Tris­(O,O′-di­methyl di­thio­phosphato-κ²S,S′)­arsenic(III)

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)°.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](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

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Computing details

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.

(I)

Crystal data

[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) Å^3

Data collection

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

Refinement on F	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.029	Weighting scheme based on measured s.u.'s w = 1/σ^2(Fo)
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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···O6^i	3.224 (3)	O2···C6^ii	3.452 (5)
O1···O6^ii	3.515 (3)	O3···C2^iv	3.297 (4)
O1···C1^iii	3.415 (4)	O3···C3^v	3.235 (4)
O1···C6^ii	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.