Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107059124/bg3062sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107059124/bg3062Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107059124/bg3062IIsup3.hkl |
CCDC references: 660610; 677093
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).
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.
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).
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).
[Co3(C9H3O6)2(C14H14N4)3] | F(000) = 2676 |
Mr = 1305.89 | Dx = 1.493 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: C -2yc | Cell parameters from 10356 reflections |
a = 40.152 (9) Å | θ = 3.2–27.5° |
b = 8.353 (3) Å | µ = 0.92 mm−1 |
c = 18.842 (5) Å | T = 293 K |
β = 113.138 (9)° | Block, purple |
V = 5811 (3) Å3 | 0.33 × 0.26 × 0.22 mm |
Z = 4 |
Bruker APEX CCD area-detector diffractometer | 11621 independent reflections |
Radiation source: fine-focus sealed tube | 10356 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −49→52 |
Tmin = 0.74, Tmax = 0.82 | k = −10→10 |
27961 measured reflections | l = −24→22 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-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 reflections | Δρmax = 1.08 e Å−3 |
800 parameters | Δρmin = −0.44 e Å−3 |
2 restraints | Absolute structure: Flack (1983), with how many Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.246 (10) |
[Co3(C9H3O6)2(C14H14N4)3] | V = 5811 (3) Å3 |
Mr = 1305.89 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 40.152 (9) Å | µ = 0.92 mm−1 |
b = 8.353 (3) Å | T = 293 K |
c = 18.842 (5) Å | 0.33 × 0.26 × 0.22 mm |
β = 113.138 (9)° |
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 = 0.82 | Rint = 0.028 |
27961 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.091 | Δρmax = 1.08 e Å−3 |
S = 1.04 | Δρmin = −0.44 e Å−3 |
11621 reflections | Absolute structure: Flack (1983), with how many Friedel pairs? |
800 parameters | Absolute structure parameter: 0.246 (10) |
2 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.833700 (10) | 0.34795 (5) | 0.23552 (2) | 0.02758 (10) | |
Co2 | 1.218513 (10) | 0.36283 (5) | 0.911351 (19) | 0.02835 (10) | |
Co3 | 1.023204 (13) | 0.89066 (5) | 0.55868 (2) | 0.03528 (12) | |
C1 | 0.87670 (9) | 0.5196 (4) | 0.46064 (18) | 0.0317 (7) | |
C2 | 0.91145 (9) | 0.5659 (4) | 0.46960 (18) | 0.0366 (7) | |
H2 | 0.9189 | 0.5513 | 0.4292 | 0.044* | |
C3 | 0.93475 (9) | 0.6328 (4) | 0.5376 (2) | 0.0370 (7) | |
C4 | 0.92436 (9) | 0.6514 (4) | 0.5987 (2) | 0.0350 (8) | |
H4 | 0.9400 | 0.6993 | 0.6441 | 0.042* | |
C5 | 0.89031 (9) | 0.5982 (4) | 0.59222 (18) | 0.0295 (6) | |
C6 | 0.86669 (8) | 0.5353 (4) | 0.52355 (18) | 0.0295 (6) | |
H6 | 0.8438 | 0.5028 | 0.5188 | 0.035* | |
C7 | 0.85084 (10) | 0.4542 (4) | 0.38543 (19) | 0.0348 (7) | |
C8 | 0.97110 (9) | 0.6922 (5) | 0.5430 (2) | 0.0450 (8) | |
C9 | 0.88050 (8) | 0.6222 (4) | 0.66050 (18) | 0.0291 (6) | |
C10 | 1.12204 (8) | 0.6835 (4) | 0.6147 (2) | 0.0340 (7) | |
C11 | 1.14568 (8) | 0.6205 (4) | 0.68378 (17) | 0.0327 (7) | |
H11 | 1.1404 | 0.6295 | 0.7274 | 0.039* | |
C12 | 1.17730 (8) | 0.5439 (4) | 0.68921 (17) | 0.0277 (6) | |
C13 | 1.18618 (8) | 0.5378 (4) | 0.62540 (16) | 0.0275 (6) | |
H13 | 1.2077 | 0.4895 | 0.6291 | 0.033* | |
C14 | 1.16285 (8) | 0.6042 (4) | 0.55538 (17) | 0.0276 (6) | |
C15 | 1.13070 (9) | 0.6730 (4) | 0.55022 (19) | 0.0323 (7) | |
H15 | 1.1146 | 0.7128 | 0.5031 | 0.039* | |
C16 | 1.08718 (9) | 0.7633 (4) | 0.6087 (2) | 0.0429 (8) | |
C17 | 1.20172 (9) | 0.4692 (4) | 0.76449 (17) | 0.0305 (6) | |
C18 | 1.17257 (9) | 0.6058 (4) | 0.48580 (16) | 0.0305 (6) | |
C19 | 1.01976 (14) | 1.3358 (5) | 0.3083 (2) | 0.0616 (12) | |
C20 | 1.04275 (14) | 1.3972 (5) | 0.2765 (2) | 0.0603 (11) | |
H20 | 1.0478 | 1.3365 | 0.2406 | 0.072* | |
C21 | 1.05817 (11) | 1.5446 (5) | 0.2965 (2) | 0.0490 (9) | |
C22 | 1.05093 (12) | 1.6375 (5) | 0.3492 (2) | 0.0535 (10) | |
H22 | 1.0611 | 1.7388 | 0.3621 | 0.064* | |
C23 | 1.02850 (14) | 1.5786 (6) | 0.3824 (3) | 0.0663 (12) | |
H23 | 1.0239 | 1.6397 | 0.4189 | 0.080* | |
C24 | 1.01265 (14) | 1.4293 (6) | 0.3622 (3) | 0.0657 (12) | |
H24 | 0.9972 | 1.3912 | 0.3845 | 0.079* | |
C25 | 1.0050 (2) | 1.1705 (7) | 0.2856 (3) | 0.0811 (2) | |
H25A | 0.9847 | 1.1752 | 0.2360 | 0.097* | |
H25B | 1.0235 | 1.1038 | 0.2797 | 0.097* | |
C26 | 1.08276 (11) | 1.6076 (6) | 0.2591 (3) | 0.0622 (11) | |
H26A | 1.1008 | 1.6781 | 0.2949 | 0.075* | |
H26B | 1.0953 | 1.5188 | 0.2474 | 0.075* | |
C27 | 1.01427 (11) | 1.0163 (4) | 0.4050 (2) | 0.0494 (8) | |
H27 | 1.0385 | 0.9916 | 0.4168 | 0.059* | |
C28 | 0.96044 (14) | 1.1094 (7) | 0.3456 (4) | 0.100 (2) | |
H28 | 0.9403 | 1.1603 | 0.3097 | 0.120* | |
C29 | 0.96214 (11) | 1.0353 (6) | 0.4103 (3) | 0.0726 (13) | |
H29 | 0.9432 | 1.0257 | 0.4268 | 0.087* | |
C30 | 1.05916 (9) | 1.8534 (5) | 0.1766 (2) | 0.0454 (8) | |
H30 | 1.0722 | 1.9293 | 0.2131 | 0.054* | |
C31 | 1.03846 (12) | 1.6258 (5) | 0.1212 (3) | 0.0547 (10) | |
H31 | 1.0340 | 1.5170 | 0.1114 | 0.066* | |
C32 | 1.02334 (13) | 1.7432 (4) | 0.0738 (2) | 0.0483 (8) | |
H32 | 1.0064 | 1.7301 | 0.0235 | 0.058* | |
C33 | 0.66493 (9) | 0.3935 (4) | 0.0907 (2) | 0.0411 (8) | |
C34 | 0.67292 (10) | 0.3682 (4) | 0.0262 (2) | 0.0411 (8) | |
H34 | 0.6957 | 0.3967 | 0.0284 | 0.049* | |
C35 | 0.64825 (10) | 0.3023 (4) | −0.0407 (2) | 0.0439 (8) | |
C36 | 0.61506 (11) | 0.2488 (6) | −0.0404 (3) | 0.0637 (12) | |
H36 | 0.5982 | 0.1988 | −0.0838 | 0.076* | |
C37 | 0.60758 (12) | 0.2704 (7) | 0.0240 (3) | 0.0771 (15) | |
H37 | 0.5855 | 0.2359 | 0.0235 | 0.092* | |
C38 | 0.63196 (11) | 0.3413 (5) | 0.0888 (3) | 0.0608 (11) | |
H38 | 0.6264 | 0.3547 | 0.1319 | 0.073* | |
C39 | 0.69031 (10) | 0.4763 (6) | 0.1622 (2) | 0.0493 (9) | |
H39A | 0.6808 | 0.5818 | 0.1649 | 0.059* | |
H39B | 0.6913 | 0.4163 | 0.2070 | 0.059* | |
C40 | 0.65591 (12) | 0.2791 (5) | −0.1116 (2) | 0.0527 (10) | |
H40A | 0.6646 | 0.1708 | −0.1121 | 0.063* | |
H40B | 0.6336 | 0.2922 | −0.1569 | 0.063* | |
C41 | 0.75422 (9) | 0.3932 (5) | 0.2001 (2) | 0.0395 (7) | |
H41 | 0.7532 | 0.3069 | 0.2304 | 0.047* | |
C42 | 0.77332 (10) | 0.5634 (5) | 0.1397 (2) | 0.0454 (9) | |
H42 | 0.7883 | 0.6167 | 0.1203 | 0.054* | |
C43 | 0.73872 (11) | 0.6045 (5) | 0.1258 (2) | 0.0500 (9) | |
H43 | 0.7256 | 0.6897 | 0.0961 | 0.060* | |
C44 | 0.68079 (11) | 0.5527 (4) | −0.1113 (2) | 0.0443 (8) | |
H44 | 0.6605 | 0.6060 | −0.1109 | 0.053* | |
C45 | 0.71658 (12) | 0.3625 (5) | −0.1148 (3) | 0.0569 (12) | |
H45 | 0.7263 | 0.2621 | −0.1162 | 0.068* | |
C46 | 0.73280 (12) | 0.5052 (5) | −0.1118 (3) | 0.0574 (11) | |
H46 | 0.7557 | 0.5195 | −0.1123 | 0.069* | |
C47 | 0.90247 (12) | −0.2141 (5) | 0.2008 (3) | 0.0539 (10) | |
C48 | 0.87886 (11) | −0.1601 (5) | 0.1295 (3) | 0.0522 (11) | |
H48 | 0.8544 | −0.1502 | 0.1203 | 0.063* | |
C49 | 0.88990 (11) | −0.1212 (5) | 0.0726 (3) | 0.0539 (10) | |
C50 | 0.92663 (13) | −0.1419 (8) | 0.0876 (4) | 0.0871 (19) | |
H50 | 0.9353 | −0.1144 | 0.0503 | 0.104* | |
C51 | 0.94985 (14) | −0.2023 (9) | 0.1570 (4) | 0.105 (2) | |
H51 | 0.9739 | −0.2216 | 0.1650 | 0.126* | |
C52 | 0.93837 (13) | −0.2346 (7) | 0.2146 (3) | 0.0754 (14) | |
H52 | 0.9546 | −0.2702 | 0.2624 | 0.090* | |
C53 | 0.89022 (15) | −0.2455 (5) | 0.2657 (3) | 0.0686 (13) | |
H53A | 0.8796 | −0.3515 | 0.2596 | 0.082* | |
H53B | 0.9110 | −0.2429 | 0.3145 | 0.082* | |
C54 | 0.86549 (11) | −0.0512 (7) | −0.0032 (3) | 0.0683 (13) | |
H54A | 0.8756 | 0.0500 | −0.0104 | 0.082* | |
H54B | 0.8650 | −0.1226 | −0.0442 | 0.082* | |
C55 | 0.86523 (10) | 0.0307 (5) | 0.2551 (2) | 0.0477 (9) | |
H55 | 0.8846 | 0.0777 | 0.2476 | 0.057* | |
C56 | 0.83185 (12) | −0.1475 (5) | 0.2756 (3) | 0.0569 (11) | |
H56 | 0.8230 | −0.2448 | 0.2848 | 0.068* | |
C57 | 0.81559 (12) | −0.0032 (5) | 0.2682 (3) | 0.0577 (11) | |
H57 | 0.7934 | 0.0160 | 0.2716 | 0.069* | |
C58 | 0.79931 (10) | −0.1172 (5) | −0.0483 (2) | 0.0443 (8) | |
H58 | 0.7997 | −0.2040 | −0.0789 | 0.053* | |
C59 | 0.81691 (11) | 0.0885 (5) | 0.0286 (3) | 0.0558 (10) | |
H59 | 0.8310 | 0.1692 | 0.0603 | 0.067* | |
C60 | 0.78207 (11) | 0.0606 (5) | 0.0121 (2) | 0.0508 (9) | |
H60 | 0.7675 | 0.1193 | 0.0306 | 0.061* | |
N1 | 0.99640 (7) | 0.9767 (4) | 0.44781 (17) | 0.0465 (7) | |
N2 | 0.99305 (12) | 1.0966 (5) | 0.3421 (2) | 0.0742 (12) | |
N3 | 1.06230 (8) | 1.6941 (4) | 0.18881 (18) | 0.0462 (7) | |
N4 | 1.03573 (8) | 1.8886 (4) | 0.10787 (17) | 0.0450 (7) | |
N5 | 0.78300 (7) | 0.4332 (4) | 0.18614 (16) | 0.0371 (6) | |
N6 | 0.72710 (7) | 0.4932 (4) | 0.16494 (18) | 0.0393 (6) | |
N7 | 0.68316 (9) | 0.3936 (4) | −0.11539 (18) | 0.0432 (7) | |
N8 | 0.71057 (9) | 0.6254 (4) | −0.10782 (17) | 0.0412 (7) | |
N9 | 0.83720 (8) | 0.1105 (3) | 0.25486 (16) | 0.0375 (6) | |
N10 | 0.86308 (9) | −0.1245 (3) | 0.2673 (2) | 0.0470 (8) | |
N11 | 0.82815 (9) | −0.0243 (4) | −0.01004 (19) | 0.0507 (8) | |
N12 | 0.77082 (8) | −0.0709 (4) | −0.03729 (16) | 0.0388 (6) | |
O1 | 0.82100 (8) | 0.4022 (4) | 0.37739 (16) | 0.0633 (9) | |
O2 | 0.86234 (7) | 0.4545 (3) | 0.33092 (13) | 0.0437 (6) | |
O3 | 0.98440 (8) | 0.6394 (4) | 0.49879 (19) | 0.0644 (8) | |
O4 | 0.98665 (7) | 0.8021 (4) | 0.59319 (16) | 0.0507 (7) | |
O5 | 0.90235 (7) | 0.6743 (4) | 0.72135 (15) | 0.0462 (6) | |
O6 | 0.84740 (6) | 0.5887 (3) | 0.64960 (12) | 0.0374 (5) | |
O7 | 1.06634 (6) | 0.8080 (3) | 0.54352 (15) | 0.0453 (6) | |
O8 | 1.08047 (8) | 0.7802 (4) | 0.66712 (17) | 0.0662 (9) | |
O9 | 1.19166 (7) | 0.4901 (3) | 0.82024 (13) | 0.0385 (5) | |
O10 | 1.22859 (7) | 0.3927 (4) | 0.77018 (14) | 0.0512 (7) | |
O11 | 1.20524 (6) | 0.5743 (3) | 0.49788 (13) | 0.0385 (5) | |
O12 | 1.14910 (7) | 0.6434 (3) | 0.42198 (14) | 0.0434 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0303 (2) | 0.0316 (2) | 0.02300 (19) | 0.00024 (17) | 0.01277 (16) | −0.00072 (16) |
Co2 | 0.0351 (2) | 0.0313 (2) | 0.0212 (2) | 0.00180 (17) | 0.01375 (18) | 0.00224 (16) |
Co3 | 0.03313 (19) | 0.0381 (2) | 0.0418 (3) | −0.00110 (19) | 0.0225 (2) | 0.00081 (18) |
C1 | 0.0349 (16) | 0.0375 (17) | 0.0241 (15) | −0.0046 (13) | 0.0130 (13) | −0.0011 (12) |
C2 | 0.0373 (16) | 0.051 (2) | 0.0301 (16) | 0.0005 (14) | 0.0224 (14) | 0.0007 (14) |
C3 | 0.0301 (15) | 0.049 (2) | 0.0348 (17) | −0.0035 (13) | 0.0156 (14) | 0.0018 (14) |
C4 | 0.0302 (16) | 0.045 (2) | 0.0309 (18) | −0.0058 (13) | 0.0135 (14) | −0.0035 (13) |
C5 | 0.0315 (15) | 0.0360 (17) | 0.0240 (15) | 0.0029 (13) | 0.0140 (13) | 0.0022 (13) |
C6 | 0.0270 (14) | 0.0382 (17) | 0.0277 (16) | −0.0057 (13) | 0.0153 (13) | 0.0019 (13) |
C7 | 0.0442 (18) | 0.0360 (18) | 0.0278 (16) | −0.0030 (14) | 0.0180 (15) | 0.0026 (13) |
C8 | 0.0314 (16) | 0.064 (2) | 0.044 (2) | −0.0013 (15) | 0.0195 (16) | 0.0092 (17) |
C9 | 0.0299 (15) | 0.0352 (16) | 0.0247 (15) | 0.0046 (13) | 0.0134 (13) | 0.0031 (13) |
C10 | 0.0285 (14) | 0.0422 (18) | 0.0350 (17) | 0.0010 (13) | 0.0166 (14) | 0.0037 (13) |
C11 | 0.0308 (14) | 0.0472 (18) | 0.0262 (15) | 0.0040 (13) | 0.0179 (13) | 0.0072 (13) |
C12 | 0.0312 (14) | 0.0323 (15) | 0.0226 (15) | −0.0008 (12) | 0.0138 (13) | −0.0006 (11) |
C13 | 0.0303 (15) | 0.0336 (16) | 0.0203 (14) | −0.0036 (12) | 0.0115 (12) | 0.0008 (11) |
C14 | 0.0279 (14) | 0.0358 (16) | 0.0222 (14) | −0.0031 (13) | 0.0132 (12) | 0.0015 (12) |
C15 | 0.0280 (15) | 0.0456 (18) | 0.0232 (15) | −0.0004 (12) | 0.0101 (13) | 0.0062 (12) |
C16 | 0.0314 (15) | 0.052 (2) | 0.051 (2) | 0.0041 (14) | 0.0224 (16) | 0.0108 (16) |
C17 | 0.0400 (17) | 0.0303 (16) | 0.0215 (15) | 0.0045 (13) | 0.0124 (13) | 0.0040 (11) |
C18 | 0.0381 (17) | 0.0370 (16) | 0.0186 (15) | −0.0052 (14) | 0.0134 (13) | −0.0029 (13) |
C19 | 0.096 (3) | 0.050 (2) | 0.0300 (19) | −0.007 (2) | 0.016 (2) | 0.0088 (16) |
C20 | 0.098 (3) | 0.053 (2) | 0.0288 (19) | 0.010 (2) | 0.023 (2) | 0.0062 (16) |
C21 | 0.060 (2) | 0.048 (2) | 0.039 (2) | 0.0117 (17) | 0.0187 (18) | 0.0094 (16) |
C22 | 0.068 (3) | 0.044 (2) | 0.054 (2) | −0.0013 (18) | 0.031 (2) | −0.0015 (17) |
C23 | 0.093 (3) | 0.064 (3) | 0.054 (3) | −0.008 (2) | 0.042 (3) | −0.012 (2) |
C24 | 0.083 (3) | 0.070 (3) | 0.053 (3) | −0.013 (2) | 0.036 (2) | 0.006 (2) |
C25 | 0.101 (6) | 0.072 (3) | 0.034 (2) | −0.037 (4) | 0.012 (3) | 0.010 (2) |
C26 | 0.056 (2) | 0.081 (3) | 0.054 (2) | 0.026 (2) | 0.027 (2) | 0.029 (2) |
C27 | 0.062 (2) | 0.043 (2) | 0.0372 (19) | −0.0018 (16) | 0.0137 (17) | 0.0066 (15) |
C28 | 0.063 (3) | 0.090 (4) | 0.085 (4) | −0.011 (3) | −0.036 (3) | 0.039 (3) |
C29 | 0.0394 (19) | 0.076 (3) | 0.083 (3) | −0.0050 (19) | 0.003 (2) | 0.010 (3) |
C30 | 0.0425 (17) | 0.058 (2) | 0.0362 (19) | 0.0003 (15) | 0.0157 (16) | 0.0003 (15) |
C31 | 0.066 (3) | 0.048 (2) | 0.050 (2) | 0.0044 (18) | 0.024 (2) | 0.0058 (17) |
C32 | 0.063 (2) | 0.0434 (17) | 0.0320 (16) | −0.003 (2) | 0.0119 (15) | −0.0005 (18) |
C33 | 0.0334 (16) | 0.0413 (19) | 0.055 (2) | 0.0097 (14) | 0.0242 (16) | 0.0046 (16) |
C34 | 0.0332 (17) | 0.045 (2) | 0.048 (2) | −0.0034 (14) | 0.0192 (16) | −0.0005 (15) |
C35 | 0.0402 (18) | 0.0295 (18) | 0.061 (2) | −0.0023 (14) | 0.0188 (18) | −0.0015 (16) |
C36 | 0.044 (2) | 0.065 (3) | 0.076 (3) | −0.0137 (18) | 0.016 (2) | −0.020 (2) |
C37 | 0.046 (2) | 0.096 (4) | 0.103 (4) | −0.019 (2) | 0.044 (3) | −0.019 (3) |
C38 | 0.044 (2) | 0.075 (3) | 0.071 (3) | −0.0021 (19) | 0.032 (2) | −0.003 (2) |
C39 | 0.0334 (17) | 0.070 (3) | 0.046 (2) | 0.0090 (17) | 0.0180 (16) | −0.0026 (18) |
C40 | 0.062 (2) | 0.037 (2) | 0.053 (2) | −0.0155 (17) | 0.016 (2) | −0.0108 (16) |
C41 | 0.0369 (17) | 0.046 (2) | 0.0390 (19) | 0.0025 (15) | 0.0187 (15) | 0.0085 (16) |
C42 | 0.0419 (18) | 0.047 (2) | 0.044 (2) | −0.0026 (15) | 0.0124 (17) | 0.0144 (16) |
C43 | 0.052 (2) | 0.037 (2) | 0.051 (2) | 0.0061 (16) | 0.0092 (19) | 0.0096 (17) |
C44 | 0.055 (2) | 0.0317 (19) | 0.053 (2) | 0.0009 (15) | 0.0287 (18) | −0.0012 (15) |
C45 | 0.063 (3) | 0.034 (2) | 0.073 (3) | 0.0094 (17) | 0.027 (2) | −0.0030 (18) |
C46 | 0.057 (2) | 0.045 (2) | 0.075 (3) | 0.0027 (17) | 0.031 (2) | −0.0091 (19) |
C47 | 0.056 (2) | 0.031 (2) | 0.075 (3) | 0.0022 (16) | 0.026 (2) | −0.0008 (18) |
C48 | 0.040 (2) | 0.046 (2) | 0.076 (3) | −0.0025 (15) | 0.029 (2) | −0.0077 (19) |
C49 | 0.0373 (19) | 0.065 (3) | 0.061 (3) | −0.0113 (18) | 0.0203 (19) | −0.015 (2) |
C50 | 0.047 (3) | 0.138 (6) | 0.092 (4) | −0.005 (3) | 0.045 (3) | −0.003 (4) |
C51 | 0.043 (2) | 0.166 (7) | 0.109 (5) | 0.016 (3) | 0.035 (3) | 0.011 (5) |
C52 | 0.052 (2) | 0.087 (4) | 0.086 (4) | 0.014 (2) | 0.027 (3) | 0.005 (3) |
C53 | 0.089 (3) | 0.036 (2) | 0.094 (4) | 0.017 (2) | 0.050 (3) | 0.014 (2) |
C54 | 0.044 (2) | 0.097 (4) | 0.073 (3) | −0.023 (2) | 0.033 (2) | −0.015 (3) |
C55 | 0.049 (2) | 0.0342 (19) | 0.064 (3) | −0.0012 (15) | 0.0265 (19) | 0.0047 (16) |
C56 | 0.064 (3) | 0.039 (2) | 0.073 (3) | −0.0108 (18) | 0.033 (2) | 0.0069 (19) |
C57 | 0.054 (2) | 0.048 (2) | 0.079 (3) | −0.0028 (18) | 0.035 (2) | 0.010 (2) |
C58 | 0.0407 (19) | 0.055 (2) | 0.044 (2) | −0.0129 (17) | 0.0235 (17) | −0.0155 (17) |
C59 | 0.053 (2) | 0.048 (2) | 0.058 (3) | −0.0123 (18) | 0.013 (2) | −0.0193 (19) |
C60 | 0.051 (2) | 0.050 (2) | 0.045 (2) | 0.0028 (17) | 0.0120 (18) | −0.0127 (17) |
N1 | 0.0402 (14) | 0.0478 (17) | 0.0408 (16) | 0.0028 (12) | 0.0045 (13) | 0.0083 (13) |
N2 | 0.091 (3) | 0.065 (2) | 0.0373 (19) | −0.020 (2) | −0.0067 (19) | 0.0183 (16) |
N3 | 0.0461 (15) | 0.0520 (18) | 0.0407 (17) | 0.0064 (13) | 0.0171 (14) | 0.0080 (13) |
N4 | 0.0441 (16) | 0.0501 (18) | 0.0401 (17) | 0.0016 (12) | 0.0158 (14) | 0.0003 (12) |
N5 | 0.0317 (13) | 0.0466 (17) | 0.0342 (15) | 0.0009 (12) | 0.0142 (12) | 0.0060 (12) |
N6 | 0.0302 (14) | 0.0468 (17) | 0.0401 (16) | 0.0078 (12) | 0.0128 (13) | 0.0024 (12) |
N7 | 0.0554 (17) | 0.0328 (16) | 0.0444 (17) | −0.0019 (13) | 0.0229 (15) | −0.0051 (13) |
N8 | 0.0517 (18) | 0.0335 (15) | 0.0416 (18) | 0.0041 (12) | 0.0216 (15) | 0.0040 (12) |
N9 | 0.0451 (15) | 0.0330 (14) | 0.0369 (16) | 0.0009 (13) | 0.0187 (14) | 0.0021 (11) |
N10 | 0.062 (2) | 0.0278 (15) | 0.055 (2) | 0.0016 (13) | 0.0273 (17) | 0.0043 (13) |
N11 | 0.0424 (17) | 0.062 (2) | 0.0483 (19) | −0.0107 (15) | 0.0187 (15) | −0.0077 (15) |
N12 | 0.0387 (14) | 0.0424 (17) | 0.0362 (16) | −0.0041 (12) | 0.0156 (13) | −0.0074 (12) |
O1 | 0.0578 (18) | 0.095 (2) | 0.0349 (15) | −0.0405 (17) | 0.0152 (13) | −0.0052 (15) |
O2 | 0.0546 (14) | 0.0548 (15) | 0.0264 (12) | −0.0092 (12) | 0.0211 (11) | −0.0103 (11) |
O3 | 0.0546 (16) | 0.076 (2) | 0.082 (2) | −0.0042 (13) | 0.0476 (17) | −0.0020 (15) |
O4 | 0.0358 (13) | 0.0724 (19) | 0.0463 (16) | −0.0151 (13) | 0.0186 (12) | 0.0008 (13) |
O5 | 0.0465 (14) | 0.0647 (17) | 0.0266 (13) | −0.0065 (12) | 0.0134 (12) | −0.0148 (11) |
O6 | 0.0324 (11) | 0.0578 (16) | 0.0264 (11) | 0.0010 (10) | 0.0164 (10) | 0.0023 (10) |
O7 | 0.0299 (12) | 0.0537 (16) | 0.0479 (16) | 0.0108 (11) | 0.0107 (12) | −0.0028 (12) |
O8 | 0.0665 (17) | 0.084 (2) | 0.073 (2) | 0.0311 (15) | 0.0534 (17) | 0.0310 (16) |
O9 | 0.0526 (13) | 0.0450 (14) | 0.0242 (11) | 0.0130 (10) | 0.0216 (10) | 0.0073 (9) |
O10 | 0.0534 (16) | 0.0716 (19) | 0.0305 (13) | 0.0307 (14) | 0.0185 (12) | 0.0079 (13) |
O11 | 0.0402 (12) | 0.0542 (16) | 0.0281 (12) | 0.0005 (11) | 0.0209 (10) | 0.0013 (10) |
O12 | 0.0443 (14) | 0.0631 (18) | 0.0216 (12) | −0.0033 (11) | 0.0117 (11) | 0.0086 (11) |
Co1—O2 | 1.929 (2) | C31—N3 | 1.380 (5) |
Co1—O6i | 1.976 (2) | C31—H31 | 0.9300 |
Co1—N5 | 2.007 (3) | C32—N4 | 1.373 (4) |
Co1—N9 | 2.012 (3) | C32—H32 | 0.9300 |
Co2—O9 | 1.945 (2) | C33—C38 | 1.381 (5) |
Co2—O11ii | 1.975 (2) | C33—C34 | 1.388 (5) |
Co2—N12iii | 2.014 (3) | C33—C39 | 1.501 (6) |
Co2—N8iv | 2.019 (3) | C34—C35 | 1.376 (5) |
Co3—O4 | 1.968 (2) | C34—H34 | 0.9300 |
Co3—O7 | 1.986 (2) | C35—C36 | 1.408 (5) |
Co3—N4v | 2.036 (3) | C35—C40 | 1.497 (5) |
Co3—N1 | 2.067 (3) | C36—C37 | 1.372 (7) |
C1—C2 | 1.393 (4) | C36—H36 | 0.9300 |
C1—C6 | 1.399 (4) | C37—C38 | 1.364 (7) |
C1—C7 | 1.493 (5) | C37—H37 | 0.9300 |
C2—C3 | 1.374 (5) | C38—H38 | 0.9300 |
C2—H2 | 0.9300 | C39—N6 | 1.464 (4) |
C3—C4 | 1.379 (5) | C39—H39A | 0.9700 |
C3—C8 | 1.507 (4) | C39—H39B | 0.9700 |
C4—C5 | 1.397 (5) | C40—N7 | 1.476 (5) |
C4—H4 | 0.9300 | C40—H40A | 0.9700 |
C5—C6 | 1.373 (5) | C40—H40B | 0.9700 |
C5—C9 | 1.500 (4) | C41—N6 | 1.325 (4) |
C6—H6 | 0.9300 | C41—N5 | 1.325 (4) |
C7—O1 | 1.227 (4) | C41—H41 | 0.9300 |
C7—O2 | 1.281 (4) | C42—C43 | 1.353 (5) |
C8—O3 | 1.234 (5) | C42—N5 | 1.353 (4) |
C8—O4 | 1.290 (5) | C42—H42 | 0.9300 |
C9—O5 | 1.218 (4) | C43—N6 | 1.378 (5) |
C9—O6 | 1.293 (4) | C43—H43 | 0.9300 |
C10—C11 | 1.379 (5) | C44—N8 | 1.319 (5) |
C10—C15 | 1.391 (4) | C44—N7 | 1.337 (5) |
C10—C16 | 1.514 (4) | C44—H44 | 0.9300 |
C11—C12 | 1.389 (4) | C45—C46 | 1.348 (6) |
C11—H11 | 0.9300 | C45—N7 | 1.363 (5) |
C12—C13 | 1.383 (4) | C45—H45 | 0.9300 |
C12—C17 | 1.507 (4) | C46—N8 | 1.365 (5) |
C13—C14 | 1.398 (4) | C46—H46 | 0.9300 |
C13—H13 | 0.9300 | C47—C52 | 1.371 (6) |
C14—C15 | 1.381 (4) | C47—C48 | 1.381 (6) |
C14—C18 | 1.508 (4) | C47—C53 | 1.510 (6) |
C15—H15 | 0.9300 | C48—C49 | 1.351 (6) |
C16—O8 | 1.240 (4) | C48—H48 | 0.9300 |
C16—O7 | 1.241 (4) | C49—C50 | 1.399 (6) |
C17—O10 | 1.222 (4) | C49—C54 | 1.497 (7) |
C17—O9 | 1.277 (4) | C50—C51 | 1.370 (8) |
C18—O12 | 1.242 (4) | C50—H50 | 0.9300 |
C18—O11 | 1.268 (4) | C51—C52 | 1.361 (8) |
C19—C20 | 1.381 (6) | C51—H51 | 0.9300 |
C19—C24 | 1.396 (6) | C52—H52 | 0.9300 |
C19—C25 | 1.497 (7) | C53—N10 | 1.494 (5) |
C20—C21 | 1.363 (6) | C53—H53A | 0.9700 |
C20—H20 | 0.9300 | C53—H53B | 0.9700 |
C21—C22 | 1.379 (5) | C54—N11 | 1.471 (5) |
C21—C26 | 1.514 (5) | C54—H54A | 0.9700 |
C22—C23 | 1.374 (6) | C54—H54B | 0.9700 |
C22—H22 | 0.9300 | C55—N9 | 1.306 (5) |
C23—C24 | 1.384 (6) | C55—N10 | 1.325 (5) |
C23—H23 | 0.9300 | C55—H55 | 0.9300 |
C24—H24 | 0.9300 | C56—N10 | 1.337 (5) |
C25—N2 | 1.465 (6) | C56—C57 | 1.352 (6) |
C25—H25A | 0.9700 | C56—H56 | 0.9300 |
C25—H25B | 0.9700 | C57—N9 | 1.375 (5) |
C26—N3 | 1.448 (5) | C57—H57 | 0.9300 |
C26—H26A | 0.9700 | C58—N12 | 1.299 (4) |
C26—H26B | 0.9700 | C58—N11 | 1.344 (5) |
C27—N1 | 1.316 (5) | C58—H58 | 0.9300 |
C27—N2 | 1.336 (5) | C59—C60 | 1.329 (5) |
C27—H27 | 0.9300 | C59—N11 | 1.371 (5) |
C28—C29 | 1.345 (8) | C59—H59 | 0.9300 |
C28—N2 | 1.341 (7) | C60—N12 | 1.395 (5) |
C28—H28 | 0.9300 | C60—H60 | 0.9300 |
C29—N1 | 1.367 (5) | N4—Co3vi | 2.036 (3) |
C29—H29 | 0.9300 | N8—Co2vii | 2.019 (3) |
C30—N4 | 1.301 (5) | N12—Co2viii | 2.014 (3) |
C30—N3 | 1.348 (5) | O6—Co1ii | 1.976 (2) |
C30—H30 | 0.9300 | O11—Co2i | 1.975 (2) |
C31—C32 | 1.305 (5) | ||
O2—Co1—O6i | 112.58 (10) | C37—C36—C35 | 119.9 (4) |
O2—Co1—N5 | 113.14 (12) | C37—C36—H36 | 120.1 |
O6i—Co1—N5 | 94.78 (10) | C35—C36—H36 | 120.1 |
O2—Co1—N9 | 108.21 (12) | C38—C37—C36 | 121.3 (4) |
O6i—Co1—N9 | 112.98 (11) | C38—C37—H37 | 119.4 |
N5—Co1—N9 | 114.82 (12) | C36—C37—H37 | 119.4 |
O9—Co2—O11ii | 110.32 (10) | C37—C38—C33 | 120.2 (4) |
O9—Co2—N12iii | 112.67 (12) | C37—C38—H38 | 119.9 |
O11ii—Co2—N12iii | 95.68 (11) | C33—C38—H38 | 119.9 |
O9—Co2—N8iv | 112.65 (12) | N6—C39—C33 | 113.3 (3) |
O11ii—Co2—N8iv | 109.52 (11) | N6—C39—H39A | 108.9 |
N12iii—Co2—N8iv | 114.69 (12) | C33—C39—H39A | 108.9 |
O4—Co3—O7 | 136.24 (10) | N6—C39—H39B | 108.9 |
O4—Co3—N4v | 105.85 (12) | C33—C39—H39B | 108.9 |
O7—Co3—N4v | 107.86 (11) | H39A—C39—H39B | 107.7 |
O4—Co3—N1 | 107.75 (12) | N7—C40—C35 | 112.0 (3) |
O7—Co3—N1 | 96.46 (11) | N7—C40—H40A | 109.2 |
N4v—Co3—N1 | 94.74 (12) | C35—C40—H40A | 109.2 |
C2—C1—C6 | 118.6 (3) | N7—C40—H40B | 109.2 |
C2—C1—C7 | 120.4 (3) | C35—C40—H40B | 109.2 |
C6—C1—C7 | 121.0 (3) | H40A—C40—H40B | 107.9 |
C3—C2—C1 | 120.6 (3) | N6—C41—N5 | 110.5 (3) |
C3—C2—H2 | 119.7 | N6—C41—H41 | 124.7 |
C1—C2—H2 | 119.7 | N5—C41—H41 | 124.7 |
C2—C3—C4 | 120.4 (3) | C43—C42—N5 | 110.0 (3) |
C2—C3—C8 | 119.0 (3) | C43—C42—H42 | 125.0 |
C4—C3—C8 | 120.6 (3) | N5—C42—H42 | 125.0 |
C3—C4—C5 | 119.9 (3) | C42—C43—N6 | 105.2 (3) |
C3—C4—H4 | 120.0 | C42—C43—H43 | 127.4 |
C5—C4—H4 | 120.0 | N6—C43—H43 | 127.4 |
C6—C5—C4 | 119.6 (3) | N8—C44—N7 | 112.1 (3) |
C6—C5—C9 | 122.9 (3) | N8—C44—H44 | 123.9 |
C4—C5—C9 | 117.5 (3) | N7—C44—H44 | 123.9 |
C5—C6—C1 | 120.8 (3) | C46—C45—N7 | 106.8 (4) |
C5—C6—H6 | 119.6 | C46—C45—H45 | 126.6 |
C1—C6—H6 | 119.6 | N7—C45—H45 | 126.6 |
O1—C7—O2 | 123.0 (3) | C45—C46—N8 | 109.7 (4) |
O1—C7—C1 | 121.9 (3) | C45—C46—H46 | 125.1 |
O2—C7—C1 | 115.2 (3) | N8—C46—H46 | 125.1 |
O3—C8—O4 | 122.4 (3) | C52—C47—C48 | 119.6 (5) |
O3—C8—C3 | 120.1 (4) | C52—C47—C53 | 118.6 (5) |
O4—C8—C3 | 117.4 (3) | C48—C47—C53 | 121.8 (4) |
O5—C9—O6 | 122.8 (3) | C49—C48—C47 | 122.5 (4) |
O5—C9—C5 | 121.4 (3) | C49—C48—H48 | 118.8 |
O6—C9—C5 | 115.8 (3) | C47—C48—H48 | 118.8 |
C11—C10—C15 | 119.0 (3) | C48—C49—C50 | 117.3 (5) |
C11—C10—C16 | 120.7 (3) | C48—C49—C54 | 123.7 (4) |
C15—C10—C16 | 120.2 (3) | C50—C49—C54 | 119.0 (4) |
C10—C11—C12 | 121.0 (3) | C51—C50—C49 | 120.5 (5) |
C10—C11—H11 | 119.5 | C51—C50—H50 | 119.8 |
C12—C11—H11 | 119.5 | C49—C50—H50 | 119.8 |
C13—C12—C11 | 119.6 (3) | C52—C51—C50 | 121.1 (5) |
C13—C12—C17 | 120.6 (3) | C52—C51—H51 | 119.4 |
C11—C12—C17 | 119.9 (3) | C50—C51—H51 | 119.4 |
C12—C13—C14 | 120.0 (3) | C51—C52—C47 | 119.0 (5) |
C12—C13—H13 | 120.0 | C51—C52—H52 | 120.5 |
C14—C13—H13 | 120.0 | C47—C52—H52 | 120.5 |
C15—C14—C13 | 119.5 (3) | N10—C53—C47 | 111.7 (4) |
C15—C14—C18 | 119.3 (3) | N10—C53—H53A | 109.3 |
C13—C14—C18 | 121.2 (3) | C47—C53—H53A | 109.3 |
C14—C15—C10 | 120.8 (3) | N10—C53—H53B | 109.3 |
C14—C15—H15 | 119.6 | C47—C53—H53B | 109.3 |
C10—C15—H15 | 119.6 | H53A—C53—H53B | 107.9 |
O8—C16—O7 | 123.2 (3) | N11—C54—C49 | 114.0 (3) |
O8—C16—C10 | 120.1 (3) | N11—C54—H54A | 108.8 |
O7—C16—C10 | 116.8 (3) | C49—C54—H54A | 108.8 |
O10—C17—O9 | 123.6 (3) | N11—C54—H54B | 108.8 |
O10—C17—C12 | 121.7 (3) | C49—C54—H54B | 108.8 |
O9—C17—C12 | 114.7 (3) | H54A—C54—H54B | 107.7 |
O12—C18—O11 | 124.3 (3) | N9—C55—N10 | 112.6 (3) |
O12—C18—C14 | 119.1 (3) | N9—C55—H55 | 123.7 |
O11—C18—C14 | 116.4 (3) | N10—C55—H55 | 123.7 |
C20—C19—C24 | 118.0 (4) | N10—C56—C57 | 107.3 (3) |
C20—C19—C25 | 118.4 (4) | N10—C56—H56 | 126.4 |
C24—C19—C25 | 123.6 (4) | C57—C56—H56 | 126.4 |
C21—C20—C19 | 121.7 (4) | C56—C57—N9 | 108.7 (4) |
C21—C20—H20 | 119.2 | C56—C57—H57 | 125.6 |
C19—C20—H20 | 119.2 | N9—C57—H57 | 125.6 |
C20—C21—C22 | 120.4 (4) | N12—C58—N11 | 111.7 (3) |
C20—C21—C26 | 119.6 (4) | N12—C58—H58 | 124.2 |
C22—C21—C26 | 120.0 (4) | N11—C58—H58 | 124.2 |
C23—C22—C21 | 119.3 (4) | C60—C59—N11 | 106.9 (3) |
C23—C22—H22 | 120.4 | C60—C59—H59 | 126.5 |
C21—C22—H22 | 120.4 | N11—C59—H59 | 126.5 |
C22—C23—C24 | 120.6 (4) | C59—C60—N12 | 109.2 (3) |
C22—C23—H23 | 119.7 | C59—C60—H60 | 125.4 |
C24—C23—H23 | 119.7 | N12—C60—H60 | 125.4 |
C23—C24—C19 | 120.1 (4) | C27—N1—C29 | 105.9 (3) |
C23—C24—H24 | 119.9 | C27—N1—Co3 | 121.0 (2) |
C19—C24—H24 | 119.9 | C29—N1—Co3 | 131.7 (3) |
N2—C25—C19 | 112.7 (4) | C27—N2—C28 | 107.0 (4) |
N2—C25—H25A | 109.0 | C27—N2—C25 | 125.4 (5) |
C19—C25—H25A | 109.0 | C28—N2—C25 | 127.4 (5) |
N2—C25—H25B | 109.0 | C30—N3—C31 | 105.4 (3) |
C19—C25—H25B | 109.0 | C30—N3—C26 | 129.0 (4) |
H25A—C25—H25B | 107.8 | C31—N3—C26 | 125.2 (4) |
N3—C26—C21 | 111.1 (3) | C30—N4—C32 | 104.7 (3) |
N3—C26—H26A | 109.4 | C30—N4—Co3vi | 127.6 (3) |
C21—C26—H26A | 109.4 | C32—N4—Co3vi | 127.5 (3) |
N3—C26—H26B | 109.4 | C41—N5—C42 | 106.2 (3) |
C21—C26—H26B | 109.4 | C41—N5—Co1 | 128.5 (2) |
H26A—C26—H26B | 108.0 | C42—N5—Co1 | 124.5 (2) |
N1—C27—N2 | 111.0 (4) | C41—N6—C43 | 108.0 (3) |
N1—C27—H27 | 124.5 | C41—N6—C39 | 125.2 (3) |
N2—C27—H27 | 124.5 | C43—N6—C39 | 126.5 (3) |
C29—C28—N2 | 107.8 (4) | C44—N7—C45 | 106.3 (3) |
C29—C28—H28 | 126.1 | C44—N7—C40 | 124.8 (3) |
N2—C28—H28 | 126.1 | C45—N7—C40 | 128.5 (3) |
C28—C29—N1 | 108.4 (5) | C44—N8—C46 | 105.0 (3) |
C28—C29—H29 | 125.8 | C44—N8—Co2vii | 122.5 (2) |
N1—C29—H29 | 125.8 | C46—N8—Co2vii | 132.2 (3) |
N4—C30—N3 | 112.0 (3) | C55—N9—C57 | 104.6 (3) |
N4—C30—H30 | 124.0 | C55—N9—Co1 | 120.2 (2) |
N3—C30—H30 | 124.0 | C57—N9—Co1 | 135.2 (3) |
C32—C31—N3 | 106.8 (4) | C55—N10—C56 | 106.8 (3) |
C32—C31—H31 | 126.6 | C55—N10—C53 | 124.1 (3) |
N3—C31—H31 | 126.6 | C56—N10—C53 | 129.0 (3) |
C31—C32—N4 | 111.0 (4) | C58—N11—C59 | 106.7 (3) |
C31—C32—H32 | 124.5 | C58—N11—C54 | 126.3 (4) |
N4—C32—H32 | 124.5 | C59—N11—C54 | 126.5 (4) |
C38—C33—C34 | 118.6 (4) | C58—N12—C60 | 105.5 (3) |
C38—C33—C39 | 118.3 (4) | C58—N12—Co2viii | 131.2 (2) |
C34—C33—C39 | 123.1 (3) | C60—N12—Co2viii | 122.7 (2) |
C35—C34—C33 | 122.1 (3) | C7—O2—Co1 | 118.4 (2) |
C35—C34—H34 | 118.9 | C8—O4—Co3 | 103.5 (2) |
C33—C34—H34 | 118.9 | C9—O6—Co1ii | 114.3 (2) |
C34—C35—C36 | 117.7 (4) | C16—O7—Co3 | 104.4 (2) |
C34—C35—C40 | 122.9 (3) | C17—O9—Co2 | 114.0 (2) |
C36—C35—C40 | 119.3 (4) | C18—O11—Co2i | 113.1 (2) |
C6—C1—C2—C3 | −3.2 (5) | C28—C29—N1—Co3 | 166.0 (4) |
C7—C1—C2—C3 | 177.0 (3) | O4—Co3—N1—C27 | −167.6 (3) |
C1—C2—C3—C4 | 1.7 (5) | O7—Co3—N1—C27 | −24.5 (3) |
C1—C2—C3—C8 | −175.6 (3) | N4v—Co3—N1—C27 | 84.1 (3) |
C2—C3—C4—C5 | 1.6 (5) | O4—Co3—N1—C29 | 28.1 (4) |
C8—C3—C4—C5 | 178.9 (3) | O7—Co3—N1—C29 | 171.1 (4) |
C3—C4—C5—C6 | −3.4 (5) | N4v—Co3—N1—C29 | −80.3 (4) |
C3—C4—C5—C9 | −179.8 (3) | N1—C27—N2—C28 | 0.4 (5) |
C4—C5—C6—C1 | 1.9 (5) | N1—C27—N2—C25 | 174.4 (4) |
C9—C5—C6—C1 | 178.1 (3) | C29—C28—N2—C27 | −0.5 (6) |
C2—C1—C6—C5 | 1.4 (5) | C29—C28—N2—C25 | −174.3 (5) |
C7—C1—C6—C5 | −178.8 (3) | C19—C25—N2—C27 | −85.7 (7) |
C2—C1—C7—O1 | 174.9 (4) | C19—C25—N2—C28 | 87.1 (7) |
C6—C1—C7—O1 | −5.0 (5) | N4—C30—N3—C31 | −0.2 (4) |
C2—C1—C7—O2 | −4.1 (5) | N4—C30—N3—C26 | −173.9 (3) |
C6—C1—C7—O2 | 176.0 (3) | C32—C31—N3—C30 | 0.9 (4) |
C2—C3—C8—O3 | −22.2 (5) | C32—C31—N3—C26 | 174.9 (3) |
C4—C3—C8—O3 | 160.4 (4) | C21—C26—N3—C30 | 102.9 (5) |
C2—C3—C8—O4 | 155.5 (3) | C21—C26—N3—C31 | −69.7 (5) |
C4—C3—C8—O4 | −21.8 (5) | N3—C30—N4—C32 | −0.5 (4) |
C6—C5—C9—O5 | 178.0 (3) | N3—C30—N4—Co3vi | −176.1 (2) |
C4—C5—C9—O5 | −5.7 (5) | C31—C32—N4—C30 | 1.1 (5) |
C6—C5—C9—O6 | −4.0 (5) | C31—C32—N4—Co3vi | 176.7 (3) |
C4—C5—C9—O6 | 172.3 (3) | N6—C41—N5—C42 | −0.4 (4) |
C15—C10—C11—C12 | −1.6 (5) | N6—C41—N5—Co1 | 170.1 (2) |
C16—C10—C11—C12 | 178.5 (3) | C43—C42—N5—C41 | 0.6 (5) |
C10—C11—C12—C13 | 3.4 (5) | C43—C42—N5—Co1 | −170.4 (3) |
C10—C11—C12—C17 | −177.0 (3) | O2—Co1—N5—C41 | −84.7 (3) |
C11—C12—C13—C14 | −2.0 (5) | O6i—Co1—N5—C41 | 158.3 (3) |
C17—C12—C13—C14 | 178.5 (3) | N9—Co1—N5—C41 | 40.2 (4) |
C12—C13—C14—C15 | −1.2 (5) | O2—Co1—N5—C42 | 84.2 (3) |
C12—C13—C14—C18 | 177.3 (3) | O6i—Co1—N5—C42 | −32.8 (3) |
C13—C14—C15—C10 | 3.0 (5) | N9—Co1—N5—C42 | −150.9 (3) |
C18—C14—C15—C10 | −175.6 (3) | N5—C41—N6—C43 | 0.1 (4) |
C11—C10—C15—C14 | −1.6 (5) | N5—C41—N6—C39 | 174.2 (3) |
C16—C10—C15—C14 | 178.3 (3) | C42—C43—N6—C41 | 0.3 (4) |
C11—C10—C16—O8 | 3.8 (5) | C42—C43—N6—C39 | −173.7 (4) |
C15—C10—C16—O8 | −176.1 (3) | C33—C39—N6—C41 | −94.9 (5) |
C11—C10—C16—O7 | −175.7 (3) | C33—C39—N6—C43 | 78.1 (5) |
C15—C10—C16—O7 | 4.5 (5) | N8—C44—N7—C45 | −0.3 (5) |
C13—C12—C17—O10 | −4.8 (5) | N8—C44—N7—C40 | 173.2 (3) |
C11—C12—C17—O10 | 175.6 (3) | C46—C45—N7—C44 | −1.1 (5) |
C13—C12—C17—O9 | 176.3 (3) | C46—C45—N7—C40 | −174.2 (4) |
C11—C12—C17—O9 | −3.2 (4) | C35—C40—N7—C44 | −54.8 (5) |
C15—C14—C18—O12 | −12.2 (5) | C35—C40—N7—C45 | 117.2 (5) |
C13—C14—C18—O12 | 169.3 (3) | N7—C44—N8—C46 | 1.5 (4) |
C15—C14—C18—O11 | 164.9 (3) | N7—C44—N8—Co2vii | −172.7 (2) |
C13—C14—C18—O11 | −13.6 (5) | C45—C46—N8—C44 | −2.1 (5) |
C24—C19—C20—C21 | −0.1 (7) | C45—C46—N8—Co2vii | 171.2 (3) |
C25—C19—C20—C21 | −177.8 (5) | N10—C55—N9—C57 | 0.2 (5) |
C19—C20—C21—C22 | −0.4 (7) | N10—C55—N9—Co1 | −178.8 (3) |
C19—C20—C21—C26 | −179.1 (4) | C56—C57—N9—C55 | −0.3 (5) |
C20—C21—C22—C23 | 1.1 (7) | C56—C57—N9—Co1 | 178.6 (3) |
C26—C21—C22—C23 | 179.9 (4) | O2—Co1—N9—C55 | −81.4 (3) |
C21—C22—C23—C24 | −1.4 (7) | O6i—Co1—N9—C55 | 43.9 (3) |
C22—C23—C24—C19 | 0.9 (8) | N5—Co1—N9—C55 | 151.1 (3) |
C20—C19—C24—C23 | −0.1 (7) | O2—Co1—N9—C57 | 99.8 (4) |
C25—C19—C24—C23 | 177.4 (5) | O6i—Co1—N9—C57 | −134.8 (4) |
C20—C19—C25—N2 | 158.1 (5) | N5—Co1—N9—C57 | −27.6 (4) |
C24—C19—C25—N2 | −19.3 (8) | N9—C55—N10—C56 | −0.1 (5) |
C20—C21—C26—N3 | 89.1 (5) | N9—C55—N10—C53 | 176.1 (4) |
C22—C21—C26—N3 | −89.6 (5) | C57—C56—N10—C55 | 0.0 (5) |
N2—C28—C29—N1 | 0.4 (7) | C57—C56—N10—C53 | −176.1 (5) |
N3—C31—C32—N4 | −1.2 (5) | C47—C53—N10—C55 | −40.9 (6) |
C38—C33—C34—C35 | 4.2 (6) | C47—C53—N10—C56 | 134.5 (5) |
C39—C33—C34—C35 | −175.2 (4) | N12—C58—N11—C59 | 0.6 (5) |
C33—C34—C35—C36 | −4.9 (6) | N12—C58—N11—C54 | 173.5 (4) |
C33—C34—C35—C40 | 177.9 (4) | C60—C59—N11—C58 | −0.3 (5) |
C34—C35—C36—C37 | 3.2 (7) | C60—C59—N11—C54 | −173.3 (4) |
C40—C35—C36—C37 | −179.5 (4) | C49—C54—N11—C58 | −101.6 (5) |
C35—C36—C37—C38 | −0.9 (8) | C49—C54—N11—C59 | 70.0 (6) |
C36—C37—C38—C33 | 0.1 (8) | N11—C58—N12—C60 | −0.5 (5) |
C34—C33—C38—C37 | −1.7 (7) | N11—C58—N12—Co2viii | 170.2 (3) |
C39—C33—C38—C37 | 177.8 (4) | C59—C60—N12—C58 | 0.3 (5) |
C38—C33—C39—N6 | 166.8 (4) | C59—C60—N12—Co2viii | −171.4 (3) |
C34—C33—C39—N6 | −13.8 (5) | O1—C7—O2—Co1 | −6.8 (5) |
C34—C35—C40—N7 | −26.0 (5) | C1—C7—O2—Co1 | 172.2 (2) |
C36—C35—C40—N7 | 156.9 (4) | O6i—Co1—O2—C7 | 163.6 (2) |
N5—C42—C43—N6 | −0.6 (5) | N5—Co1—O2—C7 | 57.5 (3) |
N7—C45—C46—N8 | 2.0 (5) | N9—Co1—O2—C7 | −70.9 (3) |
C52—C47—C48—C49 | −2.2 (7) | O3—C8—O4—Co3 | 15.5 (4) |
C53—C47—C48—C49 | 175.4 (4) | C3—C8—O4—Co3 | −162.2 (3) |
C47—C48—C49—C50 | 1.8 (7) | O7—Co3—O4—C8 | −61.2 (3) |
C47—C48—C49—C54 | −175.4 (4) | N4v—Co3—O4—C8 | 159.6 (2) |
C48—C49—C50—C51 | 1.3 (8) | N1—Co3—O4—C8 | 59.1 (3) |
C54—C49—C50—C51 | 178.6 (6) | O5—C9—O6—Co1ii | 6.6 (4) |
C49—C50—C51—C52 | −4.0 (11) | C5—C9—O6—Co1ii | −171.3 (2) |
C50—C51—C52—C47 | 3.5 (10) | O8—C16—O7—Co3 | −3.3 (4) |
C48—C47—C52—C51 | −0.5 (8) | C10—C16—O7—Co3 | 176.2 (2) |
C53—C47—C52—C51 | −178.2 (5) | O4—Co3—O7—C16 | −61.5 (3) |
C52—C47—C53—N10 | 139.9 (5) | N4v—Co3—O7—C16 | 77.2 (3) |
C48—C47—C53—N10 | −37.7 (6) | N1—Co3—O7—C16 | 174.3 (2) |
C48—C49—C54—N11 | 1.4 (7) | O10—C17—O9—Co2 | −8.9 (4) |
C50—C49—C54—N11 | −175.7 (5) | C12—C17—O9—Co2 | 169.9 (2) |
N10—C56—C57—N9 | 0.2 (6) | O11ii—Co2—O9—C17 | 172.5 (2) |
N11—C59—C60—N12 | 0.0 (5) | N12iii—Co2—O9—C17 | 66.9 (3) |
N2—C27—N1—C29 | −0.2 (5) | N8iv—Co2—O9—C17 | −64.8 (3) |
N2—C27—N1—Co3 | −168.1 (3) | O12—C18—O11—Co2i | 13.0 (4) |
C28—C29—N1—C27 | −0.2 (6) | C14—C18—O11—Co2i | −163.9 (2) |
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+3, z+1/2; (vi) x, −y+3, z−1/2; (vii) x−1/2, y+1/2, z−1; (viii) x−1/2, y−1/2, z−1. |
[Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2O | F(000) = 1398 |
Mr = 1359.94 | Dx = 1.530 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2ybc | Cell parameters from 6672 reflections |
a = 14.160 (4) Å | θ = 3.0–27.5° |
b = 10.105 (3) Å | µ = 0.91 mm−1 |
c = 20.927 (4) Å | T = 293 K |
β = 99.730 (6)° | Block, violet |
V = 2951.3 (14) Å3 | 0.31 × 0.28 × 0.21 mm |
Z = 2 |
Rigaku R-AXIS RAPID diffractometer | 6651 independent reflections |
Radiation source: fine-focus sealed tube | 3309 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.114 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→18 |
Tmin = 0.77, Tmax = 0.83 | k = −12→13 |
24924 measured reflections | l = −24→27 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.074 | H 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 reflections | Δρmax = 0.71 e Å−3 |
413 parameters | Δρmin = −0.69 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0016 (4) |
[Co3(C9H3O6)2(C14H14N4)3(H2O)2]·H2O | V = 2951.3 (14) Å3 |
Mr = 1359.94 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.160 (4) Å | µ = 0.91 mm−1 |
b = 10.105 (3) Å | T = 293 K |
c = 20.927 (4) Å | 0.31 × 0.28 × 0.21 mm |
β = 99.730 (6)° |
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 = 0.83 | Rint = 0.114 |
24924 measured reflections |
R[F2 > 2σ(F2)] = 0.074 | 0 restraints |
wR(F2) = 0.165 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | Δρmax = 0.71 e Å−3 |
6651 reflections | Δρmin = −0.69 e Å−3 |
413 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.0452 (3) | |
Co2 | −0.39399 (5) | −0.31962 (6) | 0.18718 (3) | 0.0407 (2) | |
C1 | −0.2211 (4) | 0.1803 (5) | 0.0839 (2) | 0.0376 (11) | |
C2 | −0.2593 (4) | 0.0615 (4) | 0.1011 (2) | 0.0358 (11) | |
H2 | −0.2357 | −0.0175 | 0.0873 | 0.043* | |
C3 | −0.3315 (4) | 0.0576 (4) | 0.1382 (2) | 0.0345 (11) | |
C4 | −0.3659 (4) | 0.1764 (4) | 0.1587 (2) | 0.0360 (11) | |
H4 | −0.4155 | 0.1756 | 0.1827 | 0.043* | |
C5 | −0.3271 (4) | 0.2959 (4) | 0.1437 (2) | 0.0379 (11) | |
C6 | −0.2560 (4) | 0.2975 (4) | 0.1055 (2) | 0.0395 (12) | |
H6 | −0.2314 | 0.3779 | 0.0943 | 0.047* | |
C7 | −0.1441 (4) | 0.1804 (5) | 0.0434 (2) | 0.0429 (12) | |
C8 | −0.3682 (4) | −0.0701 (4) | 0.1591 (2) | 0.0380 (11) | |
C9 | −0.3577 (4) | 0.4225 (5) | 0.1720 (2) | 0.0435 (13) | |
C10 | 0.0442 (4) | 0.0452 (5) | −0.2916 (2) | 0.0490 (13) | |
C11 | 0.0323 (5) | 0.0285 (6) | −0.3577 (3) | 0.0666 (18) | |
H11 | −0.0145 | 0.0767 | −0.3845 | 0.080* | |
C12 | 0.0893 (5) | −0.0590 (6) | −0.3848 (3) | 0.0678 (18) | |
H12 | 0.0801 | −0.0690 | −0.4296 | 0.081* | |
C13 | 0.1586 (4) | −0.1309 (6) | −0.3469 (3) | 0.0512 (14) | |
C14 | 0.1706 (5) | −0.1139 (7) | −0.2816 (3) | 0.0696 (18) | |
H14 | 0.2179 | −0.1617 | −0.2551 | 0.083* | |
C15 | 0.1148 (5) | −0.0284 (7) | −0.2542 (3) | 0.0715 (19) | |
H15 | 0.1245 | −0.0195 | −0.2093 | 0.086* | |
C16 | −0.0190 (5) | 0.1358 (6) | −0.2614 (3) | 0.0630 (16) | |
H16A | 0.0152 | 0.2174 | −0.2487 | 0.076* | |
H16B | −0.0751 | 0.1575 | −0.2930 | 0.076* | |
C17 | 0.2173 (4) | −0.2320 (6) | −0.3756 (3) | 0.0592 (15) | |
H17A | 0.2216 | −0.3117 | −0.3494 | 0.071* | |
H17B | 0.1846 | −0.2547 | −0.4188 | 0.071* | |
C18 | −0.0096 (4) | 0.0952 (6) | −0.1425 (2) | 0.0528 (14) | |
H18 | 0.0372 | 0.1584 | −0.1288 | 0.063* | |
C19 | −0.1122 (5) | −0.0232 (6) | −0.2051 (3) | 0.0639 (16) | |
H19 | −0.1504 | −0.0594 | −0.2414 | 0.077* | |
C20 | −0.1101 (5) | −0.0610 (6) | −0.1432 (3) | 0.0619 (16) | |
H20 | −0.1472 | −0.1280 | −0.1297 | 0.074* | |
C21 | 0.3935 (4) | −0.2166 (5) | −0.3394 (2) | 0.0477 (13) | |
H21 | 0.3965 | −0.2733 | −0.3041 | 0.057* | |
C22 | 0.4318 (5) | −0.0816 (5) | −0.4097 (2) | 0.0509 (14) | |
H22 | 0.4673 | −0.0264 | −0.4321 | 0.061* | |
C23 | 0.3378 (5) | −0.1013 (5) | −0.4249 (3) | 0.0544 (15) | |
H23 | 0.2968 | −0.0640 | −0.4596 | 0.065* | |
C24 | −0.3740 (4) | −0.3976 (5) | 0.3275 (2) | 0.0484 (13) | |
H24 | −0.3969 | −0.4825 | 0.3171 | 0.058* | |
C25 | −0.3162 (6) | −0.2291 (7) | 0.3834 (3) | 0.089 (3) | |
H25 | −0.2905 | −0.1743 | 0.4177 | 0.107* | |
C26 | −0.3333 (6) | −0.1962 (6) | 0.3212 (3) | 0.087 (3) | |
H26 | −0.3230 | −0.1129 | 0.3048 | 0.104* | |
C27 | −0.3303 (5) | −0.4358 (6) | 0.4472 (3) | 0.0639 (17) | |
H27A | −0.2870 | −0.3897 | 0.4807 | 0.077* | |
H27B | −0.2996 | −0.5181 | 0.4385 | 0.077* | |
C28 | −0.4199 (4) | −0.4682 (5) | 0.4731 (2) | 0.0453 (13) | |
C29 | −0.4733 (4) | −0.3691 (6) | 0.4957 (2) | 0.0548 (15) | |
H29 | −0.4558 | −0.2808 | 0.4928 | 0.066* | |
C30 | −0.4476 (4) | −0.5977 (5) | 0.4776 (2) | 0.0523 (14) | |
H30 | −0.4122 | −0.6643 | 0.4621 | 0.063* | |
N1 | −0.0443 (3) | 0.0148 (4) | −0.10300 (19) | 0.0497 (11) | |
N2 | −0.0492 (4) | 0.0764 (5) | −0.2048 (2) | 0.0533 (12) | |
N3 | 0.3129 (3) | −0.1871 (4) | −0.37973 (19) | 0.0469 (11) | |
N4 | 0.4691 (3) | −0.1553 (4) | −0.35562 (18) | 0.0458 (11) | |
N5 | −0.3682 (3) | −0.3033 (4) | 0.28452 (19) | 0.0448 (10) | |
N6 | −0.3426 (3) | −0.3549 (4) | 0.38804 (19) | 0.0496 (11) | |
O1 | −0.1030 (3) | 0.2874 (4) | 0.03588 (16) | 0.0562 (10) | |
O2 | −0.1265 (3) | 0.0715 (3) | 0.01901 (16) | 0.0506 (9) | |
O3 | −0.3241 (3) | −0.1767 (3) | 0.14743 (15) | 0.0444 (8) | |
O4 | −0.4372 (3) | −0.0735 (3) | 0.18735 (16) | 0.0511 (9) | |
O5 | −0.4086 (3) | 0.4172 (3) | 0.21359 (18) | 0.0618 (11) | |
O6 | −0.3272 (3) | 0.5302 (3) | 0.15094 (16) | 0.0534 (10) | |
O1WA | 0.1962 (5) | 0.2943 (6) | −0.0782 (4) | 0.057 (2) | 0.50 |
O2W | 0.0631 (3) | 0.1971 (4) | 0.00627 (17) | 0.0593 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0479 (7) | 0.0392 (6) | 0.0539 (6) | −0.0025 (5) | 0.0246 (4) | −0.0045 (4) |
Co2 | 0.0490 (5) | 0.0264 (4) | 0.0501 (4) | −0.0002 (3) | 0.0179 (3) | 0.0018 (3) |
C1 | 0.039 (3) | 0.031 (3) | 0.044 (3) | −0.002 (2) | 0.011 (2) | 0.000 (2) |
C2 | 0.043 (3) | 0.022 (2) | 0.042 (3) | 0.005 (2) | 0.006 (2) | −0.0038 (18) |
C3 | 0.042 (3) | 0.025 (2) | 0.036 (2) | 0.000 (2) | 0.007 (2) | −0.0015 (18) |
C4 | 0.044 (3) | 0.025 (2) | 0.040 (2) | −0.002 (2) | 0.011 (2) | −0.0034 (18) |
C5 | 0.044 (3) | 0.024 (3) | 0.047 (3) | 0.004 (2) | 0.011 (2) | 0.0017 (18) |
C6 | 0.049 (3) | 0.024 (3) | 0.047 (3) | 0.000 (2) | 0.014 (2) | 0.0024 (19) |
C7 | 0.046 (3) | 0.038 (3) | 0.047 (3) | −0.003 (3) | 0.014 (2) | −0.009 (2) |
C8 | 0.046 (3) | 0.026 (3) | 0.044 (3) | −0.004 (2) | 0.013 (2) | 0.0006 (19) |
C9 | 0.050 (4) | 0.025 (3) | 0.058 (3) | 0.009 (2) | 0.014 (3) | −0.001 (2) |
C10 | 0.046 (4) | 0.053 (3) | 0.049 (3) | 0.004 (3) | 0.011 (2) | 0.006 (2) |
C11 | 0.066 (5) | 0.078 (5) | 0.052 (4) | 0.032 (4) | −0.001 (3) | 0.014 (3) |
C12 | 0.078 (5) | 0.078 (5) | 0.047 (3) | 0.016 (4) | 0.009 (3) | 0.002 (3) |
C13 | 0.044 (4) | 0.052 (3) | 0.059 (3) | −0.005 (3) | 0.011 (3) | −0.007 (3) |
C14 | 0.062 (5) | 0.085 (5) | 0.057 (4) | 0.024 (4) | −0.003 (3) | 0.002 (3) |
C15 | 0.077 (5) | 0.088 (5) | 0.047 (3) | 0.025 (4) | 0.003 (3) | 0.000 (3) |
C16 | 0.075 (5) | 0.057 (4) | 0.063 (4) | 0.008 (3) | 0.030 (3) | 0.011 (3) |
C17 | 0.046 (4) | 0.061 (4) | 0.072 (4) | −0.001 (3) | 0.012 (3) | −0.009 (3) |
C18 | 0.050 (4) | 0.057 (4) | 0.053 (3) | 0.001 (3) | 0.014 (3) | −0.007 (3) |
C19 | 0.060 (4) | 0.069 (4) | 0.064 (4) | −0.003 (3) | 0.012 (3) | −0.012 (3) |
C20 | 0.062 (5) | 0.055 (4) | 0.072 (4) | −0.007 (3) | 0.021 (3) | −0.006 (3) |
C21 | 0.058 (4) | 0.034 (3) | 0.055 (3) | 0.002 (3) | 0.018 (3) | 0.003 (2) |
C22 | 0.060 (4) | 0.037 (3) | 0.061 (3) | 0.003 (3) | 0.022 (3) | 0.012 (2) |
C23 | 0.059 (4) | 0.043 (3) | 0.062 (3) | 0.008 (3) | 0.012 (3) | 0.004 (3) |
C24 | 0.054 (4) | 0.038 (3) | 0.054 (3) | −0.006 (3) | 0.013 (2) | 0.004 (2) |
C25 | 0.162 (8) | 0.044 (4) | 0.059 (4) | 0.002 (4) | 0.009 (4) | −0.005 (3) |
C26 | 0.163 (8) | 0.033 (3) | 0.058 (4) | −0.018 (4) | 0.002 (4) | 0.005 (3) |
C27 | 0.064 (5) | 0.073 (4) | 0.058 (3) | 0.018 (3) | 0.018 (3) | 0.027 (3) |
C28 | 0.047 (4) | 0.052 (3) | 0.038 (3) | 0.009 (3) | 0.014 (2) | 0.005 (2) |
C29 | 0.069 (4) | 0.039 (3) | 0.059 (3) | −0.002 (3) | 0.018 (3) | −0.004 (2) |
C30 | 0.066 (4) | 0.042 (3) | 0.050 (3) | 0.012 (3) | 0.015 (3) | −0.002 (2) |
N1 | 0.052 (3) | 0.049 (3) | 0.055 (3) | −0.003 (2) | 0.031 (2) | −0.003 (2) |
N2 | 0.058 (3) | 0.048 (3) | 0.057 (3) | 0.004 (2) | 0.018 (2) | 0.002 (2) |
N3 | 0.046 (3) | 0.040 (3) | 0.056 (3) | 0.000 (2) | 0.011 (2) | −0.0018 (19) |
N4 | 0.054 (3) | 0.030 (2) | 0.056 (3) | 0.004 (2) | 0.016 (2) | −0.0033 (18) |
N5 | 0.049 (3) | 0.029 (2) | 0.059 (3) | −0.002 (2) | 0.016 (2) | 0.0037 (18) |
N6 | 0.054 (3) | 0.052 (3) | 0.045 (2) | 0.011 (2) | 0.014 (2) | 0.008 (2) |
O1 | 0.067 (3) | 0.044 (2) | 0.065 (2) | −0.018 (2) | 0.0334 (19) | −0.0042 (16) |
O2 | 0.046 (2) | 0.048 (2) | 0.062 (2) | −0.0053 (18) | 0.0235 (17) | −0.0117 (17) |
O3 | 0.053 (2) | 0.0233 (17) | 0.059 (2) | 0.0032 (17) | 0.0179 (16) | 0.0007 (14) |
O4 | 0.060 (3) | 0.035 (2) | 0.064 (2) | −0.0027 (18) | 0.0282 (19) | 0.0036 (15) |
O5 | 0.083 (3) | 0.036 (2) | 0.078 (3) | 0.003 (2) | 0.045 (2) | −0.0057 (17) |
O6 | 0.066 (3) | 0.0262 (19) | 0.073 (2) | 0.0035 (18) | 0.0261 (19) | 0.0013 (16) |
O1WA | 0.060 (5) | 0.028 (4) | 0.102 (5) | 0.010 (3) | 0.070 (4) | 0.013 (3) |
O2W | 0.065 (3) | 0.046 (2) | 0.070 (2) | −0.012 (2) | 0.0209 (19) | −0.0078 (17) |
Co1—O2i | 2.033 (4) | C16—H16A | 0.9700 |
Co1—O2 | 2.033 (4) | C16—H16B | 0.9700 |
Co1—N1 | 2.146 (4) | C17—N3 | 1.443 (7) |
Co1—N1i | 2.146 (4) | C17—H17A | 0.9700 |
Co1—O2W | 2.178 (4) | C17—H17B | 0.9700 |
Co1—O2Wi | 2.178 (4) | C18—N1 | 1.312 (6) |
Co2—O6ii | 2.003 (3) | C18—N2 | 1.344 (6) |
Co2—O3 | 2.008 (3) | C18—H18 | 0.9300 |
Co2—N4iii | 2.010 (4) | C19—N2 | 1.345 (7) |
Co2—N5 | 2.015 (4) | C19—C20 | 1.345 (8) |
C1—C2 | 1.388 (6) | C19—H19 | 0.9300 |
C1—C6 | 1.389 (6) | C20—N1 | 1.378 (7) |
C1—C7 | 1.488 (7) | C20—H20 | 0.9300 |
C2—C3 | 1.386 (7) | C21—N4 | 1.328 (7) |
C2—H2 | 0.9300 | C21—N3 | 1.334 (6) |
C3—C4 | 1.390 (6) | C21—H21 | 0.9300 |
C3—C8 | 1.484 (6) | C22—C23 | 1.329 (8) |
C4—C5 | 1.384 (6) | C22—N4 | 1.382 (6) |
C4—H4 | 0.9300 | C22—H22 | 0.9300 |
C5—C6 | 1.387 (7) | C23—N3 | 1.373 (7) |
C5—C9 | 1.504 (6) | C23—H23 | 0.9300 |
C6—H6 | 0.9300 | C24—N5 | 1.323 (6) |
C7—O1 | 1.251 (6) | C24—N6 | 1.341 (6) |
C7—O2 | 1.256 (6) | C24—H24 | 0.9300 |
C8—O4 | 1.225 (6) | C25—N6 | 1.333 (8) |
C8—O3 | 1.288 (5) | C25—C26 | 1.327 (8) |
C9—O5 | 1.222 (6) | C25—H25 | 0.9300 |
C9—O6 | 1.276 (6) | C26—N5 | 1.369 (6) |
C10—C11 | 1.376 (7) | C26—H26 | 0.9300 |
C10—C15 | 1.378 (7) | C27—N6 | 1.468 (6) |
C10—C16 | 1.493 (8) | C27—C28 | 1.498 (8) |
C11—C12 | 1.381 (8) | C27—H27A | 0.9700 |
C11—H11 | 0.9300 | C27—H27B | 0.9700 |
C12—C13 | 1.363 (8) | C28—C30 | 1.373 (7) |
C12—H12 | 0.9300 | C28—C29 | 1.385 (7) |
C13—C14 | 1.358 (7) | C29—C30iv | 1.376 (8) |
C13—C17 | 1.506 (7) | C29—H29 | 0.9300 |
C14—C15 | 1.361 (8) | C30—C29iv | 1.376 (8) |
C14—H14 | 0.9300 | C30—H30 | 0.9300 |
C15—H15 | 0.9300 | N4—Co2v | 2.010 (4) |
C16—N2 | 1.454 (7) | O6—Co2vi | 2.003 (3) |
O2i—Co1—O2 | 180.0 (2) | H16A—C16—H16B | 107.9 |
O2i—Co1—N1 | 86.91 (15) | N3—C17—C13 | 113.4 (5) |
O2—Co1—N1 | 93.09 (15) | N3—C17—H17A | 108.9 |
O2i—Co1—N1i | 93.09 (15) | C13—C17—H17A | 108.9 |
O2—Co1—N1i | 86.91 (15) | N3—C17—H17B | 108.9 |
N1—Co1—N1i | 180.0 (2) | C13—C17—H17B | 108.9 |
O2i—Co1—O2W | 88.31 (15) | H17A—C17—H17B | 107.7 |
O2—Co1—O2W | 91.69 (15) | N1—C18—N2 | 112.6 (5) |
N1—Co1—O2W | 92.53 (15) | N1—C18—H18 | 123.7 |
N1i—Co1—O2W | 87.47 (15) | N2—C18—H18 | 123.7 |
O2i—Co1—O2Wi | 91.69 (15) | N2—C19—C20 | 107.6 (5) |
O2—Co1—O2Wi | 88.31 (15) | N2—C19—H19 | 126.2 |
N1—Co1—O2Wi | 87.47 (15) | C20—C19—H19 | 126.2 |
N1i—Co1—O2Wi | 92.53 (15) | C19—C20—N1 | 109.4 (5) |
O2W—Co1—O2Wi | 180.00 (8) | C19—C20—H20 | 125.3 |
O6ii—Co2—O3 | 95.21 (14) | N1—C20—H20 | 125.3 |
O6ii—Co2—N4iii | 102.55 (17) | N4—C21—N3 | 112.0 (5) |
O3—Co2—N4iii | 114.31 (15) | N4—C21—H21 | 124.0 |
O6ii—Co2—N5 | 115.36 (16) | N3—C21—H21 | 124.0 |
O3—Co2—N5 | 110.01 (15) | C23—C22—N4 | 110.1 (5) |
N4iii—Co2—N5 | 117.21 (17) | C23—C22—H22 | 124.9 |
C2—C1—C6 | 118.5 (4) | N4—C22—H22 | 124.9 |
C2—C1—C7 | 120.2 (4) | C22—C23—N3 | 107.0 (5) |
C6—C1—C7 | 121.3 (4) | C22—C23—H23 | 126.5 |
C3—C2—C1 | 121.8 (4) | N3—C23—H23 | 126.5 |
C3—C2—H2 | 119.1 | N5—C24—N6 | 111.3 (5) |
C1—C2—H2 | 119.1 | N5—C24—H24 | 124.4 |
C2—C3—C4 | 118.6 (4) | N6—C24—H24 | 124.4 |
C2—C3—C8 | 121.2 (4) | N6—C25—C26 | 107.6 (5) |
C4—C3—C8 | 120.2 (4) | N6—C25—H25 | 126.2 |
C5—C4—C3 | 120.6 (4) | C26—C25—H25 | 126.2 |
C5—C4—H4 | 119.7 | C25—C26—N5 | 109.9 (5) |
C3—C4—H4 | 119.7 | C25—C26—H26 | 125.0 |
C6—C5—C4 | 119.7 (4) | N5—C26—H26 | 125.0 |
C6—C5—C9 | 120.1 (4) | N6—C27—C28 | 116.1 (5) |
C4—C5—C9 | 120.0 (4) | N6—C27—H27A | 108.3 |
C5—C6—C1 | 120.7 (4) | C28—C27—H27A | 108.3 |
C5—C6—H6 | 119.6 | N6—C27—H27B | 108.3 |
C1—C6—H6 | 119.6 | C28—C27—H27B | 108.3 |
O1—C7—O2 | 125.3 (5) | H27A—C27—H27B | 107.4 |
O1—C7—C1 | 118.3 (4) | C30—C28—C29 | 119.1 (5) |
O2—C7—C1 | 116.5 (5) | C30—C28—C27 | 120.2 (5) |
O4—C8—O3 | 121.3 (4) | C29—C28—C27 | 120.6 (5) |
O4—C8—C3 | 120.9 (4) | C30iv—C29—C28 | 119.4 (5) |
O3—C8—C3 | 117.9 (4) | C30iv—C29—H29 | 120.3 |
O5—C9—O6 | 123.9 (5) | C28—C29—H29 | 120.3 |
O5—C9—C5 | 119.1 (4) | C28—C30—C29iv | 121.5 (5) |
O6—C9—C5 | 117.0 (5) | C28—C30—H30 | 119.3 |
C11—C10—C15 | 117.3 (5) | C29iv—C30—H30 | 119.3 |
C11—C10—C16 | 121.4 (5) | C18—N1—C20 | 104.3 (5) |
C15—C10—C16 | 121.3 (5) | C18—N1—Co1 | 126.8 (4) |
C10—C11—C12 | 120.7 (5) | C20—N1—Co1 | 128.9 (4) |
C10—C11—H11 | 119.7 | C19—N2—C18 | 106.1 (5) |
C12—C11—H11 | 119.7 | C19—N2—C16 | 126.3 (5) |
C13—C12—C11 | 121.0 (5) | C18—N2—C16 | 126.9 (5) |
C13—C12—H12 | 119.5 | C21—N3—C23 | 106.5 (5) |
C11—C12—H12 | 119.5 | C21—N3—C17 | 127.1 (5) |
C14—C13—C12 | 118.2 (5) | C23—N3—C17 | 126.3 (5) |
C14—C13—C17 | 120.3 (5) | C21—N4—C22 | 104.3 (5) |
C12—C13—C17 | 121.4 (5) | C21—N4—Co2v | 125.8 (4) |
C13—C14—C15 | 121.4 (6) | C22—N4—Co2v | 129.7 (4) |
C13—C14—H14 | 119.3 | C24—N5—C26 | 104.2 (4) |
C15—C14—H14 | 119.3 | C24—N5—Co2 | 127.4 (4) |
C14—C15—C10 | 121.3 (5) | C26—N5—Co2 | 128.1 (3) |
C14—C15—H15 | 119.3 | C25—N6—C24 | 106.9 (4) |
C10—C15—H15 | 119.3 | C25—N6—C27 | 126.6 (5) |
N2—C16—C10 | 111.8 (5) | C24—N6—C27 | 126.2 (5) |
N2—C16—H16A | 109.3 | C7—O2—Co1 | 129.3 (3) |
C10—C16—H16A | 109.3 | C8—O3—Co2 | 103.6 (3) |
N2—C16—H16B | 109.3 | C9—O6—Co2vi | 107.9 (3) |
C10—C16—H16B | 109.3 | ||
C6—C1—C2—C3 | 0.9 (7) | O2W—Co1—N1—C18 | 20.7 (5) |
C7—C1—C2—C3 | −179.5 (4) | O2Wi—Co1—N1—C18 | −159.3 (5) |
C1—C2—C3—C4 | −0.2 (7) | O2i—Co1—N1—C20 | 108.3 (5) |
C1—C2—C3—C8 | −176.9 (4) | O2—Co1—N1—C20 | −71.7 (5) |
C2—C3—C4—C5 | −1.7 (7) | N1i—Co1—N1—C20 | −110 (31) |
C8—C3—C4—C5 | 175.0 (4) | O2W—Co1—N1—C20 | −163.6 (5) |
C3—C4—C5—C6 | 2.8 (7) | O2Wi—Co1—N1—C20 | 16.4 (5) |
C3—C4—C5—C9 | −173.5 (4) | C20—C19—N2—C18 | 0.7 (7) |
C4—C5—C6—C1 | −2.0 (7) | C20—C19—N2—C16 | 171.4 (5) |
C9—C5—C6—C1 | 174.2 (4) | N1—C18—N2—C19 | −0.7 (7) |
C2—C1—C6—C5 | 0.2 (7) | N1—C18—N2—C16 | −171.4 (5) |
C7—C1—C6—C5 | −179.4 (4) | C10—C16—N2—C19 | −71.6 (8) |
C2—C1—C7—O1 | −171.0 (4) | C10—C16—N2—C18 | 97.3 (6) |
C6—C1—C7—O1 | 8.7 (7) | N4—C21—N3—C23 | 0.0 (6) |
C2—C1—C7—O2 | 9.7 (7) | N4—C21—N3—C17 | −177.8 (5) |
C6—C1—C7—O2 | −170.7 (4) | C22—C23—N3—C21 | −0.6 (6) |
C2—C3—C8—O4 | −174.0 (5) | C22—C23—N3—C17 | 177.2 (5) |
C4—C3—C8—O4 | 9.4 (7) | C13—C17—N3—C21 | 100.3 (6) |
C2—C3—C8—O3 | 7.2 (7) | C13—C17—N3—C23 | −77.1 (6) |
C4—C3—C8—O3 | −169.5 (4) | N3—C21—N4—C22 | 0.6 (5) |
C6—C5—C9—O5 | −168.3 (5) | N3—C21—N4—Co2v | −175.2 (3) |
C4—C5—C9—O5 | 8.0 (7) | C23—C22—N4—C21 | −1.0 (6) |
C6—C5—C9—O6 | 11.1 (7) | C23—C22—N4—Co2v | 174.6 (3) |
C4—C5—C9—O6 | −172.7 (4) | N6—C24—N5—C26 | −1.4 (7) |
C15—C10—C11—C12 | 0.1 (10) | N6—C24—N5—Co2 | 173.8 (3) |
C16—C10—C11—C12 | −177.8 (6) | C25—C26—N5—C24 | 2.1 (8) |
C10—C11—C12—C13 | −0.1 (11) | C25—C26—N5—Co2 | −173.0 (5) |
C11—C12—C13—C14 | −0.2 (10) | O6ii—Co2—N5—C24 | −50.1 (5) |
C11—C12—C13—C17 | 176.6 (6) | O3—Co2—N5—C24 | −156.3 (4) |
C12—C13—C14—C15 | 0.5 (10) | N4iii—Co2—N5—C24 | 70.9 (5) |
C17—C13—C14—C15 | −176.3 (6) | O6ii—Co2—N5—C26 | 124.0 (6) |
C13—C14—C15—C10 | −0.5 (11) | O3—Co2—N5—C26 | 17.7 (6) |
C11—C10—C15—C14 | 0.1 (10) | N4iii—Co2—N5—C26 | −115.1 (6) |
C16—C10—C15—C14 | 178.1 (6) | C26—C25—N6—C24 | 1.1 (8) |
C11—C10—C16—N2 | 136.2 (6) | C26—C25—N6—C27 | 175.2 (6) |
C15—C10—C16—N2 | −41.7 (8) | N5—C24—N6—C25 | 0.2 (7) |
C14—C13—C17—N3 | −79.9 (7) | N5—C24—N6—C27 | −173.9 (5) |
C12—C13—C17—N3 | 103.4 (6) | C28—C27—N6—C25 | 109.2 (7) |
N2—C19—C20—N1 | −0.4 (7) | C28—C27—N6—C24 | −77.8 (7) |
N4—C22—C23—N3 | 1.0 (6) | O1—C7—O2—Co1 | 33.4 (7) |
N6—C25—C26—N5 | −2.0 (9) | C1—C7—O2—Co1 | −147.3 (3) |
N6—C27—C28—C30 | 118.6 (6) | O2i—Co1—O2—C7 | −117 (37) |
N6—C27—C28—C29 | −64.5 (7) | N1—Co1—O2—C7 | −110.4 (4) |
C30—C28—C29—C30iv | 0.5 (9) | N1i—Co1—O2—C7 | 69.6 (4) |
C27—C28—C29—C30iv | −176.5 (5) | O2W—Co1—O2—C7 | −17.8 (4) |
C29—C28—C30—C29iv | −0.5 (9) | O2Wi—Co1—O2—C7 | 162.2 (4) |
C27—C28—C30—C29iv | 176.5 (5) | O4—C8—O3—Co2 | −1.4 (6) |
N2—C18—N1—C20 | 0.4 (6) | C3—C8—O3—Co2 | 177.4 (3) |
N2—C18—N1—Co1 | 177.0 (3) | O6ii—Co2—O3—C8 | 171.7 (3) |
C19—C20—N1—C18 | 0.0 (6) | N4iii—Co2—O3—C8 | 65.4 (3) |
C19—C20—N1—Co1 | −176.4 (4) | N5—Co2—O3—C8 | −68.9 (3) |
O2i—Co1—N1—C18 | −67.5 (5) | O5—C9—O6—Co2vi | −8.8 (7) |
O2—Co1—N1—C18 | 112.5 (5) | C5—C9—O6—Co2vi | 171.9 (3) |
N1i—Co1—N1—C18 | 75 (31) |
Symmetry codes: (i) −x, −y, −z; (ii) x, y−1, z; (iii) x−1, −y−1/2, z+1/2; (iv) −x−1, −y−1, −z+1; (v) x+1, −y−1/2, z−1/2; (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 |
Mr | 1305.89 | 1359.94 |
Crystal system, space group | Monoclinic, Cc | Monoclinic, P21/c |
Temperature (K) | 293 | 293 |
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) |
V (Å3) | 5811 (3) | 2951.3 (14) |
Z | 4 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 0.92 | 0.91 |
Crystal size (mm) | 0.33 × 0.26 × 0.22 | 0.31 × 0.28 × 0.21 |
Data collection | ||
Diffractometer | Bruker APEX CCD area-detector diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.74, 0.82 | 0.77, 0.83 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27961, 11621, 10356 | 24924, 6651, 3309 |
Rint | 0.028 | 0.114 |
(sin θ/λ)max (Å−1) | 0.649 | 0.649 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.091, 1.04 | 0.074, 0.165, 1.13 |
No. of reflections | 11621 | 6651 |
No. of parameters | 800 | 413 |
No. of restraints | 2 | 0 |
H-atom treatment | H-atom parameters constrained | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.08, −0.44 | 0.71, −0.69 |
Absolute structure | Flack (1983), with how many Friedel pairs? | ? |
Absolute structure parameter | 0.246 (10) | ? |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
Co1—O2 | 1.929 (2) | Co2—N12iii | 2.014 (3) |
Co1—O6i | 1.976 (2) | Co2—N8iv | 2.019 (3) |
Co1—N5 | 2.007 (3) | Co3—O4 | 1.968 (2) |
Co1—N9 | 2.012 (3) | Co3—O7 | 1.986 (2) |
Co2—O9 | 1.945 (2) | Co3—N4v | 2.036 (3) |
Co2—O11ii | 1.975 (2) | Co3—N1 | 2.067 (3) |
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+3, z+1/2. |
Co1—O2i | 2.033 (4) | Co1—O2Wi | 2.178 (4) |
Co1—O2 | 2.033 (4) | Co2—O6ii | 2.003 (3) |
Co1—N1 | 2.146 (4) | Co2—O3 | 2.008 (3) |
Co1—N1i | 2.146 (4) | Co2—N4iii | 2.010 (4) |
Co1—O2W | 2.178 (4) | Co2—N5 | 2.015 (4) |
Symmetry codes: (i) −x, −y, −z; (ii) x, y−1, z; (iii) x−1, −y−1/2, z+1/2. |
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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).