Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805010123/bv6016sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805010123/bv6016Isup2.hkl |
CCDC reference: 271829
Data collection: XSCANS (Bruker, 1999); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XSHELL (Bruker, 1999); software used to prepare material for publication: XSCANS.
[Co(C6H8N3O2)2]·Cl0.4·NO30.6·2.5H2O | F(000) = 1877 |
Mr = 463.65 | Dx = 1.65 Mg m−3 Dm = 1.65 Mg m−3 Dm measured by floatation |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2y | Cell parameters from 62 reflections |
a = 29.398 (3) Å | θ = 12.4–17.1° |
b = 9.839 (1) Å | µ = 1.04 mm−1 |
c = 13.590 (1) Å | T = 293 K |
β = 108.189 (6)° | Plate, red |
V = 3734.4 (6) Å3 | 0.5 × 0.4 × 0.2 mm |
Z = 8 |
Siemens P4 diffractometer | 4589 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.019 |
Graphite monochromator | θmax = 27.5°, θmin = 2.5° |
θ–2θ scans | h = −38→1 |
Absorption correction: ψ scan (XSCANS; Bruker, 1999) | k = −12→1 |
Tmin = 0.769, Tmax = 0.813 | l = −16→17 |
5319 measured reflections | 3 standard reflections every 75 reflections |
5037 independent reflections | intensity decay: none |
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)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.103 | w = 1/[σ2(Fo2) + (0.0612P)2 + 2.4496P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
5037 reflections | Δρmax = 0.55 e Å−3 |
547 parameters | Δρmin = −0.45 e Å−3 |
7 restraints | Absolute structure: Flack (1983), 218 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.008 (15) |
Experimental. There is some disorder around the Cl- whch appears to be due to a small fraction of NO3- substitution at that site. Atom positions for the NO3- were found on difference maps. A model was employed that included a NO3- with positional restraints 0.20 occupancy for the atoms. The Cl- was refined with 0.80 occupancy. This composition is in agreement with elemental analysis of the crystals (Cl calc'd 3.06, found 2.94). Only one H on the isolated O12 atom was found from difference maps. No H atoms were included on O atoms with partial occupancy. |
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 | 0.711976 (17) | 0.61787 (5) | 0.42285 (3) | 0.02588 (12) | |
O1 | 0.70636 (11) | 0.4692 (3) | 0.3322 (2) | 0.0345 (6) | |
O2 | 0.69968 (12) | 0.4213 (4) | 0.1696 (3) | 0.0451 (8) | |
O3 | 0.74803 (11) | 0.5107 (3) | 0.5348 (2) | 0.0348 (6) | |
O4 | 0.77401 (13) | 0.5020 (4) | 0.7051 (2) | 0.0499 (9) | |
N1 | 0.67869 (11) | 0.7193 (4) | 0.3001 (2) | 0.0304 (7) | |
H1A | 0.6469 | 0.7164 | 0.2888 | 0.036* | |
H1B | 0.6882 | 0.8067 | 0.3067 | 0.036* | |
N2 | 0.77079 (11) | 0.6736 (4) | 0.3981 (3) | 0.0307 (7) | |
N3 | 0.84586 (13) | 0.7117 (6) | 0.4247 (3) | 0.0516 (11) | |
H3NA | 0.8760 | 0.7208 | 0.4563 | 0.062* | |
N4 | 0.71800 (13) | 0.7584 (4) | 0.5238 (2) | 0.0315 (7) | |
H4A | 0.7435 | 0.8111 | 0.5279 | 0.038* | |
H4B | 0.6916 | 0.8109 | 0.5066 | 0.038* | |
N5 | 0.65384 (12) | 0.5626 (4) | 0.4509 (2) | 0.0302 (7) | |
N6 | 0.58368 (15) | 0.4746 (5) | 0.4320 (3) | 0.0487 (11) | |
H6NA | 0.5567 | 0.4344 | 0.4043 | 0.058* | |
C1 | 0.69890 (15) | 0.5037 (5) | 0.2374 (3) | 0.0348 (9) | |
C2 | 0.69114 (15) | 0.6532 (5) | 0.2128 (3) | 0.0328 (9) | |
H2A | 0.6651 | 0.6658 | 0.1477 | 0.039* | |
C3 | 0.73693 (15) | 0.7129 (5) | 0.2041 (3) | 0.0380 (10) | |
H3A | 0.7461 | 0.6645 | 0.1510 | 0.046* | |
H3B | 0.7315 | 0.8072 | 0.1829 | 0.046* | |
C4 | 0.77703 (15) | 0.7054 (5) | 0.3040 (3) | 0.0358 (9) | |
C5 | 0.82407 (16) | 0.7290 (7) | 0.3216 (4) | 0.0500 (13) | |
H5A | 0.8388 | 0.7526 | 0.2725 | 0.060* | |
C6 | 0.81315 (15) | 0.6787 (6) | 0.4685 (4) | 0.0416 (10) | |
H6A | 0.8192 | 0.6616 | 0.5387 | 0.050* | |
C7 | 0.75119 (15) | 0.5580 (5) | 0.6246 (3) | 0.0344 (9) | |
C8 | 0.72410 (16) | 0.6890 (5) | 0.6241 (3) | 0.0352 (9) | |
H8A | 0.7421 | 0.7473 | 0.6815 | 0.042* | |
C9 | 0.67484 (17) | 0.6579 (6) | 0.6330 (3) | 0.0452 (12) | |
H9A | 0.6787 | 0.6031 | 0.6944 | 0.054* | |
H9B | 0.6597 | 0.7425 | 0.6420 | 0.054* | |
C10 | 0.64248 (15) | 0.5843 (5) | 0.5409 (3) | 0.0355 (10) | |
C11 | 0.59905 (18) | 0.5299 (6) | 0.5292 (4) | 0.0483 (12) | |
H11A | 0.5827 | 0.5298 | 0.5778 | 0.058* | |
C12 | 0.61751 (16) | 0.4940 (5) | 0.3880 (4) | 0.0392 (10) | |
H12A | 0.6160 | 0.4636 | 0.3223 | 0.047* | |
Co2 | 0.901024 (17) | 0.74604 (6) | 0.09180 (4) | 0.02714 (13) | |
O5 | 0.84316 (11) | 0.6628 (4) | 0.0966 (2) | 0.0419 (8) | |
O6 | 0.78278 (13) | 0.5398 (5) | 0.0000 (3) | 0.0622 (12) | |
O7 | 0.92940 (10) | 0.7485 (4) | 0.2396 (2) | 0.0370 (7) | |
O8 | 0.98300 (12) | 0.8615 (5) | 0.3632 (2) | 0.0504 (9) | |
N7 | 0.87244 (11) | 0.7382 (4) | −0.0555 (2) | 0.0297 (7) | |
H7B | 0.8559 | 0.8148 | −0.0790 | 0.036* | |
H7A | 0.8951 | 0.7286 | −0.0867 | 0.036* | |
N8 | 0.92751 (13) | 0.5694 (4) | 0.0848 (3) | 0.0343 (8) | |
N9 | 0.97512 (17) | 0.3957 (5) | 0.1226 (4) | 0.0563 (12) | |
H9NA | 0.9985 | 0.3440 | 0.1557 | 0.068* | |
N10 | 0.95953 (11) | 0.8342 (4) | 0.0917 (2) | 0.0285 (7) | |
H10A | 0.9818 | 0.7720 | 0.0903 | 0.034* | |
H10B | 0.9543 | 0.8884 | 0.0359 | 0.034* | |
N11 | 0.87395 (12) | 0.9225 (4) | 0.1000 (3) | 0.0333 (8) | |
N12 | 0.82189 (15) | 1.0819 (6) | 0.0954 (3) | 0.0510 (12) | |
H12N | 0.7948 | 1.1219 | 0.0857 | 0.061* | |
C13 | 0.81904 (14) | 0.6066 (6) | 0.0109 (3) | 0.0406 (10) | |
C14 | 0.84015 (14) | 0.6197 (6) | −0.0770 (3) | 0.0353 (9) | |
H14A | 0.8144 | 0.6336 | −0.1423 | 0.042* | |
C15 | 0.86779 (19) | 0.4922 (6) | −0.0840 (4) | 0.0446 (11) | |
H15A | 0.8469 | 0.4142 | −0.0904 | 0.053* | |
H15B | 0.8773 | 0.4967 | −0.1461 | 0.053* | |
C16 | 0.91115 (16) | 0.4719 (5) | 0.0069 (3) | 0.0382 (10) | |
C17 | 0.94119 (19) | 0.3658 (6) | 0.0306 (5) | 0.0537 (13) | |
H17A | 0.9393 | 0.2869 | −0.0082 | 0.064* | |
C18 | 0.96590 (17) | 0.5173 (5) | 0.1521 (4) | 0.0436 (11) | |
H18A | 0.9841 | 0.5606 | 0.2124 | 0.052* | |
C19 | 0.96276 (14) | 0.8373 (5) | 0.2712 (3) | 0.0366 (10) | |
C20 | 0.97570 (14) | 0.9147 (5) | 0.1874 (3) | 0.0344 (9) | |
H20A | 1.0105 | 0.9266 | 0.2076 | 0.041* | |
C21 | 0.95180 (17) | 1.0510 (6) | 0.1696 (4) | 0.0423 (10) | |
H21A | 0.9615 | 1.0992 | 0.1171 | 0.051* | |
H21B | 0.9626 | 1.1034 | 0.2332 | 0.051* | |
C22 | 0.89784 (16) | 1.0419 (5) | 0.1357 (3) | 0.0373 (9) | |
C23 | 0.86527 (19) | 1.1409 (6) | 0.1323 (4) | 0.0503 (13) | |
H23A | 0.8716 | 1.2314 | 0.1517 | 0.060* | |
C24 | 0.82774 (15) | 0.9528 (6) | 0.0764 (3) | 0.0406 (11) | |
H24A | 0.8029 | 0.8913 | 0.0500 | 0.049* | |
Cl | 0.57549 (8) | 0.5311 (2) | 0.11574 (14) | 0.0567 (4) | 0.80 |
N13 | 0.92413 (16) | 0.6745 (6) | 0.7476 (3) | 0.0520 (11) | |
O9 | 0.94434 (13) | 0.6911 (5) | 0.8406 (3) | 0.0627 (11) | |
O10 | 0.9476 (2) | 0.6770 (10) | 0.6887 (4) | 0.116 (3) | |
O11 | 0.88122 (17) | 0.6532 (10) | 0.7147 (4) | 0.108 (3) | |
O12 | 0.94412 (13) | 0.6848 (6) | 0.4772 (3) | 0.0627 (11) | |
H121 | 0.9640 | 0.7469 | 0.4362 | 0.080* | |
O13 | 0.8766 (2) | 0.3922 (7) | 0.5743 (5) | 0.108 (2) | |
H131 | 0.8909 | 0.4716 | 0.5827 | 0.080* | |
H132 | 0.8687 | 0.4398 | 0.6183 | 0.080* | |
O14A | 0.7760 (11) | 0.322 (3) | 0.1360 (14) | 0.070 (4) | 0.50 |
O14B | 0.7748 (11) | 0.327 (3) | 0.1044 (14) | 0.079 (5) | 0.50 |
O15A | 0.8667 (4) | 0.4404 (8) | 0.2481 (7) | 0.068 (2) | 0.50 |
O15B | 0.9324 (5) | 0.4112 (14) | 0.4295 (11) | 0.110 (4) | 0.50 |
O16 | 0.5592 (3) | 0.7594 (12) | 0.2348 (6) | 0.063 (2) | 0.50 |
O17 | 0.5472 (5) | 0.748 (2) | 0.2682 (12) | 0.042 (4)* | 0.25 |
O18 | 1.0081 (9) | 1.247 (3) | 0.3970 (18) | 0.100 (7)* | 0.25 |
N30 | 0.5645 (6) | 0.5953 (19) | 0.1272 (12) | 0.030 (4)* | 0.20 |
O31 | 0.5277 (6) | 0.586 (2) | 0.0509 (12) | 0.057 (5)* | 0.20 |
O32 | 0.5690 (7) | 0.690 (2) | 0.1909 (13) | 0.054 (5)* | 0.20 |
O33 | 0.5963 (10) | 0.505 (3) | 0.143 (3) | 0.117 (15)* | 0.20 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0292 (2) | 0.0250 (2) | 0.0221 (2) | 0.0013 (2) | 0.00596 (18) | −0.0011 (2) |
O1 | 0.0438 (16) | 0.0291 (15) | 0.0290 (13) | 0.0022 (13) | 0.0089 (12) | −0.0045 (13) |
O2 | 0.0471 (17) | 0.051 (2) | 0.0377 (16) | −0.0100 (17) | 0.0142 (14) | −0.0205 (16) |
O3 | 0.0430 (16) | 0.0308 (15) | 0.0274 (13) | 0.0057 (14) | 0.0062 (12) | 0.0020 (12) |
O4 | 0.060 (2) | 0.049 (2) | 0.0280 (15) | −0.0030 (18) | −0.0047 (14) | 0.0082 (15) |
N1 | 0.0288 (15) | 0.0331 (19) | 0.0291 (15) | 0.0047 (15) | 0.0086 (12) | 0.0015 (14) |
N2 | 0.0271 (15) | 0.0331 (18) | 0.0310 (16) | 0.0005 (15) | 0.0075 (13) | −0.0032 (15) |
N3 | 0.0293 (17) | 0.068 (3) | 0.055 (2) | −0.002 (2) | 0.0089 (16) | −0.001 (2) |
N4 | 0.0393 (17) | 0.0261 (17) | 0.0295 (15) | −0.0016 (16) | 0.0114 (13) | −0.0004 (15) |
N5 | 0.0310 (16) | 0.0324 (17) | 0.0267 (15) | −0.0040 (15) | 0.0083 (13) | −0.0021 (15) |
N6 | 0.039 (2) | 0.059 (3) | 0.045 (2) | −0.017 (2) | 0.0094 (17) | 0.000 (2) |
C1 | 0.033 (2) | 0.042 (3) | 0.0273 (19) | −0.0043 (19) | 0.0060 (16) | −0.0083 (19) |
C2 | 0.0354 (19) | 0.041 (2) | 0.0207 (16) | −0.0011 (18) | 0.0069 (15) | −0.0033 (16) |
C3 | 0.041 (2) | 0.046 (3) | 0.0296 (18) | −0.003 (2) | 0.0146 (16) | −0.0030 (19) |
C4 | 0.038 (2) | 0.039 (2) | 0.0342 (19) | −0.0021 (19) | 0.0162 (16) | −0.0037 (18) |
C5 | 0.039 (2) | 0.071 (4) | 0.044 (2) | −0.003 (3) | 0.0179 (18) | −0.002 (3) |
C6 | 0.033 (2) | 0.048 (3) | 0.039 (2) | −0.001 (2) | 0.0045 (17) | −0.002 (2) |
C7 | 0.035 (2) | 0.037 (2) | 0.0280 (19) | −0.0117 (19) | 0.0048 (16) | −0.0017 (18) |
C8 | 0.043 (2) | 0.038 (2) | 0.0231 (17) | −0.008 (2) | 0.0073 (16) | −0.0025 (18) |
C9 | 0.048 (2) | 0.057 (3) | 0.034 (2) | −0.012 (2) | 0.0183 (18) | −0.013 (2) |
C10 | 0.037 (2) | 0.040 (3) | 0.0307 (19) | −0.0038 (18) | 0.0112 (16) | −0.0002 (17) |
C11 | 0.045 (3) | 0.061 (3) | 0.041 (2) | −0.012 (3) | 0.016 (2) | 0.001 (2) |
C12 | 0.038 (2) | 0.042 (2) | 0.034 (2) | −0.010 (2) | 0.0072 (17) | −0.001 (2) |
Co2 | 0.0230 (2) | 0.0359 (3) | 0.0214 (2) | −0.0044 (2) | 0.00535 (17) | 0.0013 (2) |
O5 | 0.0336 (14) | 0.060 (2) | 0.0327 (15) | −0.0138 (15) | 0.0109 (12) | 0.0019 (15) |
O6 | 0.0419 (18) | 0.086 (3) | 0.056 (2) | −0.033 (2) | 0.0105 (16) | 0.001 (2) |
O7 | 0.0338 (13) | 0.0490 (18) | 0.0249 (12) | −0.0115 (16) | 0.0046 (10) | 0.0005 (15) |
O8 | 0.0499 (18) | 0.067 (3) | 0.0274 (14) | −0.0155 (19) | 0.0015 (13) | −0.0059 (17) |
N7 | 0.0275 (14) | 0.0354 (18) | 0.0259 (14) | 0.0013 (16) | 0.0080 (12) | 0.0024 (16) |
N8 | 0.0321 (17) | 0.0331 (18) | 0.0337 (17) | −0.0043 (15) | 0.0045 (14) | 0.0048 (16) |
N9 | 0.052 (2) | 0.041 (2) | 0.063 (3) | 0.009 (2) | −0.002 (2) | 0.009 (2) |
N10 | 0.0246 (15) | 0.0316 (18) | 0.0291 (16) | 0.0005 (14) | 0.0081 (13) | 0.0027 (14) |
N11 | 0.0265 (15) | 0.047 (2) | 0.0249 (15) | 0.0038 (16) | 0.0057 (13) | −0.0039 (16) |
N12 | 0.041 (2) | 0.068 (3) | 0.045 (2) | 0.021 (2) | 0.0145 (17) | 0.001 (2) |
C13 | 0.0295 (19) | 0.052 (3) | 0.037 (2) | −0.008 (2) | 0.0048 (15) | 0.001 (2) |
C14 | 0.0292 (18) | 0.043 (2) | 0.0289 (17) | −0.008 (2) | 0.0018 (14) | 0.002 (2) |
C15 | 0.050 (3) | 0.045 (3) | 0.034 (2) | −0.010 (2) | 0.008 (2) | −0.003 (2) |
C16 | 0.042 (2) | 0.034 (2) | 0.036 (2) | −0.0081 (19) | 0.0084 (18) | 0.0037 (19) |
C17 | 0.057 (3) | 0.037 (3) | 0.061 (3) | 0.002 (2) | 0.008 (2) | 0.002 (3) |
C18 | 0.042 (2) | 0.040 (3) | 0.040 (2) | −0.003 (2) | 0.0001 (19) | 0.007 (2) |
C19 | 0.0306 (19) | 0.045 (3) | 0.0284 (19) | 0.000 (2) | 0.0015 (15) | −0.0006 (19) |
C20 | 0.0241 (17) | 0.041 (2) | 0.034 (2) | −0.0040 (18) | 0.0035 (15) | −0.0020 (19) |
C21 | 0.042 (2) | 0.039 (2) | 0.045 (2) | −0.005 (2) | 0.011 (2) | −0.006 (2) |
C22 | 0.038 (2) | 0.038 (2) | 0.037 (2) | 0.004 (2) | 0.0133 (18) | −0.001 (2) |
C23 | 0.052 (3) | 0.046 (3) | 0.055 (3) | 0.014 (2) | 0.019 (2) | −0.002 (2) |
C24 | 0.030 (2) | 0.064 (3) | 0.0287 (19) | 0.010 (2) | 0.0107 (16) | 0.000 (2) |
Cl | 0.0572 (11) | 0.0659 (13) | 0.0496 (9) | −0.0038 (10) | 0.0205 (8) | −0.0019 (9) |
N13 | 0.052 (2) | 0.057 (3) | 0.051 (2) | 0.000 (2) | 0.021 (2) | 0.012 (2) |
O9 | 0.0408 (17) | 0.080 (3) | 0.070 (2) | −0.013 (2) | 0.0210 (17) | −0.023 (2) |
O10 | 0.097 (3) | 0.201 (9) | 0.068 (3) | 0.044 (5) | 0.049 (3) | 0.049 (4) |
O11 | 0.062 (3) | 0.187 (8) | 0.063 (3) | −0.028 (4) | 0.002 (2) | 0.008 (4) |
O12 | 0.0428 (18) | 0.091 (3) | 0.051 (2) | −0.002 (2) | 0.0101 (15) | 0.004 (2) |
O13 | 0.091 (4) | 0.069 (4) | 0.155 (6) | −0.030 (3) | 0.028 (4) | −0.015 (4) |
O14A | 0.102 (8) | 0.075 (7) | 0.056 (10) | 0.052 (6) | 0.057 (9) | 0.043 (9) |
O14B | 0.092 (9) | 0.108 (11) | 0.066 (12) | 0.055 (8) | 0.065 (11) | 0.044 (11) |
O15A | 0.117 (7) | 0.033 (4) | 0.067 (5) | 0.004 (5) | 0.046 (5) | 0.015 (4) |
O15B | 0.114 (9) | 0.071 (7) | 0.109 (9) | −0.004 (7) | −0.017 (7) | 0.004 (7) |
O16 | 0.051 (4) | 0.083 (7) | 0.042 (4) | 0.011 (5) | −0.005 (4) | −0.007 (5) |
Co1—O3 | 1.882 (3) | O8—C19 | 1.229 (5) |
Co1—O1 | 1.886 (3) | N7—C14 | 1.474 (6) |
Co1—N4 | 1.916 (3) | N7—H7B | 0.9000 |
Co1—N1 | 1.928 (3) | N7—H7A | 0.9000 |
Co1—N2 | 1.941 (3) | N8—C18 | 1.315 (6) |
Co1—N5 | 1.942 (3) | N8—C16 | 1.398 (6) |
O1—C1 | 1.282 (5) | N9—C18 | 1.316 (8) |
O2—C1 | 1.233 (6) | N9—C17 | 1.367 (7) |
O3—C7 | 1.282 (5) | N9—H9NA | 0.8600 |
O4—C7 | 1.222 (6) | N10—C20 | 1.469 (5) |
N1—C2 | 1.495 (5) | N10—H10A | 0.9000 |
N1—H1A | 0.9000 | N10—H10B | 0.9000 |
N1—H1B | 0.9000 | N11—C24 | 1.329 (5) |
N2—C6 | 1.313 (5) | N11—C22 | 1.377 (6) |
N2—C4 | 1.383 (5) | N12—C24 | 1.317 (8) |
N3—C6 | 1.319 (6) | N12—C23 | 1.348 (7) |
N3—C5 | 1.358 (6) | N12—H12N | 0.8600 |
N3—H3NA | 0.8600 | C13—C14 | 1.513 (6) |
N4—C8 | 1.484 (5) | C14—C15 | 1.513 (8) |
N4—H4A | 0.9000 | C14—H14A | 0.9800 |
N4—H4B | 0.9000 | C15—C16 | 1.485 (6) |
N5—C12 | 1.325 (6) | C15—H15A | 0.9700 |
N5—C10 | 1.381 (5) | C15—H15B | 0.9700 |
N6—C12 | 1.324 (6) | C16—C17 | 1.340 (7) |
N6—C11 | 1.368 (7) | C17—H17A | 0.9300 |
N6—H6NA | 0.8600 | C18—H18A | 0.9300 |
C1—C2 | 1.510 (7) | C19—C20 | 1.514 (6) |
C2—C3 | 1.507 (6) | C20—C21 | 1.499 (7) |
C2—H2A | 0.9800 | C20—H20A | 0.9800 |
C3—C4 | 1.496 (6) | C21—C22 | 1.510 (6) |
C3—H3A | 0.9700 | C21—H21A | 0.9700 |
C3—H3B | 0.9700 | C21—H21B | 0.9700 |
C4—C5 | 1.348 (6) | C22—C23 | 1.357 (7) |
C5—H5A | 0.9300 | C23—H23A | 0.9300 |
C6—H6A | 0.9300 | C24—H24A | 0.9300 |
C7—C8 | 1.514 (7) | Cl—O33 | 0.66 (2) |
C8—C9 | 1.522 (6) | Cl—N30 | 0.747 (17) |
C8—H8A | 0.9800 | Cl—O31 | 1.507 (16) |
C9—C10 | 1.501 (6) | Cl—O32 | 1.910 (18) |
C9—H9A | 0.9700 | N13—O10 | 1.210 (6) |
C9—H9B | 0.9700 | N13—O11 | 1.218 (6) |
C10—C11 | 1.348 (7) | N13—O9 | 1.228 (6) |
C11—H11A | 0.9300 | O12—H121 | 1.1094 |
C12—H12A | 0.9300 | O13—H131 | 0.8785 |
Co2—O5 | 1.907 (3) | O13—H132 | 0.8463 |
Co2—N7 | 1.915 (3) | O16—O17 | 0.665 (14) |
Co2—N8 | 1.919 (4) | O16—O32 | 1.006 (19) |
Co2—O7 | 1.920 (3) | O17—O32 | 1.50 (2) |
Co2—N10 | 1.926 (3) | N30—O31 | 1.247 (16) |
Co2—N11 | 1.928 (4) | N30—O32 | 1.251 (17) |
O5—C13 | 1.284 (5) | N30—O33 | 1.259 (18) |
O6—C13 | 1.222 (6) | O31—O31i | 1.78 (3) |
O7—C19 | 1.283 (6) | ||
O3—Co1—O1 | 90.36 (13) | N10—Co2—N11 | 88.83 (16) |
O3—Co1—N4 | 85.55 (14) | C13—O5—Co2 | 113.6 (3) |
O1—Co1—N4 | 175.32 (15) | C19—O7—Co2 | 113.3 (3) |
O3—Co1—N1 | 174.23 (14) | C14—N7—Co2 | 106.5 (2) |
O1—Co1—N1 | 85.33 (14) | C14—N7—H7B | 110.4 |
N4—Co1—N1 | 98.90 (15) | Co2—N7—H7B | 110.4 |
O3—Co1—N2 | 89.48 (15) | C14—N7—H7A | 110.4 |
O1—Co1—N2 | 90.41 (14) | Co2—N7—H7A | 110.4 |
N4—Co1—N2 | 91.82 (15) | H7B—N7—H7A | 108.6 |
N1—Co1—N2 | 86.73 (14) | C18—N8—C16 | 106.1 (4) |
O3—Co1—N5 | 89.56 (15) | C18—N8—Co2 | 126.3 (3) |
O1—Co1—N5 | 90.46 (15) | C16—N8—Co2 | 127.6 (3) |
N4—Co1—N5 | 87.24 (15) | C18—N9—C17 | 108.3 (5) |
N1—Co1—N5 | 94.30 (14) | C18—N9—H9NA | 125.9 |
N2—Co1—N5 | 178.71 (14) | C17—N9—H9NA | 125.9 |
C1—O1—Co1 | 113.8 (3) | C20—N10—Co2 | 106.5 (2) |
C7—O3—Co1 | 114.9 (3) | C20—N10—H10A | 110.4 |
C2—N1—Co1 | 106.1 (3) | Co2—N10—H10A | 110.4 |
C2—N1—H1A | 110.5 | C20—N10—H10B | 110.4 |
Co1—N1—H1A | 110.5 | Co2—N10—H10B | 110.4 |
C2—N1—H1B | 110.5 | H10A—N10—H10B | 108.6 |
Co1—N1—H1B | 110.5 | C24—N11—C22 | 105.3 (4) |
H1A—N1—H1B | 108.7 | C24—N11—Co2 | 126.7 (4) |
C6—N2—C4 | 107.2 (4) | C22—N11—Co2 | 127.9 (3) |
C6—N2—Co1 | 125.4 (3) | C24—N12—C23 | 108.8 (4) |
C4—N2—Co1 | 127.3 (3) | C24—N12—H12N | 125.6 |
C6—N3—C5 | 108.7 (4) | C23—N12—H12N | 125.6 |
C6—N3—H3NA | 125.6 | O6—C13—O5 | 123.7 (4) |
C5—N3—H3NA | 125.6 | O6—C13—C14 | 120.5 (4) |
C8—N4—Co1 | 106.5 (3) | O5—C13—C14 | 115.6 (4) |
C8—N4—H4A | 110.4 | N7—C14—C13 | 108.0 (4) |
Co1—N4—H4A | 110.4 | N7—C14—C15 | 110.1 (3) |
C8—N4—H4B | 110.4 | C13—C14—C15 | 109.8 (4) |
Co1—N4—H4B | 110.4 | N7—C14—H14A | 109.7 |
H4A—N4—H4B | 108.6 | C13—C14—H14A | 109.7 |
C12—N5—C10 | 106.3 (4) | C15—C14—H14A | 109.7 |
C12—N5—Co1 | 126.7 (3) | C16—C15—C14 | 113.4 (4) |
C10—N5—Co1 | 127.0 (3) | C16—C15—H15A | 108.9 |
C12—N6—C11 | 108.1 (4) | C14—C15—H15A | 108.9 |
C12—N6—H6NA | 126.0 | C16—C15—H15B | 108.9 |
C11—N6—H6NA | 126.0 | C14—C15—H15B | 108.9 |
O2—C1—O1 | 122.7 (5) | H15A—C15—H15B | 107.7 |
O2—C1—C2 | 120.7 (4) | C17—C16—N8 | 107.9 (4) |
O1—C1—C2 | 116.6 (4) | C17—C16—C15 | 129.4 (5) |
N1—C2—C3 | 109.8 (3) | N8—C16—C15 | 122.7 (4) |
N1—C2—C1 | 107.7 (3) | C16—C17—N9 | 106.9 (5) |
C3—C2—C1 | 108.7 (4) | C16—C17—H17A | 126.6 |
N1—C2—H2A | 110.2 | N9—C17—H17A | 126.6 |
C3—C2—H2A | 110.2 | N8—C18—N9 | 110.9 (5) |
C1—C2—H2A | 110.2 | N8—C18—H18A | 124.5 |
C4—C3—C2 | 112.3 (3) | N9—C18—H18A | 124.5 |
C4—C3—H3A | 109.1 | O8—C19—O7 | 123.3 (4) |
C2—C3—H3A | 109.1 | O8—C19—C20 | 120.8 (4) |
C4—C3—H3B | 109.1 | O7—C19—C20 | 115.9 (3) |
C2—C3—H3B | 109.1 | N10—C20—C21 | 109.5 (4) |
H3A—C3—H3B | 107.9 | N10—C20—C19 | 107.9 (4) |
C5—C4—N2 | 107.5 (4) | C21—C20—C19 | 110.9 (4) |
C5—C4—C3 | 128.8 (4) | N10—C20—H20A | 109.5 |
N2—C4—C3 | 123.8 (4) | C21—C20—H20A | 109.5 |
C4—C5—N3 | 106.7 (4) | C19—C20—H20A | 109.5 |
C4—C5—H5A | 126.6 | C20—C21—C22 | 113.0 (4) |
N3—C5—H5A | 126.6 | C20—C21—H21A | 109.0 |
N2—C6—N3 | 109.9 (4) | C22—C21—H21A | 109.0 |
N2—C6—H6A | 125.0 | C20—C21—H21B | 109.0 |
N3—C6—H6A | 125.0 | C22—C21—H21B | 109.0 |
O4—C7—O3 | 123.0 (5) | H21A—C21—H21B | 107.8 |
O4—C7—C8 | 122.0 (4) | C23—C22—N11 | 108.9 (4) |
O3—C7—C8 | 115.0 (4) | C23—C22—C21 | 129.1 (5) |
N4—C8—C7 | 108.0 (3) | N11—C22—C21 | 122.0 (4) |
N4—C8—C9 | 108.7 (4) | N12—C23—C22 | 106.2 (5) |
C7—C8—C9 | 109.9 (4) | N12—C23—H23A | 126.9 |
N4—C8—H8A | 110.1 | C22—C23—H23A | 126.9 |
C7—C8—H8A | 110.1 | N12—C24—N11 | 110.8 (5) |
C9—C8—H8A | 110.1 | N12—C24—H24A | 124.6 |
C10—C9—C8 | 113.7 (4) | N11—C24—H24A | 124.6 |
C10—C9—H9A | 108.8 | O33—Cl—N30 | 126 (3) |
C8—C9—H9A | 108.8 | O33—Cl—O31 | 178 (3) |
C10—C9—H9B | 108.8 | N30—Cl—O31 | 55.5 (12) |
C8—C9—H9B | 108.8 | O33—Cl—O32 | 104 (2) |
H9A—C9—H9B | 107.7 | N30—Cl—O32 | 22.3 (12) |
C11—C10—N5 | 108.4 (4) | O31—Cl—O32 | 77.7 (7) |
C11—C10—C9 | 128.3 (4) | O10—N13—O11 | 120.0 (6) |
N5—C10—C9 | 123.2 (4) | O10—N13—O9 | 119.0 (5) |
C10—C11—N6 | 106.7 (4) | O11—N13—O9 | 120.9 (4) |
C10—C11—H11A | 126.7 | H131—O13—H132 | 69.0 |
N6—C11—H11A | 126.7 | O17—O16—O32 | 127 (3) |
N6—C12—N5 | 110.5 (4) | O16—O17—O32 | 32.4 (19) |
N6—C12—H12A | 124.8 | Cl—N30—O31 | 94.9 (16) |
N5—C12—H12A | 124.8 | Cl—N30—O32 | 144.7 (18) |
O5—Co2—N7 | 85.02 (13) | O31—N30—O32 | 120.3 (14) |
O5—Co2—N8 | 89.58 (16) | Cl—N30—O33 | 25.1 (15) |
N7—Co2—N8 | 87.94 (16) | O31—N30—O33 | 119.9 (15) |
O5—Co2—O7 | 94.04 (12) | O32—N30—O33 | 119.7 (14) |
N7—Co2—O7 | 178.38 (19) | N30—O31—Cl | 29.6 (8) |
N8—Co2—O7 | 90.73 (16) | N30—O31—O31i | 173.7 (17) |
O5—Co2—N10 | 177.77 (15) | Cl—O31—O31i | 156.3 (10) |
N7—Co2—N10 | 96.78 (14) | O16—O32—N30 | 158 (2) |
N8—Co2—N10 | 91.80 (16) | O16—O32—O17 | 20.8 (11) |
O7—Co2—N10 | 84.19 (13) | N30—O32—O17 | 142.2 (19) |
O5—Co2—N11 | 89.78 (16) | O16—O32—Cl | 165.4 (18) |
N7—Co2—N11 | 92.44 (16) | N30—O32—Cl | 13.1 (7) |
N8—Co2—N11 | 179.22 (16) | O17—O32—Cl | 145.0 (15) |
O7—Co2—N11 | 88.88 (16) | Cl—O33—N30 | 28.5 (16) |
Symmetry code: (i) −x+1, y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O17 | 0.90 | 2.87 | 3.764 (15) | 171 |
N1—H1B···O4ii | 0.90 | 2.25 | 3.121 (6) | 162 |
N3—H3NA···O12 | 0.86 | 1.97 | 2.764 (5) | 154 |
N4—H4A···O3ii | 0.90 | 2.19 | 2.880 (5) | 134 |
N4—H4A···O1ii | 0.90 | 2.54 | 3.219 (5) | 133 |
N4—H4B···O13ii | 0.90 | 2.12 | 2.988 (6) | 162 |
N6—H6NA···O8iii | 0.86 | 2.18 | 3.024 (5) | 166 |
N7—H7B···O2iv | 0.90 | 2.01 | 2.845 (5) | 154 |
N7—H7A···O9v | 0.90 | 2.02 | 2.922 (5) | 175 |
N9—H9NA···O16vi | 0.86 | 1.96 | 2.807 (9) | 169 |
N9—H9NA···O17vi | 0.86 | 1.98 | 2.811 (17) | 162 |
N10—H10A···O9vii | 0.90 | 2.23 | 3.032 (5) | 149 |
N10—H10B···Cliv | 0.90 | 2.42 | 3.309 (4) | 169 |
N12—H12N···O14Bviii | 0.86 | 2.14 | 2.80 (3) | 134 |
N12—H12N···O14Aviii | 0.86 | 2.21 | 2.86 (3) | 132 |
N12—H12N···O6iv | 0.86 | 2.36 | 2.971 (6) | 129 |
Symmetry codes: (ii) −x+3/2, y+1/2, −z+1; (iii) x−1/2, y−1/2, z; (iv) −x+3/2, y+1/2, −z; (v) x, y, z−1; (vi) x+1/2, y−1/2, z; (vii) −x+2, y, −z+1; (viii) x, y+1, z. |