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The As atom in the title complex molecule, [As(C2H6O2PS2)3], is surrounded by six S atoms in a distorted octahedral arrangement. Three of the six S atoms are bonded to the As atom with an average bond distance of 2.315 (6) Å, while the other three S atoms have only secondary bonding interactions to the As atom with an average interatomic distance of 3.031 (4) Å. The three As—S bonds form a trigonal pyramid with an average apex angle of 92.2 (3)°.
Supporting information
CCDC reference: 242044
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (O-C) = 0.004 Å
- R factor = 0.029
- wR factor = 0.031
- Data-to-parameter ratio = 18.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.68 mm
PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... ?
PLAT156_ALERT_4_C Axial System Input Cell not Standard ........... ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CrystalStructure; molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: CrystalStructure.
Crystal data top
[As(C2H6O2PS2)3] | Z = 2 |
Mr = 546.45 | F(000) = 552.00 |
Triclinic, P1 | Dx = 1.678 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.7107 Å |
a = 9.091 (4) Å | Cell parameters from 25 reflections |
b = 14.789 (6) Å | θ = 22.3–23.4° |
c = 8.396 (3) Å | µ = 2.39 mm−1 |
α = 103.52 (3)° | T = 296 K |
β = 93.65 (3)° | Plate, colorless |
γ = 80.41 (4)° | 0.68 × 0.35 × 0.20 mm |
V = 1081.8 (8) Å3 | |
Data collection top
Rigaku AFC-5S diffractometer | Rint = 0.009 |
ω–2θ scans | θmax = 27.5° |
Absorption correction: ψ scan (North et al., 1968) | h = 0→11 |
Tmin = 0.381, Tmax = 0.620 | k = −18→19 |
5277 measured reflections | l = −10→10 |
4966 independent reflections | 3 standard reflections every 150 reflections |
3686 reflections with I > 3σ(I) | intensity decay: 0.5% |
Refinement top
Refinement on F | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.029 | Weighting scheme based on measured s.u.'s w = 1/σ2(Fo) |
wR(F2) = 0.031 | (Δ/σ)max < 0.001 |
S = 1.54 | Δρmax = 0.36 e Å−3 |
3686 reflections | Δρmin = −0.31 e Å−3 |
199 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
As | 0.20623 (3) | 0.26410 (2) | 0.50713 (4) | 0.04123 (8) | |
S1 | 0.4578 (1) | 0.20272 (5) | 0.4821 (1) | 0.0493 (2) | |
S2 | 0.2374 (1) | 0.33240 (6) | 0.7832 (1) | 0.0550 (2) | |
S3 | 0.1521 (1) | 0.12757 (5) | 0.5608 (1) | 0.0578 (2) | |
S4 | 0.2450 (1) | 0.18016 (7) | 0.1441 (1) | 0.0691 (3) | |
S5 | 0.2625 (1) | 0.46223 (6) | 0.5163 (1) | 0.0571 (2) | |
S6 | −0.1309 (1) | 0.29170 (6) | 0.5100 (1) | 0.0710 (3) | |
P1 | 0.4463 (1) | 0.15707 (6) | 0.2312 (1) | 0.0494 (2) | |
P2 | 0.2757 (1) | 0.45913 (5) | 0.7445 (1) | 0.0454 (2) | |
P3 | −0.0765 (1) | 0.16514 (6) | 0.5423 (1) | 0.0568 (3) | |
O1 | 0.5284 (2) | 0.0526 (1) | 0.1885 (3) | 0.0640 (7) | |
O2 | 0.5661 (2) | 0.2009 (1) | 0.1586 (3) | 0.0628 (7) | |
O3 | 0.4262 (2) | 0.4801 (1) | 0.8372 (3) | 0.0618 (7) | |
O4 | 0.1707 (2) | 0.5390 (1) | 0.8628 (3) | 0.0625 (7) | |
O5 | −0.1442 (3) | 0.1435 (2) | 0.6941 (3) | 0.0785 (9) | |
O6 | −0.1365 (3) | 0.0844 (2) | 0.4117 (3) | 0.0699 (8) | |
C1 | 0.4633 (5) | −0.0210 (2) | 0.2271 (5) | 0.085 (1) | |
C2 | 0.5470 (4) | 0.3017 (2) | 0.1732 (5) | 0.078 (1) | |
C3 | 0.5661 (3) | 0.4267 (3) | 0.7740 (4) | 0.069 (1) | |
C4 | 0.0149 (4) | 0.5605 (3) | 0.8187 (5) | 0.084 (1) | |
C5 | −0.1265 (5) | 0.2012 (3) | 0.8547 (5) | 0.111 (2) | |
C6 | −0.1009 (4) | 0.0680 (3) | 0.2424 (5) | 0.084 (1) | |
H1 | 0.4517 | −0.0080 | 0.3423 | 0.102* | |
H2 | 0.3685 | −0.0237 | 0.1734 | 0.102* | |
H3 | 0.5262 | −0.0797 | 0.1928 | 0.102* | |
H4 | 0.5449 | 0.3325 | 0.2859 | 0.097* | |
H5 | 0.6281 | 0.3167 | 0.1237 | 0.097* | |
H6 | 0.4561 | 0.3221 | 0.1204 | 0.097* | |
H7 | 0.5666 | 0.3618 | 0.7688 | 0.082* | |
H8 | 0.5774 | 0.4354 | 0.6671 | 0.082* | |
H9 | 0.6462 | 0.4477 | 0.8433 | 0.081* | |
H10 | −0.0337 | 0.6096 | 0.9016 | 0.097* | |
H11 | 0.0064 | 0.5799 | 0.7179 | 0.097* | |
H12 | −0.0304 | 0.5058 | 0.8068 | 0.097* | |
H13 | −0.0232 | 0.1985 | 0.8829 | 0.135* | |
H14 | −0.1697 | 0.2645 | 0.8563 | 0.135* | |
H15 | −0.1746 | 0.1788 | 0.9316 | 0.135* | |
H16 | −0.1461 | 0.0171 | 0.1800 | 0.100* | |
H17 | −0.1361 | 0.1231 | 0.2027 | 0.100* | |
H18 | 0.0044 | 0.0531 | 0.2327 | 0.100* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
As | 0.0397 (2) | 0.0392 (2) | 0.0461 (2) | −0.0068 (1) | 0.0032 (1) | 0.0113 (1) |
S1 | 0.0401 (4) | 0.0587 (5) | 0.0458 (4) | −0.0050 (3) | 0.0004 (3) | 0.0071 (4) |
S2 | 0.0678 (5) | 0.0575 (5) | 0.0424 (4) | −0.0076 (4) | 0.0095 (4) | 0.0160 (4) |
S3 | 0.0470 (4) | 0.0438 (4) | 0.0887 (6) | −0.0062 (3) | 0.0021 (4) | 0.0279 (4) |
S4 | 0.0593 (5) | 0.0887 (7) | 0.0574 (6) | −0.0110 (5) | −0.0124 (4) | 0.0171 (5) |
S5 | 0.0765 (6) | 0.0532 (5) | 0.0463 (5) | −0.0148 (4) | −0.0024 (4) | 0.0182 (4) |
S6 | 0.0502 (5) | 0.0558 (5) | 0.1118 (8) | 0.0014 (4) | 0.0071 (5) | 0.0341 (5) |
P1 | 0.0487 (4) | 0.0508 (5) | 0.0463 (5) | −0.0064 (4) | 0.0055 (4) | 0.0058 (4) |
P2 | 0.0451 (4) | 0.0471 (4) | 0.0398 (4) | −0.0058 (3) | 0.0002 (3) | 0.0030 (3) |
P3 | 0.0461 (5) | 0.0534 (5) | 0.0787 (6) | −0.0118 (4) | 0.0056 (4) | 0.0265 (4) |
O1 | 0.070 (1) | 0.051 (1) | 0.065 (1) | −0.004 (1) | 0.010 (1) | 0.002 (1) |
O2 | 0.063 (1) | 0.062 (1) | 0.062 (1) | −0.011 (1) | 0.021 (1) | 0.007 (1) |
O3 | 0.046 (1) | 0.075 (1) | 0.054 (1) | −0.010 (1) | −0.004 (1) | −0.005 (1) |
O4 | 0.052 (1) | 0.063 (1) | 0.057 (1) | 0.003 (1) | 0.000 (1) | −0.007 (1) |
O5 | 0.069 (2) | 0.092 (2) | 0.088 (2) | −0.021 (1) | 0.016 (1) | 0.037 (2) |
O6 | 0.066 (1) | 0.067 (1) | 0.087 (2) | −0.030 (1) | −0.005 (1) | 0.025 (1) |
C1 | 0.124 (4) | 0.054 (2) | 0.076 (3) | −0.008 (2) | 0.011 (2) | 0.014 (2) |
C2 | 0.090 (3) | 0.069 (2) | 0.083 (3) | −0.018 (2) | 0.021 (2) | 0.023 (2) |
C3 | 0.047 (2) | 0.092 (3) | 0.064 (2) | −0.009 (2) | 0.003 (2) | 0.011 (2) |
C4 | 0.056 (2) | 0.100 (3) | 0.085 (3) | 0.014 (2) | 0.008 (2) | 0.014 (2) |
C5 | 0.117 (4) | 0.130 (4) | 0.090 (4) | −0.007 (3) | 0.023 (3) | 0.037 (3) |
C6 | 0.073 (3) | 0.079 (3) | 0.098 (3) | −0.016 (2) | −0.009 (2) | 0.019 (2) |
Geometric parameters (Å, º) top
As—S1 | 2.320 (1) | O4—C4 | 1.443 (4) |
As—S2 | 2.322 (1) | O5—C5 | 1.433 (5) |
As—S3 | 2.304 (1) | O6—C6 | 1.434 (4) |
As—S4 | 3.029 (1) | C1—H1 | 0.95 |
As—S5 | 3.040 (1) | C1—H2 | 0.95 |
As—S6 | 3.025 (1) | C1—H3 | 0.95 |
S1—P1 | 2.058 (1) | C2—H4 | 0.95 |
S2—P2 | 2.063 (1) | C2—H5 | 0.95 |
S3—P3 | 2.066 (1) | C2—H6 | 0.95 |
S4—P1 | 1.933 (1) | C3—H7 | 0.95 |
S5—P2 | 1.923 (1) | C3—H8 | 0.95 |
S6—P3 | 1.932 (1) | C3—H9 | 0.95 |
P1—O1 | 1.569 (2) | C4—H10 | 0.95 |
P1—O2 | 1.575 (2) | C4—H11 | 0.95 |
P2—O3 | 1.570 (2) | C4—H12 | 0.95 |
P2—O4 | 1.578 (2) | C5—H13 | 0.95 |
P3—O5 | 1.569 (2) | C5—H14 | 0.95 |
P3—O6 | 1.566 (2) | C5—H15 | 0.95 |
O1—C1 | 1.431 (4) | C6—H16 | 0.95 |
O2—C2 | 1.449 (4) | C6—H17 | 0.95 |
O3—C3 | 1.442 (4) | C6—H18 | 0.95 |
| | | |
S3···O6i | 3.224 (3) | O2···C6ii | 3.452 (5) |
O1···O6ii | 3.515 (3) | O3···C2iv | 3.297 (4) |
O1···C1iii | 3.415 (4) | O3···C3v | 3.235 (4) |
O1···C6ii | 3.410 (4) | | |
| | | |
S1—As—S2 | 92.18 (6) | H1—C1—H2 | 109.5 |
S1—As—S3 | 91.69 (6) | H1—C1—H3 | 109.5 |
S2—As—S3 | 92.79 (5) | H2—C1—H3 | 109.5 |
As—S1—P1 | 94.79 (6) | O2—C2—H4 | 109.0 |
As—S2—P2 | 94.82 (6) | O2—C2—H5 | 109.4 |
As—S3—P3 | 94.90 (6) | O2—C2—H6 | 110.0 |
S1—P1—S4 | 112.21 (6) | H4—C2—H5 | 109.5 |
S2—P2—S5 | 112.44 (6) | H4—C2—H6 | 109.5 |
S3—P3—S6 | 111.74 (6) | H5—C2—H6 | 109.5 |
S1—P1—O1 | 107.0 (1) | O3—C3—H7 | 109.6 |
S1—P1—O2 | 107.3 (1) | O3—C3—H8 | 109.0 |
S2—P2—O3 | 106.9 (1) | O3—C3—H9 | 109.8 |
S2—P2—O4 | 106.8 (1) | H7—C3—H8 | 109.5 |
S3—P3—O5 | 106.9 (1) | H7—C3—H9 | 109.5 |
S3—P3—O6 | 107.1 (1) | H8—C3—H9 | 109.5 |
S4—P1—O1 | 116.6 (1) | O4—C4—H10 | 110.0 |
S4—P1—O2 | 115.7 (1) | O4—C4—H11 | 109.3 |
S5—P2—O3 | 116.2 (1) | O4—C4—H12 | 109.2 |
S5—P2—O4 | 116.5 (1) | H10—C4—H11 | 109.5 |
S6—P3—O5 | 116.6 (1) | H10—C4—H12 | 109.5 |
S6—P3—O6 | 117.1 (1) | H11—C4—H12 | 109.5 |
O1—P1—O2 | 96.5 (1) | O5—C5—H13 | 109.3 |
O3—P2—O4 | 96.3 (1) | O5—C5—H14 | 109.7 |
O5—P3—O6 | 95.9 (1) | O5—C5—H15 | 109.4 |
P1—O1—C1 | 120.5 (2) | H13—C5—H14 | 109.5 |
P1—O2—C2 | 119.8 (2) | H13—C5—H15 | 109.5 |
P2—O3—C3 | 120.0 (2) | H14—C5—H15 | 109.5 |
P2—O4—C4 | 119.7 (2) | O6—C6—H16 | 109.9 |
P3—O5—C5 | 120.4 (3) | O6—C6—H17 | 109.7 |
P3—O6—C6 | 120.6 (2) | O6—C6—H18 | 108.8 |
O1—C1—H1 | 108.7 | H16—C6—H17 | 109.5 |
O1—C1—H2 | 109.6 | H16—C6—H18 | 109.5 |
O1—C1—H3 | 110.1 | H17—C6—H18 | 109.5 |
| | | |
As—S1—P1—S4 | −2.5 (1) | S2—As—S3—P3 | 97.8 (1) |
As—S2—P2—S5 | 1.7 (1) | S2—As—S1—P1 | −172.1 (1) |
As—S3—P3—S6 | −4.6 (1) | S3—As—S2—P2 | −177.2 (1) |
S3—As—S1—P1 | 95.1 (1) | S1—As—S3—P3 | −169.9 (1) |
S1—As—S2—P2 | 91.0 (1) | | |
Symmetry codes: (i) −x, −y, −z+1; (ii) x+1, y, z; (iii) −x+1, −y, −z; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+1, −z+2. |
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