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In the title complex, [Cr(C2H3OS2)3], the Cr atom is coordinated by six S atoms in a distorted octahedral arrangement. The six Cr-S bond distances are in the range 2.391 (1)-2.406 (1) Å, with an average of 2.397 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802015775/ci6156sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802015775/ci6156Isup2.hkl
Contains datablock I

CCDC reference: 198292

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](O-C) = 0.005 Å
  • R factor = 0.033
  • wR factor = 0.022
  • Data-to-parameter ratio = 14.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ABSTM_02 Alert A Test not performed as the _exptl_absorpt_correction_type has not been identified. See test ABSTY_01. ABSTY_01 Alert A The absorption correction should be one of the following * none * analytical * integration * numerical * gaussian * empirical * psi-scan * multi-scan * refdelf * sphere * cylinder
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Comment top

As part of the study of metal xanthates and dialkyl dithiophosphates (Ito, 2002a,b), the crystal and molecular structure of the title complex, (I), has been determined. A displacement ellipsoid plot of (I) is shown in Fig.1. The average Cr—S distance of 2.397 (2) Å is 0.032 (7) Å shorter than that in tris(O,O'-dimethyldithiophosphato)chromium(III), (II), (Ito, 2002b), which shows that the Cr—S bonds in (I) are stronger than those in (II). On the other hand, distortions of S atoms around the Cr atom from the octahedral coordination in (I) are larger than those in (II). For example, average S—Cr—S chelate angles in (I) and (II) are 74.5 (2)° and 81.8°, respectively.

The structures of xanthic ligands in (I) are very similar to those in iron methylxanthate, (III), (Ito, 2002a). Average S—C, S2C—O and O—CH3 bond distances of 1.688 (4), 1.318 (4) and 1.446 (4) Å, respectively, are in agreement with the corresponding distances in (III) within standard uncertainties.

Experimental top

Potassium methylxanthate (2.0 g) and hexaaquachromium(III) chloride (4.0 g) were each dissolved in pure water (40 ml and 80 ml, respectively), and powder of (I) was precipitated by combining the two solutions. Recrystallization from an ether solution at room temperature gave dark-blue plate-shaped crystals of (I).

Refinement top

H atoms were placed in geometrically calculated positions and allowed to ride on their parent atoms, with Uiso parameters equal to 1.2 times the Ueq parameters of their parent atoms.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: CrystalStructure (Molecular Structure Corporation and Rigaku Corporation, 2001); 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.

Figures top
[Figure 1] Fig. 1. ORTEPIII (Burnett & Johnson, 1996) drawing of the title chromium methylxanthate complex. Displacement ellipsoids are drawn at the 50% probability level.
(I) top
Crystal data top
[Cr(C2H3OS2)3]F(000) = 756
Mr = 373.55Dx = 1.720 Mg m3
Dm = 1.715 Mg m3
Dm measured by flotation in zinc iodide (aq)
Monoclinic, P21/nMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ynCell parameters from 23 reflections
a = 9.633 (4) Åθ = 15.2–16.3°
b = 13.852 (4) ŵ = 1.65 mm1
c = 11.301 (3) ÅT = 296 K
β = 106.94 (2)°Plate, dark blue
V = 1442.5 (8) Å30.45 × 0.35 × 0.10 mm
Z = 4
Data collection top
Rigaku AFC-5S
diffractometer
Rint = 0.029
ω–2θ scansθmax = 27.5°
Absorption correction: ψ
(North, Phillips & Mathews, 1968)
h = 012
Tmin = 0.510, Tmax = 0.848k = 017
3640 measured reflectionsl = 1414
3311 independent reflections3 standard reflections every 150 reflections
2041 reflections with I > 3σ(I) intensity decay: 0.1%
Refinement top
Refinement on FH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.033Weighting scheme based on measured s.u.'s w = 1/σ2(Fo)
wR(F2) = 0.022(Δ/σ)max < 0.001
S = 1.66Δρmax = 0.26 e Å3
2041 reflectionsΔρmin = 0.29 e Å3
145 parameters
Crystal data top
[Cr(C2H3OS2)3]V = 1442.5 (8) Å3
Mr = 373.55Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.633 (4) ŵ = 1.65 mm1
b = 13.852 (4) ÅT = 296 K
c = 11.301 (3) Å0.45 × 0.35 × 0.10 mm
β = 106.94 (2)°
Data collection top
Rigaku AFC-5S
diffractometer
2041 reflections with I > 3σ(I)
Absorption correction: ψ
(North, Phillips & Mathews, 1968)
Rint = 0.029
Tmin = 0.510, Tmax = 0.8483 standard reflections every 150 reflections
3640 measured reflections intensity decay: 0.1%
3311 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.033145 parameters
wR(F2) = 0.022H-atom parameters constrained
S = 1.66Δρmax = 0.26 e Å3
2041 reflectionsΔρmin = 0.29 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cr0.67719 (6)0.48456 (4)0.26848 (6)0.0396 (2)
S10.9122 (1)0.56029 (8)0.3246 (1)0.0481 (3)
S20.8025 (1)0.41613 (8)0.1341 (1)0.0517 (3)
S30.7465 (1)0.36479 (8)0.4272 (1)0.0514 (3)
S40.4827 (1)0.37002 (8)0.2228 (1)0.0539 (3)
S50.5738 (1)0.59631 (8)0.3819 (1)0.0515 (3)
S60.5521 (1)0.60248 (7)0.1208 (1)0.0490 (3)
O11.0596 (3)0.4870 (2)0.1784 (2)0.057 (1)
O20.5307 (3)0.2378 (2)0.3902 (3)0.057 (1)
O30.4285 (3)0.7281 (2)0.2368 (3)0.060 (1)
C10.9391 (4)0.4892 (3)0.2119 (4)0.043 (1)
C20.5844 (4)0.3159 (3)0.3537 (4)0.044 (1)
C30.5103 (4)0.6512 (3)0.2419 (4)0.044 (1)
C41.1805 (4)0.5471 (3)0.2428 (4)0.070 (2)
C50.6188 (5)0.1880 (3)0.4984 (4)0.073 (2)
C60.3702 (5)0.7760 (3)0.1188 (4)0.078 (2)
H11.25790.53890.20740.085*
H21.21180.52850.32740.085*
H31.15160.61290.23670.085*
H40.56820.13420.51780.092*
H50.64290.23160.56620.092*
H60.70520.16630.48240.092*
H70.31100.82910.12650.087*
H80.44930.79850.09210.087*
H90.31430.73160.06000.087*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr0.0312 (3)0.0473 (4)0.0404 (4)0.0037 (3)0.0103 (3)0.0043 (3)
S10.0384 (6)0.0572 (7)0.0502 (7)0.0109 (5)0.0151 (5)0.0180 (6)
S20.0403 (6)0.0599 (7)0.0554 (7)0.0085 (5)0.0149 (5)0.0232 (6)
S30.0389 (6)0.0621 (8)0.0476 (7)0.0027 (5)0.0037 (5)0.0047 (6)
S40.0370 (6)0.0624 (8)0.0544 (7)0.0118 (5)0.0009 (5)0.0034 (6)
S50.0457 (6)0.0688 (8)0.0421 (7)0.0035 (6)0.0160 (5)0.0085 (6)
S60.0501 (7)0.0571 (7)0.0412 (6)0.0017 (6)0.0152 (5)0.0010 (6)
O10.038 (2)0.068 (2)0.074 (2)0.008 (2)0.027 (2)0.022 (2)
O20.062 (2)0.054 (2)0.060 (2)0.010 (2)0.026 (2)0.003 (2)
O30.054 (2)0.056 (2)0.065 (2)0.012 (2)0.010 (2)0.011 (2)
C10.034 (2)0.047 (2)0.049 (3)0.000 (2)0.013 (2)0.001 (2)
C20.041 (2)0.048 (3)0.050 (3)0.000 (2)0.023 (2)0.005 (2)
C30.032 (2)0.048 (3)0.052 (3)0.008 (2)0.010 (2)0.008 (2)
C40.031 (2)0.080 (3)0.101 (4)0.014 (2)0.024 (2)0.020 (3)
C50.104 (4)0.062 (3)0.063 (3)0.007 (3)0.041 (3)0.014 (3)
C60.078 (4)0.053 (3)0.086 (4)0.014 (3)0.003 (3)0.001 (3)
Geometric parameters (Å, º) top
Cr—S12.406 (1)O2—C21.316 (4)
Cr—S22.394 (1)O2—C51.445 (4)
Cr—S32.391 (1)O3—C31.317 (4)
Cr—S42.394 (1)O3—C61.448 (4)
Cr—S52.403 (1)C4—H10.95
Cr—S62.394 (1)C4—H20.95
S1—C11.688 (4)C4—H30.95
S2—C11.690 (4)C5—H40.95
S3—C21.682 (4)C5—H50.95
S4—C21.693 (4)C5—H60.95
S5—C31.700 (4)C6—H70.95
S6—C31.676 (4)C6—H80.95
O1—C11.322 (4)C6—H90.95
O1—C41.444 (4)
O1···C5i3.563 (5)O3···C5v3.363 (5)
O1···C5ii3.318 (5)C1···C5i3.573 (5)
O2···C4iii3.405 (5)C3···C4iv3.491 (5)
O3···C4iv3.478 (4)
S1—Cr—S274.35 (4)S2—C1—O1116.9 (3)
S1—Cr—S393.98 (5)S3—C2—S4118.1 (2)
S1—Cr—S4164.34 (5)S3—C2—O2124.7 (3)
S1—Cr—S594.76 (5)S4—C2—O2117.2 (3)
S1—Cr—S697.47 (5)S5—C3—S6118.2 (2)
S2—Cr—S396.85 (5)S5—C3—O3116.8 (3)
S2—Cr—S496.23 (5)S6—C3—O3124.9 (3)
S2—Cr—S5163.21 (5)O1—C4—H1109.6
S2—Cr—S694.15 (5)O1—C4—H2108.9
S3—Cr—S474.44 (4)H1—C4—H2109.5
S3—Cr—S596.62 (5)O1—C4—H3109.9
S3—Cr—S6165.89 (4)H1—C4—H3109.5
S4—Cr—S597.01 (5)H2—C4—H3109.5
S4—Cr—S695.64 (5)O2—C5—H4110.8
S5—Cr—S674.31 (4)O2—C5—H5108.9
Cr—S1—C183.5 (1)H4—C5—H5109.5
Cr—S2—C183.8 (1)O2—C5—H6108.7
Cr—S3—C283.9 (1)H4—C5—H6109.5
Cr—S4—C283.6 (1)H5—C5—H6109.5
Cr—S5—C383.4 (1)O3—C6—H7110.7
Cr—S6—C384.1 (1)O3—C6—H8108.1
C1—O1—C4119.3 (3)H7—C6—H8109.5
C2—O2—C5118.0 (3)O3—C6—H9109.6
C3—O3—C6118.6 (3)H7—C6—H9109.5
S1—C1—S2118.3 (2)H8—C6—H9109.5
S1—C1—O1124.8 (3)
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z1/2; (iii) x+3/2, y1/2, z+1/2; (iv) x1, y, z; (v) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Cr(C2H3OS2)3]
Mr373.55
Crystal system, space groupMonoclinic, P21/n
Temperature (K)296
a, b, c (Å)9.633 (4), 13.852 (4), 11.301 (3)
β (°) 106.94 (2)
V3)1442.5 (8)
Z4
Radiation typeMo Kα
µ (mm1)1.65
Crystal size (mm)0.45 × 0.35 × 0.10
Data collection
DiffractometerRigaku AFC-5S
diffractometer
Absorption correctionψ
(North, Phillips & Mathews, 1968)
Tmin, Tmax0.510, 0.848
No. of measured, independent and
observed [I > 3σ(I)] reflections
3640, 3311, 2041
Rint0.029
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.022, 1.66
No. of reflections2041
No. of parameters145
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.26, 0.29

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988), MSC/AFC Diffractometer Control Software, CrystalStructure (Molecular Structure Corporation and Rigaku Corporation, 2001), SIR92 (Altomare et al., 1994), CrystalStructure, ORTEPIII (Burnett & Johnson, 1996).

Selected geometric parameters (Å, º) top
Cr—S12.406 (1)S4—C21.693 (4)
Cr—S22.394 (1)S5—C31.700 (4)
Cr—S32.391 (1)S6—C31.676 (4)
Cr—S42.394 (1)O1—C11.322 (4)
Cr—S52.403 (1)O1—C41.444 (4)
Cr—S62.394 (1)O2—C21.316 (4)
S1—C11.688 (4)O2—C51.445 (4)
S2—C11.690 (4)O3—C31.317 (4)
S3—C21.682 (4)O3—C61.448 (4)
S1—Cr—S274.35 (4)S2—Cr—S694.15 (5)
S1—Cr—S393.98 (5)S3—Cr—S474.44 (4)
S1—Cr—S4164.34 (5)S3—Cr—S596.62 (5)
S1—Cr—S594.76 (5)S3—Cr—S6165.89 (4)
S1—Cr—S697.47 (5)S4—Cr—S597.01 (5)
S2—Cr—S396.85 (5)S4—Cr—S695.64 (5)
S2—Cr—S496.23 (5)S5—Cr—S674.31 (4)
S2—Cr—S5163.21 (5)
 

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