Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101019322/av0048sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768101019322/av0048sup2.hkl |
CCDC reference: 180221
Program(s) used to solve structure: SHELXS93 (Sheldrick, 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
C10.77H8N0.77S8.77 | F(000) = 873 |
Mr = 429.37 | Dx = 1.797 Mg m−3 |
Orthorhombic, Pbcm | Mo Kα radiation, λ = 0.71069 Å |
a = 6.638 (1) Å | µ = 1.21 mm−1 |
b = 8.309 (2) Å | T = 110 K |
c = 28.776 (6) Å | Rhombic plates, black |
V = 1587.1 (6) Å3 | 0.38 × 0.33 × 0.25 mm |
Z = 4 |
Bruker AXS SMART 1000 diffractometer | 1533 independent reflections |
Radiation source: fine-focus sealed tube | 1288 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
ω–scanning | θmax = 30.1°, θmin = 2.8° |
Absorption correction: semiempirical (using intensity measurements) | h = −9→4 |
k = −11→5 | |
3049 measured reflections | l = −39→15 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.057 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.141 | Hydrogen site location: inferred from neighbouring sites |
S = 0.88 | H-atom parameters not defined? |
1533 reflections | Calculated w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
103 parameters | (Δ/σ)max = 0.057 |
Experimental. omega-scanning, scanning pitch 0.3degree, frame measuring time 30 s. |
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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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) | |
S1 | 0.7771 (3) | −0.4456 (3) | 0.7500 | 0.0477 (6) | 0.771 (4) |
S2 | 0.34671 (12) | 0.36754 (10) | 0.55491 (3) | 0.02360 (19) | |
S3 | 0.77278 (12) | 0.42920 (11) | 0.53610 (3) | 0.0264 (2) | |
S4 | 0.41971 (13) | 0.17472 (11) | 0.63959 (3) | 0.0264 (2) | |
S5 | 0.92725 (13) | 0.23599 (14) | 0.61279 (4) | 0.0428 (3) | |
N1 | 0.914 (4) | −0.1034 (14) | 0.7500 | 0.340 (13) | 0.808 (18) |
C1 | 0.847 (2) | −0.223 (3) | 0.7500 | 0.170 (9) | 0.70 (2) |
C2 | 0.5205 (5) | 0.2779 (4) | 0.59233 (11) | 0.0202 (7) | |
C3 | 0.7175 (5) | 0.3036 (4) | 0.58273 (11) | 0.0236 (8) | |
C4 | 0.5246 (5) | 0.4563 (3) | 0.51915 (11) | 0.0210 (7) | |
C5 | 0.8215 (6) | 0.1316 (6) | 0.66082 (13) | 0.0537 (14) | |
H5A | 0.9187 | 0.1287 | 0.6855 | 0.080* | |
H5B | 0.8003 | 0.0228 | 0.6507 | 0.080* | |
C6 | 0.6304 (6) | 0.1811 (6) | 0.67913 (15) | 0.0543 (14) | |
H6A | 0.5975 | 0.1215 | 0.7067 | 0.080* | |
H6B | 0.6494 | 0.2914 | 0.6880 | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
S1 | 0.0408 (11) | 0.0694 (15) | 0.0330 (9) | 0.0030 (11) | 0.000 | 0.000 |
S2 | 0.0148 (4) | 0.0327 (4) | 0.0233 (3) | 0.0004 (4) | −0.0009 (3) | 0.0017 (4) |
S3 | 0.0136 (3) | 0.0358 (4) | 0.0298 (4) | −0.0031 (4) | −0.0037 (3) | 0.0072 (4) |
S4 | 0.0165 (4) | 0.0368 (5) | 0.0259 (4) | −0.0014 (4) | −0.0007 (3) | 0.0053 (4) |
S5 | 0.0141 (4) | 0.0638 (7) | 0.0504 (6) | 0.0015 (5) | −0.0029 (4) | 0.0295 (5) |
N1 | 0.86 (4) | 0.131 (8) | 0.031 (5) | 0.253 (13) | 0.000 | 0.000 |
C1 | 0.127 (10) | 0.37 (3) | 0.016 (5) | 0.149 (12) | 0.000 | 0.000 |
C2 | 0.0171 (14) | 0.0224 (15) | 0.0211 (14) | 0.0028 (14) | −0.0004 (12) | 0.0012 (13) |
C3 | 0.0168 (14) | 0.0262 (16) | 0.0278 (15) | 0.0003 (14) | −0.0032 (13) | 0.0045 (14) |
C4 | 0.0147 (14) | 0.0187 (16) | 0.0296 (15) | −0.0016 (13) | −0.0009 (13) | −0.0005 (13) |
C5 | 0.030 (2) | 0.102 (4) | 0.0286 (18) | 0.013 (2) | −0.0003 (16) | 0.020 (2) |
C6 | 0.0226 (19) | 0.099 (4) | 0.041 (2) | −0.010 (2) | −0.0115 (17) | 0.013 (3) |
S1—C1 | 1.91 (2) | S5—C3 | 1.733 (3) |
S2—C4 | 1.731 (3) | S5—C5 | 1.776 (4) |
S2—C2 | 1.745 (3) | N1—C1 | 1.09 (3) |
S3—C4 | 1.733 (3) | C2—C3 | 1.354 (5) |
S3—C3 | 1.739 (3) | C4—C4i | 1.360 (6) |
S4—C2 | 1.741 (3) | C5—C6 | 1.434 (6) |
S4—C6 | 1.804 (4) | ||
C4—S2—C2 | 95.60 (15) | C2—C3—S5 | 128.6 (3) |
C4—S3—C3 | 95.41 (15) | C2—C3—S3 | 117.1 (2) |
C2—S4—C6 | 100.42 (18) | S5—C3—S3 | 114.20 (18) |
C3—S5—C5 | 103.25 (17) | C4i—C4—S2 | 123.1 (3) |
N1—C1—S1 | 170.19 (17) | C4i—C4—S3 | 121.7 (3) |
C3—C2—S4 | 127.5 (3) | S2—C4—S3 | 115.20 (17) |
C3—C2—S2 | 116.5 (2) | C6—C5—S5 | 119.5 (3) |
S4—C2—S2 | 115.98 (18) | C5—C6—S4 | 116.5 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |