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The title complex, [Co(H2O)6][Co2(TTHA)(H2O)2]·4H2O (TTHAH6 = triethyl­enetetr­amine­hexa­acetic acid), consists of discrete [Co(H2O)6]2+ cations and [Co2(TTHA)(H2O)2]2− binuclear anionic units. Each Co(II) ion in the binuclear units is coordinated by one water and half a TTHA6− anion as a pentadentate ligand, giving a distorted octahedral arrangement. The [Co(H2O)6]2+ cation lies on a center of inversion in the crystal and exhibits strong hydrogen-bond interactions with four carboxyl­ate groups from the TTHA6− ligand and the water mol­ecules, leading to the formation of a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019445/bt6325sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019445/bt6325Isup2.hkl
Contains datablock I

CCDC reference: 225658

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.054
  • wR factor = 0.127
  • Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Co2 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT731_ALERT_1_C Bond Calc 0.83(6), Rep 0.83(2) ...... 3.00 su-Rat O10 -H10A 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(6), Rep 0.90(2) ...... 3.00 su-Rat O8 -H8C 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(6), Rep 0.90(2) ...... 3.00 su-Rat O8 -H8C 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.06(5), Rep 2.06(2) ...... 2.50 su-Rat H8C -O2 1.555 1.655 PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.21 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 8.00 Deg. O1 -O11 -H11A 1.645 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 7.00 Deg. O6 -O10 -H10B 2.786 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.00 Deg. O1 -O9 -H9C 1.655 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 3.00 Deg. O11 -O9 -H9D 2.786 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.00 Deg. O2 -O8 -H8C 1.655 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 4.00 Deg. O3 -O12 -H12A 1.645 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C18 H28 Co2 N4 O14 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H12 Co O6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 H2 O
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C18 H48 Co3 N4 O24 Atom count from _chemical_formula_moiety:C18 H36 Co2 N4 O18
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: XPREP in SHELXTL (Bruker, 1997); program(s) used to solve structure: XS in SHELXTL; program(s) used to refine structure: XL in SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: XL in SHELXTL.

Hexa-aqua-cobalt(II) (µ2-triethylenetetra-aminehexa-acetato)- diaqua-dicobalt(II) tetrahydrate top
Crystal data top
[Co(H2O)6][Co2(C18H28N4O14)]·4H2OZ = 1
Mr = 881.39F(000) = 457
Triclinic, P1Dx = 1.695 Mg m3
Hall symbol: -p 1Mo Kα radiation, λ = 0.71073 Å
a = 7.3671 (2) ÅCell parameters from 1425 reflections
b = 8.6295 (4) Åθ = 1.4–25.0°
c = 15.0272 (7) ŵ = 1.52 mm1
α = 73.543 (2)°T = 293 K
β = 83.409 (3)°Cuboid, purple
γ = 70.465 (2)°0.52 × 0.20 × 0.10 mm
V = 863.26 (6) Å3
Data collection top
Siemens SMART CCD
diffractometer
3009 independent reflections
Radiation source: fine-focus sealed tube2629 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
φ and ω scansθmax = 25.1°, θmin = 1.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.609, Tmax = 0.859k = 810
4522 measured reflectionsl = 1717
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0278P)2 + 5.0398P]
where P = (Fo2 + 2Fc2)/3
3009 reflections(Δ/σ)max = 0.003
259 parametersΔρmax = 0.53 e Å3
3 restraintsΔρmin = 0.35 e Å3
Special details top

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
Co21.50001.50000.50000.0284 (3)
Co10.61573 (9)1.63265 (9)0.82515 (5)0.0255 (2)
O111.0679 (6)1.2449 (6)0.5566 (3)0.0381 (10)
O60.7980 (5)1.5113 (5)0.7298 (2)0.0323 (8)
O70.5731 (6)1.4019 (5)0.8891 (3)0.0396 (10)
O40.4565 (5)1.7487 (5)0.9242 (3)0.0367 (9)
O101.3152 (6)1.4020 (6)0.4530 (3)0.0386 (10)
O91.2937 (6)1.7338 (6)0.4793 (3)0.0468 (11)
N10.6229 (6)1.8867 (5)0.7603 (3)0.0303 (10)
O20.4036 (5)1.7108 (5)0.7296 (3)0.0368 (9)
N20.9015 (6)1.5927 (5)0.8756 (3)0.0263 (9)
O10.2735 (6)1.9130 (5)0.6045 (3)0.0514 (12)
O81.4283 (7)1.4361 (6)0.6435 (3)0.0478 (11)
O30.2837 (7)2.0038 (6)0.9450 (3)0.0574 (12)
C51.0512 (7)1.4836 (7)0.8254 (4)0.0345 (12)
H5A1.11031.37470.86870.041*
H5B1.15051.53660.80240.041*
C90.9075 (7)1.5118 (7)0.9770 (3)0.0284 (11)
H9A0.89051.40120.98780.034*
H9B0.79961.58091.00690.034*
C80.9139 (8)1.7684 (7)0.8545 (4)0.0341 (12)
H8A1.04771.76250.85440.041*
H8B0.84521.82220.90250.041*
C30.4972 (8)1.9995 (7)0.8161 (4)0.0366 (13)
H3A0.39622.08630.77680.044*
H3B0.57292.05680.83530.044*
C20.3936 (8)1.8480 (7)0.6672 (4)0.0344 (12)
C10.5468 (8)1.9304 (7)0.6670 (4)0.0376 (13)
H1A0.65131.89250.62470.045*
H1B0.49172.05310.64490.045*
C70.8282 (8)1.8758 (7)0.7604 (4)0.0364 (13)
H7A0.83831.98930.74800.044*
H7B0.89931.82460.71190.044*
C40.4042 (8)1.9116 (7)0.9016 (4)0.0360 (13)
O51.0978 (6)1.3674 (6)0.6976 (3)0.0448 (10)
O120.8847 (8)1.1251 (7)0.8919 (4)0.0653 (14)
C60.9752 (8)1.4525 (7)0.7443 (3)0.0320 (12)
H7D0.549 (9)1.366 (8)0.943 (5)0.038*
H9C1.277 (9)1.789 (8)0.519 (4)0.038*
H10B1.274 (9)1.436 (8)0.404 (4)0.038*
H9D1.183 (9)1.734 (8)0.468 (4)0.038*
H12B0.863 (9)1.079 (7)0.9489 (19)0.038*
H12A1.003 (9)1.096 (8)0.905 (4)0.038*
H11A1.139 (9)1.153 (8)0.569 (4)0.038*
H11B1.056 (9)1.275 (8)0.601 (4)0.038*
H8C1.431 (8)1.513 (6)0.673 (4)0.038*
H8D1.342 (9)1.406 (8)0.661 (4)0.038*
H10A1.236 (7)1.359 (7)0.485 (4)0.038*
H7C0.658 (9)1.320 (8)0.883 (4)0.038*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co20.0246 (5)0.0372 (6)0.0258 (5)0.0104 (4)0.0010 (4)0.0109 (4)
Co10.0241 (4)0.0292 (4)0.0229 (4)0.0082 (3)0.0030 (3)0.0059 (3)
O110.035 (2)0.037 (2)0.042 (2)0.0048 (18)0.0078 (19)0.014 (2)
O60.0267 (19)0.046 (2)0.0273 (19)0.0102 (17)0.0013 (15)0.0155 (17)
O70.047 (3)0.031 (2)0.037 (2)0.0136 (19)0.0071 (19)0.0059 (18)
O40.041 (2)0.034 (2)0.031 (2)0.0088 (17)0.0063 (17)0.0093 (17)
O100.038 (2)0.057 (3)0.029 (2)0.026 (2)0.0053 (17)0.008 (2)
O90.036 (2)0.049 (3)0.062 (3)0.004 (2)0.015 (2)0.032 (2)
N10.035 (2)0.032 (2)0.025 (2)0.013 (2)0.0011 (18)0.0066 (18)
O20.032 (2)0.038 (2)0.041 (2)0.0115 (17)0.0110 (17)0.0086 (18)
N20.026 (2)0.030 (2)0.024 (2)0.0087 (18)0.0011 (17)0.0095 (18)
O10.059 (3)0.034 (2)0.058 (3)0.005 (2)0.039 (2)0.015 (2)
O80.057 (3)0.071 (3)0.035 (2)0.042 (3)0.015 (2)0.024 (2)
O30.052 (3)0.042 (3)0.068 (3)0.004 (2)0.017 (2)0.020 (2)
C50.027 (3)0.044 (3)0.032 (3)0.004 (2)0.005 (2)0.017 (2)
C90.024 (3)0.038 (3)0.021 (2)0.009 (2)0.009 (2)0.004 (2)
C80.029 (3)0.042 (3)0.034 (3)0.015 (2)0.008 (2)0.008 (2)
C30.043 (3)0.026 (3)0.039 (3)0.009 (2)0.005 (2)0.006 (2)
C20.037 (3)0.030 (3)0.036 (3)0.003 (2)0.006 (2)0.015 (2)
C10.043 (3)0.039 (3)0.027 (3)0.013 (3)0.013 (2)0.001 (2)
C70.034 (3)0.043 (3)0.037 (3)0.023 (3)0.002 (2)0.004 (3)
C40.027 (3)0.037 (3)0.042 (3)0.005 (2)0.003 (2)0.012 (3)
O50.034 (2)0.067 (3)0.047 (2)0.018 (2)0.0068 (18)0.036 (2)
O120.064 (3)0.052 (3)0.069 (3)0.006 (3)0.001 (3)0.015 (3)
C60.034 (3)0.042 (3)0.023 (3)0.016 (2)0.002 (2)0.010 (2)
Geometric parameters (Å, º) top
Co2—O9i2.044 (4)N2—C51.480 (6)
Co2—O92.044 (4)N2—C91.484 (6)
Co2—O102.097 (4)N2—C81.490 (7)
Co2—O10i2.097 (4)O1—C21.244 (6)
Co2—O8i2.120 (4)O8—O2iv2.953 (6)
Co2—O82.120 (4)O8—H8C0.90 (2)
Co1—O22.054 (4)O8—H8D0.76 (6)
Co1—O72.062 (4)O3—C41.239 (7)
Co1—O42.062 (4)C5—C61.520 (7)
Co1—O62.102 (3)C5—H5A0.9700
Co1—N12.148 (4)C5—H5B0.9700
Co1—N22.205 (4)C9—C9v1.526 (9)
O11—O1ii2.682 (6)C9—H9A0.9700
O11—H11A0.77 (6)C9—H9B0.9700
O11—H11B0.76 (6)C8—C71.526 (7)
O6—C61.253 (6)C8—H8A0.9700
O7—H7D0.81 (6)C8—H8B0.9700
O7—H7C0.79 (6)C3—C41.512 (8)
O4—C41.280 (7)C3—H3A0.9700
O10—O6iii2.783 (5)C3—H3B0.9700
O10—H10B0.77 (6)C2—C11.521 (8)
O10—H10A0.83 (2)C1—H1A0.9700
O9—O11iii2.714 (6)C1—H1B0.9700
O9—O1iv2.717 (6)C7—H7A0.9700
O9—H9C0.84 (6)C7—H7B0.9700
O9—H9D0.85 (6)O5—C61.245 (6)
N1—C11.471 (7)O12—O3ii2.895 (8)
N1—C31.480 (7)O12—H12B0.86 (2)
N1—C71.484 (7)O12—H12A0.85 (6)
O2—C21.271 (7)
O9i—Co2—O9180.000 (1)C5—N2—C9110.9 (4)
O9i—Co2—O1089.16 (18)C5—N2—C8112.5 (4)
O9—Co2—O1090.84 (18)C9—N2—C8111.4 (4)
O9i—Co2—O10i90.84 (18)C5—N2—Co1109.1 (3)
O9—Co2—O10i89.16 (18)C9—N2—Co1109.0 (3)
O10—Co2—O10i180.000 (1)C8—N2—Co1103.6 (3)
O9i—Co2—O8i91.8 (2)Co2—O8—O2iv111.7 (2)
O9—Co2—O8i88.2 (2)Co2—O8—H8C114 (4)
O10—Co2—O8i81.75 (16)O2iv—O8—H8C5 (4)
O10i—Co2—O8i98.25 (16)Co2—O8—H8D121 (5)
O9i—Co2—O888.2 (2)O2iv—O8—H8D108 (5)
O9—Co2—O891.8 (2)H8C—O8—H8D110 (6)
O10—Co2—O898.25 (16)N2—C5—C6113.9 (4)
O10i—Co2—O881.75 (16)N2—C5—H5A108.8
O8i—Co2—O8180.000 (1)C6—C5—H5A108.8
O2—Co1—O795.27 (17)N2—C5—H5B108.8
O2—Co1—O498.33 (16)C6—C5—H5B108.8
O7—Co1—O493.62 (16)H5A—C5—H5B107.7
O2—Co1—O686.14 (14)N2—C9—C9v114.8 (5)
O7—Co1—O687.02 (16)N2—C9—H9A108.6
O4—Co1—O6175.40 (15)C9v—C9—H9A108.6
O2—Co1—N180.23 (16)N2—C9—H9B108.6
O7—Co1—N1173.02 (18)C9v—C9—H9B108.6
O4—Co1—N181.83 (16)H9A—C9—H9B107.5
O6—Co1—N197.93 (16)N2—C8—C7111.2 (4)
O2—Co1—N2156.56 (16)N2—C8—H8A109.4
O7—Co1—N2101.78 (17)C7—C8—H8A109.4
O4—Co1—N296.53 (15)N2—C8—H8B109.4
O6—Co1—N278.88 (14)C7—C8—H8B109.4
N1—Co1—N284.07 (16)H8A—C8—H8B108.0
O1ii—O11—H11A8 (5)N1—C3—C4115.3 (4)
O1ii—O11—H11B106 (5)N1—C3—H3A108.5
H11A—O11—H11B106 (7)C4—C3—H3A108.5
C6—O6—Co1118.3 (3)N1—C3—H3B108.5
Co1—O7—H7D127 (4)C4—C3—H3B108.5
Co1—O7—H7C116 (5)H3A—C3—H3B107.5
H7D—O7—H7C98 (6)O1—C2—O2124.1 (5)
C4—O4—Co1115.8 (3)O1—C2—C1118.7 (5)
Co2—O10—O6iii124.94 (19)O2—C2—C1117.1 (5)
Co2—O10—H10B124 (5)N1—C1—C2111.4 (4)
O6iii—O10—H10B7 (5)N1—C1—H1A109.4
Co2—O10—H10A127 (4)C2—C1—H1A109.4
O6iii—O10—H10A105 (4)N1—C1—H1B109.4
H10B—O10—H10A104 (6)C2—C1—H1B109.4
Co2—O9—O11iii117.5 (2)H1A—C1—H1B108.0
Co2—O9—O1iv116.6 (2)N1—C7—C8109.7 (4)
O11iii—O9—O1iv109.2 (2)N1—C7—H7A109.7
Co2—O9—H9C119 (4)C8—C7—H7A109.7
O11iii—O9—H9C104 (4)N1—C7—H7B109.7
O1iv—O9—H9C5 (4)C8—C7—H7B109.7
Co2—O9—H9D114 (4)H7A—C7—H7B108.2
O11iii—O9—H9D3 (4)O3—C4—O4124.9 (5)
O1iv—O9—H9D112 (4)O3—C4—C3117.0 (5)
H9C—O9—H9D107 (6)O4—C4—C3118.0 (5)
C1—N1—C3111.3 (4)O3ii—O12—H12B85 (4)
C1—N1—C7113.9 (4)O3ii—O12—H12A4 (4)
C3—N1—C7112.7 (4)H12B—O12—H12A88 (6)
C1—N1—Co1105.4 (3)O5—C6—O6125.1 (5)
C3—N1—Co1107.7 (3)O5—C6—C5116.0 (5)
C7—N1—Co1105.2 (3)O6—C6—C5118.9 (5)
C2—O2—Co1116.0 (3)
Symmetry codes: (i) x+3, y+3, z+1; (ii) x+1, y1, z; (iii) x+2, y+3, z+1; (iv) x+1, y, z; (v) x+2, y+3, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9C···O1iv0.84 (6)1.89 (7)2.717 (6)172 (6)
O8—H8C···O2iv0.90 (2)2.06 (2)2.953 (6)172 (5)
O12—H12A···O3ii0.85 (6)2.05 (6)2.895 (8)174 (6)
O11—H11A···O1ii0.77 (6)1.92 (7)2.682 (6)169 (7)
O10—H10B···O6iii0.77 (6)2.02 (6)2.783 (5)170 (6)
O9—H9D···O11iii0.85 (6)1.87 (7)2.714 (6)175 (6)
Symmetry codes: (ii) x+1, y1, z; (iii) x+2, y+3, z+1; (iv) x+1, y, z.
 

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