BQ123 is a cyclic pentapeptide and a potent endothelin-1 inhibitor. The crystal structure of the BQ123 sodium salt was determined as the first example of an endothelin inhibitor. Four independent molecules and many solvent molecules were found in the asymmetric unit; the total weight was about 3000 Da. The precise structure including the solvent molecules was determined using high-resolution data collected on a synchrotron source. Sodium ions formed unique structures with five and six coordination bonds and their forms were distinguished into three classes. An ion was sandwiched by two BQ123 molecules. This peptide-sodium (2:1) complex showed a cage-like structure and octahedral coordination was observed. Sodium ions also formed a cluster composed of hydrated water molecules and peptides. Two sodium ions were contained in this cluster, making five coordination bonds. Despite having the same coordination numbers, these ions were distinguishable by differences in the polyhedra. One was trigonal bipyramidal (having six planes) and the other was square pyramidal (having five planes). Both shapes were very similar to each other, although the synchrotron data clearly revealed slight geometrical differences.
Supporting information
Data collection: RIgaku PROCESS; cell refinement: MOSFLM 6.01 (Leslie, 1999); data reduction: MOSFLM 6.01 (Leslie, 1999); program(s) used to solve structure: LODEM (Shiono, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-III (Burnett & Johnson,1996); software used to prepare material for publication: PARST (Nardelli, 1983).
BQ123:
cyclo(–D-Trp-D-Asp
-—Pro-D-Val-Leu-)·Na
+ an
endothelin-1 inhibitor
top
Crystal data top
4(C31H41N6O7Na)·8(H2O)·5.63(C3H7OH) | F(000) = 6461 |
Mr = 3013.12 | Dx = 0.883 Mg m−3 |
Orthorhombic, P212121 | Synchrotron radiation, λ = 0.83400 Å |
a = 25.3930 (4) Å | µ = 0.07 mm−1 |
b = 34.7193 (3) Å | T = 100 K |
c = 25.7201 (4) Å | Block, colorless |
V = 22675.5 (5) Å3 | 0.08 × 0.04 × 0.04 mm |
Z = 4 | |
Data collection top
Rigaku RAXIS-IV diffractometer | 22861 reflections with I > 2σ(I) |
Radiation source: double monochromated beam | Rint = 0.034 |
Diamond monochromator | θmax = 31.5°, θmin = 1.5° |
Detector resolution: 10 pixels mm-1 | h = −31→31 |
oscillation scans | k = −37→38 |
83268 measured reflections | l = 0→31 |
22865 independent reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.058 | w = 1/[σ2(Fo2) + (0.1388P)2 + 0.5089P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.164 | (Δ/σ)max = 0.656 |
S = 1.07 | Δρmax = 0.56 e Å−3 |
22865 reflections | Δρmin = −0.26 e Å−3 |
1904 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
36 restraints | Extinction coefficient: 2173 (12) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0 (10) |
Crystal data top
4(C31H41N6O7Na)·8(H2O)·5.63(C3H7OH) | V = 22675.5 (5) Å3 |
Mr = 3013.12 | Z = 4 |
Orthorhombic, P212121 | Synchrotron radiation, λ = 0.83400 Å |
a = 25.3930 (4) Å | µ = 0.07 mm−1 |
b = 34.7193 (3) Å | T = 100 K |
c = 25.7201 (4) Å | 0.08 × 0.04 × 0.04 mm |
Data collection top
Rigaku RAXIS-IV diffractometer | 22861 reflections with I > 2σ(I) |
83268 measured reflections | Rint = 0.034 |
22865 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.058 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.164 | (Δ/σ)max = 0.656 |
S = 1.07 | Δρmax = 0.56 e Å−3 |
22865 reflections | Δρmin = −0.26 e Å−3 |
1904 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
36 restraints | Absolute structure parameter: 0 (10) |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Na_1 | 0.25282 (7) | 1.02537 (5) | 0.28478 (6) | 0.0540 (4) | |
Na_2 | 0.03723 (7) | 0.73420 (6) | 0.51179 (7) | 0.0564 (4) | |
Na_3 | 0.23093 (7) | 0.90910 (6) | 0.55404 (6) | 0.0562 (4) | |
Na_4 | 0.33052 (7) | 0.83613 (6) | 0.53727 (7) | 0.0567 (4) | |
N_11 | 0.31031 (14) | 1.00883 (12) | 0.15170 (14) | 0.0537 (7) | |
H0_11 | 0.3129 | 0.9943 | 0.1787 | 0.064* | |
CA_11 | 0.35423 (16) | 1.03395 (14) | 0.13818 (16) | 0.0551 (9) | |
HA_11 | 0.3596 | 1.0325 | 0.1005 | 0.066* | |
CB_11 | 0.40502 (18) | 1.01916 (17) | 0.16522 (19) | 0.0617 (10) | |
HB1_11 | 0.4015 | 1.0225 | 0.2025 | 0.074* | |
HB2_11 | 0.4089 | 0.9918 | 0.1583 | 0.074* | |
CG_11 | 0.45326 (19) | 1.03972 (16) | 0.1471 (2) | 0.0625 (10) | |
CD1_11 | 0.4790 (2) | 1.06837 (18) | 0.1721 (3) | 0.0723 (12) | |
HD1_11 | 0.4677 | 1.0800 | 0.2027 | 0.087* | |
NE1_11 | 0.52469 (19) | 1.07784 (17) | 0.1455 (2) | 0.0790 (13) | |
HE1_11 | 0.5469 | 1.0954 | 0.1542 | 0.095* | |
CE2_11 | 0.5284 (2) | 1.05413 (19) | 0.1024 (2) | 0.0717 (13) | |
CZ2_11 | 0.5677 (2) | 1.0519 (2) | 0.0633 (3) | 0.0837 (18) | |
HZ2_11 | 0.5974 | 1.0675 | 0.0642 | 0.100* | |
CH2_11 | 0.5600 (3) | 1.0261 (3) | 0.0249 (3) | 0.094 (2) | |
HH2_11 | 0.5846 | 1.0246 | −0.0018 | 0.113* | |
CZ3_11 | 0.5156 (3) | 1.0011 (3) | 0.0239 (3) | 0.092 (2) | |
HZ3_11 | 0.5121 | 0.9833 | −0.0028 | 0.110* | |
CE3_11 | 0.4784 (2) | 1.0033 (2) | 0.0614 (2) | 0.0747 (13) | |
HE3_11 | 0.4492 | 0.9871 | 0.0603 | 0.090* | |
CD2_11 | 0.48394 (19) | 1.03021 (17) | 0.1024 (2) | 0.0646 (11) | |
C_11 | 0.33986 (15) | 1.07564 (14) | 0.15198 (16) | 0.0529 (9) | |
O_11 | 0.32972 (13) | 1.09905 (11) | 0.11833 (12) | 0.0589 (7) | |
N_12 | 0.33805 (15) | 1.08353 (12) | 0.20287 (15) | 0.0566 (8) | |
H0_12 | 0.3536 | 1.0684 | 0.2244 | 0.068* | |
CA_12 | 0.31049 (17) | 1.11691 (14) | 0.22249 (16) | 0.0554 (9) | |
HA_12 | 0.3133 | 1.1376 | 0.1968 | 0.066* | |
CB_12 | 0.33584 (18) | 1.13059 (14) | 0.27341 (17) | 0.0563 (9) | |
HB1_12 | 0.3172 | 1.1533 | 0.2854 | 0.068* | |
HB2_12 | 0.3719 | 1.1381 | 0.2663 | 0.068* | |
CG_12 | 0.33597 (18) | 1.10058 (15) | 0.31728 (17) | 0.0574 (9) | |
OD1_12 | 0.32357 (14) | 1.06680 (10) | 0.30756 (12) | 0.0591 (7) | |
OD2_12 | 0.35038 (16) | 1.11279 (11) | 0.36119 (13) | 0.0649 (8) | |
C_12 | 0.25158 (16) | 1.10686 (14) | 0.22988 (15) | 0.0521 (8) | |
O_12 | 0.23674 (12) | 1.07319 (10) | 0.22611 (12) | 0.0555 (7) | |
N_13 | 0.21854 (14) | 1.13497 (12) | 0.24165 (14) | 0.0531 (7) | |
CA_13 | 0.16396 (17) | 1.12618 (14) | 0.25802 (17) | 0.0560 (9) | |
HA_13 | 0.1638 | 1.1147 | 0.2928 | 0.067* | |
CB_13 | 0.13799 (19) | 1.16612 (16) | 0.2592 (2) | 0.0623 (10) | |
HB1_13 | 0.1025 | 1.1648 | 0.2454 | 0.075* | |
HB2_13 | 0.1364 | 1.1758 | 0.2945 | 0.075* | |
CG_13 | 0.1722 (2) | 1.19214 (17) | 0.2255 (2) | 0.0662 (11) | |
HG1_13 | 0.1637 | 1.1894 | 0.1889 | 0.079* | |
HG2_13 | 0.1687 | 1.2190 | 0.2355 | 0.079* | |
CD_13 | 0.22702 (19) | 1.17685 (15) | 0.2374 (2) | 0.0620 (10) | |
HD1_13 | 0.2515 | 1.1829 | 0.2096 | 0.074* | |
HD2_13 | 0.2404 | 1.1874 | 0.2698 | 0.074* | |
C_13 | 0.13747 (17) | 1.09950 (15) | 0.21924 (17) | 0.0564 (9) | |
O_13 | 0.13021 (13) | 1.10901 (11) | 0.17402 (13) | 0.0624 (8) | |
N_14 | 0.12035 (14) | 1.06562 (12) | 0.23932 (14) | 0.0540 (7) | |
H0_14 | 0.1178 | 1.0628 | 0.2724 | 0.065* | |
CA_14 | 0.10637 (16) | 1.03421 (14) | 0.20473 (16) | 0.0553 (9) | |
HA_14 | 0.0974 | 1.0445 | 0.1704 | 0.066* | |
CB_14 | 0.06005 (17) | 1.01011 (15) | 0.22542 (19) | 0.0599 (10) | |
HB_14 | 0.0692 | 1.0004 | 0.2600 | 0.072* | |
CG1_14 | 0.0496 (2) | 0.97580 (18) | 0.1898 (2) | 0.0698 (12) | |
H1A_14 | 0.0808 | 0.9603 | 0.1874 | 0.105* | |
H1B_14 | 0.0400 | 0.9849 | 0.1559 | 0.105* | |
H1C_14 | 0.0213 | 0.9606 | 0.2039 | 0.105* | |
CG2_14 | 0.01046 (18) | 1.03533 (18) | 0.2301 (2) | 0.0677 (12) | |
H2A_14 | 0.0177 | 1.0568 | 0.2525 | 0.102* | |
H2B_14 | −0.0178 | 1.0203 | 0.2445 | 0.102* | |
H2C_14 | 0.0005 | 1.0445 | 0.1963 | 0.102* | |
C_14 | 0.15681 (16) | 1.00919 (14) | 0.20055 (16) | 0.0526 (8) | |
O_14 | 0.17640 (12) | 0.99576 (10) | 0.24075 (11) | 0.0548 (6) | |
N_15 | 0.17531 (15) | 1.00342 (11) | 0.15333 (13) | 0.0530 (7) | |
H0_15 | 0.1589 | 1.0133 | 0.1273 | 0.064* | |
CA_15 | 0.22310 (17) | 0.98062 (14) | 0.14358 (16) | 0.0541 (9) | |
HA_15 | 0.2348 | 0.9692 | 0.1765 | 0.065* | |
CB_15 | 0.21357 (19) | 0.94831 (15) | 0.10437 (17) | 0.0577 (9) | |
HB1_15 | 0.2446 | 0.9320 | 0.1035 | 0.069* | |
HB2_15 | 0.2097 | 0.9597 | 0.0702 | 0.069* | |
CG_15 | 0.1655 (2) | 0.92285 (17) | 0.11479 (19) | 0.0656 (11) | |
HG_15 | 0.1341 | 0.9392 | 0.1135 | 0.079* | |
CD1_15 | 0.1680 (3) | 0.90428 (18) | 0.1690 (2) | 0.0746 (13) | |
H1A_15 | 0.1709 | 0.9241 | 0.1950 | 0.112* | |
H1B_15 | 0.1981 | 0.8876 | 0.1710 | 0.112* | |
H1C_15 | 0.1366 | 0.8896 | 0.1750 | 0.112* | |
CD2_15 | 0.1598 (3) | 0.8922 (2) | 0.0742 (2) | 0.0826 (17) | |
H2A_15 | 0.1292 | 0.8769 | 0.0816 | 0.124* | |
H2B_15 | 0.1905 | 0.8760 | 0.0743 | 0.124* | |
H2C_15 | 0.1560 | 0.9040 | 0.0407 | 0.124* | |
C_15 | 0.26626 (17) | 1.00762 (14) | 0.12359 (16) | 0.0532 (8) | |
O_15 | 0.25969 (12) | 1.02610 (10) | 0.08327 (12) | 0.0564 (7) | |
N_21 | 0.33800 (16) | 1.05075 (13) | 0.43043 (15) | 0.0586 (8) | |
H0_21 | 0.3430 | 1.0717 | 0.4132 | 0.070* | |
CA_21 | 0.38266 (18) | 1.02638 (14) | 0.44247 (17) | 0.0569 (9) | |
HA_21 | 0.3863 | 1.0250 | 0.4804 | 0.068* | |
CB_21 | 0.4328 (2) | 1.04524 (18) | 0.4201 (2) | 0.0685 (12) | |
HB1_21 | 0.4287 | 1.0481 | 0.3828 | 0.082* | |
HB2_21 | 0.4367 | 1.0708 | 0.4349 | 0.082* | |
CG_21 | 0.4819 (2) | 1.0221 (2) | 0.4310 (3) | 0.0801 (15) | |
CD1_21 | 0.5093 (3) | 0.9998 (2) | 0.3984 (4) | 0.093 (2) | |
HD1_21 | 0.5006 | 0.9957 | 0.3637 | 0.111* | |
NE1_21 | 0.5524 (2) | 0.9836 (2) | 0.4232 (5) | 0.122 (3) | |
HE1_21 | 0.5747 | 0.9680 | 0.4095 | 0.146* | |
CE2_21 | 0.5530 (3) | 0.9965 (3) | 0.4716 (5) | 0.097 (2) | |
CZ2_21 | 0.5911 (4) | 0.9893 (4) | 0.5100 (9) | 0.160 (8) | |
HZ2_21 | 0.6209 | 0.9747 | 0.5027 | 0.192* | |
CH2_21 | 0.5831 (5) | 1.0041 (5) | 0.5573 (8) | 0.157 (7) | |
HH2_21 | 0.6060 | 0.9977 | 0.5842 | 0.188* | |
CZ3_21 | 0.5377 (4) | 1.0310 (5) | 0.5679 (5) | 0.144 (5) | |
HZ3_21 | 0.5338 | 1.0434 | 0.5998 | 0.172* | |
CE3_21 | 0.5034 (3) | 1.0361 (3) | 0.5291 (3) | 0.103 (3) | |
HE3_21 | 0.4736 | 1.0510 | 0.5351 | 0.124* | |
CD2_21 | 0.5103 (2) | 1.0200 (2) | 0.4804 (3) | 0.090 (2) | |
C_21 | 0.37514 (15) | 0.98552 (14) | 0.42179 (16) | 0.0532 (8) | |
O_21 | 0.38672 (13) | 0.95742 (10) | 0.44873 (12) | 0.0575 (7) | |
N_22 | 0.35596 (15) | 0.98235 (12) | 0.37309 (14) | 0.0548 (8) | |
H0_22 | 0.3555 | 1.0024 | 0.3534 | 0.066* | |
CA_22 | 0.33616 (16) | 0.94637 (14) | 0.35296 (16) | 0.0530 (8) | |
HA_22 | 0.3428 | 0.9264 | 0.3791 | 0.064* | |
CB_22 | 0.36352 (17) | 0.93389 (15) | 0.30240 (16) | 0.0572 (9) | |
HB1_22 | 0.4007 | 0.9399 | 0.3056 | 0.069* | |
HB2_22 | 0.3606 | 0.9061 | 0.2996 | 0.069* | |
CG_22 | 0.34373 (18) | 0.95138 (15) | 0.25156 (16) | 0.0563 (9) | |
OD1_22 | 0.31649 (13) | 0.98123 (11) | 0.25281 (12) | 0.0586 (7) | |
OD2_22 | 0.35627 (17) | 0.93390 (12) | 0.21023 (13) | 0.0704 (9) | |
C_22 | 0.27618 (17) | 0.95044 (14) | 0.34681 (15) | 0.0540 (9) | |
O_22 | 0.25485 (11) | 0.98262 (10) | 0.35120 (11) | 0.0533 (6) | |
N_23 | 0.24722 (14) | 0.91936 (12) | 0.33534 (14) | 0.0538 (7) | |
CA_23 | 0.19071 (17) | 0.92342 (14) | 0.32273 (17) | 0.0564 (9) | |
HA_23 | 0.1865 | 0.9355 | 0.2886 | 0.068* | |
CB_23 | 0.17027 (19) | 0.88299 (15) | 0.32143 (19) | 0.0611 (10) | |
HB1_23 | 0.1429 | 0.8803 | 0.2953 | 0.073* | |
HB2_23 | 0.1560 | 0.8757 | 0.3550 | 0.073* | |
CG_23 | 0.2183 (2) | 0.85829 (17) | 0.3077 (2) | 0.0668 (11) | |
HG1_23 | 0.2249 | 0.8583 | 0.2705 | 0.080* | |
HG2_23 | 0.2140 | 0.8320 | 0.3196 | 0.080* | |
CD_23 | 0.26256 (19) | 0.87875 (15) | 0.3373 (2) | 0.0622 (10) | |
HD1_23 | 0.2646 | 0.8697 | 0.3730 | 0.075* | |
HD2_23 | 0.2963 | 0.8747 | 0.3205 | 0.075* | |
C_23 | 0.16357 (16) | 0.94830 (15) | 0.36537 (16) | 0.0546 (9) | |
O_23 | 0.16536 (13) | 0.93867 (11) | 0.41059 (13) | 0.0605 (7) | |
N_24 | 0.13757 (15) | 0.97985 (13) | 0.34877 (15) | 0.0573 (8) | |
H0_24 | 0.1283 | 0.9816 | 0.3167 | 0.069* | |
CA_24 | 0.12509 (18) | 1.01094 (15) | 0.38460 (16) | 0.0574 (9) | |
HA_24 | 0.1239 | 1.0005 | 0.4200 | 0.069* | |
CB_24 | 0.07137 (19) | 1.02977 (17) | 0.37202 (19) | 0.0650 (11) | |
HB_24 | 0.0730 | 1.0405 | 0.3368 | 0.078* | |
CG1_24 | 0.0274 (2) | 1.0003 (2) | 0.3738 (2) | 0.0753 (14) | |
H1A_24 | 0.0346 | 0.9801 | 0.3493 | 0.113* | |
H1B_24 | −0.0053 | 1.0124 | 0.3650 | 0.113* | |
H1C_24 | 0.0251 | 0.9896 | 0.4081 | 0.113* | |
CG2_24 | 0.0616 (2) | 1.0629 (2) | 0.4101 (3) | 0.0803 (15) | |
H2A_24 | 0.0901 | 1.0810 | 0.4081 | 0.120* | |
H2B_24 | 0.0593 | 1.0529 | 0.4448 | 0.120* | |
H2C_24 | 0.0291 | 1.0755 | 0.4014 | 0.120* | |
C_24 | 0.17050 (17) | 1.03940 (14) | 0.38084 (16) | 0.0541 (9) | |
O_24 | 0.18231 (13) | 1.05350 (10) | 0.33818 (12) | 0.0567 (7) | |
N_25 | 0.19614 (16) | 1.04679 (13) | 0.42508 (14) | 0.0582 (8) | |
H0_25 | 0.1831 | 1.0387 | 0.4539 | 0.070* | |
CA_25 | 0.24614 (18) | 1.06840 (15) | 0.42613 (17) | 0.0571 (9) | |
HA_25 | 0.2547 | 1.0769 | 0.3908 | 0.068* | |
CB_25 | 0.2432 (2) | 1.10315 (17) | 0.4615 (2) | 0.0673 (11) | |
HB1_25 | 0.2782 | 1.1140 | 0.4649 | 0.081* | |
HB2_25 | 0.2321 | 1.0947 | 0.4957 | 0.081* | |
CG_25 | 0.2056 (3) | 1.1350 (2) | 0.4429 (3) | 0.0804 (15) | |
HG_25 | 0.1697 | 1.1247 | 0.4412 | 0.096* | |
CD1_25 | 0.2205 (3) | 1.1512 (2) | 0.3900 (3) | 0.0902 (19) | |
H1A_25 | 0.2205 | 1.1309 | 0.3647 | 0.135* | |
H1B_25 | 0.2550 | 1.1625 | 0.3919 | 0.135* | |
H1C_25 | 0.1955 | 1.1705 | 0.3800 | 0.135* | |
CD2_25 | 0.2074 (4) | 1.1681 (3) | 0.4831 (4) | 0.113 (3) | |
H2A_25 | 0.1969 | 1.1586 | 0.5165 | 0.169* | |
H2B_25 | 0.1839 | 1.1883 | 0.4724 | 0.169* | |
H2C_25 | 0.2426 | 1.1781 | 0.4852 | 0.169* | |
C_25 | 0.28941 (18) | 1.04158 (14) | 0.44541 (15) | 0.0548 (9) | |
O_25 | 0.28050 (12) | 1.01372 (11) | 0.47431 (12) | 0.0577 (7) | |
N_31 | −0.11291 (14) | 0.74168 (12) | 0.59414 (15) | 0.0550 (8) | |
H0_31 | −0.0966 | 0.7620 | 0.6045 | 0.066* | |
CA_31 | −0.12518 (17) | 0.71170 (15) | 0.63137 (17) | 0.0562 (9) | |
HA_31 | −0.1635 | 0.7084 | 0.6324 | 0.067* | |
CB_31 | −0.1063 (2) | 0.72435 (15) | 0.68583 (17) | 0.0603 (10) | |
HB1_31 | −0.0682 | 0.7257 | 0.6860 | 0.072* | |
HB2_31 | −0.1198 | 0.7499 | 0.6932 | 0.072* | |
CG_31 | −0.1238 (2) | 0.69764 (16) | 0.72730 (18) | 0.0640 (11) | |
CD1_31 | −0.1025 (2) | 0.66382 (19) | 0.7424 (2) | 0.0708 (12) | |
HD1_31 | −0.0717 | 0.6537 | 0.7286 | 0.085* | |
NE1_31 | −0.1309 (2) | 0.64649 (16) | 0.77961 (18) | 0.0755 (11) | |
HE1_31 | −0.1234 | 0.6249 | 0.7942 | 0.091* | |
CE2_31 | −0.1749 (2) | 0.66962 (19) | 0.7907 (2) | 0.0702 (12) | |
CZ2_31 | −0.2143 (3) | 0.6642 (2) | 0.8262 (2) | 0.0841 (16) | |
HZ2_31 | −0.2146 | 0.6428 | 0.8480 | 0.101* | |
CH2_31 | −0.2528 (3) | 0.6910 (3) | 0.8286 (3) | 0.097 (2) | |
HH2_31 | −0.2800 | 0.6879 | 0.8524 | 0.116* | |
CZ3_31 | −0.2527 (3) | 0.7243 (3) | 0.7951 (3) | 0.0896 (18) | |
HZ3_31 | −0.2801 | 0.7420 | 0.7964 | 0.108* | |
CE3_31 | −0.2110 (2) | 0.7295 (2) | 0.7609 (3) | 0.0789 (14) | |
HE3_31 | −0.2100 | 0.7512 | 0.7395 | 0.095* | |
CD2_31 | −0.1709 (2) | 0.70229 (18) | 0.7587 (2) | 0.0688 (12) | |
C_31 | −0.10047 (16) | 0.67389 (15) | 0.61608 (16) | 0.0552 (9) | |
O_31 | −0.12471 (12) | 0.64295 (10) | 0.62246 (13) | 0.0576 (7) | |
N_32 | −0.05145 (14) | 0.67478 (12) | 0.59649 (14) | 0.0544 (8) | |
H0_32 | −0.0323 | 0.6949 | 0.6013 | 0.065* | |
CA_32 | −0.03017 (16) | 0.64252 (15) | 0.56735 (17) | 0.0563 (9) | |
HA_32 | −0.0565 | 0.6219 | 0.5678 | 0.068* | |
CB_32 | 0.02063 (18) | 0.62665 (15) | 0.59143 (19) | 0.0598 (10) | |
HB1_32 | 0.0132 | 0.6194 | 0.6271 | 0.072* | |
HB2_32 | 0.0302 | 0.6034 | 0.5729 | 0.072* | |
CG_32 | 0.0682 (2) | 0.65364 (19) | 0.5915 (2) | 0.0679 (12) | |
OD1_32 | 0.06552 (14) | 0.68507 (13) | 0.57043 (15) | 0.0700 (9) | |
OD2_32 | 0.1086 (2) | 0.64039 (17) | 0.6135 (4) | 0.121 (2) | |
C_32 | −0.02332 (15) | 0.65538 (13) | 0.51151 (16) | 0.0508 (8) | |
O_32 | −0.02596 (12) | 0.68984 (10) | 0.49935 (12) | 0.0559 (7) | |
N_33 | −0.01405 (14) | 0.62883 (11) | 0.47465 (15) | 0.0521 (7) | |
CA_33 | −0.00454 (16) | 0.64109 (14) | 0.42130 (17) | 0.0555 (9) | |
HA_33 | 0.0308 | 0.6522 | 0.4186 | 0.067* | |
CB_33 | −0.00716 (18) | 0.60377 (16) | 0.38970 (18) | 0.0608 (10) | |
HB1_33 | −0.0263 | 0.6077 | 0.3575 | 0.073* | |
HB2_33 | 0.0279 | 0.5945 | 0.3816 | 0.073* | |
CG_33 | −0.0359 (2) | 0.57557 (16) | 0.4246 (2) | 0.0635 (10) | |
HG1_33 | −0.0738 | 0.5783 | 0.4210 | 0.076* | |
HG2_33 | −0.0261 | 0.5492 | 0.4166 | 0.076* | |
CD_33 | −0.01817 (18) | 0.58660 (14) | 0.47887 (18) | 0.0570 (9) | |
HD1_33 | −0.0439 | 0.5791 | 0.5048 | 0.068* | |
HD2_33 | 0.0155 | 0.5751 | 0.4873 | 0.068* | |
C_33 | −0.04593 (16) | 0.67131 (15) | 0.40432 (18) | 0.0560 (9) | |
O_33 | −0.09296 (12) | 0.66562 (11) | 0.41108 (12) | 0.0571 (7) | |
N_34 | −0.02565 (14) | 0.70281 (12) | 0.38123 (15) | 0.0560 (8) | |
H0_34 | 0.0062 | 0.7029 | 0.3699 | 0.067* | |
CA_34 | −0.05898 (16) | 0.73662 (14) | 0.37585 (18) | 0.0559 (9) | |
HA_34 | −0.0952 | 0.7285 | 0.3685 | 0.067* | |
CB_34 | −0.03998 (19) | 0.76405 (15) | 0.33250 (18) | 0.0596 (10) | |
HB_34 | −0.0042 | 0.7725 | 0.3411 | 0.071* | |
CG1_34 | −0.0381 (2) | 0.74367 (18) | 0.28028 (18) | 0.0682 (12) | |
H1A_34 | −0.0152 | 0.7218 | 0.2826 | 0.102* | |
H1B_34 | −0.0252 | 0.7611 | 0.2543 | 0.102* | |
H1C_34 | −0.0729 | 0.7353 | 0.2710 | 0.102* | |
CG2_34 | −0.0757 (3) | 0.79981 (19) | 0.3311 (2) | 0.0787 (14) | |
H2A_34 | −0.0762 | 0.8117 | 0.3647 | 0.118* | |
H2B_34 | −0.1108 | 0.7922 | 0.3217 | 0.118* | |
H2C_34 | −0.0625 | 0.8177 | 0.3058 | 0.118* | |
C_34 | −0.05718 (17) | 0.75682 (14) | 0.42920 (17) | 0.0544 (9) | |
O_34 | −0.01548 (11) | 0.77104 (10) | 0.44537 (12) | 0.0552 (6) | |
N_35 | −0.10215 (13) | 0.75659 (12) | 0.45580 (14) | 0.0538 (7) | |
H0_35 | −0.1300 | 0.7478 | 0.4410 | 0.065* | |
CA_35 | −0.10611 (16) | 0.77066 (14) | 0.50883 (17) | 0.0552 (9) | |
HA_35 | −0.0709 | 0.7781 | 0.5206 | 0.066* | |
CB_35 | −0.14225 (16) | 0.80626 (15) | 0.5119 (2) | 0.0595 (10) | |
HB1_35 | −0.1761 | 0.7999 | 0.4966 | 0.071* | |
HB2_35 | −0.1482 | 0.8126 | 0.5482 | 0.071* | |
CG_35 | −0.11975 (19) | 0.84123 (17) | 0.4844 (2) | 0.0677 (12) | |
HG_35 | −0.1117 | 0.8341 | 0.4484 | 0.081* | |
CD1_35 | −0.1604 (2) | 0.8739 (2) | 0.4838 (3) | 0.0840 (17) | |
H1A_35 | −0.1459 | 0.8959 | 0.4663 | 0.126* | |
H1B_35 | −0.1695 | 0.8807 | 0.5188 | 0.126* | |
H1C_35 | −0.1915 | 0.8655 | 0.4657 | 0.126* | |
CD2_35 | −0.0693 (2) | 0.85548 (18) | 0.5100 (3) | 0.0759 (14) | |
H2A_35 | −0.0439 | 0.8350 | 0.5108 | 0.114* | |
H2B_35 | −0.0767 | 0.8636 | 0.5449 | 0.114* | |
H2C_35 | −0.0554 | 0.8768 | 0.4906 | 0.114* | |
C_35 | −0.12632 (15) | 0.73851 (14) | 0.54398 (17) | 0.0529 (8) | |
O_35 | −0.15346 (12) | 0.71159 (10) | 0.52687 (12) | 0.0552 (6) | |
N_41 | 0.17755 (16) | 0.71034 (13) | 0.58336 (16) | 0.0599 (8) | |
H0_41 | 0.1559 | 0.6914 | 0.5861 | 0.072* | |
CA_41 | 0.19235 (19) | 0.73150 (15) | 0.62966 (18) | 0.0590 (10) | |
HA_41 | 0.2309 | 0.7323 | 0.6319 | 0.071* | |
CB_41 | 0.1706 (2) | 0.71010 (17) | 0.6776 (2) | 0.0674 (11) | |
HB1_41 | 0.1325 | 0.7094 | 0.6755 | 0.081* | |
HB2_41 | 0.1833 | 0.6837 | 0.6771 | 0.081* | |
CG_41 | 0.1860 (3) | 0.72814 (19) | 0.7280 (2) | 0.0735 (13) | |
CD1_41 | 0.1556 (3) | 0.7524 (2) | 0.7589 (2) | 0.0804 (15) | |
HD1_41 | 0.1221 | 0.7614 | 0.7505 | 0.096* | |
NE1_41 | 0.1827 (3) | 0.76102 (17) | 0.80369 (19) | 0.0867 (15) | |
HE1_41 | 0.1710 | 0.7751 | 0.8286 | 0.104* | |
CE2_41 | 0.2308 (3) | 0.7438 (2) | 0.8026 (2) | 0.0798 (15) | |
CZ2_41 | 0.2719 (4) | 0.7438 (2) | 0.8404 (3) | 0.096 (2) | |
HZ2_41 | 0.2685 | 0.7565 | 0.8721 | 0.115* | |
CH2_41 | 0.3179 (4) | 0.7235 (3) | 0.8272 (4) | 0.110 (3) | |
HH2_41 | 0.3463 | 0.7237 | 0.8501 | 0.132* | |
CZ3_41 | 0.3219 (3) | 0.7038 (3) | 0.7823 (3) | 0.099 (2) | |
HZ3_41 | 0.3530 | 0.6906 | 0.7755 | 0.118* | |
CE3_41 | 0.2812 (3) | 0.7022 (2) | 0.7451 (3) | 0.0839 (16) | |
HE3_41 | 0.2847 | 0.6878 | 0.7148 | 0.101* | |
CD2_41 | 0.2352 (3) | 0.7232 (2) | 0.7557 (2) | 0.0785 (15) | |
C_41 | 0.17128 (17) | 0.77309 (14) | 0.62655 (16) | 0.0545 (9) | |
O_41 | 0.20101 (13) | 0.80074 (11) | 0.63055 (15) | 0.0630 (8) | |
N_42 | 0.11912 (15) | 0.77678 (13) | 0.61905 (15) | 0.0578 (8) | |
H0_42 | 0.0992 | 0.7570 | 0.6237 | 0.069* | |
CA_42 | 0.09564 (17) | 0.81229 (15) | 0.60366 (17) | 0.0563 (9) | |
HA_42 | 0.1195 | 0.8333 | 0.6132 | 0.068* | |
CB_42 | 0.04247 (17) | 0.81925 (16) | 0.63018 (18) | 0.0590 (10) | |
HB1_42 | 0.0312 | 0.8453 | 0.6225 | 0.071* | |
HB2_42 | 0.0474 | 0.8175 | 0.6675 | 0.071* | |
CG_42 | −0.00185 (17) | 0.79152 (14) | 0.61445 (17) | 0.0548 (9) | |
OD1_42 | 0.00944 (13) | 0.76251 (12) | 0.58955 (15) | 0.0676 (9) | |
OD2_42 | −0.04793 (14) | 0.80024 (12) | 0.62854 (16) | 0.0676 (8) | |
C_42 | 0.09010 (15) | 0.81154 (14) | 0.54367 (16) | 0.0533 (9) | |
O_42 | 0.09885 (12) | 0.78198 (10) | 0.51906 (12) | 0.0548 (6) | |
N_43 | 0.07515 (14) | 0.84429 (12) | 0.51976 (14) | 0.0545 (8) | |
CA_43 | 0.06597 (16) | 0.84422 (14) | 0.46296 (16) | 0.0531 (8) | |
HA_43 | 0.0318 | 0.8324 | 0.4554 | 0.064* | |
CB_43 | 0.06430 (18) | 0.88705 (15) | 0.4485 (2) | 0.0605 (10) | |
HB1_43 | 0.0847 | 0.8918 | 0.4173 | 0.073* | |
HB2_43 | 0.0283 | 0.8953 | 0.4425 | 0.073* | |
CG_43 | 0.0881 (2) | 0.90848 (16) | 0.49477 (19) | 0.0639 (10) | |
HG1_43 | 0.0742 | 0.9344 | 0.4975 | 0.077* | |
HG2_43 | 0.1262 | 0.9096 | 0.4924 | 0.077* | |
CD_43 | 0.07039 (18) | 0.88345 (15) | 0.54075 (18) | 0.0589 (9) | |
HD1_43 | 0.0932 | 0.8871 | 0.5706 | 0.071* | |
HD2_43 | 0.0343 | 0.8891 | 0.5506 | 0.071* | |
C_43 | 0.11015 (16) | 0.82155 (15) | 0.43490 (17) | 0.0552 (9) | |
O_43 | 0.15649 (12) | 0.83055 (10) | 0.43968 (12) | 0.0569 (7) | |
N_44 | 0.09199 (14) | 0.79406 (12) | 0.40204 (14) | 0.0546 (8) | |
H0_44 | 0.0593 | 0.7939 | 0.3933 | 0.066* | |
CA_44 | 0.12739 (17) | 0.76470 (15) | 0.38130 (18) | 0.0575 (9) | |
HA_44 | 0.1632 | 0.7752 | 0.3794 | 0.069* | |
CB_44 | 0.11103 (18) | 0.75064 (16) | 0.32779 (19) | 0.0625 (10) | |
HB_44 | 0.0766 | 0.7381 | 0.3311 | 0.075* | |
CG1_44 | 0.1507 (3) | 0.7205 (2) | 0.3086 (2) | 0.0787 (15) | |
H1A_44 | 0.1535 | 0.7001 | 0.3338 | 0.118* | |
H1B_44 | 0.1845 | 0.7323 | 0.3040 | 0.118* | |
H1C_44 | 0.1390 | 0.7100 | 0.2761 | 0.118* | |
CG2_44 | 0.1055 (2) | 0.78325 (19) | 0.28915 (19) | 0.0701 (12) | |
H2A_44 | 0.0805 | 0.8016 | 0.3020 | 0.105* | |
H2B_44 | 0.0936 | 0.7732 | 0.2564 | 0.105* | |
H2C_44 | 0.1391 | 0.7956 | 0.2845 | 0.105* | |
C_44 | 0.12598 (17) | 0.73196 (14) | 0.42174 (17) | 0.0559 (9) | |
O_44 | 0.08397 (12) | 0.71466 (11) | 0.43031 (12) | 0.0580 (7) | |
N_45 | 0.17086 (15) | 0.72418 (13) | 0.44685 (15) | 0.0581 (8) | |
H0_45 | 0.1994 | 0.7353 | 0.4370 | 0.070* | |
CA_45 | 0.17268 (17) | 0.69729 (16) | 0.49046 (19) | 0.0599 (10) | |
HA_45 | 0.1366 | 0.6897 | 0.4994 | 0.072* | |
CB_45 | 0.20479 (18) | 0.66114 (17) | 0.4787 (2) | 0.0672 (12) | |
HB1_45 | 0.2383 | 0.6687 | 0.4638 | 0.081* | |
HB2_45 | 0.2119 | 0.6477 | 0.5110 | 0.081* | |
CG_45 | 0.1773 (2) | 0.63382 (19) | 0.4414 (3) | 0.0744 (13) | |
HG_45 | 0.1670 | 0.6481 | 0.4102 | 0.089* | |
CD1_45 | 0.1286 (2) | 0.6162 (2) | 0.4657 (3) | 0.0798 (15) | |
H1A_45 | 0.1125 | 0.5988 | 0.4414 | 0.120* | |
H1B_45 | 0.1041 | 0.6363 | 0.4745 | 0.120* | |
H1C_45 | 0.1382 | 0.6024 | 0.4966 | 0.120* | |
CD2_45 | 0.2156 (3) | 0.6014 (3) | 0.4259 (4) | 0.101 (2) | |
H2A_45 | 0.1983 | 0.5841 | 0.4023 | 0.151* | |
H2B_45 | 0.2264 | 0.5876 | 0.4564 | 0.151* | |
H2C_45 | 0.2459 | 0.6124 | 0.4092 | 0.151* | |
C_45 | 0.19660 (17) | 0.71936 (15) | 0.53662 (18) | 0.0578 (9) | |
O_45 | 0.23192 (17) | 0.74233 (15) | 0.53000 (15) | 0.0780 (11) | |
O1_51 | 0.31281 (13) | 0.89349 (11) | 0.58505 (12) | 0.0601 (7) | |
H1_51 | 0.3331 | 0.8928 | 0.6161 | 0.090* | |
H2_51 | 0.3174 | 0.8890 | 0.5481 | 0.090* | |
O1_52 | 0.25057 (14) | 0.93619 (11) | 0.47300 (13) | 0.0610 (7) | |
H1_52 | 0.2206 | 0.9371 | 0.4500 | 0.091* | |
H2_52 | 0.2620 | 0.9639 | 0.4740 | 0.091* | |
O1_53 | 0.30265 (12) | 0.78214 (11) | 0.58691 (14) | 0.0606 (7) | |
H1_53 | 0.2806 | 0.7644 | 0.5599 | 0.091* | |
H2_53 | 0.2690 | 0.7915 | 0.6071 | 0.091* | |
O1_54 | 0.21917 (15) | 0.84471 (12) | 0.53127 (14) | 0.0658 (8) | |
H1_54 | 0.1975 | 0.8390 | 0.4996 | 0.099* | |
H2_54 | 0.2120 | 0.8309 | 0.5645 | 0.099* | |
O1_55 | 0.3258 (2) | 0.87739 (14) | 0.47031 (16) | 0.0854 (13) | |
H1_55 | 0.3431 | 0.8699 | 0.4373 | 0.128* | |
H2_55 | 0.2978 | 0.8992 | 0.4708 | 0.128* | |
O1_56 | 0.34921 (13) | 0.96514 (11) | 0.54999 (13) | 0.0617 (7) | |
H1_56 | 0.3620 | 0.9628 | 0.5152 | 0.093* | |
H2_56 | 0.3351 | 0.9409 | 0.5618 | 0.093* | |
O1_57 | 0.24800 (12) | 0.78512 (12) | 0.41698 (14) | 0.0632 (8) | |
H1_57 | 0.2815 | 0.7864 | 0.4370 | 0.095* | |
H2_57 | 0.2169 | 0.8000 | 0.4238 | 0.095* | |
O1_58 | 0.16080 (14) | 1.01784 (13) | 0.52212 (13) | 0.0687 (9) | |
H1_58 | 0.1525 | 1.0369 | 0.5522 | 0.103* | |
H2_58 | 0.1888 | 1.0028 | 0.5446 | 0.103* | |
O1_61 | 0.36338 (19) | 0.93024 (14) | 0.10325 (14) | 0.0784 (11) | |
H1_61 | 0.3612 | 0.9314 | 0.1401 | 0.118* | |
C1_61 | 0.3978 (3) | 0.8978 (2) | 0.0973 (2) | 0.0841 (16) | |
H1A_61 | 0.3797 | 0.8748 | 0.1103 | 0.101* | |
C2_61 | 0.4065 (5) | 0.8932 (3) | 0.0390 (3) | 0.120 (3) | |
H2A_61 | 0.3732 | 0.8900 | 0.0220 | 0.179* | |
H2B_61 | 0.4281 | 0.8710 | 0.0328 | 0.179* | |
H2C_61 | 0.4237 | 0.9157 | 0.0257 | 0.179* | |
C3_61 | 0.4491 (3) | 0.9020 (3) | 0.1259 (3) | 0.099 (2) | |
H3A_61 | 0.4424 | 0.9048 | 0.1624 | 0.149* | |
H3B_61 | 0.4674 | 0.9244 | 0.1134 | 0.149* | |
H3C_61 | 0.4704 | 0.8796 | 0.1201 | 0.149* | |
O1_62 | 0.3705 (3) | 1.18808 (17) | 0.3744 (2) | 0.115 (2) | |
H1_62 | 0.3655 | 1.1622 | 0.3705 | 0.172* | |
C1_62 | 0.3966 (6) | 1.1960 (3) | 0.4204 (4) | 0.133 (4) | |
H1A_62 | 0.4328 | 1.1884 | 0.4120 | 0.159* | |
C2_62 | 0.3863 (9) | 1.1737 (6) | 0.4675 (5) | 0.199 (9) | |
H2A_62 | 0.3873 | 1.1467 | 0.4594 | 0.298* | |
H2B_62 | 0.3521 | 1.1803 | 0.4808 | 0.298* | |
H2C_62 | 0.4126 | 1.1795 | 0.4931 | 0.298* | |
C3_62 | 0.4018 (8) | 1.2377 (3) | 0.4278 (5) | 0.157 (6) | |
H3A_62 | 0.4072 | 1.2499 | 0.3947 | 0.236* | |
H3B_62 | 0.4313 | 1.2429 | 0.4500 | 0.236* | |
H3C_62 | 0.3703 | 1.2476 | 0.4434 | 0.236* | |
O1_63 | −0.0929 (2) | 0.8623 (2) | 0.6696 (4) | 0.133 (3) | |
H1_63 | −0.0762 | 0.8389 | 0.6532 | 0.200* | |
C1_63 | −0.1463 (4) | 0.8642 (3) | 0.6664 (6) | 0.142 (5) | |
H1A_63 | −0.1501 | 0.8704 | 0.6294 | 0.170* | |
C2_63 | −0.1791 (4) | 0.8299 (3) | 0.6688 (6) | 0.129 (4) | |
H2A_63 | −0.1631 | 0.8097 | 0.6489 | 0.194* | |
H2B_63 | −0.2132 | 0.8356 | 0.6548 | 0.194* | |
H2C_63 | −0.1826 | 0.8219 | 0.7044 | 0.194* | |
C3_63 | −0.1677 (5) | 0.8999 (4) | 0.6894 (7) | 0.151 (5) | |
H3A_63 | −0.1437 | 0.9207 | 0.6834 | 0.226* | |
H3B_63 | −0.1725 | 0.8963 | 0.7261 | 0.226* | |
H3C_63 | −0.2010 | 0.9057 | 0.6736 | 0.226* | |
O1_64 | 0.1291 (3) | 0.5661 (2) | 0.6172 (5) | 0.145 (3) | |
H1_64 | 0.1210 | 0.5921 | 0.6156 | 0.218* | |
C1_64 | 0.1801 (4) | 0.5576 (5) | 0.6319 (9) | 0.183 (8) | |
H1A_64 | 0.1796 | 0.5627 | 0.6694 | 0.220* | |
C2_64 | 0.2215 (5) | 0.5834 (5) | 0.6135 (10) | 0.192 (9) | |
H2A_64 | 0.2107 | 0.6096 | 0.6183 | 0.288* | |
H2B_64 | 0.2279 | 0.5787 | 0.5772 | 0.288* | |
H2C_64 | 0.2532 | 0.5787 | 0.6328 | 0.288* | |
C3_64 | 0.1941 (12) | 0.5153 (5) | 0.6296 (11) | 0.250 (14) | |
H3A_64 | 0.1678 | 0.5006 | 0.6477 | 0.375* | |
H3B_64 | 0.2278 | 0.5113 | 0.6456 | 0.375* | |
H3C_64 | 0.1955 | 0.5071 | 0.5939 | 0.375* | |
O1_65 | 0.0466 (5) | 0.8023 (5) | 0.7840 (8) | 0.227 (7) | |
H1_65 | 0.0728 | 0.8044 | 0.8112 | 0.340* | |
C1_65 | −0.0038 (8) | 0.8206 (6) | 0.7983 (9) | 0.81 (12) | |
H1A_65 | −0.0097 | 0.8245 | 0.8356 | 0.974* | |
C2_65 | −0.0436 (10) | 0.7940 (7) | 0.7704 (7) | 0.238 (14) | |
H2A_65 | −0.0462 | 0.7700 | 0.7887 | 0.357* | |
H2B_65 | −0.0318 | 0.7893 | 0.7355 | 0.357* | |
H2C_65 | −0.0775 | 0.8062 | 0.7695 | 0.357* | |
C3_65 | −0.0046 (5) | 0.8577 (3) | 0.7641 (4) | 0.245 (13) | |
H3A_65 | 0.0190 | 0.8765 | 0.7786 | 0.368* | |
H3B_65 | −0.0396 | 0.8680 | 0.7633 | 0.368* | |
H3C_65 | 0.0064 | 0.8514 | 0.7294 | 0.368* | |
O1_66 | 0.0743 (5) | 0.6259 (3) | 0.7244 (4) | 0.158 (6) | 0.63 |
H1_66 | 0.0851 | 0.6300 | 0.6908 | 0.237* | 0.63 |
C1_66 | 0.0725 (5) | 0.6615 (3) | 0.7530 (4) | 0.33 (4) | 0.63 |
H1A_66 | 0.1085 | 0.6717 | 0.7542 | 0.399* | 0.63 |
C2_66 | 0.0382 (6) | 0.6914 (6) | 0.7245 (8) | 0.134 (7) | 0.63 |
H2A_66 | 0.0519 | 0.6954 | 0.6901 | 0.202* | 0.63 |
H2B_66 | 0.0388 | 0.7153 | 0.7433 | 0.202* | 0.63 |
H2C_66 | 0.0027 | 0.6821 | 0.7223 | 0.202* | 0.63 |
C3_66 | 0.0531 (12) | 0.6589 (11) | 0.8081 (8) | 0.25 (2) | 0.63 |
H3A_66 | 0.0724 | 0.6393 | 0.8263 | 0.370* | 0.63 |
H3B_66 | 0.0163 | 0.6526 | 0.8082 | 0.370* | 0.63 |
H3C_66 | 0.0583 | 0.6833 | 0.8251 | 0.370* | 0.63 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na_1 | 0.0557 (8) | 0.0605 (10) | 0.0460 (7) | 0.0006 (7) | −0.0004 (6) | 0.0049 (6) |
Na_2 | 0.0508 (8) | 0.0629 (10) | 0.0554 (8) | −0.0062 (7) | 0.0024 (7) | −0.0049 (7) |
Na_3 | 0.0574 (8) | 0.0642 (11) | 0.0468 (7) | 0.0017 (7) | −0.0013 (6) | −0.0040 (7) |
Na_4 | 0.0558 (8) | 0.0626 (10) | 0.0515 (8) | 0.0035 (7) | 0.0023 (7) | −0.0007 (7) |
N_11 | 0.0541 (17) | 0.062 (2) | 0.0455 (15) | 0.0006 (14) | 0.0003 (13) | 0.0024 (13) |
CA_11 | 0.0512 (19) | 0.066 (3) | 0.0480 (18) | 0.0031 (17) | 0.0017 (15) | 0.0035 (16) |
CB_11 | 0.054 (2) | 0.075 (3) | 0.056 (2) | 0.0027 (19) | −0.0039 (17) | 0.0012 (19) |
CG_11 | 0.056 (2) | 0.065 (3) | 0.067 (3) | 0.0054 (18) | −0.0049 (19) | 0.009 (2) |
CD1_11 | 0.061 (2) | 0.070 (3) | 0.086 (3) | 0.004 (2) | −0.004 (2) | 0.001 (2) |
NE1_11 | 0.061 (2) | 0.076 (3) | 0.101 (4) | −0.0043 (19) | −0.009 (2) | 0.012 (2) |
CE2_11 | 0.057 (2) | 0.082 (4) | 0.076 (3) | 0.003 (2) | 0.000 (2) | 0.011 (2) |
CZ2_11 | 0.059 (3) | 0.090 (4) | 0.102 (4) | 0.005 (2) | 0.012 (3) | 0.033 (4) |
CH2_11 | 0.077 (3) | 0.123 (6) | 0.083 (4) | 0.005 (4) | 0.023 (3) | 0.010 (4) |
CZ3_11 | 0.081 (4) | 0.126 (6) | 0.068 (3) | 0.012 (4) | 0.004 (3) | −0.006 (3) |
CE3_11 | 0.062 (3) | 0.090 (4) | 0.071 (3) | 0.000 (2) | 0.001 (2) | 0.008 (3) |
CD2_11 | 0.055 (2) | 0.078 (3) | 0.061 (2) | 0.004 (2) | −0.0035 (18) | 0.014 (2) |
C_11 | 0.0444 (17) | 0.068 (3) | 0.0464 (18) | −0.0054 (16) | 0.0031 (14) | 0.0055 (16) |
O_11 | 0.0596 (16) | 0.0655 (19) | 0.0517 (15) | −0.0031 (13) | −0.0036 (12) | 0.0035 (13) |
N_12 | 0.0578 (18) | 0.062 (2) | 0.0504 (17) | 0.0005 (15) | 0.0027 (14) | 0.0061 (15) |
CA_12 | 0.0531 (19) | 0.066 (3) | 0.0475 (19) | −0.0019 (17) | 0.0023 (15) | 0.0024 (16) |
CB_12 | 0.057 (2) | 0.062 (3) | 0.0497 (19) | −0.0054 (17) | −0.0008 (16) | 0.0008 (17) |
CG_12 | 0.056 (2) | 0.064 (3) | 0.051 (2) | −0.0056 (17) | −0.0001 (16) | −0.0023 (17) |
OD1_12 | 0.0677 (17) | 0.0591 (19) | 0.0504 (14) | −0.0066 (14) | −0.0038 (13) | 0.0017 (12) |
OD2_12 | 0.077 (2) | 0.070 (2) | 0.0482 (15) | −0.0080 (16) | −0.0069 (14) | 0.0042 (13) |
C_12 | 0.0535 (19) | 0.058 (2) | 0.0445 (17) | −0.0037 (16) | −0.0017 (15) | 0.0049 (15) |
O_12 | 0.0540 (14) | 0.0651 (19) | 0.0472 (13) | −0.0036 (13) | 0.0000 (11) | 0.0037 (12) |
N_13 | 0.0530 (17) | 0.054 (2) | 0.0524 (17) | 0.0024 (13) | 0.0036 (14) | 0.0038 (13) |
CA_13 | 0.055 (2) | 0.066 (3) | 0.0477 (19) | 0.0016 (17) | 0.0048 (16) | 0.0038 (16) |
CB_13 | 0.059 (2) | 0.065 (3) | 0.063 (2) | 0.0059 (19) | 0.0049 (19) | −0.0004 (19) |
CG_13 | 0.062 (2) | 0.068 (3) | 0.069 (3) | 0.005 (2) | 0.002 (2) | 0.007 (2) |
CD_13 | 0.062 (2) | 0.055 (3) | 0.069 (3) | −0.0038 (18) | 0.005 (2) | 0.0051 (19) |
C_13 | 0.0514 (19) | 0.069 (3) | 0.0489 (19) | 0.0059 (17) | 0.0047 (16) | 0.0084 (17) |
O_13 | 0.0629 (16) | 0.074 (2) | 0.0498 (15) | 0.0025 (14) | −0.0020 (13) | 0.0097 (14) |
N_14 | 0.0537 (16) | 0.061 (2) | 0.0472 (16) | 0.0002 (14) | 0.0008 (13) | 0.0061 (14) |
CA_14 | 0.0516 (18) | 0.065 (3) | 0.0487 (19) | 0.0030 (17) | −0.0023 (15) | 0.0024 (16) |
CB_14 | 0.0520 (19) | 0.068 (3) | 0.060 (2) | −0.0015 (18) | 0.0019 (17) | 0.0046 (19) |
CG1_14 | 0.062 (2) | 0.075 (3) | 0.072 (3) | −0.013 (2) | 0.005 (2) | −0.006 (2) |
CG2_14 | 0.051 (2) | 0.079 (3) | 0.073 (3) | 0.000 (2) | 0.0037 (19) | 0.010 (2) |
C_14 | 0.0536 (19) | 0.059 (2) | 0.0450 (18) | −0.0013 (16) | −0.0044 (15) | 0.0048 (15) |
O_14 | 0.0547 (14) | 0.0664 (19) | 0.0433 (13) | −0.0011 (12) | 0.0032 (11) | 0.0028 (11) |
N_15 | 0.0570 (17) | 0.058 (2) | 0.0438 (15) | 0.0018 (14) | 0.0003 (13) | 0.0047 (13) |
CA_15 | 0.0537 (19) | 0.063 (3) | 0.0461 (18) | 0.0024 (17) | −0.0019 (15) | 0.0040 (16) |
CB_15 | 0.063 (2) | 0.064 (3) | 0.0469 (18) | −0.0045 (18) | 0.0031 (17) | −0.0007 (16) |
CG_15 | 0.066 (2) | 0.075 (3) | 0.056 (2) | −0.008 (2) | 0.0046 (19) | −0.007 (2) |
CD1_15 | 0.089 (3) | 0.070 (3) | 0.065 (3) | −0.015 (3) | 0.011 (3) | 0.001 (2) |
CD2_15 | 0.094 (4) | 0.090 (4) | 0.064 (3) | −0.033 (3) | 0.009 (3) | −0.014 (3) |
C_15 | 0.0557 (19) | 0.059 (2) | 0.0447 (17) | 0.0032 (16) | −0.0015 (15) | 0.0001 (15) |
O_15 | 0.0569 (15) | 0.0625 (19) | 0.0498 (14) | 0.0017 (12) | 0.0007 (12) | 0.0035 (12) |
N_21 | 0.0623 (19) | 0.063 (2) | 0.0507 (17) | −0.0025 (16) | −0.0031 (15) | 0.0018 (15) |
CA_21 | 0.061 (2) | 0.058 (3) | 0.052 (2) | −0.0031 (17) | −0.0046 (17) | 0.0014 (17) |
CB_21 | 0.072 (3) | 0.069 (3) | 0.065 (3) | −0.011 (2) | −0.001 (2) | 0.003 (2) |
CG_21 | 0.066 (3) | 0.082 (4) | 0.092 (4) | −0.015 (3) | 0.002 (3) | 0.008 (3) |
CD1_21 | 0.064 (3) | 0.083 (5) | 0.131 (6) | −0.005 (3) | 0.008 (3) | −0.011 (4) |
NE1_21 | 0.065 (3) | 0.078 (4) | 0.222 (11) | −0.010 (2) | 0.020 (4) | 0.002 (5) |
CE2_21 | 0.065 (3) | 0.081 (5) | 0.146 (7) | −0.008 (3) | −0.005 (4) | 0.011 (5) |
CZ2_21 | 0.066 (4) | 0.137 (10) | 0.28 (2) | −0.010 (5) | −0.026 (7) | 0.120 (13) |
CH2_21 | 0.087 (6) | 0.195 (15) | 0.188 (13) | −0.035 (7) | −0.031 (8) | 0.101 (13) |
CZ3_21 | 0.096 (5) | 0.198 (13) | 0.136 (8) | −0.048 (7) | −0.023 (5) | 0.060 (9) |
CE3_21 | 0.083 (4) | 0.148 (8) | 0.077 (4) | −0.036 (4) | −0.009 (3) | 0.013 (4) |
CD2_21 | 0.063 (3) | 0.092 (5) | 0.116 (5) | −0.013 (3) | −0.013 (3) | 0.031 (4) |
C_21 | 0.0458 (17) | 0.066 (3) | 0.0482 (19) | −0.0022 (16) | −0.0003 (14) | −0.0006 (16) |
O_21 | 0.0611 (16) | 0.0631 (19) | 0.0483 (14) | 0.0009 (13) | −0.0028 (12) | 0.0035 (12) |
N_22 | 0.0558 (17) | 0.065 (2) | 0.0436 (16) | −0.0015 (15) | 0.0011 (13) | 0.0038 (14) |
CA_22 | 0.0505 (19) | 0.060 (2) | 0.0483 (19) | 0.0011 (16) | 0.0006 (15) | 0.0049 (16) |
CB_22 | 0.0546 (19) | 0.071 (3) | 0.0460 (19) | 0.0020 (18) | −0.0005 (16) | 0.0009 (17) |
CG_22 | 0.058 (2) | 0.064 (3) | 0.0466 (19) | −0.0028 (18) | 0.0027 (16) | 0.0037 (16) |
OD1_22 | 0.0590 (15) | 0.067 (2) | 0.0494 (14) | 0.0074 (13) | −0.0001 (12) | 0.0052 (12) |
OD2_22 | 0.090 (2) | 0.070 (2) | 0.0510 (16) | 0.0110 (18) | 0.0030 (16) | 0.0031 (14) |
C_22 | 0.053 (2) | 0.067 (3) | 0.0421 (17) | 0.0037 (17) | 0.0017 (15) | 0.0056 (16) |
O_22 | 0.0506 (13) | 0.0631 (18) | 0.0463 (13) | 0.0021 (12) | −0.0012 (11) | 0.0032 (11) |
N_23 | 0.0530 (17) | 0.058 (2) | 0.0509 (17) | −0.0024 (14) | −0.0023 (14) | 0.0029 (14) |
CA_23 | 0.055 (2) | 0.065 (3) | 0.0485 (19) | −0.0010 (17) | −0.0013 (16) | 0.0026 (16) |
CB_23 | 0.062 (2) | 0.064 (3) | 0.057 (2) | −0.0021 (19) | −0.0028 (18) | −0.0011 (18) |
CG_23 | 0.066 (2) | 0.070 (3) | 0.064 (2) | 0.000 (2) | −0.006 (2) | 0.002 (2) |
CD_23 | 0.061 (2) | 0.056 (3) | 0.070 (3) | 0.0014 (18) | −0.010 (2) | 0.0040 (19) |
C_23 | 0.0469 (18) | 0.071 (3) | 0.0461 (19) | −0.0066 (16) | −0.0020 (15) | 0.0072 (17) |
O_23 | 0.0577 (15) | 0.072 (2) | 0.0514 (15) | −0.0058 (14) | 0.0030 (12) | 0.0100 (13) |
N_24 | 0.0558 (17) | 0.064 (2) | 0.0525 (17) | 0.0000 (15) | −0.0003 (14) | 0.0008 (15) |
CA_24 | 0.057 (2) | 0.070 (3) | 0.0448 (18) | 0.0035 (18) | 0.0029 (16) | 0.0028 (17) |
CB_24 | 0.060 (2) | 0.080 (3) | 0.055 (2) | 0.006 (2) | 0.0007 (18) | −0.002 (2) |
CG1_24 | 0.058 (2) | 0.101 (4) | 0.066 (3) | 0.001 (2) | 0.003 (2) | −0.003 (3) |
CG2_24 | 0.062 (3) | 0.098 (4) | 0.081 (3) | 0.016 (3) | 0.005 (2) | −0.014 (3) |
C_24 | 0.057 (2) | 0.062 (2) | 0.0435 (18) | 0.0054 (17) | 0.0024 (15) | 0.0037 (15) |
O_24 | 0.0559 (15) | 0.0670 (19) | 0.0472 (14) | 0.0009 (13) | −0.0018 (12) | 0.0011 (12) |
N_25 | 0.0590 (18) | 0.073 (2) | 0.0431 (16) | 0.0029 (16) | 0.0014 (14) | 0.0044 (15) |
CA_25 | 0.060 (2) | 0.066 (3) | 0.0453 (18) | 0.0004 (18) | −0.0027 (16) | 0.0000 (17) |
CB_25 | 0.076 (3) | 0.067 (3) | 0.059 (2) | 0.005 (2) | −0.009 (2) | −0.004 (2) |
CG_25 | 0.083 (3) | 0.072 (4) | 0.086 (4) | 0.010 (3) | −0.018 (3) | −0.007 (3) |
CD1_25 | 0.093 (4) | 0.072 (4) | 0.106 (5) | 0.005 (3) | −0.029 (4) | 0.016 (3) |
CD2_25 | 0.136 (7) | 0.080 (5) | 0.123 (6) | 0.032 (5) | −0.031 (6) | −0.032 (4) |
C_25 | 0.064 (2) | 0.059 (3) | 0.0416 (17) | 0.0005 (17) | −0.0012 (16) | −0.0028 (15) |
O_25 | 0.0587 (15) | 0.068 (2) | 0.0465 (13) | 0.0023 (13) | 0.0009 (12) | 0.0056 (12) |
N_31 | 0.0519 (16) | 0.061 (2) | 0.0526 (18) | −0.0030 (14) | −0.0006 (14) | −0.0065 (15) |
CA_31 | 0.0503 (18) | 0.064 (3) | 0.054 (2) | −0.0009 (16) | −0.0003 (16) | −0.0038 (17) |
CB_31 | 0.066 (2) | 0.064 (3) | 0.051 (2) | −0.0027 (19) | −0.0021 (18) | −0.0078 (18) |
CG_31 | 0.072 (3) | 0.068 (3) | 0.052 (2) | −0.006 (2) | 0.0005 (19) | −0.0037 (18) |
CD1_31 | 0.078 (3) | 0.078 (4) | 0.056 (2) | 0.010 (2) | 0.001 (2) | −0.003 (2) |
NE1_31 | 0.092 (3) | 0.074 (3) | 0.061 (2) | −0.002 (2) | −0.004 (2) | 0.0023 (19) |
CE2_31 | 0.079 (3) | 0.076 (3) | 0.055 (2) | −0.010 (2) | 0.000 (2) | −0.003 (2) |
CZ2_31 | 0.101 (4) | 0.086 (4) | 0.066 (3) | −0.016 (3) | 0.009 (3) | 0.005 (3) |
CH2_31 | 0.094 (4) | 0.102 (5) | 0.096 (5) | −0.017 (4) | 0.032 (4) | −0.007 (4) |
CZ3_31 | 0.079 (3) | 0.101 (5) | 0.090 (4) | 0.001 (3) | 0.015 (3) | −0.008 (3) |
CE3_31 | 0.076 (3) | 0.085 (4) | 0.076 (3) | −0.003 (3) | 0.014 (3) | −0.001 (3) |
CD2_31 | 0.073 (3) | 0.078 (3) | 0.055 (2) | −0.007 (2) | 0.000 (2) | −0.002 (2) |
C_31 | 0.0505 (18) | 0.071 (3) | 0.0443 (17) | −0.0037 (17) | 0.0005 (15) | −0.0030 (16) |
O_31 | 0.0545 (15) | 0.0633 (19) | 0.0550 (15) | −0.0111 (12) | 0.0061 (12) | −0.0006 (12) |
N_32 | 0.0474 (15) | 0.066 (2) | 0.0500 (17) | −0.0035 (14) | −0.0016 (13) | −0.0040 (15) |
CA_32 | 0.0447 (17) | 0.072 (3) | 0.052 (2) | −0.0059 (16) | −0.0026 (15) | −0.0056 (18) |
CB_32 | 0.056 (2) | 0.062 (3) | 0.061 (2) | 0.0031 (17) | −0.0054 (18) | 0.0034 (18) |
CG_32 | 0.056 (2) | 0.084 (4) | 0.064 (3) | 0.001 (2) | −0.0050 (19) | −0.012 (2) |
OD1_32 | 0.0580 (16) | 0.084 (3) | 0.0678 (19) | −0.0122 (16) | −0.0019 (15) | 0.0072 (17) |
OD2_32 | 0.071 (2) | 0.081 (3) | 0.211 (8) | 0.003 (2) | −0.057 (4) | −0.007 (4) |
C_32 | 0.0449 (17) | 0.053 (2) | 0.054 (2) | −0.0025 (14) | 0.0023 (14) | 0.0009 (16) |
O_32 | 0.0524 (14) | 0.0575 (19) | 0.0578 (15) | −0.0031 (12) | 0.0015 (12) | −0.0004 (12) |
N_33 | 0.0512 (16) | 0.0490 (19) | 0.0560 (18) | −0.0035 (13) | 0.0022 (14) | −0.0046 (13) |
CA_33 | 0.0457 (17) | 0.068 (3) | 0.053 (2) | −0.0033 (16) | 0.0002 (15) | −0.0057 (18) |
CB_33 | 0.056 (2) | 0.071 (3) | 0.055 (2) | 0.0058 (18) | 0.0028 (17) | −0.0080 (19) |
CG_33 | 0.065 (2) | 0.064 (3) | 0.062 (2) | −0.0052 (19) | 0.002 (2) | −0.011 (2) |
CD_33 | 0.058 (2) | 0.054 (2) | 0.059 (2) | −0.0036 (16) | 0.0010 (17) | −0.0027 (17) |
C_33 | 0.0498 (19) | 0.064 (3) | 0.054 (2) | −0.0053 (17) | 0.0011 (16) | −0.0023 (17) |
O_33 | 0.0483 (13) | 0.0685 (19) | 0.0546 (15) | −0.0041 (12) | 0.0001 (11) | −0.0034 (13) |
N_34 | 0.0513 (16) | 0.066 (2) | 0.0503 (17) | −0.0029 (14) | −0.0001 (14) | −0.0027 (15) |
CA_34 | 0.0473 (18) | 0.064 (3) | 0.056 (2) | −0.0051 (16) | 0.0022 (16) | 0.0011 (18) |
CB_34 | 0.062 (2) | 0.063 (3) | 0.054 (2) | −0.0094 (18) | −0.0019 (17) | 0.0017 (18) |
CG1_34 | 0.071 (3) | 0.084 (3) | 0.049 (2) | −0.012 (2) | 0.0040 (19) | −0.002 (2) |
CG2_34 | 0.094 (4) | 0.073 (4) | 0.069 (3) | 0.007 (3) | 0.008 (3) | 0.011 (2) |
C_34 | 0.0513 (19) | 0.059 (2) | 0.053 (2) | −0.0037 (16) | −0.0011 (16) | 0.0059 (16) |
O_34 | 0.0480 (13) | 0.0628 (18) | 0.0549 (15) | −0.0075 (12) | 0.0014 (11) | −0.0010 (12) |
N_35 | 0.0452 (15) | 0.061 (2) | 0.0548 (18) | −0.0032 (13) | −0.0002 (13) | 0.0002 (14) |
CA_35 | 0.0452 (17) | 0.062 (3) | 0.058 (2) | −0.0006 (16) | 0.0037 (16) | −0.0017 (17) |
CB_35 | 0.0475 (18) | 0.067 (3) | 0.064 (2) | 0.0028 (17) | 0.0059 (17) | 0.0060 (19) |
CG_35 | 0.059 (2) | 0.064 (3) | 0.080 (3) | 0.0017 (19) | 0.012 (2) | 0.007 (2) |
CD1_35 | 0.068 (3) | 0.072 (4) | 0.112 (5) | 0.006 (2) | 0.008 (3) | 0.020 (3) |
CD2_35 | 0.056 (2) | 0.068 (3) | 0.103 (4) | −0.002 (2) | 0.007 (3) | 0.003 (3) |
C_35 | 0.0427 (16) | 0.062 (2) | 0.054 (2) | 0.0013 (15) | 0.0017 (15) | 0.0011 (17) |
O_35 | 0.0522 (14) | 0.0587 (18) | 0.0547 (15) | −0.0037 (12) | 0.0014 (12) | −0.0032 (12) |
N_41 | 0.0613 (19) | 0.060 (2) | 0.058 (2) | −0.0099 (15) | 0.0029 (16) | −0.0056 (15) |
CA_41 | 0.058 (2) | 0.063 (3) | 0.056 (2) | −0.0050 (18) | 0.0017 (18) | −0.0019 (18) |
CB_41 | 0.077 (3) | 0.063 (3) | 0.062 (2) | −0.008 (2) | 0.005 (2) | 0.004 (2) |
CG_41 | 0.088 (3) | 0.071 (3) | 0.061 (3) | −0.012 (3) | 0.006 (2) | 0.008 (2) |
CD1_41 | 0.098 (4) | 0.077 (4) | 0.066 (3) | −0.011 (3) | 0.011 (3) | 0.003 (2) |
NE1_41 | 0.128 (5) | 0.076 (3) | 0.056 (2) | −0.016 (3) | 0.006 (3) | −0.002 (2) |
CE2_41 | 0.104 (4) | 0.077 (4) | 0.059 (3) | −0.003 (3) | −0.003 (3) | 0.002 (2) |
CZ2_41 | 0.132 (6) | 0.084 (5) | 0.072 (3) | −0.025 (4) | −0.020 (4) | 0.005 (3) |
CH2_41 | 0.114 (6) | 0.111 (6) | 0.105 (6) | −0.008 (5) | −0.039 (5) | 0.011 (5) |
CZ3_41 | 0.095 (4) | 0.103 (5) | 0.098 (5) | −0.010 (4) | −0.021 (4) | 0.022 (4) |
CE3_41 | 0.092 (4) | 0.083 (4) | 0.076 (3) | −0.001 (3) | −0.004 (3) | 0.015 (3) |
CD2_41 | 0.095 (4) | 0.080 (4) | 0.060 (3) | −0.019 (3) | −0.004 (3) | 0.009 (2) |
C_41 | 0.053 (2) | 0.065 (3) | 0.0452 (18) | −0.0112 (17) | 0.0023 (15) | −0.0003 (16) |
O_41 | 0.0541 (15) | 0.069 (2) | 0.0664 (18) | −0.0059 (13) | 0.0006 (14) | −0.0055 (15) |
N_42 | 0.0537 (18) | 0.065 (2) | 0.0547 (18) | −0.0118 (15) | −0.0045 (15) | 0.0026 (15) |
CA_42 | 0.0483 (19) | 0.068 (3) | 0.052 (2) | −0.0111 (17) | 0.0010 (16) | 0.0010 (17) |
CB_42 | 0.056 (2) | 0.069 (3) | 0.052 (2) | −0.0058 (18) | 0.0023 (17) | −0.0047 (18) |
CG_42 | 0.0525 (19) | 0.064 (3) | 0.0482 (19) | −0.0006 (17) | 0.0036 (15) | −0.0016 (16) |
OD1_42 | 0.0546 (15) | 0.079 (2) | 0.0690 (19) | −0.0080 (15) | 0.0064 (14) | −0.0199 (17) |
OD2_42 | 0.0552 (16) | 0.072 (2) | 0.076 (2) | −0.0061 (14) | 0.0085 (15) | −0.0086 (17) |
C_42 | 0.0442 (17) | 0.065 (3) | 0.051 (2) | −0.0073 (15) | 0.0011 (14) | −0.0040 (16) |
O_42 | 0.0502 (13) | 0.0605 (18) | 0.0536 (15) | −0.0048 (12) | 0.0010 (11) | −0.0011 (12) |
N_43 | 0.0504 (16) | 0.062 (2) | 0.0507 (17) | −0.0009 (14) | 0.0024 (13) | −0.0025 (14) |
CA_43 | 0.0477 (17) | 0.060 (2) | 0.052 (2) | −0.0033 (15) | 0.0037 (15) | −0.0024 (16) |
CB_43 | 0.055 (2) | 0.064 (3) | 0.062 (2) | −0.0028 (17) | 0.0041 (18) | 0.0045 (19) |
CG_43 | 0.066 (2) | 0.066 (3) | 0.060 (2) | −0.007 (2) | 0.004 (2) | −0.0002 (19) |
CD_43 | 0.056 (2) | 0.063 (3) | 0.058 (2) | −0.0033 (17) | 0.0013 (17) | −0.0063 (18) |
C_43 | 0.0490 (18) | 0.066 (3) | 0.0508 (19) | −0.0053 (16) | 0.0026 (15) | −0.0024 (17) |
O_43 | 0.0498 (14) | 0.0651 (19) | 0.0558 (15) | −0.0067 (12) | 0.0022 (12) | −0.0038 (13) |
N_44 | 0.0487 (16) | 0.063 (2) | 0.0517 (17) | −0.0075 (14) | −0.0015 (13) | −0.0028 (15) |
CA_44 | 0.0505 (18) | 0.068 (3) | 0.054 (2) | −0.0056 (17) | 0.0048 (16) | −0.0030 (18) |
CB_44 | 0.056 (2) | 0.073 (3) | 0.059 (2) | −0.0117 (19) | 0.0038 (18) | −0.003 (2) |
CG1_44 | 0.087 (3) | 0.087 (4) | 0.062 (3) | −0.003 (3) | −0.001 (3) | −0.015 (2) |
CG2_44 | 0.075 (3) | 0.085 (4) | 0.051 (2) | −0.015 (2) | 0.003 (2) | −0.008 (2) |
C_44 | 0.0505 (19) | 0.063 (3) | 0.055 (2) | −0.0010 (16) | 0.0028 (16) | −0.0129 (17) |
O_44 | 0.0484 (13) | 0.071 (2) | 0.0545 (15) | −0.0049 (12) | 0.0033 (12) | −0.0047 (13) |
N_45 | 0.0495 (16) | 0.069 (2) | 0.0558 (18) | −0.0088 (15) | 0.0021 (14) | −0.0121 (16) |
CA_45 | 0.0496 (18) | 0.070 (3) | 0.060 (2) | −0.0033 (17) | −0.0018 (17) | −0.0093 (19) |
CB_45 | 0.049 (2) | 0.075 (3) | 0.078 (3) | −0.0027 (19) | −0.002 (2) | −0.009 (2) |
CG_45 | 0.064 (2) | 0.079 (4) | 0.080 (3) | 0.001 (2) | −0.007 (2) | −0.019 (3) |
CD1_45 | 0.063 (3) | 0.076 (4) | 0.100 (4) | −0.005 (2) | −0.014 (3) | −0.020 (3) |
CD2_45 | 0.097 (4) | 0.097 (5) | 0.110 (5) | 0.006 (4) | 0.007 (4) | −0.038 (4) |
C_45 | 0.0510 (19) | 0.065 (3) | 0.057 (2) | 0.0007 (17) | −0.0040 (17) | −0.0004 (18) |
O_45 | 0.077 (2) | 0.101 (3) | 0.0564 (17) | −0.036 (2) | −0.0008 (16) | −0.0009 (18) |
O1_51 | 0.0617 (16) | 0.067 (2) | 0.0519 (15) | 0.0056 (13) | −0.0033 (13) | −0.0035 (13) |
O1_52 | 0.0654 (16) | 0.067 (2) | 0.0503 (15) | 0.0026 (14) | −0.0026 (13) | −0.0001 (13) |
O1_53 | 0.0448 (13) | 0.074 (2) | 0.0626 (17) | −0.0026 (12) | −0.0024 (12) | −0.0011 (14) |
O1_54 | 0.0709 (18) | 0.071 (2) | 0.0550 (16) | −0.0111 (15) | 0.0016 (14) | −0.0024 (14) |
O1_55 | 0.114 (3) | 0.086 (3) | 0.0567 (18) | 0.034 (2) | 0.022 (2) | 0.0144 (17) |
O1_56 | 0.0588 (16) | 0.072 (2) | 0.0544 (15) | 0.0094 (14) | 0.0035 (13) | −0.0024 (14) |
O1_57 | 0.0509 (14) | 0.077 (2) | 0.0620 (17) | −0.0049 (13) | 0.0010 (13) | −0.0080 (15) |
O1_58 | 0.0653 (17) | 0.089 (3) | 0.0516 (16) | 0.0115 (17) | 0.0007 (14) | 0.0062 (15) |
O1_61 | 0.093 (3) | 0.090 (3) | 0.0517 (17) | 0.021 (2) | 0.0005 (17) | 0.0029 (16) |
C1_61 | 0.100 (4) | 0.088 (4) | 0.065 (3) | 0.011 (3) | 0.003 (3) | −0.010 (3) |
C2_61 | 0.165 (9) | 0.121 (7) | 0.073 (4) | 0.035 (7) | 0.011 (5) | −0.018 (4) |
C3_61 | 0.090 (4) | 0.118 (6) | 0.090 (4) | 0.017 (4) | 0.009 (4) | 0.018 (4) |
O1_62 | 0.164 (6) | 0.078 (3) | 0.102 (4) | −0.014 (3) | −0.053 (4) | 0.005 (3) |
C1_62 | 0.185 (11) | 0.119 (8) | 0.094 (5) | −0.005 (7) | −0.044 (7) | −0.007 (5) |
C2_62 | 0.26 (2) | 0.218 (19) | 0.118 (9) | −0.074 (18) | −0.056 (12) | −0.002 (11) |
C3_62 | 0.223 (15) | 0.120 (9) | 0.129 (8) | −0.058 (10) | −0.043 (10) | −0.015 (6) |
O1_63 | 0.097 (4) | 0.089 (4) | 0.215 (8) | −0.011 (3) | 0.065 (5) | −0.033 (4) |
C1_63 | 0.101 (6) | 0.129 (9) | 0.195 (12) | 0.012 (6) | 0.046 (7) | −0.047 (9) |
C2_63 | 0.102 (5) | 0.106 (7) | 0.180 (11) | −0.006 (5) | 0.054 (7) | −0.007 (7) |
C3_63 | 0.115 (7) | 0.110 (8) | 0.227 (16) | 0.018 (6) | 0.034 (9) | −0.041 (9) |
O1_64 | 0.087 (3) | 0.103 (5) | 0.246 (11) | 0.003 (3) | −0.043 (5) | 0.016 (6) |
C1_64 | 0.082 (5) | 0.225 (18) | 0.242 (19) | 0.044 (8) | −0.013 (8) | 0.055 (15) |
C2_64 | 0.100 (7) | 0.165 (14) | 0.31 (3) | 0.004 (7) | 0.021 (11) | 0.073 (16) |
C3_64 | 0.37 (4) | 0.150 (18) | 0.23 (2) | 0.07 (2) | 0.03 (3) | 0.035 (16) |
O1_65 | 0.159 (9) | 0.221 (15) | 0.30 (2) | −0.006 (9) | 0.032 (12) | −0.040 (14) |
C1_65 | 0.32 (4) | 1.8 (3) | 0.30 (4) | 0.54 (11) | 0.21 (4) | 0.46 (10) |
C2_65 | 0.33 (3) | 0.25 (2) | 0.130 (11) | −0.12 (2) | −0.082 (16) | 0.041 (13) |
C3_65 | 0.32 (3) | 0.24 (3) | 0.179 (19) | −0.05 (3) | −0.01 (2) | −0.014 (18) |
O1_66 | 0.195 (13) | 0.180 (13) | 0.100 (7) | −0.095 (11) | −0.029 (8) | 0.026 (8) |
C1_66 | 0.46 (7) | 0.41 (6) | 0.130 (18) | −0.37 (6) | 0.08 (3) | −0.05 (3) |
C2_66 | 0.091 (8) | 0.149 (17) | 0.163 (17) | −0.011 (9) | 0.018 (10) | −0.021 (13) |
C3_66 | 0.144 (19) | 0.32 (5) | 0.27 (4) | 0.06 (3) | 0.04 (2) | 0.14 (4) |
Geometric parameters (Å, º) top
Na_1—O_22 | 2.263 (3) | CB_25—CG_25 | 1.537 (8) |
Na_1—O_12 | 2.280 (4) | CG_25—CD1_25 | 1.521 (11) |
Na_1—OD1_12 | 2.375 (4) | CG_25—CD2_25 | 1.547 (10) |
Na_1—OD1_22 | 2.375 (4) | C_25—O_25 | 1.241 (6) |
Na_1—O_24 | 2.459 (4) | N_31—C_35 | 1.339 (6) |
Na_1—O_14 | 2.471 (4) | N_31—CA_31 | 1.448 (6) |
Na_1—C_22 | 3.109 (5) | CA_31—C_31 | 1.507 (7) |
Na_2—O_32 | 2.247 (4) | CA_31—CB_31 | 1.544 (6) |
Na_2—O_42 | 2.288 (3) | CB_31—CG_31 | 1.481 (7) |
Na_2—OD1_42 | 2.338 (4) | CG_31—CD1_31 | 1.350 (8) |
Na_2—OD1_32 | 2.387 (5) | CG_31—CD2_31 | 1.452 (8) |
Na_2—O_44 | 2.502 (4) | CD1_31—NE1_31 | 1.340 (8) |
Na_2—O_34 | 2.519 (4) | NE1_31—CE2_31 | 1.406 (9) |
Na_2—C_42 | 3.112 (5) | CE2_31—CZ2_31 | 1.368 (9) |
Na_3—O_11i | 2.277 (4) | CE2_31—CD2_31 | 1.405 (8) |
Na_3—O1_51 | 2.292 (4) | CZ2_31—CH2_31 | 1.349 (12) |
Na_3—O1_54 | 2.330 (4) | CH2_31—CZ3_31 | 1.441 (13) |
Na_3—O1_52 | 2.340 (4) | CZ3_31—CE3_31 | 1.388 (9) |
Na_3—O_15i | 2.384 (4) | CE3_31—CD2_31 | 1.392 (9) |
Na_3—Na_4 | 3.606 (3) | C_31—O_31 | 1.249 (6) |
Na_4—O1_55 | 2.243 (4) | C_31—N_32 | 1.343 (6) |
Na_4—O_33ii | 2.354 (3) | N_32—CA_32 | 1.452 (6) |
Na_4—O_35ii | 2.373 (4) | CA_32—C_32 | 1.514 (6) |
Na_4—O1_53 | 2.376 (4) | CA_32—CB_32 | 1.533 (6) |
Na_4—O1_51 | 2.383 (4) | CB_32—CG_32 | 1.529 (7) |
Na_4—O1_54 | 2.847 (4) | CG_32—OD1_32 | 1.220 (8) |
N_11—C_15 | 1.333 (6) | CG_32—OD2_32 | 1.258 (8) |
N_11—CA_11 | 1.458 (6) | C_32—O_32 | 1.238 (6) |
CA_11—C_11 | 1.534 (7) | C_32—N_33 | 1.343 (6) |
CA_11—CB_11 | 1.553 (6) | N_33—CA_33 | 1.457 (6) |
CB_11—CG_11 | 1.492 (7) | N_33—CD_33 | 1.474 (6) |
CG_11—CD1_11 | 1.353 (8) | CA_33—CB_33 | 1.531 (7) |
CG_11—CD2_11 | 1.428 (8) | CA_33—C_33 | 1.548 (7) |
CD1_11—NE1_11 | 1.387 (8) | CB_33—CG_33 | 1.517 (7) |
NE1_11—CE2_11 | 1.383 (9) | CG_33—CD_33 | 1.515 (6) |
CE2_11—CD2_11 | 1.400 (8) | C_33—O_33 | 1.223 (5) |
CE2_11—CZ2_11 | 1.419 (9) | C_33—N_34 | 1.347 (6) |
CZ2_11—CH2_11 | 1.347 (13) | O_33—Na_4iv | 2.355 (3) |
CH2_11—CZ3_11 | 1.424 (12) | N_34—CA_34 | 1.454 (6) |
CZ3_11—CE3_11 | 1.352 (9) | CA_34—CB_34 | 1.544 (6) |
CE3_11—CD2_11 | 1.416 (9) | CA_34—C_34 | 1.542 (6) |
C_11—O_11 | 1.215 (6) | CB_34—CG1_34 | 1.519 (7) |
C_11—N_12 | 1.338 (6) | CB_34—CG2_34 | 1.538 (8) |
O_11—Na_3iii | 2.277 (4) | C_34—O_34 | 1.240 (5) |
N_12—CA_12 | 1.445 (6) | C_34—N_35 | 1.331 (6) |
CA_12—CB_12 | 1.535 (6) | N_35—CA_35 | 1.452 (6) |
CA_12—C_12 | 1.548 (6) | CA_35—C_35 | 1.525 (6) |
CB_12—CG_12 | 1.536 (6) | CA_35—CB_35 | 1.542 (6) |
CG_12—OD1_12 | 1.240 (6) | CB_35—CG_35 | 1.517 (7) |
CG_12—OD2_12 | 1.261 (6) | CG_35—CD2_35 | 1.524 (8) |
C_12—O_12 | 1.232 (6) | CG_35—CD1_35 | 1.534 (8) |
C_12—N_13 | 1.322 (6) | C_35—O_35 | 1.242 (6) |
N_13—CD_13 | 1.474 (7) | O_35—Na_4iv | 2.373 (4) |
N_13—CA_13 | 1.480 (5) | N_41—C_45 | 1.333 (6) |
CA_13—C_13 | 1.518 (7) | N_41—CA_41 | 1.449 (6) |
CA_13—CB_13 | 1.536 (7) | CA_41—CB_41 | 1.542 (7) |
CB_13—CG_13 | 1.524 (7) | CA_41—C_41 | 1.542 (7) |
CG_13—CD_13 | 1.520 (7) | CB_41—CG_41 | 1.490 (8) |
C_13—O_13 | 1.223 (6) | CG_41—CD1_41 | 1.392 (10) |
C_13—N_14 | 1.357 (6) | CG_41—CD2_41 | 1.448 (9) |
N_14—CA_14 | 1.451 (6) | CD1_41—NE1_41 | 1.376 (9) |
CA_14—CB_14 | 1.538 (6) | NE1_41—CE2_41 | 1.360 (10) |
CA_14—C_14 | 1.551 (6) | CE2_41—CD2_41 | 1.407 (9) |
CB_14—CG1_14 | 1.526 (7) | CE2_41—CZ2_41 | 1.428 (10) |
CB_14—CG2_14 | 1.538 (7) | CZ2_41—CH2_41 | 1.406 (15) |
C_14—O_14 | 1.238 (5) | CH2_41—CZ3_41 | 1.348 (15) |
C_14—N_15 | 1.318 (6) | CZ3_41—CE3_41 | 1.409 (10) |
N_15—CA_15 | 1.470 (6) | CE3_41—CD2_41 | 1.405 (11) |
CA_15—CB_15 | 1.528 (6) | C_41—O_41 | 1.226 (6) |
CA_15—C_15 | 1.531 (6) | C_41—N_42 | 1.345 (6) |
CB_15—CG_15 | 1.530 (7) | N_42—CA_42 | 1.426 (7) |
CG_15—CD2_15 | 1.498 (7) | CA_42—CB_42 | 1.532 (6) |
CG_15—CD1_15 | 1.538 (8) | CA_42—C_42 | 1.550 (6) |
C_15—O_15 | 1.231 (6) | CB_42—CG_42 | 1.535 (6) |
O_15—Na_3iii | 2.384 (4) | CG_42—OD1_42 | 1.228 (6) |
N_21—C_25 | 1.331 (6) | CG_42—OD2_42 | 1.262 (6) |
N_21—CA_21 | 1.448 (6) | C_42—O_42 | 1.226 (6) |
CA_21—C_21 | 1.527 (7) | C_42—N_43 | 1.348 (6) |
CA_21—CB_21 | 1.542 (7) | N_43—CD_43 | 1.468 (6) |
CB_21—CG_21 | 1.510 (9) | N_43—CA_43 | 1.479 (5) |
CG_21—CD1_21 | 1.338 (11) | CA_43—CB_43 | 1.533 (7) |
CG_21—CD2_21 | 1.462 (10) | CA_43—C_43 | 1.549 (6) |
CD1_21—NE1_21 | 1.385 (13) | CB_43—CG_43 | 1.527 (7) |
NE1_21—CE2_21 | 1.324 (15) | CG_43—CD_43 | 1.535 (7) |
CE2_21—CD2_21 | 1.375 (12) | C_43—O_43 | 1.224 (5) |
CE2_21—CZ2_21 | 1.404 (17) | C_43—N_44 | 1.356 (6) |
CZ2_21—CH2_21 | 1.34 (3) | N_44—CA_44 | 1.460 (6) |
CH2_21—CZ3_21 | 1.51 (2) | CA_44—CB_44 | 1.518 (6) |
CZ3_21—CE3_21 | 1.338 (13) | CA_44—C_44 | 1.541 (7) |
CE3_21—CD2_21 | 1.384 (14) | CB_44—CG2_44 | 1.513 (8) |
C_21—O_21 | 1.232 (6) | CB_44—CG1_44 | 1.536 (9) |
C_21—N_22 | 1.349 (6) | C_44—O_44 | 1.244 (6) |
N_22—CA_22 | 1.442 (6) | C_44—N_45 | 1.337 (6) |
CA_22—CB_22 | 1.537 (6) | N_45—CA_45 | 1.460 (7) |
CA_22—C_22 | 1.538 (6) | CA_45—CB_45 | 1.527 (7) |
CB_22—CG_22 | 1.527 (6) | CA_45—C_45 | 1.538 (6) |
CG_22—OD1_22 | 1.246 (6) | CB_45—CG_45 | 1.518 (7) |
CG_22—OD2_22 | 1.265 (6) | CG_45—CD1_45 | 1.515 (9) |
C_22—O_22 | 1.247 (6) | CG_45—CD2_45 | 1.539 (9) |
C_22—N_23 | 1.339 (6) | C_45—O_45 | 1.212 (6) |
N_23—CD_23 | 1.464 (7) | O1_61—C1_61 | 1.433 (8) |
N_23—CA_23 | 1.478 (6) | C1_61—C3_61 | 1.505 (10) |
CA_23—CB_23 | 1.497 (7) | C1_61—C2_61 | 1.523 (9) |
CA_23—C_23 | 1.557 (6) | O1_62—C1_62 | 1.384 (10) |
CB_23—CG_23 | 1.533 (7) | C1_62—C2_62 | 1.460 (14) |
CG_23—CD_23 | 1.532 (7) | C1_62—C3_62 | 1.467 (13) |
C_23—O_23 | 1.211 (5) | O1_63—C1_63 | 1.360 (11) |
C_23—N_24 | 1.348 (6) | C1_63—C2_63 | 1.453 (12) |
N_24—CA_24 | 1.454 (6) | C1_63—C3_63 | 1.478 (12) |
CA_24—C_24 | 1.521 (7) | O1_64—C1_64 | 1.379 (11) |
CA_24—CB_24 | 1.547 (6) | C1_64—C2_64 | 1.459 (15) |
CB_24—CG1_24 | 1.516 (8) | C1_64—C3_64 | 1.514 (16) |
CB_24—CG2_24 | 1.531 (8) | O1_65—C1_65 | 1.475 (17) |
C_24—O_24 | 1.239 (5) | C1_65—C2_65 | 1.55 (2) |
C_24—N_25 | 1.336 (6) | C1_65—C3_65 | 1.560 (18) |
N_25—CA_25 | 1.475 (6) | O1_66—C1_66 | 1.4384 |
CA_25—CB_25 | 1.512 (7) | C1_66—C3_66 | 1.503 (16) |
CA_25—C_25 | 1.523 (6) | C1_66—C2_66 | 1.540 (15) |
| | | |
O_22—Na_1—O_12 | 168.77 (14) | CB_23—CA_23—C_23 | 112.5 (4) |
O_22—Na_1—OD1_12 | 101.17 (13) | CA_23—CB_23—CG_23 | 104.7 (4) |
O_12—Na_1—OD1_12 | 81.82 (13) | CB_23—CG_23—CD_23 | 102.1 (4) |
O_22—Na_1—OD1_22 | 79.79 (12) | N_23—CD_23—CG_23 | 103.5 (4) |
O_12—Na_1—OD1_22 | 111.26 (13) | O_23—C_23—N_24 | 123.1 (5) |
OD1_12—Na_1—OD1_22 | 87.78 (14) | O_23—C_23—CA_23 | 120.5 (4) |
O_22—Na_1—O_24 | 81.70 (12) | N_24—C_23—CA_23 | 116.4 (4) |
O_12—Na_1—O_24 | 87.13 (13) | C_23—N_24—CA_24 | 120.6 (4) |
OD1_12—Na_1—O_24 | 99.93 (13) | N_24—CA_24—C_24 | 106.0 (3) |
OD1_22—Na_1—O_24 | 161.01 (14) | N_24—CA_24—CB_24 | 111.9 (4) |
O_22—Na_1—O_14 | 95.23 (12) | C_24—CA_24—CB_24 | 112.4 (4) |
O_12—Na_1—O_14 | 81.89 (12) | CG1_24—CB_24—CG2_24 | 111.6 (5) |
OD1_12—Na_1—O_14 | 163.58 (13) | CG1_24—CB_24—CA_24 | 110.9 (5) |
OD1_22—Na_1—O_14 | 96.17 (13) | CG2_24—CB_24—CA_24 | 109.1 (4) |
O_24—Na_1—O_14 | 81.34 (12) | O_24—C_24—N_25 | 124.1 (4) |
O_22—Na_1—C_22 | 19.89 (11) | O_24—C_24—CA_24 | 119.8 (4) |
O_12—Na_1—C_22 | 169.42 (14) | N_25—C_24—CA_24 | 116.1 (4) |
OD1_12—Na_1—C_22 | 103.64 (13) | C_24—O_24—Na_1 | 120.9 (3) |
OD1_22—Na_1—C_22 | 60.51 (11) | C_24—N_25—CA_25 | 122.2 (4) |
O_24—Na_1—C_22 | 100.65 (12) | N_25—CA_25—CB_25 | 112.0 (4) |
O_14—Na_1—C_22 | 92.12 (13) | N_25—CA_25—C_25 | 108.4 (4) |
O_32—Na_2—O_42 | 175.50 (15) | CB_25—CA_25—C_25 | 109.1 (4) |
O_32—Na_2—OD1_42 | 101.21 (14) | CA_25—CB_25—CG_25 | 114.7 (4) |
O_42—Na_2—OD1_42 | 80.30 (13) | CD1_25—CG_25—CB_25 | 113.0 (6) |
O_32—Na_2—OD1_32 | 79.35 (14) | CD1_25—CG_25—CD2_25 | 108.3 (7) |
O_42—Na_2—OD1_32 | 105.11 (14) | CB_25—CG_25—CD2_25 | 108.0 (5) |
OD1_42—Na_2—OD1_32 | 81.42 (16) | O_25—C_25—N_21 | 121.9 (4) |
O_32—Na_2—O_44 | 91.93 (13) | O_25—C_25—CA_25 | 122.7 (4) |
O_42—Na_2—O_44 | 86.60 (12) | N_21—C_25—CA_25 | 115.4 (4) |
OD1_42—Na_2—O_44 | 166.86 (14) | C_35—N_31—CA_31 | 121.6 (4) |
OD1_32—Na_2—O_44 | 101.11 (15) | N_31—CA_31—C_31 | 111.3 (4) |
O_32—Na_2—O_34 | 82.65 (12) | N_31—CA_31—CB_31 | 109.2 (4) |
O_42—Na_2—O_34 | 92.90 (13) | C_31—CA_31—CB_31 | 110.8 (4) |
OD1_42—Na_2—O_34 | 101.91 (15) | CG_31—CB_31—CA_31 | 112.5 (4) |
OD1_32—Na_2—O_34 | 161.99 (14) | CD1_31—CG_31—CD2_31 | 105.4 (5) |
O_44—Na_2—O_34 | 79.73 (12) | CD1_31—CG_31—CB_31 | 129.3 (5) |
O_32—Na_2—C_42 | 159.55 (14) | CD2_31—CG_31—CB_31 | 125.3 (5) |
O_42—Na_2—C_42 | 19.59 (11) | NE1_31—CD1_31—CG_31 | 112.4 (5) |
OD1_42—Na_2—C_42 | 62.74 (13) | CD1_31—NE1_31—CE2_31 | 108.4 (5) |
OD1_32—Na_2—C_42 | 108.67 (14) | CZ2_31—CE2_31—CD2_31 | 123.7 (6) |
O_44—Na_2—C_42 | 104.48 (12) | CZ2_31—CE2_31—NE1_31 | 129.7 (6) |
O_34—Na_2—C_42 | 88.27 (12) | CD2_31—CE2_31—NE1_31 | 106.5 (5) |
O_11i—Na_3—O1_51 | 109.36 (14) | CH2_31—CZ2_31—CE2_31 | 117.7 (7) |
O_11i—Na_3—O1_54 | 88.67 (15) | CZ2_31—CH2_31—CZ3_31 | 121.6 (6) |
O1_51—Na_3—O1_54 | 88.67 (15) | CE3_31—CZ3_31—CH2_31 | 119.1 (7) |
O_11i—Na_3—O1_52 | 147.22 (15) | CZ3_31—CE3_31—CD2_31 | 119.6 (7) |
O1_51—Na_3—O1_52 | 102.21 (14) | CE3_31—CD2_31—CE2_31 | 118.2 (5) |
O1_54—Na_3—O1_52 | 100.89 (14) | CE3_31—CD2_31—CG_31 | 134.5 (6) |
O_11i—Na_3—O_15i | 87.47 (13) | CE2_31—CD2_31—CG_31 | 107.2 (5) |
O1_51—Na_3—O_15i | 91.30 (13) | O_31—C_31—N_32 | 121.7 (4) |
O1_54—Na_3—O_15i | 175.89 (14) | O_31—C_31—CA_31 | 120.6 (4) |
O1_52—Na_3—O_15i | 83.13 (13) | N_32—C_31—CA_31 | 117.6 (4) |
O_11i—Na_3—Na_4 | 118.29 (12) | C_31—N_32—CA_32 | 121.4 (4) |
O1_51—Na_3—Na_4 | 40.46 (10) | N_32—CA_32—C_32 | 107.7 (4) |
O1_54—Na_3—Na_4 | 52.09 (11) | N_32—CA_32—CB_32 | 112.4 (4) |
O1_52—Na_3—Na_4 | 91.51 (11) | C_32—CA_32—CB_32 | 113.1 (4) |
O_15i—Na_3—Na_4 | 129.11 (10) | CG_32—CB_32—CA_32 | 116.4 (4) |
O1_55—Na_4—O_33ii | 119.56 (19) | OD1_32—CG_32—OD2_32 | 124.9 (6) |
O1_55—Na_4—O_35ii | 85.48 (15) | OD1_32—CG_32—CB_32 | 120.2 (5) |
O_33ii—Na_4—O_35ii | 103.46 (13) | OD2_32—CG_32—CB_32 | 114.9 (6) |
O1_55—Na_4—O1_53 | 154.23 (19) | CG_32—OD1_32—Na_2 | 159.4 (4) |
O_33ii—Na_4—O1_53 | 85.55 (13) | O_32—C_32—N_33 | 119.6 (4) |
O_35ii—Na_4—O1_53 | 82.75 (14) | O_32—C_32—CA_32 | 121.2 (4) |
O1_55—Na_4—O1_51 | 81.50 (16) | N_33—C_32—CA_32 | 119.2 (4) |
O_33ii—Na_4—O1_51 | 83.47 (13) | C_32—O_32—Na_2 | 126.0 (3) |
O_35ii—Na_4—O1_51 | 166.98 (14) | C_32—N_33—CA_33 | 119.6 (4) |
O1_53—Na_4—O1_51 | 109.03 (14) | C_32—N_33—CD_33 | 128.2 (4) |
O1_55—Na_4—O1_54 | 80.72 (16) | CA_33—N_33—CD_33 | 111.8 (4) |
O_33ii—Na_4—O1_54 | 148.51 (13) | N_33—CA_33—CB_33 | 104.2 (4) |
O_35ii—Na_4—O1_54 | 101.87 (12) | N_33—CA_33—C_33 | 110.6 (3) |
O1_53—Na_4—O1_54 | 79.39 (12) | CB_33—CA_33—C_33 | 113.2 (4) |
O1_51—Na_4—O1_54 | 75.70 (12) | CG_33—CB_33—CA_33 | 104.6 (4) |
O1_55—Na_4—Na_3 | 66.79 (12) | CD_33—CG_33—CB_33 | 103.8 (4) |
O_33ii—Na_4—Na_3 | 121.97 (11) | N_33—CD_33—CG_33 | 101.8 (4) |
O_35ii—Na_4—Na_3 | 133.94 (10) | O_33—C_33—N_34 | 124.6 (4) |
O1_53—Na_4—Na_3 | 106.33 (10) | O_33—C_33—CA_33 | 120.9 (4) |
O1_51—Na_4—Na_3 | 38.62 (9) | N_34—C_33—CA_33 | 114.5 (4) |
O1_54—Na_4—Na_3 | 40.22 (9) | C_33—O_33—Na_4iv | 152.9 (3) |
C_15—N_11—CA_11 | 122.1 (4) | C_33—N_34—CA_34 | 118.4 (4) |
N_11—CA_11—C_11 | 109.1 (3) | N_34—CA_34—CB_34 | 112.6 (4) |
N_11—CA_11—CB_11 | 109.3 (4) | N_34—CA_34—C_34 | 105.4 (4) |
C_11—CA_11—CB_11 | 114.0 (4) | CB_34—CA_34—C_34 | 110.7 (4) |
CG_11—CB_11—CA_11 | 112.6 (4) | CG1_34—CB_34—CG2_34 | 111.9 (5) |
CD1_11—CG_11—CD2_11 | 106.8 (5) | CG1_34—CB_34—CA_34 | 111.2 (4) |
CD1_11—CG_11—CB_11 | 126.9 (5) | CG2_34—CB_34—CA_34 | 109.3 (4) |
CD2_11—CG_11—CB_11 | 126.1 (5) | O_34—C_34—N_35 | 124.2 (4) |
CG_11—CD1_11—NE1_11 | 110.1 (6) | O_34—C_34—CA_34 | 120.3 (4) |
CE2_11—NE1_11—CD1_11 | 108.1 (5) | N_35—C_34—CA_34 | 115.4 (4) |
NE1_11—CE2_11—CD2_11 | 107.4 (5) | C_34—O_34—Na_2 | 118.6 (3) |
NE1_11—CE2_11—CZ2_11 | 130.3 (6) | C_34—N_35—CA_35 | 122.7 (4) |
CD2_11—CE2_11—CZ2_11 | 122.3 (6) | N_35—CA_35—C_35 | 109.5 (4) |
CH2_11—CZ2_11—CE2_11 | 116.9 (6) | N_35—CA_35—CB_35 | 111.1 (4) |
CZ2_11—CH2_11—CZ3_11 | 122.3 (6) | C_35—CA_35—CB_35 | 110.8 (3) |
CE3_11—CZ3_11—CH2_11 | 120.4 (7) | CG_35—CB_35—CA_35 | 113.2 (4) |
CZ3_11—CE3_11—CD2_11 | 119.9 (6) | CB_35—CG_35—CD2_35 | 112.0 (5) |
CE2_11—CD2_11—CE3_11 | 118.1 (5) | CB_35—CG_35—CD1_35 | 110.1 (4) |
CE2_11—CD2_11—CG_11 | 107.6 (5) | CD2_35—CG_35—CD1_35 | 109.4 (5) |
CE3_11—CD2_11—CG_11 | 134.3 (5) | O_35—C_35—N_31 | 123.0 (4) |
O_11—C_11—N_12 | 123.5 (5) | O_35—C_35—CA_35 | 121.8 (4) |
O_11—C_11—CA_11 | 121.1 (4) | N_31—C_35—CA_35 | 115.2 (4) |
N_12—C_11—CA_11 | 115.3 (4) | C_35—O_35—Na_4iv | 150.1 (3) |
C_11—O_11—Na_3iii | 125.3 (3) | C_45—N_41—CA_41 | 121.9 (4) |
C_11—N_12—CA_12 | 121.5 (4) | N_41—CA_41—CB_41 | 108.7 (4) |
N_12—CA_12—CB_12 | 110.1 (4) | N_41—CA_41—C_41 | 110.0 (4) |
N_12—CA_12—C_12 | 109.3 (4) | CB_41—CA_41—C_41 | 111.6 (4) |
CB_12—CA_12—C_12 | 111.7 (3) | CG_41—CB_41—CA_41 | 113.5 (5) |
CA_12—CB_12—CG_12 | 114.7 (4) | CD1_41—CG_41—CD2_41 | 105.6 (6) |
OD1_12—CG_12—OD2_12 | 124.9 (5) | CD1_41—CG_41—CB_41 | 127.2 (6) |
OD1_12—CG_12—CB_12 | 119.6 (4) | CD2_41—CG_41—CB_41 | 127.2 (6) |
OD2_12—CG_12—CB_12 | 115.5 (4) | NE1_41—CD1_41—CG_41 | 109.4 (7) |
CG_12—OD1_12—Na_1 | 144.6 (3) | CE2_41—NE1_41—CD1_41 | 109.7 (6) |
O_12—C_12—N_13 | 121.6 (4) | NE1_41—CE2_41—CD2_41 | 108.2 (6) |
O_12—C_12—CA_12 | 120.0 (4) | NE1_41—CE2_41—CZ2_41 | 130.0 (7) |
N_13—C_12—CA_12 | 118.4 (4) | CD2_41—CE2_41—CZ2_41 | 121.7 (7) |
C_12—O_12—Na_1 | 125.7 (3) | CH2_41—CZ2_41—CE2_41 | 116.4 (7) |
C_12—N_13—CD_13 | 128.2 (4) | CZ3_41—CH2_41—CZ2_41 | 121.6 (8) |
C_12—N_13—CA_13 | 120.5 (4) | CH2_41—CZ3_41—CE3_41 | 123.2 (9) |
CD_13—N_13—CA_13 | 111.2 (4) | CD2_41—CE3_41—CZ3_41 | 117.3 (7) |
N_13—CA_13—C_13 | 110.7 (4) | CE3_41—CD2_41—CE2_41 | 119.7 (6) |
N_13—CA_13—CB_13 | 102.8 (4) | CE3_41—CD2_41—CG_41 | 133.1 (6) |
C_13—CA_13—CB_13 | 111.9 (4) | CE2_41—CD2_41—CG_41 | 107.1 (6) |
CG_13—CB_13—CA_13 | 106.2 (4) | O_41—C_41—N_42 | 123.0 (5) |
CD_13—CG_13—CB_13 | 101.6 (4) | O_41—C_41—CA_41 | 121.0 (4) |
N_13—CD_13—CG_13 | 103.0 (4) | N_42—C_41—CA_41 | 116.0 (4) |
O_13—C_13—N_14 | 123.2 (5) | C_41—N_42—CA_42 | 122.3 (4) |
O_13—C_13—CA_13 | 121.8 (5) | N_42—CA_42—CB_42 | 112.4 (4) |
N_14—C_13—CA_13 | 114.9 (4) | N_42—CA_42—C_42 | 107.4 (4) |
C_13—N_14—CA_14 | 119.8 (4) | CB_42—CA_42—C_42 | 111.5 (4) |
N_14—CA_14—CB_14 | 112.6 (4) | CA_42—CB_42—CG_42 | 115.5 (4) |
N_14—CA_14—C_14 | 105.1 (3) | OD1_42—CG_42—OD2_42 | 124.3 (4) |
CB_14—CA_14—C_14 | 110.5 (4) | OD1_42—CG_42—CB_42 | 118.7 (4) |
CG1_14—CB_14—CA_14 | 110.5 (4) | OD2_42—CG_42—CB_42 | 117.0 (4) |
CG1_14—CB_14—CG2_14 | 110.4 (4) | CG_42—OD1_42—Na_2 | 149.5 (4) |
CA_14—CB_14—CG2_14 | 110.1 (4) | O_42—C_42—N_43 | 121.4 (4) |
O_14—C_14—N_15 | 124.7 (4) | O_42—C_42—CA_42 | 120.8 (4) |
O_14—C_14—CA_14 | 119.0 (4) | N_43—C_42—CA_42 | 117.8 (4) |
N_15—C_14—CA_14 | 116.3 (3) | O_42—C_42—Na_2 | 38.73 (19) |
C_14—O_14—Na_1 | 122.8 (3) | N_43—C_42—Na_2 | 119.1 (3) |
C_14—N_15—CA_15 | 122.2 (3) | CA_42—C_42—Na_2 | 108.4 (3) |
N_15—CA_15—CB_15 | 112.1 (4) | C_42—O_42—Na_2 | 121.7 (3) |
N_15—CA_15—C_15 | 108.6 (4) | C_42—N_43—CD_43 | 129.6 (4) |
CB_15—CA_15—C_15 | 109.9 (3) | C_42—N_43—CA_43 | 119.6 (4) |
CA_15—CB_15—CG_15 | 115.8 (4) | CD_43—N_43—CA_43 | 110.6 (4) |
CD2_15—CG_15—CB_15 | 111.5 (4) | N_43—CA_43—CB_43 | 104.0 (4) |
CD2_15—CG_15—CD1_15 | 109.7 (5) | N_43—CA_43—C_43 | 110.3 (4) |
CB_15—CG_15—CD1_15 | 111.6 (4) | CB_43—CA_43—C_43 | 113.6 (4) |
O_15—C_15—N_11 | 123.7 (4) | CG_43—CB_43—CA_43 | 105.8 (4) |
O_15—C_15—CA_15 | 120.3 (4) | CB_43—CG_43—CD_43 | 102.1 (4) |
N_11—C_15—CA_15 | 116.0 (4) | N_43—CD_43—CG_43 | 102.5 (4) |
C_15—O_15—Na_3iii | 138.1 (3) | O_43—C_43—N_44 | 124.7 (4) |
C_25—N_21—CA_21 | 121.6 (4) | O_43—C_43—CA_43 | 121.3 (4) |
N_21—CA_21—C_21 | 111.7 (4) | N_44—C_43—CA_43 | 113.7 (4) |
N_21—CA_21—CB_21 | 108.5 (4) | C_43—N_44—CA_44 | 120.6 (4) |
C_21—CA_21—CB_21 | 111.6 (4) | N_44—CA_44—CB_44 | 112.8 (4) |
CG_21—CB_21—CA_21 | 112.7 (5) | N_44—CA_44—C_44 | 104.7 (3) |
CD1_21—CG_21—CD2_21 | 104.9 (7) | CB_44—CA_44—C_44 | 111.6 (4) |
CD1_21—CG_21—CB_21 | 128.4 (7) | CG2_44—CB_44—CA_44 | 112.3 (4) |
CD2_21—CG_21—CB_21 | 126.7 (7) | CG2_44—CB_44—CG1_44 | 111.1 (5) |
CG_21—CD1_21—NE1_21 | 111.0 (9) | CA_44—CB_44—CG1_44 | 109.3 (4) |
CE2_21—NE1_21—CD1_21 | 107.7 (8) | O_44—C_44—N_45 | 123.2 (5) |
NE1_21—CE2_21—CD2_21 | 110.2 (8) | O_44—C_44—CA_44 | 119.7 (4) |
NE1_21—CE2_21—CZ2_21 | 127.5 (13) | N_45—C_44—CA_44 | 117.1 (4) |
CD2_21—CE2_21—CZ2_21 | 122.2 (13) | C_44—O_44—Na_2 | 115.1 (3) |
CH2_21—CZ2_21—CE2_21 | 117.8 (14) | C_44—N_45—CA_45 | 121.8 (4) |
CZ2_21—CH2_21—CZ3_21 | 121.3 (12) | N_45—CA_45—CB_45 | 112.9 (4) |
CE3_21—CZ3_21—CH2_21 | 116.4 (15) | N_45—CA_45—C_45 | 106.7 (4) |
CZ3_21—CE3_21—CD2_21 | 122.7 (11) | CB_45—CA_45—C_45 | 110.6 (4) |
CE2_21—CD2_21—CE3_21 | 119.2 (8) | CG_45—CB_45—CA_45 | 113.2 (4) |
CE2_21—CD2_21—CG_21 | 106.1 (8) | CD1_45—CG_45—CB_45 | 111.6 (5) |
CE3_21—CD2_21—CG_21 | 134.6 (8) | CD1_45—CG_45—CD2_45 | 109.2 (6) |
O_21—C_21—N_22 | 122.9 (4) | CB_45—CG_45—CD2_45 | 109.3 (5) |
O_21—C_21—CA_21 | 120.7 (4) | O_45—C_45—N_41 | 123.4 (4) |
N_22—C_21—CA_21 | 116.4 (4) | O_45—C_45—CA_45 | 120.7 (4) |
C_21—N_22—CA_22 | 122.0 (4) | N_41—C_45—CA_45 | 115.8 (4) |
N_22—CA_22—CB_22 | 113.0 (4) | Na_3—O1_51—Na_4 | 100.92 (14) |
N_22—CA_22—C_22 | 107.6 (4) | Na_3—O1_54—Na_4 | 87.69 (13) |
CB_22—CA_22—C_22 | 112.7 (4) | O1_61—C1_61—C3_61 | 113.6 (6) |
CG_22—CB_22—CA_22 | 117.6 (4) | O1_61—C1_61—C2_61 | 106.0 (6) |
OD1_22—CG_22—OD2_22 | 124.1 (4) | C3_61—C1_61—C2_61 | 111.4 (8) |
OD1_22—CG_22—CB_22 | 119.4 (4) | O1_62—C1_62—C2_62 | 121.2 (11) |
OD2_22—CG_22—CB_22 | 116.5 (4) | O1_62—C1_62—C3_62 | 110.4 (9) |
CG_22—OD1_22—Na_1 | 157.4 (3) | C2_62—C1_62—C3_62 | 115.5 (12) |
O_22—C_22—N_23 | 120.2 (4) | O1_63—C1_63—C2_63 | 122.0 (10) |
O_22—C_22—CA_22 | 120.2 (4) | O1_63—C1_63—C3_63 | 112.5 (10) |
N_23—C_22—CA_22 | 119.5 (4) | C2_63—C1_63—C3_63 | 117.2 (9) |
O_22—C_22—Na_1 | 38.16 (19) | O1_64—C1_64—C2_64 | 117.2 (12) |
N_23—C_22—Na_1 | 117.2 (3) | O1_64—C1_64—C3_64 | 114.6 (17) |
CA_22—C_22—Na_1 | 108.6 (3) | C2_64—C1_64—C3_64 | 114.4 (16) |
C_22—O_22—Na_1 | 121.9 (3) | O1_65—C1_65—C2_65 | 101.2 (19) |
C_22—N_23—CD_23 | 128.5 (4) | O1_65—C1_65—C3_65 | 103.1 (14) |
C_22—N_23—CA_23 | 120.3 (4) | C2_65—C1_65—C3_65 | 102.8 (16) |
CD_23—N_23—CA_23 | 111.0 (4) | O1_66—C1_66—C3_66 | 116.2 (16) |
N_23—CA_23—CB_23 | 104.6 (4) | O1_66—C1_66—C2_66 | 110.6 (9) |
N_23—CA_23—C_23 | 109.2 (4) | C3_66—C1_66—C2_66 | 107.7 (15) |
Symmetry codes: (i) −x+1/2, −y+2, z+1/2; (ii) x+1/2, −y+3/2, −z+1; (iii) −x+1/2, −y+2, z−1/2; (iv) x−1/2, −y+3/2, −z+1. |
Experimental details
Crystal data |
Chemical formula | 4(C31H41N6O7Na)·8(H2O)·5.63(C3H7OH) |
Mr | 3013.12 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 100 |
a, b, c (Å) | 25.3930 (4), 34.7193 (3), 25.7201 (4) |
V (Å3) | 22675.5 (5) |
Z | 4 |
Radiation type | Synchrotron, λ = 0.83400 Å |
µ (mm−1) | 0.07 |
Crystal size (mm) | 0.08 × 0.04 × 0.04 |
|
Data collection |
Diffractometer | Rigaku RAXIS-IV diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 83268, 22865, 22861 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.626 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.164, 1.07 |
No. of reflections | 22865 |
No. of parameters | 1904 |
No. of restraints | 36 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
(Δ/σ)max | 0.656 |
Δρmax, Δρmin (e Å−3) | 0.56, −0.26 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0 (10) |