Download citation
Download citation
link to html
The use of mixed-ligand (iodide and thio­cyanate) coordination with cobalt has led to the crystallization of the title compound, (C24H20As)2[CoI2(NCS)2]. The structure comprises tetra­hedral (C6H5)4As+ cations and tetra­hedral [CoI2(NCS)2]2- anions, the latter lying on crystallographic twofold axes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806042565/bi2072sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806042565/bi2072Isup2.hkl
Contains datablock I

CCDC reference: 627322

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.015 Å
  • R factor = 0.065
  • wR factor = 0.217
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 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 (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Tetraphenylarsonium diiododiisothiocyanatocobaltate(II) top
Crystal data top
(C24H20As)2[CoI2(NCS)2]F(000) = 2340
Mr = 1195.55Dx = 1.615 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 5456 reflections
a = 15.699 (5) Åθ = 2.3–22.6°
b = 13.915 (4) ŵ = 3.06 mm1
c = 23.465 (7) ÅT = 298 K
β = 106.472 (5)°Block, green
V = 4916 (3) Å30.32 × 0.15 × 0.13 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
4341 independent reflections
Radiation source: fine-focus sealed tube3435 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
φ and ω scansθmax = 25.1°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1818
Tmin = 0.571, Tmax = 0.677k = 1616
23014 measured reflectionsl = 2727
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.065Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.217H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.1343P)2 + 18.6113P]
where P = (Fo2 + 2Fc2)/3
4341 reflections(Δ/σ)max = 0.007
267 parametersΔρmax = 1.95 e Å3
0 restraintsΔρmin = 1.36 e Å3
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
As10.08297 (5)0.64534 (5)0.41791 (3)0.0458 (3)
I10.12254 (5)0.24902 (5)0.31946 (3)0.0878 (3)
Co10.00000.13776 (13)0.25000.0892 (7)
S10.1275 (2)0.07191 (18)0.14025 (11)0.0834 (7)
N10.0581 (8)0.0465 (8)0.1996 (5)0.106 (3)
C10.1571 (5)0.5509 (5)0.4675 (3)0.0546 (17)
C20.1740 (6)0.5600 (7)0.5288 (4)0.073 (2)
H20.14950.60990.54530.087*
C30.2294 (7)0.4911 (9)0.5647 (5)0.093 (3)
H30.24220.49540.60580.111*
C40.2648 (7)0.4175 (9)0.5399 (5)0.101 (4)
H40.30030.37150.56420.121*
C50.2483 (7)0.4116 (8)0.4802 (6)0.096 (3)
H50.27260.36150.46370.116*
C60.1956 (6)0.4791 (7)0.4435 (4)0.075 (2)
H60.18640.47590.40260.090*
C70.0177 (3)0.5883 (4)0.3637 (2)0.0517 (16)
C80.0121 (7)0.4977 (8)0.3414 (6)0.098 (3)
H80.03860.46070.35650.118*
C90.0838 (9)0.4623 (10)0.2959 (7)0.133 (6)
H90.08120.40080.28090.160*
C100.1581 (7)0.5185 (9)0.2733 (5)0.097 (3)
H100.20440.49640.24180.116*
C110.1632 (7)0.6057 (8)0.2973 (5)0.087 (3)
H110.21430.64250.28320.105*
C120.0940 (6)0.6406 (6)0.3419 (4)0.072 (2)
H120.09860.70080.35800.086*
C130.1472 (5)0.7137 (6)0.3725 (3)0.0529 (16)
C140.2329 (5)0.6922 (6)0.3757 (4)0.065 (2)
H140.26280.64540.40220.078*
C150.2757 (8)0.7391 (9)0.3399 (6)0.095 (3)
H150.33470.72560.34250.114*
C160.2286 (8)0.8071 (9)0.2999 (5)0.099 (4)
H160.25590.83820.27470.119*
C170.1439 (9)0.8285 (9)0.2971 (5)0.099 (3)
H170.11350.87460.27030.118*
C180.1015 (7)0.7822 (8)0.3342 (4)0.083 (3)
H180.04330.79760.33280.100*
C190.0446 (5)0.7320 (5)0.4679 (3)0.0503 (16)
C200.0806 (5)0.8226 (6)0.4782 (4)0.063 (2)
H200.12070.84400.45840.076*
C210.0560 (7)0.8815 (7)0.5187 (5)0.083 (3)
H210.07950.94310.52620.099*
C220.0038 (7)0.8480 (8)0.5478 (5)0.089 (3)
H220.01950.88780.57510.106*
C230.0402 (7)0.7581 (7)0.5376 (5)0.083 (3)
H230.07920.73600.55810.100*
C240.0169 (6)0.7002 (7)0.4951 (4)0.072 (2)
H240.04320.64020.48540.087*
C250.0797 (7)0.0072 (6)0.1775 (3)0.057 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.0499 (4)0.0461 (4)0.0421 (4)0.0044 (3)0.0143 (3)0.0013 (3)
I10.1088 (6)0.0864 (5)0.0706 (5)0.0080 (3)0.0292 (4)0.0124 (3)
Co10.1425 (19)0.0734 (12)0.0707 (11)0.0000.0609 (12)0.000
S10.114 (2)0.0736 (14)0.0696 (14)0.0061 (13)0.0366 (13)0.0007 (11)
N10.127 (9)0.084 (8)0.067 (7)0.014 (7)0.045 (6)0.038 (6)
C10.054 (4)0.060 (4)0.049 (4)0.007 (3)0.013 (3)0.016 (3)
C20.076 (6)0.090 (6)0.052 (4)0.012 (5)0.017 (4)0.017 (4)
C30.088 (7)0.122 (9)0.064 (6)0.011 (6)0.014 (5)0.042 (6)
C40.085 (7)0.122 (9)0.103 (8)0.041 (7)0.037 (6)0.070 (7)
C50.089 (7)0.097 (8)0.109 (9)0.045 (6)0.039 (6)0.035 (7)
C60.078 (6)0.081 (6)0.067 (5)0.028 (5)0.022 (4)0.016 (4)
C70.051 (4)0.050 (4)0.054 (4)0.003 (3)0.014 (3)0.009 (3)
C80.067 (6)0.053 (6)0.094 (9)0.001 (5)0.012 (6)0.043 (6)
C90.083 (9)0.092 (9)0.091 (4)0.020 (8)0.029 (9)0.050 (10)
C100.076 (7)0.118 (9)0.085 (7)0.035 (6)0.006 (5)0.021 (6)
C110.068 (6)0.087 (7)0.090 (7)0.001 (5)0.005 (5)0.008 (6)
C120.069 (5)0.066 (5)0.073 (5)0.011 (4)0.008 (4)0.010 (4)
C130.056 (4)0.060 (4)0.043 (4)0.004 (3)0.016 (3)0.000 (3)
C140.065 (5)0.071 (5)0.061 (5)0.003 (4)0.021 (4)0.002 (4)
C150.087 (7)0.112 (9)0.099 (8)0.007 (6)0.046 (7)0.011 (6)
C160.117 (10)0.109 (9)0.087 (7)0.028 (8)0.056 (7)0.007 (7)
C170.103 (9)0.112 (8)0.083 (7)0.004 (7)0.029 (6)0.038 (6)
C180.082 (6)0.089 (6)0.077 (6)0.009 (5)0.020 (5)0.036 (5)
C190.052 (4)0.051 (4)0.048 (4)0.007 (3)0.014 (3)0.008 (3)
C200.055 (4)0.062 (5)0.066 (5)0.006 (4)0.008 (4)0.009 (4)
C210.072 (6)0.071 (5)0.090 (7)0.011 (5)0.002 (5)0.030 (5)
C220.067 (6)0.114 (9)0.076 (6)0.019 (6)0.007 (5)0.045 (6)
C230.083 (7)0.104 (8)0.070 (6)0.010 (5)0.036 (5)0.015 (5)
C240.079 (6)0.069 (5)0.073 (5)0.005 (4)0.029 (5)0.010 (4)
C250.097 (7)0.076 (4)0.052 (3)0.007 (4)0.018 (4)0.007 (3)
Geometric parameters (Å, º) top
As1—C11.915 (7)C10—C111.350 (16)
As1—C71.899 (5)C10—H100.930
As1—C131.914 (7)C11—C121.366 (13)
As1—C191.896 (7)C11—H110.930
Co1—I12.6412 (14)C12—H120.930
Co1—N1i2.110 (12)C13—C141.358 (11)
Co1—N12.110 (12)C13—C181.366 (12)
Co1—I1i2.6412 (14)C14—C151.380 (13)
S1—C251.706 (10)C14—H140.930
N1—C250.886 (11)C15—C161.388 (16)
C1—C61.369 (11)C15—H150.930
C1—C21.392 (11)C16—C171.345 (16)
C2—C31.403 (13)C16—H160.930
C2—H20.930C17—C181.394 (14)
C3—C41.372 (17)C17—H170.930
C3—H30.930C18—H180.930
C4—C51.353 (16)C19—C201.374 (11)
C4—H40.930C19—C241.373 (12)
C5—C61.380 (12)C20—C211.390 (12)
C5—H50.930C20—H200.930
C6—H60.930C21—C221.391 (15)
C7—C81.374 (12)C21—H210.930
C7—C121.371 (11)C22—C231.367 (14)
C8—C91.403 (16)C22—H220.930
C8—H80.930C23—C241.410 (12)
C9—C101.379 (18)C23—H230.930
C9—H90.930C24—H240.930
C1—As1—C7111.8 (3)C12—C11—H11120.0
C1—As1—C13110.7 (3)C10—C11—H11119.3
C1—As1—C19107.8 (3)C11—C12—C7120.8 (8)
C7—As1—C13107.5 (3)C11—C12—H12120.0
C7—As1—C19109.3 (3)C7—C12—H12119.2
C13—As1—C19109.8 (3)C14—C13—C18121.1 (8)
N1—Co1—I1110.1 (4)C14—C13—As1122.0 (6)
N1—Co1—I1i111.2 (3)C18—C13—As1116.8 (6)
N1i—Co1—N1106.0 (5)C15—C14—C13120.5 (9)
I1—Co1—I1i108.23 (7)C15—C14—H14119.1
C25—N1—Co1177.0 (15)C13—C14—H14120.3
C6—C1—C2121.0 (7)C14—C15—C16118.4 (11)
C6—C1—As1120.9 (6)C14—C15—H15120.8
C2—C1—As1118.0 (6)C16—C15—H15120.7
C1—C2—C3117.6 (9)C15—C16—C17120.9 (10)
C1—C2—H2121.2C15—C16—H16119.2
C3—C2—H2121.2C17—C16—H16119.8
C4—C3—C2120.7 (10)C18—C17—C16120.5 (10)
C4—C3—H3119.7C18—C17—H17119.4
C2—C3—H3119.6C16—C17—H17120.2
C5—C4—C3120.2 (9)C17—C18—C13118.6 (10)
C5—C4—H4120.0C17—C18—H18120.6
C3—C4—H4119.8C13—C18—H18120.7
C4—C5—C6120.6 (10)C20—C19—C24121.6 (7)
C4—C5—H5119.6C20—C19—As1120.3 (6)
C6—C5—H5119.8C24—C19—As1118.1 (6)
C1—C6—C5119.7 (9)C19—C20—C21118.7 (9)
C1—C6—H6120.2C19—C20—H20120.7
C5—C6—H6120.1C21—C20—H20120.6
C8—C7—C12119.2 (7)C20—C21—C22119.7 (9)
C8—C7—As1120.4 (6)C20—C21—H21120.1
C12—C7—As1119.8 (6)C22—C21—H21120.1
C9—C8—C7118.5 (10)C23—C22—C21121.9 (9)
C9—C8—H8120.5C23—C22—H22119.1
C7—C8—H8120.0C21—C22—H22119.0
C10—C9—C8120.2 (11)C22—C23—C24117.9 (10)
C10—C9—H9120.3C22—C23—H23121.1
C8—C9—H9119.5C24—C23—H23121.0
C9—C10—C11119.5 (10)C19—C24—C23120.1 (9)
C9—C10—H10119.7C19—C24—H24119.9
C11—C10—H10120.7C23—C24—H24120.0
C12—C11—C10120.7 (10)N1—C25—S1175.1 (12)
C19—As1—C1—C6179.2 (7)C19—As1—C13—C14120.9 (7)
C13—As1—C1—C659.1 (8)C7—As1—C13—C14120.3 (7)
C7—As1—C1—C660.7 (8)C1—As1—C13—C142.0 (8)
C19—As1—C1—C22.1 (8)C19—As1—C13—C1862.4 (8)
C13—As1—C1—C2118.0 (7)C7—As1—C13—C1856.4 (8)
C7—As1—C1—C2122.2 (7)C1—As1—C13—C18178.7 (7)
C6—C1—C2—C32.1 (13)C18—C13—C14—C150.2 (14)
As1—C1—C2—C3179.2 (7)As1—C13—C14—C15176.3 (8)
C1—C2—C3—C40.3 (15)C13—C14—C15—C161.3 (16)
C2—C3—C4—C51.5 (18)C14—C15—C16—C171.7 (18)
C3—C4—C5—C60.1 (19)C15—C16—C17—C180.5 (19)
C2—C1—C6—C53.5 (15)C16—C17—C18—C131.1 (19)
As1—C1—C6—C5179.5 (8)C14—C13—C18—C171.4 (16)
C4—C5—C6—C12.3 (17)As1—C13—C18—C17175.3 (9)
C19—As1—C7—C8151.2 (8)C13—As1—C19—C2015.2 (7)
C13—As1—C7—C889.7 (9)C7—As1—C19—C20132.9 (6)
C1—As1—C7—C832.0 (9)C1—As1—C19—C20105.5 (6)
C19—As1—C7—C1234.3 (8)C13—As1—C19—C24167.5 (6)
C13—As1—C7—C1284.8 (7)C7—As1—C19—C2449.8 (7)
C1—As1—C7—C12153.6 (7)C1—As1—C19—C2471.9 (7)
C12—C7—C8—C92.1 (17)C24—C19—C20—C212.2 (12)
As1—C7—C8—C9172.3 (10)As1—C19—C20—C21175.0 (6)
C7—C8—C9—C101 (2)C19—C20—C21—C220.2 (13)
C8—C9—C10—C113 (2)C20—C21—C22—C230.5 (16)
C9—C10—C11—C122.8 (19)C21—C22—C23—C241.5 (17)
C10—C11—C12—C70.2 (16)C20—C19—C24—C234.2 (13)
C8—C7—C12—C112.7 (15)As1—C19—C24—C23173.1 (7)
As1—C7—C12—C11171.7 (8)C22—C23—C24—C193.8 (15)
Symmetry code: (i) x, y, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds