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The title compound, [Co(C11H19N4O2)(C5H11)(H2O)]ClO4, is one of the coenzyme B12 models with the equatorial ligand having the same −1 formal charge as B12 corrin. In the complex, the Co atom has a distorted octahedral coordination, with the n-pentyl and water ligands in axial positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801005086/ob6033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801005086/ob6033Isup2.hkl
Contains datablock I

CCDC reference: 165628

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in solvent or counterion
  • R factor = 0.066
  • wR factor = 0.189
  • Data-to-parameter ratio = 12.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 44.00 Perc. PLAT_601 Alert C Structure Contains Solvent Accessible VOIDS of 49.00 A   3 PLAT_731 Alert C Bond Calc 0.85(3), Rep 0.849(10) .... 3.00 s.u-Ratio O1W -H1WB 1.555 1.555 PLAT_732 Alert C Angle Calc 110(4), Rep 109.8(18) .... 2.22 s.u-Ratio H1WA -O1W -H1WB 1.555 1.555 1.555 PLAT_735 Alert C D-H Calc 0.88(8), Rep 0.87(17) .... 2.12 s.u-Ratio O2 -H2 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.849(10) .... 3.00 s.u-Ratio O1W -H1WB 1.555 1.555 PLAT_737 Alert C D...A Calc 2.439(5), Rep 2.441(12) .... 2.40 s.u-Ratio O2 -O1 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
7 Alert Level C = Please check

Comment top

As important coenzyme B12 models, several Costa-type organocobalt complexes, [LCo(DO-DOH-pn)R]X, where L = neutral base, DO-DOH-pn = 3,3'-(propane-1,3-diyldinitrilo)bis(butan-2-one)dioximato, R = alkyl and X = anion group (PF6- or ClO4- etc.), have been reported (Finke et al., 1983). But only a few structures are available, especially with aqua as the axial ligand (Randaccio et al., 1989). In this report, we describe the structure of the title compound, (I), with L = H2O and R = pentyl.

The Co atom has a distorted octahedral coordination with the R and H2O ligands in axial positions (Fig. 1). The four equatorial N atoms of the DO-DOH-pn ligand are coplanar within 0.004 Å, and the Co atom is displaced by 0.025 (6) Å from this mean plane towards the axial alkyl group. The two chemically equivalent halves of the equatorial macrocycle, with the exclusion of C6, have a dihedral angle of 6.3 (7)° and bend toward the aqua ligand. Compared with the complex having R = hexyl, which we have previously reported (Xiang et al., 2000), the Co—C bond length is slightly shorter. The Co—C bond lengths are 1.993 (5) and 2.022 (5) Å for R = pentyl and hexyl, respectively. Other bond lengths and angles agree with those in related compounds (Zagrando et al., 1987; Parker et al., 1985; Marzilli et al., 1985).

Experimental top

The title compound was synthesized as described by Parker et al. (1985). A crystal suitable for X-ray diffraction was grown from an acetone–water solution in the dark under aerobic conditions.

Refinement top

The perchlorate anion shows an orientational disorder. The positional parameters of the O atoms were refined with Cl—O constrained to 1.43 (1) Å and O···O to 2.32 (2) Å. The site-occupation factor of the O11–O14 atoms was refined using a free variable as 0.729 (11) and that of the O11'–O14' atoms as 0.271 (11). The hydroxy and aqua H atoms were located from difference Fourier maps and were refined isotropically. The positional parameters of the other H atoms were calculated geometrically and were refined using a riding model.

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1995); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. ORTEP drawing of (I) with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.
Aqua(n-pentyl)[3,3'-(propane-1,3-diyldinitrilo)bis(butan-2-one)dioximato- 4N]cobalt(III)perchlorate top
Crystal data top
[Co(C5H11)(C11H19N4O2)(H2O)]ClO4F(000) = 1024
Mr = 486.84Dx = 1.433 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 17.761 (4) ÅCell parameters from 60 reflections
b = 6.6774 (13) Åθ = 5.3–10.0°
c = 19.173 (4) ŵ = 0.92 mm1
β = 96.91 (2)°T = 293 K
V = 2257.3 (8) Å3Prism, red
Z = 40.55 × 0.30 × 0.30 mm
Data collection top
Bruker P4
diffractometer
2709 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.070
Graphite monochromatorθmax = 25.0°, θmin = 2.1°
2θ/ω scansh = 121
Absorption correction: ψ scan
(North et al., 1968)
k = 17
Tmin = 0.641, Tmax = 0.759l = 2222
5163 measured reflections3 standard reflections every 97 reflections
3956 independent reflections intensity decay: 9.7%
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.189H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.1023P)2 + 2.2665P]
where P = (Fo2 + 2Fc2)/3
3956 reflections(Δ/σ)max < 0.001
313 parametersΔρmax = 0.56 e Å3
59 restraintsΔρmin = 0.79 e Å3
Crystal data top
[Co(C5H11)(C11H19N4O2)(H2O)]ClO4V = 2257.3 (8) Å3
Mr = 486.84Z = 4
Monoclinic, P21/nMo Kα radiation
a = 17.761 (4) ŵ = 0.92 mm1
b = 6.6774 (13) ÅT = 293 K
c = 19.173 (4) Å0.55 × 0.30 × 0.30 mm
β = 96.91 (2)°
Data collection top
Bruker P4
diffractometer
2709 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.070
Tmin = 0.641, Tmax = 0.7593 standard reflections every 97 reflections
5163 measured reflections intensity decay: 9.7%
3956 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06659 restraints
wR(F2) = 0.189H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.56 e Å3
3956 reflectionsΔρmin = 0.79 e Å3
313 parameters
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*/UeqOcc. (<1)
Co10.21442 (3)1.25797 (10)0.45904 (3)0.0355 (2)
N10.2254 (2)1.4165 (6)0.3801 (2)0.0406 (10)
N20.1520 (2)1.1049 (6)0.3910 (2)0.0438 (10)
N30.2022 (3)1.1065 (7)0.5413 (2)0.0475 (11)
N40.2745 (2)1.4159 (7)0.5252 (2)0.0450 (10)
O10.2657 (2)1.5843 (5)0.3831 (2)0.0514 (9)
O20.3087 (2)1.5841 (6)0.5088 (2)0.0584 (11)
H20.298 (4)1.587 (10)0.463 (4)0.070*
C10.1845 (4)1.4823 (11)0.2565 (3)0.0722 (19)
H1A0.20791.61020.26680.108*
H1B0.13261.50130.23700.108*
H1C0.21121.41250.22320.108*
C20.1873 (3)1.3629 (9)0.3221 (3)0.0460 (13)
C30.1449 (3)1.1768 (9)0.3289 (3)0.0488 (13)
C40.0994 (4)1.0879 (12)0.2659 (4)0.082 (2)
H4A0.07430.96940.27940.123*
H4B0.13241.05400.23150.123*
H4C0.06231.18320.24620.123*
C50.1146 (4)0.9197 (9)0.4084 (4)0.0638 (17)
H5A0.14870.80760.40470.077*
H5B0.06980.89870.37500.077*
C60.0925 (3)0.9277 (9)0.4811 (4)0.0653 (18)
H6A0.05920.81550.48720.078*
H6B0.06371.04950.48590.078*
C70.1573 (4)0.9222 (9)0.5388 (4)0.0680 (18)
H7A0.13780.90360.58350.082*
H7B0.18970.80890.53150.082*
C80.2344 (5)1.0920 (14)0.6695 (3)0.088 (2)
H8A0.22020.95340.66500.132*
H8B0.19811.16280.69340.132*
H8C0.28371.10300.69590.132*
C90.2363 (3)1.1800 (10)0.5984 (3)0.0534 (15)
C100.2786 (3)1.3644 (10)0.5899 (3)0.0531 (14)
C110.3195 (5)1.4819 (13)0.6477 (4)0.087 (2)
H11A0.35351.57370.62890.131*
H11B0.34791.39300.68030.131*
H11C0.28371.55530.67140.131*
C120.3035 (3)1.0888 (8)0.4441 (3)0.0451 (12)
H12A0.31981.01930.48770.054*
H12B0.28650.98770.40940.054*
C130.3715 (3)1.1902 (9)0.4208 (3)0.0572 (15)
H13A0.39001.29060.45520.069*
H13B0.35681.25770.37640.069*
C140.4342 (3)1.0432 (11)0.4121 (3)0.0620 (17)
H14A0.44950.97950.45710.074*
H14B0.41440.93970.37950.074*
C150.5022 (4)1.1325 (15)0.3865 (4)0.095 (3)
H15A0.52311.23230.42010.114*
H15B0.48651.20100.34250.114*
C160.5640 (4)0.9850 (17)0.3750 (5)0.123 (4)
H16A0.60701.05600.36160.184*
H16B0.54550.89300.33840.184*
H16C0.57870.91240.41760.184*
Cl10.05350 (9)1.4968 (3)0.34438 (8)0.0691 (5)
O110.0698 (6)1.6479 (14)0.3937 (5)0.136 (4)0.729 (11)
O120.0058 (7)1.5779 (19)0.3001 (5)0.134 (5)0.729 (11)
O130.1226 (5)1.422 (2)0.3136 (8)0.156 (6)0.729 (11)
O140.0111 (5)1.3465 (14)0.3873 (5)0.127 (4)0.729 (11)
O1W0.1210 (2)1.4376 (6)0.4753 (2)0.0493 (9)
H1WA0.117 (3)1.415 (9)0.5183 (8)0.059*
H1WB0.0781 (15)1.424 (9)0.4510 (19)0.059*
O11'0.0731 (18)1.671 (3)0.3023 (14)0.164 (12)0.271 (11)
O12'0.0883 (15)1.326 (3)0.3105 (14)0.145 (13)0.271 (11)
O13'0.0645 (19)1.520 (5)0.4148 (7)0.183 (11)0.271 (11)
O14'0.0262 (6)1.476 (4)0.3418 (15)0.135 (10)0.271 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0351 (4)0.0337 (4)0.0388 (4)0.0032 (3)0.0084 (2)0.0021 (3)
N10.039 (2)0.036 (2)0.048 (2)0.0045 (19)0.0108 (19)0.0028 (19)
N20.033 (2)0.035 (2)0.063 (3)0.0005 (18)0.0037 (19)0.004 (2)
N30.049 (3)0.041 (2)0.056 (3)0.012 (2)0.021 (2)0.013 (2)
N40.043 (2)0.047 (3)0.046 (3)0.005 (2)0.0076 (19)0.006 (2)
O10.051 (2)0.041 (2)0.064 (2)0.0085 (17)0.0093 (18)0.0100 (18)
O20.063 (3)0.047 (2)0.065 (2)0.011 (2)0.005 (2)0.009 (2)
C10.077 (4)0.090 (5)0.048 (3)0.004 (4)0.003 (3)0.015 (3)
C20.042 (3)0.054 (3)0.042 (3)0.005 (3)0.003 (2)0.007 (3)
C30.039 (3)0.056 (3)0.049 (3)0.010 (3)0.002 (2)0.010 (3)
C40.062 (4)0.095 (5)0.083 (5)0.001 (4)0.015 (4)0.023 (4)
C50.053 (3)0.040 (3)0.099 (5)0.006 (3)0.011 (3)0.004 (3)
C60.047 (3)0.041 (3)0.113 (5)0.000 (3)0.033 (4)0.012 (3)
C70.079 (4)0.050 (4)0.082 (4)0.008 (3)0.036 (4)0.020 (3)
C80.098 (5)0.117 (7)0.053 (4)0.033 (5)0.025 (4)0.026 (4)
C90.057 (3)0.060 (4)0.046 (3)0.023 (3)0.018 (3)0.010 (3)
C100.051 (3)0.067 (4)0.041 (3)0.018 (3)0.003 (2)0.005 (3)
C110.098 (5)0.108 (6)0.053 (4)0.015 (5)0.004 (4)0.016 (4)
C120.040 (3)0.049 (3)0.046 (3)0.008 (2)0.006 (2)0.001 (2)
C130.043 (3)0.065 (4)0.066 (4)0.008 (3)0.018 (3)0.002 (3)
C140.042 (3)0.100 (5)0.043 (3)0.016 (3)0.002 (2)0.006 (3)
C150.056 (4)0.135 (8)0.101 (6)0.019 (5)0.036 (4)0.007 (6)
C160.067 (5)0.212 (12)0.093 (6)0.050 (7)0.022 (4)0.010 (7)
Cl10.0502 (8)0.1036 (14)0.0546 (9)0.0016 (9)0.0114 (7)0.0000 (9)
O110.194 (10)0.113 (8)0.121 (8)0.051 (8)0.097 (7)0.013 (6)
O120.150 (10)0.179 (12)0.083 (6)0.078 (9)0.054 (6)0.015 (6)
O130.077 (7)0.190 (13)0.180 (10)0.040 (7)0.071 (7)0.061 (9)
O140.077 (6)0.123 (7)0.174 (10)0.014 (6)0.017 (6)0.030 (7)
O1W0.045 (2)0.044 (2)0.061 (2)0.0123 (18)0.0125 (17)0.002 (2)
O11'0.15 (2)0.16 (2)0.18 (2)0.06 (2)0.01 (2)0.05 (2)
O12'0.10 (2)0.20 (3)0.114 (18)0.09 (2)0.049 (17)0.02 (2)
O13'0.28 (2)0.16 (2)0.122 (19)0.00 (2)0.073 (19)0.008 (18)
O14'0.123 (17)0.15 (2)0.14 (2)0.041 (16)0.068 (16)0.023 (17)
Geometric parameters (Å, º) top
Co1—N11.876 (4)Cl1—O141.450 (6)
Co1—N41.880 (4)O2—H20.87 (7)
Co1—N21.905 (4)C1—H1A0.9600
Co1—N31.908 (4)C1—H1B0.9600
Co1—C121.993 (5)C1—H1C0.9600
Co1—O1W2.100 (3)C4—H4A0.9600
N1—C21.281 (7)C4—H4B0.9600
N1—O11.327 (5)C4—H4C0.9600
N2—C31.276 (7)C5—H5A0.9700
N2—C51.461 (7)C5—H5B0.9700
N3—C91.284 (7)C6—H6A0.9700
N3—C71.464 (8)C6—H6B0.9700
N4—C101.280 (7)C7—H7A0.9700
N4—O21.332 (6)C7—H7B0.9700
C1—C21.485 (8)C8—H8A0.9600
C2—C31.467 (8)C8—H8B0.9600
C3—C41.492 (8)C8—H8C0.9600
C5—C61.496 (9)C11—H11A0.9600
C6—C71.498 (9)C11—H11B0.9600
C8—C91.488 (8)C11—H11C0.9600
C9—C101.462 (9)C12—H12A0.9700
C10—C111.475 (9)C12—H12B0.9700
C12—C131.498 (7)C13—H13A0.9700
C13—C141.509 (8)C13—H13B0.9700
C14—C151.482 (9)C14—H14A0.9700
C15—C161.511 (11)C14—H14B0.9700
Cl1—O121.380 (6)C15—H15A0.9700
Cl1—O131.391 (7)C15—H15B0.9700
Cl1—O13'1.396 (9)C16—H16A0.9600
Cl1—O12'1.416 (9)C16—H16B0.9600
Cl1—O14'1.430 (9)C16—H16C0.9600
Cl1—O111.436 (7)O1W—H1WA0.850 (10)
Cl1—O11'1.437 (9)O1W—H1WB0.849 (10)
N1—Co1—N497.0 (2)O11—Cl1—O14104.1 (6)
N1—Co1—N281.86 (19)O11'—Cl1—O14162.7 (13)
N4—Co1—N2178.32 (19)N4—O2—H2102 (5)
N1—Co1—N3177.65 (18)C2—C1—H1A109.5
N4—Co1—N381.4 (2)C2—C1—H1B109.5
N2—Co1—N399.6 (2)H1A—C1—H1B109.5
N1—Co1—C1292.4 (2)C2—C1—H1C109.5
N4—Co1—C1291.1 (2)H1A—C1—H1C109.5
N2—Co1—C1290.2 (2)H1B—C1—H1C109.5
N3—Co1—C1289.4 (2)C3—C4—H4A109.5
N1—Co1—O1W87.62 (16)C3—C4—H4B109.5
N4—Co1—O1W88.50 (17)H4A—C4—H4B109.5
N2—Co1—O1W90.19 (17)C3—C4—H4C109.5
N3—Co1—O1W90.56 (17)H4A—C4—H4C109.5
C12—Co1—O1W179.6 (2)H4B—C4—H4C109.5
C2—N1—O1119.9 (4)N2—C5—H5A109.4
C2—N1—Co1116.6 (4)C6—C5—H5A109.4
O1—N1—Co1123.3 (3)N2—C5—H5B109.4
C3—N2—C5122.3 (5)C6—C5—H5B109.4
C3—N2—Co1114.9 (4)H5A—C5—H5B108.0
C5—N2—Co1122.7 (4)C5—C6—H6A108.5
C9—N3—C7123.2 (5)C7—C6—H6A108.5
C9—N3—Co1114.5 (4)C5—C6—H6B108.5
C7—N3—Co1122.3 (4)C7—C6—H6B108.5
C10—N4—O2118.7 (5)H6A—C6—H6B107.5
C10—N4—Co1117.7 (4)N3—C7—H7A109.3
O2—N4—Co1123.5 (3)C6—C7—H7A109.3
N1—C2—C3112.5 (5)N3—C7—H7B109.3
N1—C2—C1123.1 (5)C6—C7—H7B109.3
C3—C2—C1124.4 (5)H7A—C7—H7B107.9
N2—C3—C2114.0 (5)C9—C8—H8A109.5
N2—C3—C4126.1 (6)C9—C8—H8B109.5
C2—C3—C4119.9 (6)H8A—C8—H8B109.5
N2—C5—C6111.2 (5)C9—C8—H8C109.5
C5—C6—C7115.0 (5)H8A—C8—H8C109.5
N3—C7—C6111.8 (5)H8B—C8—H8C109.5
N3—C9—C10115.0 (5)C10—C11—H11A109.5
N3—C9—C8124.8 (7)C10—C11—H11B109.5
C10—C9—C8120.3 (6)H11A—C11—H11B109.5
N4—C10—C9111.4 (5)C10—C11—H11C109.5
N4—C10—C11123.4 (6)H11A—C11—H11C109.5
C9—C10—C11125.2 (6)H11B—C11—H11C109.5
C13—C12—Co1118.0 (4)C13—C12—H12A107.8
C12—C13—C14111.8 (5)Co1—C12—H12A107.8
C15—C14—C13114.6 (6)C13—C12—H12B107.8
C14—C15—C16114.9 (8)Co1—C12—H12B107.8
O12—Cl1—O13117.2 (7)H12A—C12—H12B107.2
O12—Cl1—O13'136.0 (14)C12—C13—H13A109.3
O13—Cl1—O13'103.3 (16)C14—C13—H13A109.3
O12—Cl1—O12'107.5 (13)C12—C13—H13B109.3
O13—Cl1—O12'36.9 (12)C14—C13—H13B109.3
O13'—Cl1—O12'115.3 (13)H13A—C13—H13B107.9
O12—Cl1—O14'48.2 (10)C15—C14—H14A108.6
O13—Cl1—O14'141.1 (12)C13—C14—H14A108.6
O13'—Cl1—O14'107.4 (13)C15—C14—H14B108.6
O12'—Cl1—O14'106.5 (12)C13—C14—H14B108.6
O12—Cl1—O11108.4 (6)H14A—C14—H14B107.6
O13—Cl1—O11107.2 (7)C14—C15—H15A108.5
O13'—Cl1—O1139.0 (12)C16—C15—H15A108.5
O12'—Cl1—O11139.1 (13)C14—C15—H15B108.5
O14'—Cl1—O11111.7 (11)C16—C15—H15B108.5
O12—Cl1—O11'57.4 (11)H15A—C15—H15B107.5
O13—Cl1—O11'85.0 (13)C15—C16—H16A109.5
O13'—Cl1—O11'113.7 (13)C15—C16—H16B109.5
O12'—Cl1—O11'109.4 (12)H16A—C16—H16B109.5
O14'—Cl1—O11'103.5 (12)C15—C16—H16C109.5
O11—Cl1—O11'75.3 (12)H16A—C16—H16C109.5
O12—Cl1—O14107.8 (7)H16B—C16—H16C109.5
O13—Cl1—O14111.2 (6)Co1—O1W—H1WA102 (4)
O13'—Cl1—O1469.5 (13)Co1—O1W—H1WB122 (4)
O12'—Cl1—O1482.6 (12)H1WA—O1W—H1WB109.8 (18)
O14'—Cl1—O1460.2 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O11i0.85 (1)2.01 (2)2.830 (13)160 (4)
O2—H2···O10.87 (17)1.57 (7)2.441 (12)170 (6)
O1W—H1WB···O140.85 (1)1.95 (18)2.788 (14)168 (6)
Symmetry code: (i) x, y+3, z+1.

Experimental details

Crystal data
Chemical formula[Co(C5H11)(C11H19N4O2)(H2O)]ClO4
Mr486.84
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)17.761 (4), 6.6774 (13), 19.173 (4)
β (°) 96.91 (2)
V3)2257.3 (8)
Z4
Radiation typeMo Kα
µ (mm1)0.92
Crystal size (mm)0.55 × 0.30 × 0.30
Data collection
DiffractometerBruker P4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.641, 0.759
No. of measured, independent and
observed [I > 2σ(I)] reflections
5163, 3956, 2709
Rint0.070
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.066, 0.189, 1.04
No. of reflections3956
No. of parameters313
No. of restraints59
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.56, 0.79

Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Siemens, 1995), SHELXTL.

Selected geometric parameters (Å, º) top
Co1—N11.876 (4)N2—C31.276 (7)
Co1—N41.880 (4)N2—C51.461 (7)
Co1—N21.905 (4)N3—C91.284 (7)
Co1—N31.908 (4)N3—C71.464 (8)
Co1—C121.993 (5)N4—C101.280 (7)
Co1—O1W2.100 (3)N4—O21.332 (6)
N1—C21.281 (7)C5—C61.496 (9)
N1—O11.327 (5)C6—C71.498 (9)
N1—Co1—N497.0 (2)N3—Co1—C1289.4 (2)
N1—Co1—N281.86 (19)N1—Co1—O1W87.62 (16)
N4—Co1—N2178.32 (19)N4—Co1—O1W88.50 (17)
N1—Co1—N3177.65 (18)N2—Co1—O1W90.19 (17)
N4—Co1—N381.4 (2)N3—Co1—O1W90.56 (17)
N2—Co1—N399.6 (2)C12—Co1—O1W179.6 (2)
N1—Co1—C1292.4 (2)N2—C5—C6111.2 (5)
N4—Co1—C1291.1 (2)C5—C6—C7115.0 (5)
N2—Co1—C1290.2 (2)N3—C7—C6111.8 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O11i0.850 (10)2.01 (2)2.830 (13)160 (4)
O2—H2···O10.87 (17)1.57 (7)2.441 (12)170 (6)
O1W—H1WB···O140.849 (10)1.95 (18)2.788 (14)168 (6)
Symmetry code: (i) x, y+3, z+1.
 

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