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Acta Crystallogr Sect E Struct Rep Online. 2010 January 1; 66(Pt 1): m68.
Published online 2009 December 16. doi:  10.1107/S1600536809053471
PMCID: PMC2980073

Bis(benzo-15-crown-5-κ5 O)barium tetrakis­(isothio­cyanato-κN)cobaltate(II)

Abstract

In the title compound, [Ba(C14H20O5)2][Co(NCS)4], the BaII and CoII ions are situated on twofold rotational axes, so asymmetric unit contains half each of the complex cations and anions. The CoII ion is coordinated by four N atoms [Co—N 1.83 (2), 1.95 (3) Å] in a distorted tetra­hedral geometry. The BaII ion is coordinated by ten O atoms [Ba—O 2.766 (19)–2.859 (19) Å] from two benzo-15-crown-5 ligands in a sandwich-like configuration.

Related literature

For related structures, see: Drew et al. (1983 [triangle]); Owen (1983 [triangle]); Nunez & Rogers (1993 [triangle]).

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Object name is e-66-00m68-scheme1.jpg

Experimental

Crystal data

  • [Ba(C14H20O5)2][Co(NCS)4]
  • M r = 965.19
  • Trigonal, An external file that holds a picture, illustration, etc.
Object name is e-66-00m68-efi2.jpg
  • a = 12.5772 (13) Å
  • c = 23.758 (3) Å
  • V = 3254.7 (6) Å3
  • Z = 3
  • Mo Kα radiation
  • μ = 1.53 mm−1
  • T = 298 K
  • 0.43 × 0.40 × 0.28 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.559, T max = 0.674
  • 14488 measured reflections
  • 3786 independent reflections
  • 2749 reflections with I > 2σ(I)
  • R int = 0.059

Refinement

  • R[F 2 > 2σ(F 2)] = 0.068
  • wR(F 2) = 0.196
  • S = 1.00
  • 3786 reflections
  • 236 parameters
  • 1 restraint
  • H-atom parameters constrained
  • Δρmax = 1.68 e Å−3
  • Δρmin = −1.38 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 1623 Friedel pairs
  • Flack parameter: −0.01 (12)

Data collection: SMART (Siemens, 1996 [triangle]); cell refinement: SAINT (Siemens, 1996 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809053471/cv2669sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809053471/cv2669Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

In continuation of structural study of benzo-15-crown-5 ligands and their barium(II) complexes (Nunez et al., 1993), we report here the synthesis and crystal structure of the title compound, (I).

In (I) (Fig. 1), the BaII ions are sandwiched between the 15-crown-5 rings from two ligands (Owen, 1983). The CoII ions are coordinated by four N atoms from the thiocyanate ligands in a distorted tetrahedal geometry. The Ba—O and Co—N coordinating bond lengths are comparable with those observed in other BaII (Nunez et al., 1993) and CoII complexes (Drew et al., 1983).

Experimental

Potassium thiocyanate (1 mmol, 97.18 mg) and cobalt(II) dichloride (0.25 mmol, 59.49 mg) were dissolved and stirred at 293 K in H2O solution (10 ml) for 0.5 h and then added dropwise to a 1,2-dichloroethane solution (10 ml) of benzo-15-crown-5 (0.5 mmol,134.16 mg). The mixture was then stirred at 293 K for 0.5 h. An aqueous solution (2 ml) of barium(II) chloride (0.25 mmol, 52.07 mg) was then added dropwise and the mixture stirred for another 5 h. The lower clear liquid was held at room temperature for about one week, whereupon blue square block crystal suitable for X-ray diffraction analysis were obtained.

Refinement

All H atoms were placed in geometrically idealized positions (C—H 0.93-0.97 Å) and treated as riding on their parent atoms, with Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
The molecular structure of (I), showing 30% probability displacement ellipsoids and atomic numbering for non-C atoms [symmetry codes: (A) -x, -x + y, 4/3 - z; (B)1 + x-y,2 - y, 5/3 - z]. H atoms omitted for clarity.

Crystal data

[Ba(C14H20O5)2][Co(NCS)4]Dx = 1.477 Mg m3
Mr = 965.19Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3121Cell parameters from 2944 reflections
a = 12.5772 (13) Åθ = 2.5–18.7°
c = 23.758 (3) ŵ = 1.53 mm1
V = 3254.7 (6) Å3T = 298 K
Z = 3Block, blue
F(000) = 14610.43 × 0.40 × 0.28 mm

Data collection

Bruker SMART CCD area-detector diffractometer3786 independent reflections
Radiation source: fine-focus sealed tube2749 reflections with I > 2σ(I)
graphiteRint = 0.059
phi and ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −10→14
Tmin = 0.559, Tmax = 0.674k = −14→14
14488 measured reflectionsl = −28→26

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.068H-atom parameters constrained
wR(F2) = 0.196w = 1/[σ2(Fo2) + (0.1148P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
3786 reflectionsΔρmax = 1.68 e Å3
236 parametersΔρmin = −1.38 e Å3
1 restraintAbsolute structure: Flack (1983), 1623 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: −0.01 (12)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Ba10.00000.58989 (14)0.66670.0538 (6)
Co10.5798 (5)1.00000.83330.1076 (17)
N10.553 (2)1.113 (2)0.7970 (9)0.069 (6)
N20.615 (3)0.900 (3)0.7820 (13)0.119 (9)
O1−0.0086 (19)0.409 (2)0.7422 (9)0.087 (6)
O20.1988 (19)0.561 (2)0.6987 (9)0.097 (7)
O30.222 (2)0.794 (2)0.6989 (9)0.102 (6)
O40.002 (2)0.773 (2)0.7356 (9)0.096 (6)
O5−0.130 (2)0.530 (2)0.7666 (9)0.111 (7)
S10.5021 (12)1.3067 (13)0.7753 (4)0.127 (4)
S20.6535 (14)0.7424 (14)0.7203 (5)0.147 (5)
C10.068 (3)0.364 (3)0.7324 (14)0.094 (9)
C20.028 (4)0.241 (4)0.7438 (16)0.118 (13)
H2−0.04870.18900.75940.141*
C30.110 (5)0.201 (4)0.7304 (16)0.126 (14)
H30.09060.12130.73850.151*
C40.218 (4)0.281 (4)0.7053 (15)0.108 (11)
H40.26890.24990.69540.129*
C50.260 (4)0.403 (4)0.6928 (14)0.111 (12)
H50.33400.45230.67430.133*
C60.182 (3)0.445 (4)0.7105 (13)0.090 (9)
C70.300 (4)0.651 (4)0.7258 (19)0.124 (13)
H7A0.36950.63770.72020.149*
H7B0.28460.64820.76590.149*
C80.329 (4)0.774 (4)0.7017 (17)0.131 (13)
H8A0.39270.83800.72450.157*
H8B0.36170.78080.66400.157*
C90.228 (4)0.877 (4)0.7402 (16)0.119 (13)
H9A0.30140.95700.73550.143*
H9B0.22810.84700.77770.143*
C100.113 (4)0.884 (4)0.7295 (17)0.121 (13)
H10A0.11250.94380.75530.145*
H10B0.11710.91480.69160.145*
C11−0.059 (4)0.743 (3)0.7883 (14)0.106 (11)
H11A−0.09320.79580.79560.128*
H11B−0.00130.75520.81820.128*
C12−0.160 (3)0.610 (4)0.7861 (14)0.101 (11)
H12A−0.19200.58490.82390.121*
H12B−0.22610.60480.76310.121*
C13−0.126 (3)0.453 (4)0.8075 (13)0.102 (10)
H13A−0.20860.38620.81490.122*
H13B−0.09350.49830.84220.122*
C14−0.047 (5)0.401 (4)0.7888 (16)0.128 (14)
H14A0.02410.43600.81340.154*
H14B−0.09290.31360.79740.154*
C150.529 (3)1.183 (2)0.7886 (11)0.098 (11)
C160.639 (3)0.835 (3)0.7554 (14)0.094 (9)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ba10.0643 (13)0.0576 (9)0.0417 (9)0.0321 (6)−0.0018 (10)−0.0009 (5)
Co10.101 (3)0.091 (4)0.128 (5)0.045 (2)−0.003 (2)−0.007 (4)
N10.088 (16)0.076 (14)0.078 (14)0.067 (13)−0.009 (11)−0.004 (11)
N20.13 (2)0.12 (2)0.11 (2)0.06 (2)0.010 (17)−0.002 (18)
O10.094 (14)0.119 (17)0.072 (12)0.070 (14)0.009 (11)0.025 (12)
O20.081 (14)0.130 (19)0.082 (14)0.053 (14)−0.005 (11)0.012 (13)
O30.104 (15)0.099 (16)0.094 (14)0.044 (14)−0.009 (12)−0.020 (13)
O40.116 (18)0.092 (15)0.087 (14)0.059 (15)0.003 (13)−0.021 (11)
O50.133 (19)0.126 (18)0.083 (13)0.070 (17)0.038 (14)0.007 (14)
S10.159 (9)0.182 (11)0.091 (5)0.123 (8)0.024 (6)0.023 (7)
S20.170 (11)0.177 (12)0.150 (9)0.129 (10)0.032 (9)0.023 (9)
C10.12 (3)0.11 (3)0.08 (2)0.08 (2)−0.021 (19)−0.01 (2)
C20.14 (3)0.13 (4)0.10 (3)0.08 (3)−0.03 (2)0.00 (2)
C30.15 (4)0.14 (4)0.10 (3)0.08 (4)−0.03 (3)−0.01 (3)
C40.14 (3)0.14 (3)0.10 (2)0.11 (3)−0.02 (2)−0.02 (2)
C50.13 (3)0.14 (3)0.10 (2)0.09 (3)−0.03 (2)−0.01 (2)
C60.11 (3)0.13 (3)0.081 (18)0.09 (3)−0.009 (18)−0.004 (19)
C70.12 (3)0.13 (3)0.12 (3)0.06 (3)−0.01 (3)0.00 (3)
C80.11 (3)0.13 (3)0.11 (3)0.03 (3)−0.01 (2)−0.01 (3)
C90.12 (3)0.11 (3)0.11 (3)0.04 (2)0.00 (2)−0.01 (2)
C100.14 (4)0.10 (3)0.12 (3)0.05 (2)−0.01 (2)−0.03 (2)
C110.13 (3)0.13 (3)0.09 (2)0.09 (3)0.01 (2)−0.010 (19)
C120.12 (3)0.13 (3)0.09 (2)0.09 (3)0.035 (19)0.01 (2)
C130.11 (2)0.14 (3)0.061 (17)0.06 (2)0.019 (17)0.02 (2)
C140.16 (4)0.13 (3)0.09 (3)0.07 (3)0.00 (3)0.01 (3)
C150.062 (17)0.15 (3)0.056 (16)0.031 (19)0.008 (14)−0.024 (19)
C160.10 (2)0.11 (2)0.10 (2)0.063 (19)0.011 (18)0.018 (18)

Geometric parameters (Å, °)

Ba1—O52.766 (19)C1—C21.39 (5)
Ba1—O5i2.766 (19)C2—C31.39 (6)
Ba1—O32.79 (2)C2—H20.9300
Ba1—O3i2.79 (2)C3—C41.36 (5)
Ba1—O22.81 (2)C3—H30.9300
Ba1—O2i2.81 (2)C4—C51.38 (5)
Ba1—O42.816 (18)C4—H40.9300
Ba1—O4i2.816 (18)C5—C61.40 (4)
Ba1—O12.859 (19)C5—H50.9300
Ba1—O1i2.859 (19)C7—C81.51 (6)
Co1—N11.834 (19)C7—H7A0.9700
Co1—N1ii1.83 (2)C7—H7B0.9700
Co1—N21.95 (3)C8—H8A0.9700
Co1—N2ii1.95 (3)C8—H8B0.9700
N1—C151.07 (3)C9—C101.52 (5)
N2—C161.19 (4)C9—H9A0.9700
O1—C141.19 (4)C9—H9B0.9700
O1—C11.36 (4)C10—H10A0.9700
O2—C71.37 (4)C10—H10B0.9700
O2—C61.39 (4)C11—C121.52 (5)
O3—C91.41 (4)C11—H11A0.9700
O3—C81.49 (5)C11—H11B0.9700
O4—C101.40 (5)C12—H12A0.9700
O4—C111.42 (4)C12—H12B0.9700
O5—C121.32 (4)C13—C141.51 (5)
O5—C131.40 (4)C13—H13A0.9700
S1—C151.79 (2)C13—H13B0.9700
S2—C161.51 (4)C14—H14A0.9700
C1—C61.38 (5)C14—H14B0.9700
O5—Ba1—O5i177.1 (11)O1—C1—C6117 (3)
O5—Ba1—O3101.4 (7)O1—C1—C2120 (4)
O5i—Ba1—O377.3 (7)C6—C1—C2124 (3)
O5—Ba1—O3i77.3 (7)C3—C2—C1116 (4)
O5i—Ba1—O3i101.4 (7)C3—C2—H2122.0
O3—Ba1—O3i130.4 (10)C1—C2—H2122.0
O5—Ba1—O2100.2 (7)C4—C3—C2119 (4)
O5i—Ba1—O281.5 (7)C4—C3—H3120.5
O3—Ba1—O259.9 (8)C2—C3—H3120.5
O3i—Ba1—O2169.6 (7)C3—C4—C5127 (4)
O5—Ba1—O2i81.5 (7)C3—C4—H4116.7
O5i—Ba1—O2i100.2 (7)C5—C4—H4116.7
O3—Ba1—O2i169.6 (7)C4—C5—C6114 (4)
O3i—Ba1—O2i59.9 (8)C4—C5—H5123.0
O2—Ba1—O2i109.9 (11)C6—C5—H5123.0
O5—Ba1—O459.0 (7)C1—C6—O2114 (3)
O5i—Ba1—O4118.2 (8)C1—C6—C5120 (3)
O3—Ba1—O459.4 (7)O2—C6—C5125 (4)
O3i—Ba1—O480.0 (7)O2—C7—C8108 (3)
O2—Ba1—O4107.6 (7)O2—C7—H7A110.1
O2i—Ba1—O4129.2 (7)C8—C7—H7A110.1
O5—Ba1—O4i118.2 (8)O2—C7—H7B110.1
O5i—Ba1—O4i59.0 (7)C8—C7—H7B110.1
O3—Ba1—O4i80.0 (7)H7A—C7—H7B108.4
O3i—Ba1—O4i59.4 (7)O3—C8—C7115 (3)
O2—Ba1—O4i129.2 (7)O3—C8—H8A108.6
O2i—Ba1—O4i107.6 (7)C7—C8—H8A108.6
O4—Ba1—O4i71.1 (9)O3—C8—H8B108.6
O5—Ba1—O157.6 (7)C7—C8—H8B108.6
O5i—Ba1—O1125.1 (7)H8A—C8—H8B107.6
O3—Ba1—O1100.5 (6)O3—C9—C10103 (3)
O3i—Ba1—O1118.0 (6)O3—C9—H9A111.1
O2—Ba1—O153.7 (6)C10—C9—H9A111.1
O2i—Ba1—O172.4 (7)O3—C9—H9B111.1
O4—Ba1—O1105.6 (6)C10—C9—H9B111.1
O4i—Ba1—O1175.9 (7)H9A—C9—H9B109.1
O5—Ba1—O1i125.1 (7)O4—C10—C9115 (3)
O5i—Ba1—O1i57.6 (7)O4—C10—H10A108.4
O3—Ba1—O1i118.0 (6)C9—C10—H10A108.4
O3i—Ba1—O1i100.5 (6)O4—C10—H10B108.4
O2—Ba1—O1i72.4 (7)C9—C10—H10B108.4
O2i—Ba1—O1i53.7 (6)H10A—C10—H10B107.5
O4—Ba1—O1i175.9 (7)O4—C11—C12108 (3)
O4i—Ba1—O1i105.6 (6)O4—C11—H11A110.1
O1—Ba1—O1i77.9 (9)C12—C11—H11A110.1
N1—Co1—N1ii110.4 (15)O4—C11—H11B110.1
N1—Co1—N2113.2 (12)C12—C11—H11B110.1
N1ii—Co1—N2103.5 (11)H11A—C11—H11B108.4
N1—Co1—N2ii103.5 (11)O5—C12—C11117 (3)
N1ii—Co1—N2ii113.2 (12)O5—C12—H12A108.1
N2—Co1—N2ii113.2 (19)C11—C12—H12A108.1
C15—N1—Co1162 (3)O5—C12—H12B108.1
C16—N2—Co1173 (3)C11—C12—H12B108.1
C14—O1—C1118 (3)H12A—C12—H12B107.3
C14—O1—Ba1120 (3)O5—C13—C14111 (3)
C1—O1—Ba1118.2 (19)O5—C13—H13A109.4
C7—O2—C6111 (3)C14—C13—H13A109.4
C7—O2—Ba1123 (2)O5—C13—H13B109.4
C6—O2—Ba1120.6 (19)C14—C13—H13B109.4
C9—O3—C8112 (3)H13A—C13—H13B108.0
C9—O3—Ba1122 (2)O1—C14—C13124 (4)
C8—O3—Ba1115 (2)O1—C14—H14A106.2
C10—O4—C11119 (3)C13—C14—H14A106.2
C10—O4—Ba1110.8 (19)O1—C14—H14B106.2
C11—O4—Ba1120.9 (19)C13—C14—H14B106.2
C12—O5—C13114 (2)H14A—C14—H14B106.4
C12—O5—Ba1117 (2)N1—C15—S1176 (3)
C13—O5—Ba1124 (2)N2—C16—S2173 (3)
N1ii—Co1—N1—C1555 (8)O5—Ba1—O4—C114(2)
N2—Co1—N1—C15171 (8)O5i—Ba1—O4—C11−178 (2)
N2ii—Co1—N1—C15−66 (9)O3—Ba1—O4—C11−125 (3)
N1—Co1—N2—C16174 (26)O3i—Ba1—O4—C1185 (2)
N1ii—Co1—N2—C16−66 (26)O2—Ba1—O4—C11−88 (2)
N2ii—Co1—N2—C1657 (26)O2i—Ba1—O4—C1148 (3)
O5—Ba1—O1—C14−13 (3)O4i—Ba1—O4—C11146 (3)
O5i—Ba1—O1—C14166 (3)O1—Ba1—O4—C11−32 (2)
O3—Ba1—O1—C1484 (3)O1i—Ba1—O4—C11−178 (9)
O3i—Ba1—O1—C14−64 (3)O5i—Ba1—O5—C122(2)
O2—Ba1—O1—C14123 (3)O3—Ba1—O5—C1266 (2)
O2i—Ba1—O1—C14−104 (3)O3i—Ba1—O5—C12−63 (2)
O4—Ba1—O1—C1423 (3)O2—Ba1—O5—C12127 (2)
O4i—Ba1—O1—C14−13 (12)O2i—Ba1—O5—C12−124 (3)
O1i—Ba1—O1—C14−160 (4)O4—Ba1—O5—C1223 (2)
O5—Ba1—O1—C1−170 (2)O4i—Ba1—O5—C12−18 (3)
O5i—Ba1—O1—C18(3)O1—Ba1—O5—C12162 (3)
O3—Ba1—O1—C1−74 (2)O1i—Ba1—O5—C12−157 (2)
O3i—Ba1—O1—C1139 (2)O5i—Ba1—O5—C13−152 (3)
O2—Ba1—O1—C1−34 (2)O3—Ba1—O5—C13−88 (3)
O2i—Ba1—O1—C199 (2)O3i—Ba1—O5—C13143 (3)
O4—Ba1—O1—C1−134 (2)O2—Ba1—O5—C13−27 (3)
O4i—Ba1—O1—C1−170 (9)O2i—Ba1—O5—C1382 (3)
O1i—Ba1—O1—C143 (2)O4—Ba1—O5—C13−131 (3)
O5—Ba1—O2—C7−83 (3)O4i—Ba1—O5—C13−173 (2)
O5i—Ba1—O2—C794 (3)O1—Ba1—O5—C137(2)
O3—Ba1—O2—C714 (3)O1i—Ba1—O5—C1349 (3)
O3i—Ba1—O2—C7−159 (4)C14—O1—C1—C6−123 (4)
O2i—Ba1—O2—C7−168 (3)Ba1—O1—C1—C635 (4)
O4—Ba1—O2—C7−23 (3)C14—O1—C1—C258 (5)
O4i—Ba1—O2—C757 (3)Ba1—O1—C1—C2−144 (3)
O1—Ba1—O2—C7−119 (3)O1—C1—C2—C3177 (3)
O1i—Ba1—O2—C7153 (3)C6—C1—C2—C3−2(5)
O5—Ba1—O2—C669 (2)C1—C2—C3—C4−3(5)
O5i—Ba1—O2—C6−114 (2)C2—C3—C4—C53(6)
O3—Ba1—O2—C6166 (2)C3—C4—C5—C62(5)
O3i—Ba1—O2—C6−7(5)O1—C1—C6—O2−3(4)
O2i—Ba1—O2—C6−15.7 (18)C2—C1—C6—O2176 (3)
O4—Ba1—O2—C6129 (2)O1—C1—C6—C5−172 (3)
O4i—Ba1—O2—C6−151.0 (19)C2—C1—C6—C57(5)
O1—Ba1—O2—C632.7 (19)C7—O2—C6—C1124 (3)
O1i—Ba1—O2—C6−55 (2)Ba1—O2—C6—C1−31 (3)
O5—Ba1—O3—C9−33 (3)C7—O2—C6—C5−67 (4)
O5i—Ba1—O3—C9144 (3)Ba1—O2—C6—C5137 (3)
O3i—Ba1—O3—C950 (2)C4—C5—C6—C1−7(5)
O2—Ba1—O3—C9−128 (3)C4—C5—C6—O2−174 (3)
O2i—Ba1—O3—C9−138 (4)C6—O2—C7—C8168 (3)
O4—Ba1—O3—C910 (2)Ba1—O2—C7—C8−37 (4)
O4i—Ba1—O3—C984 (3)C9—O3—C8—C7106 (4)
O1—Ba1—O3—C9−92 (2)Ba1—O3—C8—C7−40 (4)
O1i—Ba1—O3—C9−173 (2)O2—C7—C8—O350 (5)
O5—Ba1—O3—C8109 (2)C8—O3—C9—C10180 (3)
O5i—Ba1—O3—C8−73 (2)Ba1—O3—C9—C10−37 (4)
O3i—Ba1—O3—C8−168 (2)C11—O4—C10—C992 (4)
O2—Ba1—O3—C814 (2)Ba1—O4—C10—C9−55 (4)
O2i—Ba1—O3—C84(5)O3—C9—C10—O461 (4)
O4—Ba1—O3—C8153 (2)C10—O4—C11—C12−169 (3)
O4i—Ba1—O3—C8−134 (2)Ba1—O4—C11—C12−25 (4)
O1—Ba1—O3—C851 (2)C13—O5—C12—C11109 (3)
O1i—Ba1—O3—C8−31 (2)Ba1—O5—C12—C11−48 (4)
O5—Ba1—O4—C10151 (2)O4—C11—C12—O548 (5)
O5i—Ba1—O4—C10−31 (2)C12—O5—C13—C14−158 (3)
O3—Ba1—O4—C1022 (2)Ba1—O5—C13—C14−3(4)
O3i—Ba1—O4—C10−128 (2)C1—O1—C14—C13176 (4)
O2—Ba1—O4—C1059 (2)Ba1—O1—C14—C1319 (6)
O2i—Ba1—O4—C10−165 (2)O5—C13—C14—O1−11 (6)
O4i—Ba1—O4—C10−67 (2)Co1—N1—C15—S195 (36)
O1—Ba1—O4—C10115 (2)Co1—N2—C16—S2105 (33)
O1i—Ba1—O4—C10−31 (11)

Symmetry codes: (i) −x, −x+y, −z+4/3; (ii) xy+1, −y+2, −z+5/3.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C12—H12B···S2iii0.972.993.83 (4)145
C8—H8B···S1iv0.972.973.93 (4)170

Symmetry codes: (iii) x−1, y, z; (iv) −x+1, −x+y, −z+4/3.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV2669).

References

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  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Nunez, L. & Rogers, D. R. (1993). J. Coord. Chem.28, 347–354.
  • Owen, J. D. (1983). J. Chem. Soc. Perkin Trans. 2, pp. 407–415.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst A64, 112–122. [PubMed]
  • Siemens (1996). SMART and SAINT Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

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