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The mol­ecules of the title bis­(thio­morpholine) adduct of bis­(1,3-diphenyl­propane-1,3-dionato)cobalt(II), [Co(C15H12O2)2(C4H8NS)2], in the crystal structure are positioned on an inversion center at the inter­section of a twofold rotation axis and a perpendicular mirror plane. The two thio­morpholine ligands bond to the octahedral cobalt(II) ion in the axial coordination sites (trans configuration).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806000596/su6258sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806000596/su6258Isup2.hkl
Contains datablock I

CCDC reference: 298548

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.059
  • wR factor = 0.109
  • Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT420_ALERT_2_C D-H Without Acceptor N21 - H21 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H21A .. O11 .. 2.82 Ang.
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 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997), Mercury (Bruno et al., 2002), RasTop (Valadon, 2004) and POVRay (Persistence of Vision Pty, 2004); software used to prepare material for publication: WinGX (Farrugia, 1999).

bis(1,3-diphenylpropane-1,3-dionato)bis(thiomorpholine)cobalt(II) top
Crystal data top
[Co(C15H12O2)2(C4H8NS)2]F(000) = 1492
Mr = 711.79Dx = 1.352 Mg m3
Orthorhombic, CmcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2bc 2Cell parameters from 2147 reflections
a = 19.345 (2) Åθ = 4–54°
b = 8.1767 (9) ŵ = 0.65 mm1
c = 22.104 (2) ÅT = 295 K
V = 3496.4 (6) Å3Plate, orange
Z = 40.26 × 0.25 × 0.04 mm
Data collection top
Oxford Diffraction Xcalibur-3 CCD area-detector
diffractometer
1597 independent reflections
Radiation source: fine-focus sealed tube1493 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.054
ω scansθmax = 25.1°, θmin = 4.1°
Absorption correction: analytical
(Alcock, 1970)
h = 2222
Tmin = 0.825, Tmax = 0.972k = 99
23809 measured reflectionsl = 2626
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)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H-atom parameters constrained
S = 1.33 w = 1/[σ2(Fo2) + (0.0351P)2 + 3.3855P]
where P = (Fo2 + 2Fc2)/3
1597 reflections(Δ/σ)max = 0.001
113 parametersΔρmax = 0.33 e Å3
0 restraintsΔρmin = 0.2 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
Co0.500.50.0375 (3)
S210.50.30100 (17)0.71615 (6)0.0668 (4)
O110.42603 (9)0.1616 (2)0.47184 (9)0.0442 (5)
N210.50.0938 (4)0.59383 (14)0.0408 (8)
H210.50.00080.61650.049*
C110.43539 (14)0.2643 (3)0.42952 (12)0.0375 (7)
C130.37154 (14)0.3387 (3)0.40346 (12)0.0389 (7)
C180.31418 (16)0.3614 (4)0.43977 (14)0.0509 (8)
H180.31550.32810.480.061*
C120.50.3134 (5)0.40736 (18)0.0426 (10)
H120.50.38540.37480.051*
C140.36748 (16)0.3850 (4)0.34340 (14)0.0542 (9)
H140.40530.36940.31810.065*
C150.30783 (17)0.4542 (5)0.32074 (16)0.0687 (11)
H150.30550.48380.28020.082*
C160.25201 (19)0.4797 (4)0.35778 (17)0.0648 (10)
H160.21220.52860.34260.078*
C170.25493 (18)0.4329 (5)0.41721 (16)0.0627 (9)
H170.2170.44930.44240.075*
C210.43708 (15)0.1776 (4)0.61363 (14)0.0527 (8)
H21A0.39730.11960.59770.063*
H21B0.43670.2870.59670.063*
C220.43020 (17)0.1897 (4)0.68190 (15)0.0594 (9)
H22A0.42870.08030.69890.071*
H22B0.38690.24340.69170.071*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0337 (4)0.0459 (5)0.0329 (4)000.0078 (3)
S210.0814 (10)0.0713 (9)0.0477 (7)000.0127 (6)
O110.0377 (11)0.0544 (12)0.0406 (11)0.0035 (10)0.0051 (9)0.0122 (10)
N210.0355 (19)0.051 (2)0.0358 (18)000.0041 (16)
C110.0387 (17)0.0408 (16)0.0329 (15)0.0022 (13)0.0010 (13)0.0019 (13)
C130.0351 (16)0.0407 (16)0.0410 (16)0.0013 (13)0.0013 (13)0.0030 (13)
C180.0434 (19)0.067 (2)0.0428 (16)0.0084 (16)0.0017 (14)0.0035 (16)
C120.037 (2)0.049 (2)0.042 (2)000.011 (2)
C140.0401 (18)0.077 (2)0.0451 (18)0.0002 (17)0.0026 (14)0.0140 (17)
C150.048 (2)0.105 (3)0.053 (2)0.002 (2)0.0108 (17)0.027 (2)
C160.0437 (19)0.076 (2)0.075 (2)0.0079 (19)0.0171 (18)0.013 (2)
C170.0439 (19)0.086 (3)0.059 (2)0.0123 (19)0.0015 (17)0.0032 (19)
C210.0416 (19)0.068 (2)0.0482 (18)0.0052 (16)0.0019 (15)0.0028 (16)
C220.054 (2)0.073 (2)0.0510 (19)0.0087 (18)0.0130 (16)0.0047 (17)
Geometric parameters (Å, º) top
Co—O11i2.0447 (19)C18—C171.380 (4)
Co—O11ii2.0447 (19)C18—H180.93
Co—O112.0447 (19)C12—C11ii1.401 (3)
Co—O11iii2.0447 (19)C12—H120.93
Co—N21iii2.211 (3)C14—C151.380 (4)
Co—N212.211 (3)C14—H140.93
S21—C221.796 (4)C15—C161.371 (5)
S21—C22ii1.796 (4)C15—H150.93
S21—S21iv4.3536 (10)C16—C171.369 (5)
O11—C111.270 (3)C16—H160.93
N21—C211.464 (3)C17—H170.93
N21—C21ii1.464 (3)C21—C221.518 (4)
N21—H210.91C21—H21A0.97
C11—C121.401 (3)C21—H21B0.97
C11—C131.492 (4)C22—H22A0.97
C13—C181.382 (4)C22—H22B0.97
C13—C141.383 (4)
O11i—Co—O11ii180.00 (13)C17—C18—C13120.9 (3)
O11i—Co—O1191.17 (11)C17—C18—H18119.5
O11ii—Co—O1188.83 (11)C13—C18—H18119.5
O11i—Co—O11iii88.83 (11)C11ii—C12—C11126.3 (4)
O11ii—Co—O11iii91.17 (11)C11ii—C12—H12116.9
O11—Co—O11iii180.00 (10)C11—C12—H12116.9
O11i—Co—N21iii93.53 (8)C15—C14—C13120.6 (3)
O11ii—Co—N21iii86.47 (8)C15—C14—H14119.7
O11—Co—N21iii86.47 (8)C13—C14—H14119.7
O11iii—Co—N21iii93.53 (8)C16—C15—C14120.3 (3)
O11i—Co—N2186.47 (8)C16—C15—H15119.9
O11ii—Co—N2193.53 (8)C14—C15—H15119.9
O11—Co—N2193.53 (8)C17—C16—C15119.9 (3)
O11iii—Co—N2186.47 (8)C17—C16—H16120.1
N21iii—Co—N21180C15—C16—H16120.1
C22—S21—C22ii97.5 (2)C16—C17—C18119.9 (3)
C22—S21—S21iv70.67 (12)C16—C17—H17120
C22ii—S21—S21iv70.67 (12)C18—C17—H17120
C11—O11—Co123.49 (17)N21—C21—C22113.6 (3)
C21—N21—C21ii112.5 (3)N21—C21—H21A108.8
C21—N21—Co116.29 (17)C22—C21—H21A108.8
C21ii—N21—Co116.29 (17)N21—C21—H21B108.8
C21—N21—H21103.1C22—C21—H21B108.8
C21ii—N21—H21103.1H21A—C21—H21B107.7
Co—N21—H21103.1C21—C22—S21112.7 (2)
O11—C11—C12125.0 (3)C21—C22—H22A109
O11—C11—C13115.8 (2)S21—C22—H22A109
C12—C11—C13119.1 (3)C21—C22—H22B109
C18—C13—C14118.4 (3)S21—C22—H22B109
C18—C13—C11119.7 (2)H22A—C22—H22B107.8
C14—C13—C11121.9 (3)
O11i—Co—O11—C11152.6 (3)C12—C11—C13—C1433.1 (4)
O11ii—Co—O11—C1127.4 (3)C14—C13—C18—C171.8 (5)
N21iii—Co—O11—C1159.1 (2)C11—C13—C18—C17178.7 (3)
N21—Co—O11—C11120.9 (2)O11—C11—C12—C11ii3.2 (7)
O11i—Co—N21—C2167.4 (2)C13—C11—C12—C11ii175.3 (3)
O11ii—Co—N21—C21112.6 (2)C18—C13—C14—C150.9 (5)
O11—Co—N21—C2123.5 (2)C11—C13—C14—C15179.7 (3)
O11iii—Co—N21—C21156.5 (2)C13—C14—C15—C160.7 (6)
O11i—Co—N21—C21ii156.5 (2)C14—C15—C16—C171.4 (6)
O11ii—Co—N21—C21ii23.5 (2)C15—C16—C17—C180.5 (6)
O11—Co—N21—C21ii112.6 (2)C13—C18—C17—C161.2 (5)
O11iii—Co—N21—C21ii67.4 (2)C21ii—N21—C21—C2261.2 (4)
Co—O11—C11—C1218.0 (4)Co—N21—C21—C22161.2 (2)
Co—O11—C11—C13163.46 (18)N21—C21—C22—S2160.5 (4)
O11—C11—C13—C1831.2 (4)C22ii—S21—C22—C2151.6 (3)
C12—C11—C13—C18147.5 (3)S21iv—S21—C22—C21118.0 (3)
O11—C11—C13—C14148.3 (3)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z; (iii) x+1, y, z+1; (iv) x+1, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C21—H21A···O11i0.972.823.362 (4)116
N21—H21···C12i0.912.623.329 (5)135
Symmetry code: (i) x, y, z+1.
 

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