The pentacoordinated [Cr(CO)5]2- dianion in [2,2,2-crypt-K]2[Cr(CO)5] ethylenediamine monosolvate
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270111018233/bi3018sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270111018233/bi3018Isup2.hkl |
CCDC reference: 833408
Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[K(C18H36N2O6)]2[Cr(CO)5]·C2H8N2 | Z = 1 |
Mr = 1083.33 | F(000) = 578 |
Triclinic, P1 | Dx = 1.326 Mg m−3 |
Hall symbol: P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.034 (3) Å | Cell parameters from 3395 reflections |
b = 11.741 (4) Å | θ = 3.3–27.5° |
c = 12.818 (3) Å | µ = 0.43 mm−1 |
α = 63.883 (7)° | T = 293 K |
β = 66.841 (10)° | Prism, red |
γ = 86.820 (13)° | 0.42 × 0.41 × 0.28 mm |
V = 1356.9 (7) Å3 |
Rigaku Saturn 70 CCD area-detector diffractometer | 7850 independent reflections |
Radiation source: fine-focus sealed tube | 5037 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
φ and ω scans | θmax = 27.5°, θmin = 2.5° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008) | h = −14→10 |
Tmin = 0.838, Tmax = 0.888 | k = −15→14 |
10684 measured reflections | l = −16→15 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.048 | H-atom parameters constrained |
wR(F2) = 0.120 | w = 1/[σ2(Fo2) + (0.0604P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.96 | (Δ/σ)max = 0.001 |
7850 reflections | Δρmax = 0.36 e Å−3 |
623 parameters | Δρmin = −0.28 e Å−3 |
3 restraints | Absolute structure: Flack (1983), with how many Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.49 (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. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Cr1 | 0.80701 (7) | 0.81576 (6) | 0.87888 (7) | 0.0552 (2) | |
K1 | 0.20830 (8) | 0.47631 (7) | 0.46529 (8) | 0.0497 (2) | |
K2 | 0.13116 (8) | 0.15982 (8) | 0.11966 (8) | 0.0494 (2) | |
O1 | 0.8992 (5) | 0.6286 (4) | 1.0730 (4) | 0.0998 (14) | |
O2 | 0.6560 (5) | 0.9025 (5) | 1.0769 (4) | 0.1049 (15) | |
O3 | 0.7004 (4) | 1.0345 (4) | 0.7177 (4) | 0.0862 (12) | |
O4 | 1.0958 (4) | 0.9069 (4) | 0.7017 (4) | 0.0912 (12) | |
O5 | 0.6768 (4) | 0.6096 (4) | 0.8637 (4) | 0.0958 (13) | |
O6 | 0.3662 (4) | 0.6916 (4) | 0.4149 (4) | 0.0812 (11) | |
O7 | 0.0917 (3) | 0.6581 (3) | 0.5440 (4) | 0.0720 (10) | |
O8 | 0.0950 (3) | 0.5281 (3) | 0.2902 (3) | 0.0640 (8) | |
O9 | 0.3582 (3) | 0.4736 (3) | 0.2269 (3) | 0.0585 (8) | |
O10 | 0.0385 (3) | 0.2551 (3) | 0.6718 (3) | 0.0615 (8) | |
O11 | 0.3106 (3) | 0.2768 (3) | 0.6247 (3) | 0.0658 (9) | |
O12 | 0.2472 (3) | 0.1148 (3) | 0.2938 (3) | 0.0563 (7) | |
O13 | −0.0182 (3) | 0.1629 (3) | 0.3578 (3) | 0.0570 (8) | |
O14 | 0.0233 (4) | 0.3521 (3) | −0.0386 (3) | 0.0659 (9) | |
O15 | 0.2957 (3) | 0.3905 (3) | −0.0877 (3) | 0.0697 (9) | |
O16 | 0.2582 (4) | −0.0109 (3) | 0.0249 (4) | 0.0732 (10) | |
O17 | −0.0169 (4) | −0.0621 (3) | 0.1745 (4) | 0.0793 (11) | |
N1 | 0.5008 (4) | 0.4781 (4) | 0.3793 (4) | 0.0603 (10) | |
N2 | −0.0813 (4) | 0.4743 (4) | 0.5546 (4) | 0.0555 (9) | |
N3 | 0.4215 (4) | 0.1744 (4) | 0.0292 (4) | 0.0585 (10) | |
N4 | −0.1582 (4) | 0.1466 (4) | 0.2085 (4) | 0.0570 (10) | |
C1 | 0.8633 (5) | 0.6991 (4) | 0.9975 (5) | 0.0636 (12) | |
C2 | 0.7159 (6) | 0.8695 (5) | 0.9985 (5) | 0.0698 (13) | |
C3 | 0.7445 (5) | 0.9479 (5) | 0.7768 (4) | 0.0617 (12) | |
C4 | 0.9811 (5) | 0.8732 (5) | 0.7690 (5) | 0.0669 (13) | |
C5 | 0.7278 (5) | 0.6913 (5) | 0.8690 (4) | 0.0672 (12) | |
C6 | 0.5637 (5) | 0.6098 (5) | 0.3279 (6) | 0.0762 (15) | |
H6A | 0.5628 | 0.6616 | 0.2429 | 0.091* | |
H6B | 0.6579 | 0.6077 | 0.3157 | 0.091* | |
C7 | 0.4994 (6) | 0.6755 (6) | 0.4087 (7) | 0.092 (2) | |
H7A | 0.4956 | 0.6235 | 0.4954 | 0.111* | |
H7B | 0.5520 | 0.7601 | 0.3713 | 0.111* | |
C8 | 0.3033 (6) | 0.7609 (5) | 0.4817 (6) | 0.0787 (16) | |
H8A | 0.3574 | 0.8456 | 0.4405 | 0.094* | |
H8B | 0.2961 | 0.7144 | 0.5702 | 0.094* | |
C9 | 0.1719 (7) | 0.7786 (5) | 0.4835 (6) | 0.0807 (16) | |
H9A | 0.1295 | 0.8289 | 0.5299 | 0.097* | |
H9B | 0.1792 | 0.8271 | 0.3951 | 0.097* | |
C10 | −0.0433 (7) | 0.6742 (6) | 0.5664 (7) | 0.0855 (18) | |
H10A | −0.0504 | 0.7282 | 0.4847 | 0.103* | |
H10B | −0.0774 | 0.7174 | 0.6215 | 0.103* | |
C11 | −0.1241 (5) | 0.5442 (6) | 0.6307 (6) | 0.0809 (17) | |
H11A | −0.1176 | 0.4924 | 0.7131 | 0.097* | |
H11B | −0.2187 | 0.5549 | 0.6491 | 0.097* | |
C12 | −0.1127 (6) | 0.5363 (6) | 0.4412 (6) | 0.0738 (14) | |
H12A | −0.0870 | 0.6301 | 0.4019 | 0.089* | |
H12B | −0.2102 | 0.5199 | 0.4696 | 0.089* | |
C13 | −0.0450 (6) | 0.4920 (5) | 0.3423 (5) | 0.0722 (14) | |
H13A | −0.0660 | 0.3977 | 0.3810 | 0.087* | |
H13B | −0.0774 | 0.5312 | 0.2739 | 0.087* | |
C14 | 0.1638 (6) | 0.5027 (5) | 0.1860 (5) | 0.0699 (14) | |
H14A | 0.1313 | 0.5497 | 0.1186 | 0.084* | |
H14B | 0.1464 | 0.4099 | 0.2135 | 0.084* | |
C15 | 0.3075 (6) | 0.5424 (5) | 0.1348 (5) | 0.0746 (16) | |
H15A | 0.3541 | 0.5277 | 0.0592 | 0.090* | |
H15B | 0.3245 | 0.6353 | 0.1074 | 0.090* | |
C16 | 0.5002 (5) | 0.5040 (5) | 0.1760 (5) | 0.0721 (15) | |
H16A | 0.5251 | 0.5979 | 0.1365 | 0.086* | |
H16B | 0.5432 | 0.4758 | 0.1092 | 0.086* | |
C17 | 0.5476 (5) | 0.4395 (5) | 0.2784 (5) | 0.0674 (14) | |
H17A | 0.5204 | 0.3461 | 0.3174 | 0.081* | |
H17B | 0.6462 | 0.4553 | 0.2389 | 0.081* | |
C18 | −0.1483 (5) | 0.3414 (5) | 0.6316 (5) | 0.0674 (13) | |
H18A | −0.1347 | 0.3018 | 0.5745 | 0.081* | |
H18B | −0.2451 | 0.3416 | 0.6735 | 0.081* | |
C19 | −0.0999 (5) | 0.2614 (5) | 0.7313 (5) | 0.0704 (14) | |
H19A | −0.1138 | 0.2993 | 0.7898 | 0.085* | |
H19B | −0.1507 | 0.1740 | 0.7818 | 0.085* | |
C20 | 0.0860 (5) | 0.1744 (5) | 0.7650 (5) | 0.0685 (13) | |
H20A | 0.0290 | 0.0900 | 0.8193 | 0.082* | |
H20B | 0.0826 | 0.2136 | 0.8203 | 0.082* | |
C21 | 0.2246 (5) | 0.1578 (5) | 0.6994 (5) | 0.0717 (14) | |
H21A | 0.2563 | 0.0981 | 0.7634 | 0.086* | |
H21B | 0.2273 | 0.1194 | 0.6436 | 0.086* | |
C22 | 0.4439 (6) | 0.2624 (6) | 0.5663 (6) | 0.0811 (17) | |
H22A | 0.4511 | 0.2211 | 0.5118 | 0.097* | |
H22B | 0.4750 | 0.2065 | 0.6324 | 0.097* | |
C23 | 0.5292 (5) | 0.3892 (6) | 0.4875 (5) | 0.0753 (15) | |
H23A | 0.5190 | 0.4300 | 0.5430 | 0.090* | |
H23B | 0.6233 | 0.3754 | 0.4548 | 0.090* | |
C24 | 0.4542 (5) | 0.1093 (5) | 0.1391 (5) | 0.0673 (13) | |
H24A | 0.5519 | 0.1255 | 0.1098 | 0.081* | |
H24B | 0.4287 | 0.0159 | 0.1757 | 0.081* | |
C25 | 0.3873 (5) | 0.1497 (5) | 0.2426 (6) | 0.0691 (14) | |
H25A | 0.4197 | 0.1070 | 0.3106 | 0.083* | |
H25B | 0.4089 | 0.2436 | 0.2070 | 0.083* | |
C26 | 0.1767 (5) | 0.1420 (5) | 0.3985 (5) | 0.0651 (13) | |
H26A | 0.1910 | 0.2355 | 0.3693 | 0.078* | |
H26B | 0.2111 | 0.0987 | 0.4650 | 0.078* | |
C27 | 0.0333 (5) | 0.0972 (5) | 0.4523 (4) | 0.0620 (12) | |
H27A | 0.0189 | 0.0038 | 0.4816 | 0.074* | |
H27B | −0.0145 | 0.1136 | 0.5267 | 0.074* | |
C28 | −0.1573 (5) | 0.1270 (6) | 0.4095 (5) | 0.0721 (14) | |
H28A | −0.2024 | 0.1536 | 0.4772 | 0.087* | |
H28B | −0.1779 | 0.0326 | 0.4483 | 0.087* | |
C29 | −0.2072 (5) | 0.1885 (6) | 0.3081 (5) | 0.0710 (14) | |
H29A | −0.3057 | 0.1709 | 0.3483 | 0.085* | |
H29B | −0.1817 | 0.2824 | 0.2675 | 0.085* | |
C30 | −0.1935 (6) | 0.2320 (5) | 0.1014 (6) | 0.0734 (14) | |
H30A | −0.2888 | 0.2415 | 0.1364 | 0.088* | |
H30B | −0.1813 | 0.1909 | 0.0457 | 0.088* | |
C31 | −0.1117 (6) | 0.3634 (5) | 0.0219 (6) | 0.0735 (14) | |
H31A | −0.1447 | 0.4179 | −0.0431 | 0.088* | |
H31B | −0.1202 | 0.4043 | 0.0770 | 0.088* | |
C32 | 0.1058 (6) | 0.4737 (5) | −0.1173 (5) | 0.0767 (15) | |
H32A | 0.1013 | 0.5165 | −0.0646 | 0.092* | |
H32B | 0.0734 | 0.5288 | −0.1825 | 0.092* | |
C33 | 0.2440 (6) | 0.4571 (5) | −0.1799 (5) | 0.0754 (15) | |
H33A | 0.2476 | 0.4084 | −0.2272 | 0.091* | |
H33B | 0.2986 | 0.5420 | −0.2416 | 0.091* | |
C34 | 0.4351 (6) | 0.3892 (5) | −0.1444 (6) | 0.0831 (18) | |
H34A | 0.4826 | 0.4778 | −0.1911 | 0.100* | |
H34B | 0.4547 | 0.3545 | −0.2062 | 0.100* | |
C35 | 0.4827 (5) | 0.3092 (5) | −0.0449 (6) | 0.0805 (17) | |
H35A | 0.5803 | 0.3127 | −0.0863 | 0.097* | |
H35B | 0.4650 | 0.3467 | 0.0145 | 0.097* | |
C36 | 0.4675 (5) | 0.1079 (5) | −0.0498 (5) | 0.0695 (14) | |
H36A | 0.5628 | 0.1003 | −0.0689 | 0.083* | |
H36B | 0.4606 | 0.1613 | −0.1318 | 0.083* | |
C37 | 0.3942 (6) | −0.0207 (6) | 0.0074 (6) | 0.0760 (15) | |
H37A | 0.4358 | −0.0614 | −0.0489 | 0.091* | |
H37B | 0.3980 | −0.0749 | 0.0907 | 0.091* | |
C38 | 0.1836 (6) | −0.1330 (5) | 0.0871 (6) | 0.0826 (17) | |
H38A | 0.1804 | −0.1798 | 0.1742 | 0.099* | |
H38B | 0.2271 | −0.1824 | 0.0400 | 0.099* | |
C39 | 0.0506 (7) | −0.1219 (5) | 0.0942 (6) | 0.0852 (18) | |
H39A | 0.0018 | −0.2079 | 0.1298 | 0.102* | |
H39B | 0.0536 | −0.0696 | 0.0077 | 0.102* | |
C40 | −0.1469 (6) | −0.0489 (6) | 0.1761 (7) | 0.0891 (18) | |
H40A | −0.1965 | −0.1344 | 0.2110 | 0.107* | |
H40B | −0.1400 | 0.0031 | 0.0882 | 0.107* | |
C41 | −0.2196 (5) | 0.0150 (5) | 0.2571 (6) | 0.0760 (15) | |
H41A | −0.3120 | 0.0171 | 0.2637 | 0.091* | |
H41B | −0.2239 | −0.0373 | 0.3440 | 0.091* | |
N5 | 0.3144 (13) | 0.7557 (10) | 0.8075 (11) | 0.218 (5) | |
H51 | 0.2610 | 0.7377 | 0.8876 | 0.327* | |
H52 | 0.2705 | 0.7901 | 0.7582 | 0.327* | |
N6 | 0.6100 (12) | 0.8010 (12) | 0.6106 (10) | 0.216 (5) | |
H61 | 0.5744 | 0.7203 | 0.6430 | 0.324* | |
H62 | 0.6595 | 0.8043 | 0.6500 | 0.324* | |
C42 | 0.4196 (9) | 0.8366 (13) | 0.7623 (13) | 0.169 (5) | |
H42A | 0.4702 | 0.7970 | 0.8153 | 0.203* | |
H42B | 0.3896 | 0.9133 | 0.7731 | 0.203* | |
C43 | 0.5086 (15) | 0.8783 (13) | 0.6327 (13) | 0.192 (5) | |
H43A | 0.5516 | 0.9666 | 0.5981 | 0.230* | |
H43B | 0.4562 | 0.8819 | 0.5842 | 0.230* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.0637 (5) | 0.0497 (4) | 0.0437 (4) | 0.0022 (3) | −0.0199 (3) | −0.0155 (3) |
K1 | 0.0513 (6) | 0.0453 (5) | 0.0477 (5) | 0.0013 (4) | −0.0150 (4) | −0.0213 (4) |
K2 | 0.0492 (6) | 0.0468 (5) | 0.0494 (5) | 0.0045 (4) | −0.0166 (4) | −0.0224 (4) |
O1 | 0.143 (4) | 0.081 (3) | 0.097 (3) | 0.048 (3) | −0.080 (3) | −0.036 (2) |
O2 | 0.138 (4) | 0.126 (4) | 0.097 (3) | 0.077 (3) | −0.069 (3) | −0.078 (3) |
O3 | 0.102 (3) | 0.079 (3) | 0.061 (2) | 0.024 (2) | −0.036 (2) | −0.016 (2) |
O4 | 0.065 (2) | 0.095 (3) | 0.082 (3) | −0.0093 (19) | −0.017 (2) | −0.024 (2) |
O5 | 0.115 (3) | 0.096 (3) | 0.070 (2) | −0.027 (2) | −0.016 (2) | −0.047 (2) |
O6 | 0.066 (3) | 0.080 (2) | 0.108 (3) | −0.0031 (17) | −0.0214 (19) | −0.061 (2) |
O7 | 0.070 (2) | 0.0508 (19) | 0.093 (3) | 0.0121 (15) | −0.0247 (18) | −0.0397 (19) |
O8 | 0.072 (2) | 0.071 (2) | 0.0575 (19) | 0.0138 (16) | −0.0331 (16) | −0.0315 (17) |
O9 | 0.068 (2) | 0.0500 (17) | 0.0420 (16) | 0.0069 (14) | −0.0163 (13) | −0.0136 (14) |
O10 | 0.066 (2) | 0.0502 (17) | 0.0475 (17) | −0.0016 (14) | −0.0173 (14) | −0.0094 (14) |
O11 | 0.066 (2) | 0.0565 (19) | 0.064 (2) | 0.0077 (15) | −0.0249 (16) | −0.0203 (17) |
O12 | 0.056 (2) | 0.0640 (19) | 0.0538 (17) | 0.0062 (14) | −0.0233 (14) | −0.0298 (15) |
O13 | 0.061 (2) | 0.0561 (18) | 0.0423 (16) | 0.0098 (14) | −0.0191 (13) | −0.0153 (14) |
O14 | 0.074 (2) | 0.0536 (18) | 0.065 (2) | 0.0093 (15) | −0.0297 (17) | −0.0214 (17) |
O15 | 0.074 (2) | 0.0560 (19) | 0.0502 (18) | −0.0008 (15) | −0.0156 (15) | −0.0079 (16) |
O16 | 0.080 (3) | 0.0495 (19) | 0.088 (3) | 0.0058 (16) | −0.0248 (18) | −0.0378 (19) |
O17 | 0.056 (2) | 0.060 (2) | 0.119 (3) | 0.0019 (15) | −0.0267 (19) | −0.047 (2) |
N1 | 0.046 (2) | 0.057 (2) | 0.073 (3) | −0.0009 (17) | −0.0161 (18) | −0.033 (2) |
N2 | 0.048 (2) | 0.056 (2) | 0.058 (2) | 0.0056 (16) | −0.0178 (16) | −0.0249 (19) |
N3 | 0.052 (2) | 0.053 (2) | 0.070 (2) | 0.0079 (16) | −0.0190 (18) | −0.032 (2) |
N4 | 0.050 (2) | 0.057 (2) | 0.054 (2) | 0.0020 (17) | −0.0144 (17) | −0.0225 (19) |
C1 | 0.081 (3) | 0.054 (3) | 0.059 (3) | 0.012 (2) | −0.027 (2) | −0.030 (2) |
C2 | 0.097 (4) | 0.066 (3) | 0.061 (3) | 0.034 (3) | −0.048 (3) | −0.030 (2) |
C3 | 0.061 (3) | 0.068 (3) | 0.044 (2) | 0.001 (2) | −0.0121 (19) | −0.022 (2) |
C4 | 0.072 (4) | 0.066 (3) | 0.051 (3) | −0.001 (2) | −0.023 (2) | −0.017 (2) |
C5 | 0.081 (3) | 0.064 (3) | 0.043 (2) | −0.006 (2) | −0.016 (2) | −0.020 (2) |
C6 | 0.055 (3) | 0.075 (3) | 0.094 (4) | −0.011 (2) | −0.017 (3) | −0.043 (3) |
C7 | 0.077 (5) | 0.082 (4) | 0.119 (5) | −0.018 (3) | −0.027 (3) | −0.056 (4) |
C8 | 0.094 (5) | 0.052 (3) | 0.089 (4) | −0.003 (3) | −0.034 (3) | −0.032 (3) |
C9 | 0.111 (5) | 0.044 (3) | 0.088 (4) | 0.009 (3) | −0.040 (3) | −0.032 (3) |
C10 | 0.094 (5) | 0.070 (3) | 0.102 (5) | 0.021 (3) | −0.028 (3) | −0.058 (3) |
C11 | 0.066 (4) | 0.085 (4) | 0.082 (4) | 0.008 (3) | −0.007 (3) | −0.050 (3) |
C12 | 0.060 (3) | 0.077 (4) | 0.080 (4) | 0.015 (3) | −0.036 (3) | −0.027 (3) |
C13 | 0.078 (4) | 0.075 (3) | 0.073 (3) | 0.011 (3) | −0.052 (3) | −0.024 (3) |
C14 | 0.104 (4) | 0.067 (3) | 0.055 (3) | 0.034 (3) | −0.049 (3) | −0.029 (2) |
C15 | 0.110 (5) | 0.060 (3) | 0.045 (3) | 0.034 (3) | −0.030 (3) | −0.021 (2) |
C16 | 0.065 (3) | 0.066 (3) | 0.058 (3) | −0.009 (2) | 0.004 (2) | −0.028 (3) |
C17 | 0.051 (3) | 0.069 (3) | 0.079 (4) | 0.008 (2) | −0.012 (2) | −0.044 (3) |
C18 | 0.051 (3) | 0.069 (3) | 0.062 (3) | −0.009 (2) | −0.013 (2) | −0.021 (3) |
C19 | 0.060 (3) | 0.067 (3) | 0.052 (3) | −0.012 (2) | −0.006 (2) | −0.013 (2) |
C20 | 0.082 (4) | 0.057 (3) | 0.053 (3) | −0.003 (2) | −0.026 (2) | −0.015 (2) |
C21 | 0.094 (4) | 0.051 (3) | 0.064 (3) | 0.006 (2) | −0.038 (3) | −0.017 (2) |
C22 | 0.080 (4) | 0.079 (4) | 0.084 (4) | 0.025 (3) | −0.047 (3) | −0.028 (3) |
C23 | 0.053 (3) | 0.091 (4) | 0.081 (4) | 0.004 (3) | −0.029 (3) | −0.036 (3) |
C24 | 0.050 (3) | 0.077 (3) | 0.086 (4) | 0.018 (2) | −0.034 (2) | −0.042 (3) |
C25 | 0.053 (3) | 0.077 (3) | 0.082 (4) | 0.002 (2) | −0.027 (2) | −0.040 (3) |
C26 | 0.085 (4) | 0.063 (3) | 0.057 (3) | 0.015 (3) | −0.037 (2) | −0.029 (2) |
C27 | 0.074 (3) | 0.053 (3) | 0.042 (2) | 0.011 (2) | −0.020 (2) | −0.012 (2) |
C28 | 0.064 (3) | 0.086 (4) | 0.054 (3) | 0.008 (3) | −0.013 (2) | −0.032 (3) |
C29 | 0.048 (3) | 0.086 (4) | 0.074 (3) | 0.018 (2) | −0.024 (2) | −0.035 (3) |
C30 | 0.066 (4) | 0.079 (4) | 0.081 (4) | 0.017 (3) | −0.043 (3) | −0.031 (3) |
C31 | 0.078 (4) | 0.072 (3) | 0.076 (3) | 0.020 (3) | −0.044 (3) | −0.029 (3) |
C32 | 0.097 (5) | 0.048 (3) | 0.071 (3) | 0.005 (3) | −0.044 (3) | −0.007 (2) |
C33 | 0.088 (4) | 0.057 (3) | 0.058 (3) | −0.008 (3) | −0.022 (3) | −0.010 (2) |
C34 | 0.072 (4) | 0.057 (3) | 0.070 (3) | −0.004 (2) | −0.001 (3) | −0.012 (3) |
C35 | 0.050 (3) | 0.059 (3) | 0.099 (4) | −0.009 (2) | −0.006 (3) | −0.029 (3) |
C36 | 0.059 (3) | 0.079 (3) | 0.065 (3) | 0.011 (2) | −0.011 (2) | −0.041 (3) |
C37 | 0.067 (4) | 0.081 (4) | 0.095 (4) | 0.033 (3) | −0.030 (3) | −0.058 (3) |
C38 | 0.085 (4) | 0.063 (3) | 0.104 (5) | 0.010 (3) | −0.030 (3) | −0.050 (3) |
C39 | 0.124 (6) | 0.052 (3) | 0.093 (4) | 0.002 (3) | −0.051 (4) | −0.037 (3) |
C40 | 0.074 (4) | 0.079 (4) | 0.115 (5) | −0.008 (3) | −0.034 (3) | −0.046 (4) |
C41 | 0.051 (3) | 0.066 (3) | 0.088 (4) | −0.006 (2) | −0.015 (2) | −0.026 (3) |
N5 | 0.217 (12) | 0.187 (10) | 0.174 (10) | −0.020 (8) | −0.078 (8) | −0.017 (8) |
N6 | 0.260 (12) | 0.242 (12) | 0.125 (8) | 0.080 (10) | −0.045 (7) | −0.100 (8) |
C42 | 0.073 (6) | 0.232 (12) | 0.196 (12) | −0.021 (6) | −0.020 (6) | −0.119 (10) |
C43 | 0.196 (12) | 0.197 (13) | 0.166 (12) | −0.032 (10) | −0.032 (10) | −0.099 (11) |
Cr1—C1 | 1.841 (5) | C14—C15 | 1.468 (8) |
Cr1—C2 | 1.824 (5) | C14—H14A | 0.9900 |
Cr1—C3 | 1.844 (5) | C14—H14B | 0.9900 |
Cr1—C4 | 1.819 (5) | C15—H15A | 0.9900 |
Cr1—C5 | 1.818 (5) | C15—H15B | 0.9900 |
K1—O7 | 2.793 (3) | C16—C17 | 1.480 (8) |
K1—O10 | 2.802 (3) | C16—H16A | 0.9900 |
K1—O8 | 2.809 (4) | C16—H16B | 0.9900 |
K1—O6 | 2.830 (4) | C17—H17A | 0.9900 |
K1—O9 | 2.860 (3) | C17—H17B | 0.9900 |
K1—O11 | 2.872 (4) | C18—C19 | 1.491 (8) |
K1—N2 | 2.938 (4) | C18—H18A | 0.9900 |
K1—N1 | 2.970 (4) | C18—H18B | 0.9900 |
K2—O17 | 2.812 (4) | C19—H19A | 0.9900 |
K2—O16 | 2.820 (3) | C19—H19B | 0.9900 |
K2—O12 | 2.834 (3) | C20—C21 | 1.478 (7) |
K2—O15 | 2.848 (3) | C20—H20A | 0.9900 |
K2—O13 | 2.858 (3) | C20—H20B | 0.9900 |
K2—O14 | 2.863 (4) | C21—H21A | 0.9900 |
K2—N4 | 2.925 (4) | C21—H21B | 0.9900 |
K2—N3 | 2.933 (4) | C22—C23 | 1.485 (8) |
O1—C1 | 1.157 (6) | C22—H22A | 0.9900 |
O2—C2 | 1.179 (6) | C22—H22B | 0.9900 |
O3—C3 | 1.184 (6) | C23—H23A | 0.9900 |
O4—C4 | 1.183 (6) | C23—H23B | 0.9900 |
O5—C5 | 1.178 (6) | C24—C25 | 1.508 (7) |
O6—C8 | 1.400 (6) | C24—H24A | 0.9900 |
O6—C7 | 1.447 (8) | C24—H24B | 0.9900 |
O7—C10 | 1.421 (7) | C25—H25A | 0.9900 |
O7—C9 | 1.421 (6) | C25—H25B | 0.9900 |
O8—C14 | 1.405 (6) | C26—C27 | 1.474 (7) |
O8—C13 | 1.423 (6) | C26—H26A | 0.9900 |
O9—C15 | 1.410 (6) | C26—H26B | 0.9900 |
O9—C16 | 1.436 (6) | C27—H27A | 0.9900 |
O10—C19 | 1.428 (6) | C27—H27B | 0.9900 |
O10—C20 | 1.429 (6) | C28—C29 | 1.486 (7) |
O11—C22 | 1.404 (6) | C28—H28A | 0.9900 |
O11—C21 | 1.423 (6) | C28—H28B | 0.9900 |
O12—C25 | 1.423 (6) | C29—H29A | 0.9900 |
O12—C26 | 1.427 (5) | C29—H29B | 0.9900 |
O13—C28 | 1.413 (6) | C30—C31 | 1.510 (8) |
O13—C27 | 1.434 (6) | C30—H30A | 0.9900 |
O14—C31 | 1.414 (6) | C30—H30B | 0.9900 |
O14—C32 | 1.428 (6) | C31—H31A | 0.9900 |
O15—C33 | 1.414 (7) | C31—H31B | 0.9900 |
O15—C34 | 1.422 (6) | C32—C33 | 1.466 (7) |
O16—C38 | 1.406 (6) | C32—H32A | 0.9900 |
O16—C37 | 1.433 (7) | C32—H32B | 0.9900 |
O17—C40 | 1.428 (7) | C33—H33A | 0.9900 |
O17—C39 | 1.443 (7) | C33—H33B | 0.9900 |
N1—C17 | 1.452 (6) | C34—C35 | 1.484 (9) |
N1—C23 | 1.463 (7) | C34—H34A | 0.9900 |
N1—C6 | 1.473 (6) | C34—H34B | 0.9900 |
N2—C11 | 1.466 (6) | C35—H35A | 0.9900 |
N2—C18 | 1.467 (6) | C35—H35B | 0.9900 |
N2—C12 | 1.482 (7) | C36—C37 | 1.472 (8) |
N3—C24 | 1.456 (7) | C36—H36A | 0.9900 |
N3—C36 | 1.462 (6) | C36—H36B | 0.9900 |
N3—C35 | 1.467 (6) | C37—H37A | 0.9900 |
N4—C29 | 1.465 (6) | C37—H37B | 0.9900 |
N4—C41 | 1.473 (6) | C38—C39 | 1.436 (9) |
N4—C30 | 1.485 (7) | C38—H38A | 0.9900 |
C6—C7 | 1.495 (8) | C38—H38B | 0.9900 |
C6—H6A | 0.9900 | C39—H39A | 0.9900 |
C6—H6B | 0.9900 | C39—H39B | 0.9900 |
C7—H7A | 0.9900 | C40—C41 | 1.499 (8) |
C7—H7B | 0.9900 | C40—H40A | 0.9900 |
C8—C9 | 1.445 (9) | C40—H40B | 0.9900 |
C8—H8A | 0.9900 | C41—H41A | 0.9900 |
C8—H8B | 0.9900 | C41—H41B | 0.9900 |
C9—H9A | 0.9900 | N5—C42 | 1.301 (12) |
C9—H9B | 0.9900 | N5—H51 | 0.8900 |
C10—C11 | 1.506 (8) | N5—H52 | 0.8900 |
C10—H10A | 0.9900 | N6—C43 | 1.421 (16) |
C10—H10B | 0.9900 | N6—H61 | 0.8900 |
C11—H11A | 0.9900 | N6—H62 | 0.8900 |
C11—H11B | 0.9900 | C42—C43 | 1.420 (15) |
C12—C13 | 1.493 (8) | C42—H42A | 0.9900 |
C12—H12A | 0.9900 | C42—H42B | 0.9900 |
C12—H12B | 0.9900 | C43—H43A | 0.9900 |
C13—H13A | 0.9900 | C43—H43B | 0.9900 |
C13—H13B | 0.9900 | ||
C1—Cr1—C2 | 86.4 (2) | C15—C14—H14B | 109.6 |
C1—Cr1—C3 | 170.0 (2) | H14A—C14—H14B | 108.1 |
C1—Cr1—C4 | 88.1 (2) | O9—C15—C14 | 111.1 (4) |
C1—Cr1—C5 | 93.0 (2) | O9—C15—H15A | 109.4 |
C2—Cr1—C3 | 84.2 (2) | C14—C15—H15A | 109.4 |
C2—Cr1—C4 | 124.0 (3) | O9—C15—H15B | 109.4 |
C2—Cr1—C5 | 120.5 (2) | C14—C15—H15B | 109.4 |
C3—Cr1—C4 | 94.3 (2) | H15A—C15—H15B | 108.0 |
C3—Cr1—C5 | 94.8 (2) | O9—C16—C17 | 110.3 (4) |
C4—Cr1—C5 | 115.4 (2) | O9—C16—H16A | 109.6 |
O7—K1—O10 | 99.17 (11) | C17—C16—H16A | 109.6 |
O7—K1—O8 | 95.49 (11) | O9—C16—H16B | 109.6 |
O10—K1—O8 | 100.50 (11) | C17—C16—H16B | 109.6 |
O7—K1—O6 | 59.06 (11) | H16A—C16—H16B | 108.1 |
O10—K1—O6 | 140.06 (12) | N1—C17—C16 | 116.2 (4) |
O8—K1—O6 | 113.74 (12) | N1—C17—H17A | 108.2 |
O7—K1—O9 | 136.20 (10) | C16—C17—H17A | 108.2 |
O10—K1—O9 | 119.21 (10) | N1—C17—H17B | 108.2 |
O8—K1—O9 | 59.42 (10) | C16—C17—H17B | 108.2 |
O6—K1—O9 | 96.41 (10) | H17A—C17—H17B | 107.4 |
O7—K1—O11 | 118.25 (12) | N2—C18—C19 | 113.6 (4) |
O10—K1—O11 | 59.67 (10) | N2—C18—H18A | 108.8 |
O8—K1—O11 | 142.06 (10) | C19—C18—H18A | 108.8 |
O6—K1—O11 | 99.12 (13) | N2—C18—H18B | 108.8 |
O9—K1—O11 | 100.00 (10) | C19—C18—H18B | 108.8 |
O7—K1—N2 | 60.38 (11) | H18A—C18—H18B | 107.7 |
O10—K1—N2 | 60.63 (10) | O10—C19—C18 | 109.5 (4) |
O8—K1—N2 | 61.85 (11) | O10—C19—H19A | 109.8 |
O6—K1—N2 | 118.30 (11) | C18—C19—H19A | 109.8 |
O9—K1—N2 | 119.81 (11) | O10—C19—H19B | 109.8 |
O11—K1—N2 | 118.78 (11) | C18—C19—H19B | 109.8 |
O7—K1—N1 | 119.05 (11) | H19A—C19—H19B | 108.2 |
O10—K1—N1 | 118.97 (11) | O10—C20—C21 | 109.0 (4) |
O8—K1—N1 | 119.14 (12) | O10—C20—H20A | 109.9 |
O6—K1—N1 | 61.31 (11) | C21—C20—H20A | 109.9 |
O9—K1—N1 | 61.20 (11) | O10—C20—H20B | 109.9 |
O11—K1—N1 | 60.62 (11) | C21—C20—H20B | 109.9 |
N2—K1—N1 | 178.99 (13) | H20A—C20—H20B | 108.3 |
O17—K2—O16 | 59.71 (11) | O11—C21—C20 | 111.4 (4) |
O17—K2—O12 | 112.79 (12) | O11—C21—H21A | 109.3 |
O16—K2—O12 | 97.97 (11) | C20—C21—H21A | 109.3 |
O17—K2—O15 | 141.89 (13) | O11—C21—H21B | 109.3 |
O16—K2—O15 | 97.74 (10) | C20—C21—H21B | 109.3 |
O12—K2—O15 | 99.75 (11) | H21A—C21—H21B | 108.0 |
O17—K2—O13 | 96.63 (11) | O11—C22—C23 | 110.3 (4) |
O16—K2—O13 | 139.71 (10) | O11—C22—H22A | 109.6 |
O12—K2—O13 | 59.19 (9) | C23—C22—H22A | 109.6 |
O15—K2—O13 | 117.47 (10) | O11—C22—H22B | 109.6 |
O17—K2—O14 | 100.00 (12) | C23—C22—H22B | 109.6 |
O16—K2—O14 | 114.82 (12) | H22A—C22—H22B | 108.1 |
O12—K2—O14 | 142.34 (10) | N1—C23—C22 | 115.2 (5) |
O15—K2—O14 | 59.55 (11) | N1—C23—H23A | 108.5 |
O13—K2—O14 | 100.35 (10) | C22—C23—H23A | 108.5 |
O17—K2—N4 | 61.46 (11) | N1—C23—H23B | 108.5 |
O16—K2—N4 | 118.78 (11) | C22—C23—H23B | 108.5 |
O12—K2—N4 | 119.09 (10) | H23A—C23—H23B | 107.5 |
O15—K2—N4 | 119.09 (11) | N3—C24—C25 | 114.4 (4) |
O13—K2—N4 | 61.59 (10) | N3—C24—H24A | 108.7 |
O14—K2—N4 | 61.20 (11) | C25—C24—H24A | 108.7 |
O17—K2—N3 | 118.69 (10) | N3—C24—H24B | 108.7 |
O16—K2—N3 | 61.27 (11) | C25—C24—H24B | 108.7 |
O12—K2—N3 | 61.18 (11) | H24A—C24—H24B | 107.6 |
O15—K2—N3 | 60.60 (11) | O12—C25—C24 | 108.9 (4) |
O13—K2—N3 | 118.61 (11) | O12—C25—H25A | 109.9 |
O14—K2—N3 | 118.46 (11) | C24—C25—H25A | 109.9 |
N4—K2—N3 | 179.66 (14) | O12—C25—H25B | 109.9 |
C8—O6—C7 | 111.8 (4) | C24—C25—H25B | 109.9 |
C8—O6—K1 | 116.4 (3) | H25A—C25—H25B | 108.3 |
C7—O6—K1 | 117.0 (3) | O12—C26—C27 | 110.1 (4) |
C10—O7—C9 | 110.7 (4) | O12—C26—H26A | 109.6 |
C10—O7—K1 | 120.9 (3) | C27—C26—H26A | 109.6 |
C9—O7—K1 | 116.1 (3) | O12—C26—H26B | 109.6 |
C14—O8—C13 | 112.3 (4) | C27—C26—H26B | 109.6 |
C14—O8—K1 | 117.7 (3) | H26A—C26—H26B | 108.1 |
C13—O8—K1 | 116.5 (3) | O13—C27—C26 | 110.0 (4) |
C15—O9—C16 | 112.0 (4) | O13—C27—H27A | 109.7 |
C15—O9—K1 | 112.8 (2) | C26—C27—H27A | 109.7 |
C16—O9—K1 | 116.4 (3) | O13—C27—H27B | 109.7 |
C19—O10—C20 | 110.6 (4) | C26—C27—H27B | 109.7 |
C19—O10—K1 | 119.4 (3) | H27A—C27—H27B | 108.2 |
C20—O10—K1 | 117.7 (3) | O13—C28—C29 | 110.1 (4) |
C22—O11—C21 | 112.4 (4) | O13—C28—H28A | 109.6 |
C22—O11—K1 | 116.4 (3) | C29—C28—H28A | 109.6 |
C21—O11—K1 | 113.2 (3) | O13—C28—H28B | 109.6 |
C25—O12—C26 | 112.5 (4) | C29—C28—H28B | 109.6 |
C25—O12—K2 | 117.5 (3) | H28A—C28—H28B | 108.2 |
C26—O12—K2 | 117.5 (3) | N4—C29—C28 | 115.0 (4) |
C28—O13—C27 | 110.9 (4) | N4—C29—H29A | 108.5 |
C28—O13—K2 | 115.6 (3) | C28—C29—H29A | 108.5 |
C27—O13—K2 | 114.3 (2) | N4—C29—H29B | 108.5 |
C31—O14—C32 | 112.2 (4) | C28—C29—H29B | 108.5 |
C31—O14—K2 | 116.1 (3) | H29A—C29—H29B | 107.5 |
C32—O14—K2 | 114.2 (3) | N4—C30—C31 | 113.6 (4) |
C33—O15—C34 | 112.2 (4) | N4—C30—H30A | 108.8 |
C33—O15—K2 | 114.1 (3) | C31—C30—H30A | 108.8 |
C34—O15—K2 | 118.6 (3) | N4—C30—H30B | 108.8 |
C38—O16—C37 | 110.9 (4) | C31—C30—H30B | 108.8 |
C38—O16—K2 | 114.2 (3) | H30A—C30—H30B | 107.7 |
C37—O16—K2 | 117.2 (3) | O14—C31—C30 | 109.5 (4) |
C40—O17—C39 | 107.7 (5) | O14—C31—H31A | 109.8 |
C40—O17—K2 | 116.0 (3) | C30—C31—H31A | 109.8 |
C39—O17—K2 | 114.4 (3) | O14—C31—H31B | 109.8 |
C17—N1—C23 | 110.9 (4) | C30—C31—H31B | 109.8 |
C17—N1—C6 | 109.0 (4) | H31A—C31—H31B | 108.2 |
C23—N1—C6 | 111.2 (4) | O14—C32—C33 | 110.1 (4) |
C17—N1—K1 | 108.2 (3) | O14—C32—H32A | 109.6 |
C23—N1—K1 | 109.0 (3) | C33—C32—H32A | 109.6 |
C6—N1—K1 | 108.4 (3) | O14—C32—H32B | 109.6 |
C11—N2—C18 | 110.2 (4) | C33—C32—H32B | 109.6 |
C11—N2—C12 | 110.6 (4) | H32A—C32—H32B | 108.2 |
C18—N2—C12 | 109.2 (4) | O15—C33—C32 | 109.9 (4) |
C11—N2—K1 | 109.3 (3) | O15—C33—H33A | 109.7 |
C18—N2—K1 | 109.5 (3) | C32—C33—H33A | 109.7 |
C12—N2—K1 | 108.1 (3) | O15—C33—H33B | 109.7 |
C24—N3—C36 | 108.9 (4) | C32—C33—H33B | 109.7 |
C24—N3—C35 | 110.9 (5) | H33A—C33—H33B | 108.2 |
C36—N3—C35 | 110.5 (4) | O15—C34—C35 | 110.2 (4) |
C24—N3—K2 | 108.6 (3) | O15—C34—H34A | 109.6 |
C36—N3—K2 | 108.3 (3) | C35—C34—H34A | 109.6 |
C35—N3—K2 | 109.5 (3) | O15—C34—H34B | 109.6 |
C29—N4—C41 | 111.1 (4) | C35—C34—H34B | 109.6 |
C29—N4—C30 | 109.5 (4) | H34A—C34—H34B | 108.1 |
C41—N4—C30 | 107.8 (4) | N3—C35—C34 | 114.7 (5) |
C29—N4—K2 | 108.1 (3) | N3—C35—H35A | 108.6 |
C41—N4—K2 | 110.2 (3) | C34—C35—H35A | 108.6 |
C30—N4—K2 | 110.1 (3) | N3—C35—H35B | 108.6 |
O1—C1—Cr1 | 177.9 (4) | C34—C35—H35B | 108.6 |
O2—C2—Cr1 | 179.0 (6) | H35A—C35—H35B | 107.6 |
O3—C3—Cr1 | 175.7 (4) | N3—C36—C37 | 114.9 (4) |
O4—C4—Cr1 | 177.1 (5) | N3—C36—H36A | 108.5 |
O5—C5—Cr1 | 179.3 (5) | C37—C36—H36A | 108.5 |
N1—C6—C7 | 115.1 (4) | N3—C36—H36B | 108.5 |
N1—C6—H6A | 108.5 | C37—C36—H36B | 108.5 |
C7—C6—H6A | 108.5 | H36A—C36—H36B | 107.5 |
N1—C6—H6B | 108.5 | O16—C37—C36 | 109.6 (4) |
C7—C6—H6B | 108.5 | O16—C37—H37A | 109.7 |
H6A—C6—H6B | 107.5 | C36—C37—H37A | 109.7 |
O6—C7—C6 | 108.7 (5) | O16—C37—H37B | 109.7 |
O6—C7—H7A | 110.0 | C36—C37—H37B | 109.7 |
C6—C7—H7A | 110.0 | H37A—C37—H37B | 108.2 |
O6—C7—H7B | 110.0 | O16—C38—C39 | 110.4 (5) |
C6—C7—H7B | 110.0 | O16—C38—H38A | 109.6 |
H7A—C7—H7B | 108.3 | C39—C38—H38A | 109.6 |
O6—C8—C9 | 110.7 (5) | O16—C38—H38B | 109.6 |
O6—C8—H8A | 109.5 | C39—C38—H38B | 109.6 |
C9—C8—H8A | 109.5 | H38A—C38—H38B | 108.1 |
O6—C8—H8B | 109.5 | C38—C39—O17 | 109.2 (5) |
C9—C8—H8B | 109.5 | C38—C39—H39A | 109.8 |
H8A—C8—H8B | 108.1 | O17—C39—H39A | 109.8 |
O7—C9—C8 | 110.4 (4) | C38—C39—H39B | 109.8 |
O7—C9—H9A | 109.6 | O17—C39—H39B | 109.8 |
C8—C9—H9A | 109.6 | H39A—C39—H39B | 108.3 |
O7—C9—H9B | 109.6 | O17—C40—C41 | 109.3 (5) |
C8—C9—H9B | 109.6 | O17—C40—H40A | 109.8 |
H9A—C9—H9B | 108.1 | C41—C40—H40A | 109.8 |
O7—C10—C11 | 108.6 (4) | O17—C40—H40B | 109.8 |
O7—C10—H10A | 110.0 | C41—C40—H40B | 109.8 |
C11—C10—H10A | 110.0 | H40A—C40—H40B | 108.3 |
O7—C10—H10B | 110.0 | N4—C41—C40 | 114.1 (4) |
C11—C10—H10B | 110.0 | N4—C41—H41A | 108.7 |
H10A—C10—H10B | 108.3 | C40—C41—H41A | 108.7 |
N2—C11—C10 | 113.6 (4) | N4—C41—H41B | 108.7 |
N2—C11—H11A | 108.9 | C40—C41—H41B | 108.7 |
C10—C11—H11A | 108.9 | H41A—C41—H41B | 107.6 |
N2—C11—H11B | 108.9 | C42—N5—H51 | 112.2 |
C10—C11—H11B | 108.9 | C42—N5—H52 | 108.0 |
H11A—C11—H11B | 107.7 | H51—N5—H52 | 109.5 |
N2—C12—C13 | 114.5 (4) | C43—N6—H61 | 110.5 |
N2—C12—H12A | 108.6 | C43—N6—H62 | 106.7 |
C13—C12—H12A | 108.6 | H61—N6—H62 | 109.5 |
N2—C12—H12B | 108.6 | N5—C42—C43 | 117.4 (12) |
C13—C12—H12B | 108.6 | N5—C42—H42A | 108.0 |
H12A—C12—H12B | 107.6 | C43—C42—H42A | 108.0 |
O8—C13—C12 | 109.3 (4) | N5—C42—H42B | 108.0 |
O8—C13—H13A | 109.8 | C43—C42—H42B | 108.0 |
C12—C13—H13A | 109.8 | H42A—C42—H42B | 107.2 |
O8—C13—H13B | 109.8 | C42—C43—N6 | 115.5 (14) |
C12—C13—H13B | 109.8 | C42—C43—H43A | 108.4 |
H13A—C13—H13B | 108.3 | N6—C43—H43A | 108.4 |
O8—C14—C15 | 110.3 (4) | C42—C43—H43B | 108.4 |
O8—C14—H14A | 109.6 | N6—C43—H43B | 108.4 |
C15—C14—H14A | 109.6 | H43A—C43—H43B | 107.5 |
O8—C14—H14B | 109.6 | ||
O7—K1—O6—C8 | 13.8 (4) | O9—K1—N1—C17 | −16.2 (3) |
O10—K1—O6—C8 | −51.0 (5) | O11—K1—N1—C17 | 106.3 (3) |
O8—K1—O6—C8 | 95.6 (4) | O7—K1—N1—C23 | 93.6 (3) |
O9—K1—O6—C8 | 155.0 (4) | O10—K1—N1—C23 | −27.5 (3) |
O11—K1—O6—C8 | −103.8 (4) | O8—K1—N1—C23 | −150.7 (3) |
N2—K1—O6—C8 | 26.0 (4) | O6—K1—N1—C23 | 106.6 (3) |
N1—K1—O6—C8 | −152.9 (4) | O9—K1—N1—C23 | −136.9 (3) |
O7—K1—O6—C7 | 149.7 (5) | O11—K1—N1—C23 | −14.4 (3) |
O10—K1—O6—C7 | 85.0 (4) | O7—K1—N1—C6 | −27.7 (4) |
O8—K1—O6—C7 | −128.4 (4) | O10—K1—N1—C6 | −148.7 (3) |
O9—K1—O6—C7 | −69.1 (4) | O8—K1—N1—C6 | 88.1 (3) |
O11—K1—O6—C7 | 32.2 (4) | O6—K1—N1—C6 | −14.6 (3) |
N2—K1—O6—C7 | 162.0 (4) | O9—K1—N1—C6 | 101.9 (4) |
N1—K1—O6—C7 | −16.9 (4) | O11—K1—N1—C6 | −135.7 (4) |
O10—K1—O7—C10 | −59.5 (4) | O7—K1—N2—C11 | −19.8 (3) |
O8—K1—O7—C10 | 42.1 (4) | O10—K1—N2—C11 | 102.3 (3) |
O6—K1—O7—C10 | 156.5 (5) | O8—K1—N2—C11 | −135.2 (3) |
O9—K1—O7—C10 | 92.4 (4) | O6—K1—N2—C11 | −31.8 (4) |
O11—K1—O7—C10 | −119.9 (4) | O9—K1—N2—C11 | −148.9 (3) |
N2—K1—O7—C10 | −11.1 (4) | O11—K1—N2—C11 | 88.2 (3) |
N1—K1—O7—C10 | 169.9 (4) | O7—K1—N2—C18 | −140.5 (3) |
O10—K1—O7—C9 | 161.8 (4) | O10—K1—N2—C18 | −18.5 (3) |
O8—K1—O7—C9 | −96.6 (4) | O8—K1—N2—C18 | 104.1 (3) |
O6—K1—O7—C9 | 17.8 (4) | O6—K1—N2—C18 | −152.6 (3) |
O9—K1—O7—C9 | −46.3 (4) | O9—K1—N2—C18 | 90.4 (3) |
O11—K1—O7—C9 | 101.4 (4) | O11—K1—N2—C18 | −32.5 (3) |
N2—K1—O7—C9 | −149.8 (4) | O7—K1—N2—C12 | 100.7 (3) |
N1—K1—O7—C9 | 31.2 (4) | O10—K1—N2—C12 | −137.3 (3) |
O7—K1—O8—C14 | 153.1 (3) | O8—K1—N2—C12 | −14.7 (3) |
O10—K1—O8—C14 | −106.5 (3) | O6—K1—N2—C12 | 88.6 (3) |
O6—K1—O8—C14 | 94.5 (3) | O9—K1—N2—C12 | −28.4 (3) |
O9—K1—O8—C14 | 11.3 (3) | O11—K1—N2—C12 | −151.3 (3) |
O11—K1—O8—C14 | −53.2 (4) | O17—K2—N3—C24 | −83.6 (3) |
N2—K1—O8—C14 | −154.9 (3) | O16—K2—N3—C24 | −100.7 (3) |
N1—K1—O8—C14 | 25.3 (4) | O12—K2—N3—C24 | 18.1 (3) |
O7—K1—O8—C13 | −69.1 (3) | O15—K2—N3—C24 | 140.3 (3) |
O10—K1—O8—C13 | 31.3 (3) | O13—K2—N3—C24 | 33.1 (3) |
O6—K1—O8—C13 | −127.6 (3) | O14—K2—N3—C24 | 155.0 (3) |
O9—K1—O8—C13 | 149.2 (3) | O17—K2—N3—C36 | 34.6 (3) |
O11—K1—O8—C13 | 84.6 (3) | O16—K2—N3—C36 | 17.4 (3) |
N2—K1—O8—C13 | −17.0 (3) | O12—K2—N3—C36 | 136.3 (3) |
N1—K1—O8—C13 | 163.2 (3) | O15—K2—N3—C36 | −101.6 (3) |
O7—K1—O9—C15 | −42.3 (4) | O13—K2—N3—C36 | 151.2 (3) |
O10—K1—O9—C15 | 105.6 (3) | O14—K2—N3—C36 | −86.9 (3) |
O8—K1—O9—C15 | 20.6 (3) | O17—K2—N3—C35 | 155.2 (4) |
O6—K1—O9—C15 | −93.2 (3) | O16—K2—N3—C35 | 138.0 (4) |
O11—K1—O9—C15 | 166.3 (3) | O12—K2—N3—C35 | −103.1 (4) |
N2—K1—O9—C15 | 34.7 (4) | O15—K2—N3—C35 | 19.0 (4) |
N1—K1—O9—C15 | −145.4 (4) | O13—K2—N3—C35 | −88.2 (4) |
O7—K1—O9—C16 | 89.3 (3) | O14—K2—N3—C35 | 33.7 (4) |
O10—K1—O9—C16 | −122.9 (3) | O17—K2—N4—C29 | 133.4 (3) |
O8—K1—O9—C16 | 152.2 (3) | O16—K2—N4—C29 | 150.9 (3) |
O6—K1—O9—C16 | 38.4 (3) | O12—K2—N4—C29 | 31.8 (3) |
O11—K1—O9—C16 | −62.1 (3) | O15—K2—N4—C29 | −90.3 (3) |
N2—K1—O9—C16 | 166.2 (3) | O13—K2—N4—C29 | 17.1 (3) |
N1—K1—O9—C16 | −13.8 (3) | O14—K2—N4—C29 | −105.0 (3) |
O7—K1—O10—C19 | 36.0 (3) | O17—K2—N4—C41 | 11.8 (3) |
O8—K1—O10—C19 | −61.4 (3) | O16—K2—N4—C41 | 29.3 (4) |
O6—K1—O10—C19 | 87.8 (4) | O12—K2—N4—C41 | −89.9 (4) |
O9—K1—O10—C19 | −122.1 (3) | O15—K2—N4—C41 | 148.1 (3) |
O11—K1—O10—C19 | 153.5 (4) | O13—K2—N4—C41 | −104.5 (4) |
N2—K1—O10—C19 | −12.3 (3) | O14—K2—N4—C41 | 133.4 (4) |
N1—K1—O10—C19 | 166.7 (3) | O17—K2—N4—C30 | −107.0 (3) |
O7—K1—O10—C20 | −102.6 (3) | O16—K2—N4—C30 | −89.5 (3) |
O8—K1—O10—C20 | 160.0 (3) | O12—K2—N4—C30 | 151.4 (3) |
O6—K1—O10—C20 | −50.8 (4) | O15—K2—N4—C30 | 29.3 (3) |
O9—K1—O10—C20 | 99.3 (3) | O13—K2—N4—C30 | 136.7 (3) |
O11—K1—O10—C20 | 14.8 (3) | O14—K2—N4—C30 | 14.7 (3) |
N2—K1—O10—C20 | −150.9 (3) | C17—N1—C6—C7 | 164.3 (5) |
N1—K1—O10—C20 | 28.0 (3) | C23—N1—C6—C7 | −73.1 (6) |
O7—K1—O11—C22 | −125.9 (4) | K1—N1—C6—C7 | 46.8 (6) |
O10—K1—O11—C22 | 150.1 (4) | C8—O6—C7—C6 | −175.7 (5) |
O8—K1—O11—C22 | 84.1 (4) | K1—O6—C7—C6 | 46.5 (6) |
O6—K1—O11—C22 | −66.2 (4) | N1—C6—C7—O6 | −64.5 (7) |
O9—K1—O11—C22 | 32.0 (4) | C7—O6—C8—C9 | 178.5 (5) |
N2—K1—O11—C22 | 164.3 (4) | K1—O6—C8—C9 | −43.4 (6) |
N1—K1—O11—C22 | −16.6 (4) | C10—O7—C9—C8 | 169.7 (5) |
O7—K1—O11—C21 | 101.6 (3) | K1—O7—C9—C8 | −47.5 (6) |
O10—K1—O11—C21 | 17.7 (3) | O6—C8—C9—O7 | 60.1 (6) |
O8—K1—O11—C21 | −48.3 (4) | C9—O7—C10—C11 | −179.9 (5) |
O6—K1—O11—C21 | 161.3 (3) | K1—O7—C10—C11 | 39.4 (6) |
O9—K1—O11—C21 | −100.4 (3) | C18—N2—C11—C10 | 170.2 (5) |
N2—K1—O11—C21 | 31.8 (3) | C12—N2—C11—C10 | −69.0 (6) |
N1—K1—O11—C21 | −149.1 (3) | K1—N2—C11—C10 | 49.8 (6) |
O17—K2—O12—C25 | 124.9 (3) | O7—C10—C11—N2 | −60.4 (7) |
O16—K2—O12—C25 | 64.4 (3) | C11—N2—C12—C13 | 166.1 (4) |
O15—K2—O12—C25 | −34.9 (3) | C18—N2—C12—C13 | −72.5 (5) |
O13—K2—O12—C25 | −151.1 (3) | K1—N2—C12—C13 | 46.4 (5) |
O14—K2—O12—C25 | −86.6 (3) | C14—O8—C13—C12 | −173.0 (4) |
N4—K2—O12—C25 | −166.2 (3) | K1—O8—C13—C12 | 46.9 (5) |
N3—K2—O12—C25 | 13.6 (3) | N2—C12—C13—O8 | −64.9 (6) |
O17—K2—O12—C26 | −95.8 (3) | C13—O8—C14—C15 | 179.5 (4) |
O16—K2—O12—C26 | −156.3 (3) | K1—O8—C14—C15 | −41.0 (5) |
O15—K2—O12—C26 | 104.4 (3) | C16—O9—C15—C14 | 175.6 (4) |
O13—K2—O12—C26 | −11.9 (3) | K1—O9—C15—C14 | −50.6 (5) |
O14—K2—O12—C26 | 52.7 (3) | O8—C14—C15—O9 | 61.6 (5) |
N4—K2—O12—C26 | −26.9 (3) | C15—O9—C16—C17 | 174.5 (4) |
N3—K2—O12—C26 | 152.9 (3) | K1—O9—C16—C17 | 42.6 (5) |
O17—K2—O13—C28 | −38.4 (3) | C23—N1—C17—C16 | 167.3 (4) |
O16—K2—O13—C28 | −88.0 (3) | C6—N1—C17—C16 | −69.9 (6) |
O12—K2—O13—C28 | −151.1 (3) | K1—N1—C17—C16 | 47.8 (5) |
O15—K2—O13—C28 | 124.0 (3) | O9—C16—C17—N1 | −63.6 (6) |
O14—K2—O13—C28 | 63.0 (3) | C11—N2—C18—C19 | −71.4 (5) |
N4—K2—O13—C28 | 14.0 (3) | C12—N2—C18—C19 | 166.9 (4) |
N3—K2—O13—C28 | −166.3 (3) | K1—N2—C18—C19 | 48.8 (5) |
O17—K2—O13—C27 | 92.2 (3) | C20—O10—C19—C18 | −177.5 (4) |
O16—K2—O13—C27 | 42.6 (4) | K1—O10—C19—C18 | 41.2 (5) |
O12—K2—O13—C27 | −20.4 (3) | N2—C18—C19—O10 | −61.3 (6) |
O15—K2—O13—C27 | −105.4 (3) | C19—O10—C20—C21 | 173.3 (4) |
O14—K2—O13—C27 | −166.3 (3) | K1—O10—C20—C21 | −44.6 (5) |
N4—K2—O13—C27 | 144.6 (3) | C22—O11—C21—C20 | 177.2 (5) |
N3—K2—O13—C27 | −35.7 (3) | K1—O11—C21—C20 | −48.4 (5) |
O17—K2—O14—C31 | 66.8 (3) | O10—C20—C21—O11 | 62.1 (6) |
O16—K2—O14—C31 | 128.0 (3) | C21—O11—C22—C23 | 178.8 (5) |
O12—K2—O14—C31 | −83.9 (4) | K1—O11—C22—C23 | 46.0 (6) |
O15—K2—O14—C31 | −147.8 (4) | C17—N1—C23—C22 | −73.4 (5) |
O13—K2—O14—C31 | −31.9 (3) | C6—N1—C23—C22 | 165.1 (5) |
N4—K2—O14—C31 | 17.4 (3) | K1—N1—C23—C22 | 45.6 (5) |
N3—K2—O14—C31 | −162.6 (3) | O11—C22—C23—N1 | −63.9 (6) |
O17—K2—O14—C32 | −160.2 (3) | C36—N3—C24—C25 | −167.6 (4) |
O16—K2—O14—C32 | −99.0 (3) | C35—N3—C24—C25 | 70.6 (5) |
O12—K2—O14—C32 | 49.1 (4) | K2—N3—C24—C25 | −49.8 (5) |
O15—K2—O14—C32 | −14.8 (3) | C26—O12—C25—C24 | 176.1 (4) |
O13—K2—O14—C32 | 101.1 (3) | K2—O12—C25—C24 | −42.7 (5) |
N4—K2—O14—C32 | 150.4 (4) | N3—C24—C25—O12 | 64.2 (6) |
N3—K2—O14—C32 | −29.6 (4) | C25—O12—C26—C27 | −176.7 (4) |
O17—K2—O15—C33 | 46.1 (4) | K2—O12—C26—C27 | 42.0 (4) |
O16—K2—O15—C33 | 95.5 (3) | C28—O13—C27—C26 | −176.5 (4) |
O12—K2—O15—C33 | −165.0 (3) | K2—O13—C27—C26 | 50.6 (4) |
O13—K2—O15—C33 | −104.8 (3) | O12—C26—C27—O13 | −61.3 (5) |
O14—K2—O15—C33 | −18.8 (3) | C27—O13—C28—C29 | −175.8 (4) |
N4—K2—O15—C33 | −33.7 (3) | K2—O13—C28—C29 | −43.6 (5) |
N3—K2—O15—C33 | 146.2 (4) | C41—N4—C29—C28 | 72.0 (6) |
O17—K2—O15—C34 | −89.5 (4) | C30—N4—C29—C28 | −169.1 (4) |
O16—K2—O15—C34 | −40.1 (4) | K2—N4—C29—C28 | −49.1 (5) |
O12—K2—O15—C34 | 59.4 (4) | O13—C28—C29—N4 | 65.3 (6) |
O13—K2—O15—C34 | 119.6 (4) | C29—N4—C30—C31 | 72.9 (5) |
O14—K2—O15—C34 | −154.4 (4) | C41—N4—C30—C31 | −166.1 (4) |
N4—K2—O15—C34 | −169.3 (4) | K2—N4—C30—C31 | −45.9 (5) |
N3—K2—O15—C34 | 10.6 (4) | C32—O14—C31—C30 | 179.0 (4) |
O17—K2—O16—C38 | −17.3 (4) | K2—O14—C31—C30 | −47.1 (5) |
O12—K2—O16—C38 | 94.5 (4) | N4—C30—C31—O14 | 64.1 (6) |
O15—K2—O16—C38 | −164.5 (4) | C31—O14—C32—C33 | −178.7 (5) |
O13—K2—O16—C38 | 43.9 (5) | K2—O14—C32—C33 | 46.4 (5) |
O14—K2—O16—C38 | −104.5 (4) | C34—O15—C33—C32 | −170.8 (4) |
N4—K2—O16—C38 | −35.1 (4) | K2—O15—C33—C32 | 50.7 (5) |
N3—K2—O16—C38 | 145.3 (4) | O14—C32—C33—O15 | −65.7 (6) |
O17—K2—O16—C37 | −149.5 (4) | C33—O15—C34—C35 | −175.2 (5) |
O12—K2—O16—C37 | −37.7 (4) | K2—O15—C34—C35 | −38.8 (6) |
O15—K2—O16—C37 | 63.4 (4) | C24—N3—C35—C34 | −169.2 (4) |
O13—K2—O16—C37 | −88.3 (4) | C36—N3—C35—C34 | 70.0 (5) |
O14—K2—O16—C37 | 123.3 (4) | K2—N3—C35—C34 | −49.3 (5) |
N4—K2—O16—C37 | −167.2 (3) | O15—C34—C35—N3 | 60.6 (6) |
N3—K2—O16—C37 | 13.1 (3) | C24—N3—C36—C37 | 68.8 (6) |
O16—K2—O17—C40 | −142.3 (4) | C35—N3—C36—C37 | −169.2 (5) |
O12—K2—O17—C40 | 131.8 (4) | K2—N3—C36—C37 | −49.2 (5) |
O15—K2—O17—C40 | −81.8 (4) | C38—O16—C37—C36 | −176.1 (5) |
O13—K2—O17—C40 | 72.5 (4) | K2—O16—C37—C36 | −42.5 (5) |
O14—K2—O17—C40 | −29.3 (4) | N3—C36—C37—O16 | 63.7 (6) |
N4—K2—O17—C40 | 20.0 (4) | C37—O16—C38—C39 | −175.0 (5) |
N3—K2—O17—C40 | −159.7 (4) | K2—O16—C38—C39 | 49.9 (6) |
O16—K2—O17—C39 | −15.9 (3) | O16—C38—C39—O17 | −65.4 (6) |
O12—K2—O17—C39 | −101.8 (4) | C40—O17—C39—C38 | 178.2 (5) |
O15—K2—O17—C39 | 44.6 (4) | K2—O17—C39—C38 | 47.6 (5) |
O13—K2—O17—C39 | −161.1 (4) | C39—O17—C40—C41 | −179.1 (5) |
O14—K2—O17—C39 | 97.1 (4) | K2—O17—C40—C41 | −49.4 (6) |
N4—K2—O17—C39 | 146.3 (4) | C29—N4—C41—C40 | −162.5 (5) |
N3—K2—O17—C39 | −33.3 (4) | C30—N4—C41—C40 | 77.5 (6) |
O7—K1—N1—C17 | −145.8 (3) | K2—N4—C41—C40 | −42.7 (6) |
O10—K1—N1—C17 | 93.2 (3) | O17—C40—C41—N4 | 63.2 (7) |
O8—K1—N1—C17 | −30.0 (3) | N5—C42—C43—N6 | −88.6 (17) |
O6—K1—N1—C17 | −132.7 (3) |
Cation | Axial | Equatorial | Reference |
[2,2,2-crypt-K]+ | 1.813 (2) | 1.881 (6) | Borrmann et al. (1997b) |
[2,2,2-crypt-Na]+ | 1.828 (2) | 1.876 (4) | Borrmann et al. (1997a) |
K+ | 1.802 (6) | 1.861 (6) | Hey-Hawkins & von Schnering (1991) |
PPN+ | 1.792 (4) | 1.879 (4) | Lee et al. (1996) |