Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768199016560/cf0010sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768199016560/cf0010tdasbtsup2.hkl |
CCDC reference: 117020
Data collection: EXPOSE (Stoe IPDS); cell refinement: SELECT (Stoe IPDS); data reduction: INTEGRATE (Stoe IPDS); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
C504N24S36 | Dx = 1.870 Mg m−3 |
Mr = 7543.44 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, I23 | Cell parameters from 5000 reflections |
Hall symbol: I 2 2 3 | θ = 1.5–25.2° |
a = 18.8492 (10) Å | µ = 0.38 mm−1 |
V = 6697.0 (6) Å3 | T = 100 K |
Z = 1 | Plate-like, black |
F(000) = 3768 | 0.37 × 0.27 × 0.23 mm |
Stoe IPDS diffractometer | 1764 independent reflections |
Radiation source: fine-focus sealed tube | 1243 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
Detector resolution: 6.66 pixels mm-1 | θmax = 25.2°, θmin = 2.2° |
Rotation, Δϕ=1.2° scans | h = −14→14 |
Absorption correction: part of the refinement model (ΔF) ABSCOR (Stoe, IPDS) | k = 0→15 |
Tmin = 0.871, Tmax = 0.916 | l = 2→21 |
12851 measured 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)] = 0.046 | Calculated w = 1/[σ2(Fo2) + (0.1321P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.116 | (Δ/σ)max = 0.001 |
S = 0.56 | Δρmax = 0.46 e Å−3 |
1764 reflections | Δρmin = −0.22 e Å−3 |
213 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
0 restraints | Absolute structure parameter: −0.04 (15) |
C504N24S36 | Z = 1 |
Mr = 7543.44 | Mo Kα radiation |
Cubic, I23 | µ = 0.38 mm−1 |
a = 18.8492 (10) Å | T = 100 K |
V = 6697.0 (6) Å3 | 0.37 × 0.27 × 0.23 mm |
Stoe IPDS diffractometer | 1764 independent reflections |
Absorption correction: part of the refinement model (ΔF) ABSCOR (Stoe, IPDS) | 1243 reflections with I > 2σ(I) |
Tmin = 0.871, Tmax = 0.916 | Rint = 0.014 |
12851 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.116 | Δρmax = 0.46 e Å−3 |
S = 0.56 | Δρmin = −0.22 e Å−3 |
1764 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
213 parameters | Absolute structure parameter: −0.04 (15) |
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 | ||
S1 | 1.0000 | 0.5000 | 0.77492 (8) | 0.0218 (4) | |
S2 | 0.91245 (6) | 0.45675 (7) | 0.96721 (6) | 0.0299 (4) | |
N1 | 1.0595 (2) | 0.5267 (2) | 0.8308 (2) | 0.0241 (9) | |
C1 | 0.9651 (2) | 0.4843 (2) | 0.8958 (2) | 0.0158 (9) | |
C2 | 0.8494 (3) | 0.9308 (3) | 0.9509 (3) | 0.051 (2) | |
C3 | 0.8678 (4) | 0.9719 (3) | 0.8913 (4) | 0.056 (2) | |
C4 | 0.7768 (3) | 0.9162 (3) | 0.9632 (3) | 0.0373 (14) | |
C5 | 0.8135 (4) | 0.9972 (3) | 0.8409 (4) | 0.053 (2) | |
C6 | 0.7680 (3) | 0.8441 (3) | 0.9913 (3) | 0.043 (2) | |
C7 | 0.7455 (5) | 0.9824 (3) | 0.8520 (4) | 0.063 (2) | |
C8 | 0.7237 (3) | 0.9421 (3) | 0.9154 (3) | 0.0350 (14) | |
C9 | 0.7122 (4) | 0.8044 (3) | 0.9702 (3) | 0.046 (2) | |
C10 | 0.6994 (3) | 0.9602 (3) | 0.7898 (4) | 0.044 (2) | |
C11 | 0.6672 (3) | 0.8984 (3) | 0.8951 (3) | 0.044 (2) | |
C12 | 1.1622 (3) | 0.6678 (4) | 0.5778 (3) | 0.045 (2) | |
C13 | 0.7281 (3) | 0.9549 (3) | 0.7254 (3) | 0.0421 (15) | |
C14 | 0.6515 (3) | 0.9095 (4) | 0.8185 (3) | 0.043 (2) | |
C15 | 0.7087 (3) | 0.8981 (3) | 0.6810 (3) | 0.0363 (15) | |
C16 | 0.7710 (4) | 0.8757 (4) | 0.6412 (3) | 0.053 (2) | |
C17 | 0.6324 (3) | 0.8535 (4) | 0.7775 (4) | 0.047 (2) | |
C18 | 0.6605 (3) | 0.8484 (3) | 0.7074 (3) | 0.0341 (14) | |
C19 | 0.6267 (3) | 0.7815 (4) | 0.8078 (5) | 0.059 (2) | |
C20 | 0.7304 (4) | 0.7546 (4) | 0.6533 (3) | 0.056 (2) | |
C21 | 0.6719 (4) | 0.7733 (4) | 0.6919 (4) | 0.050 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
S1 | 0.0260 (9) | 0.0242 (9) | 0.0150 (8) | 0.0032 (8) | 0.000 | 0.000 |
S2 | 0.0203 (7) | 0.0497 (9) | 0.0195 (7) | −0.0168 (6) | −0.0004 (5) | 0.0062 (6) |
N1 | 0.025 (2) | 0.030 (2) | 0.018 (2) | −0.005 (2) | 0.005 (2) | −0.002 (2) |
C1 | 0.016 (2) | 0.016 (2) | 0.015 (2) | −0.001 (2) | −0.002 (2) | 0.001 (2) |
C2 | 0.058 (4) | 0.050 (4) | 0.043 (4) | −0.005 (3) | −0.005 (3) | −0.037 (3) |
C3 | 0.082 (5) | 0.030 (3) | 0.055 (4) | −0.035 (3) | 0.009 (4) | −0.032 (3) |
C4 | 0.038 (3) | 0.048 (3) | 0.026 (3) | 0.000 (3) | 0.009 (3) | −0.029 (3) |
C5 | 0.079 (5) | 0.016 (3) | 0.065 (4) | −0.006 (3) | 0.013 (4) | −0.010 (3) |
C6 | 0.063 (4) | 0.054 (4) | 0.011 (3) | 0.022 (3) | 0.015 (3) | −0.004 (3) |
C7 | 0.111 (7) | 0.019 (4) | 0.058 (4) | 0.042 (4) | 0.010 (4) | −0.003 (3) |
C8 | 0.050 (4) | 0.026 (3) | 0.029 (3) | 0.021 (3) | 0.012 (3) | −0.013 (2) |
C9 | 0.064 (4) | 0.049 (4) | 0.024 (3) | −0.008 (3) | 0.030 (3) | 0.000 (3) |
C10 | 0.042 (4) | 0.021 (3) | 0.068 (5) | 0.019 (3) | −0.011 (3) | −0.001 (3) |
C11 | 0.029 (3) | 0.062 (4) | 0.040 (4) | 0.023 (3) | 0.008 (3) | −0.019 (3) |
C12 | 0.035 (4) | 0.061 (4) | 0.039 (4) | −0.010 (3) | −0.025 (3) | 0.002 (3) |
C13 | 0.043 (3) | 0.029 (3) | 0.054 (4) | 0.007 (3) | −0.009 (3) | 0.017 (3) |
C14 | 0.025 (3) | 0.053 (4) | 0.050 (4) | 0.027 (3) | 0.002 (3) | 0.006 (3) |
C15 | 0.031 (3) | 0.050 (4) | 0.028 (3) | 0.014 (3) | −0.007 (2) | 0.020 (3) |
C16 | 0.044 (4) | 0.091 (6) | 0.023 (3) | 0.018 (4) | −0.005 (3) | 0.023 (4) |
C17 | 0.018 (3) | 0.060 (5) | 0.062 (4) | 0.015 (3) | −0.001 (3) | 0.031 (4) |
C18 | 0.023 (3) | 0.033 (3) | 0.047 (4) | 0.008 (2) | −0.024 (3) | −0.001 (3) |
C19 | 0.015 (3) | 0.064 (5) | 0.098 (6) | −0.010 (3) | 0.001 (3) | 0.022 (5) |
C20 | 0.050 (4) | 0.090 (6) | 0.028 (3) | 0.011 (4) | −0.024 (3) | −0.032 (3) |
C21 | 0.047 (4) | 0.050 (4) | 0.052 (4) | −0.009 (4) | −0.030 (3) | −0.010 (3) |
S1—N1i | 1.619 (4) | C10—C13 | 1.333 (9) |
S1—N1 | 1.619 (4) | C10—C14 | 1.421 (9) |
S2—C1 | 1.752 (4) | C11—C12v | 1.353 (8) |
S2—S2ii | 2.046 (3) | C11—C14 | 1.489 (9) |
N1—C1i | 1.326 (5) | C12—C11vi | 1.353 (8) |
C1—N1i | 1.327 (5) | C12—C9vi | 1.407 (9) |
C1—C1i | 1.442 (9) | C12—C16vii | 1.503 (10) |
C2—C3 | 1.409 (9) | C13—C15 | 1.407 (9) |
C2—C4 | 1.415 (8) | C13—C9iv | 1.488 (9) |
C2—C3iii | 1.479 (9) | C14—C17 | 1.356 (10) |
C3—C2iv | 1.479 (9) | C15—C18 | 1.396 (8) |
C3—C5 | 1.475 (10) | C15—C16 | 1.455 (9) |
C4—C8 | 1.431 (9) | C16—C19iv | 1.323 (10) |
C4—C6 | 1.470 (8) | C16—C12viii | 1.503 (10) |
C5—C7 | 1.329 (10) | C17—C18 | 1.426 (9) |
C5—C6iv | 1.493 (8) | C17—C19 | 1.476 (9) |
C6—C9 | 1.350 (9) | C18—C21 | 1.461 (9) |
C6—C5iii | 1.493 (9) | C19—C16iii | 1.323 (10) |
C7—C10 | 1.518 (10) | C19—C20iii | 1.479 (11) |
C7—C8 | 1.474 (9) | C20—C21 | 1.367 (10) |
C8—C11 | 1.400 (9) | C20—C21iv | 1.475 (10) |
C9—C12v | 1.407 (9) | C20—C19iv | 1.479 (11) |
C9—C13iii | 1.488 (9) | C21—C20iii | 1.475 (10) |
N1i—S1—N1 | 98.8 (3) | C12v—C11—C8 | 119.4 (6) |
C1—S2—S2ii | 103.2 (2) | C12v—C11—C14 | 118.9 (6) |
C1i—N1—S1 | 108.0 (3) | C8—C11—C14 | 109.6 (6) |
N1i—C1—C1i | 112.6 (3) | C11vi—C12—C9vi | 122.7 (6) |
N1i—C1—S2 | 117.7 (3) | C11vi—C12—C16vii | 120.4 (6) |
C1i—C1—S2 | 129.70 (14) | C9vi—C12—C16vii | 105.5 (6) |
C3—C2—C4 | 118.3 (6) | C10—C13—C15 | 119.6 (6) |
C3—C2—C3iii | 121.7 (7) | C10—C13—C9iv | 122.0 (6) |
C4—C2—C3iii | 108.5 (6) | C15—C13—C9iv | 107.4 (5) |
C2—C3—C2iv | 118.3 (7) | C17—C14—C10 | 118.3 (6) |
C2—C3—C5 | 121.4 (6) | C17—C14—C11 | 119.7 (6) |
C2iv—C3—C5 | 107.4 (6) | C10—C14—C11 | 109.6 (6) |
C8—C4—C2 | 120.6 (6) | C18—C15—C13 | 117.8 (5) |
C8—C4—C6 | 117.6 (5) | C18—C15—C16 | 121.0 (6) |
C2—C4—C6 | 110.3 (5) | C13—C15—C16 | 108.6 (6) |
C7—C5—C3 | 120.0 (6) | C19iv—C16—C15 | 120.5 (7) |
C7—C5—C6iv | 120.2 (7) | C19iv—C16—C12viii | 120.2 (6) |
C3—C5—C6iv | 107.5 (6) | C15—C16—C12viii | 108.3 (6) |
C9—C6—C4 | 119.6 (6) | C14—C17—C18 | 118.8 (5) |
C9—C6—C5iii | 121.6 (6) | C14—C17—C19 | 120.9 (6) |
C4—C6—C5iii | 106.3 (6) | C18—C17—C19 | 108.9 (6) |
C5—C7—C10 | 119.1 (6) | C15—C18—C17 | 121.8 (5) |
C5—C7—C8 | 120.3 (7) | C15—C18—C21 | 118.8 (5) |
C10—C7—C8 | 109.0 (7) | C17—C18—C21 | 107.8 (6) |
C11—C8—C4 | 120.3 (5) | C16iii—C19—C20iii | 119.2 (6) |
C11—C8—C7 | 107.0 (6) | C16iii—C19—C17 | 119.8 (7) |
C4—C8—C7 | 119.4 (6) | C20iii—C19—C17 | 108.2 (7) |
C6—C9—C12v | 120.3 (6) | C21—C20—C21iv | 121.6 (8) |
C6—C9—C13iii | 117.5 (6) | C21—C20—C19iv | 122.1 (7) |
C12v—C9—C13iii | 110.3 (6) | C21iv—C20—C19iv | 105.4 (6) |
C13—C10—C14 | 123.6 (6) | C20—C21—C20iii | 118.3 (8) |
C13—C10—C7 | 119.5 (6) | C20—C21—C18 | 118.4 (6) |
C14—C10—C7 | 104.8 (6) | C20iii—C21—C18 | 109.7 (7) |
Symmetry codes: (i) −x+2, −y+1, z; (ii) x, −y+1, −z+2; (iii) z, x, y; (iv) y, z, x; (v) x−1/2, −y+3/2, −z+3/2; (vi) x+1/2, −y+3/2, −z+3/2; (vii) z+1/2, −x+3/2, −y+3/2; (viii) −y+3/2, −z+3/2, x−1/2. |
Experimental details
Crystal data | |
Chemical formula | C504N24S36 |
Mr | 7543.44 |
Crystal system, space group | Cubic, I23 |
Temperature (K) | 100 |
a (Å) | 18.8492 (10) |
V (Å3) | 6697.0 (6) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.38 |
Crystal size (mm) | 0.37 × 0.27 × 0.23 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Part of the refinement model (ΔF) ABSCOR (Stoe, IPDS) |
Tmin, Tmax | 0.871, 0.916 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12851, 1764, 1243 |
Rint | 0.014 |
(sin θ/λ)max (Å−1) | 0.598 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.116, 0.56 |
No. of reflections | 1764 |
No. of parameters | 213 |
Δρmax, Δρmin (e Å−3) | 0.46, −0.22 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | −0.04 (15) |
Computer programs: EXPOSE (Stoe IPDS), SELECT (Stoe IPDS), INTEGRATE (Stoe IPDS), SHELXS86 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP (Johnson, 1976).
S1—N1i | 1.619 (4) | C10—C13 | 1.333 (9) |
S1—N1 | 1.619 (4) | C10—C14 | 1.421 (9) |
S2—C1 | 1.752 (4) | C11—C12v | 1.353 (8) |
S2—S2ii | 2.046 (3) | C11—C14 | 1.489 (9) |
N1—C1i | 1.326 (5) | C12—C11vi | 1.353 (8) |
C1—N1i | 1.327 (5) | C12—C9vi | 1.407 (9) |
C1—C1i | 1.442 (9) | C12—C16vii | 1.503 (10) |
C2—C3 | 1.409 (9) | C13—C15 | 1.407 (9) |
C2—C4 | 1.415 (8) | C13—C9iv | 1.488 (9) |
C2—C3iii | 1.479 (9) | C14—C17 | 1.356 (10) |
C3—C2iv | 1.479 (9) | C15—C18 | 1.396 (8) |
C3—C5 | 1.475 (10) | C15—C16 | 1.455 (9) |
C4—C8 | 1.431 (9) | C16—C19iv | 1.323 (10) |
C4—C6 | 1.470 (8) | C16—C12viii | 1.503 (10) |
C5—C7 | 1.329 (10) | C17—C18 | 1.426 (9) |
C5—C6iv | 1.493 (8) | C17—C19 | 1.476 (9) |
C6—C9 | 1.350 (9) | C18—C21 | 1.461 (9) |
C6—C5iii | 1.493 (9) | C19—C16iii | 1.323 (10) |
C7—C10 | 1.518 (10) | C19—C20iii | 1.479 (11) |
C7—C8 | 1.474 (9) | C20—C21 | 1.367 (10) |
C8—C11 | 1.400 (9) | C20—C21iv | 1.475 (10) |
C9—C12v | 1.407 (9) | C20—C19iv | 1.479 (11) |
C9—C13iii | 1.488 (9) | C21—C20iii | 1.475 (10) |
Symmetry codes: (i) −x+2, −y+1, z; (ii) x, −y+1, −z+2; (iii) z, x, y; (iv) y, z, x; (v) x−1/2, −y+3/2, −z+3/2; (vi) x+1/2, −y+3/2, −z+3/2; (vii) z+1/2, −x+3/2, −y+3/2; (viii) −y+3/2, −z+3/2, x−1/2. |