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The title cobalt(II) coordination polymers, [Co3(C9H3O6)2(C14H14N4)3]n, (I), and {[Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2O}n, (II), present very different coordination and packing properties in spite of the ligand similarity. In (I), three crystallographically distinct CoII cations are all four-coordinated by O2N2 donor sets in distorted tetra­hedral geometries. The CoII centres are connected by benzene-1,3,5-tricarboxyl­ate (BTC) anions and 1,3-bis­(imidazol-1-yl­methyl)­benzene (L1) ligands into a (64.82)2(86)(6.82)2 topology framework. The structure of (II) contains two kinds of crystallographically unique CoII cations. One Co atom lies on a symmetry centre and is six-coordinated by an O4N2 donor set, and the other Co atom is four-coordinated by an O2N2 donor set. The CoII centres are connected by BTC anions and 1,4-bis­(imidazol-1-yl­methyl)­benzene (L2) ligands into a (62.84)2(64.82)(63)2 framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107059124/bg3062sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107059124/bg3062Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107059124/bg3062IIsup3.hkl
Contains datablock II

CCDC references: 660610; 677093

Comment top

Extended framework solids are of current importance because they may offer new materials with a range of potentially useful properties, as well as intriguing molecular topological nets and entanglements (Huang et al., 2004; Kitagawa et al., 2004). The main strategy popularly used in this area is a building-block approach (Eddaoudi et al., 2001), and much effort has been made towards the connection of suitable predetermined building blocks into networks in order to obtain the desired materials. In this regard, the characterization of metal–organic hybrid materials based on carboxylates and flexible ligands is a domain of special interest (Li et al., 2006; Lu et al., 2007). As an extension of our previous work (Yang et al., 2006), we present here the two title compounds, (I) and (II), both of which were obtained by combining benzenetricarboxylic and bis(imidazole) ligands and both of which yield (3,4)-connected non-uniform entangled frameworks.

As shown in Fig. 1, the structure of (I) contains three crystallographically distinct CoII cations, two kinds of unique BTC anions and three kinds of unique L1 ligands. Each CoII cation has a distorted tetrahedral coordination environment and is coordinated by two O atoms from two BTC anions and two N atoms from two L1 ligands (Table 1). Each BTC anion coordinates to three CoII ions, and a rhomb-like chain propagated by BTC anions via fusing CoII cations is formed along the c axis (Fig. 2a).

The three crystallographically distinct L1 ligands adopt two kinds of conformations. One is in a trans conformation (Sun et al., 2000), with a Co···Co distance of 13.870 (3) Å. Each trans L1 molecule coordinates to two Co3 cations, acting as a bridging ligand to form an infinite zigzag chain structure. The [Co3(BTC)2] chains are extended by these zigzag chains to form a two-dimensional network (Fig. 2b). The other two L1 ligands display cis conformations (Hammes et al., 2005), linking cations at Co···Co distances of 7.275 (2) and 7.416 (2) Å. Atoms Co1 and Co2 are connected by cis L1 ligands to form a helix (Fig. 2c). These helices further link the two-dimensional networks, as shown in Fig. 2(b), to form a complicated three-dimensional structure. If the BTC anions are considered as three-connected nodes, the structure of (I) can be simplified to a unique (3,4)-connected net with (64.82)2(86)(6.82)2 topology (Fig. 2d) (Wells, 1977, 1979; Dolomanov et al., 2003).

A related compound, (III) (Liu et al., 2007), displays a quite different structure, though it features the same general formula as (I), {[Co3(BTC)2(L1)3]}n. The structure of (III) can be symbolized as a net with (64.82)2(62.82.102)(63)2 topology. Although it is hard to propose definitive reasons as to why compounds (I) and (III) adopt different configurations, it can be speculated that pH values may exert an important influence on the resulting architectures.

As illustrated in Fig. 3, the structure of (II) contains two unique CoII cations (one of them, Co1, lies on an inversion centre), one BTC anion and two unique L2 ligands, one of which is also bisected by a symmetry centre. Atom Co1 is six-coordinated by two O atoms from two BTC anions, two aqua ligands and two N atoms from two L2 ligands. Atom Co2 is four-coordinated by two O atoms from two BTC anions and two N atoms from two L2 ligands (Table 2). Each BTC anion coordinates to three CoII cations, and the Co atoms are bridged by BTC anions to form a ladder (Fig. 4a). The two unique L2 ligands display different conformations. One L2 ligand shows a cis conformation (Carlucci et al., 2005), spanning a Co···Co distance of 11.782 (3) Å, while the other adopts a trans conformation instead (Fan et al., 2006), with a Co···Co distance of 14.388 (3) Å. The [Co3(BTC)2] ladders are connected by these two L2 ligands to form two kinds of two-dimensional networks (Figs. 4b and 4c) The whole structure displays a unique (3,4)-connected three-dimensional framework (Fig. 4d). The structure can be symbolized as a net with (62.84)2(64.82)(63)2 topology, with the BTC anions being considered as three-connected nodes. The solvent water molecule is hydrogen-bonded to the organic unit (Table 3).

Related literature top

For related literature, see: Carlucci et al. (2005); Dolomanov et al. (2003); Eddaoudi et al. (2001); Fan et al. (2006); Flack (1983); Hammes et al. (2005); Huang et al. (2004); Kitagawa et al. (2004); Li et al. (2006); Liu et al. (2007); Lu et al. (2007); Spek (2003); Sun et al. (2000); Wells (1977, 1979); Yang et al. (2006).

Experimental top

The ligands L1 and L2 were synthesized according to the literature (Liu et al., 2007). A mixture of Co(NO3)2·6H2O (0.12 g, 0.45 mmol), H3BTC (0.06 g, 0.30 mmol), L1 (0.11 g, 0.45 mmol) and water (7 ml) was stirred for 10 min in air. The mixture was sealed in a Teflon reactor (15 ml) and heated at 433 K for 3 d. After the mixture had been cooled to room temperature at 10 K h-1, purple crystals of (I) were obtained.

A mixture of Co(NO3)2·6H2O (0.12 g, 0.45 mmol), H3BTC (0.10 g, 0.15 mmol), L2 (0.11 g, 0.45 mmol) and water (7 ml) was stirred for 10 min in air. The mixture was sealed in a Teflon reactor and heated at 433 K for 3 d. After the mixture had been cooled to room temperature at 10 K h-1, purple crystals of (II) were obtained.

Refinement top

A PLATON (Spek, 2003) alert on a possible C2/c symmetry in structure (I) proved to be false, since the position of the eventual symmetry centre was incompatible with the remaining symmetry elements. In addition, the structure presented a refined Flack parameter (Flack, 1983) of 0.246 (10), suggesting a considerable degree of inversion twinning.

H atoms bound to carbon were located in idealized positions and refined using a riding model, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic H, and C—H = 0.97 Å and Uiso(H) = 1.5Ueq(C) for CH2 atoms. Water H atoms were located in a difference Fourier map and refined as riding, with Uiso(H) = 1.5Ueq(O).

Computing details top

For both compounds, data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. A view of the local coordination of the CoII cations in (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) x, -y + 1, z + 1/2; (ii) x, -y + 1, z - 1/2; (iii) x - 1/2, y - 1/2, z - 1; (iv) x - 1/2, y + 1/2, z - 1; (v) x, -y - 1, z - 1/2.]
[Figure 2] Fig. 2. (a) Side and front views of the one-dimensional rhomb-like chain constructed from CoII atoms and BTC anions in (I). (b) The two-dimensional structure of (I) extended by trans L1 ligands between adjacent [Co3(BTC)2] chains. (c) The helix formed by CoII and the cis L1 ligands in (I). (d) Schematic diagram (OLEX; Dolomanov et al., 2003) showing the (64.82)2(86)(6.82)2 topology network of (I).
[Figure 3] Fig. 3. A view of the local coordination of the CoII cations in (II), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) -x, -y, -z; (ii) x, y - 1, z; (iii) x - 1, -y - 1/2, z + 1/2.]
[Figure 4] Fig. 4. (a) View of the one-dimensional ladder made of CoII atoms and BTC anions in (II). (b) The extended two-dimensional structure of (II) when trans L2 ligands are neglected. (c) The extended two-dimensional structure of (II) when cis L2 ligands are neglected. (d) Schematic diagram (OLEX; Dolomanov et al., 2003) showing the (62.84)2(64.82)(63)2 topology network of (II).
(I) Poly[bis[µ3-benzene-1,3,5-tricarboxylato- κ3O1:O3:O5]tris[µ2-1,3-bis(imidazol-1- ylmethyl)benzene-κ2N:N']tricobalt(II)] top
Crystal data top
[Co3(C9H3O6)2(C14H14N4)3]F(000) = 2676
Mr = 1305.89Dx = 1.493 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71069 Å
Hall symbol: C -2ycCell parameters from 10356 reflections
a = 40.152 (9) Åθ = 3.2–27.5°
b = 8.353 (3) ŵ = 0.92 mm1
c = 18.842 (5) ÅT = 293 K
β = 113.138 (9)°Block, purple
V = 5811 (3) Å30.33 × 0.26 × 0.22 mm
Z = 4
Data collection top
Bruker APEX CCD area-detector
diffractometer
11621 independent reflections
Radiation source: fine-focus sealed tube10356 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 4952
Tmin = 0.74, Tmax = 0.82k = 1010
27961 measured reflectionsl = 2422
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.091 w = 1/[σ2(Fo2) + (0.0519P)2 + 1.8287P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.003
11621 reflectionsΔρmax = 1.08 e Å3
800 parametersΔρmin = 0.44 e Å3
2 restraintsAbsolute structure: Flack (1983), with how many Friedel pairs?
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.246 (10)
Crystal data top
[Co3(C9H3O6)2(C14H14N4)3]V = 5811 (3) Å3
Mr = 1305.89Z = 4
Monoclinic, CcMo Kα radiation
a = 40.152 (9) ŵ = 0.92 mm1
b = 8.353 (3) ÅT = 293 K
c = 18.842 (5) Å0.33 × 0.26 × 0.22 mm
β = 113.138 (9)°
Data collection top
Bruker APEX CCD area-detector
diffractometer
11621 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
10356 reflections with I > 2σ(I)
Tmin = 0.74, Tmax = 0.82Rint = 0.028
27961 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.091Δρmax = 1.08 e Å3
S = 1.04Δρmin = 0.44 e Å3
11621 reflectionsAbsolute structure: Flack (1983), with how many Friedel pairs?
800 parametersAbsolute structure parameter: 0.246 (10)
2 restraints
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
Co10.833700 (10)0.34795 (5)0.23552 (2)0.02758 (10)
Co21.218513 (10)0.36283 (5)0.911351 (19)0.02835 (10)
Co31.023204 (13)0.89066 (5)0.55868 (2)0.03528 (12)
C10.87670 (9)0.5196 (4)0.46064 (18)0.0317 (7)
C20.91145 (9)0.5659 (4)0.46960 (18)0.0366 (7)
H20.91890.55130.42920.044*
C30.93475 (9)0.6328 (4)0.5376 (2)0.0370 (7)
C40.92436 (9)0.6514 (4)0.5987 (2)0.0350 (8)
H40.94000.69930.64410.042*
C50.89031 (9)0.5982 (4)0.59222 (18)0.0295 (6)
C60.86669 (8)0.5353 (4)0.52355 (18)0.0295 (6)
H60.84380.50280.51880.035*
C70.85084 (10)0.4542 (4)0.38543 (19)0.0348 (7)
C80.97110 (9)0.6922 (5)0.5430 (2)0.0450 (8)
C90.88050 (8)0.6222 (4)0.66050 (18)0.0291 (6)
C101.12204 (8)0.6835 (4)0.6147 (2)0.0340 (7)
C111.14568 (8)0.6205 (4)0.68378 (17)0.0327 (7)
H111.14040.62950.72740.039*
C121.17730 (8)0.5439 (4)0.68921 (17)0.0277 (6)
C131.18618 (8)0.5378 (4)0.62540 (16)0.0275 (6)
H131.20770.48950.62910.033*
C141.16285 (8)0.6042 (4)0.55538 (17)0.0276 (6)
C151.13070 (9)0.6730 (4)0.55022 (19)0.0323 (7)
H151.11460.71280.50310.039*
C161.08718 (9)0.7633 (4)0.6087 (2)0.0429 (8)
C171.20172 (9)0.4692 (4)0.76449 (17)0.0305 (6)
C181.17257 (9)0.6058 (4)0.48580 (16)0.0305 (6)
C191.01976 (14)1.3358 (5)0.3083 (2)0.0616 (12)
C201.04275 (14)1.3972 (5)0.2765 (2)0.0603 (11)
H201.04781.33650.24060.072*
C211.05817 (11)1.5446 (5)0.2965 (2)0.0490 (9)
C221.05093 (12)1.6375 (5)0.3492 (2)0.0535 (10)
H221.06111.73880.36210.064*
C231.02850 (14)1.5786 (6)0.3824 (3)0.0663 (12)
H231.02391.63970.41890.080*
C241.01265 (14)1.4293 (6)0.3622 (3)0.0657 (12)
H240.99721.39120.38450.079*
C251.0050 (2)1.1705 (7)0.2856 (3)0.0811 (2)
H25A0.98471.17520.23600.097*
H25B1.02351.10380.27970.097*
C261.08276 (11)1.6076 (6)0.2591 (3)0.0622 (11)
H26A1.10081.67810.29490.075*
H26B1.09531.51880.24740.075*
C271.01427 (11)1.0163 (4)0.4050 (2)0.0494 (8)
H271.03850.99160.41680.059*
C280.96044 (14)1.1094 (7)0.3456 (4)0.100 (2)
H280.94031.16030.30970.120*
C290.96214 (11)1.0353 (6)0.4103 (3)0.0726 (13)
H290.94321.02570.42680.087*
C301.05916 (9)1.8534 (5)0.1766 (2)0.0454 (8)
H301.07221.92930.21310.054*
C311.03846 (12)1.6258 (5)0.1212 (3)0.0547 (10)
H311.03401.51700.11140.066*
C321.02334 (13)1.7432 (4)0.0738 (2)0.0483 (8)
H321.00641.73010.02350.058*
C330.66493 (9)0.3935 (4)0.0907 (2)0.0411 (8)
C340.67292 (10)0.3682 (4)0.0262 (2)0.0411 (8)
H340.69570.39670.02840.049*
C350.64825 (10)0.3023 (4)0.0407 (2)0.0439 (8)
C360.61506 (11)0.2488 (6)0.0404 (3)0.0637 (12)
H360.59820.19880.08380.076*
C370.60758 (12)0.2704 (7)0.0240 (3)0.0771 (15)
H370.58550.23590.02350.092*
C380.63196 (11)0.3413 (5)0.0888 (3)0.0608 (11)
H380.62640.35470.13190.073*
C390.69031 (10)0.4763 (6)0.1622 (2)0.0493 (9)
H39A0.68080.58180.16490.059*
H39B0.69130.41630.20700.059*
C400.65591 (12)0.2791 (5)0.1116 (2)0.0527 (10)
H40A0.66460.17080.11210.063*
H40B0.63360.29220.15690.063*
C410.75422 (9)0.3932 (5)0.2001 (2)0.0395 (7)
H410.75320.30690.23040.047*
C420.77332 (10)0.5634 (5)0.1397 (2)0.0454 (9)
H420.78830.61670.12030.054*
C430.73872 (11)0.6045 (5)0.1258 (2)0.0500 (9)
H430.72560.68970.09610.060*
C440.68079 (11)0.5527 (4)0.1113 (2)0.0443 (8)
H440.66050.60600.11090.053*
C450.71658 (12)0.3625 (5)0.1148 (3)0.0569 (12)
H450.72630.26210.11620.068*
C460.73280 (12)0.5052 (5)0.1118 (3)0.0574 (11)
H460.75570.51950.11230.069*
C470.90247 (12)0.2141 (5)0.2008 (3)0.0539 (10)
C480.87886 (11)0.1601 (5)0.1295 (3)0.0522 (11)
H480.85440.15020.12030.063*
C490.88990 (11)0.1212 (5)0.0726 (3)0.0539 (10)
C500.92663 (13)0.1419 (8)0.0876 (4)0.0871 (19)
H500.93530.11440.05030.104*
C510.94985 (14)0.2023 (9)0.1570 (4)0.105 (2)
H510.97390.22160.16500.126*
C520.93837 (13)0.2346 (7)0.2146 (3)0.0754 (14)
H520.95460.27020.26240.090*
C530.89022 (15)0.2455 (5)0.2657 (3)0.0686 (13)
H53A0.87960.35150.25960.082*
H53B0.91100.24290.31450.082*
C540.86549 (11)0.0512 (7)0.0032 (3)0.0683 (13)
H54A0.87560.05000.01040.082*
H54B0.86500.12260.04420.082*
C550.86523 (10)0.0307 (5)0.2551 (2)0.0477 (9)
H550.88460.07770.24760.057*
C560.83185 (12)0.1475 (5)0.2756 (3)0.0569 (11)
H560.82300.24480.28480.068*
C570.81559 (12)0.0032 (5)0.2682 (3)0.0577 (11)
H570.79340.01600.27160.069*
C580.79931 (10)0.1172 (5)0.0483 (2)0.0443 (8)
H580.79970.20400.07890.053*
C590.81691 (11)0.0885 (5)0.0286 (3)0.0558 (10)
H590.83100.16920.06030.067*
C600.78207 (11)0.0606 (5)0.0121 (2)0.0508 (9)
H600.76750.11930.03060.061*
N10.99640 (7)0.9767 (4)0.44781 (17)0.0465 (7)
N20.99305 (12)1.0966 (5)0.3421 (2)0.0742 (12)
N31.06230 (8)1.6941 (4)0.18881 (18)0.0462 (7)
N41.03573 (8)1.8886 (4)0.10787 (17)0.0450 (7)
N50.78300 (7)0.4332 (4)0.18614 (16)0.0371 (6)
N60.72710 (7)0.4932 (4)0.16494 (18)0.0393 (6)
N70.68316 (9)0.3936 (4)0.11539 (18)0.0432 (7)
N80.71057 (9)0.6254 (4)0.10782 (17)0.0412 (7)
N90.83720 (8)0.1105 (3)0.25486 (16)0.0375 (6)
N100.86308 (9)0.1245 (3)0.2673 (2)0.0470 (8)
N110.82815 (9)0.0243 (4)0.01004 (19)0.0507 (8)
N120.77082 (8)0.0709 (4)0.03729 (16)0.0388 (6)
O10.82100 (8)0.4022 (4)0.37739 (16)0.0633 (9)
O20.86234 (7)0.4545 (3)0.33092 (13)0.0437 (6)
O30.98440 (8)0.6394 (4)0.49879 (19)0.0644 (8)
O40.98665 (7)0.8021 (4)0.59319 (16)0.0507 (7)
O50.90235 (7)0.6743 (4)0.72135 (15)0.0462 (6)
O60.84740 (6)0.5887 (3)0.64960 (12)0.0374 (5)
O71.06634 (6)0.8080 (3)0.54352 (15)0.0453 (6)
O81.08047 (8)0.7802 (4)0.66712 (17)0.0662 (9)
O91.19166 (7)0.4901 (3)0.82024 (13)0.0385 (5)
O101.22859 (7)0.3927 (4)0.77018 (14)0.0512 (7)
O111.20524 (6)0.5743 (3)0.49788 (13)0.0385 (5)
O121.14910 (7)0.6434 (3)0.42198 (14)0.0434 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0303 (2)0.0316 (2)0.02300 (19)0.00024 (17)0.01277 (16)0.00072 (16)
Co20.0351 (2)0.0313 (2)0.0212 (2)0.00180 (17)0.01375 (18)0.00224 (16)
Co30.03313 (19)0.0381 (2)0.0418 (3)0.00110 (19)0.0225 (2)0.00081 (18)
C10.0349 (16)0.0375 (17)0.0241 (15)0.0046 (13)0.0130 (13)0.0011 (12)
C20.0373 (16)0.051 (2)0.0301 (16)0.0005 (14)0.0224 (14)0.0007 (14)
C30.0301 (15)0.049 (2)0.0348 (17)0.0035 (13)0.0156 (14)0.0018 (14)
C40.0302 (16)0.045 (2)0.0309 (18)0.0058 (13)0.0135 (14)0.0035 (13)
C50.0315 (15)0.0360 (17)0.0240 (15)0.0029 (13)0.0140 (13)0.0022 (13)
C60.0270 (14)0.0382 (17)0.0277 (16)0.0057 (13)0.0153 (13)0.0019 (13)
C70.0442 (18)0.0360 (18)0.0278 (16)0.0030 (14)0.0180 (15)0.0026 (13)
C80.0314 (16)0.064 (2)0.044 (2)0.0013 (15)0.0195 (16)0.0092 (17)
C90.0299 (15)0.0352 (16)0.0247 (15)0.0046 (13)0.0134 (13)0.0031 (13)
C100.0285 (14)0.0422 (18)0.0350 (17)0.0010 (13)0.0166 (14)0.0037 (13)
C110.0308 (14)0.0472 (18)0.0262 (15)0.0040 (13)0.0179 (13)0.0072 (13)
C120.0312 (14)0.0323 (15)0.0226 (15)0.0008 (12)0.0138 (13)0.0006 (11)
C130.0303 (15)0.0336 (16)0.0203 (14)0.0036 (12)0.0115 (12)0.0008 (11)
C140.0279 (14)0.0358 (16)0.0222 (14)0.0031 (13)0.0132 (12)0.0015 (12)
C150.0280 (15)0.0456 (18)0.0232 (15)0.0004 (12)0.0101 (13)0.0062 (12)
C160.0314 (15)0.052 (2)0.051 (2)0.0041 (14)0.0224 (16)0.0108 (16)
C170.0400 (17)0.0303 (16)0.0215 (15)0.0045 (13)0.0124 (13)0.0040 (11)
C180.0381 (17)0.0370 (16)0.0186 (15)0.0052 (14)0.0134 (13)0.0029 (13)
C190.096 (3)0.050 (2)0.0300 (19)0.007 (2)0.016 (2)0.0088 (16)
C200.098 (3)0.053 (2)0.0288 (19)0.010 (2)0.023 (2)0.0062 (16)
C210.060 (2)0.048 (2)0.039 (2)0.0117 (17)0.0187 (18)0.0094 (16)
C220.068 (3)0.044 (2)0.054 (2)0.0013 (18)0.031 (2)0.0015 (17)
C230.093 (3)0.064 (3)0.054 (3)0.008 (2)0.042 (3)0.012 (2)
C240.083 (3)0.070 (3)0.053 (3)0.013 (2)0.036 (2)0.006 (2)
C250.101 (6)0.072 (3)0.034 (2)0.037 (4)0.012 (3)0.010 (2)
C260.056 (2)0.081 (3)0.054 (2)0.026 (2)0.027 (2)0.029 (2)
C270.062 (2)0.043 (2)0.0372 (19)0.0018 (16)0.0137 (17)0.0066 (15)
C280.063 (3)0.090 (4)0.085 (4)0.011 (3)0.036 (3)0.039 (3)
C290.0394 (19)0.076 (3)0.083 (3)0.0050 (19)0.003 (2)0.010 (3)
C300.0425 (17)0.058 (2)0.0362 (19)0.0003 (15)0.0157 (16)0.0003 (15)
C310.066 (3)0.048 (2)0.050 (2)0.0044 (18)0.024 (2)0.0058 (17)
C320.063 (2)0.0434 (17)0.0320 (16)0.003 (2)0.0119 (15)0.0005 (18)
C330.0334 (16)0.0413 (19)0.055 (2)0.0097 (14)0.0242 (16)0.0046 (16)
C340.0332 (17)0.045 (2)0.048 (2)0.0034 (14)0.0192 (16)0.0005 (15)
C350.0402 (18)0.0295 (18)0.061 (2)0.0023 (14)0.0188 (18)0.0015 (16)
C360.044 (2)0.065 (3)0.076 (3)0.0137 (18)0.016 (2)0.020 (2)
C370.046 (2)0.096 (4)0.103 (4)0.019 (2)0.044 (3)0.019 (3)
C380.044 (2)0.075 (3)0.071 (3)0.0021 (19)0.032 (2)0.003 (2)
C390.0334 (17)0.070 (3)0.046 (2)0.0090 (17)0.0180 (16)0.0026 (18)
C400.062 (2)0.037 (2)0.053 (2)0.0155 (17)0.016 (2)0.0108 (16)
C410.0369 (17)0.046 (2)0.0390 (19)0.0025 (15)0.0187 (15)0.0085 (16)
C420.0419 (18)0.047 (2)0.044 (2)0.0026 (15)0.0124 (17)0.0144 (16)
C430.052 (2)0.037 (2)0.051 (2)0.0061 (16)0.0092 (19)0.0096 (17)
C440.055 (2)0.0317 (19)0.053 (2)0.0009 (15)0.0287 (18)0.0012 (15)
C450.063 (3)0.034 (2)0.073 (3)0.0094 (17)0.027 (2)0.0030 (18)
C460.057 (2)0.045 (2)0.075 (3)0.0027 (17)0.031 (2)0.0091 (19)
C470.056 (2)0.031 (2)0.075 (3)0.0022 (16)0.026 (2)0.0008 (18)
C480.040 (2)0.046 (2)0.076 (3)0.0025 (15)0.029 (2)0.0077 (19)
C490.0373 (19)0.065 (3)0.061 (3)0.0113 (18)0.0203 (19)0.015 (2)
C500.047 (3)0.138 (6)0.092 (4)0.005 (3)0.045 (3)0.003 (4)
C510.043 (2)0.166 (7)0.109 (5)0.016 (3)0.035 (3)0.011 (5)
C520.052 (2)0.087 (4)0.086 (4)0.014 (2)0.027 (3)0.005 (3)
C530.089 (3)0.036 (2)0.094 (4)0.017 (2)0.050 (3)0.014 (2)
C540.044 (2)0.097 (4)0.073 (3)0.023 (2)0.033 (2)0.015 (3)
C550.049 (2)0.0342 (19)0.064 (3)0.0012 (15)0.0265 (19)0.0047 (16)
C560.064 (3)0.039 (2)0.073 (3)0.0108 (18)0.033 (2)0.0069 (19)
C570.054 (2)0.048 (2)0.079 (3)0.0028 (18)0.035 (2)0.010 (2)
C580.0407 (19)0.055 (2)0.044 (2)0.0129 (17)0.0235 (17)0.0155 (17)
C590.053 (2)0.048 (2)0.058 (3)0.0123 (18)0.013 (2)0.0193 (19)
C600.051 (2)0.050 (2)0.045 (2)0.0028 (17)0.0120 (18)0.0127 (17)
N10.0402 (14)0.0478 (17)0.0408 (16)0.0028 (12)0.0045 (13)0.0083 (13)
N20.091 (3)0.065 (2)0.0373 (19)0.020 (2)0.0067 (19)0.0183 (16)
N30.0461 (15)0.0520 (18)0.0407 (17)0.0064 (13)0.0171 (14)0.0080 (13)
N40.0441 (16)0.0501 (18)0.0401 (17)0.0016 (12)0.0158 (14)0.0003 (12)
N50.0317 (13)0.0466 (17)0.0342 (15)0.0009 (12)0.0142 (12)0.0060 (12)
N60.0302 (14)0.0468 (17)0.0401 (16)0.0078 (12)0.0128 (13)0.0024 (12)
N70.0554 (17)0.0328 (16)0.0444 (17)0.0019 (13)0.0229 (15)0.0051 (13)
N80.0517 (18)0.0335 (15)0.0416 (18)0.0041 (12)0.0216 (15)0.0040 (12)
N90.0451 (15)0.0330 (14)0.0369 (16)0.0009 (13)0.0187 (14)0.0021 (11)
N100.062 (2)0.0278 (15)0.055 (2)0.0016 (13)0.0273 (17)0.0043 (13)
N110.0424 (17)0.062 (2)0.0483 (19)0.0107 (15)0.0187 (15)0.0077 (15)
N120.0387 (14)0.0424 (17)0.0362 (16)0.0041 (12)0.0156 (13)0.0074 (12)
O10.0578 (18)0.095 (2)0.0349 (15)0.0405 (17)0.0152 (13)0.0052 (15)
O20.0546 (14)0.0548 (15)0.0264 (12)0.0092 (12)0.0211 (11)0.0103 (11)
O30.0546 (16)0.076 (2)0.082 (2)0.0042 (13)0.0476 (17)0.0020 (15)
O40.0358 (13)0.0724 (19)0.0463 (16)0.0151 (13)0.0186 (12)0.0008 (13)
O50.0465 (14)0.0647 (17)0.0266 (13)0.0065 (12)0.0134 (12)0.0148 (11)
O60.0324 (11)0.0578 (16)0.0264 (11)0.0010 (10)0.0164 (10)0.0023 (10)
O70.0299 (12)0.0537 (16)0.0479 (16)0.0108 (11)0.0107 (12)0.0028 (12)
O80.0665 (17)0.084 (2)0.073 (2)0.0311 (15)0.0534 (17)0.0310 (16)
O90.0526 (13)0.0450 (14)0.0242 (11)0.0130 (10)0.0216 (10)0.0073 (9)
O100.0534 (16)0.0716 (19)0.0305 (13)0.0307 (14)0.0185 (12)0.0079 (13)
O110.0402 (12)0.0542 (16)0.0281 (12)0.0005 (11)0.0209 (10)0.0013 (10)
O120.0443 (14)0.0631 (18)0.0216 (12)0.0033 (11)0.0117 (11)0.0086 (11)
Geometric parameters (Å, º) top
Co1—O21.929 (2)C31—N31.380 (5)
Co1—O6i1.976 (2)C31—H310.9300
Co1—N52.007 (3)C32—N41.373 (4)
Co1—N92.012 (3)C32—H320.9300
Co2—O91.945 (2)C33—C381.381 (5)
Co2—O11ii1.975 (2)C33—C341.388 (5)
Co2—N12iii2.014 (3)C33—C391.501 (6)
Co2—N8iv2.019 (3)C34—C351.376 (5)
Co3—O41.968 (2)C34—H340.9300
Co3—O71.986 (2)C35—C361.408 (5)
Co3—N4v2.036 (3)C35—C401.497 (5)
Co3—N12.067 (3)C36—C371.372 (7)
C1—C21.393 (4)C36—H360.9300
C1—C61.399 (4)C37—C381.364 (7)
C1—C71.493 (5)C37—H370.9300
C2—C31.374 (5)C38—H380.9300
C2—H20.9300C39—N61.464 (4)
C3—C41.379 (5)C39—H39A0.9700
C3—C81.507 (4)C39—H39B0.9700
C4—C51.397 (5)C40—N71.476 (5)
C4—H40.9300C40—H40A0.9700
C5—C61.373 (5)C40—H40B0.9700
C5—C91.500 (4)C41—N61.325 (4)
C6—H60.9300C41—N51.325 (4)
C7—O11.227 (4)C41—H410.9300
C7—O21.281 (4)C42—C431.353 (5)
C8—O31.234 (5)C42—N51.353 (4)
C8—O41.290 (5)C42—H420.9300
C9—O51.218 (4)C43—N61.378 (5)
C9—O61.293 (4)C43—H430.9300
C10—C111.379 (5)C44—N81.319 (5)
C10—C151.391 (4)C44—N71.337 (5)
C10—C161.514 (4)C44—H440.9300
C11—C121.389 (4)C45—C461.348 (6)
C11—H110.9300C45—N71.363 (5)
C12—C131.383 (4)C45—H450.9300
C12—C171.507 (4)C46—N81.365 (5)
C13—C141.398 (4)C46—H460.9300
C13—H130.9300C47—C521.371 (6)
C14—C151.381 (4)C47—C481.381 (6)
C14—C181.508 (4)C47—C531.510 (6)
C15—H150.9300C48—C491.351 (6)
C16—O81.240 (4)C48—H480.9300
C16—O71.241 (4)C49—C501.399 (6)
C17—O101.222 (4)C49—C541.497 (7)
C17—O91.277 (4)C50—C511.370 (8)
C18—O121.242 (4)C50—H500.9300
C18—O111.268 (4)C51—C521.361 (8)
C19—C201.381 (6)C51—H510.9300
C19—C241.396 (6)C52—H520.9300
C19—C251.497 (7)C53—N101.494 (5)
C20—C211.363 (6)C53—H53A0.9700
C20—H200.9300C53—H53B0.9700
C21—C221.379 (5)C54—N111.471 (5)
C21—C261.514 (5)C54—H54A0.9700
C22—C231.374 (6)C54—H54B0.9700
C22—H220.9300C55—N91.306 (5)
C23—C241.384 (6)C55—N101.325 (5)
C23—H230.9300C55—H550.9300
C24—H240.9300C56—N101.337 (5)
C25—N21.465 (6)C56—C571.352 (6)
C25—H25A0.9700C56—H560.9300
C25—H25B0.9700C57—N91.375 (5)
C26—N31.448 (5)C57—H570.9300
C26—H26A0.9700C58—N121.299 (4)
C26—H26B0.9700C58—N111.344 (5)
C27—N11.316 (5)C58—H580.9300
C27—N21.336 (5)C59—C601.329 (5)
C27—H270.9300C59—N111.371 (5)
C28—C291.345 (8)C59—H590.9300
C28—N21.341 (7)C60—N121.395 (5)
C28—H280.9300C60—H600.9300
C29—N11.367 (5)N4—Co3vi2.036 (3)
C29—H290.9300N8—Co2vii2.019 (3)
C30—N41.301 (5)N12—Co2viii2.014 (3)
C30—N31.348 (5)O6—Co1ii1.976 (2)
C30—H300.9300O11—Co2i1.975 (2)
C31—C321.305 (5)
O2—Co1—O6i112.58 (10)C37—C36—C35119.9 (4)
O2—Co1—N5113.14 (12)C37—C36—H36120.1
O6i—Co1—N594.78 (10)C35—C36—H36120.1
O2—Co1—N9108.21 (12)C38—C37—C36121.3 (4)
O6i—Co1—N9112.98 (11)C38—C37—H37119.4
N5—Co1—N9114.82 (12)C36—C37—H37119.4
O9—Co2—O11ii110.32 (10)C37—C38—C33120.2 (4)
O9—Co2—N12iii112.67 (12)C37—C38—H38119.9
O11ii—Co2—N12iii95.68 (11)C33—C38—H38119.9
O9—Co2—N8iv112.65 (12)N6—C39—C33113.3 (3)
O11ii—Co2—N8iv109.52 (11)N6—C39—H39A108.9
N12iii—Co2—N8iv114.69 (12)C33—C39—H39A108.9
O4—Co3—O7136.24 (10)N6—C39—H39B108.9
O4—Co3—N4v105.85 (12)C33—C39—H39B108.9
O7—Co3—N4v107.86 (11)H39A—C39—H39B107.7
O4—Co3—N1107.75 (12)N7—C40—C35112.0 (3)
O7—Co3—N196.46 (11)N7—C40—H40A109.2
N4v—Co3—N194.74 (12)C35—C40—H40A109.2
C2—C1—C6118.6 (3)N7—C40—H40B109.2
C2—C1—C7120.4 (3)C35—C40—H40B109.2
C6—C1—C7121.0 (3)H40A—C40—H40B107.9
C3—C2—C1120.6 (3)N6—C41—N5110.5 (3)
C3—C2—H2119.7N6—C41—H41124.7
C1—C2—H2119.7N5—C41—H41124.7
C2—C3—C4120.4 (3)C43—C42—N5110.0 (3)
C2—C3—C8119.0 (3)C43—C42—H42125.0
C4—C3—C8120.6 (3)N5—C42—H42125.0
C3—C4—C5119.9 (3)C42—C43—N6105.2 (3)
C3—C4—H4120.0C42—C43—H43127.4
C5—C4—H4120.0N6—C43—H43127.4
C6—C5—C4119.6 (3)N8—C44—N7112.1 (3)
C6—C5—C9122.9 (3)N8—C44—H44123.9
C4—C5—C9117.5 (3)N7—C44—H44123.9
C5—C6—C1120.8 (3)C46—C45—N7106.8 (4)
C5—C6—H6119.6C46—C45—H45126.6
C1—C6—H6119.6N7—C45—H45126.6
O1—C7—O2123.0 (3)C45—C46—N8109.7 (4)
O1—C7—C1121.9 (3)C45—C46—H46125.1
O2—C7—C1115.2 (3)N8—C46—H46125.1
O3—C8—O4122.4 (3)C52—C47—C48119.6 (5)
O3—C8—C3120.1 (4)C52—C47—C53118.6 (5)
O4—C8—C3117.4 (3)C48—C47—C53121.8 (4)
O5—C9—O6122.8 (3)C49—C48—C47122.5 (4)
O5—C9—C5121.4 (3)C49—C48—H48118.8
O6—C9—C5115.8 (3)C47—C48—H48118.8
C11—C10—C15119.0 (3)C48—C49—C50117.3 (5)
C11—C10—C16120.7 (3)C48—C49—C54123.7 (4)
C15—C10—C16120.2 (3)C50—C49—C54119.0 (4)
C10—C11—C12121.0 (3)C51—C50—C49120.5 (5)
C10—C11—H11119.5C51—C50—H50119.8
C12—C11—H11119.5C49—C50—H50119.8
C13—C12—C11119.6 (3)C52—C51—C50121.1 (5)
C13—C12—C17120.6 (3)C52—C51—H51119.4
C11—C12—C17119.9 (3)C50—C51—H51119.4
C12—C13—C14120.0 (3)C51—C52—C47119.0 (5)
C12—C13—H13120.0C51—C52—H52120.5
C14—C13—H13120.0C47—C52—H52120.5
C15—C14—C13119.5 (3)N10—C53—C47111.7 (4)
C15—C14—C18119.3 (3)N10—C53—H53A109.3
C13—C14—C18121.2 (3)C47—C53—H53A109.3
C14—C15—C10120.8 (3)N10—C53—H53B109.3
C14—C15—H15119.6C47—C53—H53B109.3
C10—C15—H15119.6H53A—C53—H53B107.9
O8—C16—O7123.2 (3)N11—C54—C49114.0 (3)
O8—C16—C10120.1 (3)N11—C54—H54A108.8
O7—C16—C10116.8 (3)C49—C54—H54A108.8
O10—C17—O9123.6 (3)N11—C54—H54B108.8
O10—C17—C12121.7 (3)C49—C54—H54B108.8
O9—C17—C12114.7 (3)H54A—C54—H54B107.7
O12—C18—O11124.3 (3)N9—C55—N10112.6 (3)
O12—C18—C14119.1 (3)N9—C55—H55123.7
O11—C18—C14116.4 (3)N10—C55—H55123.7
C20—C19—C24118.0 (4)N10—C56—C57107.3 (3)
C20—C19—C25118.4 (4)N10—C56—H56126.4
C24—C19—C25123.6 (4)C57—C56—H56126.4
C21—C20—C19121.7 (4)C56—C57—N9108.7 (4)
C21—C20—H20119.2C56—C57—H57125.6
C19—C20—H20119.2N9—C57—H57125.6
C20—C21—C22120.4 (4)N12—C58—N11111.7 (3)
C20—C21—C26119.6 (4)N12—C58—H58124.2
C22—C21—C26120.0 (4)N11—C58—H58124.2
C23—C22—C21119.3 (4)C60—C59—N11106.9 (3)
C23—C22—H22120.4C60—C59—H59126.5
C21—C22—H22120.4N11—C59—H59126.5
C22—C23—C24120.6 (4)C59—C60—N12109.2 (3)
C22—C23—H23119.7C59—C60—H60125.4
C24—C23—H23119.7N12—C60—H60125.4
C23—C24—C19120.1 (4)C27—N1—C29105.9 (3)
C23—C24—H24119.9C27—N1—Co3121.0 (2)
C19—C24—H24119.9C29—N1—Co3131.7 (3)
N2—C25—C19112.7 (4)C27—N2—C28107.0 (4)
N2—C25—H25A109.0C27—N2—C25125.4 (5)
C19—C25—H25A109.0C28—N2—C25127.4 (5)
N2—C25—H25B109.0C30—N3—C31105.4 (3)
C19—C25—H25B109.0C30—N3—C26129.0 (4)
H25A—C25—H25B107.8C31—N3—C26125.2 (4)
N3—C26—C21111.1 (3)C30—N4—C32104.7 (3)
N3—C26—H26A109.4C30—N4—Co3vi127.6 (3)
C21—C26—H26A109.4C32—N4—Co3vi127.5 (3)
N3—C26—H26B109.4C41—N5—C42106.2 (3)
C21—C26—H26B109.4C41—N5—Co1128.5 (2)
H26A—C26—H26B108.0C42—N5—Co1124.5 (2)
N1—C27—N2111.0 (4)C41—N6—C43108.0 (3)
N1—C27—H27124.5C41—N6—C39125.2 (3)
N2—C27—H27124.5C43—N6—C39126.5 (3)
C29—C28—N2107.8 (4)C44—N7—C45106.3 (3)
C29—C28—H28126.1C44—N7—C40124.8 (3)
N2—C28—H28126.1C45—N7—C40128.5 (3)
C28—C29—N1108.4 (5)C44—N8—C46105.0 (3)
C28—C29—H29125.8C44—N8—Co2vii122.5 (2)
N1—C29—H29125.8C46—N8—Co2vii132.2 (3)
N4—C30—N3112.0 (3)C55—N9—C57104.6 (3)
N4—C30—H30124.0C55—N9—Co1120.2 (2)
N3—C30—H30124.0C57—N9—Co1135.2 (3)
C32—C31—N3106.8 (4)C55—N10—C56106.8 (3)
C32—C31—H31126.6C55—N10—C53124.1 (3)
N3—C31—H31126.6C56—N10—C53129.0 (3)
C31—C32—N4111.0 (4)C58—N11—C59106.7 (3)
C31—C32—H32124.5C58—N11—C54126.3 (4)
N4—C32—H32124.5C59—N11—C54126.5 (4)
C38—C33—C34118.6 (4)C58—N12—C60105.5 (3)
C38—C33—C39118.3 (4)C58—N12—Co2viii131.2 (2)
C34—C33—C39123.1 (3)C60—N12—Co2viii122.7 (2)
C35—C34—C33122.1 (3)C7—O2—Co1118.4 (2)
C35—C34—H34118.9C8—O4—Co3103.5 (2)
C33—C34—H34118.9C9—O6—Co1ii114.3 (2)
C34—C35—C36117.7 (4)C16—O7—Co3104.4 (2)
C34—C35—C40122.9 (3)C17—O9—Co2114.0 (2)
C36—C35—C40119.3 (4)C18—O11—Co2i113.1 (2)
C6—C1—C2—C33.2 (5)C28—C29—N1—Co3166.0 (4)
C7—C1—C2—C3177.0 (3)O4—Co3—N1—C27167.6 (3)
C1—C2—C3—C41.7 (5)O7—Co3—N1—C2724.5 (3)
C1—C2—C3—C8175.6 (3)N4v—Co3—N1—C2784.1 (3)
C2—C3—C4—C51.6 (5)O4—Co3—N1—C2928.1 (4)
C8—C3—C4—C5178.9 (3)O7—Co3—N1—C29171.1 (4)
C3—C4—C5—C63.4 (5)N4v—Co3—N1—C2980.3 (4)
C3—C4—C5—C9179.8 (3)N1—C27—N2—C280.4 (5)
C4—C5—C6—C11.9 (5)N1—C27—N2—C25174.4 (4)
C9—C5—C6—C1178.1 (3)C29—C28—N2—C270.5 (6)
C2—C1—C6—C51.4 (5)C29—C28—N2—C25174.3 (5)
C7—C1—C6—C5178.8 (3)C19—C25—N2—C2785.7 (7)
C2—C1—C7—O1174.9 (4)C19—C25—N2—C2887.1 (7)
C6—C1—C7—O15.0 (5)N4—C30—N3—C310.2 (4)
C2—C1—C7—O24.1 (5)N4—C30—N3—C26173.9 (3)
C6—C1—C7—O2176.0 (3)C32—C31—N3—C300.9 (4)
C2—C3—C8—O322.2 (5)C32—C31—N3—C26174.9 (3)
C4—C3—C8—O3160.4 (4)C21—C26—N3—C30102.9 (5)
C2—C3—C8—O4155.5 (3)C21—C26—N3—C3169.7 (5)
C4—C3—C8—O421.8 (5)N3—C30—N4—C320.5 (4)
C6—C5—C9—O5178.0 (3)N3—C30—N4—Co3vi176.1 (2)
C4—C5—C9—O55.7 (5)C31—C32—N4—C301.1 (5)
C6—C5—C9—O64.0 (5)C31—C32—N4—Co3vi176.7 (3)
C4—C5—C9—O6172.3 (3)N6—C41—N5—C420.4 (4)
C15—C10—C11—C121.6 (5)N6—C41—N5—Co1170.1 (2)
C16—C10—C11—C12178.5 (3)C43—C42—N5—C410.6 (5)
C10—C11—C12—C133.4 (5)C43—C42—N5—Co1170.4 (3)
C10—C11—C12—C17177.0 (3)O2—Co1—N5—C4184.7 (3)
C11—C12—C13—C142.0 (5)O6i—Co1—N5—C41158.3 (3)
C17—C12—C13—C14178.5 (3)N9—Co1—N5—C4140.2 (4)
C12—C13—C14—C151.2 (5)O2—Co1—N5—C4284.2 (3)
C12—C13—C14—C18177.3 (3)O6i—Co1—N5—C4232.8 (3)
C13—C14—C15—C103.0 (5)N9—Co1—N5—C42150.9 (3)
C18—C14—C15—C10175.6 (3)N5—C41—N6—C430.1 (4)
C11—C10—C15—C141.6 (5)N5—C41—N6—C39174.2 (3)
C16—C10—C15—C14178.3 (3)C42—C43—N6—C410.3 (4)
C11—C10—C16—O83.8 (5)C42—C43—N6—C39173.7 (4)
C15—C10—C16—O8176.1 (3)C33—C39—N6—C4194.9 (5)
C11—C10—C16—O7175.7 (3)C33—C39—N6—C4378.1 (5)
C15—C10—C16—O74.5 (5)N8—C44—N7—C450.3 (5)
C13—C12—C17—O104.8 (5)N8—C44—N7—C40173.2 (3)
C11—C12—C17—O10175.6 (3)C46—C45—N7—C441.1 (5)
C13—C12—C17—O9176.3 (3)C46—C45—N7—C40174.2 (4)
C11—C12—C17—O93.2 (4)C35—C40—N7—C4454.8 (5)
C15—C14—C18—O1212.2 (5)C35—C40—N7—C45117.2 (5)
C13—C14—C18—O12169.3 (3)N7—C44—N8—C461.5 (4)
C15—C14—C18—O11164.9 (3)N7—C44—N8—Co2vii172.7 (2)
C13—C14—C18—O1113.6 (5)C45—C46—N8—C442.1 (5)
C24—C19—C20—C210.1 (7)C45—C46—N8—Co2vii171.2 (3)
C25—C19—C20—C21177.8 (5)N10—C55—N9—C570.2 (5)
C19—C20—C21—C220.4 (7)N10—C55—N9—Co1178.8 (3)
C19—C20—C21—C26179.1 (4)C56—C57—N9—C550.3 (5)
C20—C21—C22—C231.1 (7)C56—C57—N9—Co1178.6 (3)
C26—C21—C22—C23179.9 (4)O2—Co1—N9—C5581.4 (3)
C21—C22—C23—C241.4 (7)O6i—Co1—N9—C5543.9 (3)
C22—C23—C24—C190.9 (8)N5—Co1—N9—C55151.1 (3)
C20—C19—C24—C230.1 (7)O2—Co1—N9—C5799.8 (4)
C25—C19—C24—C23177.4 (5)O6i—Co1—N9—C57134.8 (4)
C20—C19—C25—N2158.1 (5)N5—Co1—N9—C5727.6 (4)
C24—C19—C25—N219.3 (8)N9—C55—N10—C560.1 (5)
C20—C21—C26—N389.1 (5)N9—C55—N10—C53176.1 (4)
C22—C21—C26—N389.6 (5)C57—C56—N10—C550.0 (5)
N2—C28—C29—N10.4 (7)C57—C56—N10—C53176.1 (5)
N3—C31—C32—N41.2 (5)C47—C53—N10—C5540.9 (6)
C38—C33—C34—C354.2 (6)C47—C53—N10—C56134.5 (5)
C39—C33—C34—C35175.2 (4)N12—C58—N11—C590.6 (5)
C33—C34—C35—C364.9 (6)N12—C58—N11—C54173.5 (4)
C33—C34—C35—C40177.9 (4)C60—C59—N11—C580.3 (5)
C34—C35—C36—C373.2 (7)C60—C59—N11—C54173.3 (4)
C40—C35—C36—C37179.5 (4)C49—C54—N11—C58101.6 (5)
C35—C36—C37—C380.9 (8)C49—C54—N11—C5970.0 (6)
C36—C37—C38—C330.1 (8)N11—C58—N12—C600.5 (5)
C34—C33—C38—C371.7 (7)N11—C58—N12—Co2viii170.2 (3)
C39—C33—C38—C37177.8 (4)C59—C60—N12—C580.3 (5)
C38—C33—C39—N6166.8 (4)C59—C60—N12—Co2viii171.4 (3)
C34—C33—C39—N613.8 (5)O1—C7—O2—Co16.8 (5)
C34—C35—C40—N726.0 (5)C1—C7—O2—Co1172.2 (2)
C36—C35—C40—N7156.9 (4)O6i—Co1—O2—C7163.6 (2)
N5—C42—C43—N60.6 (5)N5—Co1—O2—C757.5 (3)
N7—C45—C46—N82.0 (5)N9—Co1—O2—C770.9 (3)
C52—C47—C48—C492.2 (7)O3—C8—O4—Co315.5 (4)
C53—C47—C48—C49175.4 (4)C3—C8—O4—Co3162.2 (3)
C47—C48—C49—C501.8 (7)O7—Co3—O4—C861.2 (3)
C47—C48—C49—C54175.4 (4)N4v—Co3—O4—C8159.6 (2)
C48—C49—C50—C511.3 (8)N1—Co3—O4—C859.1 (3)
C54—C49—C50—C51178.6 (6)O5—C9—O6—Co1ii6.6 (4)
C49—C50—C51—C524.0 (11)C5—C9—O6—Co1ii171.3 (2)
C50—C51—C52—C473.5 (10)O8—C16—O7—Co33.3 (4)
C48—C47—C52—C510.5 (8)C10—C16—O7—Co3176.2 (2)
C53—C47—C52—C51178.2 (5)O4—Co3—O7—C1661.5 (3)
C52—C47—C53—N10139.9 (5)N4v—Co3—O7—C1677.2 (3)
C48—C47—C53—N1037.7 (6)N1—Co3—O7—C16174.3 (2)
C48—C49—C54—N111.4 (7)O10—C17—O9—Co28.9 (4)
C50—C49—C54—N11175.7 (5)C12—C17—O9—Co2169.9 (2)
N10—C56—C57—N90.2 (6)O11ii—Co2—O9—C17172.5 (2)
N11—C59—C60—N120.0 (5)N12iii—Co2—O9—C1766.9 (3)
N2—C27—N1—C290.2 (5)N8iv—Co2—O9—C1764.8 (3)
N2—C27—N1—Co3168.1 (3)O12—C18—O11—Co2i13.0 (4)
C28—C29—N1—C270.2 (6)C14—C18—O11—Co2i163.9 (2)
Symmetry codes: (i) x, y+1, z1/2; (ii) x, y+1, z+1/2; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y1/2, z+1; (v) x, y+3, z+1/2; (vi) x, y+3, z1/2; (vii) x1/2, y+1/2, z1; (viii) x1/2, y1/2, z1.
(II) poly[diaquabis[µ3-benzene-1,3,5-tricarboxylato- κ3O1:O3:O5]tris[µ2-1,4-bis(imidazol-1- ylmethyl)benzene-κ2N:N']tricobalt(II)] monohydrate] top
Crystal data top
[Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2OF(000) = 1398
Mr = 1359.94Dx = 1.530 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 6672 reflections
a = 14.160 (4) Åθ = 3.0–27.5°
b = 10.105 (3) ŵ = 0.91 mm1
c = 20.927 (4) ÅT = 293 K
β = 99.730 (6)°Block, violet
V = 2951.3 (14) Å30.31 × 0.28 × 0.21 mm
Z = 2
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6651 independent reflections
Radiation source: fine-focus sealed tube3309 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.114
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1818
Tmin = 0.77, Tmax = 0.83k = 1213
24924 measured reflectionsl = 2427
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.074H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.165 w = 1/[σ2(Fo2) + (0.0501P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max < 0.001
6651 reflectionsΔρmax = 0.71 e Å3
413 parametersΔρmin = 0.69 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0016 (4)
Crystal data top
[Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2OV = 2951.3 (14) Å3
Mr = 1359.94Z = 2
Monoclinic, P21/cMo Kα radiation
a = 14.160 (4) ŵ = 0.91 mm1
b = 10.105 (3) ÅT = 293 K
c = 20.927 (4) Å0.31 × 0.28 × 0.21 mm
β = 99.730 (6)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6651 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3309 reflections with I > 2σ(I)
Tmin = 0.77, Tmax = 0.83Rint = 0.114
24924 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0740 restraints
wR(F2) = 0.165H atoms treated by a mixture of independent and constrained refinement
S = 1.13Δρmax = 0.71 e Å3
6651 reflectionsΔρmin = 0.69 e Å3
413 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)
Co10.00000.00000.00000.0452 (3)
Co20.39399 (5)0.31962 (6)0.18718 (3)0.0407 (2)
C10.2211 (4)0.1803 (5)0.0839 (2)0.0376 (11)
C20.2593 (4)0.0615 (4)0.1011 (2)0.0358 (11)
H20.23570.01750.08730.043*
C30.3315 (4)0.0576 (4)0.1382 (2)0.0345 (11)
C40.3659 (4)0.1764 (4)0.1587 (2)0.0360 (11)
H40.41550.17560.18270.043*
C50.3271 (4)0.2959 (4)0.1437 (2)0.0379 (11)
C60.2560 (4)0.2975 (4)0.1055 (2)0.0395 (12)
H60.23140.37790.09430.047*
C70.1441 (4)0.1804 (5)0.0434 (2)0.0429 (12)
C80.3682 (4)0.0701 (4)0.1591 (2)0.0380 (11)
C90.3577 (4)0.4225 (5)0.1720 (2)0.0435 (13)
C100.0442 (4)0.0452 (5)0.2916 (2)0.0490 (13)
C110.0323 (5)0.0285 (6)0.3577 (3)0.0666 (18)
H110.01450.07670.38450.080*
C120.0893 (5)0.0590 (6)0.3848 (3)0.0678 (18)
H120.08010.06900.42960.081*
C130.1586 (4)0.1309 (6)0.3469 (3)0.0512 (14)
C140.1706 (5)0.1139 (7)0.2816 (3)0.0696 (18)
H140.21790.16170.25510.083*
C150.1148 (5)0.0284 (7)0.2542 (3)0.0715 (19)
H150.12450.01950.20930.086*
C160.0190 (5)0.1358 (6)0.2614 (3)0.0630 (16)
H16A0.01520.21740.24870.076*
H16B0.07510.15750.29300.076*
C170.2173 (4)0.2320 (6)0.3756 (3)0.0592 (15)
H17A0.22160.31170.34940.071*
H17B0.18460.25470.41880.071*
C180.0096 (4)0.0952 (6)0.1425 (2)0.0528 (14)
H180.03720.15840.12880.063*
C190.1122 (5)0.0232 (6)0.2051 (3)0.0639 (16)
H190.15040.05940.24140.077*
C200.1101 (5)0.0610 (6)0.1432 (3)0.0619 (16)
H200.14720.12800.12970.074*
C210.3935 (4)0.2166 (5)0.3394 (2)0.0477 (13)
H210.39650.27330.30410.057*
C220.4318 (5)0.0816 (5)0.4097 (2)0.0509 (14)
H220.46730.02640.43210.061*
C230.3378 (5)0.1013 (5)0.4249 (3)0.0544 (15)
H230.29680.06400.45960.065*
C240.3740 (4)0.3976 (5)0.3275 (2)0.0484 (13)
H240.39690.48250.31710.058*
C250.3162 (6)0.2291 (7)0.3834 (3)0.089 (3)
H250.29050.17430.41770.107*
C260.3333 (6)0.1962 (6)0.3212 (3)0.087 (3)
H260.32300.11290.30480.104*
C270.3303 (5)0.4358 (6)0.4472 (3)0.0639 (17)
H27A0.28700.38970.48070.077*
H27B0.29960.51810.43850.077*
C280.4199 (4)0.4682 (5)0.4731 (2)0.0453 (13)
C290.4733 (4)0.3691 (6)0.4957 (2)0.0548 (15)
H290.45580.28080.49280.066*
C300.4476 (4)0.5977 (5)0.4776 (2)0.0523 (14)
H300.41220.66430.46210.063*
N10.0443 (3)0.0148 (4)0.10300 (19)0.0497 (11)
N20.0492 (4)0.0764 (5)0.2048 (2)0.0533 (12)
N30.3129 (3)0.1871 (4)0.37973 (19)0.0469 (11)
N40.4691 (3)0.1553 (4)0.35562 (18)0.0458 (11)
N50.3682 (3)0.3033 (4)0.28452 (19)0.0448 (10)
N60.3426 (3)0.3549 (4)0.38804 (19)0.0496 (11)
O10.1030 (3)0.2874 (4)0.03588 (16)0.0562 (10)
O20.1265 (3)0.0715 (3)0.01901 (16)0.0506 (9)
O30.3241 (3)0.1767 (3)0.14743 (15)0.0444 (8)
O40.4372 (3)0.0735 (3)0.18735 (16)0.0511 (9)
O50.4086 (3)0.4172 (3)0.21359 (18)0.0618 (11)
O60.3272 (3)0.5302 (3)0.15094 (16)0.0534 (10)
O1WA0.1962 (5)0.2943 (6)0.0782 (4)0.057 (2)0.50
O2W0.0631 (3)0.1971 (4)0.00627 (17)0.0593 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0479 (7)0.0392 (6)0.0539 (6)0.0025 (5)0.0246 (4)0.0045 (4)
Co20.0490 (5)0.0264 (4)0.0501 (4)0.0002 (3)0.0179 (3)0.0018 (3)
C10.039 (3)0.031 (3)0.044 (3)0.002 (2)0.011 (2)0.000 (2)
C20.043 (3)0.022 (2)0.042 (3)0.005 (2)0.006 (2)0.0038 (18)
C30.042 (3)0.025 (2)0.036 (2)0.000 (2)0.007 (2)0.0015 (18)
C40.044 (3)0.025 (2)0.040 (2)0.002 (2)0.011 (2)0.0034 (18)
C50.044 (3)0.024 (3)0.047 (3)0.004 (2)0.011 (2)0.0017 (18)
C60.049 (3)0.024 (3)0.047 (3)0.000 (2)0.014 (2)0.0024 (19)
C70.046 (3)0.038 (3)0.047 (3)0.003 (3)0.014 (2)0.009 (2)
C80.046 (3)0.026 (3)0.044 (3)0.004 (2)0.013 (2)0.0006 (19)
C90.050 (4)0.025 (3)0.058 (3)0.009 (2)0.014 (3)0.001 (2)
C100.046 (4)0.053 (3)0.049 (3)0.004 (3)0.011 (2)0.006 (2)
C110.066 (5)0.078 (5)0.052 (4)0.032 (4)0.001 (3)0.014 (3)
C120.078 (5)0.078 (5)0.047 (3)0.016 (4)0.009 (3)0.002 (3)
C130.044 (4)0.052 (3)0.059 (3)0.005 (3)0.011 (3)0.007 (3)
C140.062 (5)0.085 (5)0.057 (4)0.024 (4)0.003 (3)0.002 (3)
C150.077 (5)0.088 (5)0.047 (3)0.025 (4)0.003 (3)0.000 (3)
C160.075 (5)0.057 (4)0.063 (4)0.008 (3)0.030 (3)0.011 (3)
C170.046 (4)0.061 (4)0.072 (4)0.001 (3)0.012 (3)0.009 (3)
C180.050 (4)0.057 (4)0.053 (3)0.001 (3)0.014 (3)0.007 (3)
C190.060 (4)0.069 (4)0.064 (4)0.003 (3)0.012 (3)0.012 (3)
C200.062 (5)0.055 (4)0.072 (4)0.007 (3)0.021 (3)0.006 (3)
C210.058 (4)0.034 (3)0.055 (3)0.002 (3)0.018 (3)0.003 (2)
C220.060 (4)0.037 (3)0.061 (3)0.003 (3)0.022 (3)0.012 (2)
C230.059 (4)0.043 (3)0.062 (3)0.008 (3)0.012 (3)0.004 (3)
C240.054 (4)0.038 (3)0.054 (3)0.006 (3)0.013 (2)0.004 (2)
C250.162 (8)0.044 (4)0.059 (4)0.002 (4)0.009 (4)0.005 (3)
C260.163 (8)0.033 (3)0.058 (4)0.018 (4)0.002 (4)0.005 (3)
C270.064 (5)0.073 (4)0.058 (3)0.018 (3)0.018 (3)0.027 (3)
C280.047 (4)0.052 (3)0.038 (3)0.009 (3)0.014 (2)0.005 (2)
C290.069 (4)0.039 (3)0.059 (3)0.002 (3)0.018 (3)0.004 (2)
C300.066 (4)0.042 (3)0.050 (3)0.012 (3)0.015 (3)0.002 (2)
N10.052 (3)0.049 (3)0.055 (3)0.003 (2)0.031 (2)0.003 (2)
N20.058 (3)0.048 (3)0.057 (3)0.004 (2)0.018 (2)0.002 (2)
N30.046 (3)0.040 (3)0.056 (3)0.000 (2)0.011 (2)0.0018 (19)
N40.054 (3)0.030 (2)0.056 (3)0.004 (2)0.016 (2)0.0033 (18)
N50.049 (3)0.029 (2)0.059 (3)0.002 (2)0.016 (2)0.0037 (18)
N60.054 (3)0.052 (3)0.045 (2)0.011 (2)0.014 (2)0.008 (2)
O10.067 (3)0.044 (2)0.065 (2)0.018 (2)0.0334 (19)0.0042 (16)
O20.046 (2)0.048 (2)0.062 (2)0.0053 (18)0.0235 (17)0.0117 (17)
O30.053 (2)0.0233 (17)0.059 (2)0.0032 (17)0.0179 (16)0.0007 (14)
O40.060 (3)0.035 (2)0.064 (2)0.0027 (18)0.0282 (19)0.0036 (15)
O50.083 (3)0.036 (2)0.078 (3)0.003 (2)0.045 (2)0.0057 (17)
O60.066 (3)0.0262 (19)0.073 (2)0.0035 (18)0.0261 (19)0.0013 (16)
O1WA0.060 (5)0.028 (4)0.102 (5)0.010 (3)0.070 (4)0.013 (3)
O2W0.065 (3)0.046 (2)0.070 (2)0.012 (2)0.0209 (19)0.0078 (17)
Geometric parameters (Å, º) top
Co1—O2i2.033 (4)C16—H16A0.9700
Co1—O22.033 (4)C16—H16B0.9700
Co1—N12.146 (4)C17—N31.443 (7)
Co1—N1i2.146 (4)C17—H17A0.9700
Co1—O2W2.178 (4)C17—H17B0.9700
Co1—O2Wi2.178 (4)C18—N11.312 (6)
Co2—O6ii2.003 (3)C18—N21.344 (6)
Co2—O32.008 (3)C18—H180.9300
Co2—N4iii2.010 (4)C19—N21.345 (7)
Co2—N52.015 (4)C19—C201.345 (8)
C1—C21.388 (6)C19—H190.9300
C1—C61.389 (6)C20—N11.378 (7)
C1—C71.488 (7)C20—H200.9300
C2—C31.386 (7)C21—N41.328 (7)
C2—H20.9300C21—N31.334 (6)
C3—C41.390 (6)C21—H210.9300
C3—C81.484 (6)C22—C231.329 (8)
C4—C51.384 (6)C22—N41.382 (6)
C4—H40.9300C22—H220.9300
C5—C61.387 (7)C23—N31.373 (7)
C5—C91.504 (6)C23—H230.9300
C6—H60.9300C24—N51.323 (6)
C7—O11.251 (6)C24—N61.341 (6)
C7—O21.256 (6)C24—H240.9300
C8—O41.225 (6)C25—N61.333 (8)
C8—O31.288 (5)C25—C261.327 (8)
C9—O51.222 (6)C25—H250.9300
C9—O61.276 (6)C26—N51.369 (6)
C10—C111.376 (7)C26—H260.9300
C10—C151.378 (7)C27—N61.468 (6)
C10—C161.493 (8)C27—C281.498 (8)
C11—C121.381 (8)C27—H27A0.9700
C11—H110.9300C27—H27B0.9700
C12—C131.363 (8)C28—C301.373 (7)
C12—H120.9300C28—C291.385 (7)
C13—C141.358 (7)C29—C30iv1.376 (8)
C13—C171.506 (7)C29—H290.9300
C14—C151.361 (8)C30—C29iv1.376 (8)
C14—H140.9300C30—H300.9300
C15—H150.9300N4—Co2v2.010 (4)
C16—N21.454 (7)O6—Co2vi2.003 (3)
O2i—Co1—O2180.0 (2)H16A—C16—H16B107.9
O2i—Co1—N186.91 (15)N3—C17—C13113.4 (5)
O2—Co1—N193.09 (15)N3—C17—H17A108.9
O2i—Co1—N1i93.09 (15)C13—C17—H17A108.9
O2—Co1—N1i86.91 (15)N3—C17—H17B108.9
N1—Co1—N1i180.0 (2)C13—C17—H17B108.9
O2i—Co1—O2W88.31 (15)H17A—C17—H17B107.7
O2—Co1—O2W91.69 (15)N1—C18—N2112.6 (5)
N1—Co1—O2W92.53 (15)N1—C18—H18123.7
N1i—Co1—O2W87.47 (15)N2—C18—H18123.7
O2i—Co1—O2Wi91.69 (15)N2—C19—C20107.6 (5)
O2—Co1—O2Wi88.31 (15)N2—C19—H19126.2
N1—Co1—O2Wi87.47 (15)C20—C19—H19126.2
N1i—Co1—O2Wi92.53 (15)C19—C20—N1109.4 (5)
O2W—Co1—O2Wi180.00 (8)C19—C20—H20125.3
O6ii—Co2—O395.21 (14)N1—C20—H20125.3
O6ii—Co2—N4iii102.55 (17)N4—C21—N3112.0 (5)
O3—Co2—N4iii114.31 (15)N4—C21—H21124.0
O6ii—Co2—N5115.36 (16)N3—C21—H21124.0
O3—Co2—N5110.01 (15)C23—C22—N4110.1 (5)
N4iii—Co2—N5117.21 (17)C23—C22—H22124.9
C2—C1—C6118.5 (4)N4—C22—H22124.9
C2—C1—C7120.2 (4)C22—C23—N3107.0 (5)
C6—C1—C7121.3 (4)C22—C23—H23126.5
C3—C2—C1121.8 (4)N3—C23—H23126.5
C3—C2—H2119.1N5—C24—N6111.3 (5)
C1—C2—H2119.1N5—C24—H24124.4
C2—C3—C4118.6 (4)N6—C24—H24124.4
C2—C3—C8121.2 (4)N6—C25—C26107.6 (5)
C4—C3—C8120.2 (4)N6—C25—H25126.2
C5—C4—C3120.6 (4)C26—C25—H25126.2
C5—C4—H4119.7C25—C26—N5109.9 (5)
C3—C4—H4119.7C25—C26—H26125.0
C6—C5—C4119.7 (4)N5—C26—H26125.0
C6—C5—C9120.1 (4)N6—C27—C28116.1 (5)
C4—C5—C9120.0 (4)N6—C27—H27A108.3
C5—C6—C1120.7 (4)C28—C27—H27A108.3
C5—C6—H6119.6N6—C27—H27B108.3
C1—C6—H6119.6C28—C27—H27B108.3
O1—C7—O2125.3 (5)H27A—C27—H27B107.4
O1—C7—C1118.3 (4)C30—C28—C29119.1 (5)
O2—C7—C1116.5 (5)C30—C28—C27120.2 (5)
O4—C8—O3121.3 (4)C29—C28—C27120.6 (5)
O4—C8—C3120.9 (4)C30iv—C29—C28119.4 (5)
O3—C8—C3117.9 (4)C30iv—C29—H29120.3
O5—C9—O6123.9 (5)C28—C29—H29120.3
O5—C9—C5119.1 (4)C28—C30—C29iv121.5 (5)
O6—C9—C5117.0 (5)C28—C30—H30119.3
C11—C10—C15117.3 (5)C29iv—C30—H30119.3
C11—C10—C16121.4 (5)C18—N1—C20104.3 (5)
C15—C10—C16121.3 (5)C18—N1—Co1126.8 (4)
C10—C11—C12120.7 (5)C20—N1—Co1128.9 (4)
C10—C11—H11119.7C19—N2—C18106.1 (5)
C12—C11—H11119.7C19—N2—C16126.3 (5)
C13—C12—C11121.0 (5)C18—N2—C16126.9 (5)
C13—C12—H12119.5C21—N3—C23106.5 (5)
C11—C12—H12119.5C21—N3—C17127.1 (5)
C14—C13—C12118.2 (5)C23—N3—C17126.3 (5)
C14—C13—C17120.3 (5)C21—N4—C22104.3 (5)
C12—C13—C17121.4 (5)C21—N4—Co2v125.8 (4)
C13—C14—C15121.4 (6)C22—N4—Co2v129.7 (4)
C13—C14—H14119.3C24—N5—C26104.2 (4)
C15—C14—H14119.3C24—N5—Co2127.4 (4)
C14—C15—C10121.3 (5)C26—N5—Co2128.1 (3)
C14—C15—H15119.3C25—N6—C24106.9 (4)
C10—C15—H15119.3C25—N6—C27126.6 (5)
N2—C16—C10111.8 (5)C24—N6—C27126.2 (5)
N2—C16—H16A109.3C7—O2—Co1129.3 (3)
C10—C16—H16A109.3C8—O3—Co2103.6 (3)
N2—C16—H16B109.3C9—O6—Co2vi107.9 (3)
C10—C16—H16B109.3
C6—C1—C2—C30.9 (7)O2W—Co1—N1—C1820.7 (5)
C7—C1—C2—C3179.5 (4)O2Wi—Co1—N1—C18159.3 (5)
C1—C2—C3—C40.2 (7)O2i—Co1—N1—C20108.3 (5)
C1—C2—C3—C8176.9 (4)O2—Co1—N1—C2071.7 (5)
C2—C3—C4—C51.7 (7)N1i—Co1—N1—C20110 (31)
C8—C3—C4—C5175.0 (4)O2W—Co1—N1—C20163.6 (5)
C3—C4—C5—C62.8 (7)O2Wi—Co1—N1—C2016.4 (5)
C3—C4—C5—C9173.5 (4)C20—C19—N2—C180.7 (7)
C4—C5—C6—C12.0 (7)C20—C19—N2—C16171.4 (5)
C9—C5—C6—C1174.2 (4)N1—C18—N2—C190.7 (7)
C2—C1—C6—C50.2 (7)N1—C18—N2—C16171.4 (5)
C7—C1—C6—C5179.4 (4)C10—C16—N2—C1971.6 (8)
C2—C1—C7—O1171.0 (4)C10—C16—N2—C1897.3 (6)
C6—C1—C7—O18.7 (7)N4—C21—N3—C230.0 (6)
C2—C1—C7—O29.7 (7)N4—C21—N3—C17177.8 (5)
C6—C1—C7—O2170.7 (4)C22—C23—N3—C210.6 (6)
C2—C3—C8—O4174.0 (5)C22—C23—N3—C17177.2 (5)
C4—C3—C8—O49.4 (7)C13—C17—N3—C21100.3 (6)
C2—C3—C8—O37.2 (7)C13—C17—N3—C2377.1 (6)
C4—C3—C8—O3169.5 (4)N3—C21—N4—C220.6 (5)
C6—C5—C9—O5168.3 (5)N3—C21—N4—Co2v175.2 (3)
C4—C5—C9—O58.0 (7)C23—C22—N4—C211.0 (6)
C6—C5—C9—O611.1 (7)C23—C22—N4—Co2v174.6 (3)
C4—C5—C9—O6172.7 (4)N6—C24—N5—C261.4 (7)
C15—C10—C11—C120.1 (10)N6—C24—N5—Co2173.8 (3)
C16—C10—C11—C12177.8 (6)C25—C26—N5—C242.1 (8)
C10—C11—C12—C130.1 (11)C25—C26—N5—Co2173.0 (5)
C11—C12—C13—C140.2 (10)O6ii—Co2—N5—C2450.1 (5)
C11—C12—C13—C17176.6 (6)O3—Co2—N5—C24156.3 (4)
C12—C13—C14—C150.5 (10)N4iii—Co2—N5—C2470.9 (5)
C17—C13—C14—C15176.3 (6)O6ii—Co2—N5—C26124.0 (6)
C13—C14—C15—C100.5 (11)O3—Co2—N5—C2617.7 (6)
C11—C10—C15—C140.1 (10)N4iii—Co2—N5—C26115.1 (6)
C16—C10—C15—C14178.1 (6)C26—C25—N6—C241.1 (8)
C11—C10—C16—N2136.2 (6)C26—C25—N6—C27175.2 (6)
C15—C10—C16—N241.7 (8)N5—C24—N6—C250.2 (7)
C14—C13—C17—N379.9 (7)N5—C24—N6—C27173.9 (5)
C12—C13—C17—N3103.4 (6)C28—C27—N6—C25109.2 (7)
N2—C19—C20—N10.4 (7)C28—C27—N6—C2477.8 (7)
N4—C22—C23—N31.0 (6)O1—C7—O2—Co133.4 (7)
N6—C25—C26—N52.0 (9)C1—C7—O2—Co1147.3 (3)
N6—C27—C28—C30118.6 (6)O2i—Co1—O2—C7117 (37)
N6—C27—C28—C2964.5 (7)N1—Co1—O2—C7110.4 (4)
C30—C28—C29—C30iv0.5 (9)N1i—Co1—O2—C769.6 (4)
C27—C28—C29—C30iv176.5 (5)O2W—Co1—O2—C717.8 (4)
C29—C28—C30—C29iv0.5 (9)O2Wi—Co1—O2—C7162.2 (4)
C27—C28—C30—C29iv176.5 (5)O4—C8—O3—Co21.4 (6)
N2—C18—N1—C200.4 (6)C3—C8—O3—Co2177.4 (3)
N2—C18—N1—Co1177.0 (3)O6ii—Co2—O3—C8171.7 (3)
C19—C20—N1—C180.0 (6)N4iii—Co2—O3—C865.4 (3)
C19—C20—N1—Co1176.4 (4)N5—Co2—O3—C868.9 (3)
O2i—Co1—N1—C1867.5 (5)O5—C9—O6—Co2vi8.8 (7)
O2—Co1—N1—C18112.5 (5)C5—C9—O6—Co2vi171.9 (3)
N1i—Co1—N1—C1875 (31)
Symmetry codes: (i) x, y, z; (ii) x, y1, z; (iii) x1, y1/2, z+1/2; (iv) x1, y1, z+1; (v) x+1, y1/2, z1/2; (vi) x, y+1, z.

Experimental details

(I)(II)
Crystal data
Chemical formula[Co3(C9H3O6)2(C14H14N4)3][Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2O
Mr1305.891359.94
Crystal system, space groupMonoclinic, CcMonoclinic, P21/c
Temperature (K)293293
a, b, c (Å)40.152 (9), 8.353 (3), 18.842 (5)14.160 (4), 10.105 (3), 20.927 (4)
β (°) 113.138 (9) 99.730 (6)
V3)5811 (3)2951.3 (14)
Z42
Radiation typeMo KαMo Kα
µ (mm1)0.920.91
Crystal size (mm)0.33 × 0.26 × 0.220.31 × 0.28 × 0.21
Data collection
DiffractometerBruker APEX CCD area-detector
diffractometer
Rigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Multi-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.74, 0.820.77, 0.83
No. of measured, independent and
observed [I > 2σ(I)] reflections
27961, 11621, 10356 24924, 6651, 3309
Rint0.0280.114
(sin θ/λ)max1)0.6490.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.091, 1.04 0.074, 0.165, 1.13
No. of reflections116216651
No. of parameters800413
No. of restraints20
H-atom treatmentH-atom parameters constrainedH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.08, 0.440.71, 0.69
Absolute structureFlack (1983), with how many Friedel pairs??
Absolute structure parameter0.246 (10)?

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).

Selected bond lengths (Å) for (I) top
Co1—O21.929 (2)Co2—N12iii2.014 (3)
Co1—O6i1.976 (2)Co2—N8iv2.019 (3)
Co1—N52.007 (3)Co3—O41.968 (2)
Co1—N92.012 (3)Co3—O71.986 (2)
Co2—O91.945 (2)Co3—N4v2.036 (3)
Co2—O11ii1.975 (2)Co3—N12.067 (3)
Symmetry codes: (i) x, y+1, z1/2; (ii) x, y+1, z+1/2; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y1/2, z+1; (v) x, y+3, z+1/2.
Selected bond lengths (Å) for (II) top
Co1—O2i2.033 (4)Co1—O2Wi2.178 (4)
Co1—O22.033 (4)Co2—O6ii2.003 (3)
Co1—N12.146 (4)Co2—O32.008 (3)
Co1—N1i2.146 (4)Co2—N4iii2.010 (4)
Co1—O2W2.178 (4)Co2—N52.015 (4)
Symmetry codes: (i) x, y, z; (ii) x, y1, z; (iii) x1, y1/2, z+1/2.
 

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