.0224 (5) | |
H26 | 0.2763 | 0.5059 | 0.2392 | 0.027* | |
C27 | 0.17453 (12) | 0.95762 (14) | 0.15605 (13) | 0.0193 (5) | |
C28 | 0.16746 (13) | 1.09056 (15) | 0.23204 (13) | 0.0211 (5) | |
H28A | 0.1553 | 1.1508 | 0.2178 | 0.025* | |
H28B | 0.2204 | 1.0863 | 0.2360 | 0.025* | |
C29 | 0.13528 (13) | 1.07032 (16) | 0.30966 (14) | 0.0251 (5) | |
H29A | 0.0824 | 1.0757 | 0.3064 | 0.030* | |
H29B | 0.1470 | 1.0100 | 0.3241 | 0.030* | |
C30 | 0.16433 (14) | 1.13174 (17) | 0.37031 (14) | 0.0285 (6) | |
H30A | 0.1434 | 1.1173 | 0.4196 | 0.043* | |
H30B | 0.1517 | 1.1913 | 0.3567 | 0.043* | |
H30C | 0.2166 | 1.1262 | 0.3738 | 0.043* | |
C31 | 0.08007 (13) | 1.06331 (15) | 0.12656 (14) | 0.0242 (5) | |
H31A | 0.0485 | 1.0981 | 0.1595 | 0.029* | |
H31B | 0.0521 | 1.0133 | 0.1073 | 0.029* | |
C32 | 0.10403 (14) | 1.11850 (17) | 0.05937 (15) | 0.0304 (6) | |
H32A | 0.1276 | 1.1716 | 0.0788 | 0.036* | |
H32B | 0.1397 | 1.0859 | 0.0295 | 0.036* | |
C33 | 0.04147 (17) | 1.1435 (2) | 0.00780 (19) | 0.0479 (8) | |
H33A | 0.0589 | 1.1792 | −0.0342 | 0.072* | |
H33B | 0.0063 | 1.1763 | 0.0370 | 0.072* | |
H33C | 0.0188 | 1.0911 | −0.0128 | 0.072* | |
C34 | 0.30891 (12) | 0.71559 (15) | −0.01075 (13) | 0.0191 (5) | |
C35 | 0.32439 (13) | 0.62269 (16) | −0.12376 (13) | 0.0235 (5) | |
H35A | 0.3371 | 0.6462 | −0.1742 | 0.028* | |
H35B | 0.2714 | 0.6199 | −0.1214 | 0.028* | |
C36 | 0.35456 (14) | 0.53096 (16) | −0.11662 (15) | 0.0283 (5) | |
H36A | 0.3379 | 0.4965 | −0.1609 | 0.034* | |
H36B | 0.4076 | 0.5337 | −0.1183 | 0.034* | |
C37 | 0.33268 (16) | 0.48523 (17) | −0.04401 (15) | 0.0340 (6) | |
H37A | 0.3537 | 0.4271 | −0.0428 | 0.051* | |
H37B | 0.2803 | 0.4808 | −0.0426 | 0.051* | |
H37C | 0.3500 | 0.5183 | 0.0002 | 0.051* | |
C38 | 0.42600 (13) | 0.71040 (15) | −0.07166 (14) | 0.0209 (5) | |
H38A | 0.4537 | 0.6631 | −0.0952 | 0.025* | |
H38B | 0.4464 | 0.7206 | −0.0201 | 0.025* | |
C39 | 0.43520 (14) | 0.79207 (16) | −0.11890 (15) | 0.0269 (5) | |
H39A | 0.4223 | 0.7801 | −0.1727 | 0.032* | |
H39B | 0.4029 | 0.8379 | −0.1000 | 0.032* | |
C40 | 0.51250 (14) | 0.82263 (17) | −0.11344 (16) | 0.0310 (6) | |
H40A | 0.5183 | 0.8750 | −0.1442 | 0.046* | |
H40B | 0.5443 | 0.7772 | −0.1324 | 0.046* | |
H40C | 0.5248 | 0.8354 | −0.0602 | 0.046* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01984 (14) | 0.01810 (14) | 0.01781 (14) | −0.00116 (10) | −0.00162 (10) | 0.00323 (10) |
Zn2 | 0.02074 (14) | 0.01852 (14) | 0.01832 (14) | 0.00293 (10) | 0.00090 (11) | 0.00377 (10) |
S1 | 0.0264 (3) | 0.0201 (3) | 0.0216 (3) | −0.0050 (2) | 0.0031 (2) | −0.0030 (2) |
S2 | 0.0238 (3) | 0.0234 (3) | 0.0196 (3) | −0.0045 (2) | 0.0012 (2) | −0.0015 (2) |
S3 | 0.0239 (3) | 0.0168 (3) | 0.0196 (3) | 0.0009 (2) | −0.0034 (2) | −0.0014 (2) |
S4 | 0.0219 (3) | 0.0182 (3) | 0.0180 (3) | 0.0021 (2) | −0.0028 (2) | −0.0004 (2) |
S5 | 0.0230 (3) | 0.0191 (3) | 0.0226 (3) | 0.0028 (2) | −0.0059 (2) | −0.0028 (2) |
S6 | 0.0253 (3) | 0.0186 (3) | 0.0206 (3) | 0.0018 (2) | −0.0063 (2) | 0.0012 (2) |
S7 | 0.0196 (3) | 0.0236 (3) | 0.0207 (3) | −0.0013 (2) | 0.0001 (2) | −0.0038 (2) |
S8 | 0.0199 (3) | 0.0237 (3) | 0.0188 (3) | −0.0016 (2) | −0.0010 (2) | −0.0006 (2) |
N1 | 0.0235 (10) | 0.0208 (10) | 0.0240 (10) | −0.0029 (8) | 0.0007 (8) | −0.0021 (8) |
N2 | 0.0209 (10) | 0.0181 (10) | 0.0186 (10) | 0.0005 (7) | −0.0034 (8) | −0.0003 (8) |
N3 | 0.0215 (10) | 0.0157 (9) | 0.0173 (10) | 0.0007 (7) | −0.0005 (8) | 0.0018 (7) |
N4 | 0.0217 (10) | 0.0155 (9) | 0.0183 (10) | 0.0011 (7) | −0.0003 (8) | 0.0000 (7) |
N5 | 0.0232 (10) | 0.0170 (9) | 0.0207 (10) | −0.0009 (8) | −0.0009 (8) | −0.0008 (8) |
N6 | 0.0211 (10) | 0.0218 (10) | 0.0177 (10) | 0.0006 (8) | −0.0010 (8) | −0.0017 (8) |
C1 | 0.0232 (11) | 0.0142 (11) | 0.0218 (11) | −0.0016 (9) | −0.0009 (9) | 0.0027 (9) |
C2 | 0.0299 (13) | 0.0257 (13) | 0.0317 (14) | −0.0072 (11) | 0.0108 (11) | −0.0016 (11) |
C3 | 0.0294 (14) | 0.0285 (14) | 0.0534 (18) | −0.0032 (11) | 0.0134 (13) | −0.0024 (13) |
C4 | 0.0307 (15) | 0.0302 (16) | 0.090 (3) | 0.0008 (12) | 0.0138 (16) | 0.0025 (16) |
C5 | 0.0230 (12) | 0.0219 (12) | 0.0291 (13) | −0.0040 (10) | −0.0019 (10) | −0.0020 (10) |
C6 | 0.0277 (13) | 0.0235 (13) | 0.0410 (15) | −0.0013 (10) | −0.0029 (12) | −0.0059 (11) |
C7 | 0.0319 (15) | 0.0314 (15) | 0.062 (2) | −0.0014 (12) | −0.0045 (14) | −0.0186 (14) |
C8 | 0.0231 (12) | 0.0171 (11) | 0.0155 (11) | −0.0044 (9) | −0.0003 (9) | 0.0040 (9) |
C9 | 0.0238 (12) | 0.0196 (11) | 0.0191 (11) | −0.0026 (9) | −0.0054 (9) | −0.0006 (9) |
C10 | 0.0375 (14) | 0.0230 (13) | 0.0237 (13) | −0.0076 (11) | −0.0072 (11) | 0.0033 (10) |
C11 | 0.0390 (15) | 0.0215 (13) | 0.0300 (14) | −0.0059 (11) | −0.0076 (11) | 0.0035 (11) |
C12 | 0.0201 (11) | 0.0210 (12) | 0.0229 (12) | 0.0026 (9) | −0.0007 (9) | 0.0017 (9) |
C13 | 0.0278 (12) | 0.0219 (12) | 0.0215 (12) | 0.0037 (10) | −0.0017 (10) | 0.0018 (10) |
C14 | 0.0329 (14) | 0.0243 (13) | 0.0238 (13) | −0.0027 (10) | −0.0020 (10) | 0.0027 (10) |
C15 | 0.0238 (12) | 0.0207 (12) | 0.0168 (11) | 0.0008 (9) | −0.0003 (9) | −0.0019 (9) |
C16 | 0.0252 (12) | 0.0160 (11) | 0.0209 (11) | −0.0022 (9) | −0.0009 (9) | 0.0020 (9) |
C17 | 0.0215 (11) | 0.0230 (12) | 0.0201 (11) | 0.0025 (9) | 0.0003 (9) | 0.0047 (9) |
C18 | 0.0348 (14) | 0.0227 (12) | 0.0162 (11) | 0.0011 (10) | 0.0006 (10) | 0.0008 (10) |
C19 | 0.0326 (13) | 0.0179 (11) | 0.0188 (11) | 0.0005 (10) | −0.0015 (10) | −0.0018 (9) |
C20 | 0.0293 (13) | 0.0259 (13) | 0.0201 (12) | −0.0016 (10) | −0.0009 (10) | 0.0073 (10) |
C21 | 0.0308 (13) | 0.0210 (12) | 0.0178 (11) | 0.0025 (10) | 0.0014 (10) | 0.0027 (9) |
C22 | 0.0245 (12) | 0.0183 (11) | 0.0187 (11) | −0.0005 (9) | −0.0004 (9) | 0.0009 (9) |
C23 | 0.0300 (13) | 0.0196 (12) | 0.0180 (11) | 0.0010 (10) | 0.0021 (10) | −0.0008 (9) |
C24 | 0.0275 (12) | 0.0173 (11) | 0.0224 (12) | 0.0034 (9) | 0.0024 (10) | −0.0011 (9) |
C25 | 0.0279 (12) | 0.0222 (12) | 0.0180 (11) | 0.0039 (10) | −0.0003 (10) | −0.0002 (9) |
C26 | 0.0297 (13) | 0.0173 (11) | 0.0201 (12) | 0.0052 (9) | −0.0003 (10) | −0.0001 (9) |
C27 | 0.0234 (11) | 0.0164 (11) | 0.0182 (11) | −0.0028 (9) | 0.0012 (9) | 0.0026 (9) |
C28 | 0.0236 (12) | 0.0180 (11) | 0.0218 (12) | −0.0036 (9) | 0.0017 (9) | −0.0030 (9) |
C29 | 0.0266 (12) | 0.0241 (12) | 0.0247 (13) | −0.0038 (10) | 0.0009 (10) | −0.0021 (10) |
C30 | 0.0329 (14) | 0.0316 (14) | 0.0209 (12) | −0.0039 (11) | −0.0009 (10) | −0.0016 (11) |
C31 | 0.0203 (11) | 0.0198 (12) | 0.0326 (13) | 0.0035 (9) | −0.0046 (10) | −0.0018 (10) |
C32 | 0.0289 (13) | 0.0297 (14) | 0.0324 (14) | 0.0030 (11) | −0.0068 (11) | 0.0060 (11) |
C33 | 0.0469 (18) | 0.0470 (19) | 0.0491 (19) | 0.0063 (15) | −0.0201 (15) | 0.0101 (15) |
C34 | 0.0211 (11) | 0.0200 (11) | 0.0163 (11) | 0.0024 (9) | −0.0018 (9) | 0.0041 (9) |
C35 | 0.0274 (12) | 0.0273 (13) | 0.0157 (11) | 0.0022 (10) | −0.0020 (9) | −0.0038 (10) |
C36 | 0.0313 (13) | 0.0240 (13) | 0.0295 (13) | 0.0010 (10) | −0.0016 (11) | −0.0045 (11) |
C37 | 0.0438 (16) | 0.0254 (13) | 0.0326 (15) | −0.0059 (12) | −0.0059 (12) | 0.0007 (11) |
C38 | 0.0213 (12) | 0.0215 (12) | 0.0200 (12) | 0.0003 (9) | 0.0011 (9) | 0.0001 (9) |
C39 | 0.0314 (14) | 0.0252 (13) | 0.0243 (13) | 0.0017 (10) | 0.0077 (11) | 0.0031 (10) |
C40 | 0.0348 (14) | 0.0249 (13) | 0.0336 (15) | −0.0038 (11) | 0.0114 (12) | −0.0045 (11) |
Zn1—S1 | 2.3627 (8) | C13—H13A | 0.9900 |
Zn1—S2 | 2.5573 (8) | C13—H13B | 0.9900 |
Zn1—S3 | 2.3437 (8) | C14—H14A | 0.9800 |
Zn1—S4 | 2.5978 (8) | C14—H14B | 0.9800 |
Zn1—N3 | 2.0882 (19) | C14—H14C | 0.9800 |
Zn2—S5 | 2.3295 (8) | C15—C16 | 1.386 (3) |
Zn2—S6 | 2.6166 (9) | C15—H15 | 0.9500 |
Zn2—S7 | 2.3327 (9) | C16—C17 | 1.379 (3) |
Zn2—S8 | 2.5829 (8) | C16—H16 | 0.9500 |
Zn2—N4 | 2.0691 (19) | C17—C18 | 1.394 (3) |
S1—C1 | 1.731 (2) | C17—C20 | 1.511 (3) |
S2—C1 | 1.720 (2) | C18—C19 | 1.382 (3) |
S3—C8 | 1.740 (2) | C18—H18 | 0.9500 |
S4—C8 | 1.715 (2) | C19—H19 | 0.9500 |
S5—C27 | 1.738 (2) | C20—C21 | 1.524 (3) |
S6—C27 | 1.702 (2) | C20—H20A | 0.9900 |
S7—C34 | 1.738 (2) | C20—H20B | 0.9900 |
S8—C34 | 1.716 (2) | C21—C22 | 1.508 (3) |
N1—C1 | 1.331 (3) | C21—H21A | 0.9900 |
N1—C5 | 1.473 (3) | C21—H21B | 0.9900 |
N1—C2 | 1.476 (3) | C22—C23 | 1.389 (3) |
N2—C8 | 1.326 (3) | C22—C26 | 1.398 (3) |
N2—C9 | 1.474 (3) | C23—C24 | 1.381 (3) |
N2—C12 | 1.475 (3) | C23—H23 | 0.9500 |
N3—C19 | 1.346 (3) | C24—H24 | 0.9500 |
N3—C15 | 1.347 (3) | C25—C26 | 1.378 (3) |
N4—C24 | 1.345 (3) | C25—H25 | 0.9500 |
N4—C25 | 1.346 (3) | C26—H26 | 0.9500 |
N5—C27 | 1.333 (3) | C28—C29 | 1.529 (3) |
N5—C31 | 1.467 (3) | C28—H28A | 0.9900 |
N5—C28 | 1.473 (3) | C28—H28B | 0.9900 |
N6—C34 | 1.334 (3) | C29—C30 | 1.522 (3) |
N6—C38 | 1.474 (3) | C29—H29A | 0.9900 |
N6—C35 | 1.474 (3) | C29—H29B | 0.9900 |
C2—C3 | 1.519 (4) | C30—H30A | 0.9800 |
C2—H2A | 0.9900 | C30—H30B | 0.9800 |
C2—H2B | 0.9900 | C30—H30C | 0.9800 |
C3—C4 | 1.519 (4) | C31—C32 | 1.528 (4) |
C3—H3A | 0.9900 | C31—H31A | 0.9900 |
C3—H3B | 0.9900 | C31—H31B | 0.9900 |
C4—H4A | 0.9800 | C32—C33 | 1.517 (4) |
C4—H4B | 0.9800 | C32—H32A | 0.9900 |
C4—H4C | 0.9800 | C32—H32B | 0.9900 |
C5—C6 | 1.521 (3) | C33—H33A | 0.9800 |
C5—H5A | 0.9900 | C33—H33B | 0.9800 |
C5—H5B | 0.9900 | C33—H33C | 0.9800 |
C6—C7 | 1.521 (4) | C35—C36 | 1.530 (3) |
C6—H6A | 0.9900 | C35—H35A | 0.9900 |
C6—H6B | 0.9900 | C35—H35B | 0.9900 |
C7—H7A | 0.9800 | C36—C37 | 1.519 (4) |
C7—H7B | 0.9800 | C36—H36A | 0.9900 |
C7—H7C | 0.9800 | C36—H36B | 0.9900 |
C9—C10 | 1.522 (3) | C37—H37A | 0.9800 |
C9—H9A | 0.9900 | C37—H37B | 0.9800 |
C9—H9B | 0.9900 | C37—H37C | 0.9800 |
C10—C11 | 1.521 (3) | C38—C39 | 1.522 (3) |
C10—H10A | 0.9900 | C38—H38A | 0.9900 |
C10—H10B | 0.9900 | C38—H38B | 0.9900 |
C11—H11A | 0.9800 | C39—C40 | 1.519 (4) |
C11—H11B | 0.9800 | C39—H39A | 0.9900 |
C11—H11C | 0.9800 | C39—H39B | 0.9900 |
C12—C13 | 1.529 (3) | C40—H40A | 0.9800 |
C12—H12A | 0.9900 | C40—H40B | 0.9800 |
C12—H12B | 0.9900 | C40—H40C | 0.9800 |
C13—C14 | 1.524 (3) | ||
N3—Zn1—S3 | 112.50 (6) | H14A—C14—H14C | 109.5 |
N3—Zn1—S1 | 125.92 (6) | H14B—C14—H14C | 109.5 |
S3—Zn1—S1 | 121.26 (3) | N3—C15—C16 | 122.7 (2) |
N3—Zn1—S2 | 97.87 (6) | N3—C15—H15 | 118.6 |
S3—Zn1—S2 | 106.22 (3) | C16—C15—H15 | 118.6 |
S1—Zn1—S2 | 73.42 (3) | C17—C16—C15 | 120.0 (2) |
N3—Zn1—S4 | 96.47 (6) | C17—C16—H16 | 120.0 |
S3—Zn1—S4 | 73.68 (3) | C15—C16—H16 | 120.0 |
S1—Zn1—S4 | 93.09 (3) | C16—C17—C18 | 117.4 (2) |
S2—Zn1—S4 | 164.37 (2) | C16—C17—C20 | 121.9 (2) |
N4—Zn2—S5 | 123.52 (6) | C18—C17—C20 | 120.6 (2) |
N4—Zn2—S7 | 112.26 (6) | C19—C18—C17 | 119.6 (2) |
S5—Zn2—S7 | 124.05 (3) | C19—C18—H18 | 120.2 |
N4—Zn2—S8 | 98.21 (6) | C17—C18—H18 | 120.2 |
S5—Zn2—S8 | 101.15 (3) | N3—C19—C18 | 123.0 (2) |
S7—Zn2—S8 | 73.37 (2) | N3—C19—H19 | 118.5 |
N4—Zn2—S6 | 94.42 (6) | C18—C19—H19 | 118.5 |
S5—Zn2—S6 | 72.81 (3) | C17—C20—C21 | 111.0 (2) |
S7—Zn2—S6 | 100.40 (2) | C17—C20—H20A | 109.4 |
S6—Zn2—S8 | 167.27 (2) | C21—C20—H20A | 109.4 |
C1—S1—Zn1 | 87.50 (8) | C17—C20—H20B | 109.4 |
C1—S2—Zn1 | 81.66 (8) | C21—C20—H20B | 109.4 |
C8—S3—Zn1 | 87.58 (8) | H20A—C20—H20B | 108.0 |
C8—S4—Zn1 | 80.22 (8) | C22—C21—C20 | 112.6 (2) |
C27—S5—Zn2 | 88.89 (8) | C22—C21—H21A | 109.1 |
C27—S6—Zn2 | 80.60 (8) | C20—C21—H21A | 109.1 |
C34—S7—Zn2 | 88.49 (8) | C22—C21—H21B | 109.1 |
C34—S8—Zn2 | 81.14 (8) | C20—C21—H21B | 109.1 |
C1—N1—C5 | 121.4 (2) | H21A—C21—H21B | 107.8 |
C1—N1—C2 | 123.4 (2) | C23—C22—C26 | 117.0 (2) |
C5—N1—C2 | 115.10 (19) | C23—C22—C21 | 121.6 (2) |
C8—N2—C9 | 121.23 (19) | C26—C22—C21 | 121.4 (2) |
C8—N2—C12 | 122.10 (19) | C24—C23—C22 | 119.8 (2) |
C9—N2—C12 | 116.61 (18) | C24—C23—H23 | 120.1 |
C19—N3—C15 | 117.24 (19) | C22—C23—H23 | 120.1 |
C19—N3—Zn1 | 120.18 (15) | N4—C24—C23 | 123.2 (2) |
C15—N3—Zn1 | 122.54 (15) | N4—C24—H24 | 118.4 |
C24—N4—C25 | 117.1 (2) | C23—C24—H24 | 118.4 |
C24—N4—Zn2 | 122.21 (15) | N4—C25—C26 | 123.0 (2) |
C25—N4—Zn2 | 120.62 (15) | N4—C25—H25 | 118.5 |
C27—N5—C31 | 122.23 (19) | C26—C25—H25 | 118.5 |
C27—N5—C28 | 122.1 (2) | C25—C26—C22 | 119.9 (2) |
C31—N5—C28 | 115.58 (19) | C25—C26—H26 | 120.1 |
C34—N6—C38 | 121.05 (19) | C22—C26—H26 | 120.1 |
C34—N6—C35 | 123.2 (2) | N5—C27—S6 | 121.86 (17) |
C38—N6—C35 | 115.55 (19) | N5—C27—S5 | 120.44 (18) |
N1—C1—S2 | 121.91 (18) | S6—C27—S5 | 117.70 (13) |
N1—C1—S1 | 120.88 (18) | N5—C28—C29 | 112.82 (19) |
S2—C1—S1 | 117.21 (13) | N5—C28—H28A | 109.0 |
N1—C2—C3 | 113.3 (2) | C29—C28—H28A | 109.0 |
N1—C2—H2A | 108.9 | N5—C28—H28B | 109.0 |
C3—C2—H2A | 108.9 | C29—C28—H28B | 109.0 |
N1—C2—H2B | 108.9 | H28A—C28—H28B | 107.8 |
C3—C2—H2B | 108.9 | C30—C29—C28 | 110.9 (2) |
H2A—C2—H2B | 107.7 | C30—C29—H29A | 109.5 |
C4—C3—C2 | 113.6 (2) | C28—C29—H29A | 109.5 |
C4—C3—H3A | 108.8 | C30—C29—H29B | 109.5 |
C2—C3—H3A | 108.8 | C28—C29—H29B | 109.5 |
C4—C3—H3B | 108.8 | H29A—C29—H29B | 108.1 |
C2—C3—H3B | 108.8 | C29—C30—H30A | 109.5 |
H3A—C3—H3B | 107.7 | C29—C30—H30B | 109.5 |
C3—C4—H4A | 109.5 | H30A—C30—H30B | 109.5 |
C3—C4—H4B | 109.5 | C29—C30—H30C | 109.5 |
H4A—C4—H4B | 109.5 | H30A—C30—H30C | 109.5 |
C3—C4—H4C | 109.5 | H30B—C30—H30C | 109.5 |
H4A—C4—H4C | 109.5 | N5—C31—C32 | 111.5 (2) |
H4B—C4—H4C | 109.5 | N5—C31—H31A | 109.3 |
N1—C5—C6 | 112.6 (2) | C32—C31—H31A | 109.3 |
N1—C5—H5A | 109.1 | N5—C31—H31B | 109.3 |
C6—C5—H5A | 109.1 | C32—C31—H31B | 109.3 |
N1—C5—H5B | 109.1 | H31A—C31—H31B | 108.0 |
C6—C5—H5B | 109.1 | C33—C32—C31 | 111.9 (2) |
H5A—C5—H5B | 107.8 | C33—C32—H32A | 109.2 |
C5—C6—C7 | 111.8 (2) | C31—C32—H32A | 109.2 |
C5—C6—H6A | 109.3 | C33—C32—H32B | 109.2 |
C7—C6—H6A | 109.3 | C31—C32—H32B | 109.2 |
C5—C6—H6B | 109.3 | H32A—C32—H32B | 107.9 |
C7—C6—H6B | 109.3 | C32—C33—H33A | 109.5 |
H6A—C6—H6B | 107.9 | C32—C33—H33B | 109.5 |
C6—C7—H7A | 109.5 | H33A—C33—H33B | 109.5 |
C6—C7—H7B | 109.5 | C32—C33—H33C | 109.5 |
H7A—C7—H7B | 109.5 | H33A—C33—H33C | 109.5 |
C6—C7—H7C | 109.5 | H33B—C33—H33C | 109.5 |
H7A—C7—H7C | 109.5 | N6—C34—S8 | 123.47 (18) |
H7B—C7—H7C | 109.5 | N6—C34—S7 | 119.62 (18) |
N2—C8—S4 | 121.63 (17) | S8—C34—S7 | 116.92 (13) |
N2—C8—S3 | 119.85 (18) | N6—C35—C36 | 113.9 (2) |
S4—C8—S3 | 118.52 (13) | N6—C35—H35A | 108.8 |
N2—C9—C10 | 113.1 (2) | C36—C35—H35A | 108.8 |
N2—C9—H9A | 109.0 | N6—C35—H35B | 108.8 |
C10—C9—H9A | 109.0 | C36—C35—H35B | 108.8 |
N2—C9—H9B | 109.0 | H35A—C35—H35B | 107.7 |
C10—C9—H9B | 109.0 | C37—C36—C35 | 113.4 (2) |
H9A—C9—H9B | 107.8 | C37—C36—H36A | 108.9 |
C11—C10—C9 | 111.4 (2) | C35—C36—H36A | 108.9 |
C11—C10—H10A | 109.3 | C37—C36—H36B | 108.9 |
C9—C10—H10A | 109.3 | C35—C36—H36B | 108.9 |
C11—C10—H10B | 109.3 | H36A—C36—H36B | 107.7 |
C9—C10—H10B | 109.3 | C36—C37—H37A | 109.5 |
H10A—C10—H10B | 108.0 | C36—C37—H37B | 109.5 |
C10—C11—H11A | 109.5 | H37A—C37—H37B | 109.5 |
C10—C11—H11B | 109.5 | C36—C37—H37C | 109.5 |
H11A—C11—H11B | 109.5 | H37A—C37—H37C | 109.5 |
C10—C11—H11C | 109.5 | H37B—C37—H37C | 109.5 |
H11A—C11—H11C | 109.5 | N6—C38—C39 | 113.84 (19) |
H11B—C11—H11C | 109.5 | N6—C38—H38A | 108.8 |
N2—C12—C13 | 113.74 (19) | C39—C38—H38A | 108.8 |
N2—C12—H12A | 108.8 | N6—C38—H38B | 108.8 |
C13—C12—H12A | 108.8 | C39—C38—H38B | 108.8 |
N2—C12—H12B | 108.8 | H38A—C38—H38B | 107.7 |
C13—C12—H12B | 108.8 | C40—C39—C38 | 109.7 (2) |
H12A—C12—H12B | 107.7 | C40—C39—H39A | 109.7 |
C14—C13—C12 | 114.1 (2) | C38—C39—H39A | 109.7 |
C14—C13—H13A | 108.7 | C40—C39—H39B | 109.7 |
C12—C13—H13A | 108.7 | C38—C39—H39B | 109.7 |
C14—C13—H13B | 108.7 | H39A—C39—H39B | 108.2 |
C12—C13—H13B | 108.7 | C39—C40—H40A | 109.5 |
H13A—C13—H13B | 107.6 | C39—C40—H40B | 109.5 |
C13—C14—H14A | 109.5 | H40A—C40—H40B | 109.5 |
C13—C14—H14B | 109.5 | C39—C40—H40C | 109.5 |
H14A—C14—H14B | 109.5 | H40A—C40—H40C | 109.5 |
C13—C14—H14C | 109.5 | H40B—C40—H40C | 109.5 |
N3—Zn1—S1—C1 | 84.91 (10) | C12—N2—C8—S3 | 4.3 (3) |
S3—Zn1—S1—C1 | −102.05 (8) | Zn1—S4—C8—N2 | 179.3 (2) |
S2—Zn1—S1—C1 | −2.83 (8) | Zn1—S4—C8—S3 | −0.32 (11) |
S4—Zn1—S1—C1 | −174.81 (8) | Zn1—S3—C8—N2 | −179.31 (18) |
N3—Zn1—S2—C1 | −122.35 (9) | Zn1—S3—C8—S4 | 0.35 (12) |
S3—Zn1—S2—C1 | 121.38 (8) | C8—N2—C9—C10 | −87.7 (3) |
S1—Zn1—S2—C1 | 2.88 (8) | C12—N2—C9—C10 | 89.4 (2) |
S4—Zn1—S2—C1 | 34.02 (12) | N2—C9—C10—C11 | −173.2 (2) |
N3—Zn1—S3—C8 | 90.13 (10) | C8—N2—C12—C13 | −82.4 (3) |
S1—Zn1—S3—C8 | −83.78 (8) | C9—N2—C12—C13 | 100.6 (2) |
S2—Zn1—S3—C8 | −163.92 (7) | N2—C12—C13—C14 | −53.5 (3) |
S4—Zn1—S3—C8 | −0.21 (7) | C19—N3—C15—C16 | 1.3 (3) |
N3—Zn1—S4—C8 | −111.38 (9) | Zn1—N3—C15—C16 | 179.25 (17) |
S3—Zn1—S4—C8 | 0.22 (8) | N3—C15—C16—C17 | −1.1 (4) |
S1—Zn1—S4—C8 | 121.93 (8) | C15—C16—C17—C18 | 0.2 (3) |
S2—Zn1—S4—C8 | 92.17 (11) | C15—C16—C17—C20 | 177.9 (2) |
N4—Zn2—S5—C27 | 83.52 (10) | C16—C17—C18—C19 | 0.5 (4) |
S7—Zn2—S5—C27 | −91.36 (8) | C20—C17—C18—C19 | −177.2 (2) |
S8—Zn2—S5—C27 | −168.71 (8) | C15—N3—C19—C18 | −0.5 (4) |
S6—Zn2—S5—C27 | −0.27 (8) | Zn1—N3—C19—C18 | −178.53 (19) |
N4—Zn2—S6—C27 | −123.49 (9) | C17—C18—C19—N3 | −0.4 (4) |
S5—Zn2—S6—C27 | 0.28 (8) | C16—C17—C20—C21 | −94.6 (3) |
S7—Zn2—S6—C27 | 122.90 (8) | C18—C17—C20—C21 | 83.0 (3) |
S8—Zn2—S6—C27 | 63.46 (13) | C17—C20—C21—C22 | −179.6 (2) |
N4—Zn2—S7—C34 | 90.49 (10) | C20—C21—C22—C23 | −122.9 (2) |
S5—Zn2—S7—C34 | −94.13 (8) | C20—C21—C22—C26 | 57.3 (3) |
S8—Zn2—S7—C34 | −1.74 (7) | C26—C22—C23—C24 | 0.8 (3) |
S6—Zn2—S7—C34 | −170.32 (8) | C21—C22—C23—C24 | −179.1 (2) |
N4—Zn2—S8—C34 | −109.09 (9) | C25—N4—C24—C23 | −1.0 (3) |
S5—Zn2—S8—C34 | 124.24 (8) | Zn2—N4—C24—C23 | −179.50 (18) |
S7—Zn2—S8—C34 | 1.78 (8) | C22—C23—C24—N4 | 0.2 (4) |
S6—Zn2—S8—C34 | 63.91 (12) | C24—N4—C25—C26 | 0.7 (3) |
S3—Zn1—N3—C19 | 90.38 (18) | Zn2—N4—C25—C26 | 179.25 (18) |
S1—Zn1—N3—C19 | −96.06 (18) | N4—C25—C26—C22 | 0.3 (4) |
S2—Zn1—N3—C19 | −20.87 (18) | C23—C22—C26—C25 | −1.0 (3) |
S4—Zn1—N3—C19 | 165.37 (17) | C21—C22—C26—C25 | 178.8 (2) |
S3—Zn1—N3—C15 | −87.53 (18) | C31—N5—C27—S6 | 174.39 (17) |
S1—Zn1—N3—C15 | 86.03 (18) | C28—N5—C27—S6 | −1.5 (3) |
S2—Zn1—N3—C15 | 161.22 (17) | C31—N5—C27—S5 | −6.4 (3) |
S4—Zn1—N3—C15 | −12.54 (18) | C28—N5—C27—S5 | 177.64 (16) |
S5—Zn2—N4—C24 | −41.6 (2) | Zn2—S6—C27—N5 | 178.8 (2) |
S7—Zn2—N4—C24 | 133.80 (17) | Zn2—S6—C27—S5 | −0.41 (11) |
S8—Zn2—N4—C24 | −150.88 (18) | Zn2—S5—C27—N5 | −178.76 (18) |
S6—Zn2—N4—C24 | 30.66 (18) | Zn2—S5—C27—S6 | 0.45 (13) |
S5—Zn2—N4—C25 | 139.88 (16) | C27—N5—C28—C29 | −89.1 (3) |
S7—Zn2—N4—C25 | −44.70 (19) | C31—N5—C28—C29 | 94.7 (2) |
S8—Zn2—N4—C25 | 30.62 (18) | N5—C28—C29—C30 | 179.3 (2) |
S6—Zn2—N4—C25 | −147.83 (17) | C27—N5—C31—C32 | −89.0 (3) |
C5—N1—C1—S2 | 2.1 (3) | C28—N5—C31—C32 | 87.1 (2) |
C2—N1—C1—S2 | 178.98 (18) | N5—C31—C32—C33 | 174.1 (2) |
C5—N1—C1—S1 | −177.72 (17) | C38—N6—C34—S8 | −179.81 (16) |
C2—N1—C1—S1 | −0.9 (3) | C35—N6—C34—S8 | 5.8 (3) |
Zn1—S2—C1—N1 | 175.9 (2) | C38—N6—C34—S7 | 0.3 (3) |
Zn1—S2—C1—S1 | −4.24 (11) | C35—N6—C34—S7 | −174.08 (17) |
Zn1—S1—C1—N1 | −175.59 (19) | Zn2—S8—C34—N6 | 177.6 (2) |
Zn1—S1—C1—S2 | 4.54 (12) | Zn2—S8—C34—S7 | −2.57 (11) |
C1—N1—C2—C3 | 103.4 (3) | Zn2—S7—C34—N6 | −177.32 (18) |
C5—N1—C2—C3 | −79.6 (3) | Zn2—S7—C34—S8 | 2.82 (12) |
N1—C2—C3—C4 | −65.2 (3) | C34—N6—C35—C36 | −112.6 (2) |
C1—N1—C5—C6 | 87.4 (3) | C38—N6—C35—C36 | 72.7 (3) |
C2—N1—C5—C6 | −89.7 (3) | N6—C35—C36—C37 | 63.7 (3) |
N1—C5—C6—C7 | 176.1 (2) | C34—N6—C38—C39 | −84.9 (3) |
C9—N2—C8—S4 | 1.6 (3) | C35—N6—C38—C39 | 90.0 (2) |
C12—N2—C8—S4 | −175.34 (16) | N6—C38—C39—C40 | 171.8 (2) |
C9—N2—C8—S3 | −178.76 (16) |
D—H···A | D—H | H···A | D···A | D—H···A |
C28—H28a···S1i | 0.99 | 2.82 | 3.706 (3) | 149 |
C40—H40b···S3ii | 0.98 | 2.87 | 3.834 (3) | 170 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C7H14NS2)4(C12H12N2)] |
Mr | 1020.22 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 98 |
a, b, c (Å) | 18.645 (5), 15.464 (5), 17.567 (4) |
β (°) | 90.756 (11) |
V (Å3) | 5064 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.31 |
Crystal size (mm) | 0.15 × 0.11 × 0.11 |
Data collection | |
Diffractometer | Rigaku AFC12K/SATURN724 diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.757, 1 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 52873, 10501, 9945 |
Rint | 0.040 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.089, 1.14 |
No. of reflections | 10501 |
No. of parameters | 505 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.41 |
Computer programs: CrystalClear (Rigaku, 2005), PATTY in DIRDIF92 (Beurskens et al., 1992), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006).
Zn1—S1 | 2.3627 (8) | Zn2—S5 | 2.3295 (8) |
Zn1—S2 | 2.5573 (8) | Zn2—S6 | 2.6166 (9) |
Zn1—S3 | 2.3437 (8) | Zn2—S7 | 2.3327 (9) |
Zn1—S4 | 2.5978 (8) | Zn2—S8 | 2.5829 (8) |
Zn1—N3 | 2.0882 (19) | Zn2—N4 | 2.0691 (19) |
N3—Zn1—S1 | 125.92 (6) | S5—Zn2—S7 | 124.05 (3) |
S2—Zn1—S4 | 164.37 (2) | S6—Zn2—S8 | 167.27 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
C28—H28a···S1i | 0.99 | 2.82 | 3.706 (3) | 149 |
C40—H40b···S3ii | 0.98 | 2.87 | 3.834 (3) | 170 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, y+1/2, −z+1/2. |
Interest in the title compound (I), Fig. 1 & Table 1, rests with an on-going investigation of the aggregation patterns of zinc and cadmium 1,1-dithiolates (Lai et al., 2004, Chen et al., 2006 & Benson et al., 2007). The dimeric structure features two highly distorted trigonal bipyramidal NS4 coordination geometries with values of τ = 0.64 and 0.72 for Zn1 and Zn2, respectively (Addison et al., 1984). The dithiocarbamate ligands coordinate forming almost symmetrical Zn—S bond distances in accord with expectation (Tiekink, 2006). The primary interactions between molecules are of the type C—H···S, Table 2. Each dimer participates in four such interactions. Dimers are arranged in an herringbone fashion in the bc-plane, Fig. 2. The resultant layers are basically flat with the n-propyl groups projecting above and below to inter-digitate with adjacent layers, Fig. 3.