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The title compound, [Co(C2H8N2)3]AsS4, was synthesized under solvothermal conditions in ethyl­enediamine (en) at 413 K. The compound consists of octa­hedral [Co(en)3]3+ cations and tetra­hedral AsS43− anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806039031/bi2068sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806039031/bi2068Isup2.hkl
Contains datablock I

CCDC reference: 620308

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.027
  • wR factor = 0.047
  • Data-to-parameter ratio = 24.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT411_ALERT_2_B Short Inter H...H Contact H2B .. H2B .. 2.07 Ang.
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N3 .. 5.01 su PLAT411_ALERT_2_C Short Inter H...H Contact H4B .. H6B .. 2.14 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4D ... ? PLAT420_ALERT_2_C D-H Without Acceptor N5 - H5C ... ?
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 29.10 From the CIF: _reflns_number_total 3981 Count of symmetry unique reflns 2217 Completeness (_total/calc) 179.57% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1764 Fraction of Friedel pairs measured 0.796 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Tris(ethylenediamine)cobalt(III) tetrathioarsenate top
Crystal data top
[Co(C2H8N2)3](AsS4)Dx = 1.857 Mg m3
Mr = 442.40Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42bcCell parameters from 4416 reflections
Hall symbol: P 4c -2abθ = 3.0–27.6°
a = 15.2781 (19) ŵ = 3.68 mm1
c = 13.559 (4) ÅT = 293 K
V = 3165.1 (10) Å3Block, orange
Z = 80.30 × 0.18 × 0.15 mm
F(000) = 1808
Data collection top
Bruker SMART APEXII CCD
diffractometer
3981 independent reflections
Radiation source: fine-focus sealed tube3343 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
φ and ω scansθmax = 29.1°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1720
Tmin = 0.384, Tmax = 0.576k = 2015
18629 measured reflectionsl = 1817
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.0093P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.007
3981 reflectionsΔρmax = 0.32 e Å3
163 parametersΔρmin = 0.42 e Å3
1 restraintAbsolute structure: Flack (1983), 1845 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.002 (7)
Special details top

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 of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
As10.443626 (18)0.744313 (17)0.43418 (2)0.01990 (7)
Co10.75511 (2)0.01805 (2)0.53001 (4)0.01823 (8)
S10.32953 (5)0.75961 (5)0.34060 (6)0.02945 (18)
S20.39538 (5)0.71727 (5)0.58207 (6)0.03019 (19)
S30.51915 (5)0.63814 (6)0.37062 (7)0.03091 (19)
S40.52010 (5)0.86241 (5)0.44181 (9)0.0387 (2)
N10.70976 (16)0.09913 (15)0.56034 (17)0.0253 (6)
H1A0.67060.11550.51430.030*
H1D0.75380.13830.56070.030*
N20.67381 (16)0.06016 (16)0.63210 (19)0.0284 (6)
H2A0.70410.07950.68470.034*
H2D0.64180.10490.60840.034*
N30.66889 (15)0.03688 (15)0.4251 (2)0.0263 (6)
H3A0.61580.01900.44570.032*
H3D0.66550.09440.41110.032*
N40.82892 (16)0.02735 (16)0.4225 (2)0.0261 (6)
H4A0.88300.00440.42730.031*
H4D0.83340.08590.42780.031*
N50.80314 (16)0.13692 (15)0.5150 (2)0.0270 (6)
H5A0.83260.14090.45770.032*
H5C0.75920.17620.51390.032*
N60.84943 (15)0.00060 (15)0.6260 (2)0.0233 (6)
H6A0.82710.00050.68740.028*
H6C0.87620.05090.61460.028*
C10.6676 (2)0.0959 (2)0.6585 (2)0.0363 (8)
H1B0.71160.09610.71010.044*
H1C0.62970.14620.66760.044*
C20.6151 (2)0.0127 (2)0.6621 (3)0.0362 (9)
H2B0.56560.01650.61760.043*
H2C0.59330.00280.72830.043*
C30.6936 (2)0.0118 (2)0.3357 (3)0.0331 (8)
H3B0.66500.01310.27830.040*
H3C0.67640.07270.34150.040*
C40.7911 (2)0.0047 (2)0.3257 (3)0.0346 (9)
H4B0.81210.04470.27550.042*
H4C0.80750.05440.30720.042*
C50.86258 (19)0.15600 (18)0.5983 (2)0.0268 (7)
H5B0.82930.17240.65640.032*
H5D0.90190.20360.58170.032*
C60.91361 (19)0.07308 (18)0.6172 (2)0.0253 (7)
H6D0.95360.06190.56310.030*
H6B0.94730.07850.67750.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.01777 (14)0.01977 (14)0.02216 (14)0.00053 (11)0.00066 (14)0.00069 (15)
Co10.01725 (19)0.01863 (19)0.01881 (19)0.00025 (17)0.00074 (18)0.00063 (19)
S10.0232 (4)0.0355 (5)0.0296 (5)0.0039 (4)0.0070 (3)0.0070 (4)
S20.0344 (5)0.0331 (5)0.0231 (4)0.0016 (4)0.0047 (4)0.0007 (4)
S30.0312 (4)0.0355 (5)0.0260 (5)0.0133 (4)0.0020 (4)0.0049 (4)
S40.0280 (4)0.0293 (4)0.0588 (6)0.0109 (3)0.0098 (5)0.0058 (5)
N10.0243 (13)0.0223 (13)0.0292 (17)0.0019 (11)0.0026 (11)0.0001 (10)
N20.0256 (14)0.0312 (15)0.0285 (16)0.0051 (12)0.0025 (12)0.0031 (12)
N30.0240 (13)0.0258 (13)0.0291 (15)0.0013 (10)0.0001 (13)0.0030 (13)
N40.0235 (13)0.0287 (13)0.0259 (16)0.0040 (10)0.0045 (12)0.0013 (12)
N50.0297 (14)0.0227 (13)0.0286 (16)0.0002 (11)0.0023 (12)0.0006 (11)
N60.0201 (14)0.0249 (14)0.0249 (15)0.0031 (11)0.0010 (11)0.0028 (10)
C10.040 (2)0.041 (2)0.027 (2)0.0150 (18)0.0020 (15)0.0065 (16)
C20.0248 (18)0.049 (2)0.035 (2)0.0084 (16)0.0089 (15)0.0046 (17)
C30.034 (2)0.040 (2)0.024 (2)0.0075 (15)0.0078 (15)0.0019 (15)
C40.040 (2)0.041 (2)0.023 (2)0.0034 (16)0.0040 (16)0.0054 (15)
C50.0288 (17)0.0242 (16)0.0274 (19)0.0064 (14)0.0020 (14)0.0054 (13)
C60.0229 (16)0.0312 (17)0.0217 (17)0.0050 (14)0.0025 (13)0.0009 (13)
Geometric parameters (Å, º) top
As1—S12.1687 (8)N5—C51.479 (4)
As1—S22.1761 (10)N5—H5A0.900
As1—S32.1692 (9)N5—H5C0.900
As1—S42.1520 (8)N6—C61.484 (3)
Co1—N11.963 (2)N6—H6A0.900
Co1—N21.968 (2)N6—H6C0.900
Co1—N31.960 (3)C1—C21.504 (4)
Co1—N41.970 (3)C1—H1B0.970
Co1—N51.969 (2)C1—H1C0.970
Co1—N61.960 (3)C2—H2B0.970
N1—C11.479 (4)C2—H2C0.970
N1—H1A0.900C3—C41.499 (5)
N1—H1D0.900C3—H3B0.970
N2—C21.486 (4)C3—H3C0.970
N2—H2A0.900C4—H4B0.970
N2—H2D0.900C4—H4C0.970
N3—C31.471 (4)C5—C61.509 (4)
N3—H3A0.900C5—H5B0.970
N3—H3D0.900C5—H5D0.970
N4—C41.475 (4)C6—H6D0.970
N4—H4A0.900C6—H6B0.970
N4—H4D0.900
S1—As1—S2106.70 (4)Co1—N5—H5A109.8
S1—As1—S3106.00 (4)C5—N5—H5C109.8
S1—As1—S4111.97 (3)Co1—N5—H5C109.8
S2—As1—S3113.85 (4)H5A—N5—H5C108.3
S2—As1—S4107.38 (4)C6—N6—Co1109.32 (18)
S3—As1—S4110.93 (4)C6—N6—H6A109.8
N3—Co1—N6174.89 (11)Co1—N6—H6A109.8
N3—Co1—N192.80 (10)C6—N6—H6C109.8
N6—Co1—N189.79 (10)Co1—N6—H6C109.8
N3—Co1—N292.21 (11)H6A—N6—H6C108.3
N6—Co1—N292.37 (11)N1—C1—C2106.8 (3)
N1—Co1—N285.87 (10)N1—C1—H1B110.4
N3—Co1—N484.19 (12)C2—C1—H1B110.4
N6—Co1—N491.31 (11)N1—C1—H1C110.4
N1—Co1—N492.07 (10)C2—C1—H1C110.4
N2—Co1—N4175.77 (11)H1B—C1—H1C108.6
N3—Co1—N592.29 (10)N2—C2—C1107.6 (2)
N6—Co1—N585.42 (10)N2—C2—H2B110.2
N1—Co1—N5173.79 (11)C1—C2—H2B110.2
N2—Co1—N590.37 (11)N2—C2—H2C110.2
N4—Co1—N591.99 (11)C1—C2—H2C110.2
C1—N1—Co1108.16 (19)H2B—C2—H2C108.5
C1—N1—H1A110.1N3—C3—C4107.0 (3)
Co1—N1—H1A110.1N3—C3—H3B110.3
C1—N1—H1D110.1C4—C3—H3B110.3
Co1—N1—H1D110.1N3—C3—H3C110.3
H1A—N1—H1D108.4C4—C3—H3C110.3
C2—N2—Co1109.19 (18)H3B—C3—H3C108.6
C2—N2—H2A109.8N4—C4—C3107.0 (3)
Co1—N2—H2A109.8N4—C4—H4B110.3
C2—N2—H2D109.8C3—C4—H4B110.3
Co1—N2—H2D109.8N4—C4—H4C110.3
H2A—N2—H2D108.3C3—C4—H4C110.3
C3—N3—Co1110.56 (18)H4B—C4—H4C108.6
C3—N3—H3A109.5N5—C5—C6106.3 (2)
Co1—N3—H3A109.5N5—C5—H5B110.5
C3—N3—H3D109.5C6—C5—H5B110.5
Co1—N3—H3D109.5N5—C5—H5D110.5
H3A—N3—H3D108.1C6—C5—H5D110.5
C4—N4—Co1110.58 (19)H5B—C5—H5D108.7
C4—N4—H4A109.5N6—C6—C5107.4 (2)
Co1—N4—H4A109.5N6—C6—H6D110.2
C4—N4—H4D109.5C5—C6—H6D110.2
Co1—N4—H4D109.5N6—C6—H6B110.2
H4A—N4—H4D108.1C5—C6—H6B110.2
C5—N5—Co1109.36 (18)H6D—C6—H6B108.5
C5—N5—H5A109.8
N3—Co1—N1—C1111.0 (2)N6—Co1—N5—C515.62 (19)
N6—Co1—N1—C173.4 (2)N2—Co1—N5—C576.7 (2)
N2—Co1—N1—C119.0 (2)N4—Co1—N5—C5106.8 (2)
N4—Co1—N1—C1164.7 (2)N1—Co1—N6—C6170.9 (2)
N3—Co1—N2—C283.3 (2)N2—Co1—N6—C6103.2 (2)
N6—Co1—N2—C298.9 (2)N4—Co1—N6—C678.83 (19)
N1—Co1—N2—C29.3 (2)N5—Co1—N6—C613.07 (19)
N5—Co1—N2—C2175.6 (2)Co1—N1—C1—C242.9 (3)
N1—Co1—N3—C376.7 (2)Co1—N2—C2—C135.2 (3)
N2—Co1—N3—C3162.7 (2)N1—C1—C2—N251.2 (3)
N4—Co1—N3—C315.1 (2)Co1—N3—C3—C439.2 (3)
N5—Co1—N3—C3106.8 (2)Co1—N4—C4—C337.2 (3)
N3—Co1—N4—C412.9 (2)N3—C3—C4—N449.1 (3)
N6—Co1—N4—C4164.7 (2)Co1—N5—C5—C640.1 (3)
N1—Co1—N4—C4105.5 (2)Co1—N6—C6—C538.5 (3)
N5—Co1—N4—C479.2 (2)N5—C5—C6—N651.1 (3)
N3—Co1—N5—C5169.0 (2)
 

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