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Two conformational polymorphs of (
N,
N-dibutyldithiocarbamato-κ
2S,
S′)[tris(3,5-diphenylpyrazol-1-yl-κ
N2)hydroborato]cobalt(II), [Co(C
45H
34BN
6)(C
9H
18NS
2)] or [Tp
Ph2Co(S
2CNBu
2)],
1, are accessible by recrystallization from dichloromethane–methanol to give orthorhombic polymorph
1a, while slow evaporation from acetonitrile produces triclinic polymorph
1b. The two polymorphs have been characterized by IR spectroscopy and single-crystal X-ray crystallography at 150 K. Polymorphs
1a and
1b crystallize in the orthorhombic space group
Pbca and the triclinic space group
P, respectively. The polymorphs have a
trans (
1a) and
cis (
1b) orientation of the butyl groups with respect to the S
2CN plane of the dithiocarbamate ligand, which results in an intermediate five-coordinate geometry for
1a and a square-pyramidal geometry for
1b. Hirshfeld surface analysis reveals minor differences between the two polymorphs, with
1a exhibiting stronger C—H
S interactions and
1b favouring C—H
π interactions.
Supporting information
CCDC references: 2021203; 2021202
Data collection: CrysAlis PRO (Rigaku OD, 2018) for (1a); CrysAlis PRO (Rigaku OD, 2020) for (1b). Cell refinement: CrysAlis PRO (Rigaku OD, 2018) for (1a); CrysAlis PRO (Rigaku OD, 2020) for (1b). Data reduction: CrysAlis PRO (Rigaku OD, 2018) for (1a); CrysAlis PRO (Rigaku OD, 2020) for (1b). For both structures, program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
(
N,
N-Dibutyldithiocarbamato-
κ2S,
S')[tris(3,5-diphenylpyrazol-1-yl-
κN2)hydroborato]cobalt(II) (1a)
top
Crystal data top
[Co(C45H34BN6)(C9H18NS2)] | Dx = 1.304 Mg m−3 |
Mr = 932.88 | Cu Kα radiation, λ = 1.54184 Å |
Orthorhombic, Pbca | Cell parameters from 24286 reflections |
a = 26.26089 (17) Å | θ = 3.0–69.1° |
b = 12.39989 (8) Å | µ = 4.00 mm−1 |
c = 29.17764 (19) Å | T = 150 K |
V = 9501.18 (11) Å3 | Block, red |
Z = 8 | 0.27 × 0.19 × 0.14 mm |
F(000) = 3912 | |
Data collection top
Rigaku SuperNova (Single source at offset/far, HyPix3000) diffractometer | 8785 independent reflections |
Radiation source: micro-focus sealed X-ray tube, SuperNova (Cu) X-ray Source | 7986 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.039 |
ω scans | θmax = 69.3°, θmin = 3.0° |
Absorption correction: analytical (CrysAlis PRO; Rigaku OD, 2018) | h = −31→31 |
Tmin = 0.964, Tmax = 0.977 | k = −10→15 |
41879 measured reflections | l = −35→35 |
Refinement top
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.036 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.092 | w = 1/[σ2(Fo2) + (0.0437P)2 + 5.2719P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
8785 reflections | Δρmax = 0.29 e Å−3 |
662 parameters | Δρmin = −0.44 e Å−3 |
69 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.64309 (2) | 0.76052 (2) | 0.39413 (2) | 0.02174 (8) | |
S1 | 0.68195 (2) | 0.73821 (4) | 0.31858 (2) | 0.02905 (11) | |
S2 | 0.63564 (2) | 0.92976 (4) | 0.35827 (2) | 0.03668 (13) | |
N1 | 0.60184 (5) | 0.61779 (11) | 0.40274 (5) | 0.0212 (3) | |
N2 | 0.60858 (5) | 0.56806 (11) | 0.44419 (5) | 0.0207 (3) | |
N3 | 0.70286 (5) | 0.71869 (11) | 0.43702 (5) | 0.0228 (3) | |
N4 | 0.69193 (5) | 0.64899 (11) | 0.47210 (5) | 0.0214 (3) | |
N5 | 0.60036 (5) | 0.80324 (11) | 0.45545 (5) | 0.0217 (3) | |
N6 | 0.60826 (5) | 0.73572 (11) | 0.49199 (5) | 0.0211 (3) | |
N7 | 0.68947 (8) | 0.93428 (14) | 0.28050 (6) | 0.0461 (5) | |
C1 | 0.56820 (6) | 0.55842 (13) | 0.37924 (6) | 0.0221 (3) | |
C2 | 0.55324 (6) | 0.46921 (14) | 0.40526 (6) | 0.0238 (3) | |
H2 | 0.529870 | 0.414388 | 0.396618 | 0.029* | |
C3 | 0.57954 (6) | 0.47733 (13) | 0.44619 (6) | 0.0217 (3) | |
C4 | 0.55160 (6) | 0.58729 (14) | 0.33256 (6) | 0.0251 (4) | |
C5 | 0.55046 (7) | 0.69411 (16) | 0.31781 (6) | 0.0317 (4) | |
H5 | 0.559919 | 0.750185 | 0.338303 | 0.038* | |
C6 | 0.53565 (9) | 0.71921 (18) | 0.27355 (7) | 0.0436 (5) | |
H6 | 0.535526 | 0.792225 | 0.263692 | 0.052* | |
C7 | 0.52109 (10) | 0.6387 (2) | 0.24371 (7) | 0.0498 (6) | |
H7 | 0.510981 | 0.656210 | 0.213341 | 0.060* | |
C8 | 0.52124 (9) | 0.5324 (2) | 0.25810 (7) | 0.0470 (5) | |
H8 | 0.510936 | 0.476875 | 0.237658 | 0.056* | |
C9 | 0.53637 (8) | 0.50672 (16) | 0.30215 (6) | 0.0348 (4) | |
H9 | 0.536382 | 0.433550 | 0.311804 | 0.042* | |
C10 | 0.57929 (6) | 0.40335 (13) | 0.48585 (6) | 0.0227 (3) | |
C11 | 0.53308 (7) | 0.37342 (14) | 0.50580 (6) | 0.0277 (4) | |
H11 | 0.502124 | 0.402016 | 0.494138 | 0.033* | |
C12 | 0.53194 (8) | 0.30251 (16) | 0.54240 (7) | 0.0347 (4) | |
H12 | 0.500327 | 0.283315 | 0.555974 | 0.042* | |
C13 | 0.57688 (9) | 0.25950 (16) | 0.55926 (7) | 0.0374 (5) | |
H13 | 0.576127 | 0.210883 | 0.584411 | 0.045* | |
C14 | 0.62298 (8) | 0.28757 (15) | 0.53934 (7) | 0.0345 (4) | |
H14 | 0.653768 | 0.257646 | 0.550765 | 0.041* | |
C15 | 0.62433 (7) | 0.35899 (14) | 0.50287 (6) | 0.0283 (4) | |
H15 | 0.656029 | 0.377859 | 0.489380 | 0.034* | |
C16 | 0.75401 (7) | 0.71947 (14) | 0.43240 (6) | 0.0250 (4) | |
C17 | 0.77562 (7) | 0.64829 (15) | 0.46373 (6) | 0.0281 (4) | |
H17 | 0.810789 | 0.632431 | 0.467267 | 0.034* | |
C18 | 0.73575 (6) | 0.60522 (14) | 0.48870 (6) | 0.0243 (4) | |
C19 | 0.78030 (7) | 0.79204 (15) | 0.40033 (6) | 0.0276 (4) | |
C20 | 0.76383 (8) | 0.89789 (16) | 0.39419 (6) | 0.0328 (4) | |
H20 | 0.735009 | 0.923312 | 0.410629 | 0.039* | |
C21 | 0.78913 (9) | 0.96655 (18) | 0.36430 (7) | 0.0412 (5) | |
H21 | 0.777488 | 1.038422 | 0.360113 | 0.049* | |
C22 | 0.83140 (8) | 0.92983 (19) | 0.34060 (7) | 0.0430 (5) | |
H22 | 0.848544 | 0.976222 | 0.319785 | 0.052* | |
C23 | 0.84864 (8) | 0.8257 (2) | 0.34722 (7) | 0.0427 (5) | |
H23 | 0.878034 | 0.801401 | 0.331313 | 0.051* | |
C24 | 0.82344 (7) | 0.75633 (17) | 0.37688 (7) | 0.0344 (4) | |
H24 | 0.835511 | 0.684825 | 0.381194 | 0.041* | |
C25 | 0.73854 (6) | 0.52674 (14) | 0.52653 (6) | 0.0262 (4) | |
C26 | 0.76977 (7) | 0.43597 (15) | 0.52125 (7) | 0.0326 (4) | |
H26 | 0.788709 | 0.426825 | 0.493780 | 0.039* | |
C27 | 0.77330 (8) | 0.35958 (17) | 0.55562 (8) | 0.0421 (5) | |
H27 | 0.794513 | 0.298239 | 0.551586 | 0.050* | |
C28 | 0.74606 (9) | 0.37212 (18) | 0.59589 (8) | 0.0454 (5) | |
H28 | 0.748163 | 0.319093 | 0.619312 | 0.055* | |
C29 | 0.71569 (8) | 0.46244 (19) | 0.60184 (7) | 0.0409 (5) | |
H29 | 0.697115 | 0.471405 | 0.629516 | 0.049* | |
C30 | 0.71222 (7) | 0.53979 (16) | 0.56768 (6) | 0.0310 (4) | |
H30 | 0.691804 | 0.602082 | 0.572334 | 0.037* | |
C31 | 0.57721 (6) | 0.89154 (13) | 0.47201 (6) | 0.0215 (3) | |
C32 | 0.57145 (7) | 0.88336 (14) | 0.51939 (6) | 0.0257 (4) | |
H32 | 0.557031 | 0.935384 | 0.539458 | 0.031* | |
C33 | 0.59118 (6) | 0.78338 (14) | 0.53106 (6) | 0.0230 (3) | |
C34 | 0.55808 (6) | 0.97752 (14) | 0.44154 (5) | 0.0218 (3) | |
C35 | 0.57101 (7) | 1.08472 (14) | 0.44947 (6) | 0.0266 (4) | |
H35 | 0.592253 | 1.102731 | 0.474692 | 0.032* | |
C36 | 0.55308 (8) | 1.16545 (15) | 0.42080 (6) | 0.0322 (4) | |
H36 | 0.562917 | 1.238183 | 0.425923 | 0.039* | |
C37 | 0.52090 (8) | 1.14043 (15) | 0.38472 (6) | 0.0315 (4) | |
H37 | 0.508506 | 1.195932 | 0.365241 | 0.038* | |
C38 | 0.50683 (7) | 1.03413 (15) | 0.37710 (6) | 0.0305 (4) | |
H38 | 0.484293 | 1.016832 | 0.352711 | 0.037* | |
C39 | 0.52567 (7) | 0.95320 (14) | 0.40510 (6) | 0.0257 (4) | |
H39 | 0.516421 | 0.880345 | 0.399421 | 0.031* | |
C40 | 0.59361 (7) | 0.73552 (15) | 0.57748 (6) | 0.0275 (4) | |
C41 | 0.57756 (7) | 0.63078 (17) | 0.58711 (7) | 0.0352 (4) | |
H41 | 0.566254 | 0.584974 | 0.563077 | 0.042* | |
C42 | 0.57819 (8) | 0.5937 (2) | 0.63208 (8) | 0.0494 (6) | |
H42 | 0.567349 | 0.522282 | 0.638657 | 0.059* | |
C43 | 0.59444 (9) | 0.6599 (2) | 0.66732 (7) | 0.0563 (7) | |
H43 | 0.594537 | 0.633958 | 0.697966 | 0.068* | |
C44 | 0.61042 (10) | 0.7629 (2) | 0.65801 (8) | 0.0525 (6) | |
H44 | 0.621709 | 0.808272 | 0.682200 | 0.063* | |
C45 | 0.61009 (8) | 0.80087 (19) | 0.61333 (6) | 0.0367 (5) | |
H45 | 0.621232 | 0.872270 | 0.607102 | 0.044* | |
C46 | 0.67157 (7) | 0.87436 (15) | 0.31451 (6) | 0.0310 (4) | |
B1 | 0.63569 (7) | 0.62678 (15) | 0.48418 (6) | 0.0210 (4) | |
H1 | 0.6333 (7) | 0.5768 (15) | 0.5136 (6) | 0.020 (5)* | |
C47 | 0.67345 (16) | 1.0496 (2) | 0.27578 (10) | 0.0410 (8) | 0.768 (6) |
H47A | 0.704108 | 1.094620 | 0.270832 | 0.049* | 0.768 (6) |
H47B | 0.657408 | 1.073233 | 0.304795 | 0.049* | 0.768 (6) |
C48 | 0.63671 (15) | 1.0687 (3) | 0.23702 (13) | 0.0488 (10) | 0.768 (6) |
H48B | 0.607039 | 1.020287 | 0.240817 | 0.059* | 0.768 (6) |
H48A | 0.653548 | 1.049913 | 0.207734 | 0.059* | 0.768 (6) |
C49 | 0.61771 (16) | 1.1867 (3) | 0.23447 (13) | 0.0575 (10) | 0.768 (6) |
H49B | 0.592739 | 1.199988 | 0.259255 | 0.069* | 0.768 (6) |
H49A | 0.646751 | 1.236556 | 0.238898 | 0.069* | 0.768 (6) |
C50 | 0.59327 (18) | 1.2079 (4) | 0.18882 (14) | 0.0664 (11) | 0.768 (6) |
H50A | 0.617884 | 1.193636 | 0.164322 | 0.100* | 0.768 (6) |
H50B | 0.582313 | 1.283413 | 0.187293 | 0.100* | 0.768 (6) |
H50C | 0.563665 | 1.160655 | 0.185070 | 0.100* | 0.768 (6) |
C51 | 0.7141 (3) | 0.8829 (8) | 0.2397 (3) | 0.0491 (13) | 0.710 (13) |
H51B | 0.689361 | 0.882985 | 0.214109 | 0.059* | 0.710 (13) |
H51A | 0.721696 | 0.806779 | 0.247243 | 0.059* | 0.710 (13) |
C52 | 0.7623 (2) | 0.9357 (6) | 0.2235 (2) | 0.0561 (14) | 0.710 (13) |
H52A | 0.787489 | 0.936159 | 0.248780 | 0.067* | 0.710 (13) |
H52B | 0.755114 | 1.011529 | 0.215057 | 0.067* | 0.710 (13) |
C53 | 0.7851 (2) | 0.8766 (5) | 0.18192 (16) | 0.0586 (13) | 0.710 (13) |
H53A | 0.795535 | 0.802980 | 0.191090 | 0.070* | 0.710 (13) |
H53B | 0.758995 | 0.870144 | 0.157624 | 0.070* | 0.710 (13) |
C54 | 0.8315 (2) | 0.9377 (6) | 0.1631 (3) | 0.094 (2) | 0.710 (13) |
H54A | 0.857127 | 0.945153 | 0.187269 | 0.141* | 0.710 (13) |
H54B | 0.820867 | 1.009435 | 0.152672 | 0.141* | 0.710 (13) |
H54C | 0.846015 | 0.897604 | 0.137269 | 0.141* | 0.710 (13) |
C47A | 0.7024 (6) | 1.0537 (8) | 0.2880 (6) | 0.063 (3) | 0.232 (6) |
H47C | 0.689971 | 1.077394 | 0.318438 | 0.076* | 0.232 (6) |
H47D | 0.739703 | 1.064306 | 0.286921 | 0.076* | 0.232 (6) |
C48A | 0.6777 (5) | 1.1172 (11) | 0.2518 (5) | 0.079 (4) | 0.232 (6) |
H48C | 0.693473 | 1.098475 | 0.221988 | 0.095* | 0.232 (6) |
H48D | 0.684292 | 1.194692 | 0.257499 | 0.095* | 0.232 (6) |
C49A | 0.6225 (6) | 1.1002 (13) | 0.2485 (8) | 0.096 (5) | 0.232 (6) |
H49C | 0.605015 | 1.131104 | 0.275582 | 0.116* | 0.232 (6) |
H49D | 0.614571 | 1.022254 | 0.246850 | 0.116* | 0.232 (6) |
C50A | 0.6044 (7) | 1.1600 (14) | 0.2027 (7) | 0.098 (5) | 0.232 (6) |
H50D | 0.630884 | 1.152992 | 0.179228 | 0.147* | 0.232 (6) |
H50E | 0.598587 | 1.236580 | 0.209252 | 0.147* | 0.232 (6) |
H50F | 0.572794 | 1.127214 | 0.191669 | 0.147* | 0.232 (6) |
C51A | 0.7263 (7) | 0.891 (2) | 0.2469 (7) | 0.0491 (13) | 0.290 (13) |
H51D | 0.707793 | 0.863753 | 0.219745 | 0.059* | 0.290 (13) |
H51C | 0.745272 | 0.830439 | 0.260699 | 0.059* | 0.290 (13) |
C52A | 0.7645 (6) | 0.9800 (14) | 0.2316 (6) | 0.065 (4) | 0.290 (13) |
H52D | 0.746873 | 1.037433 | 0.214171 | 0.078* | 0.290 (13) |
H52C | 0.781551 | 1.012719 | 0.258480 | 0.078* | 0.290 (13) |
C53A | 0.8016 (6) | 0.9229 (17) | 0.2023 (8) | 0.104 (6) | 0.290 (13) |
H53C | 0.785357 | 0.899662 | 0.173335 | 0.124* | 0.290 (13) |
H53D | 0.814939 | 0.858304 | 0.218272 | 0.124* | 0.290 (13) |
C54A | 0.8439 (7) | 1.001 (2) | 0.1927 (11) | 0.154 (10) | 0.290 (13) |
H54D | 0.855077 | 1.034246 | 0.221511 | 0.230* | 0.290 (13) |
H54E | 0.831765 | 1.057123 | 0.171776 | 0.230* | 0.290 (13) |
H54F | 0.872584 | 0.962679 | 0.178674 | 0.230* | 0.290 (13) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02604 (15) | 0.01711 (14) | 0.02207 (15) | −0.00044 (11) | 0.00287 (11) | 0.00376 (11) |
S1 | 0.0360 (2) | 0.0235 (2) | 0.0276 (2) | 0.00221 (18) | 0.00739 (18) | 0.00304 (17) |
S2 | 0.0551 (3) | 0.0215 (2) | 0.0334 (2) | 0.0071 (2) | 0.0166 (2) | 0.00763 (18) |
N1 | 0.0248 (7) | 0.0187 (7) | 0.0201 (6) | 0.0008 (6) | 0.0017 (5) | 0.0027 (6) |
N2 | 0.0240 (7) | 0.0168 (7) | 0.0211 (7) | −0.0012 (5) | 0.0017 (5) | 0.0044 (5) |
N3 | 0.0253 (7) | 0.0173 (7) | 0.0259 (7) | −0.0024 (6) | 0.0029 (6) | 0.0019 (6) |
N4 | 0.0238 (7) | 0.0172 (7) | 0.0233 (7) | 0.0002 (6) | −0.0003 (6) | 0.0017 (6) |
N5 | 0.0262 (7) | 0.0177 (7) | 0.0211 (7) | 0.0020 (6) | 0.0008 (6) | 0.0029 (6) |
N6 | 0.0242 (7) | 0.0183 (7) | 0.0209 (7) | 0.0015 (6) | 0.0016 (6) | 0.0043 (5) |
N7 | 0.0713 (13) | 0.0308 (9) | 0.0361 (9) | −0.0040 (9) | 0.0190 (9) | 0.0080 (8) |
C1 | 0.0237 (8) | 0.0197 (8) | 0.0228 (8) | 0.0015 (7) | 0.0023 (7) | −0.0013 (7) |
C2 | 0.0258 (8) | 0.0203 (8) | 0.0255 (8) | −0.0023 (7) | 0.0009 (7) | −0.0003 (7) |
C3 | 0.0224 (8) | 0.0167 (8) | 0.0261 (8) | 0.0006 (6) | 0.0039 (6) | −0.0005 (7) |
C4 | 0.0256 (8) | 0.0272 (9) | 0.0226 (8) | −0.0014 (7) | 0.0017 (7) | 0.0021 (7) |
C5 | 0.0374 (10) | 0.0288 (10) | 0.0288 (9) | −0.0005 (8) | −0.0026 (8) | 0.0028 (8) |
C6 | 0.0577 (14) | 0.0387 (12) | 0.0342 (11) | −0.0012 (10) | −0.0046 (10) | 0.0126 (9) |
C7 | 0.0652 (15) | 0.0593 (15) | 0.0249 (10) | −0.0067 (12) | −0.0088 (10) | 0.0093 (10) |
C8 | 0.0635 (14) | 0.0499 (13) | 0.0275 (10) | −0.0124 (12) | −0.0052 (10) | −0.0044 (10) |
C9 | 0.0432 (11) | 0.0311 (10) | 0.0301 (9) | −0.0070 (9) | 0.0000 (8) | −0.0014 (8) |
C10 | 0.0289 (9) | 0.0142 (7) | 0.0250 (8) | −0.0022 (7) | 0.0006 (7) | −0.0003 (7) |
C11 | 0.0297 (9) | 0.0213 (8) | 0.0322 (9) | −0.0011 (7) | 0.0034 (7) | 0.0011 (7) |
C12 | 0.0405 (11) | 0.0288 (10) | 0.0347 (10) | −0.0066 (9) | 0.0074 (8) | 0.0054 (8) |
C13 | 0.0541 (13) | 0.0279 (10) | 0.0302 (10) | −0.0079 (9) | −0.0032 (9) | 0.0101 (8) |
C14 | 0.0411 (11) | 0.0235 (9) | 0.0390 (10) | −0.0008 (8) | −0.0107 (9) | 0.0059 (8) |
C15 | 0.0287 (9) | 0.0205 (9) | 0.0357 (10) | −0.0023 (7) | −0.0009 (8) | 0.0023 (8) |
C16 | 0.0252 (8) | 0.0218 (8) | 0.0281 (8) | −0.0036 (7) | 0.0017 (7) | −0.0060 (7) |
C17 | 0.0222 (8) | 0.0274 (9) | 0.0347 (9) | −0.0004 (7) | −0.0003 (7) | −0.0007 (8) |
C18 | 0.0246 (8) | 0.0203 (8) | 0.0278 (8) | 0.0008 (7) | −0.0021 (7) | −0.0029 (7) |
C19 | 0.0260 (9) | 0.0283 (9) | 0.0284 (9) | −0.0076 (8) | 0.0006 (7) | −0.0026 (7) |
C20 | 0.0376 (10) | 0.0265 (10) | 0.0344 (10) | −0.0083 (8) | 0.0053 (8) | −0.0024 (8) |
C21 | 0.0524 (13) | 0.0318 (11) | 0.0394 (11) | −0.0154 (10) | 0.0019 (10) | 0.0013 (9) |
C22 | 0.0452 (12) | 0.0502 (13) | 0.0337 (10) | −0.0254 (11) | 0.0016 (9) | 0.0034 (10) |
C23 | 0.0313 (10) | 0.0619 (15) | 0.0350 (10) | −0.0135 (10) | 0.0068 (8) | −0.0052 (10) |
C24 | 0.0276 (9) | 0.0396 (11) | 0.0358 (11) | −0.0052 (8) | 0.0019 (8) | −0.0044 (9) |
C25 | 0.0256 (9) | 0.0226 (9) | 0.0303 (9) | −0.0007 (7) | −0.0068 (7) | −0.0008 (7) |
C26 | 0.0313 (9) | 0.0291 (10) | 0.0373 (10) | 0.0071 (8) | −0.0061 (8) | −0.0033 (8) |
C27 | 0.0473 (12) | 0.0279 (10) | 0.0510 (12) | 0.0098 (9) | −0.0152 (10) | 0.0011 (9) |
C28 | 0.0553 (13) | 0.0364 (12) | 0.0446 (11) | 0.0024 (10) | −0.0135 (11) | 0.0149 (10) |
C29 | 0.0445 (12) | 0.0449 (12) | 0.0334 (10) | 0.0030 (10) | −0.0029 (9) | 0.0084 (9) |
C30 | 0.0330 (9) | 0.0297 (10) | 0.0304 (9) | 0.0037 (8) | −0.0037 (8) | −0.0010 (8) |
C31 | 0.0217 (8) | 0.0182 (8) | 0.0245 (8) | 0.0009 (6) | 0.0006 (6) | 0.0005 (7) |
C32 | 0.0295 (9) | 0.0240 (9) | 0.0236 (8) | 0.0063 (7) | 0.0021 (7) | 0.0003 (7) |
C33 | 0.0227 (8) | 0.0244 (8) | 0.0219 (8) | 0.0021 (7) | 0.0008 (7) | 0.0010 (7) |
C34 | 0.0232 (8) | 0.0206 (8) | 0.0217 (8) | 0.0027 (7) | 0.0041 (6) | 0.0016 (7) |
C35 | 0.0309 (9) | 0.0219 (9) | 0.0269 (8) | 0.0027 (7) | −0.0012 (7) | −0.0039 (7) |
C36 | 0.0457 (11) | 0.0181 (9) | 0.0327 (9) | 0.0045 (8) | 0.0016 (8) | −0.0001 (7) |
C37 | 0.0431 (11) | 0.0242 (9) | 0.0272 (9) | 0.0110 (8) | 0.0020 (8) | 0.0068 (7) |
C38 | 0.0349 (10) | 0.0321 (10) | 0.0244 (9) | 0.0024 (8) | −0.0023 (7) | 0.0007 (8) |
C39 | 0.0309 (9) | 0.0209 (8) | 0.0253 (8) | −0.0011 (7) | −0.0002 (7) | 0.0004 (7) |
C40 | 0.0235 (8) | 0.0341 (10) | 0.0250 (9) | 0.0097 (8) | 0.0039 (7) | 0.0067 (8) |
C41 | 0.0286 (9) | 0.0404 (11) | 0.0368 (10) | 0.0087 (8) | 0.0082 (8) | 0.0139 (9) |
C42 | 0.0418 (12) | 0.0562 (14) | 0.0502 (13) | 0.0178 (11) | 0.0165 (10) | 0.0299 (12) |
C43 | 0.0567 (14) | 0.0849 (19) | 0.0273 (11) | 0.0301 (14) | 0.0076 (10) | 0.0229 (12) |
C44 | 0.0552 (14) | 0.0763 (18) | 0.0260 (10) | 0.0227 (13) | −0.0027 (10) | 0.0034 (11) |
C45 | 0.0363 (10) | 0.0476 (12) | 0.0262 (9) | 0.0129 (9) | 0.0003 (8) | −0.0003 (9) |
C46 | 0.0382 (10) | 0.0264 (9) | 0.0283 (9) | −0.0015 (8) | 0.0051 (8) | 0.0054 (8) |
B1 | 0.0233 (9) | 0.0159 (9) | 0.0238 (9) | 0.0003 (7) | 0.0014 (7) | 0.0030 (7) |
C47 | 0.064 (2) | 0.0258 (15) | 0.0337 (14) | −0.0129 (15) | 0.0075 (13) | 0.0085 (11) |
C48 | 0.063 (2) | 0.0352 (19) | 0.0477 (17) | −0.0045 (15) | −0.0013 (14) | 0.0010 (14) |
C49 | 0.077 (2) | 0.0341 (17) | 0.061 (2) | −0.0054 (15) | −0.0135 (17) | 0.0030 (14) |
C50 | 0.080 (3) | 0.056 (3) | 0.062 (2) | 0.001 (2) | −0.0133 (18) | 0.0080 (18) |
C51 | 0.057 (3) | 0.0473 (19) | 0.043 (3) | −0.006 (2) | 0.015 (2) | 0.006 (2) |
C52 | 0.049 (2) | 0.070 (3) | 0.050 (2) | −0.011 (2) | 0.0049 (15) | 0.000 (2) |
C53 | 0.056 (2) | 0.071 (3) | 0.048 (2) | 0.019 (2) | 0.0135 (17) | 0.0187 (19) |
C54 | 0.072 (3) | 0.096 (4) | 0.114 (5) | 0.022 (3) | 0.045 (3) | 0.044 (4) |
C47A | 0.062 (6) | 0.033 (6) | 0.094 (8) | −0.006 (5) | 0.031 (6) | 0.020 (6) |
C48A | 0.094 (7) | 0.047 (7) | 0.097 (8) | 0.011 (5) | 0.007 (6) | 0.005 (6) |
C49A | 0.095 (7) | 0.034 (8) | 0.160 (14) | 0.014 (6) | −0.011 (8) | −0.010 (8) |
C50A | 0.085 (9) | 0.051 (9) | 0.158 (14) | 0.003 (8) | −0.016 (8) | −0.006 (9) |
C51A | 0.057 (3) | 0.0473 (19) | 0.043 (3) | −0.006 (2) | 0.015 (2) | 0.006 (2) |
C52A | 0.059 (5) | 0.073 (7) | 0.063 (8) | −0.007 (4) | 0.007 (5) | 0.045 (6) |
C53A | 0.068 (7) | 0.133 (11) | 0.109 (12) | 0.021 (7) | 0.039 (8) | 0.059 (10) |
C54A | 0.090 (9) | 0.169 (16) | 0.20 (2) | −0.004 (10) | 0.073 (12) | 0.049 (18) |
Geometric parameters (Å, º) top
Co1—S1 | 2.4449 (5) | C30—H30 | 0.9500 |
Co1—S2 | 2.3531 (5) | C31—C32 | 1.394 (2) |
Co1—N1 | 2.0901 (14) | C31—C34 | 1.476 (2) |
Co1—N3 | 2.0733 (15) | C32—H32 | 0.9500 |
Co1—N5 | 2.1774 (14) | C32—C33 | 1.386 (2) |
S1—C46 | 1.7143 (19) | C33—C40 | 1.480 (2) |
S2—C46 | 1.7298 (19) | C34—C35 | 1.391 (2) |
N1—N2 | 1.3692 (18) | C34—C39 | 1.395 (2) |
N1—C1 | 1.339 (2) | C35—H35 | 0.9500 |
N2—C3 | 1.360 (2) | C35—C36 | 1.387 (3) |
N2—B1 | 1.549 (2) | C36—H36 | 0.9500 |
N3—N4 | 1.3701 (19) | C36—C37 | 1.385 (3) |
N3—C16 | 1.350 (2) | C37—H37 | 0.9500 |
N4—C18 | 1.361 (2) | C37—C38 | 1.387 (3) |
N4—B1 | 1.543 (2) | C38—H38 | 0.9500 |
N5—N6 | 1.3713 (19) | C38—C39 | 1.386 (3) |
N5—C31 | 1.342 (2) | C39—H39 | 0.9500 |
N6—C33 | 1.360 (2) | C40—C41 | 1.394 (3) |
N6—B1 | 1.548 (2) | C40—C45 | 1.392 (3) |
N7—C46 | 1.326 (2) | C41—H41 | 0.9500 |
N7—C47 | 1.497 (4) | C41—C42 | 1.390 (3) |
N7—C51 | 1.497 (9) | C42—H42 | 0.9500 |
N7—C47A | 1.535 (11) | C42—C43 | 1.383 (4) |
N7—C51A | 1.48 (2) | C43—H43 | 0.9500 |
C1—C2 | 1.398 (2) | C43—C44 | 1.372 (4) |
C1—C4 | 1.474 (2) | C44—H44 | 0.9500 |
C2—H2 | 0.9500 | C44—C45 | 1.386 (3) |
C2—C3 | 1.383 (2) | C45—H45 | 0.9500 |
C3—C10 | 1.477 (2) | B1—H1 | 1.061 (18) |
C4—C5 | 1.393 (3) | C47—H47A | 0.9900 |
C4—C9 | 1.395 (3) | C47—H47B | 0.9900 |
C5—H5 | 0.9500 | C47—C48 | 1.505 (5) |
C5—C6 | 1.384 (3) | C48—H48B | 0.9900 |
C6—H6 | 0.9500 | C48—H48A | 0.9900 |
C6—C7 | 1.379 (3) | C48—C49 | 1.548 (5) |
C7—H7 | 0.9500 | C49—H49B | 0.9900 |
C7—C8 | 1.384 (3) | C49—H49A | 0.9900 |
C8—H8 | 0.9500 | C49—C50 | 1.502 (5) |
C8—C9 | 1.382 (3) | C50—H50A | 0.9800 |
C9—H9 | 0.9500 | C50—H50B | 0.9800 |
C10—C11 | 1.396 (2) | C50—H50C | 0.9800 |
C10—C15 | 1.396 (2) | C51—H51B | 0.9900 |
C11—H11 | 0.9500 | C51—H51A | 0.9900 |
C11—C12 | 1.384 (3) | C51—C52 | 1.502 (6) |
C12—H12 | 0.9500 | C52—H52A | 0.9900 |
C12—C13 | 1.385 (3) | C52—H52B | 0.9900 |
C13—H13 | 0.9500 | C52—C53 | 1.539 (6) |
C13—C14 | 1.387 (3) | C53—H53A | 0.9900 |
C14—H14 | 0.9500 | C53—H53B | 0.9900 |
C14—C15 | 1.385 (3) | C53—C54 | 1.535 (6) |
C15—H15 | 0.9500 | C54—H54A | 0.9800 |
C16—C17 | 1.392 (3) | C54—H54B | 0.9800 |
C16—C19 | 1.470 (2) | C54—H54C | 0.9800 |
C17—H17 | 0.9500 | C47A—H47C | 0.9900 |
C17—C18 | 1.383 (2) | C47A—H47D | 0.9900 |
C18—C25 | 1.473 (2) | C47A—C48A | 1.47 (2) |
C19—C20 | 1.393 (3) | C48A—H48C | 0.9900 |
C19—C24 | 1.396 (3) | C48A—H48D | 0.9900 |
C20—H20 | 0.9500 | C48A—C49A | 1.470 (16) |
C20—C21 | 1.388 (3) | C49A—H49C | 0.9900 |
C21—H21 | 0.9500 | C49A—H49D | 0.9900 |
C21—C22 | 1.385 (3) | C49A—C50A | 1.600 (17) |
C22—H22 | 0.9500 | C50A—H50D | 0.9800 |
C22—C23 | 1.381 (3) | C50A—H50E | 0.9800 |
C23—H23 | 0.9500 | C50A—H50F | 0.9800 |
C23—C24 | 1.388 (3) | C51A—H51D | 0.9900 |
C24—H24 | 0.9500 | C51A—H51C | 0.9900 |
C25—C26 | 1.401 (3) | C51A—C52A | 1.552 (14) |
C25—C30 | 1.395 (3) | C52A—H52D | 0.9900 |
C26—H26 | 0.9500 | C52A—H52C | 0.9900 |
C26—C27 | 1.383 (3) | C52A—C53A | 1.478 (14) |
C27—H27 | 0.9500 | C53A—H53C | 0.9900 |
C27—C28 | 1.384 (3) | C53A—H53D | 0.9900 |
C28—H28 | 0.9500 | C53A—C54A | 1.500 (15) |
C28—C29 | 1.386 (3) | C54A—H54D | 0.9800 |
C29—H29 | 0.9500 | C54A—H54E | 0.9800 |
C29—C30 | 1.386 (3) | C54A—H54F | 0.9800 |
| | | |
S2—Co1—S1 | 74.611 (17) | C34—C35—H35 | 119.8 |
N1—Co1—S1 | 103.23 (4) | C36—C35—C34 | 120.42 (16) |
N1—Co1—S2 | 139.95 (4) | C36—C35—H35 | 119.8 |
N1—Co1—N5 | 80.80 (5) | C35—C36—H36 | 119.9 |
N3—Co1—S1 | 101.53 (4) | C37—C36—C35 | 120.26 (17) |
N3—Co1—S2 | 123.67 (4) | C37—C36—H36 | 119.9 |
N3—Co1—N1 | 96.20 (5) | C36—C37—H37 | 120.1 |
N3—Co1—N5 | 87.42 (5) | C36—C37—C38 | 119.82 (17) |
N5—Co1—S1 | 169.60 (4) | C38—C37—H37 | 120.1 |
N5—Co1—S2 | 96.07 (4) | C37—C38—H38 | 120.0 |
C46—S1—Co1 | 83.38 (6) | C39—C38—C37 | 119.92 (17) |
C46—S2—Co1 | 85.92 (6) | C39—C38—H38 | 120.0 |
N2—N1—Co1 | 114.87 (10) | C34—C39—H39 | 119.6 |
C1—N1—Co1 | 138.25 (11) | C38—C39—C34 | 120.72 (17) |
C1—N1—N2 | 106.86 (13) | C38—C39—H39 | 119.6 |
N1—N2—B1 | 120.88 (13) | C41—C40—C33 | 123.03 (18) |
C3—N2—N1 | 109.74 (13) | C45—C40—C33 | 117.87 (17) |
C3—N2—B1 | 127.90 (14) | C45—C40—C41 | 118.99 (18) |
N4—N3—Co1 | 116.75 (10) | C40—C41—H41 | 120.2 |
C16—N3—Co1 | 133.73 (12) | C42—C41—C40 | 119.6 (2) |
C16—N3—N4 | 106.71 (14) | C42—C41—H41 | 120.2 |
N3—N4—B1 | 118.93 (13) | C41—C42—H42 | 119.7 |
C18—N4—N3 | 109.89 (13) | C43—C42—C41 | 120.6 (2) |
C18—N4—B1 | 131.04 (14) | C43—C42—H42 | 119.7 |
N6—N5—Co1 | 114.36 (10) | C42—C43—H43 | 120.0 |
C31—N5—Co1 | 136.69 (11) | C44—C43—C42 | 120.0 (2) |
C31—N5—N6 | 106.66 (13) | C44—C43—H43 | 120.0 |
N5—N6—B1 | 119.25 (13) | C43—C44—H44 | 120.0 |
C33—N6—N5 | 109.66 (13) | C43—C44—C45 | 120.0 (2) |
C33—N6—B1 | 131.01 (14) | C45—C44—H44 | 120.0 |
C46—N7—C47 | 120.3 (2) | C40—C45—H45 | 119.6 |
C46—N7—C51 | 120.7 (4) | C44—C45—C40 | 120.7 (2) |
C46—N7—C47A | 120.8 (6) | C44—C45—H45 | 119.6 |
C46—N7—C51A | 121.8 (9) | S1—C46—S2 | 115.25 (10) |
C51—N7—C47 | 117.0 (4) | N7—C46—S1 | 123.19 (15) |
C51A—N7—C47A | 107.3 (9) | N7—C46—S2 | 121.55 (15) |
N1—C1—C2 | 110.03 (15) | N2—B1—H1 | 108.0 (10) |
N1—C1—C4 | 122.32 (15) | N4—B1—N2 | 110.60 (13) |
C2—C1—C4 | 127.64 (16) | N4—B1—N6 | 108.86 (13) |
C1—C2—H2 | 127.1 | N4—B1—H1 | 110.2 (10) |
C3—C2—C1 | 105.72 (15) | N6—B1—N2 | 107.90 (13) |
C3—C2—H2 | 127.1 | N6—B1—H1 | 111.3 (10) |
N2—C3—C2 | 107.64 (14) | N7—C47—H47A | 108.9 |
N2—C3—C10 | 123.34 (15) | N7—C47—H47B | 108.9 |
C2—C3—C10 | 129.00 (15) | N7—C47—C48 | 113.6 (3) |
C5—C4—C1 | 121.50 (16) | H47A—C47—H47B | 107.7 |
C5—C4—C9 | 118.60 (16) | C48—C47—H47A | 108.9 |
C9—C4—C1 | 119.90 (16) | C48—C47—H47B | 108.9 |
C4—C5—H5 | 119.7 | C47—C48—H48B | 109.0 |
C6—C5—C4 | 120.52 (19) | C47—C48—H48A | 109.0 |
C6—C5—H5 | 119.7 | C47—C48—C49 | 113.0 (3) |
C5—C6—H6 | 119.9 | H48B—C48—H48A | 107.8 |
C7—C6—C5 | 120.3 (2) | C49—C48—H48B | 109.0 |
C7—C6—H6 | 119.9 | C49—C48—H48A | 109.0 |
C6—C7—H7 | 120.1 | C48—C49—H49B | 109.6 |
C6—C7—C8 | 119.82 (19) | C48—C49—H49A | 109.6 |
C8—C7—H7 | 120.1 | H49B—C49—H49A | 108.1 |
C7—C8—H8 | 119.9 | C50—C49—C48 | 110.3 (3) |
C9—C8—C7 | 120.1 (2) | C50—C49—H49B | 109.6 |
C9—C8—H8 | 119.9 | C50—C49—H49A | 109.6 |
C4—C9—H9 | 119.7 | C49—C50—H50A | 109.5 |
C8—C9—C4 | 120.59 (19) | C49—C50—H50B | 109.5 |
C8—C9—H9 | 119.7 | C49—C50—H50C | 109.5 |
C11—C10—C3 | 119.71 (15) | H50A—C50—H50B | 109.5 |
C15—C10—C3 | 121.33 (15) | H50A—C50—H50C | 109.5 |
C15—C10—C11 | 118.92 (16) | H50B—C50—H50C | 109.5 |
C10—C11—H11 | 119.7 | N7—C51—H51B | 108.4 |
C12—C11—C10 | 120.64 (17) | N7—C51—H51A | 108.4 |
C12—C11—H11 | 119.7 | N7—C51—C52 | 115.4 (6) |
C11—C12—H12 | 120.0 | H51B—C51—H51A | 107.5 |
C11—C12—C13 | 120.01 (18) | C52—C51—H51B | 108.4 |
C13—C12—H12 | 120.0 | C52—C51—H51A | 108.4 |
C12—C13—H13 | 120.1 | C51—C52—H52A | 109.3 |
C12—C13—C14 | 119.88 (18) | C51—C52—H52B | 109.3 |
C14—C13—H13 | 120.1 | C51—C52—C53 | 111.6 (5) |
C13—C14—H14 | 119.8 | H52A—C52—H52B | 108.0 |
C15—C14—C13 | 120.31 (18) | C53—C52—H52A | 109.3 |
C15—C14—H14 | 119.8 | C53—C52—H52B | 109.3 |
C10—C15—H15 | 119.9 | C52—C53—H53A | 109.5 |
C14—C15—C10 | 120.24 (17) | C52—C53—H53B | 109.5 |
C14—C15—H15 | 119.9 | H53A—C53—H53B | 108.1 |
N3—C16—C17 | 109.61 (15) | C54—C53—C52 | 110.8 (4) |
N3—C16—C19 | 122.34 (16) | C54—C53—H53A | 109.5 |
C17—C16—C19 | 127.94 (16) | C54—C53—H53B | 109.5 |
C16—C17—H17 | 126.8 | C53—C54—H54A | 109.5 |
C18—C17—C16 | 106.40 (15) | C53—C54—H54B | 109.5 |
C18—C17—H17 | 126.8 | C53—C54—H54C | 109.5 |
N4—C18—C17 | 107.37 (15) | H54A—C54—H54B | 109.5 |
N4—C18—C25 | 124.88 (15) | H54A—C54—H54C | 109.5 |
C17—C18—C25 | 127.74 (16) | H54B—C54—H54C | 109.5 |
C20—C19—C16 | 120.84 (17) | N7—C47A—H47C | 110.0 |
C20—C19—C24 | 119.20 (18) | N7—C47A—H47D | 110.0 |
C24—C19—C16 | 119.93 (18) | H47C—C47A—H47D | 108.4 |
C19—C20—H20 | 119.7 | C48A—C47A—N7 | 108.5 (12) |
C21—C20—C19 | 120.67 (19) | C48A—C47A—H47C | 110.0 |
C21—C20—H20 | 119.7 | C48A—C47A—H47D | 110.0 |
C20—C21—H21 | 120.1 | C47A—C48A—H48C | 108.8 |
C22—C21—C20 | 119.7 (2) | C47A—C48A—H48D | 108.8 |
C22—C21—H21 | 120.1 | C47A—C48A—C49A | 113.9 (13) |
C21—C22—H22 | 120.0 | H48C—C48A—H48D | 107.7 |
C23—C22—C21 | 120.01 (19) | C49A—C48A—H48C | 108.8 |
C23—C22—H22 | 120.0 | C49A—C48A—H48D | 108.8 |
C22—C23—H23 | 119.7 | C48A—C49A—H49C | 110.5 |
C22—C23—C24 | 120.7 (2) | C48A—C49A—H49D | 110.5 |
C24—C23—H23 | 119.7 | C48A—C49A—C50A | 106.2 (15) |
C19—C24—H24 | 120.1 | H49C—C49A—H49D | 108.7 |
C23—C24—C19 | 119.7 (2) | C50A—C49A—H49C | 110.5 |
C23—C24—H24 | 120.1 | C50A—C49A—H49D | 110.5 |
C26—C25—C18 | 118.51 (16) | C49A—C50A—H50D | 109.5 |
C30—C25—C18 | 122.93 (16) | C49A—C50A—H50E | 109.5 |
C30—C25—C26 | 118.55 (17) | C49A—C50A—H50F | 109.5 |
C25—C26—H26 | 119.7 | H50D—C50A—H50E | 109.5 |
C27—C26—C25 | 120.65 (19) | H50D—C50A—H50F | 109.5 |
C27—C26—H26 | 119.7 | H50E—C50A—H50F | 109.5 |
C26—C27—H27 | 119.9 | N7—C51A—H51D | 109.4 |
C26—C27—C28 | 120.26 (19) | N7—C51A—H51C | 109.4 |
C28—C27—H27 | 119.9 | N7—C51A—C52A | 111.0 (17) |
C27—C28—H28 | 120.2 | H51D—C51A—H51C | 108.0 |
C27—C28—C29 | 119.64 (19) | C52A—C51A—H51D | 109.4 |
C29—C28—H28 | 120.2 | C52A—C51A—H51C | 109.4 |
C28—C29—H29 | 119.8 | C51A—C52A—H52D | 110.8 |
C28—C29—C30 | 120.5 (2) | C51A—C52A—H52C | 110.8 |
C30—C29—H29 | 119.8 | H52D—C52A—H52C | 108.9 |
C25—C30—H30 | 119.8 | C53A—C52A—C51A | 104.6 (13) |
C29—C30—C25 | 120.40 (18) | C53A—C52A—H52D | 110.8 |
C29—C30—H30 | 119.8 | C53A—C52A—H52C | 110.8 |
N5—C31—C32 | 110.28 (15) | C52A—C53A—H53C | 110.4 |
N5—C31—C34 | 121.76 (14) | C52A—C53A—H53D | 110.4 |
C32—C31—C34 | 127.79 (15) | C52A—C53A—C54A | 106.7 (13) |
C31—C32—H32 | 127.2 | H53C—C53A—H53D | 108.6 |
C33—C32—C31 | 105.56 (15) | C54A—C53A—H53C | 110.4 |
C33—C32—H32 | 127.2 | C54A—C53A—H53D | 110.4 |
N6—C33—C32 | 107.81 (14) | C53A—C54A—H54D | 109.5 |
N6—C33—C40 | 125.34 (15) | C53A—C54A—H54E | 109.5 |
C32—C33—C40 | 126.85 (16) | C53A—C54A—H54F | 109.5 |
C35—C34—C31 | 120.44 (15) | H54D—C54A—H54E | 109.5 |
C35—C34—C39 | 118.84 (16) | H54D—C54A—H54F | 109.5 |
C39—C34—C31 | 120.70 (15) | H54E—C54A—H54F | 109.5 |
| | | |
Co1—S1—C46—S2 | −8.33 (10) | C16—N3—N4—C18 | −1.05 (18) |
Co1—S1—C46—N7 | 171.71 (19) | C16—N3—N4—B1 | −177.19 (14) |
Co1—S2—C46—S1 | 8.62 (10) | C16—C17—C18—N4 | 0.7 (2) |
Co1—S2—C46—N7 | −171.41 (18) | C16—C17—C18—C25 | −179.15 (17) |
Co1—N1—N2—C3 | 179.18 (10) | C16—C19—C20—C21 | 179.21 (17) |
Co1—N1—N2—B1 | 12.00 (17) | C16—C19—C24—C23 | −178.91 (18) |
Co1—N1—C1—C2 | −178.51 (13) | C17—C16—C19—C20 | −136.7 (2) |
Co1—N1—C1—C4 | 2.2 (3) | C17—C16—C19—C24 | 40.9 (3) |
Co1—N3—N4—C18 | 162.60 (11) | C17—C18—C25—C26 | −46.0 (3) |
Co1—N3—N4—B1 | −13.54 (18) | C17—C18—C25—C30 | 132.8 (2) |
Co1—N3—C16—C17 | −158.16 (13) | C18—N4—B1—N2 | −109.72 (19) |
Co1—N3—C16—C19 | 25.4 (3) | C18—N4—B1—N6 | 131.89 (17) |
Co1—N5—N6—C33 | 164.24 (11) | C18—C25—C26—C27 | −179.43 (17) |
Co1—N5—N6—B1 | −12.91 (17) | C18—C25—C30—C29 | 179.02 (18) |
Co1—N5—C31—C32 | −158.99 (13) | C19—C16—C17—C18 | 174.85 (17) |
Co1—N5—C31—C34 | 25.4 (3) | C19—C20—C21—C22 | −0.5 (3) |
N1—N2—C3—C2 | −0.52 (18) | C20—C19—C24—C23 | −1.3 (3) |
N1—N2—C3—C10 | 178.08 (14) | C20—C21—C22—C23 | −0.9 (3) |
N1—N2—B1—N4 | −65.04 (18) | C21—C22—C23—C24 | 1.2 (3) |
N1—N2—B1—N6 | 53.93 (18) | C22—C23—C24—C19 | −0.1 (3) |
N1—C1—C2—C3 | 0.16 (19) | C24—C19—C20—C21 | 1.6 (3) |
N1—C1—C4—C5 | −29.0 (3) | C25—C26—C27—C28 | −0.2 (3) |
N1—C1—C4—C9 | 151.27 (17) | C26—C25—C30—C29 | −2.2 (3) |
N2—N1—C1—C2 | −0.47 (18) | C26—C27—C28—C29 | −0.8 (3) |
N2—N1—C1—C4 | −179.80 (14) | C27—C28—C29—C30 | 0.4 (3) |
N2—C3—C10—C11 | 128.59 (18) | C28—C29—C30—C25 | 1.2 (3) |
N2—C3—C10—C15 | −54.0 (2) | C30—C25—C26—C27 | 1.7 (3) |
N3—N4—C18—C17 | 0.21 (19) | C31—N5—N6—C33 | −1.48 (18) |
N3—N4—C18—C25 | −179.95 (15) | C31—N5—N6—B1 | −178.63 (14) |
N3—N4—B1—N2 | 65.46 (18) | C31—C32—C33—N6 | 0.61 (19) |
N3—N4—B1—N6 | −52.92 (19) | C31—C32—C33—C40 | −179.39 (17) |
N3—C16—C17—C18 | −1.4 (2) | C31—C34—C35—C36 | 179.91 (16) |
N3—C16—C19—C20 | 39.0 (3) | C31—C34—C39—C38 | 178.60 (16) |
N3—C16—C19—C24 | −143.35 (18) | C32—C31—C34—C35 | 56.2 (2) |
N4—N3—C16—C17 | 1.48 (19) | C32—C31—C34—C39 | −122.1 (2) |
N4—N3—C16—C19 | −174.98 (15) | C32—C33—C40—C41 | 131.3 (2) |
N4—C18—C25—C26 | 134.24 (18) | C32—C33—C40—C45 | −45.0 (3) |
N4—C18—C25—C30 | −47.0 (3) | C33—N6—B1—N2 | 132.20 (17) |
N5—N6—C33—C32 | 0.52 (19) | C33—N6—B1—N4 | −107.73 (19) |
N5—N6—C33—C40 | −179.48 (16) | C33—C40—C41—C42 | −176.15 (17) |
N5—N6—B1—N2 | −51.36 (18) | C33—C40—C45—C44 | 176.22 (18) |
N5—N6—B1—N4 | 68.71 (18) | C34—C31—C32—C33 | 173.69 (16) |
N5—C31—C32—C33 | −1.6 (2) | C34—C35—C36—C37 | 1.9 (3) |
N5—C31—C34—C35 | −129.06 (18) | C35—C34—C39—C38 | 0.3 (3) |
N5—C31—C34—C39 | 52.7 (2) | C35—C36—C37—C38 | −0.4 (3) |
N6—N5—C31—C32 | 1.88 (19) | C36—C37—C38—C39 | −1.1 (3) |
N6—N5—C31—C34 | −173.71 (14) | C37—C38—C39—C34 | 1.1 (3) |
N6—C33—C40—C41 | −48.7 (3) | C39—C34—C35—C36 | −1.8 (3) |
N6—C33—C40—C45 | 134.98 (18) | C40—C41—C42—C43 | 0.2 (3) |
N7—C47—C48—C49 | 176.2 (3) | C41—C40—C45—C44 | −0.3 (3) |
N7—C51—C52—C53 | 179.3 (5) | C41—C42—C43—C44 | −0.4 (3) |
N7—C47A—C48A—C49A | 55.3 (16) | C42—C43—C44—C45 | 0.2 (4) |
N7—C51A—C52A—C53A | 174.2 (13) | C43—C44—C45—C40 | 0.1 (3) |
C1—N1—N2—C3 | 0.62 (17) | C45—C40—C41—C42 | 0.1 (3) |
C1—N1—N2—B1 | −166.56 (14) | C46—N7—C47—C48 | −106.2 (3) |
C1—C2—C3—N2 | 0.22 (18) | C46—N7—C51—C52 | −136.1 (6) |
C1—C2—C3—C10 | −178.28 (16) | C46—N7—C47A—C48A | −129.7 (8) |
C1—C4—C5—C6 | 178.77 (18) | C46—N7—C51A—C52A | −145.2 (11) |
C1—C4—C9—C8 | −179.26 (19) | B1—N2—C3—C2 | 165.51 (15) |
C2—C1—C4—C5 | 151.79 (18) | B1—N2—C3—C10 | −15.9 (3) |
C2—C1—C4—C9 | −27.9 (3) | B1—N4—C18—C17 | 175.73 (16) |
C2—C3—C10—C11 | −53.1 (3) | B1—N4—C18—C25 | −4.4 (3) |
C2—C3—C10—C15 | 124.3 (2) | B1—N6—C33—C32 | 177.22 (16) |
C3—N2—B1—N4 | 130.31 (16) | B1—N6—C33—C40 | −2.8 (3) |
C3—N2—B1—N6 | −110.72 (17) | C47—N7—C46—S1 | 172.1 (2) |
C3—C10—C11—C12 | 178.70 (16) | C47—N7—C46—S2 | −7.9 (3) |
C3—C10—C15—C14 | −178.28 (17) | C47—N7—C51—C52 | 59.9 (8) |
C4—C1—C2—C3 | 179.44 (16) | C47—C48—C49—C50 | 164.6 (3) |
C4—C5—C6—C7 | 1.0 (3) | C51—N7—C46—S1 | 8.6 (4) |
C5—C4—C9—C8 | 1.0 (3) | C51—N7—C46—S2 | −171.4 (3) |
C5—C6—C7—C8 | 0.1 (4) | C51—N7—C47—C48 | 57.8 (5) |
C6—C7—C8—C9 | −0.6 (4) | C51—C52—C53—C54 | 174.6 (6) |
C7—C8—C9—C4 | 0.0 (3) | C47A—N7—C46—S1 | −150.4 (7) |
C9—C4—C5—C6 | −1.5 (3) | C47A—N7—C46—S2 | 29.6 (8) |
C10—C11—C12—C13 | −0.8 (3) | C47A—N7—C51A—C52A | 0.4 (17) |
C11—C10—C15—C14 | −0.8 (3) | C47A—C48A—C49A—C50A | −171.0 (13) |
C11—C12—C13—C14 | −0.1 (3) | C51A—N7—C46—S1 | −9.3 (9) |
C12—C13—C14—C15 | 0.5 (3) | C51A—N7—C46—S2 | 170.8 (9) |
C13—C14—C15—C10 | 0.0 (3) | C51A—N7—C47A—C48A | 84.2 (13) |
C15—C10—C11—C12 | 1.2 (3) | C51A—C52A—C53A—C54A | −171.2 (15) |
(
N,
N-Dibutyldithiocarbamato-
κ2S,
S')[tris(3,5-diphenylpyrazol-1-yl-
κN2)hydroborato]cobalt(II) (1b)
top
Crystal data top
[Co(C45H34BN6)(C9H18NS2)] | Z = 2 |
Mr = 932.88 | F(000) = 978 |
Triclinic, P1 | Dx = 1.311 Mg m−3 |
a = 11.69503 (10) Å | Cu Kα radiation, λ = 1.54184 Å |
b = 15.27162 (13) Å | Cell parameters from 22677 reflections |
c = 15.43643 (16) Å | θ = 3.3–68.4° |
α = 117.4408 (9)° | µ = 4.02 mm−1 |
β = 100.7910 (8)° | T = 150 K |
γ = 94.2199 (7)° | Block, red |
V = 2362.76 (4) Å3 | 0.26 × 0.22 × 0.18 mm |
Data collection top
Rigaku SuperNova (Single source at offset/far, HyPix3000) diffractometer | 8636 independent reflections |
Radiation source: micro-focus sealed X-ray tube, SuperNova (Cu) X-ray Source | 8250 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.048 |
Detector resolution: 10.0000 pixels mm-1 | θmax = 68.5°, θmin = 3.3° |
ω scans | h = −14→12 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2020) | k = −18→18 |
Tmin = 0.631, Tmax = 1.000 | l = −18→18 |
31970 measured reflections | |
Refinement top
Refinement on F2 | 37 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.035 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0504P)2 + 0.7689P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
8636 reflections | Δρmax = 0.46 e Å−3 |
630 parameters | Δρmin = −0.31 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.67469 (2) | 0.41937 (2) | 0.70877 (2) | 0.01895 (8) | |
S1 | 0.63988 (4) | 0.58822 (3) | 0.76749 (3) | 0.02751 (11) | |
S2 | 0.76723 (4) | 0.50606 (3) | 0.88528 (3) | 0.03307 (11) | |
N1 | 0.54286 (11) | 0.34115 (10) | 0.56900 (10) | 0.0191 (3) | |
N2 | 0.57705 (11) | 0.26241 (10) | 0.49498 (10) | 0.0191 (3) | |
N3 | 0.80540 (12) | 0.39736 (10) | 0.62988 (10) | 0.0197 (3) | |
N4 | 0.79945 (11) | 0.30288 (10) | 0.55204 (10) | 0.0188 (3) | |
N5 | 0.66200 (12) | 0.27225 (10) | 0.69499 (10) | 0.0204 (3) | |
N6 | 0.68462 (12) | 0.20111 (10) | 0.60836 (10) | 0.0195 (3) | |
N7 | 0.75119 (16) | 0.70004 (12) | 0.96305 (12) | 0.0385 (4) | |
C1 | 0.44845 (14) | 0.36209 (12) | 0.52235 (12) | 0.0212 (3) | |
C2 | 0.42374 (15) | 0.29942 (13) | 0.41809 (13) | 0.0250 (3) | |
H2 | 0.364047 | 0.299509 | 0.368980 | 0.030* | |
C3 | 0.50662 (14) | 0.23735 (12) | 0.40335 (12) | 0.0216 (3) | |
C4 | 0.38095 (13) | 0.43744 (12) | 0.57805 (12) | 0.0214 (3) | |
C5 | 0.35199 (15) | 0.44405 (13) | 0.66423 (13) | 0.0258 (4) | |
H5 | 0.377866 | 0.401470 | 0.688451 | 0.031* | |
C6 | 0.28516 (15) | 0.51327 (14) | 0.71422 (14) | 0.0285 (4) | |
H6 | 0.265917 | 0.516545 | 0.771307 | 0.034* | |
C7 | 0.24691 (15) | 0.57769 (13) | 0.67920 (14) | 0.0291 (4) | |
H7 | 0.202601 | 0.624596 | 0.712958 | 0.035* | |
C8 | 0.27512 (16) | 0.57172 (14) | 0.59367 (15) | 0.0300 (4) | |
H8 | 0.249518 | 0.614791 | 0.570024 | 0.036* | |
C9 | 0.34123 (15) | 0.50203 (13) | 0.54297 (13) | 0.0261 (4) | |
H9 | 0.359182 | 0.498320 | 0.485306 | 0.031* | |
C10 | 0.52455 (14) | 0.15942 (13) | 0.30711 (12) | 0.0236 (3) | |
C11 | 0.54449 (16) | 0.18677 (14) | 0.23586 (13) | 0.0284 (4) | |
H11 | 0.543177 | 0.252242 | 0.248102 | 0.034* | |
C12 | 0.56630 (17) | 0.11619 (16) | 0.14658 (14) | 0.0352 (4) | |
H12 | 0.581331 | 0.134994 | 0.099842 | 0.042* | |
C13 | 0.56582 (17) | 0.01842 (15) | 0.12684 (14) | 0.0350 (4) | |
H13 | 0.580073 | −0.028494 | 0.066725 | 0.042* | |
C14 | 0.54415 (17) | −0.01018 (14) | 0.19626 (14) | 0.0331 (4) | |
H14 | 0.542693 | −0.076356 | 0.182485 | 0.040* | |
C15 | 0.52464 (15) | 0.06054 (13) | 0.28652 (13) | 0.0279 (4) | |
H15 | 0.511505 | 0.041683 | 0.333681 | 0.034* | |
C16 | 0.90739 (14) | 0.45271 (12) | 0.64211 (12) | 0.0217 (3) | |
C17 | 0.96854 (14) | 0.39394 (13) | 0.57334 (13) | 0.0249 (3) | |
H17 | 1.041811 | 0.414250 | 0.566639 | 0.030* | |
C18 | 0.89862 (14) | 0.29956 (12) | 0.51717 (12) | 0.0212 (3) | |
C19 | 0.94663 (14) | 0.56111 (13) | 0.71491 (13) | 0.0234 (3) | |
C20 | 1.01150 (17) | 0.59454 (14) | 0.81253 (14) | 0.0323 (4) | |
H20 | 1.022399 | 0.549470 | 0.836884 | 0.039* | |
C21 | 1.06063 (18) | 0.69637 (16) | 0.87447 (15) | 0.0397 (5) | |
H21 | 1.104713 | 0.718790 | 0.939959 | 0.048* | |
C22 | 1.04434 (18) | 0.76321 (14) | 0.83945 (16) | 0.0389 (5) | |
H22 | 1.078448 | 0.830624 | 0.880795 | 0.047* | |
C23 | 0.97755 (18) | 0.73102 (14) | 0.74309 (16) | 0.0368 (4) | |
H23 | 0.964889 | 0.776881 | 0.720016 | 0.044* | |
C24 | 0.92939 (16) | 0.63035 (13) | 0.68077 (14) | 0.0297 (4) | |
H24 | 0.885108 | 0.608672 | 0.615498 | 0.036* | |
C25 | 0.92623 (15) | 0.20986 (12) | 0.43611 (13) | 0.0228 (3) | |
C26 | 0.84642 (16) | 0.14686 (13) | 0.34368 (13) | 0.0269 (4) | |
H26 | 0.770836 | 0.160434 | 0.330366 | 0.032* | |
C27 | 0.87903 (18) | 0.06390 (14) | 0.27129 (15) | 0.0341 (4) | |
H27 | 0.824801 | 0.021435 | 0.210141 | 0.041* | |
C28 | 0.99230 (19) | 0.04410 (14) | 0.28988 (16) | 0.0360 (4) | |
H28 | 1.013714 | −0.011894 | 0.241471 | 0.043* | |
C29 | 1.07299 (18) | 0.10740 (16) | 0.38003 (16) | 0.0368 (4) | |
H29 | 1.149360 | 0.094809 | 0.391971 | 0.044* | |
C30 | 1.04056 (16) | 0.18993 (15) | 0.45309 (14) | 0.0304 (4) | |
H30 | 1.095406 | 0.232352 | 0.513886 | 0.037* | |
C31 | 0.65223 (14) | 0.22883 (12) | 0.75218 (12) | 0.0213 (3) | |
C32 | 0.67073 (14) | 0.12991 (12) | 0.70315 (13) | 0.0229 (3) | |
H32 | 0.669807 | 0.083958 | 0.726918 | 0.028* | |
C33 | 0.69067 (13) | 0.11451 (12) | 0.61213 (12) | 0.0205 (3) | |
C34 | 0.61664 (15) | 0.27707 (12) | 0.84809 (13) | 0.0239 (3) | |
C35 | 0.66535 (18) | 0.25881 (15) | 0.92593 (14) | 0.0335 (4) | |
H35 | 0.723739 | 0.219586 | 0.918823 | 0.040* | |
C36 | 0.6277 (2) | 0.29863 (17) | 1.01456 (15) | 0.0429 (5) | |
H36 | 0.661463 | 0.286389 | 1.066526 | 0.051* | |
C37 | 0.54081 (19) | 0.35591 (17) | 1.02570 (16) | 0.0437 (5) | |
H37 | 0.515951 | 0.382627 | 1.085130 | 0.052* | |
C38 | 0.49040 (18) | 0.37374 (17) | 0.94817 (16) | 0.0411 (5) | |
H38 | 0.430854 | 0.411833 | 0.955196 | 0.049* | |
C39 | 0.52843 (16) | 0.33496 (15) | 0.85999 (14) | 0.0325 (4) | |
H39 | 0.494681 | 0.347752 | 0.808414 | 0.039* | |
C40 | 0.71008 (14) | 0.02183 (12) | 0.52925 (12) | 0.0215 (3) | |
C41 | 0.80796 (16) | 0.02057 (13) | 0.48917 (14) | 0.0282 (4) | |
H41 | 0.863171 | 0.079082 | 0.514959 | 0.034* | |
C42 | 0.82282 (18) | −0.06777 (15) | 0.41106 (16) | 0.0356 (4) | |
H42 | 0.887780 | −0.068127 | 0.384231 | 0.043* | |
C43 | 0.74192 (19) | −0.15539 (14) | 0.37264 (15) | 0.0357 (4) | |
H43 | 0.752122 | −0.214278 | 0.319768 | 0.043* | |
C44 | 0.64565 (17) | −0.15545 (13) | 0.41295 (14) | 0.0318 (4) | |
H44 | 0.591688 | −0.214528 | 0.387831 | 0.038* | |
C45 | 0.62990 (15) | −0.06706 (13) | 0.49095 (13) | 0.0249 (3) | |
H45 | 0.565147 | −0.067247 | 0.517876 | 0.030* | |
C46 | 0.72412 (15) | 0.60980 (13) | 0.88158 (13) | 0.0261 (4) | |
C47 | 0.71402 (18) | 0.78904 (13) | 0.96084 (14) | 0.0327 (4) | |
H47A | 0.710383 | 0.837213 | 1.028228 | 0.039* | |
H47B | 0.634720 | 0.769319 | 0.917345 | 0.039* | |
C48 | 0.79424 (18) | 0.84017 (15) | 0.92440 (17) | 0.0391 (5) | |
H48A | 0.875485 | 0.851436 | 0.961416 | 0.047* | |
H48B | 0.788788 | 0.795731 | 0.853690 | 0.047* | |
C49 | 0.76408 (18) | 0.93956 (15) | 0.93704 (17) | 0.0379 (4) | |
H49A | 0.680430 | 0.929725 | 0.906709 | 0.046* | |
H49B | 0.778453 | 0.986576 | 1.008390 | 0.046* | |
C50 | 0.8345 (2) | 0.98442 (19) | 0.8902 (2) | 0.0557 (6) | |
H50A | 0.814986 | 0.941276 | 0.818504 | 0.084* | |
H50B | 0.917508 | 0.991398 | 0.917436 | 0.084* | |
H50C | 0.815853 | 1.049183 | 0.904695 | 0.084* | |
B1 | 0.68992 (16) | 0.22226 (13) | 0.52053 (14) | 0.0193 (4) | |
H1 | 0.6949 (15) | 0.1543 (13) | 0.4577 (14) | 0.017 (4)* | |
C51 | 0.8044 (2) | 0.71341 (19) | 1.06424 (19) | 0.0301 (8) | 0.725 (6) |
H51A | 0.785243 | 0.650913 | 1.064993 | 0.036* | 0.725 (6) |
H51B | 0.771582 | 0.764110 | 1.113914 | 0.036* | 0.725 (6) |
C52 | 0.9373 (3) | 0.7450 (3) | 1.0912 (3) | 0.0438 (9) | 0.725 (6) |
H52A | 0.955889 | 0.805879 | 1.087411 | 0.053* | 0.725 (6) |
H52B | 0.969852 | 0.693026 | 1.042486 | 0.053* | 0.725 (6) |
C53 | 0.9952 (4) | 0.7634 (3) | 1.1968 (3) | 0.0491 (10) | 0.725 (6) |
H53A | 1.078141 | 0.792458 | 1.213824 | 0.059* | 0.725 (6) |
H53B | 0.958532 | 0.812299 | 1.244393 | 0.059* | 0.725 (6) |
C54 | 0.9868 (6) | 0.6717 (5) | 1.2094 (5) | 0.0789 (17) | 0.725 (6) |
H54C | 1.024562 | 0.689890 | 1.277717 | 0.118* | 0.725 (6) |
H54A | 1.025437 | 0.623599 | 1.164481 | 0.118* | 0.725 (6) |
H54B | 0.905027 | 0.642915 | 1.194132 | 0.118* | 0.725 (6) |
C51A | 0.8768 (6) | 0.7233 (6) | 1.0377 (6) | 0.036 (2) | 0.275 (6) |
H51C | 0.921826 | 0.670807 | 1.008539 | 0.043* | 0.275 (6) |
H51D | 0.922117 | 0.787064 | 1.053865 | 0.043* | 0.275 (6) |
C52A | 0.8460 (9) | 0.7269 (9) | 1.1315 (8) | 0.066 (3) | 0.275 (6) |
H52C | 0.799634 | 0.662574 | 1.112365 | 0.079* | 0.275 (6) |
H52D | 0.797227 | 0.777398 | 1.156261 | 0.079* | 0.275 (6) |
C53A | 0.9559 (11) | 0.7510 (10) | 1.2176 (9) | 0.063 (4) | 0.275 (6) |
H53C | 1.002095 | 0.816191 | 1.239169 | 0.076* | 0.275 (6) |
H53D | 0.931356 | 0.752636 | 1.274857 | 0.076* | 0.275 (6) |
C54A | 1.0273 (11) | 0.6730 (10) | 1.1800 (12) | 0.067 (4) | 0.275 (6) |
H54F | 1.085175 | 0.677509 | 1.235664 | 0.100* | 0.275 (6) |
H54D | 1.066765 | 0.682162 | 1.134732 | 0.100* | 0.275 (6) |
H54E | 0.976901 | 0.608177 | 1.144949 | 0.100* | 0.275 (6) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02038 (14) | 0.01792 (14) | 0.01800 (14) | 0.00440 (10) | 0.00586 (10) | 0.00774 (11) |
S1 | 0.0312 (2) | 0.0228 (2) | 0.0232 (2) | 0.00803 (16) | 0.00143 (17) | 0.00832 (17) |
S2 | 0.0463 (3) | 0.0242 (2) | 0.0231 (2) | 0.00727 (19) | −0.00060 (19) | 0.01010 (18) |
N1 | 0.0196 (6) | 0.0179 (6) | 0.0194 (7) | 0.0055 (5) | 0.0056 (5) | 0.0080 (5) |
N2 | 0.0195 (6) | 0.0188 (6) | 0.0173 (6) | 0.0040 (5) | 0.0055 (5) | 0.0071 (5) |
N3 | 0.0210 (6) | 0.0179 (6) | 0.0201 (7) | 0.0039 (5) | 0.0054 (5) | 0.0090 (5) |
N4 | 0.0202 (6) | 0.0182 (6) | 0.0188 (6) | 0.0054 (5) | 0.0066 (5) | 0.0086 (5) |
N5 | 0.0231 (7) | 0.0185 (6) | 0.0188 (7) | 0.0036 (5) | 0.0049 (5) | 0.0087 (5) |
N6 | 0.0219 (6) | 0.0173 (6) | 0.0200 (7) | 0.0051 (5) | 0.0063 (5) | 0.0090 (5) |
N7 | 0.0511 (10) | 0.0241 (8) | 0.0272 (8) | 0.0076 (7) | −0.0034 (7) | 0.0066 (7) |
C1 | 0.0195 (7) | 0.0221 (8) | 0.0221 (8) | 0.0036 (6) | 0.0047 (6) | 0.0110 (7) |
C2 | 0.0224 (8) | 0.0290 (8) | 0.0211 (8) | 0.0056 (7) | 0.0024 (7) | 0.0112 (7) |
C3 | 0.0218 (8) | 0.0221 (8) | 0.0182 (8) | 0.0013 (6) | 0.0039 (6) | 0.0083 (7) |
C4 | 0.0168 (7) | 0.0225 (8) | 0.0223 (8) | 0.0024 (6) | 0.0019 (6) | 0.0099 (7) |
C5 | 0.0267 (8) | 0.0271 (8) | 0.0256 (9) | 0.0077 (7) | 0.0068 (7) | 0.0139 (7) |
C6 | 0.0251 (8) | 0.0325 (9) | 0.0258 (9) | 0.0061 (7) | 0.0086 (7) | 0.0116 (8) |
C7 | 0.0214 (8) | 0.0254 (8) | 0.0342 (10) | 0.0073 (7) | 0.0065 (7) | 0.0090 (8) |
C8 | 0.0254 (8) | 0.0273 (9) | 0.0394 (10) | 0.0085 (7) | 0.0047 (8) | 0.0185 (8) |
C9 | 0.0238 (8) | 0.0295 (9) | 0.0274 (9) | 0.0063 (7) | 0.0047 (7) | 0.0161 (7) |
C10 | 0.0192 (7) | 0.0255 (8) | 0.0198 (8) | 0.0021 (6) | 0.0020 (6) | 0.0072 (7) |
C11 | 0.0293 (9) | 0.0311 (9) | 0.0230 (9) | 0.0045 (7) | 0.0030 (7) | 0.0130 (7) |
C12 | 0.0377 (10) | 0.0450 (11) | 0.0221 (9) | 0.0068 (9) | 0.0085 (8) | 0.0154 (9) |
C13 | 0.0331 (10) | 0.0393 (10) | 0.0201 (9) | 0.0079 (8) | 0.0065 (7) | 0.0040 (8) |
C14 | 0.0326 (9) | 0.0248 (9) | 0.0308 (10) | 0.0032 (7) | 0.0061 (8) | 0.0053 (8) |
C15 | 0.0286 (9) | 0.0260 (8) | 0.0246 (9) | 0.0002 (7) | 0.0075 (7) | 0.0089 (7) |
C16 | 0.0195 (7) | 0.0234 (8) | 0.0226 (8) | 0.0033 (6) | 0.0045 (6) | 0.0118 (7) |
C17 | 0.0189 (8) | 0.0263 (8) | 0.0270 (9) | 0.0033 (6) | 0.0075 (7) | 0.0104 (7) |
C18 | 0.0195 (7) | 0.0238 (8) | 0.0229 (8) | 0.0069 (6) | 0.0058 (6) | 0.0128 (7) |
C19 | 0.0186 (7) | 0.0243 (8) | 0.0251 (8) | 0.0018 (6) | 0.0083 (7) | 0.0093 (7) |
C20 | 0.0325 (9) | 0.0327 (10) | 0.0282 (9) | 0.0018 (8) | 0.0055 (8) | 0.0133 (8) |
C21 | 0.0341 (10) | 0.0406 (11) | 0.0262 (10) | −0.0027 (8) | 0.0034 (8) | 0.0042 (9) |
C22 | 0.0360 (10) | 0.0237 (9) | 0.0430 (12) | −0.0037 (8) | 0.0176 (9) | 0.0032 (8) |
C23 | 0.0421 (11) | 0.0250 (9) | 0.0456 (12) | 0.0062 (8) | 0.0193 (9) | 0.0160 (9) |
C24 | 0.0322 (9) | 0.0266 (9) | 0.0299 (9) | 0.0048 (7) | 0.0093 (8) | 0.0129 (8) |
C25 | 0.0248 (8) | 0.0236 (8) | 0.0259 (8) | 0.0078 (7) | 0.0108 (7) | 0.0147 (7) |
C26 | 0.0272 (9) | 0.0277 (9) | 0.0265 (9) | 0.0053 (7) | 0.0110 (7) | 0.0121 (7) |
C27 | 0.0409 (10) | 0.0277 (9) | 0.0305 (10) | 0.0018 (8) | 0.0170 (8) | 0.0093 (8) |
C28 | 0.0518 (12) | 0.0268 (9) | 0.0411 (11) | 0.0176 (9) | 0.0292 (10) | 0.0180 (9) |
C29 | 0.0401 (10) | 0.0429 (11) | 0.0448 (12) | 0.0269 (9) | 0.0230 (9) | 0.0281 (10) |
C30 | 0.0285 (9) | 0.0372 (10) | 0.0301 (9) | 0.0140 (8) | 0.0096 (8) | 0.0178 (8) |
C31 | 0.0193 (7) | 0.0238 (8) | 0.0203 (8) | 0.0012 (6) | 0.0026 (6) | 0.0114 (7) |
C32 | 0.0240 (8) | 0.0220 (8) | 0.0259 (8) | 0.0024 (6) | 0.0046 (7) | 0.0150 (7) |
C33 | 0.0177 (7) | 0.0200 (8) | 0.0244 (8) | 0.0022 (6) | 0.0030 (6) | 0.0122 (7) |
C34 | 0.0249 (8) | 0.0236 (8) | 0.0214 (8) | −0.0013 (6) | 0.0054 (7) | 0.0103 (7) |
C35 | 0.0422 (11) | 0.0334 (10) | 0.0254 (9) | 0.0069 (8) | 0.0072 (8) | 0.0151 (8) |
C36 | 0.0575 (13) | 0.0474 (12) | 0.0247 (10) | 0.0021 (10) | 0.0104 (9) | 0.0194 (9) |
C37 | 0.0413 (11) | 0.0530 (13) | 0.0283 (10) | −0.0038 (10) | 0.0171 (9) | 0.0115 (9) |
C38 | 0.0289 (9) | 0.0496 (12) | 0.0354 (11) | 0.0060 (9) | 0.0140 (8) | 0.0108 (9) |
C39 | 0.0265 (9) | 0.0398 (10) | 0.0285 (9) | 0.0053 (8) | 0.0071 (7) | 0.0143 (8) |
C40 | 0.0235 (8) | 0.0208 (8) | 0.0241 (8) | 0.0078 (6) | 0.0054 (7) | 0.0138 (7) |
C41 | 0.0295 (9) | 0.0250 (8) | 0.0391 (10) | 0.0092 (7) | 0.0144 (8) | 0.0201 (8) |
C42 | 0.0438 (11) | 0.0346 (10) | 0.0446 (11) | 0.0204 (9) | 0.0259 (9) | 0.0252 (9) |
C43 | 0.0495 (12) | 0.0275 (9) | 0.0330 (10) | 0.0182 (9) | 0.0159 (9) | 0.0134 (8) |
C44 | 0.0346 (10) | 0.0223 (8) | 0.0328 (10) | 0.0045 (7) | 0.0045 (8) | 0.0103 (8) |
C45 | 0.0231 (8) | 0.0238 (8) | 0.0293 (9) | 0.0057 (7) | 0.0061 (7) | 0.0139 (7) |
C46 | 0.0270 (8) | 0.0245 (8) | 0.0240 (9) | 0.0033 (7) | 0.0059 (7) | 0.0099 (7) |
C47 | 0.0412 (10) | 0.0232 (9) | 0.0273 (9) | 0.0082 (8) | 0.0076 (8) | 0.0070 (7) |
C48 | 0.0334 (10) | 0.0338 (10) | 0.0464 (12) | 0.0085 (8) | 0.0140 (9) | 0.0147 (9) |
C49 | 0.0376 (10) | 0.0337 (10) | 0.0431 (12) | 0.0069 (8) | 0.0142 (9) | 0.0175 (9) |
C50 | 0.0646 (15) | 0.0513 (14) | 0.0585 (15) | 0.0055 (12) | 0.0252 (13) | 0.0298 (13) |
B1 | 0.0209 (8) | 0.0182 (8) | 0.0197 (9) | 0.0049 (7) | 0.0065 (7) | 0.0092 (7) |
C51 | 0.0327 (15) | 0.0312 (13) | 0.0208 (14) | 0.0031 (10) | 0.0053 (11) | 0.0089 (11) |
C52 | 0.0335 (16) | 0.0566 (19) | 0.0396 (17) | −0.0031 (14) | 0.0021 (14) | 0.0262 (15) |
C53 | 0.0407 (19) | 0.060 (2) | 0.0394 (18) | 0.0078 (17) | 0.0002 (14) | 0.0219 (17) |
C54 | 0.088 (4) | 0.092 (3) | 0.080 (4) | 0.032 (3) | 0.009 (3) | 0.063 (3) |
C51A | 0.019 (4) | 0.033 (4) | 0.037 (4) | 0.003 (3) | −0.001 (3) | 0.006 (3) |
C52A | 0.057 (5) | 0.096 (8) | 0.049 (5) | 0.040 (5) | 0.021 (4) | 0.033 (5) |
C53A | 0.068 (6) | 0.072 (7) | 0.047 (5) | 0.028 (6) | 0.013 (4) | 0.026 (5) |
C54A | 0.041 (5) | 0.057 (6) | 0.072 (9) | 0.009 (4) | 0.000 (5) | 0.012 (5) |
Geometric parameters (Å, º) top
Co1—S1 | 2.4030 (5) | C27—C28 | 1.388 (3) |
Co1—S2 | 2.3892 (5) | C28—H28 | 0.9300 |
Co1—N1 | 2.1371 (14) | C28—C29 | 1.377 (3) |
Co1—N3 | 2.0804 (13) | C29—H29 | 0.9300 |
Co1—N5 | 2.1480 (13) | C29—C30 | 1.387 (3) |
S1—C46 | 1.7169 (18) | C30—H30 | 0.9300 |
S2—C46 | 1.7199 (18) | C31—C32 | 1.399 (2) |
N1—N2 | 1.3737 (18) | C31—C34 | 1.476 (2) |
N1—C1 | 1.344 (2) | C32—H32 | 0.9300 |
N2—C3 | 1.358 (2) | C32—C33 | 1.382 (2) |
N2—B1 | 1.556 (2) | C33—C40 | 1.476 (2) |
N3—N4 | 1.3735 (18) | C34—C35 | 1.386 (2) |
N3—C16 | 1.339 (2) | C34—C39 | 1.391 (3) |
N4—C18 | 1.362 (2) | C35—H35 | 0.9300 |
N4—B1 | 1.541 (2) | C35—C36 | 1.391 (3) |
N5—N6 | 1.3691 (18) | C36—H36 | 0.9300 |
N5—C31 | 1.341 (2) | C36—C37 | 1.373 (3) |
N6—C33 | 1.357 (2) | C37—H37 | 0.9300 |
N6—B1 | 1.542 (2) | C37—C38 | 1.383 (3) |
N7—C46 | 1.331 (2) | C38—H38 | 0.9300 |
N7—C47 | 1.470 (2) | C38—C39 | 1.387 (3) |
N7—C51 | 1.481 (3) | C39—H39 | 0.9300 |
N7—C51A | 1.588 (8) | C40—C41 | 1.397 (2) |
C1—C2 | 1.398 (2) | C40—C45 | 1.392 (2) |
C1—C4 | 1.470 (2) | C41—H41 | 0.9300 |
C2—H2 | 0.9300 | C41—C42 | 1.385 (3) |
C2—C3 | 1.382 (2) | C42—H42 | 0.9300 |
C3—C10 | 1.480 (2) | C42—C43 | 1.382 (3) |
C4—C5 | 1.395 (2) | C43—H43 | 0.9300 |
C4—C9 | 1.396 (2) | C43—C44 | 1.385 (3) |
C5—H5 | 0.9300 | C44—H44 | 0.9300 |
C5—C6 | 1.385 (2) | C44—C45 | 1.388 (2) |
C6—H6 | 0.9300 | C45—H45 | 0.9300 |
C6—C7 | 1.387 (3) | C47—H47A | 0.9700 |
C7—H7 | 0.9300 | C47—H47B | 0.9700 |
C7—C8 | 1.384 (3) | C47—C48 | 1.517 (3) |
C8—H8 | 0.9300 | C48—H48A | 0.9700 |
C8—C9 | 1.387 (3) | C48—H48B | 0.9700 |
C9—H9 | 0.9300 | C48—C49 | 1.516 (3) |
C10—C11 | 1.394 (2) | C49—H49A | 0.9700 |
C10—C15 | 1.393 (3) | C49—H49B | 0.9700 |
C11—H11 | 0.9300 | C49—C50 | 1.506 (3) |
C11—C12 | 1.389 (3) | C50—H50A | 0.9600 |
C12—H12 | 0.9300 | C50—H50B | 0.9600 |
C12—C13 | 1.379 (3) | C50—H50C | 0.9600 |
C13—H13 | 0.9300 | B1—H1 | 1.060 (18) |
C13—C14 | 1.386 (3) | C51—H51A | 0.9700 |
C14—H14 | 0.9300 | C51—H51B | 0.9700 |
C14—C15 | 1.389 (3) | C51—C52 | 1.512 (4) |
C15—H15 | 0.9300 | C52—H52A | 0.9700 |
C16—C17 | 1.394 (2) | C52—H52B | 0.9700 |
C16—C19 | 1.481 (2) | C52—C53 | 1.527 (5) |
C17—H17 | 0.9300 | C53—H53A | 0.9700 |
C17—C18 | 1.381 (2) | C53—H53B | 0.9700 |
C18—C25 | 1.478 (2) | C53—C54 | 1.499 (7) |
C19—C20 | 1.383 (3) | C54—H54C | 0.9600 |
C19—C24 | 1.393 (3) | C54—H54A | 0.9600 |
C20—H20 | 0.9300 | C54—H54B | 0.9600 |
C20—C21 | 1.398 (3) | C51A—H51C | 0.9700 |
C21—H21 | 0.9300 | C51A—H51D | 0.9700 |
C21—C22 | 1.367 (3) | C51A—C52A | 1.535 (14) |
C22—H22 | 0.9300 | C52A—H52C | 0.9700 |
C22—C23 | 1.378 (3) | C52A—H52D | 0.9700 |
C23—H23 | 0.9300 | C52A—C53A | 1.548 (13) |
C23—C24 | 1.383 (3) | C53A—H53C | 0.9700 |
C24—H24 | 0.9300 | C53A—H53D | 0.9700 |
C25—C26 | 1.392 (2) | C53A—C54A | 1.465 (14) |
C25—C30 | 1.397 (2) | C54A—H54F | 0.9600 |
C26—H26 | 0.9300 | C54A—H54D | 0.9600 |
C26—C27 | 1.387 (3) | C54A—H54E | 0.9600 |
C27—H27 | 0.9300 | | |
| | | |
S2—Co1—S1 | 74.746 (16) | N5—C31—C34 | 123.94 (15) |
N1—Co1—S1 | 101.13 (4) | C32—C31—C34 | 125.97 (15) |
N1—Co1—S2 | 161.55 (4) | C31—C32—H32 | 127.1 |
N1—Co1—N5 | 82.10 (5) | C33—C32—C31 | 105.87 (14) |
N3—Co1—S1 | 109.37 (4) | C33—C32—H32 | 127.1 |
N3—Co1—S2 | 108.76 (4) | N6—C33—C32 | 107.52 (14) |
N3—Co1—N1 | 89.62 (5) | N6—C33—C40 | 123.86 (14) |
N3—Co1—N5 | 92.96 (5) | C32—C33—C40 | 128.57 (15) |
N5—Co1—S1 | 157.38 (4) | C35—C34—C31 | 119.74 (16) |
N5—Co1—S2 | 95.05 (4) | C35—C34—C39 | 118.66 (17) |
C46—S1—Co1 | 84.51 (6) | C39—C34—C31 | 121.43 (16) |
C46—S2—Co1 | 84.88 (6) | C34—C35—H35 | 119.7 |
N2—N1—Co1 | 113.93 (9) | C34—C35—C36 | 120.59 (19) |
C1—N1—Co1 | 136.42 (11) | C36—C35—H35 | 119.7 |
C1—N1—N2 | 106.47 (13) | C35—C36—H36 | 119.8 |
N1—N2—B1 | 120.91 (12) | C37—C36—C35 | 120.3 (2) |
C3—N2—N1 | 109.72 (12) | C37—C36—H36 | 119.8 |
C3—N2—B1 | 129.02 (13) | C36—C37—H37 | 120.1 |
N4—N3—Co1 | 117.84 (10) | C36—C37—C38 | 119.74 (18) |
C16—N3—Co1 | 134.87 (11) | C38—C37—H37 | 120.1 |
C16—N3—N4 | 106.88 (13) | C37—C38—H38 | 119.9 |
N3—N4—B1 | 118.44 (12) | C37—C38—C39 | 120.2 (2) |
C18—N4—N3 | 109.68 (13) | C39—C38—H38 | 119.9 |
C18—N4—B1 | 131.87 (13) | C34—C39—H39 | 119.7 |
N6—N5—Co1 | 114.09 (10) | C38—C39—C34 | 120.52 (19) |
C31—N5—Co1 | 138.64 (11) | C38—C39—H39 | 119.7 |
C31—N5—N6 | 106.64 (12) | C41—C40—C33 | 121.71 (15) |
N5—N6—B1 | 120.78 (12) | C45—C40—C33 | 119.27 (15) |
C33—N6—N5 | 110.09 (13) | C45—C40—C41 | 119.01 (16) |
C33—N6—B1 | 128.94 (13) | C40—C41—H41 | 120.0 |
C46—N7—C47 | 122.22 (16) | C42—C41—C40 | 120.03 (17) |
C46—N7—C51 | 121.38 (17) | C42—C41—H41 | 120.0 |
C46—N7—C51A | 115.0 (3) | C41—C42—H42 | 119.7 |
C47—N7—C51 | 115.75 (17) | C43—C42—C41 | 120.54 (17) |
C47—N7—C51A | 113.8 (3) | C43—C42—H42 | 119.7 |
N1—C1—C2 | 110.20 (14) | C42—C43—H43 | 120.0 |
N1—C1—C4 | 122.40 (14) | C42—C43—C44 | 119.95 (17) |
C2—C1—C4 | 127.33 (15) | C44—C43—H43 | 120.0 |
C1—C2—H2 | 127.2 | C43—C44—H44 | 120.1 |
C3—C2—C1 | 105.55 (14) | C43—C44—C45 | 119.82 (18) |
C3—C2—H2 | 127.2 | C45—C44—H44 | 120.1 |
N2—C3—C2 | 108.02 (14) | C40—C45—H45 | 119.7 |
N2—C3—C10 | 123.39 (14) | C44—C45—C40 | 120.64 (16) |
C2—C3—C10 | 128.52 (15) | C44—C45—H45 | 119.7 |
C5—C4—C1 | 121.37 (15) | S1—C46—S2 | 115.64 (10) |
C5—C4—C9 | 118.67 (15) | N7—C46—S1 | 122.51 (14) |
C9—C4—C1 | 119.93 (15) | N7—C46—S2 | 121.81 (14) |
C4—C5—H5 | 119.6 | N7—C47—H47A | 108.6 |
C6—C5—C4 | 120.82 (16) | N7—C47—H47B | 108.6 |
C6—C5—H5 | 119.6 | N7—C47—C48 | 114.60 (16) |
C5—C6—H6 | 120.0 | H47A—C47—H47B | 107.6 |
C5—C6—C7 | 120.06 (17) | C48—C47—H47A | 108.6 |
C7—C6—H6 | 120.0 | C48—C47—H47B | 108.6 |
C6—C7—H7 | 120.2 | C47—C48—H48A | 108.9 |
C8—C7—C6 | 119.58 (16) | C47—C48—H48B | 108.9 |
C8—C7—H7 | 120.2 | H48A—C48—H48B | 107.7 |
C7—C8—H8 | 119.7 | C49—C48—C47 | 113.36 (16) |
C7—C8—C9 | 120.54 (17) | C49—C48—H48A | 108.9 |
C9—C8—H8 | 119.7 | C49—C48—H48B | 108.9 |
C4—C9—H9 | 119.8 | C48—C49—H49A | 108.9 |
C8—C9—C4 | 120.33 (17) | C48—C49—H49B | 108.9 |
C8—C9—H9 | 119.8 | H49A—C49—H49B | 107.7 |
C11—C10—C3 | 118.69 (15) | C50—C49—C48 | 113.24 (18) |
C15—C10—C3 | 122.17 (16) | C50—C49—H49A | 108.9 |
C15—C10—C11 | 119.13 (16) | C50—C49—H49B | 108.9 |
C10—C11—H11 | 120.0 | C49—C50—H50A | 109.5 |
C12—C11—C10 | 119.97 (17) | C49—C50—H50B | 109.5 |
C12—C11—H11 | 120.0 | C49—C50—H50C | 109.5 |
C11—C12—H12 | 119.8 | H50A—C50—H50B | 109.5 |
C13—C12—C11 | 120.39 (18) | H50A—C50—H50C | 109.5 |
C13—C12—H12 | 119.8 | H50B—C50—H50C | 109.5 |
C12—C13—H13 | 119.9 | N2—B1—H1 | 110.8 (10) |
C12—C13—C14 | 120.22 (17) | N4—B1—N2 | 108.59 (13) |
C14—C13—H13 | 119.9 | N4—B1—N6 | 109.61 (13) |
C13—C14—H14 | 120.2 | N4—B1—H1 | 110.5 (10) |
C13—C14—C15 | 119.62 (18) | N6—B1—N2 | 109.24 (13) |
C15—C14—H14 | 120.2 | N6—B1—H1 | 108.1 (10) |
C10—C15—H15 | 119.7 | N7—C51—H51A | 109.6 |
C14—C15—C10 | 120.63 (17) | N7—C51—H51B | 109.6 |
C14—C15—H15 | 119.7 | N7—C51—C52 | 110.4 (2) |
N3—C16—C17 | 109.77 (14) | H51A—C51—H51B | 108.1 |
N3—C16—C19 | 124.93 (14) | C52—C51—H51A | 109.6 |
C17—C16—C19 | 125.25 (15) | C52—C51—H51B | 109.6 |
C16—C17—H17 | 126.8 | C51—C52—H52A | 109.2 |
C18—C17—C16 | 106.32 (14) | C51—C52—H52B | 109.2 |
C18—C17—H17 | 126.8 | C51—C52—C53 | 112.0 (3) |
N4—C18—C17 | 107.34 (14) | H52A—C52—H52B | 107.9 |
N4—C18—C25 | 125.59 (15) | C53—C52—H52A | 109.2 |
C17—C18—C25 | 127.05 (15) | C53—C52—H52B | 109.2 |
C20—C19—C16 | 121.62 (16) | C52—C53—H53A | 108.6 |
C20—C19—C24 | 119.10 (17) | C52—C53—H53B | 108.6 |
C24—C19—C16 | 118.87 (16) | H53A—C53—H53B | 107.5 |
C19—C20—H20 | 120.1 | C54—C53—C52 | 114.8 (4) |
C19—C20—C21 | 119.75 (19) | C54—C53—H53A | 108.6 |
C21—C20—H20 | 120.1 | C54—C53—H53B | 108.6 |
C20—C21—H21 | 119.8 | C53—C54—H54C | 109.5 |
C22—C21—C20 | 120.48 (19) | C53—C54—H54A | 109.5 |
C22—C21—H21 | 119.8 | C53—C54—H54B | 109.5 |
C21—C22—H22 | 119.9 | H54C—C54—H54A | 109.5 |
C21—C22—C23 | 120.20 (18) | H54C—C54—H54B | 109.5 |
C23—C22—H22 | 119.9 | H54A—C54—H54B | 109.5 |
C22—C23—H23 | 120.1 | N7—C51A—H51C | 111.0 |
C22—C23—C24 | 119.86 (19) | N7—C51A—H51D | 111.0 |
C24—C23—H23 | 120.1 | H51C—C51A—H51D | 109.0 |
C19—C24—H24 | 119.7 | C52A—C51A—N7 | 103.6 (6) |
C23—C24—C19 | 120.58 (18) | C52A—C51A—H51C | 111.0 |
C23—C24—H24 | 119.7 | C52A—C51A—H51D | 111.0 |
C26—C25—C18 | 123.76 (15) | C51A—C52A—H52C | 108.9 |
C26—C25—C30 | 118.79 (16) | C51A—C52A—H52D | 108.9 |
C30—C25—C18 | 117.41 (16) | C51A—C52A—C53A | 113.5 (9) |
C25—C26—H26 | 119.8 | H52C—C52A—H52D | 107.7 |
C27—C26—C25 | 120.35 (17) | C53A—C52A—H52C | 108.9 |
C27—C26—H26 | 119.8 | C53A—C52A—H52D | 108.9 |
C26—C27—H27 | 119.9 | C52A—C53A—H53C | 110.0 |
C26—C27—C28 | 120.19 (19) | C52A—C53A—H53D | 110.0 |
C28—C27—H27 | 119.9 | H53C—C53A—H53D | 108.4 |
C27—C28—H28 | 120.0 | C54A—C53A—C52A | 108.4 (10) |
C29—C28—C27 | 119.96 (17) | C54A—C53A—H53C | 110.0 |
C29—C28—H28 | 120.0 | C54A—C53A—H53D | 110.0 |
C28—C29—H29 | 119.9 | C53A—C54A—H54F | 109.5 |
C28—C29—C30 | 120.11 (18) | C53A—C54A—H54D | 109.5 |
C30—C29—H29 | 119.9 | C53A—C54A—H54E | 109.5 |
C25—C30—H30 | 119.7 | H54F—C54A—H54D | 109.5 |
C29—C30—C25 | 120.56 (18) | H54F—C54A—H54E | 109.5 |
C29—C30—H30 | 119.7 | H54D—C54A—H54E | 109.5 |
N5—C31—C32 | 109.88 (14) | | |
| | | |
Co1—S1—C46—S2 | −4.36 (9) | C15—C10—C11—C12 | −1.2 (3) |
Co1—S1—C46—N7 | 177.89 (17) | C16—N3—N4—C18 | 0.86 (17) |
Co1—S2—C46—S1 | 4.38 (9) | C16—N3—N4—B1 | −179.75 (13) |
Co1—S2—C46—N7 | −177.85 (16) | C16—C17—C18—N4 | −0.05 (19) |
Co1—N1—N2—C3 | −161.33 (10) | C16—C17—C18—C25 | −178.35 (16) |
Co1—N1—N2—B1 | 12.51 (17) | C16—C19—C20—C21 | 171.21 (17) |
Co1—N1—C1—C2 | 155.63 (13) | C16—C19—C24—C23 | −172.00 (16) |
Co1—N1—C1—C4 | −27.3 (2) | C17—C16—C19—C20 | −93.7 (2) |
Co1—N3—N4—C18 | −172.90 (10) | C17—C16—C19—C24 | 78.9 (2) |
Co1—N3—N4—B1 | 6.48 (17) | C17—C18—C25—C26 | −133.92 (19) |
Co1—N3—C16—C17 | 171.32 (12) | C17—C18—C25—C30 | 44.0 (2) |
Co1—N3—C16—C19 | −11.0 (3) | C18—N4—B1—N2 | −125.13 (17) |
Co1—N5—N6—C33 | 171.69 (10) | C18—N4—B1—N6 | 115.60 (18) |
Co1—N5—N6—B1 | −13.01 (17) | C18—C25—C26—C27 | −179.97 (16) |
Co1—N5—C31—C32 | −168.66 (12) | C18—C25—C30—C29 | −179.55 (17) |
Co1—N5—C31—C34 | 16.3 (3) | C19—C16—C17—C18 | −177.03 (16) |
N1—N2—C3—C2 | −1.21 (18) | C19—C20—C21—C22 | 0.4 (3) |
N1—N2—C3—C10 | 176.13 (14) | C20—C19—C24—C23 | 0.8 (3) |
N1—N2—B1—N4 | −68.23 (17) | C20—C21—C22—C23 | 1.1 (3) |
N1—N2—B1—N6 | 51.27 (18) | C21—C22—C23—C24 | −1.7 (3) |
N1—C1—C2—C3 | 1.24 (19) | C22—C23—C24—C19 | 0.7 (3) |
N1—C1—C4—C5 | −42.8 (2) | C24—C19—C20—C21 | −1.3 (3) |
N1—C1—C4—C9 | 139.30 (17) | C25—C26—C27—C28 | −1.1 (3) |
N2—N1—C1—C2 | −1.96 (18) | C26—C25—C30—C29 | −1.6 (3) |
N2—N1—C1—C4 | 175.07 (14) | C26—C27—C28—C29 | −0.6 (3) |
N2—C3—C10—C11 | −120.61 (18) | C27—C28—C29—C30 | 1.2 (3) |
N2—C3—C10—C15 | 58.0 (2) | C28—C29—C30—C25 | −0.1 (3) |
N3—N4—C18—C17 | −0.50 (18) | C30—C25—C26—C27 | 2.2 (3) |
N3—N4—C18—C25 | 177.84 (14) | C31—N5—N6—C33 | −0.91 (17) |
N3—N4—B1—N2 | 55.64 (17) | C31—N5—N6—B1 | 174.40 (13) |
N3—N4—B1—N6 | −63.63 (17) | C31—C32—C33—N6 | 0.28 (18) |
N3—C16—C17—C18 | 0.59 (19) | C31—C32—C33—C40 | −177.15 (16) |
N3—C16—C19—C20 | 89.0 (2) | C31—C34—C35—C36 | −176.06 (18) |
N3—C16—C19—C24 | −98.4 (2) | C31—C34—C39—C38 | 175.39 (17) |
N4—N3—C16—C17 | −0.89 (18) | C32—C31—C34—C35 | 40.3 (2) |
N4—N3—C16—C19 | 176.74 (15) | C32—C31—C34—C39 | −134.85 (19) |
N4—C18—C25—C26 | 48.1 (2) | C32—C33—C40—C41 | −127.23 (19) |
N4—C18—C25—C30 | −134.06 (18) | C32—C33—C40—C45 | 51.8 (2) |
N5—N6—C33—C32 | 0.38 (17) | C33—N6—B1—N2 | 123.65 (16) |
N5—N6—C33—C40 | 177.95 (14) | C33—N6—B1—N4 | −117.48 (16) |
N5—N6—B1—N2 | −50.68 (18) | C33—C40—C41—C42 | −179.67 (16) |
N5—N6—B1—N4 | 68.19 (17) | C33—C40—C45—C44 | 179.93 (16) |
N5—C31—C32—C33 | −0.86 (18) | C34—C31—C32—C33 | 174.04 (15) |
N5—C31—C34—C35 | −145.47 (17) | C34—C35—C36—C37 | 0.6 (3) |
N5—C31—C34—C39 | 39.4 (2) | C35—C34—C39—C38 | 0.2 (3) |
N6—N5—C31—C32 | 1.08 (17) | C35—C36—C37—C38 | 0.2 (3) |
N6—N5—C31—C34 | −173.94 (14) | C36—C37—C38—C39 | −0.8 (3) |
N6—C33—C40—C41 | 55.7 (2) | C37—C38—C39—C34 | 0.6 (3) |
N6—C33—C40—C45 | −125.29 (17) | C39—C34—C35—C36 | −0.8 (3) |
N7—C47—C48—C49 | −171.71 (17) | C40—C41—C42—C43 | −0.5 (3) |
N7—C51—C52—C53 | 177.9 (3) | C41—C40—C45—C44 | −1.1 (3) |
N7—C51A—C52A—C53A | −178.9 (8) | C41—C42—C43—C44 | −0.6 (3) |
C1—N1—N2—C3 | 1.96 (17) | C42—C43—C44—C45 | 0.9 (3) |
C1—N1—N2—B1 | 175.80 (14) | C43—C44—C45—C40 | −0.1 (3) |
C1—C2—C3—N2 | 0.00 (19) | C45—C40—C41—C42 | 1.3 (3) |
C1—C2—C3—C10 | −177.16 (16) | C46—N7—C47—C48 | −83.4 (2) |
C1—C4—C5—C6 | −177.94 (15) | C46—N7—C51—C52 | 97.5 (3) |
C1—C4—C9—C8 | 178.46 (16) | C46—N7—C51A—C52A | −111.6 (6) |
C2—C1—C4—C5 | 133.69 (19) | C47—N7—C46—S1 | −1.9 (3) |
C2—C1—C4—C9 | −44.2 (2) | C47—N7—C46—S2 | −179.54 (14) |
C2—C3—C10—C11 | 56.2 (2) | C47—N7—C51—C52 | −91.5 (3) |
C2—C3—C10—C15 | −125.2 (2) | C47—N7—C51A—C52A | 100.2 (6) |
C3—N2—B1—N4 | 104.30 (18) | C47—C48—C49—C50 | −173.42 (19) |
C3—N2—B1—N6 | −136.19 (16) | B1—N2—C3—C2 | −174.41 (15) |
C3—C10—C11—C12 | 177.43 (16) | B1—N2—C3—C10 | 2.9 (3) |
C3—C10—C15—C14 | −178.67 (16) | B1—N4—C18—C17 | −179.77 (16) |
C4—C1—C2—C3 | −175.60 (16) | B1—N4—C18—C25 | −1.4 (3) |
C4—C5—C6—C7 | −0.5 (3) | B1—N6—C33—C32 | −174.43 (15) |
C5—C4—C9—C8 | 0.5 (2) | B1—N6—C33—C40 | 3.1 (2) |
C5—C6—C7—C8 | 0.5 (3) | C51—N7—C46—S1 | 168.49 (17) |
C6—C7—C8—C9 | −0.1 (3) | C51—N7—C46—S2 | −9.1 (3) |
C7—C8—C9—C4 | −0.5 (3) | C51—N7—C47—C48 | 105.7 (2) |
C9—C4—C5—C6 | 0.0 (3) | C51—C52—C53—C54 | 66.4 (5) |
C10—C11—C12—C13 | 1.4 (3) | C51A—N7—C46—S1 | −147.1 (4) |
C11—C10—C15—C14 | −0.1 (3) | C51A—N7—C46—S2 | 35.2 (4) |
C11—C12—C13—C14 | −0.4 (3) | C51A—N7—C47—C48 | 62.2 (4) |
C12—C13—C14—C15 | −0.9 (3) | C51A—C52A—C53A—C54A | −59.9 (16) |
C13—C14—C15—C10 | 1.1 (3) | | |
Selected bond lengths (Å) and τ values
in polymorphs 1a and 1b top | 1a | 1b |
Co—N1 | 2.0901 (14) | 2.1371 (14) |
Co—N3 | 2.0733 (15) | 2.0804 (13) |
Co—N5 | 2.1774 (14) | 2.1480 (13) |
Co—S1 | 2.4449 (5) | 2.4030 (5) |
Co—S2 | 2.3531 (5) | 2.3892 (5) |
τ | 0.49 | 0.07 |
Torsion angles (°) of the butyl chains in polymorphs 1a and 1b top | 1a | 1b |
C46—N7—C47—C48 | -106.3 (3) | -83.4 (2) |
C46—N7—C51—C52 | -136.1 (5) | 97.6 (3) |
C46—N7—C47A—C48A | -129.7 (9) | – |
C46—N7—C51A—C52A | -145.3 (11) | -111.6 (6) |
C47—C48—C49—C50 | 164.6 (3) | -173.4 (2) |
C47A—C48A—C49A—C50A | -170.9 (13) | – |
C51—C52—C53—C54 | 174.7 (6) | 66.4 (5) |
C51A—C52A—C53A—C54A | -171.2 (17) | -59.9 (13) |
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