Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229624004224/zo3044sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229624004224/zo3044NiPhTPYsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229624004224/zo3044MnMeOTPYsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229624004224/zo3044MnPhTPYsup4.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229624004224/zo3044sup5.pdf |
CCDC references: 2331329; 2331330; 2331331
[Mn(C22H17N3O)2](ClO4)2 | Z = 2 |
Mr = 932.61 | F(000) = 958 |
Triclinic, P1 | Dx = 1.505 Mg m−3 |
a = 8.93282 (10) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.32698 (13) Å | Cell parameters from 44860 reflections |
c = 18.86081 (19) Å | θ = 2.6–34.1° |
α = 89.8757 (8)° | µ = 0.52 mm−1 |
β = 85.6122 (8)° | T = 100 K |
γ = 83.5667 (9)° | Block, light yellow |
V = 2057.68 (4) Å3 | 0.15 × 0.10 × 0.08 mm |
Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector | 10630 independent reflections |
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Mo) X-ray Source | 9347 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.029 |
Detector resolution: 10.0000 pixels mm-1 | θmax = 28.7°, θmin = 2.5° |
ω scans | h = −12→12 |
Absorption correction: gaussian (CrysAlis PRO; Rigaku OD, 2022) | k = −16→16 |
Tmin = 0.662, Tmax = 1.000 | l = −25→25 |
57826 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0393P)2 + 0.9933P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
10630 reflections | Δρmax = 0.49 e Å−3 |
570 parameters | Δρmin = −0.42 e Å−3 |
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. |
Refinement. Single crystals suitable for X-ray analysis were obtained by slow evaporation from acetonitrile using diethyl ether as antisolvent. Diffraction data for all the compounds were collected at room temperature on a Rigaku Synergy S diffractometer using photonjet microfocus source Mo Kα (λ = 0.71073 Å) radiation. The unit-cell parameters were determined using all reflections with CrysAlis PRO software (Agilent, 2014). Data integration and scaling were performed using CrysAlis PRO software (Agilent, 2014). The structures were solved and refined with SHELXT (Sheldrick, 2015a) and SHELXL (Sheldrick, 2015b) software, respectively, including in OLEX2 (Dolomanov et al., 2009). In all cases, non-H atoms were clearly resolved and full-matrix least-squares refinement with anisotropic displacement parameters was performed. In addition, the H atoms were stereochemically positioned and refined using the riding model (Sheldrick, 2008). The Mn compound [which one?] was refined using the SQUEEZE routine (Spek, 2015) in PLATON (Spek, 2020) to decrease the contribution of the disordered solvent (water molecule) to calculate the structure factors and improve the refinement values. Displacement ellipsoid plots for all structures were prepared with DIAMOND (Brandenburg et al., 2006). MERCURY were used for the preparation of artwork (Macrae et al., 2020). The CIF file of the complexes was deposited in the Cambridge Structural Data Base under the codes CCDC 2331329-2331331. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.84071 (2) | 0.20014 (2) | 0.74163 (2) | 0.01322 (5) | |
Cl2 | 0.27866 (3) | 0.73931 (2) | 0.86546 (2) | 0.01663 (7) | |
Cl1 | 0.44773 (4) | 0.27267 (3) | 0.51211 (2) | 0.01862 (7) | |
O2 | 1.04363 (12) | 0.38092 (8) | 0.19702 (5) | 0.0220 (2) | |
O1 | 0.61146 (13) | −0.26205 (9) | 1.20844 (5) | 0.0259 (2) | |
O8 | 0.13467 (11) | 0.80637 (8) | 0.87487 (5) | 0.0219 (2) | |
O7 | 0.32762 (13) | 0.73117 (9) | 0.79090 (5) | 0.0267 (2) | |
O9 | 0.26411 (13) | 0.63223 (8) | 0.89400 (6) | 0.0276 (2) | |
O10 | 0.38971 (12) | 0.78935 (9) | 0.90230 (6) | 0.0276 (2) | |
N4 | 0.71778 (12) | 0.36568 (9) | 0.72566 (6) | 0.0156 (2) | |
N5 | 0.90456 (12) | 0.25287 (8) | 0.63304 (5) | 0.0136 (2) | |
N1 | 0.94458 (12) | 0.27627 (9) | 0.83268 (6) | 0.0147 (2) | |
N2 | 0.78219 (12) | 0.11127 (8) | 0.83983 (5) | 0.01317 (19) | |
N6 | 1.01949 (12) | 0.06923 (9) | 0.69056 (6) | 0.0147 (2) | |
O5 | 0.38629 (13) | 0.17013 (9) | 0.52369 (7) | 0.0359 (3) | |
N3 | 0.68141 (12) | 0.07699 (9) | 0.71536 (5) | 0.0147 (2) | |
O3 | 0.50570 (17) | 0.27764 (11) | 0.43929 (6) | 0.0432 (3) | |
O6 | 0.33038 (15) | 0.36195 (10) | 0.52570 (7) | 0.0391 (3) | |
O4 | 0.56453 (17) | 0.27922 (11) | 0.55862 (8) | 0.0502 (4) | |
C11 | 0.64293 (14) | 0.00707 (10) | 0.76733 (6) | 0.0135 (2) | |
C10 | 0.69668 (13) | 0.02828 (10) | 0.83820 (6) | 0.0128 (2) | |
C6 | 0.83885 (13) | 0.13535 (10) | 0.90126 (6) | 0.0131 (2) | |
C5 | 0.92485 (14) | 0.23205 (10) | 0.89801 (6) | 0.0134 (2) | |
C7 | 0.81556 (14) | 0.07495 (10) | 0.96256 (6) | 0.0138 (2) | |
H7 | 0.860232 | 0.092242 | 1.004630 | 0.017* | |
C27 | 0.83919 (14) | 0.34763 (10) | 0.60817 (6) | 0.0133 (2) | |
C19 | 0.64295 (15) | −0.19800 (11) | 1.15164 (7) | 0.0171 (2) | |
C37 | 0.99495 (14) | 0.33887 (10) | 0.41620 (6) | 0.0153 (2) | |
C12 | 0.56352 (14) | −0.08050 (10) | 0.75412 (7) | 0.0161 (2) | |
H12 | 0.535070 | −0.127319 | 0.791654 | 0.019* | |
C4 | 0.97795 (15) | 0.27649 (10) | 0.95764 (7) | 0.0168 (2) | |
H4 | 0.962878 | 0.244320 | 1.003077 | 0.020* | |
C16 | 0.69693 (14) | −0.07642 (10) | 1.02729 (6) | 0.0130 (2) | |
C9 | 0.66467 (14) | −0.03336 (10) | 0.89824 (6) | 0.0135 (2) | |
H9 | 0.601377 | −0.090036 | 0.895816 | 0.016* | |
C26 | 0.72713 (14) | 0.40883 (10) | 0.65978 (6) | 0.0138 (2) | |
C18 | 0.72148 (14) | −0.10719 (10) | 1.15389 (6) | 0.0157 (2) | |
H18 | 0.757195 | −0.085778 | 1.197323 | 0.019* | |
C8 | 0.72601 (13) | −0.01167 (10) | 0.96239 (6) | 0.0126 (2) | |
C29 | 0.96743 (14) | 0.31363 (10) | 0.49237 (6) | 0.0146 (2) | |
C17 | 0.74767 (14) | −0.04769 (10) | 1.09233 (6) | 0.0152 (2) | |
H17 | 0.801575 | 0.014272 | 1.094492 | 0.018* | |
C31 | 1.00055 (14) | 0.18737 (10) | 0.58924 (6) | 0.0138 (2) | |
C13 | 0.52625 (15) | −0.09870 (11) | 0.68529 (7) | 0.0181 (2) | |
H13 | 0.473910 | −0.159061 | 0.674975 | 0.022* | |
C25 | 0.63432 (15) | 0.50116 (10) | 0.64175 (7) | 0.0174 (2) | |
H25 | 0.641606 | 0.529612 | 0.594921 | 0.021* | |
C40 | 1.03554 (15) | 0.36605 (10) | 0.26877 (6) | 0.0163 (2) | |
C32 | 1.05891 (14) | 0.08155 (10) | 0.62066 (6) | 0.0141 (2) | |
C15 | 0.64223 (15) | 0.05958 (11) | 0.64927 (7) | 0.0180 (2) | |
H15 | 0.667643 | 0.109285 | 0.612925 | 0.022* | |
C28 | 0.87030 (14) | 0.38170 (10) | 0.53876 (6) | 0.0151 (2) | |
H28 | 0.825980 | 0.450420 | 0.523158 | 0.018* | |
C39 | 0.90529 (15) | 0.41530 (11) | 0.30658 (7) | 0.0182 (2) | |
H39 | 0.830398 | 0.458098 | 0.282286 | 0.022* | |
C2 | 1.07214 (15) | 0.41551 (11) | 0.88302 (7) | 0.0193 (3) | |
H2 | 1.122655 | 0.479037 | 0.876440 | 0.023* | |
C30 | 1.03336 (14) | 0.21484 (10) | 0.51903 (7) | 0.0155 (2) | |
H30 | 1.100492 | 0.166791 | 0.488934 | 0.019* | |
C38 | 0.88507 (15) | 0.40186 (11) | 0.37951 (7) | 0.0176 (2) | |
H38 | 0.796116 | 0.435527 | 0.404955 | 0.021* | |
C33 | 1.14230 (15) | −0.00195 (11) | 0.58015 (7) | 0.0183 (2) | |
H33 | 1.171358 | 0.009268 | 0.531410 | 0.022* | |
C21 | 0.61682 (16) | −0.16794 (11) | 1.02645 (7) | 0.0185 (2) | |
H21 | 0.580120 | −0.189282 | 0.983226 | 0.022* | |
C42 | 1.12654 (15) | 0.29330 (11) | 0.37761 (7) | 0.0175 (2) | |
H42 | 1.203204 | 0.252366 | 0.401874 | 0.021* | |
C24 | 0.53044 (16) | 0.55112 (11) | 0.69369 (7) | 0.0204 (3) | |
H24 | 0.464647 | 0.613768 | 0.682531 | 0.024* | |
C20 | 0.59031 (17) | −0.22761 (11) | 1.08730 (7) | 0.0215 (3) | |
H20 | 0.535822 | −0.289320 | 1.085407 | 0.026* | |
C41 | 1.14771 (15) | 0.30650 (11) | 0.30466 (7) | 0.0178 (2) | |
H41 | 1.238156 | 0.275115 | 0.279320 | 0.021* | |
C34 | 1.18242 (15) | −0.10165 (11) | 0.61178 (7) | 0.0196 (3) | |
H34 | 1.238636 | −0.159698 | 0.584944 | 0.023* | |
C1 | 1.01489 (15) | 0.36672 (10) | 0.82639 (7) | 0.0175 (2) | |
H1 | 1.026035 | 0.399002 | 0.780781 | 0.021* | |
C14 | 0.56647 (15) | −0.02757 (12) | 0.63175 (7) | 0.0195 (3) | |
H14 | 0.542599 | −0.038407 | 0.584233 | 0.023* | |
C36 | 1.05989 (15) | −0.02783 (11) | 0.72056 (7) | 0.0173 (2) | |
H36 | 1.032639 | −0.036698 | 0.769740 | 0.021* | |
C22 | 0.61991 (16) | 0.41617 (11) | 0.77528 (7) | 0.0203 (3) | |
H22 | 0.616045 | 0.387219 | 0.822024 | 0.024* | |
C23 | 0.52374 (16) | 0.50879 (11) | 0.76177 (8) | 0.0223 (3) | |
H23 | 0.454971 | 0.542401 | 0.798274 | 0.027* | |
C35 | 1.13919 (15) | −0.11532 (11) | 0.68323 (7) | 0.0192 (3) | |
H35 | 1.163471 | −0.183154 | 0.705976 | 0.023* | |
C3 | 1.05346 (15) | 0.36884 (11) | 0.94953 (7) | 0.0190 (3) | |
H3 | 1.092140 | 0.399852 | 0.989435 | 0.023* | |
C44 | 0.66597 (17) | −0.23664 (13) | 1.27535 (7) | 0.0239 (3) | |
H44A | 0.776624 | −0.242867 | 1.270677 | 0.036* | |
H44B | 0.632577 | −0.287756 | 1.311509 | 0.036* | |
H44C | 0.625952 | −0.161930 | 1.289560 | 0.036* | |
C43 | 1.16290 (18) | 0.31801 (13) | 0.15575 (7) | 0.0268 (3) | |
H43A | 1.151537 | 0.331365 | 0.105101 | 0.040* | |
H43B | 1.158859 | 0.240288 | 0.165714 | 0.040* | |
H43C | 1.260281 | 0.339129 | 0.168069 | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.01649 (10) | 0.01185 (9) | 0.01116 (9) | −0.00133 (7) | −0.00057 (7) | 0.00234 (6) |
Cl2 | 0.02027 (15) | 0.01290 (13) | 0.01747 (14) | −0.00286 (11) | −0.00480 (11) | 0.00059 (10) |
Cl1 | 0.01966 (15) | 0.01990 (15) | 0.01669 (14) | −0.00161 (11) | −0.00475 (11) | 0.00003 (11) |
O2 | 0.0324 (5) | 0.0215 (5) | 0.0112 (4) | 0.0017 (4) | −0.0022 (4) | 0.0034 (3) |
O1 | 0.0392 (6) | 0.0274 (5) | 0.0136 (4) | −0.0154 (5) | −0.0022 (4) | 0.0073 (4) |
O8 | 0.0209 (5) | 0.0186 (5) | 0.0260 (5) | −0.0003 (4) | −0.0035 (4) | −0.0028 (4) |
O7 | 0.0361 (6) | 0.0235 (5) | 0.0181 (5) | 0.0055 (4) | −0.0003 (4) | 0.0000 (4) |
O9 | 0.0326 (6) | 0.0167 (5) | 0.0349 (6) | −0.0062 (4) | −0.0066 (5) | 0.0092 (4) |
O10 | 0.0264 (5) | 0.0257 (5) | 0.0331 (6) | −0.0076 (4) | −0.0118 (4) | −0.0033 (4) |
N4 | 0.0178 (5) | 0.0138 (5) | 0.0150 (5) | −0.0007 (4) | −0.0001 (4) | 0.0015 (4) |
N5 | 0.0144 (5) | 0.0129 (5) | 0.0134 (5) | −0.0009 (4) | −0.0019 (4) | 0.0014 (4) |
N1 | 0.0165 (5) | 0.0127 (5) | 0.0151 (5) | −0.0018 (4) | −0.0016 (4) | 0.0022 (4) |
N2 | 0.0144 (5) | 0.0126 (5) | 0.0125 (5) | −0.0011 (4) | −0.0009 (4) | 0.0006 (4) |
N6 | 0.0153 (5) | 0.0140 (5) | 0.0150 (5) | −0.0012 (4) | −0.0029 (4) | 0.0024 (4) |
O5 | 0.0305 (6) | 0.0240 (6) | 0.0554 (8) | −0.0103 (5) | −0.0075 (5) | −0.0013 (5) |
N3 | 0.0154 (5) | 0.0159 (5) | 0.0128 (5) | −0.0004 (4) | −0.0025 (4) | 0.0024 (4) |
O3 | 0.0614 (9) | 0.0381 (7) | 0.0224 (6) | 0.0185 (6) | 0.0113 (5) | 0.0058 (5) |
O6 | 0.0411 (7) | 0.0273 (6) | 0.0439 (7) | 0.0083 (5) | 0.0111 (5) | −0.0045 (5) |
O4 | 0.0582 (9) | 0.0434 (8) | 0.0599 (9) | −0.0259 (7) | −0.0461 (7) | 0.0206 (6) |
C11 | 0.0131 (5) | 0.0139 (5) | 0.0129 (5) | 0.0005 (4) | −0.0012 (4) | 0.0003 (4) |
C10 | 0.0129 (5) | 0.0123 (5) | 0.0127 (5) | 0.0007 (4) | −0.0006 (4) | −0.0001 (4) |
C6 | 0.0135 (5) | 0.0118 (5) | 0.0138 (5) | −0.0004 (4) | −0.0006 (4) | −0.0001 (4) |
C5 | 0.0138 (5) | 0.0117 (5) | 0.0142 (5) | −0.0003 (4) | −0.0003 (4) | 0.0015 (4) |
C7 | 0.0159 (6) | 0.0139 (5) | 0.0120 (5) | −0.0018 (4) | −0.0018 (4) | 0.0003 (4) |
C27 | 0.0143 (5) | 0.0123 (5) | 0.0135 (5) | −0.0016 (4) | −0.0019 (4) | 0.0007 (4) |
C19 | 0.0209 (6) | 0.0172 (6) | 0.0127 (5) | −0.0023 (5) | 0.0012 (5) | 0.0035 (4) |
C37 | 0.0170 (6) | 0.0164 (6) | 0.0127 (5) | −0.0027 (5) | −0.0011 (4) | 0.0023 (4) |
C12 | 0.0165 (6) | 0.0161 (6) | 0.0157 (6) | −0.0019 (5) | −0.0013 (4) | 0.0002 (4) |
C4 | 0.0197 (6) | 0.0160 (6) | 0.0153 (6) | −0.0035 (5) | −0.0026 (5) | 0.0018 (4) |
C16 | 0.0143 (5) | 0.0120 (5) | 0.0123 (5) | −0.0003 (4) | 0.0003 (4) | 0.0020 (4) |
C9 | 0.0146 (5) | 0.0119 (5) | 0.0143 (5) | −0.0020 (4) | −0.0010 (4) | 0.0004 (4) |
C26 | 0.0156 (6) | 0.0120 (5) | 0.0139 (5) | −0.0020 (4) | −0.0011 (4) | 0.0004 (4) |
C18 | 0.0175 (6) | 0.0170 (6) | 0.0125 (5) | −0.0013 (5) | −0.0014 (4) | 0.0008 (4) |
C8 | 0.0131 (5) | 0.0116 (5) | 0.0125 (5) | 0.0011 (4) | 0.0008 (4) | 0.0009 (4) |
C29 | 0.0148 (5) | 0.0169 (6) | 0.0125 (5) | −0.0029 (4) | −0.0009 (4) | 0.0025 (4) |
C17 | 0.0173 (6) | 0.0140 (6) | 0.0146 (6) | −0.0018 (4) | −0.0019 (4) | 0.0011 (4) |
C31 | 0.0139 (5) | 0.0136 (5) | 0.0137 (5) | −0.0010 (4) | −0.0017 (4) | 0.0010 (4) |
C13 | 0.0179 (6) | 0.0180 (6) | 0.0187 (6) | −0.0026 (5) | −0.0033 (5) | −0.0023 (5) |
C25 | 0.0204 (6) | 0.0144 (6) | 0.0168 (6) | 0.0009 (5) | −0.0015 (5) | 0.0022 (4) |
C40 | 0.0228 (6) | 0.0148 (6) | 0.0120 (5) | −0.0048 (5) | −0.0019 (5) | 0.0027 (4) |
C32 | 0.0132 (5) | 0.0138 (5) | 0.0153 (5) | −0.0009 (4) | −0.0029 (4) | 0.0017 (4) |
C15 | 0.0192 (6) | 0.0213 (6) | 0.0137 (6) | −0.0016 (5) | −0.0030 (5) | 0.0028 (5) |
C28 | 0.0175 (6) | 0.0137 (5) | 0.0142 (5) | −0.0009 (4) | −0.0019 (4) | 0.0030 (4) |
C39 | 0.0206 (6) | 0.0164 (6) | 0.0175 (6) | 0.0001 (5) | −0.0047 (5) | 0.0053 (5) |
C2 | 0.0214 (6) | 0.0137 (6) | 0.0238 (6) | −0.0046 (5) | −0.0042 (5) | 0.0033 (5) |
C30 | 0.0148 (6) | 0.0170 (6) | 0.0143 (6) | 0.0003 (4) | −0.0009 (4) | 0.0009 (4) |
C38 | 0.0192 (6) | 0.0165 (6) | 0.0163 (6) | 0.0004 (5) | −0.0008 (5) | 0.0025 (5) |
C33 | 0.0190 (6) | 0.0179 (6) | 0.0171 (6) | 0.0008 (5) | −0.0013 (5) | 0.0006 (5) |
C21 | 0.0240 (6) | 0.0193 (6) | 0.0134 (6) | −0.0069 (5) | −0.0027 (5) | 0.0010 (5) |
C42 | 0.0160 (6) | 0.0208 (6) | 0.0157 (6) | −0.0005 (5) | −0.0025 (4) | 0.0033 (5) |
C24 | 0.0208 (6) | 0.0161 (6) | 0.0228 (6) | 0.0033 (5) | 0.0004 (5) | 0.0015 (5) |
C20 | 0.0293 (7) | 0.0203 (6) | 0.0172 (6) | −0.0126 (5) | −0.0020 (5) | 0.0027 (5) |
C41 | 0.0182 (6) | 0.0211 (6) | 0.0137 (6) | −0.0015 (5) | 0.0001 (4) | 0.0013 (5) |
C34 | 0.0178 (6) | 0.0155 (6) | 0.0249 (7) | 0.0017 (5) | −0.0032 (5) | −0.0013 (5) |
C1 | 0.0204 (6) | 0.0143 (6) | 0.0181 (6) | −0.0030 (5) | −0.0015 (5) | 0.0042 (5) |
C14 | 0.0198 (6) | 0.0248 (7) | 0.0142 (6) | −0.0014 (5) | −0.0046 (5) | −0.0010 (5) |
C36 | 0.0171 (6) | 0.0168 (6) | 0.0184 (6) | −0.0024 (5) | −0.0032 (5) | 0.0049 (5) |
C22 | 0.0246 (7) | 0.0186 (6) | 0.0161 (6) | 0.0001 (5) | 0.0042 (5) | 0.0030 (5) |
C23 | 0.0236 (7) | 0.0183 (6) | 0.0226 (7) | 0.0033 (5) | 0.0060 (5) | 0.0001 (5) |
C35 | 0.0170 (6) | 0.0147 (6) | 0.0264 (7) | −0.0011 (5) | −0.0055 (5) | 0.0045 (5) |
C3 | 0.0219 (6) | 0.0169 (6) | 0.0196 (6) | −0.0049 (5) | −0.0063 (5) | 0.0002 (5) |
C44 | 0.0294 (7) | 0.0297 (7) | 0.0127 (6) | −0.0048 (6) | −0.0005 (5) | 0.0042 (5) |
C43 | 0.0310 (8) | 0.0343 (8) | 0.0137 (6) | 0.0001 (6) | 0.0017 (5) | 0.0008 (5) |
Mn1—N4 | 2.2375 (11) | C9—C8 | 1.4042 (17) |
Mn1—N5 | 2.2002 (10) | C26—C25 | 1.3886 (17) |
Mn1—N1 | 2.2666 (11) | C18—H18 | 0.9500 |
Mn1—N2 | 2.2081 (10) | C18—C17 | 1.3906 (17) |
Mn1—N6 | 2.2970 (11) | C29—C28 | 1.3951 (17) |
Mn1—N3 | 2.2738 (11) | C29—C30 | 1.4017 (17) |
Cl2—O8 | 1.4480 (10) | C17—H17 | 0.9500 |
Cl2—O7 | 1.4406 (10) | C31—C32 | 1.4886 (17) |
Cl2—O9 | 1.4401 (10) | C31—C30 | 1.3838 (17) |
Cl2—O10 | 1.4462 (10) | C13—H13 | 0.9500 |
Cl1—O5 | 1.4432 (12) | C13—C14 | 1.3888 (19) |
Cl1—O3 | 1.4338 (12) | C25—H25 | 0.9500 |
Cl1—O6 | 1.4413 (12) | C25—C24 | 1.3911 (18) |
Cl1—O4 | 1.4226 (12) | C40—C39 | 1.3956 (19) |
O2—C40 | 1.3626 (15) | C40—C41 | 1.3920 (18) |
O2—C43 | 1.4259 (17) | C32—C33 | 1.3939 (18) |
O1—C19 | 1.3602 (15) | C15—H15 | 0.9500 |
O1—C44 | 1.4344 (17) | C15—C14 | 1.3856 (19) |
N4—C26 | 1.3509 (16) | C28—H28 | 0.9500 |
N4—C22 | 1.3353 (17) | C39—H39 | 0.9500 |
N5—C27 | 1.3461 (15) | C39—C38 | 1.3856 (18) |
N5—C31 | 1.3450 (16) | C2—H2 | 0.9500 |
N1—C5 | 1.3535 (15) | C2—C1 | 1.3855 (19) |
N1—C1 | 1.3403 (16) | C2—C3 | 1.3852 (18) |
N2—C10 | 1.3453 (16) | C30—H30 | 0.9500 |
N2—C6 | 1.3459 (15) | C38—H38 | 0.9500 |
N6—C32 | 1.3509 (16) | C33—H33 | 0.9500 |
N6—C36 | 1.3467 (16) | C33—C34 | 1.3877 (18) |
N3—C11 | 1.3537 (15) | C21—H21 | 0.9500 |
N3—C15 | 1.3443 (16) | C21—C20 | 1.3812 (18) |
C11—C10 | 1.4878 (16) | C42—H42 | 0.9500 |
C11—C12 | 1.3894 (17) | C42—C41 | 1.3863 (17) |
C10—C9 | 1.3916 (16) | C24—H24 | 0.9500 |
C6—C5 | 1.4873 (17) | C24—C23 | 1.3846 (19) |
C6—C7 | 1.3887 (16) | C20—H20 | 0.9500 |
C5—C4 | 1.3902 (17) | C41—H41 | 0.9500 |
C7—H7 | 0.9500 | C34—H34 | 0.9500 |
C7—C8 | 1.4042 (17) | C34—C35 | 1.3882 (19) |
C27—C26 | 1.4845 (17) | C1—H1 | 0.9500 |
C27—C28 | 1.3912 (16) | C14—H14 | 0.9500 |
C19—C18 | 1.3883 (18) | C36—H36 | 0.9500 |
C19—C20 | 1.3982 (18) | C36—C35 | 1.3844 (19) |
C37—C29 | 1.4773 (16) | C22—H22 | 0.9500 |
C37—C38 | 1.4057 (17) | C22—C23 | 1.3853 (19) |
C37—C42 | 1.3964 (18) | C23—H23 | 0.9500 |
C12—H12 | 0.9500 | C35—H35 | 0.9500 |
C12—C13 | 1.3895 (17) | C3—H3 | 0.9500 |
C4—H4 | 0.9500 | C44—H44A | 0.9800 |
C4—C3 | 1.3892 (18) | C44—H44B | 0.9800 |
C16—C8 | 1.4820 (16) | C44—H44C | 0.9800 |
C16—C17 | 1.3995 (17) | C43—H43A | 0.9800 |
C16—C21 | 1.4028 (17) | C43—H43B | 0.9800 |
C9—H9 | 0.9500 | C43—H43C | 0.9800 |
N4—Mn1—N1 | 86.42 (4) | C28—C29—C30 | 117.88 (11) |
N4—Mn1—N6 | 143.89 (4) | C30—C29—C37 | 119.53 (11) |
N4—Mn1—N3 | 106.58 (4) | C16—C17—H17 | 119.0 |
N5—Mn1—N4 | 72.05 (4) | C18—C17—C16 | 121.92 (12) |
N5—Mn1—N1 | 117.76 (4) | C18—C17—H17 | 119.0 |
N5—Mn1—N2 | 167.42 (4) | N5—C31—C32 | 114.98 (10) |
N5—Mn1—N6 | 72.00 (4) | N5—C31—C30 | 121.56 (11) |
N5—Mn1—N3 | 98.94 (4) | C30—C31—C32 | 123.34 (11) |
N1—Mn1—N6 | 107.36 (4) | C12—C13—H13 | 120.4 |
N1—Mn1—N3 | 143.30 (4) | C14—C13—C12 | 119.18 (12) |
N2—Mn1—N4 | 118.25 (4) | C14—C13—H13 | 120.4 |
N2—Mn1—N1 | 71.82 (4) | C26—C25—H25 | 120.7 |
N2—Mn1—N6 | 97.84 (4) | C26—C25—C24 | 118.64 (12) |
N2—Mn1—N3 | 71.82 (4) | C24—C25—H25 | 120.7 |
N3—Mn1—N6 | 82.42 (4) | O2—C40—C39 | 116.01 (11) |
O7—Cl2—O8 | 109.56 (6) | O2—C40—C41 | 124.01 (12) |
O7—Cl2—O10 | 108.81 (7) | C41—C40—C39 | 119.98 (12) |
O9—Cl2—O8 | 109.74 (6) | N6—C32—C31 | 115.67 (11) |
O9—Cl2—O7 | 109.98 (7) | N6—C32—C33 | 121.80 (11) |
O9—Cl2—O10 | 109.41 (7) | C33—C32—C31 | 122.45 (11) |
O10—Cl2—O8 | 109.33 (6) | N3—C15—H15 | 118.5 |
O3—Cl1—O5 | 108.85 (8) | N3—C15—C14 | 122.99 (12) |
O3—Cl1—O6 | 108.44 (7) | C14—C15—H15 | 118.5 |
O6—Cl1—O5 | 109.88 (8) | C27—C28—C29 | 119.13 (11) |
O4—Cl1—O5 | 108.68 (8) | C27—C28—H28 | 120.4 |
O4—Cl1—O3 | 110.75 (10) | C29—C28—H28 | 120.4 |
O4—Cl1—O6 | 110.22 (9) | C40—C39—H39 | 120.0 |
C40—O2—C43 | 117.30 (11) | C38—C39—C40 | 120.08 (12) |
C19—O1—C44 | 118.33 (11) | C38—C39—H39 | 120.0 |
C26—N4—Mn1 | 117.98 (8) | C1—C2—H2 | 121.0 |
C22—N4—Mn1 | 122.76 (9) | C3—C2—H2 | 121.0 |
C22—N4—C26 | 118.57 (11) | C3—C2—C1 | 117.97 (12) |
C27—N5—Mn1 | 120.08 (8) | C29—C30—H30 | 120.0 |
C31—N5—Mn1 | 120.43 (8) | C31—C30—C29 | 119.93 (11) |
C31—N5—C27 | 119.31 (10) | C31—C30—H30 | 120.0 |
C5—N1—Mn1 | 117.79 (8) | C37—C38—H38 | 119.7 |
C1—N1—Mn1 | 123.69 (8) | C39—C38—C37 | 120.61 (12) |
C1—N1—C5 | 118.35 (11) | C39—C38—H38 | 119.7 |
C10—N2—Mn1 | 120.46 (8) | C32—C33—H33 | 120.4 |
C10—N2—C6 | 119.11 (10) | C34—C33—C32 | 119.28 (12) |
C6—N2—Mn1 | 120.32 (8) | C34—C33—H33 | 120.4 |
C32—N6—Mn1 | 116.15 (8) | C16—C21—H21 | 119.4 |
C36—N6—Mn1 | 123.91 (9) | C20—C21—C16 | 121.23 (12) |
C36—N6—C32 | 118.19 (11) | C20—C21—H21 | 119.4 |
C11—N3—Mn1 | 117.30 (8) | C37—C42—H42 | 119.3 |
C15—N3—Mn1 | 123.53 (9) | C41—C42—C37 | 121.41 (12) |
C15—N3—C11 | 118.41 (11) | C41—C42—H42 | 119.3 |
N3—C11—C10 | 115.35 (11) | C25—C24—H24 | 120.3 |
N3—C11—C12 | 121.82 (11) | C23—C24—C25 | 119.45 (12) |
C12—C11—C10 | 122.80 (11) | C23—C24—H24 | 120.3 |
N2—C10—C11 | 114.65 (10) | C19—C20—H20 | 119.7 |
N2—C10—C9 | 121.95 (11) | C21—C20—C19 | 120.58 (12) |
C9—C10—C11 | 123.38 (11) | C21—C20—H20 | 119.7 |
N2—C6—C5 | 114.61 (10) | C40—C41—H41 | 120.2 |
N2—C6—C7 | 121.95 (11) | C42—C41—C40 | 119.56 (12) |
C7—C6—C5 | 123.43 (11) | C42—C41—H41 | 120.2 |
N1—C5—C6 | 115.12 (11) | C33—C34—H34 | 120.5 |
N1—C5—C4 | 121.87 (11) | C33—C34—C35 | 119.02 (12) |
C4—C5—C6 | 122.99 (11) | C35—C34—H34 | 120.5 |
C6—C7—H7 | 120.0 | N1—C1—C2 | 123.33 (12) |
C6—C7—C8 | 120.03 (11) | N1—C1—H1 | 118.3 |
C8—C7—H7 | 120.0 | C2—C1—H1 | 118.3 |
N5—C27—C26 | 114.31 (10) | C13—C14—H14 | 120.8 |
N5—C27—C28 | 122.14 (11) | C15—C14—C13 | 118.43 (12) |
C28—C27—C26 | 123.49 (11) | C15—C14—H14 | 120.8 |
O1—C19—C18 | 124.66 (12) | N6—C36—H36 | 118.4 |
O1—C19—C20 | 116.13 (12) | N6—C36—C35 | 123.19 (12) |
C18—C19—C20 | 119.20 (11) | C35—C36—H36 | 118.4 |
C38—C37—C29 | 121.13 (11) | N4—C22—H22 | 118.5 |
C42—C37—C29 | 120.39 (11) | N4—C22—C23 | 123.05 (12) |
C42—C37—C38 | 118.29 (11) | C23—C22—H22 | 118.5 |
C11—C12—H12 | 120.4 | C24—C23—C22 | 118.28 (12) |
C11—C12—C13 | 119.14 (12) | C24—C23—H23 | 120.9 |
C13—C12—H12 | 120.4 | C22—C23—H23 | 120.9 |
C5—C4—H4 | 120.6 | C34—C35—H35 | 120.8 |
C3—C4—C5 | 118.74 (12) | C36—C35—C34 | 118.49 (12) |
C3—C4—H4 | 120.6 | C36—C35—H35 | 120.8 |
C17—C16—C8 | 120.96 (11) | C4—C3—H3 | 120.1 |
C17—C16—C21 | 117.28 (11) | C2—C3—C4 | 119.72 (12) |
C21—C16—C8 | 121.75 (11) | C2—C3—H3 | 120.1 |
C10—C9—H9 | 120.0 | O1—C44—H44A | 109.5 |
C10—C9—C8 | 119.92 (11) | O1—C44—H44B | 109.5 |
C8—C9—H9 | 120.0 | O1—C44—H44C | 109.5 |
N4—C26—C27 | 114.89 (11) | H44A—C44—H44B | 109.5 |
N4—C26—C25 | 121.96 (11) | H44A—C44—H44C | 109.5 |
C25—C26—C27 | 123.11 (11) | H44B—C44—H44C | 109.5 |
C19—C18—H18 | 120.1 | O2—C43—H43A | 109.5 |
C19—C18—C17 | 119.77 (12) | O2—C43—H43B | 109.5 |
C17—C18—H18 | 120.1 | O2—C43—H43C | 109.5 |
C7—C8—C16 | 121.30 (11) | H43A—C43—H43B | 109.5 |
C9—C8—C7 | 116.97 (11) | H43A—C43—H43C | 109.5 |
C9—C8—C16 | 121.73 (11) | H43B—C43—H43C | 109.5 |
C28—C29—C37 | 122.47 (11) | ||
Mn1—N4—C26—C27 | −9.44 (14) | C27—N5—C31—C30 | −0.27 (18) |
Mn1—N4—C26—C25 | 168.29 (10) | C27—C26—C25—C24 | 178.49 (12) |
Mn1—N4—C22—C23 | −168.08 (11) | C19—C18—C17—C16 | 0.04 (19) |
Mn1—N5—C27—C26 | 0.53 (14) | C37—C29—C28—C27 | 174.07 (11) |
Mn1—N5—C27—C28 | −176.72 (9) | C37—C29—C30—C31 | −175.90 (11) |
Mn1—N5—C31—C32 | −1.14 (14) | C37—C42—C41—C40 | −0.2 (2) |
Mn1—N5—C31—C30 | 174.88 (9) | C12—C11—C10—N2 | 174.79 (11) |
Mn1—N1—C5—C6 | 1.48 (14) | C12—C11—C10—C9 | −3.98 (19) |
Mn1—N1—C5—C4 | −176.77 (9) | C12—C13—C14—C15 | −0.2 (2) |
Mn1—N1—C1—C2 | 177.01 (10) | C16—C21—C20—C19 | 0.0 (2) |
Mn1—N2—C10—C11 | −2.43 (14) | C26—N4—C22—C23 | 2.2 (2) |
Mn1—N2—C10—C9 | 176.36 (9) | C26—C27—C28—C29 | −174.25 (11) |
Mn1—N2—C6—C5 | 6.85 (14) | C26—C25—C24—C23 | 0.9 (2) |
Mn1—N2—C6—C7 | −174.19 (9) | C18—C19—C20—C21 | 0.5 (2) |
Mn1—N6—C32—C31 | 9.74 (14) | C8—C16—C17—C18 | 179.92 (11) |
Mn1—N6—C32—C33 | −167.10 (10) | C8—C16—C21—C20 | −179.95 (12) |
Mn1—N6—C36—C35 | 164.11 (10) | C29—C37—C38—C39 | −173.07 (12) |
Mn1—N3—C11—C10 | 6.67 (13) | C29—C37—C42—C41 | 173.18 (12) |
Mn1—N3—C11—C12 | −171.06 (9) | C17—C16—C8—C7 | 5.23 (18) |
Mn1—N3—C15—C14 | 168.71 (10) | C17—C16—C8—C9 | −174.26 (12) |
O2—C40—C39—C38 | 178.05 (12) | C17—C16—C21—C20 | −0.5 (2) |
O2—C40—C41—C42 | −177.99 (12) | C31—N5—C27—C26 | 175.70 (11) |
O1—C19—C18—C17 | 179.83 (12) | C31—N5—C27—C28 | −1.55 (18) |
O1—C19—C20—C21 | −179.83 (13) | C31—C32—C33—C34 | −174.73 (12) |
N4—C26—C25—C24 | 1.0 (2) | C25—C24—C23—C22 | −1.2 (2) |
N4—C22—C23—C24 | −0.4 (2) | C40—C39—C38—C37 | 0.1 (2) |
N5—C27—C26—N4 | 5.83 (16) | C32—N6—C36—C35 | −0.20 (19) |
N5—C27—C26—C25 | −171.86 (12) | C32—C31—C30—C29 | 176.52 (12) |
N5—C27—C28—C29 | 2.75 (19) | C32—C33—C34—C35 | −0.4 (2) |
N5—C31—C32—N6 | −5.90 (16) | C15—N3—C11—C10 | 177.08 (11) |
N5—C31—C32—C33 | 170.91 (12) | C15—N3—C11—C12 | −0.65 (18) |
N5—C31—C30—C29 | 0.84 (19) | C28—C27—C26—N4 | −176.96 (12) |
N1—C5—C4—C3 | −0.08 (19) | C28—C27—C26—C25 | 5.3 (2) |
N2—C10—C9—C8 | −1.93 (18) | C28—C29—C30—C31 | 0.36 (19) |
N2—C6—C5—N1 | −5.27 (16) | C39—C40—C41—C42 | 2.3 (2) |
N2—C6—C5—C4 | 172.95 (11) | C30—C29—C28—C27 | −2.07 (18) |
N2—C6—C7—C8 | −2.40 (18) | C30—C31—C32—N6 | 178.16 (12) |
N6—C32—C33—C34 | 1.90 (19) | C30—C31—C32—C33 | −5.02 (19) |
N6—C36—C35—C34 | 1.6 (2) | C38—C37—C29—C28 | −27.63 (19) |
N3—C11—C10—N2 | −2.91 (16) | C38—C37—C29—C30 | 148.45 (13) |
N3—C11—C10—C9 | 178.31 (11) | C38—C37—C42—C41 | −1.9 (2) |
N3—C11—C12—C13 | 1.86 (19) | C33—C34—C35—C36 | −1.2 (2) |
N3—C15—C14—C13 | 1.5 (2) | C21—C16—C8—C7 | −175.33 (12) |
C11—N3—C15—C14 | −1.06 (19) | C21—C16—C8—C9 | 5.17 (18) |
C11—C10—C9—C8 | 176.75 (11) | C21—C16—C17—C18 | 0.46 (19) |
C11—C12—C13—C14 | −1.37 (19) | C42—C37—C29—C28 | 157.44 (13) |
C10—N2—C6—C5 | −176.95 (10) | C42—C37—C29—C30 | −26.48 (18) |
C10—N2—C6—C7 | 2.01 (18) | C42—C37—C38—C39 | 2.0 (2) |
C10—C11—C12—C13 | −175.70 (11) | C20—C19—C18—C17 | −0.5 (2) |
C10—C9—C8—C7 | 1.49 (17) | C41—C40—C39—C38 | −2.2 (2) |
C10—C9—C8—C16 | −178.99 (11) | C1—N1—C5—C6 | 176.91 (11) |
C6—N2—C10—C11 | −178.63 (10) | C1—N1—C5—C4 | −1.34 (18) |
C6—N2—C10—C9 | 0.16 (18) | C1—C2—C3—C4 | −0.6 (2) |
C6—C5—C4—C3 | −178.19 (12) | C36—N6—C32—C31 | 175.27 (11) |
C6—C7—C8—C16 | −178.95 (11) | C36—N6—C32—C33 | −1.57 (18) |
C6—C7—C8—C9 | 0.58 (17) | C22—N4—C26—C27 | 179.77 (11) |
C5—N1—C1—C2 | 1.87 (19) | C22—N4—C26—C25 | −2.51 (19) |
C5—C6—C7—C8 | 176.47 (11) | C3—C2—C1—N1 | −0.9 (2) |
C5—C4—C3—C2 | 1.0 (2) | C44—O1—C19—C18 | −1.7 (2) |
C7—C6—C5—N1 | 175.78 (11) | C44—O1—C19—C20 | 178.59 (13) |
C7—C6—C5—C4 | −5.99 (19) | C43—O2—C40—C39 | −170.34 (12) |
C27—N5—C31—C32 | −176.28 (11) | C43—O2—C40—C41 | 9.96 (19) |
[Mn(C21H15N3)2](ClO4)2 | F(000) = 1788 |
Mr = 872.56 | Dx = 1.567 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.51026 (18) Å | Cell parameters from 38088 reflections |
b = 12.5149 (2) Å | θ = 2.6–34.1° |
c = 31.2962 (6) Å | µ = 0.57 mm−1 |
β = 96.8780 (18)° | T = 100 K |
V = 3698.07 (12) Å3 | Block, yellow |
Z = 4 | 0.30 × 0.11 × 0.03 mm |
Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector | 9547 independent reflections |
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Mo) X-ray Source | 8250 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.032 |
Detector resolution: 10.0000 pixels mm-1 | θmax = 28.7°, θmin = 2.6° |
ω scans | h = −13→14 |
Absorption correction: gaussian (CrysAlis PRO; Rigaku OD, 2022) | k = −19→19 |
l = −48→45 | |
63288 measured reflections |
Refinement on F2 | 3 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.084 | w = 1/[σ2(Fo2) + (0.0383P)2 + 2.5012P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.002 |
9547 reflections | Δρmax = 0.43 e Å−3 |
560 parameters | Δρmin = −0.51 e Å−3 |
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. |
Refinement. Single crystals suitable for X-ray analysis were obtained by slow evaporation from acetonitrile using diethyl ether as antisolvent. Diffraction data for all the compounds were collected at room temperature on a Rigaku Synergy S diffractometer using photonjet microfocus source Mo Kα (λ = 0.71073 Å) radiation. The unit-cell parameters were determined using all reflections with CrysAlis PRO software (Agilent, 2014). Data integration and scaling were performed using CrysAlis PRO software (Agilent, 2014). The structures were solved and refined with SHELXT (Sheldrick, 2015a) and SHELXL (Sheldrick, 2015b) software, respectively, including in OLEX2 (Dolomanov et al., 2009). In all cases, non-H atoms were clearly resolved and full-matrix least-squares refinement with anisotropic displacement parameters was performed. In addition, the H atoms were stereochemically positioned and refined using the riding model (Sheldrick, 2008). The Mn compound [which one?] was refined using the SQUEEZE routine (Spek, 2015) in PLATON (Spek, 2020) to decrease the contribution of the disordered solvent (water molecule) to calculate the structure factors and improve the refinement values. Displacement ellipsoid plots for all structures were prepared with DIAMOND (Brandenburg et al., 2006). MERCURY were used for the preparation of artwork (Macrae et al., 2020). The CIF file of the complexes was deposited in the Cambridge Structural Data Base under the codes CCDC 2331329-2331331. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Mn1 | 0.55217 (2) | 0.66511 (2) | 0.61483 (2) | 0.01214 (6) | |
Cl2 | 0.03899 (4) | 0.78696 (3) | 0.51551 (2) | 0.01592 (7) | |
Cl1 | 0.76703 (4) | 0.90467 (3) | 0.74675 (2) | 0.02234 (8) | |
O8 | 0.03068 (13) | 0.67290 (8) | 0.50689 (4) | 0.0236 (2) | |
O7 | −0.02540 (12) | 0.80943 (9) | 0.55382 (3) | 0.0241 (2) | |
O5 | 0.18577 (11) | 0.81940 (9) | 0.52167 (3) | 0.0213 (2) | |
N5 | 0.60249 (12) | 0.63127 (9) | 0.68354 (3) | 0.0132 (2) | |
O6 | −0.03368 (13) | 0.84378 (9) | 0.47935 (4) | 0.0276 (3) | |
N6 | 0.36831 (12) | 0.72376 (9) | 0.64782 (4) | 0.0139 (2) | |
N2 | 0.48224 (12) | 0.67389 (9) | 0.54501 (4) | 0.0123 (2) | |
N4 | 0.77714 (12) | 0.60523 (9) | 0.62545 (4) | 0.0138 (2) | |
N1 | 0.43169 (12) | 0.51278 (9) | 0.59496 (4) | 0.0141 (2) | |
N3 | 0.63622 (12) | 0.81781 (9) | 0.59029 (4) | 0.0137 (2) | |
O1 | 0.65906 (16) | 0.85930 (12) | 0.71679 (4) | 0.0420 (4) | |
C10 | 0.51562 (14) | 0.75998 (10) | 0.52251 (4) | 0.0123 (2) | |
C11 | 0.60971 (14) | 0.83862 (10) | 0.54766 (4) | 0.0129 (2) | |
C7 | 0.33460 (14) | 0.60963 (11) | 0.48354 (4) | 0.0142 (2) | |
H7 | 0.273413 | 0.555629 | 0.470614 | 0.017* | |
C9 | 0.46060 (14) | 0.77417 (11) | 0.47975 (4) | 0.0139 (2) | |
H9 | 0.487664 | 0.834390 | 0.464158 | 0.017* | |
C27 | 0.50548 (15) | 0.65035 (11) | 0.71035 (4) | 0.0150 (3) | |
O3 | 0.7117 (8) | 0.9230 (7) | 0.78654 (16) | 0.0558 (17) | 0.63 (3) |
C32 | 0.83040 (15) | 0.58016 (10) | 0.66632 (4) | 0.0134 (2) | |
C37 | 0.69504 (15) | 0.56670 (11) | 0.81747 (4) | 0.0140 (2) | |
C5 | 0.36273 (14) | 0.50937 (10) | 0.55456 (4) | 0.0130 (2) | |
C39 | 0.85716 (15) | 0.58695 (11) | 0.88276 (4) | 0.0165 (3) | |
H39 | 0.946484 | 0.609258 | 0.896764 | 0.020* | |
C29 | 0.66243 (15) | 0.58427 (11) | 0.77054 (4) | 0.0144 (3) | |
C38 | 0.82713 (15) | 0.59734 (11) | 0.83840 (4) | 0.0159 (3) | |
H38 | 0.896841 | 0.625481 | 0.822166 | 0.019* | |
C28 | 0.53130 (15) | 0.62540 (12) | 0.75376 (4) | 0.0175 (3) | |
H28 | 0.459662 | 0.636353 | 0.772015 | 0.021* | |
C31 | 0.72924 (14) | 0.59099 (10) | 0.69895 (4) | 0.0128 (2) | |
C22 | 0.25461 (15) | 0.77547 (11) | 0.62823 (4) | 0.0160 (3) | |
H22 | 0.249169 | 0.788010 | 0.598135 | 0.019* | |
C30 | 0.76353 (15) | 0.56662 (11) | 0.74226 (4) | 0.0149 (3) | |
H30 | 0.854065 | 0.538437 | 0.752509 | 0.018* | |
C16 | 0.29350 (15) | 0.71704 (10) | 0.41567 (4) | 0.0141 (2) | |
C33 | 0.97100 (15) | 0.55131 (11) | 0.67687 (5) | 0.0174 (3) | |
H33 | 1.006288 | 0.534072 | 0.705735 | 0.021* | |
C26 | 0.37499 (15) | 0.70548 (11) | 0.69054 (4) | 0.0156 (3) | |
C1 | 0.40786 (15) | 0.43499 (11) | 0.62260 (4) | 0.0170 (3) | |
H1 | 0.456432 | 0.437461 | 0.650936 | 0.020* | |
C15 | 0.71934 (15) | 0.88546 (11) | 0.61525 (4) | 0.0170 (3) | |
H15 | 0.737822 | 0.870942 | 0.645190 | 0.020* | |
C23 | 0.14478 (15) | 0.81139 (11) | 0.64994 (5) | 0.0177 (3) | |
H23 | 0.065895 | 0.847533 | 0.634981 | 0.021* | |
C40 | 0.75682 (16) | 0.54398 (11) | 0.90670 (4) | 0.0170 (3) | |
H40 | 0.777778 | 0.535894 | 0.936980 | 0.020* | |
C6 | 0.39392 (14) | 0.59966 (10) | 0.52607 (4) | 0.0127 (2) | |
C12 | 0.66710 (15) | 0.92730 (11) | 0.52940 (4) | 0.0162 (3) | |
H12 | 0.647298 | 0.940444 | 0.499385 | 0.019* | |
C42 | 0.59376 (15) | 0.52416 (11) | 0.84167 (4) | 0.0162 (3) | |
H42 | 0.503634 | 0.503029 | 0.827872 | 0.019* | |
C36 | 0.86477 (16) | 0.60294 (11) | 0.59492 (4) | 0.0166 (3) | |
H36 | 0.828109 | 0.621775 | 0.566335 | 0.020* | |
C35 | 1.00601 (16) | 0.57446 (11) | 0.60306 (5) | 0.0183 (3) | |
H35 | 1.064774 | 0.573173 | 0.580567 | 0.022* | |
C8 | 0.36532 (14) | 0.69952 (11) | 0.45980 (4) | 0.0136 (2) | |
C14 | 0.77917 (16) | 0.97545 (11) | 0.59913 (5) | 0.0186 (3) | |
H14 | 0.836793 | 1.022020 | 0.617733 | 0.022* | |
C24 | 0.15228 (16) | 0.79362 (12) | 0.69374 (5) | 0.0213 (3) | |
H24 | 0.079328 | 0.818195 | 0.709534 | 0.026* | |
C34 | 1.05955 (16) | 0.54793 (12) | 0.64472 (5) | 0.0193 (3) | |
H34 | 1.155959 | 0.527595 | 0.651278 | 0.023* | |
C17 | 0.15410 (16) | 0.68177 (11) | 0.40447 (4) | 0.0167 (3) | |
H17 | 0.105846 | 0.645968 | 0.425177 | 0.020* | |
O2 | 0.8790 (7) | 0.8296 (7) | 0.7535 (3) | 0.068 (2) | 0.63 (3) |
C18 | 0.08613 (16) | 0.69891 (12) | 0.36322 (5) | 0.0185 (3) | |
H18 | −0.007989 | 0.674014 | 0.355797 | 0.022* | |
C41 | 0.62557 (16) | 0.51291 (12) | 0.88606 (4) | 0.0179 (3) | |
H41 | 0.556852 | 0.483697 | 0.902399 | 0.021* | |
C21 | 0.36073 (16) | 0.77218 (12) | 0.38509 (4) | 0.0196 (3) | |
H21 | 0.454548 | 0.797856 | 0.392359 | 0.023* | |
C25 | 0.26879 (16) | 0.73902 (13) | 0.71425 (5) | 0.0217 (3) | |
H25 | 0.275578 | 0.724815 | 0.744243 | 0.026* | |
C4 | 0.26772 (15) | 0.42783 (11) | 0.54152 (4) | 0.0170 (3) | |
H4 | 0.219498 | 0.427119 | 0.513126 | 0.020* | |
C13 | 0.75362 (16) | 0.99655 (11) | 0.55536 (5) | 0.0187 (3) | |
H13 | 0.794524 | 1.057186 | 0.543389 | 0.022* | |
C19 | 0.15471 (17) | 0.75212 (13) | 0.33278 (5) | 0.0217 (3) | |
H19 | 0.108514 | 0.762657 | 0.304466 | 0.026* | |
C2 | 0.31509 (16) | 0.35074 (11) | 0.61163 (5) | 0.0188 (3) | |
H2 | 0.300879 | 0.296708 | 0.632004 | 0.023* | |
O4 | 0.8043 (11) | 1.0058 (4) | 0.7301 (3) | 0.0469 (14) | 0.63 (3) |
C20 | 0.29110 (18) | 0.78976 (14) | 0.34403 (5) | 0.0248 (3) | |
H20 | 0.337486 | 0.827917 | 0.323519 | 0.030* | |
C3 | 0.24407 (16) | 0.34735 (11) | 0.57048 (5) | 0.0188 (3) | |
H3 | 0.179972 | 0.290843 | 0.562074 | 0.023* | |
O3A | 0.7150 (9) | 0.9475 (18) | 0.7823 (4) | 0.071 (4) | 0.37 (3) |
O2A | 0.8771 (11) | 0.8339 (10) | 0.7614 (4) | 0.060 (3) | 0.37 (3) |
O4A | 0.852 (2) | 0.9827 (19) | 0.7260 (5) | 0.064 (4) | 0.37 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.01269 (10) | 0.01436 (10) | 0.00917 (9) | −0.00060 (7) | 0.00045 (7) | 0.00137 (7) |
Cl2 | 0.01597 (16) | 0.01960 (16) | 0.01186 (14) | 0.00072 (11) | 0.00028 (11) | 0.00258 (11) |
Cl1 | 0.02685 (19) | 0.02322 (17) | 0.01604 (16) | −0.00158 (14) | −0.00119 (13) | −0.00172 (13) |
O8 | 0.0293 (6) | 0.0202 (5) | 0.0213 (5) | −0.0026 (4) | 0.0025 (4) | 0.0004 (4) |
O7 | 0.0227 (6) | 0.0319 (6) | 0.0189 (5) | 0.0048 (5) | 0.0079 (4) | 0.0014 (4) |
O5 | 0.0160 (5) | 0.0282 (6) | 0.0198 (5) | −0.0017 (4) | 0.0025 (4) | −0.0006 (4) |
N5 | 0.0133 (5) | 0.0149 (5) | 0.0113 (5) | 0.0008 (4) | 0.0009 (4) | 0.0003 (4) |
O6 | 0.0316 (7) | 0.0293 (6) | 0.0191 (5) | −0.0003 (5) | −0.0084 (5) | 0.0089 (4) |
N6 | 0.0141 (6) | 0.0151 (5) | 0.0122 (5) | −0.0002 (4) | 0.0005 (4) | 0.0023 (4) |
N2 | 0.0116 (5) | 0.0133 (5) | 0.0121 (5) | 0.0004 (4) | 0.0013 (4) | 0.0000 (4) |
N4 | 0.0151 (6) | 0.0143 (5) | 0.0123 (5) | −0.0001 (4) | 0.0025 (4) | 0.0001 (4) |
N1 | 0.0145 (6) | 0.0144 (5) | 0.0134 (5) | 0.0000 (4) | 0.0013 (4) | 0.0015 (4) |
N3 | 0.0136 (5) | 0.0148 (5) | 0.0126 (5) | −0.0001 (4) | 0.0011 (4) | 0.0001 (4) |
O1 | 0.0525 (9) | 0.0480 (8) | 0.0220 (6) | −0.0249 (7) | −0.0098 (6) | −0.0014 (5) |
C10 | 0.0114 (6) | 0.0126 (6) | 0.0133 (6) | 0.0013 (4) | 0.0032 (5) | 0.0004 (4) |
C11 | 0.0112 (6) | 0.0146 (6) | 0.0129 (6) | 0.0019 (5) | 0.0012 (5) | −0.0002 (5) |
C7 | 0.0141 (6) | 0.0144 (6) | 0.0135 (6) | 0.0009 (5) | −0.0003 (5) | −0.0013 (5) |
C9 | 0.0143 (6) | 0.0147 (6) | 0.0129 (6) | 0.0010 (5) | 0.0020 (5) | 0.0017 (5) |
C27 | 0.0136 (6) | 0.0189 (6) | 0.0124 (6) | 0.0019 (5) | 0.0012 (5) | 0.0012 (5) |
O3 | 0.074 (4) | 0.079 (3) | 0.0167 (19) | −0.008 (2) | 0.0153 (17) | −0.009 (2) |
C32 | 0.0156 (6) | 0.0123 (6) | 0.0126 (6) | 0.0001 (5) | 0.0022 (5) | 0.0000 (5) |
C37 | 0.0157 (6) | 0.0150 (6) | 0.0110 (6) | 0.0026 (5) | 0.0003 (5) | 0.0006 (5) |
C5 | 0.0130 (6) | 0.0135 (6) | 0.0127 (6) | 0.0015 (5) | 0.0020 (5) | −0.0003 (4) |
C39 | 0.0155 (7) | 0.0190 (6) | 0.0144 (6) | 0.0013 (5) | −0.0011 (5) | −0.0025 (5) |
C29 | 0.0164 (7) | 0.0157 (6) | 0.0104 (6) | 0.0000 (5) | −0.0009 (5) | 0.0005 (5) |
C38 | 0.0155 (7) | 0.0188 (6) | 0.0134 (6) | −0.0004 (5) | 0.0021 (5) | −0.0002 (5) |
C28 | 0.0166 (7) | 0.0237 (7) | 0.0126 (6) | 0.0040 (5) | 0.0037 (5) | 0.0021 (5) |
C31 | 0.0129 (6) | 0.0128 (6) | 0.0126 (6) | 0.0003 (5) | 0.0011 (5) | −0.0004 (4) |
C22 | 0.0171 (7) | 0.0157 (6) | 0.0145 (6) | −0.0007 (5) | −0.0011 (5) | 0.0031 (5) |
C30 | 0.0141 (6) | 0.0170 (6) | 0.0132 (6) | 0.0015 (5) | −0.0003 (5) | 0.0008 (5) |
C16 | 0.0169 (7) | 0.0140 (6) | 0.0113 (6) | 0.0029 (5) | 0.0010 (5) | −0.0010 (5) |
C33 | 0.0161 (7) | 0.0187 (6) | 0.0173 (6) | 0.0022 (5) | 0.0014 (5) | 0.0023 (5) |
C26 | 0.0138 (6) | 0.0187 (6) | 0.0140 (6) | 0.0024 (5) | 0.0001 (5) | 0.0026 (5) |
C1 | 0.0186 (7) | 0.0173 (6) | 0.0147 (6) | −0.0003 (5) | 0.0007 (5) | 0.0029 (5) |
C15 | 0.0158 (7) | 0.0198 (7) | 0.0150 (6) | −0.0005 (5) | 0.0004 (5) | −0.0014 (5) |
C23 | 0.0141 (7) | 0.0176 (6) | 0.0203 (7) | 0.0012 (5) | −0.0022 (5) | 0.0021 (5) |
C40 | 0.0218 (7) | 0.0186 (6) | 0.0103 (6) | 0.0031 (5) | 0.0004 (5) | 0.0000 (5) |
C6 | 0.0123 (6) | 0.0124 (6) | 0.0136 (6) | 0.0016 (5) | 0.0024 (5) | 0.0003 (4) |
C12 | 0.0161 (7) | 0.0172 (6) | 0.0154 (6) | 0.0000 (5) | 0.0023 (5) | 0.0024 (5) |
C42 | 0.0146 (7) | 0.0196 (6) | 0.0141 (6) | 0.0009 (5) | −0.0002 (5) | 0.0012 (5) |
C36 | 0.0203 (7) | 0.0164 (6) | 0.0138 (6) | −0.0006 (5) | 0.0042 (5) | 0.0005 (5) |
C35 | 0.0194 (7) | 0.0169 (6) | 0.0200 (7) | 0.0003 (5) | 0.0084 (5) | 0.0008 (5) |
C8 | 0.0139 (6) | 0.0155 (6) | 0.0116 (6) | 0.0031 (5) | 0.0024 (5) | −0.0002 (5) |
C14 | 0.0156 (7) | 0.0185 (7) | 0.0211 (7) | −0.0025 (5) | 0.0002 (5) | −0.0031 (5) |
C24 | 0.0167 (7) | 0.0264 (7) | 0.0210 (7) | 0.0056 (6) | 0.0032 (6) | −0.0001 (6) |
C34 | 0.0144 (7) | 0.0194 (7) | 0.0246 (7) | 0.0030 (5) | 0.0046 (6) | 0.0018 (5) |
C17 | 0.0186 (7) | 0.0155 (6) | 0.0157 (6) | 0.0003 (5) | 0.0009 (5) | 0.0018 (5) |
O2 | 0.043 (3) | 0.069 (4) | 0.098 (4) | 0.025 (3) | 0.038 (3) | 0.011 (3) |
C18 | 0.0179 (7) | 0.0194 (7) | 0.0173 (6) | 0.0014 (5) | −0.0015 (5) | −0.0014 (5) |
C41 | 0.0188 (7) | 0.0206 (7) | 0.0146 (6) | 0.0002 (5) | 0.0037 (5) | 0.0028 (5) |
C21 | 0.0180 (7) | 0.0266 (7) | 0.0143 (6) | −0.0010 (6) | 0.0025 (5) | 0.0005 (5) |
C25 | 0.0196 (7) | 0.0321 (8) | 0.0136 (6) | 0.0071 (6) | 0.0033 (5) | 0.0029 (6) |
C4 | 0.0180 (7) | 0.0173 (6) | 0.0151 (6) | −0.0017 (5) | 0.0002 (5) | −0.0006 (5) |
C13 | 0.0175 (7) | 0.0158 (6) | 0.0232 (7) | −0.0024 (5) | 0.0035 (6) | 0.0019 (5) |
C19 | 0.0231 (8) | 0.0296 (8) | 0.0116 (6) | 0.0027 (6) | −0.0011 (5) | 0.0003 (5) |
C2 | 0.0198 (7) | 0.0168 (6) | 0.0201 (7) | −0.0013 (5) | 0.0040 (5) | 0.0045 (5) |
O4 | 0.053 (3) | 0.0302 (18) | 0.052 (2) | −0.0182 (17) | −0.014 (2) | 0.0109 (14) |
C20 | 0.0255 (8) | 0.0369 (9) | 0.0124 (6) | −0.0022 (6) | 0.0043 (6) | 0.0035 (6) |
C3 | 0.0176 (7) | 0.0160 (6) | 0.0229 (7) | −0.0035 (5) | 0.0027 (6) | 0.0001 (5) |
O3A | 0.021 (3) | 0.112 (8) | 0.076 (7) | 0.016 (3) | −0.005 (3) | −0.078 (6) |
O2A | 0.054 (6) | 0.055 (5) | 0.059 (4) | 0.032 (4) | −0.041 (5) | −0.016 (3) |
O4A | 0.061 (7) | 0.081 (8) | 0.044 (4) | −0.047 (6) | −0.019 (4) | 0.030 (5) |
Mn1—N5 | 2.1876 (11) | C38—H38 | 0.9500 |
Mn1—N2 | 2.2091 (11) | C28—H28 | 0.9500 |
Mn1—N3 | 2.2423 (12) | C31—C30 | 1.3894 (18) |
Mn1—N4 | 2.2537 (12) | C22—C23 | 1.387 (2) |
Mn1—N6 | 2.2571 (12) | C22—H22 | 0.9500 |
Mn1—N1 | 2.2723 (12) | C30—H30 | 0.9500 |
Cl2—O7 | 1.4378 (11) | C16—C21 | 1.396 (2) |
Cl2—O6 | 1.4412 (11) | C16—C17 | 1.401 (2) |
Cl2—O5 | 1.4443 (11) | C16—C8 | 1.4819 (18) |
Cl2—O8 | 1.4530 (11) | C33—C34 | 1.388 (2) |
Cl1—O3A | 1.381 (8) | C33—H33 | 0.9500 |
Cl1—O2A | 1.406 (8) | C26—C25 | 1.388 (2) |
Cl1—O2 | 1.417 (6) | C1—C2 | 1.391 (2) |
Cl1—O1 | 1.4231 (13) | C1—H1 | 0.9500 |
Cl1—O3 | 1.427 (5) | C15—C14 | 1.384 (2) |
Cl1—O4 | 1.429 (6) | C15—H15 | 0.9500 |
Cl1—O4A | 1.466 (9) | C23—C24 | 1.382 (2) |
N5—C27 | 1.3408 (18) | C23—H23 | 0.9500 |
N5—C31 | 1.3418 (17) | C40—C41 | 1.391 (2) |
N6—C22 | 1.3437 (18) | C40—H40 | 0.9500 |
N6—C26 | 1.3504 (17) | C12—C13 | 1.389 (2) |
N2—C6 | 1.3419 (17) | C12—H12 | 0.9500 |
N2—C10 | 1.3459 (17) | C42—C41 | 1.3929 (19) |
N4—C36 | 1.3415 (18) | C42—H42 | 0.9500 |
N4—C32 | 1.3547 (17) | C36—C35 | 1.384 (2) |
N1—C1 | 1.3397 (18) | C36—H36 | 0.9500 |
N1—C5 | 1.3532 (17) | C35—C34 | 1.382 (2) |
N3—C15 | 1.3431 (18) | C35—H35 | 0.9500 |
N3—C11 | 1.3530 (17) | C14—C13 | 1.388 (2) |
C10—C9 | 1.3885 (18) | C14—H14 | 0.9500 |
C10—C11 | 1.4901 (18) | C24—C25 | 1.391 (2) |
C11—C12 | 1.3896 (19) | C24—H24 | 0.9500 |
C7—C6 | 1.3877 (18) | C34—H34 | 0.9500 |
C7—C8 | 1.3982 (19) | C17—C18 | 1.3896 (19) |
C7—H7 | 0.9500 | C17—H17 | 0.9500 |
C9—C8 | 1.3958 (19) | C18—C19 | 1.387 (2) |
C9—H9 | 0.9500 | C18—H18 | 0.9500 |
C27—C28 | 1.3870 (18) | C41—H41 | 0.9500 |
C27—C26 | 1.4887 (19) | C21—C20 | 1.391 (2) |
C32—C33 | 1.3862 (19) | C21—H21 | 0.9500 |
C32—C31 | 1.4909 (18) | C25—H25 | 0.9500 |
C37—C38 | 1.3991 (19) | C4—C3 | 1.391 (2) |
C37—C42 | 1.400 (2) | C4—H4 | 0.9500 |
C37—C29 | 1.4807 (18) | C13—H13 | 0.9500 |
C5—C4 | 1.3914 (19) | C19—C20 | 1.385 (2) |
C5—C6 | 1.4911 (18) | C19—H19 | 0.9500 |
C39—C38 | 1.3895 (19) | C2—C3 | 1.381 (2) |
C39—C40 | 1.390 (2) | C2—H2 | 0.9500 |
C39—H39 | 0.9500 | C20—H20 | 0.9500 |
C29—C28 | 1.3925 (19) | C3—H3 | 0.9500 |
C29—C30 | 1.4003 (19) | ||
N5—Mn1—N2 | 170.51 (4) | C30—C31—C32 | 123.57 (12) |
N5—Mn1—N3 | 117.17 (4) | N6—C22—C23 | 122.99 (13) |
N2—Mn1—N3 | 72.32 (4) | N6—C22—H22 | 118.5 |
N5—Mn1—N4 | 72.45 (4) | C23—C22—H22 | 118.5 |
N2—Mn1—N4 | 109.30 (4) | C31—C30—C29 | 118.90 (12) |
N3—Mn1—N4 | 87.87 (4) | C31—C30—H30 | 120.5 |
N5—Mn1—N6 | 72.76 (4) | C29—C30—H30 | 120.5 |
N2—Mn1—N6 | 106.16 (4) | C21—C16—C17 | 118.78 (13) |
N3—Mn1—N6 | 101.95 (4) | C21—C16—C8 | 120.96 (13) |
N4—Mn1—N6 | 144.53 (4) | C17—C16—C8 | 120.21 (12) |
N5—Mn1—N1 | 98.65 (4) | C32—C33—C34 | 119.13 (13) |
N2—Mn1—N1 | 71.87 (4) | C32—C33—H33 | 120.4 |
N3—Mn1—N1 | 144.10 (4) | C34—C33—H33 | 120.4 |
N4—Mn1—N1 | 101.55 (4) | N6—C26—C25 | 121.81 (13) |
N6—Mn1—N1 | 90.29 (4) | N6—C26—C27 | 115.39 (12) |
O7—Cl2—O6 | 110.25 (7) | C25—C26—C27 | 122.77 (12) |
O7—Cl2—O5 | 109.58 (7) | N1—C1—C2 | 122.87 (13) |
O6—Cl2—O5 | 109.33 (7) | N1—C1—H1 | 118.6 |
O7—Cl2—O8 | 109.14 (7) | C2—C1—H1 | 118.6 |
O6—Cl2—O8 | 109.18 (7) | N3—C15—C14 | 122.69 (13) |
O5—Cl2—O8 | 109.34 (7) | N3—C15—H15 | 118.7 |
O3A—Cl1—O2A | 107.8 (7) | C14—C15—H15 | 118.7 |
O3A—Cl1—O1 | 112.7 (5) | C24—C23—C22 | 118.76 (13) |
O2A—Cl1—O1 | 114.5 (5) | C24—C23—H23 | 120.6 |
O2—Cl1—O1 | 107.6 (4) | C22—C23—H23 | 120.6 |
O2—Cl1—O3 | 109.0 (4) | C39—C40—C41 | 119.58 (13) |
O1—Cl1—O3 | 109.1 (3) | C39—C40—H40 | 120.2 |
O2—Cl1—O4 | 115.2 (5) | C41—C40—H40 | 120.2 |
O1—Cl1—O4 | 107.7 (3) | N2—C6—C7 | 121.51 (12) |
O3—Cl1—O4 | 108.0 (4) | N2—C6—C5 | 114.79 (11) |
O3A—Cl1—O4A | 111.6 (8) | C7—C6—C5 | 123.68 (12) |
O2A—Cl1—O4A | 97.9 (10) | C13—C12—C11 | 119.48 (13) |
O1—Cl1—O4A | 111.4 (5) | C13—C12—H12 | 120.3 |
C27—N5—C31 | 119.85 (11) | C11—C12—H12 | 120.3 |
C27—N5—Mn1 | 119.65 (9) | C41—C42—C37 | 119.78 (13) |
C31—N5—Mn1 | 120.50 (9) | C41—C42—H42 | 120.1 |
C22—N6—C26 | 118.25 (12) | C37—C42—H42 | 120.1 |
C22—N6—Mn1 | 124.96 (9) | N4—C36—C35 | 123.12 (13) |
C26—N6—Mn1 | 116.79 (9) | N4—C36—H36 | 118.4 |
C6—N2—C10 | 119.83 (11) | C35—C36—H36 | 118.4 |
C6—N2—Mn1 | 120.06 (9) | C34—C35—C36 | 118.40 (13) |
C10—N2—Mn1 | 119.70 (9) | C34—C35—H35 | 120.8 |
C36—N4—C32 | 118.27 (12) | C36—C35—H35 | 120.8 |
C36—N4—Mn1 | 124.18 (9) | C9—C8—C7 | 117.82 (12) |
C32—N4—Mn1 | 117.22 (9) | C9—C8—C16 | 121.33 (12) |
C1—N1—C5 | 118.68 (12) | C7—C8—C16 | 120.79 (12) |
C1—N1—Mn1 | 123.48 (9) | C15—C14—C13 | 118.92 (13) |
C5—N1—Mn1 | 117.01 (9) | C15—C14—H14 | 120.5 |
C15—N3—C11 | 118.64 (12) | C13—C14—H14 | 120.5 |
C15—N3—Mn1 | 123.18 (9) | C23—C24—C25 | 118.70 (14) |
C11—N3—Mn1 | 118.02 (9) | C23—C24—H24 | 120.7 |
N2—C10—C9 | 121.43 (12) | C25—C24—H24 | 120.7 |
N2—C10—C11 | 114.62 (11) | C35—C34—C33 | 119.31 (14) |
C9—C10—C11 | 123.91 (12) | C35—C34—H34 | 120.3 |
N3—C11—C12 | 121.56 (12) | C33—C34—H34 | 120.3 |
N3—C11—C10 | 115.03 (11) | C18—C17—C16 | 120.31 (13) |
C12—C11—C10 | 123.42 (12) | C18—C17—H17 | 119.8 |
C6—C7—C8 | 119.68 (12) | C16—C17—H17 | 119.8 |
C6—C7—H7 | 120.2 | C19—C18—C17 | 120.49 (14) |
C8—C7—H7 | 120.2 | C19—C18—H18 | 119.8 |
C10—C9—C8 | 119.67 (12) | C17—C18—H18 | 119.8 |
C10—C9—H9 | 120.2 | C40—C41—C42 | 120.72 (13) |
C8—C9—H9 | 120.2 | C40—C41—H41 | 119.6 |
N5—C27—C28 | 121.24 (13) | C42—C41—H41 | 119.6 |
N5—C27—C26 | 115.07 (12) | C20—C21—C16 | 120.36 (14) |
C28—C27—C26 | 123.59 (13) | C20—C21—H21 | 119.8 |
N4—C32—C33 | 121.75 (12) | C16—C21—H21 | 119.8 |
N4—C32—C31 | 115.25 (12) | C26—C25—C24 | 119.49 (13) |
C33—C32—C31 | 122.93 (12) | C26—C25—H25 | 120.3 |
C38—C37—C42 | 119.23 (12) | C24—C25—H25 | 120.3 |
C38—C37—C29 | 119.57 (12) | C3—C4—C5 | 119.33 (13) |
C42—C37—C29 | 121.15 (12) | C3—C4—H4 | 120.3 |
N1—C5—C4 | 121.48 (12) | C5—C4—H4 | 120.3 |
N1—C5—C6 | 115.21 (12) | C14—C13—C12 | 118.70 (13) |
C4—C5—C6 | 123.30 (12) | C14—C13—H13 | 120.6 |
C38—C39—C40 | 120.17 (13) | C12—C13—H13 | 120.6 |
C38—C39—H39 | 119.9 | C20—C19—C18 | 119.45 (13) |
C40—C39—H39 | 119.9 | C20—C19—H19 | 120.3 |
C28—C29—C30 | 118.14 (12) | C18—C19—H19 | 120.3 |
C28—C29—C37 | 120.05 (12) | C3—C2—C1 | 118.56 (13) |
C30—C29—C37 | 121.70 (12) | C3—C2—H2 | 120.7 |
C39—C38—C37 | 120.52 (13) | C1—C2—H2 | 120.7 |
C39—C38—H38 | 119.7 | C19—C20—C21 | 120.58 (14) |
C37—C38—H38 | 119.7 | C19—C20—H20 | 119.7 |
C27—C28—C29 | 119.88 (13) | C21—C20—H20 | 119.7 |
C27—C28—H28 | 120.1 | C2—C3—C4 | 119.08 (13) |
C29—C28—H28 | 120.1 | C2—C3—H3 | 120.5 |
N5—C31—C30 | 121.94 (12) | C4—C3—H3 | 120.5 |
N5—C31—C32 | 114.42 (11) | ||
C6—N2—C10—C9 | −0.04 (19) | C28—C27—C26—N6 | 179.68 (13) |
Mn1—N2—C10—C9 | −172.69 (10) | N5—C27—C26—C25 | −174.73 (14) |
C6—N2—C10—C11 | 177.57 (12) | C28—C27—C26—C25 | 1.5 (2) |
Mn1—N2—C10—C11 | 4.92 (15) | C5—N1—C1—C2 | −0.1 (2) |
C15—N3—C11—C12 | 0.5 (2) | Mn1—N1—C1—C2 | 169.18 (11) |
Mn1—N3—C11—C12 | −175.00 (10) | C11—N3—C15—C14 | −0.1 (2) |
C15—N3—C11—C10 | −179.51 (12) | Mn1—N3—C15—C14 | 175.09 (11) |
Mn1—N3—C11—C10 | 5.02 (15) | N6—C22—C23—C24 | 0.2 (2) |
N2—C10—C11—N3 | −6.41 (17) | C38—C39—C40—C41 | −0.9 (2) |
C9—C10—C11—N3 | 171.12 (12) | C10—N2—C6—C7 | −0.4 (2) |
N2—C10—C11—C12 | 173.61 (13) | Mn1—N2—C6—C7 | 172.17 (10) |
C9—C10—C11—C12 | −8.9 (2) | C10—N2—C6—C5 | −178.75 (11) |
N2—C10—C9—C8 | 1.9 (2) | Mn1—N2—C6—C5 | −6.13 (15) |
C11—C10—C9—C8 | −175.48 (12) | C8—C7—C6—N2 | −0.9 (2) |
C31—N5—C27—C28 | −2.5 (2) | C8—C7—C6—C5 | 177.22 (12) |
Mn1—N5—C27—C28 | 177.06 (11) | N1—C5—C6—N2 | −2.35 (17) |
C31—N5—C27—C26 | 173.85 (12) | C4—C5—C6—N2 | 176.36 (13) |
Mn1—N5—C27—C26 | −6.57 (16) | N1—C5—C6—C7 | 179.39 (12) |
C36—N4—C32—C33 | −0.84 (19) | C4—C5—C6—C7 | −1.9 (2) |
Mn1—N4—C32—C33 | −174.46 (10) | N3—C11—C12—C13 | −0.1 (2) |
C36—N4—C32—C31 | 176.34 (12) | C10—C11—C12—C13 | 179.88 (13) |
Mn1—N4—C32—C31 | 2.72 (15) | C38—C37—C42—C41 | 0.0 (2) |
C1—N1—C5—C4 | 0.5 (2) | C29—C37—C42—C41 | −177.20 (13) |
Mn1—N1—C5—C4 | −169.42 (10) | C32—N4—C36—C35 | 1.1 (2) |
C1—N1—C5—C6 | 179.25 (12) | Mn1—N4—C36—C35 | 174.29 (10) |
Mn1—N1—C5—C6 | 9.31 (15) | N4—C36—C35—C34 | −0.5 (2) |
C38—C37—C29—C28 | −136.00 (14) | C10—C9—C8—C7 | −3.2 (2) |
C42—C37—C29—C28 | 41.19 (19) | C10—C9—C8—C16 | 173.95 (12) |
C38—C37—C29—C30 | 40.11 (19) | C6—C7—C8—C9 | 2.7 (2) |
C42—C37—C29—C30 | −142.71 (14) | C6—C7—C8—C16 | −174.43 (12) |
C40—C39—C38—C37 | 1.2 (2) | C21—C16—C8—C9 | 32.5 (2) |
C42—C37—C38—C39 | −0.8 (2) | C17—C16—C8—C9 | −145.05 (14) |
C29—C37—C38—C39 | 176.49 (13) | C21—C16—C8—C7 | −150.48 (14) |
N5—C27—C28—C29 | 3.0 (2) | C17—C16—C8—C7 | 31.98 (19) |
C26—C27—C28—C29 | −173.07 (13) | N3—C15—C14—C13 | −0.6 (2) |
C30—C29—C28—C27 | −1.8 (2) | C22—C23—C24—C25 | −0.9 (2) |
C37—C29—C28—C27 | 174.48 (13) | C36—C35—C34—C33 | −0.4 (2) |
C27—N5—C31—C30 | 0.9 (2) | C32—C33—C34—C35 | 0.7 (2) |
Mn1—N5—C31—C30 | −178.69 (10) | C21—C16—C17—C18 | 1.9 (2) |
C27—N5—C31—C32 | −176.25 (12) | C8—C16—C17—C18 | 179.45 (13) |
Mn1—N5—C31—C32 | 4.17 (15) | C16—C17—C18—C19 | −0.7 (2) |
N4—C32—C31—N5 | −4.42 (17) | C39—C40—C41—C42 | 0.1 (2) |
C33—C32—C31—N5 | 172.73 (13) | C37—C42—C41—C40 | 0.3 (2) |
N4—C32—C31—C30 | 178.50 (12) | C17—C16—C21—C20 | −1.2 (2) |
C33—C32—C31—C30 | −4.4 (2) | C8—C16—C21—C20 | −178.81 (14) |
C26—N6—C22—C23 | 0.5 (2) | N6—C26—C25—C24 | −0.4 (2) |
Mn1—N6—C22—C23 | −179.10 (10) | C27—C26—C25—C24 | 177.60 (14) |
N5—C31—C30—C29 | 0.3 (2) | C23—C24—C25—C26 | 1.0 (2) |
C32—C31—C30—C29 | 177.14 (12) | N1—C5—C4—C3 | −0.7 (2) |
C28—C29—C30—C31 | 0.2 (2) | C6—C5—C4—C3 | −179.30 (13) |
C37—C29—C30—C31 | −175.98 (12) | C15—C14—C13—C12 | 0.9 (2) |
N4—C32—C33—C34 | −0.1 (2) | C11—C12—C13—C14 | −0.6 (2) |
C31—C32—C33—C34 | −177.02 (13) | C17—C18—C19—C20 | −1.1 (2) |
C22—N6—C26—C25 | −0.3 (2) | N1—C1—C2—C3 | −0.2 (2) |
Mn1—N6—C26—C25 | 179.27 (12) | C18—C19—C20—C21 | 1.7 (2) |
C22—N6—C26—C27 | −178.49 (12) | C16—C21—C20—C19 | −0.5 (2) |
Mn1—N6—C26—C27 | 1.11 (16) | C1—C2—C3—C4 | 0.1 (2) |
N5—C27—C26—N6 | 3.41 (18) | C5—C4—C3—C2 | 0.4 (2) |
[Ni(C21H15N3)2](ClO4)2 | F(000) = 1800 |
Mr = 876.33 | Dx = 1.581 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.3581 (2) Å | Cell parameters from 24227 reflections |
b = 12.6255 (3) Å | θ = 2.5–33.3° |
c = 31.4046 (8) Å | µ = 0.74 mm−1 |
β = 97.038 (2)° | T = 100 K |
V = 3682.52 (15) Å3 | Block, light orange |
Z = 4 | 0.10 × 0.08 × 0.06 mm |
Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector | 9514 independent reflections |
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Mo) X-ray Source | 7295 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.053 |
Detector resolution: 10.0000 pixels mm-1 | θmax = 28.7°, θmin = 2.5° |
ω scans | h = −12→12 |
Absorption correction: gaussian (CrysAlis PRO; Rigaku OD, 2022) | k = −16→17 |
Tmin = 0.815, Tmax = 1.000 | l = −41→42 |
52589 measured reflections |
Refinement on F2 | 435 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.094 | w = 1/[σ2(Fo2) + (0.0352P)2 + 3.3821P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
9514 reflections | Δρmax = 0.64 e Å−3 |
560 parameters | Δρmin = −0.54 e Å−3 |
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. |
Refinement. Single crystals suitable for X-ray analysis were obtained by slow evaporation from acetonitrile using diethyl ether as antisolvent. Diffraction data for all the compounds were collected at room temperature on a Rigaku Synergy S diffractometer using photonjet microfocus source Mo Kα (λ = 0.71073 Å) radiation. The unit-cell parameters were determined using all reflections with CrysAlis PRO software (Agilent, 2014). Data integration and scaling were performed using CrysAlis PRO software (Agilent, 2014). The structures were solved and refined with SHELXT (Sheldrick, 2015a) and SHELXL (Sheldrick, 2015b) software, respectively, including in OLEX2 (Dolomanov et al., 2009). In all cases, non-H atoms were clearly resolved and full-matrix least-squares refinement with anisotropic displacement parameters was performed. In addition, the H atoms were stereochemically positioned and refined using the riding model (Sheldrick, 2008). The Mn compound [which one?] was refined using the SQUEEZE routine (Spek, 2015) in PLATON (Spek, 2020) to decrease the contribution of the disordered solvent (water molecule) to calculate the structure factors and improve the refinement values. Displacement ellipsoid plots for all structures were prepared with DIAMOND (Brandenburg et al., 2006). MERCURY were used for the preparation of artwork (Macrae et al., 2020). The CIF file of the complexes was deposited in the Cambridge Structural Data Base under the codes CCDC 2331329-2331331. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.45313 (2) | 0.67165 (2) | 0.38521 (2) | 0.01333 (7) | |
Cl2 | 0.97887 (5) | 0.78974 (4) | 0.49141 (2) | 0.02213 (11) | |
Cl1 | 0.21363 (5) | 0.92269 (4) | 0.24853 (2) | 0.02422 (11) | |
O8 | 0.97982 (18) | 0.67651 (12) | 0.50010 (5) | 0.0281 (3) | |
N2 | 0.51734 (16) | 0.68107 (12) | 0.44827 (5) | 0.0141 (3) | |
N5 | 0.39922 (17) | 0.65160 (12) | 0.32226 (5) | 0.0149 (3) | |
N3 | 0.36801 (16) | 0.81949 (12) | 0.40160 (5) | 0.0150 (3) | |
N4 | 0.63665 (17) | 0.73271 (12) | 0.35939 (5) | 0.0153 (3) | |
O7 | 1.03924 (17) | 0.80845 (13) | 0.45232 (5) | 0.0300 (4) | |
O5 | 0.83213 (17) | 0.82817 (13) | 0.48676 (5) | 0.0305 (4) | |
N1 | 0.56197 (16) | 0.52504 (12) | 0.39778 (5) | 0.0150 (3) | |
N6 | 0.24101 (17) | 0.61193 (12) | 0.38221 (5) | 0.0148 (3) | |
O6 | 1.0601 (2) | 0.84318 (14) | 0.52657 (6) | 0.0431 (5) | |
O1 | 0.3281 (2) | 0.86989 (15) | 0.27412 (6) | 0.0432 (5) | |
C11 | 0.39025 (19) | 0.84361 (14) | 0.44381 (6) | 0.0150 (4) | |
C10 | 0.48180 (19) | 0.76651 (14) | 0.47042 (6) | 0.0139 (4) | |
C6 | 0.60250 (19) | 0.60519 (14) | 0.46752 (6) | 0.0144 (4) | |
C9 | 0.5328 (2) | 0.77833 (14) | 0.51354 (6) | 0.0158 (4) | |
H9 | 0.505366 | 0.838169 | 0.528984 | 0.019* | |
C31 | 0.27142 (19) | 0.60874 (14) | 0.30761 (6) | 0.0151 (4) | |
C7 | 0.6573 (2) | 0.61277 (14) | 0.51031 (6) | 0.0160 (4) | |
H7 | 0.716632 | 0.557990 | 0.523523 | 0.019* | |
C32 | 0.1769 (2) | 0.59386 (14) | 0.34180 (6) | 0.0150 (4) | |
C33 | 0.0324 (2) | 0.56748 (15) | 0.33329 (7) | 0.0182 (4) | |
H33 | −0.010507 | 0.555517 | 0.304683 | 0.022* | |
C22 | 0.7524 (2) | 0.78050 (14) | 0.38051 (7) | 0.0168 (4) | |
H22 | 0.758400 | 0.787381 | 0.410801 | 0.020* | |
C15 | 0.2843 (2) | 0.88344 (15) | 0.37516 (7) | 0.0182 (4) | |
H15 | 0.268385 | 0.866400 | 0.345495 | 0.022* | |
C26 | 0.6302 (2) | 0.72212 (15) | 0.31626 (6) | 0.0175 (4) | |
C4 | 0.7234 (2) | 0.43312 (15) | 0.45043 (7) | 0.0189 (4) | |
H4 | 0.771109 | 0.428984 | 0.478880 | 0.023* | |
C28 | 0.4712 (2) | 0.64245 (16) | 0.25252 (6) | 0.0187 (4) | |
H28 | 0.543636 | 0.651977 | 0.234154 | 0.022* | |
C27 | 0.4976 (2) | 0.67007 (15) | 0.29544 (6) | 0.0167 (4) | |
C12 | 0.3292 (2) | 0.93257 (15) | 0.46021 (7) | 0.0179 (4) | |
H12 | 0.346711 | 0.948280 | 0.489981 | 0.022* | |
C1 | 0.5830 (2) | 0.44934 (15) | 0.36943 (7) | 0.0185 (4) | |
H1 | 0.533945 | 0.454587 | 0.341178 | 0.022* | |
C5 | 0.63146 (19) | 0.51687 (14) | 0.43826 (6) | 0.0156 (4) | |
C37 | 0.3043 (2) | 0.57916 (14) | 0.18980 (6) | 0.0163 (4) | |
C16 | 0.6910 (2) | 0.71515 (14) | 0.57908 (6) | 0.0157 (4) | |
C35 | 0.0159 (2) | 0.57788 (15) | 0.40844 (7) | 0.0196 (4) | |
H35 | −0.037684 | 0.572543 | 0.432174 | 0.024* | |
C8 | 0.6249 (2) | 0.70170 (14) | 0.53421 (6) | 0.0156 (4) | |
C29 | 0.3376 (2) | 0.60056 (15) | 0.23647 (6) | 0.0173 (4) | |
C36 | 0.1606 (2) | 0.60499 (15) | 0.41440 (6) | 0.0172 (4) | |
H36 | 0.204585 | 0.619275 | 0.442713 | 0.021* | |
C30 | 0.2357 (2) | 0.58350 (15) | 0.26470 (6) | 0.0173 (4) | |
H30 | 0.143624 | 0.555153 | 0.254680 | 0.021* | |
C34 | −0.0484 (2) | 0.55889 (15) | 0.36731 (7) | 0.0207 (4) | |
H34 | −0.147292 | 0.540038 | 0.362293 | 0.025* | |
C23 | 0.8639 (2) | 0.82028 (15) | 0.35977 (7) | 0.0188 (4) | |
H23 | 0.944400 | 0.853616 | 0.375677 | 0.023* | |
C41 | 0.1443 (2) | 0.59859 (15) | 0.12386 (6) | 0.0184 (4) | |
H41 | 0.055045 | 0.621815 | 0.109131 | 0.022* | |
C38 | 0.4062 (2) | 0.53171 (15) | 0.16699 (7) | 0.0184 (4) | |
H38 | 0.495769 | 0.508838 | 0.181598 | 0.022* | |
C17 | 0.8301 (2) | 0.67636 (15) | 0.59224 (6) | 0.0179 (4) | |
H17 | 0.881722 | 0.641089 | 0.572203 | 0.021* | |
C39 | 0.3764 (2) | 0.51794 (15) | 0.12283 (7) | 0.0192 (4) | |
H39 | 0.445643 | 0.485270 | 0.107395 | 0.023* | |
C40 | 0.2459 (2) | 0.55169 (15) | 0.10117 (7) | 0.0194 (4) | |
H40 | 0.226335 | 0.542719 | 0.070986 | 0.023* | |
C13 | 0.2422 (2) | 0.99840 (15) | 0.43267 (7) | 0.0212 (4) | |
H13 | 0.198772 | 1.059359 | 0.443304 | 0.025* | |
C42 | 0.1725 (2) | 0.61162 (15) | 0.16785 (7) | 0.0185 (4) | |
H42 | 0.101948 | 0.642816 | 0.183223 | 0.022* | |
C14 | 0.2201 (2) | 0.97352 (15) | 0.38943 (7) | 0.0203 (4) | |
H14 | 0.161769 | 1.017505 | 0.369838 | 0.024* | |
C18 | 0.8925 (2) | 0.68926 (15) | 0.63440 (7) | 0.0207 (4) | |
H18 | 0.986327 | 0.662215 | 0.643073 | 0.025* | |
C25 | 0.7372 (2) | 0.76024 (17) | 0.29377 (7) | 0.0219 (4) | |
H25 | 0.729760 | 0.752056 | 0.263507 | 0.026* | |
C2 | 0.6733 (2) | 0.36346 (16) | 0.37950 (7) | 0.0217 (4) | |
H2 | 0.685611 | 0.311102 | 0.358536 | 0.026* | |
C21 | 0.6194 (2) | 0.76877 (16) | 0.60888 (7) | 0.0202 (4) | |
H21 | 0.526164 | 0.796943 | 0.600356 | 0.024* | |
C24 | 0.8561 (2) | 0.81078 (16) | 0.31587 (7) | 0.0217 (4) | |
H24 | 0.930358 | 0.838190 | 0.300956 | 0.026* | |
C19 | 0.8188 (2) | 0.74132 (16) | 0.66385 (7) | 0.0227 (4) | |
H19 | 0.861245 | 0.749420 | 0.692732 | 0.027* | |
C20 | 0.6825 (2) | 0.78154 (17) | 0.65077 (7) | 0.0247 (4) | |
H20 | 0.631991 | 0.818131 | 0.670745 | 0.030* | |
C3 | 0.7451 (2) | 0.35530 (15) | 0.42056 (7) | 0.0216 (4) | |
H3 | 0.808152 | 0.297560 | 0.428217 | 0.026* | |
O3 | 0.2592 (13) | 0.9531 (12) | 0.2092 (3) | 0.060 (3) | 0.54 (2) |
O4 | 0.1845 (15) | 1.0198 (6) | 0.2704 (2) | 0.061 (2) | 0.54 (2) |
O2 | 0.0905 (8) | 0.8607 (9) | 0.2423 (3) | 0.087 (3) | 0.54 (2) |
O3A | 0.2646 (12) | 0.9837 (15) | 0.2166 (5) | 0.062 (4) | 0.46 (2) |
O4A | 0.1294 (12) | 0.9826 (13) | 0.2744 (2) | 0.053 (3) | 0.46 (2) |
O2A | 0.1196 (17) | 0.8454 (6) | 0.2258 (6) | 0.085 (5) | 0.46 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.01241 (11) | 0.01601 (12) | 0.01128 (12) | −0.00111 (9) | 0.00028 (9) | −0.00063 (9) |
Cl2 | 0.0235 (2) | 0.0274 (2) | 0.0151 (2) | −0.00382 (18) | 0.00064 (19) | −0.00390 (18) |
Cl1 | 0.0238 (2) | 0.0324 (3) | 0.0158 (2) | 0.00260 (19) | −0.00016 (19) | 0.0049 (2) |
O8 | 0.0349 (9) | 0.0294 (8) | 0.0202 (8) | −0.0002 (7) | 0.0036 (7) | −0.0005 (6) |
N2 | 0.0116 (7) | 0.0155 (7) | 0.0149 (8) | −0.0020 (6) | 0.0009 (6) | −0.0005 (6) |
N5 | 0.0146 (7) | 0.0167 (7) | 0.0132 (8) | −0.0023 (6) | 0.0006 (6) | 0.0001 (6) |
N3 | 0.0131 (7) | 0.0170 (7) | 0.0147 (8) | −0.0021 (6) | 0.0003 (6) | 0.0011 (6) |
N4 | 0.0140 (7) | 0.0178 (7) | 0.0137 (8) | −0.0005 (6) | −0.0002 (6) | −0.0006 (6) |
O7 | 0.0284 (8) | 0.0374 (9) | 0.0254 (9) | −0.0042 (7) | 0.0081 (7) | 0.0011 (7) |
O5 | 0.0242 (8) | 0.0382 (9) | 0.0303 (9) | 0.0025 (7) | 0.0078 (7) | −0.0003 (7) |
N1 | 0.0131 (7) | 0.0169 (7) | 0.0149 (8) | −0.0022 (6) | 0.0013 (6) | −0.0014 (6) |
N6 | 0.0151 (7) | 0.0163 (7) | 0.0127 (8) | −0.0003 (6) | 0.0008 (6) | 0.0001 (6) |
O6 | 0.0548 (12) | 0.0402 (10) | 0.0284 (10) | −0.0048 (8) | −0.0185 (9) | −0.0116 (8) |
O1 | 0.0499 (11) | 0.0502 (11) | 0.0260 (10) | 0.0235 (9) | −0.0090 (8) | 0.0041 (8) |
C11 | 0.0128 (8) | 0.0157 (8) | 0.0163 (10) | −0.0030 (6) | 0.0011 (7) | 0.0013 (7) |
C10 | 0.0113 (8) | 0.0160 (8) | 0.0144 (9) | −0.0016 (6) | 0.0022 (7) | 0.0007 (7) |
C6 | 0.0141 (8) | 0.0145 (8) | 0.0146 (9) | −0.0007 (6) | 0.0023 (7) | 0.0012 (7) |
C9 | 0.0172 (9) | 0.0152 (8) | 0.0152 (10) | −0.0008 (7) | 0.0029 (7) | −0.0007 (7) |
C31 | 0.0136 (8) | 0.0169 (9) | 0.0143 (10) | −0.0013 (7) | 0.0005 (7) | 0.0004 (7) |
C7 | 0.0147 (8) | 0.0161 (9) | 0.0166 (10) | −0.0004 (7) | −0.0002 (7) | 0.0025 (7) |
C32 | 0.0147 (8) | 0.0143 (8) | 0.0159 (10) | −0.0011 (6) | 0.0011 (7) | −0.0003 (7) |
C33 | 0.0159 (9) | 0.0197 (9) | 0.0188 (10) | −0.0015 (7) | 0.0004 (8) | −0.0039 (7) |
C22 | 0.0163 (9) | 0.0180 (9) | 0.0156 (10) | 0.0001 (7) | −0.0004 (7) | −0.0017 (7) |
C15 | 0.0165 (9) | 0.0212 (9) | 0.0159 (10) | −0.0017 (7) | −0.0017 (7) | 0.0033 (7) |
C26 | 0.0161 (9) | 0.0216 (9) | 0.0148 (10) | −0.0039 (7) | 0.0012 (7) | −0.0017 (7) |
C4 | 0.0176 (9) | 0.0197 (9) | 0.0192 (10) | 0.0001 (7) | 0.0015 (8) | 0.0023 (7) |
C28 | 0.0168 (9) | 0.0253 (10) | 0.0143 (10) | −0.0026 (7) | 0.0037 (8) | 0.0006 (7) |
C27 | 0.0147 (8) | 0.0191 (9) | 0.0162 (10) | −0.0027 (7) | 0.0015 (7) | 0.0009 (7) |
C12 | 0.0181 (9) | 0.0187 (9) | 0.0168 (10) | −0.0014 (7) | 0.0016 (8) | −0.0015 (7) |
C1 | 0.0164 (9) | 0.0208 (9) | 0.0184 (10) | −0.0019 (7) | 0.0020 (8) | −0.0037 (8) |
C5 | 0.0139 (8) | 0.0164 (8) | 0.0168 (10) | −0.0024 (7) | 0.0031 (7) | −0.0002 (7) |
C37 | 0.0186 (9) | 0.0169 (8) | 0.0128 (9) | −0.0038 (7) | −0.0006 (7) | −0.0002 (7) |
C16 | 0.0186 (9) | 0.0151 (8) | 0.0129 (9) | −0.0030 (7) | 0.0005 (7) | 0.0027 (7) |
C35 | 0.0188 (9) | 0.0204 (9) | 0.0210 (11) | −0.0020 (7) | 0.0083 (8) | −0.0023 (8) |
C8 | 0.0148 (8) | 0.0175 (9) | 0.0147 (10) | −0.0030 (7) | 0.0018 (7) | 0.0010 (7) |
C29 | 0.0180 (9) | 0.0191 (9) | 0.0142 (10) | −0.0009 (7) | −0.0001 (7) | −0.0005 (7) |
C36 | 0.0190 (9) | 0.0172 (9) | 0.0155 (10) | −0.0002 (7) | 0.0019 (7) | −0.0006 (7) |
C30 | 0.0149 (9) | 0.0196 (9) | 0.0166 (10) | −0.0024 (7) | −0.0010 (7) | −0.0005 (7) |
C34 | 0.0150 (9) | 0.0210 (9) | 0.0265 (11) | −0.0038 (7) | 0.0044 (8) | −0.0046 (8) |
C23 | 0.0136 (9) | 0.0192 (9) | 0.0229 (11) | −0.0021 (7) | −0.0005 (8) | −0.0013 (8) |
C41 | 0.0174 (9) | 0.0199 (9) | 0.0168 (10) | −0.0010 (7) | −0.0024 (8) | 0.0024 (7) |
C38 | 0.0167 (9) | 0.0199 (9) | 0.0177 (10) | −0.0012 (7) | −0.0016 (8) | −0.0001 (7) |
C17 | 0.0195 (9) | 0.0184 (9) | 0.0160 (10) | −0.0001 (7) | 0.0027 (8) | −0.0004 (7) |
C39 | 0.0201 (9) | 0.0204 (9) | 0.0171 (10) | −0.0003 (7) | 0.0017 (8) | −0.0016 (7) |
C40 | 0.0230 (10) | 0.0205 (9) | 0.0141 (10) | −0.0030 (7) | −0.0006 (8) | 0.0010 (7) |
C13 | 0.0184 (9) | 0.0171 (9) | 0.0283 (12) | 0.0018 (7) | 0.0033 (8) | 0.0004 (8) |
C42 | 0.0174 (9) | 0.0195 (9) | 0.0189 (10) | −0.0006 (7) | 0.0033 (8) | −0.0009 (7) |
C14 | 0.0173 (9) | 0.0195 (9) | 0.0233 (11) | 0.0012 (7) | −0.0006 (8) | 0.0058 (8) |
C18 | 0.0202 (9) | 0.0223 (10) | 0.0184 (10) | −0.0002 (7) | −0.0020 (8) | 0.0014 (8) |
C25 | 0.0185 (9) | 0.0324 (11) | 0.0154 (10) | −0.0045 (8) | 0.0039 (8) | −0.0011 (8) |
C2 | 0.0210 (10) | 0.0193 (9) | 0.0250 (11) | −0.0001 (7) | 0.0042 (8) | −0.0060 (8) |
C21 | 0.0201 (10) | 0.0240 (10) | 0.0165 (10) | 0.0006 (8) | 0.0024 (8) | 0.0022 (8) |
C24 | 0.0169 (9) | 0.0259 (10) | 0.0230 (11) | −0.0052 (8) | 0.0057 (8) | −0.0001 (8) |
C19 | 0.0273 (11) | 0.0276 (10) | 0.0125 (10) | −0.0028 (8) | −0.0012 (8) | 0.0019 (8) |
C20 | 0.0273 (11) | 0.0318 (11) | 0.0158 (10) | 0.0019 (9) | 0.0063 (9) | −0.0012 (8) |
C3 | 0.0200 (10) | 0.0170 (9) | 0.0278 (12) | 0.0024 (7) | 0.0037 (8) | −0.0016 (8) |
O3 | 0.057 (5) | 0.106 (8) | 0.022 (3) | 0.038 (4) | 0.017 (2) | 0.031 (3) |
O4 | 0.077 (5) | 0.050 (3) | 0.060 (3) | 0.026 (3) | 0.029 (3) | −0.004 (2) |
O2 | 0.053 (3) | 0.144 (7) | 0.067 (5) | −0.057 (4) | 0.019 (4) | −0.004 (4) |
O3A | 0.018 (3) | 0.095 (8) | 0.075 (8) | 0.002 (4) | 0.016 (4) | 0.060 (6) |
O4A | 0.040 (4) | 0.091 (7) | 0.030 (3) | 0.034 (4) | 0.011 (3) | 0.003 (3) |
O2A | 0.107 (8) | 0.049 (4) | 0.081 (8) | −0.029 (4) | −0.069 (6) | 0.012 (4) |
Ni1—N2 | 2.0014 (16) | C4—C3 | 1.390 (3) |
Ni1—N5 | 1.9956 (16) | C28—H28 | 0.9500 |
Ni1—N3 | 2.1174 (16) | C28—C27 | 1.385 (3) |
Ni1—N4 | 2.1313 (16) | C28—C29 | 1.394 (3) |
Ni1—N1 | 2.1263 (16) | C12—H12 | 0.9500 |
Ni1—N6 | 2.1148 (16) | C12—C13 | 1.389 (3) |
Cl2—O8 | 1.4552 (16) | C1—H1 | 0.9500 |
Cl2—O7 | 1.4325 (17) | C1—C2 | 1.387 (3) |
Cl2—O5 | 1.4468 (16) | C37—C29 | 1.485 (3) |
Cl2—O6 | 1.4306 (17) | C37—C38 | 1.396 (3) |
Cl1—O1 | 1.4239 (17) | C37—C42 | 1.398 (3) |
Cl1—O3 | 1.407 (8) | C16—C8 | 1.478 (3) |
Cl1—O4 | 1.447 (5) | C16—C17 | 1.404 (3) |
Cl1—O2 | 1.387 (8) | C16—C21 | 1.392 (3) |
Cl1—O3A | 1.394 (9) | C35—H35 | 0.9500 |
Cl1—O4A | 1.417 (6) | C35—C36 | 1.388 (3) |
Cl1—O2A | 1.443 (7) | C35—C34 | 1.377 (3) |
N2—C10 | 1.347 (2) | C29—C30 | 1.396 (3) |
N2—C6 | 1.342 (2) | C36—H36 | 0.9500 |
N5—C31 | 1.342 (2) | C30—H30 | 0.9500 |
N5—C27 | 1.342 (2) | C34—H34 | 0.9500 |
N3—C11 | 1.351 (2) | C23—H23 | 0.9500 |
N3—C15 | 1.340 (2) | C23—C24 | 1.377 (3) |
N4—C22 | 1.342 (2) | C41—H41 | 0.9500 |
N4—C26 | 1.355 (3) | C41—C40 | 1.389 (3) |
N1—C1 | 1.337 (2) | C41—C42 | 1.384 (3) |
N1—C5 | 1.359 (3) | C38—H38 | 0.9500 |
N6—C32 | 1.355 (2) | C38—C39 | 1.391 (3) |
N6—C36 | 1.335 (2) | C17—H17 | 0.9500 |
C11—C10 | 1.485 (3) | C17—C18 | 1.390 (3) |
C11—C12 | 1.388 (3) | C39—H39 | 0.9500 |
C10—C9 | 1.387 (3) | C39—C40 | 1.390 (3) |
C6—C7 | 1.382 (3) | C40—H40 | 0.9500 |
C6—C5 | 1.491 (3) | C13—H13 | 0.9500 |
C9—H9 | 0.9500 | C13—C14 | 1.385 (3) |
C9—C8 | 1.401 (3) | C42—H42 | 0.9500 |
C31—C32 | 1.485 (3) | C14—H14 | 0.9500 |
C31—C30 | 1.385 (3) | C18—H18 | 0.9500 |
C7—H7 | 0.9500 | C18—C19 | 1.385 (3) |
C7—C8 | 1.404 (3) | C25—H25 | 0.9500 |
C32—C33 | 1.387 (3) | C25—C24 | 1.392 (3) |
C33—H33 | 0.9500 | C2—H2 | 0.9500 |
C33—C34 | 1.386 (3) | C2—C3 | 1.383 (3) |
C22—H22 | 0.9500 | C21—H21 | 0.9500 |
C22—C23 | 1.389 (3) | C21—C20 | 1.384 (3) |
C15—H15 | 0.9500 | C24—H24 | 0.9500 |
C15—C14 | 1.386 (3) | C19—H19 | 0.9500 |
C26—C27 | 1.484 (3) | C19—C20 | 1.388 (3) |
C26—C25 | 1.381 (3) | C20—H20 | 0.9500 |
C4—H4 | 0.9500 | C3—H3 | 0.9500 |
C4—C5 | 1.387 (3) | ||
N2—Ni1—N3 | 77.49 (6) | C29—C28—H28 | 120.2 |
N2—Ni1—N4 | 101.35 (6) | N5—C27—C26 | 113.66 (17) |
N2—Ni1—N1 | 77.82 (6) | N5—C27—C28 | 120.86 (17) |
N2—Ni1—N6 | 103.39 (6) | C28—C27—C26 | 125.48 (17) |
N5—Ni1—N2 | 175.27 (6) | C11—C12—H12 | 120.3 |
N5—Ni1—N3 | 107.20 (6) | C11—C12—C13 | 119.32 (19) |
N5—Ni1—N4 | 77.68 (6) | C13—C12—H12 | 120.3 |
N5—Ni1—N1 | 97.51 (6) | N1—C1—H1 | 118.6 |
N5—Ni1—N6 | 77.80 (6) | N1—C1—C2 | 122.82 (19) |
N3—Ni1—N4 | 96.80 (6) | C2—C1—H1 | 118.6 |
N3—Ni1—N1 | 155.25 (6) | N1—C5—C6 | 114.67 (16) |
N1—Ni1—N4 | 89.75 (6) | N1—C5—C4 | 121.68 (18) |
N6—Ni1—N3 | 86.91 (6) | C4—C5—C6 | 123.63 (18) |
N6—Ni1—N4 | 155.20 (6) | C38—C37—C29 | 120.70 (17) |
N6—Ni1—N1 | 97.09 (6) | C38—C37—C42 | 119.30 (18) |
O7—Cl2—O8 | 109.18 (10) | C42—C37—C29 | 119.91 (17) |
O7—Cl2—O5 | 109.10 (10) | C17—C16—C8 | 120.36 (17) |
O5—Cl2—O8 | 109.41 (10) | C21—C16—C8 | 121.14 (17) |
O6—Cl2—O8 | 109.16 (10) | C21—C16—C17 | 118.48 (18) |
O6—Cl2—O7 | 110.83 (11) | C36—C35—H35 | 120.8 |
O6—Cl2—O5 | 109.14 (11) | C34—C35—H35 | 120.8 |
O1—Cl1—O4 | 107.5 (4) | C34—C35—C36 | 118.44 (19) |
O1—Cl1—O2A | 109.5 (4) | C9—C8—C7 | 117.73 (18) |
O3—Cl1—O1 | 109.5 (5) | C9—C8—C16 | 121.64 (17) |
O3—Cl1—O4 | 106.3 (6) | C7—C8—C16 | 120.59 (17) |
O2—Cl1—O1 | 111.7 (4) | C28—C29—C37 | 119.75 (17) |
O2—Cl1—O3 | 111.5 (6) | C28—C29—C30 | 118.76 (18) |
O2—Cl1—O4 | 110.1 (5) | C30—C29—C37 | 121.44 (17) |
O3A—Cl1—O1 | 111.4 (5) | N6—C36—C35 | 123.06 (19) |
O3A—Cl1—O4A | 112.3 (7) | N6—C36—H36 | 118.5 |
O3A—Cl1—O2A | 105.0 (7) | C35—C36—H36 | 118.5 |
O4A—Cl1—O1 | 111.1 (3) | C31—C30—C29 | 118.68 (17) |
O4A—Cl1—O2A | 107.2 (6) | C31—C30—H30 | 120.7 |
C10—N2—Ni1 | 119.70 (13) | C29—C30—H30 | 120.7 |
C6—N2—Ni1 | 119.55 (12) | C33—C34—H34 | 120.2 |
C6—N2—C10 | 120.63 (16) | C35—C34—C33 | 119.51 (18) |
C31—N5—Ni1 | 119.83 (13) | C35—C34—H34 | 120.2 |
C31—N5—C27 | 120.40 (17) | C22—C23—H23 | 120.4 |
C27—N5—Ni1 | 119.35 (13) | C24—C23—C22 | 119.15 (18) |
C11—N3—Ni1 | 114.82 (12) | C24—C23—H23 | 120.4 |
C15—N3—Ni1 | 126.11 (13) | C40—C41—H41 | 119.9 |
C15—N3—C11 | 118.69 (16) | C42—C41—H41 | 119.9 |
C22—N4—Ni1 | 127.86 (13) | C42—C41—C40 | 120.24 (18) |
C22—N4—C26 | 118.20 (16) | C37—C38—H38 | 120.0 |
C26—N4—Ni1 | 113.93 (12) | C39—C38—C37 | 119.92 (18) |
C1—N1—Ni1 | 127.21 (14) | C39—C38—H38 | 120.0 |
C1—N1—C5 | 118.43 (16) | C16—C17—H17 | 119.8 |
C5—N1—Ni1 | 113.78 (12) | C18—C17—C16 | 120.40 (19) |
C32—N6—Ni1 | 114.04 (12) | C18—C17—H17 | 119.8 |
C36—N6—Ni1 | 127.06 (13) | C38—C39—H39 | 119.8 |
C36—N6—C32 | 118.18 (16) | C40—C39—C38 | 120.42 (18) |
N3—C11—C10 | 114.42 (16) | C40—C39—H39 | 119.8 |
N3—C11—C12 | 121.72 (17) | C41—C40—C39 | 119.69 (19) |
C12—C11—C10 | 123.85 (18) | C41—C40—H40 | 120.2 |
N2—C10—C11 | 113.33 (16) | C39—C40—H40 | 120.2 |
N2—C10—C9 | 120.86 (17) | C12—C13—H13 | 120.6 |
C9—C10—C11 | 125.77 (16) | C14—C13—C12 | 118.75 (18) |
N2—C6—C7 | 121.19 (17) | C14—C13—H13 | 120.6 |
N2—C6—C5 | 113.53 (16) | C37—C42—H42 | 119.8 |
C7—C6—C5 | 125.28 (17) | C41—C42—C37 | 120.41 (18) |
C10—C9—H9 | 120.1 | C41—C42—H42 | 119.8 |
C10—C9—C8 | 119.76 (17) | C15—C14—H14 | 120.5 |
C8—C9—H9 | 120.1 | C13—C14—C15 | 118.98 (18) |
N5—C31—C32 | 112.85 (16) | C13—C14—H14 | 120.5 |
N5—C31—C30 | 121.69 (17) | C17—C18—H18 | 119.8 |
C30—C31—C32 | 125.46 (17) | C19—C18—C17 | 120.38 (19) |
C6—C7—H7 | 120.1 | C19—C18—H18 | 119.8 |
C6—C7—C8 | 119.77 (17) | C26—C25—H25 | 120.3 |
C8—C7—H7 | 120.1 | C26—C25—C24 | 119.34 (19) |
N6—C32—C31 | 114.91 (16) | C24—C25—H25 | 120.3 |
N6—C32—C33 | 122.05 (18) | C1—C2—H2 | 120.5 |
C33—C32—C31 | 123.00 (18) | C3—C2—C1 | 118.93 (19) |
C32—C33—H33 | 120.6 | C3—C2—H2 | 120.5 |
C34—C33—C32 | 118.75 (19) | C16—C21—H21 | 119.6 |
C34—C33—H33 | 120.6 | C20—C21—C16 | 120.78 (19) |
N4—C22—H22 | 118.7 | C20—C21—H21 | 119.6 |
N4—C22—C23 | 122.51 (19) | C23—C24—C25 | 118.72 (18) |
C23—C22—H22 | 118.7 | C23—C24—H24 | 120.6 |
N3—C15—H15 | 118.7 | C25—C24—H24 | 120.6 |
N3—C15—C14 | 122.54 (19) | C18—C19—H19 | 120.3 |
C14—C15—H15 | 118.7 | C18—C19—C20 | 119.4 (2) |
N4—C26—C27 | 114.62 (16) | C20—C19—H19 | 120.3 |
N4—C26—C25 | 122.07 (18) | C21—C20—C19 | 120.5 (2) |
C25—C26—C27 | 123.28 (18) | C21—C20—H20 | 119.7 |
C5—C4—H4 | 120.3 | C19—C20—H20 | 119.7 |
C5—C4—C3 | 119.32 (19) | C4—C3—H3 | 120.6 |
C3—C4—H4 | 120.3 | C2—C3—C4 | 118.81 (18) |
C27—C28—H28 | 120.2 | C2—C3—H3 | 120.6 |
C27—C28—C29 | 119.52 (18) | ||
Ni1—N2—C10—C11 | 2.4 (2) | C22—N4—C26—C25 | −1.0 (3) |
Ni1—N2—C10—C9 | −175.73 (13) | C22—C23—C24—C25 | −0.8 (3) |
Ni1—N2—C6—C7 | 175.37 (13) | C15—N3—C11—C10 | 178.71 (16) |
Ni1—N2—C6—C5 | −3.7 (2) | C15—N3—C11—C12 | −0.2 (3) |
Ni1—N5—C31—C32 | 7.4 (2) | C26—N4—C22—C23 | 0.9 (3) |
Ni1—N5—C31—C30 | −173.34 (14) | C26—C25—C24—C23 | 0.6 (3) |
Ni1—N5—C27—C26 | −10.1 (2) | C28—C29—C30—C31 | −0.1 (3) |
Ni1—N5—C27—C28 | 170.51 (14) | C27—N5—C31—C32 | 179.84 (16) |
Ni1—N3—C11—C10 | 5.28 (19) | C27—N5—C31—C30 | −0.9 (3) |
Ni1—N3—C11—C12 | −173.62 (14) | C27—C26—C25—C24 | 178.11 (19) |
Ni1—N3—C15—C14 | 172.82 (14) | C27—C28—C29—C37 | 174.92 (17) |
Ni1—N4—C22—C23 | −177.83 (14) | C27—C28—C29—C30 | −2.6 (3) |
Ni1—N4—C26—C27 | −0.2 (2) | C12—C11—C10—N2 | 173.82 (17) |
Ni1—N4—C26—C25 | 177.81 (16) | C12—C11—C10—C9 | −8.1 (3) |
Ni1—N1—C1—C2 | 170.22 (14) | C12—C13—C14—C15 | 0.5 (3) |
Ni1—N1—C5—C6 | 7.63 (19) | C1—N1—C5—C6 | 179.54 (16) |
Ni1—N1—C5—C4 | −171.35 (14) | C1—N1—C5—C4 | 0.6 (3) |
Ni1—N6—C32—C31 | 5.90 (19) | C1—C2—C3—C4 | 0.5 (3) |
Ni1—N6—C32—C33 | −171.75 (14) | C5—N1—C1—C2 | −0.5 (3) |
Ni1—N6—C36—C35 | 171.14 (14) | C5—C6—C7—C8 | 178.28 (17) |
N2—C10—C9—C8 | 1.3 (3) | C5—C4—C3—C2 | −0.4 (3) |
N2—C6—C7—C8 | −0.6 (3) | C37—C29—C30—C31 | −177.60 (17) |
N2—C6—C5—N1 | −3.0 (2) | C37—C38—C39—C40 | 0.4 (3) |
N2—C6—C5—C4 | 175.97 (17) | C16—C17—C18—C19 | −0.5 (3) |
N5—C31—C32—N6 | −8.5 (2) | C16—C21—C20—C19 | 0.2 (3) |
N5—C31—C32—C33 | 169.08 (17) | C8—C16—C17—C18 | 179.80 (17) |
N5—C31—C30—C29 | 1.9 (3) | C8—C16—C21—C20 | −179.63 (18) |
N3—C11—C10—N2 | −5.1 (2) | C29—C28—C27—N5 | 3.7 (3) |
N3—C11—C10—C9 | 172.98 (17) | C29—C28—C27—C26 | −175.53 (18) |
N3—C11—C12—C13 | 0.4 (3) | C29—C37—C38—C39 | −176.21 (17) |
N3—C15—C14—C13 | −0.4 (3) | C29—C37—C42—C41 | 175.59 (17) |
N4—C22—C23—C24 | 0.1 (3) | C36—N6—C32—C31 | 176.85 (16) |
N4—C26—C27—N5 | 6.3 (2) | C36—N6—C32—C33 | −0.8 (3) |
N4—C26—C27—C28 | −174.36 (18) | C36—C35—C34—C33 | −0.1 (3) |
N4—C26—C25—C24 | 0.3 (3) | C30—C31—C32—N6 | 172.21 (18) |
N1—C1—C2—C3 | 0.0 (3) | C30—C31—C32—C33 | −10.2 (3) |
N6—C32—C33—C34 | −0.3 (3) | C34—C35—C36—N6 | −1.1 (3) |
C11—N3—C15—C14 | 0.2 (3) | C38—C37—C29—C28 | 43.2 (3) |
C11—C10—C9—C8 | −176.58 (17) | C38—C37—C29—C30 | −139.3 (2) |
C11—C12—C13—C14 | −0.5 (3) | C38—C37—C42—C41 | −1.1 (3) |
C10—N2—C6—C7 | −0.7 (3) | C38—C39—C40—C41 | −0.6 (3) |
C10—N2—C6—C5 | −179.68 (15) | C17—C16—C8—C9 | −145.75 (19) |
C10—C11—C12—C13 | −178.43 (17) | C17—C16—C8—C7 | 31.7 (3) |
C10—C9—C8—C7 | −2.5 (3) | C17—C16—C21—C20 | −1.4 (3) |
C10—C9—C8—C16 | 175.05 (17) | C17—C18—C19—C20 | −0.7 (3) |
C6—N2—C10—C11 | 178.45 (16) | C40—C41—C42—C37 | 0.9 (3) |
C6—N2—C10—C9 | 0.3 (3) | C42—C37—C29—C28 | −133.4 (2) |
C6—C7—C8—C9 | 2.2 (3) | C42—C37—C29—C30 | 44.0 (3) |
C6—C7—C8—C16 | −175.42 (17) | C42—C37—C38—C39 | 0.5 (3) |
C31—N5—C27—C26 | 177.36 (16) | C42—C41—C40—C39 | −0.1 (3) |
C31—N5—C27—C28 | −2.0 (3) | C18—C19—C20—C21 | 0.8 (3) |
C31—C32—C33—C34 | −177.79 (17) | C25—C26—C27—N5 | −171.62 (19) |
C7—C6—C5—N1 | 178.03 (17) | C25—C26—C27—C28 | 7.7 (3) |
C7—C6—C5—C4 | −3.0 (3) | C21—C16—C8—C9 | 32.4 (3) |
C32—N6—C36—C35 | 1.5 (3) | C21—C16—C8—C7 | −150.07 (19) |
C32—C31—C30—C29 | −178.91 (18) | C21—C16—C17—C18 | 1.6 (3) |
C32—C33—C34—C35 | 0.8 (3) | C3—C4—C5—N1 | −0.1 (3) |
C22—N4—C26—C27 | −179.02 (16) | C3—C4—C5—C6 | −179.01 (18) |
15d | 17c | 15c | |
M—N1 | 2.1263 (15) | 2.2723 (12) | 2.2664 (12) |
M—N2 | 2.0014 (17) | 2.2093 (14) | 2.2080 (10) |
M—N3 | 2.1175 (15) | 2.2423 (12) | 2.2738 (11) |
M—N4 | 2.1313 (16) | 2.2537 (12) | 2.2375 (11) |
M—N5 | 1.9956 (17) | 2.1877 (11) | 2.2002 (10) |
M—N6 | 2.1147 (16) | 2.2571 (12) | 2.2970 (11) |
15d | 17c | 15c | |
N1—C5—N3—C11 | -8.59 | -10.072 | -3.66 |
N4—C26—N6—C32 | -4.5 | -3.412 | -0.47 |
C17—C16—C8—C7 | 31.77 | 31.98 | 5.23 |
C30—C29—C37—C42 | 43.24 | 40.09 | -27.63 |
Ring 1–Ring 2 | 7.28 | 8.496 | 1.49 |
Ring 3–Ring 4 | 14.39 | 14.38 | 16.63 |