Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0907444901002797/he0271sup1.cif
Contains datablock bq123

Computing details top

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 = 3013.12Dx = 0.883 Mg m3
Orthorhombic, P212121Synchrotron radiation, λ = 0.83400 Å
a = 25.3930 (4) ŵ = 0.07 mm1
b = 34.7193 (3) ÅT = 100 K
c = 25.7201 (4) ÅBlock, colorless
V = 22675.5 (5) Å30.08 × 0.04 × 0.04 mm
Z = 4
Data collection top
Rigaku RAXIS-IV
diffractometer
22861 reflections with I > 2σ(I)
Radiation source: double monochromated beamRint = 0.034
Diamond monochromatorθmax = 31.5°, θmin = 1.5°
Detector resolution: 10 pixels mm-1h = 3131
oscillation scansk = 3738
83268 measured reflectionsl = 031
22865 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH 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 = 1.07Δρmax = 0.56 e Å3
22865 reflectionsΔρmin = 0.26 e Å3
1904 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
36 restraintsExtinction coefficient: 2173 (12)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0 (10)
Crystal data top
4(C31H41N6O7Na)·8(H2O)·5.63(C3H7OH)V = 22675.5 (5) Å3
Mr = 3013.12Z = 4
Orthorhombic, P212121Synchrotron radiation, λ = 0.83400 Å
a = 25.3930 (4) ŵ = 0.07 mm1
b = 34.7193 (3) ÅT = 100 K
c = 25.7201 (4) Å0.08 × 0.04 × 0.04 mm
Data collection top
Rigaku RAXIS-IV
diffractometer
22861 reflections with I > 2σ(I)
83268 measured reflectionsRint = 0.034
22865 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.058H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.164(Δ/σ)max = 0.656
S = 1.07Δρmax = 0.56 e Å3
22865 reflectionsΔρmin = 0.26 e Å3
1904 parametersAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
36 restraintsAbsolute 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
xyzUiso*/UeqOcc. (<1)
Na_10.25282 (7)1.02537 (5)0.28478 (6)0.0540 (4)
Na_20.03723 (7)0.73420 (6)0.51179 (7)0.0564 (4)
Na_30.23093 (7)0.90910 (6)0.55404 (6)0.0562 (4)
Na_40.33052 (7)0.83613 (6)0.53727 (7)0.0567 (4)
N_110.31031 (14)1.00883 (12)0.15170 (14)0.0537 (7)
H0_110.31290.99430.17870.064*
CA_110.35423 (16)1.03395 (14)0.13818 (16)0.0551 (9)
HA_110.35961.03250.10050.066*
CB_110.40502 (18)1.01916 (17)0.16522 (19)0.0617 (10)
HB1_110.40151.02250.20250.074*
HB2_110.40890.99180.15830.074*
CG_110.45326 (19)1.03972 (16)0.1471 (2)0.0625 (10)
CD1_110.4790 (2)1.06837 (18)0.1721 (3)0.0723 (12)
HD1_110.46771.08000.20270.087*
NE1_110.52469 (19)1.07784 (17)0.1455 (2)0.0790 (13)
HE1_110.54691.09540.15420.095*
CE2_110.5284 (2)1.05413 (19)0.1024 (2)0.0717 (13)
CZ2_110.5677 (2)1.0519 (2)0.0633 (3)0.0837 (18)
HZ2_110.59741.06750.06420.100*
CH2_110.5600 (3)1.0261 (3)0.0249 (3)0.094 (2)
HH2_110.58461.02460.00180.113*
CZ3_110.5156 (3)1.0011 (3)0.0239 (3)0.092 (2)
HZ3_110.51210.98330.00280.110*
CE3_110.4784 (2)1.0033 (2)0.0614 (2)0.0747 (13)
HE3_110.44920.98710.06030.090*
CD2_110.48394 (19)1.03021 (17)0.1024 (2)0.0646 (11)
C_110.33986 (15)1.07564 (14)0.15198 (16)0.0529 (9)
O_110.32972 (13)1.09905 (11)0.11833 (12)0.0589 (7)
N_120.33805 (15)1.08353 (12)0.20287 (15)0.0566 (8)
H0_120.35361.06840.22440.068*
CA_120.31049 (17)1.11691 (14)0.22249 (16)0.0554 (9)
HA_120.31331.13760.19680.066*
CB_120.33584 (18)1.13059 (14)0.27341 (17)0.0563 (9)
HB1_120.31721.15330.28540.068*
HB2_120.37191.13810.26630.068*
CG_120.33597 (18)1.10058 (15)0.31728 (17)0.0574 (9)
OD1_120.32357 (14)1.06680 (10)0.30756 (12)0.0591 (7)
OD2_120.35038 (16)1.11279 (11)0.36119 (13)0.0649 (8)
C_120.25158 (16)1.10686 (14)0.22988 (15)0.0521 (8)
O_120.23674 (12)1.07319 (10)0.22611 (12)0.0555 (7)
N_130.21854 (14)1.13497 (12)0.24165 (14)0.0531 (7)
CA_130.16396 (17)1.12618 (14)0.25802 (17)0.0560 (9)
HA_130.16381.11470.29280.067*
CB_130.13799 (19)1.16612 (16)0.2592 (2)0.0623 (10)
HB1_130.10251.16480.24540.075*
HB2_130.13641.17580.29450.075*
CG_130.1722 (2)1.19214 (17)0.2255 (2)0.0662 (11)
HG1_130.16371.18940.18890.079*
HG2_130.16871.21900.23550.079*
CD_130.22702 (19)1.17685 (15)0.2374 (2)0.0620 (10)
HD1_130.25151.18290.20960.074*
HD2_130.24041.18740.26980.074*
C_130.13747 (17)1.09950 (15)0.21924 (17)0.0564 (9)
O_130.13021 (13)1.10901 (11)0.17402 (13)0.0624 (8)
N_140.12035 (14)1.06562 (12)0.23932 (14)0.0540 (7)
H0_140.11781.06280.27240.065*
CA_140.10637 (16)1.03421 (14)0.20473 (16)0.0553 (9)
HA_140.09741.04450.17040.066*
CB_140.06005 (17)1.01011 (15)0.22542 (19)0.0599 (10)
HB_140.06921.00040.26000.072*
CG1_140.0496 (2)0.97580 (18)0.1898 (2)0.0698 (12)
H1A_140.08080.96030.18740.105*
H1B_140.04000.98490.15590.105*
H1C_140.02130.96060.20390.105*
CG2_140.01046 (18)1.03533 (18)0.2301 (2)0.0677 (12)
H2A_140.01771.05680.25250.102*
H2B_140.01781.02030.24450.102*
H2C_140.00051.04450.19630.102*
C_140.15681 (16)1.00919 (14)0.20055 (16)0.0526 (8)
O_140.17640 (12)0.99576 (10)0.24075 (11)0.0548 (6)
N_150.17531 (15)1.00342 (11)0.15333 (13)0.0530 (7)
H0_150.15891.01330.12730.064*
CA_150.22310 (17)0.98062 (14)0.14358 (16)0.0541 (9)
HA_150.23480.96920.17650.065*
CB_150.21357 (19)0.94831 (15)0.10437 (17)0.0577 (9)
HB1_150.24460.93200.10350.069*
HB2_150.20970.95970.07020.069*
CG_150.1655 (2)0.92285 (17)0.11479 (19)0.0656 (11)
HG_150.13410.93920.11350.079*
CD1_150.1680 (3)0.90428 (18)0.1690 (2)0.0746 (13)
H1A_150.17090.92410.19500.112*
H1B_150.19810.88760.17100.112*
H1C_150.13660.88960.17500.112*
CD2_150.1598 (3)0.8922 (2)0.0742 (2)0.0826 (17)
H2A_150.12920.87690.08160.124*
H2B_150.19050.87600.07430.124*
H2C_150.15600.90400.04070.124*
C_150.26626 (17)1.00762 (14)0.12359 (16)0.0532 (8)
O_150.25969 (12)1.02610 (10)0.08327 (12)0.0564 (7)
N_210.33800 (16)1.05075 (13)0.43043 (15)0.0586 (8)
H0_210.34301.07170.41320.070*
CA_210.38266 (18)1.02638 (14)0.44247 (17)0.0569 (9)
HA_210.38631.02500.48040.068*
CB_210.4328 (2)1.04524 (18)0.4201 (2)0.0685 (12)
HB1_210.42871.04810.38280.082*
HB2_210.43671.07080.43490.082*
CG_210.4819 (2)1.0221 (2)0.4310 (3)0.0801 (15)
CD1_210.5093 (3)0.9998 (2)0.3984 (4)0.093 (2)
HD1_210.50060.99570.36370.111*
NE1_210.5524 (2)0.9836 (2)0.4232 (5)0.122 (3)
HE1_210.57470.96800.40950.146*
CE2_210.5530 (3)0.9965 (3)0.4716 (5)0.097 (2)
CZ2_210.5911 (4)0.9893 (4)0.5100 (9)0.160 (8)
HZ2_210.62090.97470.50270.192*
CH2_210.5831 (5)1.0041 (5)0.5573 (8)0.157 (7)
HH2_210.60600.99770.58420.188*
CZ3_210.5377 (4)1.0310 (5)0.5679 (5)0.144 (5)
HZ3_210.53381.04340.59980.172*
CE3_210.5034 (3)1.0361 (3)0.5291 (3)0.103 (3)
HE3_210.47361.05100.53510.124*
CD2_210.5103 (2)1.0200 (2)0.4804 (3)0.090 (2)
C_210.37514 (15)0.98552 (14)0.42179 (16)0.0532 (8)
O_210.38672 (13)0.95742 (10)0.44873 (12)0.0575 (7)
N_220.35596 (15)0.98235 (12)0.37309 (14)0.0548 (8)
H0_220.35551.00240.35340.066*
CA_220.33616 (16)0.94637 (14)0.35296 (16)0.0530 (8)
HA_220.34280.92640.37910.064*
CB_220.36352 (17)0.93389 (15)0.30240 (16)0.0572 (9)
HB1_220.40070.93990.30560.069*
HB2_220.36060.90610.29960.069*
CG_220.34373 (18)0.95138 (15)0.25156 (16)0.0563 (9)
OD1_220.31649 (13)0.98123 (11)0.25281 (12)0.0586 (7)
OD2_220.35627 (17)0.93390 (12)0.21023 (13)0.0704 (9)
C_220.27618 (17)0.95044 (14)0.34681 (15)0.0540 (9)
O_220.25485 (11)0.98262 (10)0.35120 (11)0.0533 (6)
N_230.24722 (14)0.91936 (12)0.33534 (14)0.0538 (7)
CA_230.19071 (17)0.92342 (14)0.32273 (17)0.0564 (9)
HA_230.18650.93550.28860.068*
CB_230.17027 (19)0.88299 (15)0.32143 (19)0.0611 (10)
HB1_230.14290.88030.29530.073*
HB2_230.15600.87570.35500.073*
CG_230.2183 (2)0.85829 (17)0.3077 (2)0.0668 (11)
HG1_230.22490.85830.27050.080*
HG2_230.21400.83200.31960.080*
CD_230.26256 (19)0.87875 (15)0.3373 (2)0.0622 (10)
HD1_230.26460.86970.37300.075*
HD2_230.29630.87470.32050.075*
C_230.16357 (16)0.94830 (15)0.36537 (16)0.0546 (9)
O_230.16536 (13)0.93867 (11)0.41059 (13)0.0605 (7)
N_240.13757 (15)0.97985 (13)0.34877 (15)0.0573 (8)
H0_240.12830.98160.31670.069*
CA_240.12509 (18)1.01094 (15)0.38460 (16)0.0574 (9)
HA_240.12391.00050.42000.069*
CB_240.07137 (19)1.02977 (17)0.37202 (19)0.0650 (11)
HB_240.07301.04050.33680.078*
CG1_240.0274 (2)1.0003 (2)0.3738 (2)0.0753 (14)
H1A_240.03460.98010.34930.113*
H1B_240.00531.01240.36500.113*
H1C_240.02510.98960.40810.113*
CG2_240.0616 (2)1.0629 (2)0.4101 (3)0.0803 (15)
H2A_240.09011.08100.40810.120*
H2B_240.05931.05290.44480.120*
H2C_240.02911.07550.40140.120*
C_240.17050 (17)1.03940 (14)0.38084 (16)0.0541 (9)
O_240.18231 (13)1.05350 (10)0.33818 (12)0.0567 (7)
N_250.19614 (16)1.04679 (13)0.42508 (14)0.0582 (8)
H0_250.18311.03870.45390.070*
CA_250.24614 (18)1.06840 (15)0.42613 (17)0.0571 (9)
HA_250.25471.07690.39080.068*
CB_250.2432 (2)1.10315 (17)0.4615 (2)0.0673 (11)
HB1_250.27821.11400.46490.081*
HB2_250.23211.09470.49570.081*
CG_250.2056 (3)1.1350 (2)0.4429 (3)0.0804 (15)
HG_250.16971.12470.44120.096*
CD1_250.2205 (3)1.1512 (2)0.3900 (3)0.0902 (19)
H1A_250.22051.13090.36470.135*
H1B_250.25501.16250.39190.135*
H1C_250.19551.17050.38000.135*
CD2_250.2074 (4)1.1681 (3)0.4831 (4)0.113 (3)
H2A_250.19691.15860.51650.169*
H2B_250.18391.18830.47240.169*
H2C_250.24261.17810.48520.169*
C_250.28941 (18)1.04158 (14)0.44541 (15)0.0548 (9)
O_250.28050 (12)1.01372 (11)0.47431 (12)0.0577 (7)
N_310.11291 (14)0.74168 (12)0.59414 (15)0.0550 (8)
H0_310.09660.76200.60450.066*
CA_310.12518 (17)0.71170 (15)0.63137 (17)0.0562 (9)
HA_310.16350.70840.63240.067*
CB_310.1063 (2)0.72435 (15)0.68583 (17)0.0603 (10)
HB1_310.06820.72570.68600.072*
HB2_310.11980.74990.69320.072*
CG_310.1238 (2)0.69764 (16)0.72730 (18)0.0640 (11)
CD1_310.1025 (2)0.66382 (19)0.7424 (2)0.0708 (12)
HD1_310.07170.65370.72860.085*
NE1_310.1309 (2)0.64649 (16)0.77961 (18)0.0755 (11)
HE1_310.12340.62490.79420.091*
CE2_310.1749 (2)0.66962 (19)0.7907 (2)0.0702 (12)
CZ2_310.2143 (3)0.6642 (2)0.8262 (2)0.0841 (16)
HZ2_310.21460.64280.84800.101*
CH2_310.2528 (3)0.6910 (3)0.8286 (3)0.097 (2)
HH2_310.28000.68790.85240.116*
CZ3_310.2527 (3)0.7243 (3)0.7951 (3)0.0896 (18)
HZ3_310.28010.74200.79640.108*
CE3_310.2110 (2)0.7295 (2)0.7609 (3)0.0789 (14)
HE3_310.21000.75120.73950.095*
CD2_310.1709 (2)0.70229 (18)0.7587 (2)0.0688 (12)
C_310.10047 (16)0.67389 (15)0.61608 (16)0.0552 (9)
O_310.12471 (12)0.64295 (10)0.62246 (13)0.0576 (7)
N_320.05145 (14)0.67478 (12)0.59649 (14)0.0544 (8)
H0_320.03230.69490.60130.065*
CA_320.03017 (16)0.64252 (15)0.56735 (17)0.0563 (9)
HA_320.05650.62190.56780.068*
CB_320.02063 (18)0.62665 (15)0.59143 (19)0.0598 (10)
HB1_320.01320.61940.62710.072*
HB2_320.03020.60340.57290.072*
CG_320.0682 (2)0.65364 (19)0.5915 (2)0.0679 (12)
OD1_320.06552 (14)0.68507 (13)0.57043 (15)0.0700 (9)
OD2_320.1086 (2)0.64039 (17)0.6135 (4)0.121 (2)
C_320.02332 (15)0.65538 (13)0.51151 (16)0.0508 (8)
O_320.02596 (12)0.68984 (10)0.49935 (12)0.0559 (7)
N_330.01405 (14)0.62883 (11)0.47465 (15)0.0521 (7)
CA_330.00454 (16)0.64109 (14)0.42130 (17)0.0555 (9)
HA_330.03080.65220.41860.067*
CB_330.00716 (18)0.60377 (16)0.38970 (18)0.0608 (10)
HB1_330.02630.60770.35750.073*
HB2_330.02790.59450.38160.073*
CG_330.0359 (2)0.57557 (16)0.4246 (2)0.0635 (10)
HG1_330.07380.57830.42100.076*
HG2_330.02610.54920.41660.076*
CD_330.01817 (18)0.58660 (14)0.47887 (18)0.0570 (9)
HD1_330.04390.57910.50480.068*
HD2_330.01550.57510.48730.068*
C_330.04593 (16)0.67131 (15)0.40432 (18)0.0560 (9)
O_330.09296 (12)0.66562 (11)0.41108 (12)0.0571 (7)
N_340.02565 (14)0.70281 (12)0.38123 (15)0.0560 (8)
H0_340.00620.70290.36990.067*
CA_340.05898 (16)0.73662 (14)0.37585 (18)0.0559 (9)
HA_340.09520.72850.36850.067*
CB_340.03998 (19)0.76405 (15)0.33250 (18)0.0596 (10)
HB_340.00420.77250.34110.071*
CG1_340.0381 (2)0.74367 (18)0.28028 (18)0.0682 (12)
H1A_340.01520.72180.28260.102*
H1B_340.02520.76110.25430.102*
H1C_340.07290.73530.27100.102*
CG2_340.0757 (3)0.79981 (19)0.3311 (2)0.0787 (14)
H2A_340.07620.81170.36470.118*
H2B_340.11080.79220.32170.118*
H2C_340.06250.81770.30580.118*
C_340.05718 (17)0.75682 (14)0.42920 (17)0.0544 (9)
O_340.01548 (11)0.77104 (10)0.44537 (12)0.0552 (6)
N_350.10215 (13)0.75659 (12)0.45580 (14)0.0538 (7)
H0_350.13000.74780.44100.065*
CA_350.10611 (16)0.77066 (14)0.50883 (17)0.0552 (9)
HA_350.07090.77810.52060.066*
CB_350.14225 (16)0.80626 (15)0.5119 (2)0.0595 (10)
HB1_350.17610.79990.49660.071*
HB2_350.14820.81260.54820.071*
CG_350.11975 (19)0.84123 (17)0.4844 (2)0.0677 (12)
HG_350.11170.83410.44840.081*
CD1_350.1604 (2)0.8739 (2)0.4838 (3)0.0840 (17)
H1A_350.14590.89590.46630.126*
H1B_350.16950.88070.51880.126*
H1C_350.19150.86550.46570.126*
CD2_350.0693 (2)0.85548 (18)0.5100 (3)0.0759 (14)
H2A_350.04390.83500.51080.114*
H2B_350.07670.86360.54490.114*
H2C_350.05540.87680.49060.114*
C_350.12632 (15)0.73851 (14)0.54398 (17)0.0529 (8)
O_350.15346 (12)0.71159 (10)0.52687 (12)0.0552 (6)
N_410.17755 (16)0.71034 (13)0.58336 (16)0.0599 (8)
H0_410.15590.69140.58610.072*
CA_410.19235 (19)0.73150 (15)0.62966 (18)0.0590 (10)
HA_410.23090.73230.63190.071*
CB_410.1706 (2)0.71010 (17)0.6776 (2)0.0674 (11)
HB1_410.13250.70940.67550.081*
HB2_410.18330.68370.67710.081*
CG_410.1860 (3)0.72814 (19)0.7280 (2)0.0735 (13)
CD1_410.1556 (3)0.7524 (2)0.7589 (2)0.0804 (15)
HD1_410.12210.76140.75050.096*
NE1_410.1827 (3)0.76102 (17)0.80369 (19)0.0867 (15)
HE1_410.17100.77510.82860.104*
CE2_410.2308 (3)0.7438 (2)0.8026 (2)0.0798 (15)
CZ2_410.2719 (4)0.7438 (2)0.8404 (3)0.096 (2)
HZ2_410.26850.75650.87210.115*
CH2_410.3179 (4)0.7235 (3)0.8272 (4)0.110 (3)
HH2_410.34630.72370.85010.132*
CZ3_410.3219 (3)0.7038 (3)0.7823 (3)0.099 (2)
HZ3_410.35300.69060.77550.118*
CE3_410.2812 (3)0.7022 (2)0.7451 (3)0.0839 (16)
HE3_410.28470.68780.71480.101*
CD2_410.2352 (3)0.7232 (2)0.7557 (2)0.0785 (15)
C_410.17128 (17)0.77309 (14)0.62655 (16)0.0545 (9)
O_410.20101 (13)0.80074 (11)0.63055 (15)0.0630 (8)
N_420.11912 (15)0.77678 (13)0.61905 (15)0.0578 (8)
H0_420.09920.75700.62370.069*
CA_420.09564 (17)0.81229 (15)0.60366 (17)0.0563 (9)
HA_420.11950.83330.61320.068*
CB_420.04247 (17)0.81925 (16)0.63018 (18)0.0590 (10)
HB1_420.03120.84530.62250.071*
HB2_420.04740.81750.66750.071*
CG_420.00185 (17)0.79152 (14)0.61445 (17)0.0548 (9)
OD1_420.00944 (13)0.76251 (12)0.58955 (15)0.0676 (9)
OD2_420.04793 (14)0.80024 (12)0.62854 (16)0.0676 (8)
C_420.09010 (15)0.81154 (14)0.54367 (16)0.0533 (9)
O_420.09885 (12)0.78198 (10)0.51906 (12)0.0548 (6)
N_430.07515 (14)0.84429 (12)0.51976 (14)0.0545 (8)
CA_430.06597 (16)0.84422 (14)0.46296 (16)0.0531 (8)
HA_430.03180.83240.45540.064*
CB_430.06430 (18)0.88705 (15)0.4485 (2)0.0605 (10)
HB1_430.08470.89180.41730.073*
HB2_430.02830.89530.44250.073*
CG_430.0881 (2)0.90848 (16)0.49477 (19)0.0639 (10)
HG1_430.07420.93440.49750.077*
HG2_430.12620.90960.49240.077*
CD_430.07039 (18)0.88345 (15)0.54075 (18)0.0589 (9)
HD1_430.09320.88710.57060.071*
HD2_430.03430.88910.55060.071*
C_430.11015 (16)0.82155 (15)0.43490 (17)0.0552 (9)
O_430.15649 (12)0.83055 (10)0.43968 (12)0.0569 (7)
N_440.09199 (14)0.79406 (12)0.40204 (14)0.0546 (8)
H0_440.05930.79390.39330.066*
CA_440.12739 (17)0.76470 (15)0.38130 (18)0.0575 (9)
HA_440.16320.77520.37940.069*
CB_440.11103 (18)0.75064 (16)0.32779 (19)0.0625 (10)
HB_440.07660.73810.33110.075*
CG1_440.1507 (3)0.7205 (2)0.3086 (2)0.0787 (15)
H1A_440.15350.70010.33380.118*
H1B_440.18450.73230.30400.118*
H1C_440.13900.71000.27610.118*
CG2_440.1055 (2)0.78325 (19)0.28915 (19)0.0701 (12)
H2A_440.08050.80160.30200.105*
H2B_440.09360.77320.25640.105*
H2C_440.13910.79560.28450.105*
C_440.12598 (17)0.73196 (14)0.42174 (17)0.0559 (9)
O_440.08397 (12)0.71466 (11)0.43031 (12)0.0580 (7)
N_450.17086 (15)0.72418 (13)0.44685 (15)0.0581 (8)
H0_450.19940.73530.43700.070*
CA_450.17268 (17)0.69729 (16)0.49046 (19)0.0599 (10)
HA_450.13660.68970.49940.072*
CB_450.20479 (18)0.66114 (17)0.4787 (2)0.0672 (12)
HB1_450.23830.66870.46380.081*
HB2_450.21190.64770.51100.081*
CG_450.1773 (2)0.63382 (19)0.4414 (3)0.0744 (13)
HG_450.16700.64810.41020.089*
CD1_450.1286 (2)0.6162 (2)0.4657 (3)0.0798 (15)
H1A_450.11250.59880.44140.120*
H1B_450.10410.63630.47450.120*
H1C_450.13820.60240.49660.120*
CD2_450.2156 (3)0.6014 (3)0.4259 (4)0.101 (2)
H2A_450.19830.58410.40230.151*
H2B_450.22640.58760.45640.151*
H2C_450.24590.61240.40920.151*
C_450.19660 (17)0.71936 (15)0.53662 (18)0.0578 (9)
O_450.23192 (17)0.74233 (15)0.53000 (15)0.0780 (11)
O1_510.31281 (13)0.89349 (11)0.58505 (12)0.0601 (7)
H1_510.33310.89280.61610.090*
H2_510.31740.88900.54810.090*
O1_520.25057 (14)0.93619 (11)0.47300 (13)0.0610 (7)
H1_520.22060.93710.45000.091*
H2_520.26200.96390.47400.091*
O1_530.30265 (12)0.78214 (11)0.58691 (14)0.0606 (7)
H1_530.28060.76440.55990.091*
H2_530.26900.79150.60710.091*
O1_540.21917 (15)0.84471 (12)0.53127 (14)0.0658 (8)
H1_540.19750.83900.49960.099*
H2_540.21200.83090.56450.099*
O1_550.3258 (2)0.87739 (14)0.47031 (16)0.0854 (13)
H1_550.34310.86990.43730.128*
H2_550.29780.89920.47080.128*
O1_560.34921 (13)0.96514 (11)0.54999 (13)0.0617 (7)
H1_560.36200.96280.51520.093*
H2_560.33510.94090.56180.093*
O1_570.24800 (12)0.78512 (12)0.41698 (14)0.0632 (8)
H1_570.28150.78640.43700.095*
H2_570.21690.80000.42380.095*
O1_580.16080 (14)1.01784 (13)0.52212 (13)0.0687 (9)
H1_580.15251.03690.55220.103*
H2_580.18881.00280.54460.103*
O1_610.36338 (19)0.93024 (14)0.10325 (14)0.0784 (11)
H1_610.36120.93140.14010.118*
C1_610.3978 (3)0.8978 (2)0.0973 (2)0.0841 (16)
H1A_610.37970.87480.11030.101*
C2_610.4065 (5)0.8932 (3)0.0390 (3)0.120 (3)
H2A_610.37320.89000.02200.179*
H2B_610.42810.87100.03280.179*
H2C_610.42370.91570.02570.179*
C3_610.4491 (3)0.9020 (3)0.1259 (3)0.099 (2)
H3A_610.44240.90480.16240.149*
H3B_610.46740.92440.11340.149*
H3C_610.47040.87960.12010.149*
O1_620.3705 (3)1.18808 (17)0.3744 (2)0.115 (2)
H1_620.36551.16220.37050.172*
C1_620.3966 (6)1.1960 (3)0.4204 (4)0.133 (4)
H1A_620.43281.18840.41200.159*
C2_620.3863 (9)1.1737 (6)0.4675 (5)0.199 (9)
H2A_620.38731.14670.45940.298*
H2B_620.35211.18030.48080.298*
H2C_620.41261.17950.49310.298*
C3_620.4018 (8)1.2377 (3)0.4278 (5)0.157 (6)
H3A_620.40721.24990.39470.236*
H3B_620.43131.24290.45000.236*
H3C_620.37031.24760.44340.236*
O1_630.0929 (2)0.8623 (2)0.6696 (4)0.133 (3)
H1_630.07620.83890.65320.200*
C1_630.1463 (4)0.8642 (3)0.6664 (6)0.142 (5)
H1A_630.15010.87040.62940.170*
C2_630.1791 (4)0.8299 (3)0.6688 (6)0.129 (4)
H2A_630.16310.80970.64890.194*
H2B_630.21320.83560.65480.194*
H2C_630.18260.82190.70440.194*
C3_630.1677 (5)0.8999 (4)0.6894 (7)0.151 (5)
H3A_630.14370.92070.68340.226*
H3B_630.17250.89630.72610.226*
H3C_630.20100.90570.67360.226*
O1_640.1291 (3)0.5661 (2)0.6172 (5)0.145 (3)
H1_640.12100.59210.61560.218*
C1_640.1801 (4)0.5576 (5)0.6319 (9)0.183 (8)
H1A_640.17960.56270.66940.220*
C2_640.2215 (5)0.5834 (5)0.6135 (10)0.192 (9)
H2A_640.21070.60960.61830.288*
H2B_640.22790.57870.57720.288*
H2C_640.25320.57870.63280.288*
C3_640.1941 (12)0.5153 (5)0.6296 (11)0.250 (14)
H3A_640.16780.50060.64770.375*
H3B_640.22780.51130.64560.375*
H3C_640.19550.50710.59390.375*
O1_650.0466 (5)0.8023 (5)0.7840 (8)0.227 (7)
H1_650.07280.80440.81120.340*
C1_650.0038 (8)0.8206 (6)0.7983 (9)0.81 (12)
H1A_650.00970.82450.83560.974*
C2_650.0436 (10)0.7940 (7)0.7704 (7)0.238 (14)
H2A_650.04620.77000.78870.357*
H2B_650.03180.78930.73550.357*
H2C_650.07750.80620.76950.357*
C3_650.0046 (5)0.8577 (3)0.7641 (4)0.245 (13)
H3A_650.01900.87650.77860.368*
H3B_650.03960.86800.76330.368*
H3C_650.00640.85140.72940.368*
O1_660.0743 (5)0.6259 (3)0.7244 (4)0.158 (6)0.63
H1_660.08510.63000.69080.237*0.63
C1_660.0725 (5)0.6615 (3)0.7530 (4)0.33 (4)0.63
H1A_660.10850.67170.75420.399*0.63
C2_660.0382 (6)0.6914 (6)0.7245 (8)0.134 (7)0.63
H2A_660.05190.69540.69010.202*0.63
H2B_660.03880.71530.74330.202*0.63
H2C_660.00270.68210.72230.202*0.63
C3_660.0531 (12)0.6589 (11)0.8081 (8)0.25 (2)0.63
H3A_660.07240.63930.82630.370*0.63
H3B_660.01630.65260.80820.370*0.63
H3C_660.05830.68330.82510.370*0.63
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na_10.0557 (8)0.0605 (10)0.0460 (7)0.0006 (7)0.0004 (6)0.0049 (6)
Na_20.0508 (8)0.0629 (10)0.0554 (8)0.0062 (7)0.0024 (7)0.0049 (7)
Na_30.0574 (8)0.0642 (11)0.0468 (7)0.0017 (7)0.0013 (6)0.0040 (7)
Na_40.0558 (8)0.0626 (10)0.0515 (8)0.0035 (7)0.0023 (7)0.0007 (7)
N_110.0541 (17)0.062 (2)0.0455 (15)0.0006 (14)0.0003 (13)0.0024 (13)
CA_110.0512 (19)0.066 (3)0.0480 (18)0.0031 (17)0.0017 (15)0.0035 (16)
CB_110.054 (2)0.075 (3)0.056 (2)0.0027 (19)0.0039 (17)0.0012 (19)
CG_110.056 (2)0.065 (3)0.067 (3)0.0054 (18)0.0049 (19)0.009 (2)
CD1_110.061 (2)0.070 (3)0.086 (3)0.004 (2)0.004 (2)0.001 (2)
NE1_110.061 (2)0.076 (3)0.101 (4)0.0043 (19)0.009 (2)0.012 (2)
CE2_110.057 (2)0.082 (4)0.076 (3)0.003 (2)0.000 (2)0.011 (2)
CZ2_110.059 (3)0.090 (4)0.102 (4)0.005 (2)0.012 (3)0.033 (4)
CH2_110.077 (3)0.123 (6)0.083 (4)0.005 (4)0.023 (3)0.010 (4)
CZ3_110.081 (4)0.126 (6)0.068 (3)0.012 (4)0.004 (3)0.006 (3)
CE3_110.062 (3)0.090 (4)0.071 (3)0.000 (2)0.001 (2)0.008 (3)
CD2_110.055 (2)0.078 (3)0.061 (2)0.004 (2)0.0035 (18)0.014 (2)
C_110.0444 (17)0.068 (3)0.0464 (18)0.0054 (16)0.0031 (14)0.0055 (16)
O_110.0596 (16)0.0655 (19)0.0517 (15)0.0031 (13)0.0036 (12)0.0035 (13)
N_120.0578 (18)0.062 (2)0.0504 (17)0.0005 (15)0.0027 (14)0.0061 (15)
CA_120.0531 (19)0.066 (3)0.0475 (19)0.0019 (17)0.0023 (15)0.0024 (16)
CB_120.057 (2)0.062 (3)0.0497 (19)0.0054 (17)0.0008 (16)0.0008 (17)
CG_120.056 (2)0.064 (3)0.051 (2)0.0056 (17)0.0001 (16)0.0023 (17)
OD1_120.0677 (17)0.0591 (19)0.0504 (14)0.0066 (14)0.0038 (13)0.0017 (12)
OD2_120.077 (2)0.070 (2)0.0482 (15)0.0080 (16)0.0069 (14)0.0042 (13)
C_120.0535 (19)0.058 (2)0.0445 (17)0.0037 (16)0.0017 (15)0.0049 (15)
O_120.0540 (14)0.0651 (19)0.0472 (13)0.0036 (13)0.0000 (11)0.0037 (12)
N_130.0530 (17)0.054 (2)0.0524 (17)0.0024 (13)0.0036 (14)0.0038 (13)
CA_130.055 (2)0.066 (3)0.0477 (19)0.0016 (17)0.0048 (16)0.0038 (16)
CB_130.059 (2)0.065 (3)0.063 (2)0.0059 (19)0.0049 (19)0.0004 (19)
CG_130.062 (2)0.068 (3)0.069 (3)0.005 (2)0.002 (2)0.007 (2)
CD_130.062 (2)0.055 (3)0.069 (3)0.0038 (18)0.005 (2)0.0051 (19)
C_130.0514 (19)0.069 (3)0.0489 (19)0.0059 (17)0.0047 (16)0.0084 (17)
O_130.0629 (16)0.074 (2)0.0498 (15)0.0025 (14)0.0020 (13)0.0097 (14)
N_140.0537 (16)0.061 (2)0.0472 (16)0.0002 (14)0.0008 (13)0.0061 (14)
CA_140.0516 (18)0.065 (3)0.0487 (19)0.0030 (17)0.0023 (15)0.0024 (16)
CB_140.0520 (19)0.068 (3)0.060 (2)0.0015 (18)0.0019 (17)0.0046 (19)
CG1_140.062 (2)0.075 (3)0.072 (3)0.013 (2)0.005 (2)0.006 (2)
CG2_140.051 (2)0.079 (3)0.073 (3)0.000 (2)0.0037 (19)0.010 (2)
C_140.0536 (19)0.059 (2)0.0450 (18)0.0013 (16)0.0044 (15)0.0048 (15)
O_140.0547 (14)0.0664 (19)0.0433 (13)0.0011 (12)0.0032 (11)0.0028 (11)
N_150.0570 (17)0.058 (2)0.0438 (15)0.0018 (14)0.0003 (13)0.0047 (13)
CA_150.0537 (19)0.063 (3)0.0461 (18)0.0024 (17)0.0019 (15)0.0040 (16)
CB_150.063 (2)0.064 (3)0.0469 (18)0.0045 (18)0.0031 (17)0.0007 (16)
CG_150.066 (2)0.075 (3)0.056 (2)0.008 (2)0.0046 (19)0.007 (2)
CD1_150.089 (3)0.070 (3)0.065 (3)0.015 (3)0.011 (3)0.001 (2)
CD2_150.094 (4)0.090 (4)0.064 (3)0.033 (3)0.009 (3)0.014 (3)
C_150.0557 (19)0.059 (2)0.0447 (17)0.0032 (16)0.0015 (15)0.0001 (15)
O_150.0569 (15)0.0625 (19)0.0498 (14)0.0017 (12)0.0007 (12)0.0035 (12)
N_210.0623 (19)0.063 (2)0.0507 (17)0.0025 (16)0.0031 (15)0.0018 (15)
CA_210.061 (2)0.058 (3)0.052 (2)0.0031 (17)0.0046 (17)0.0014 (17)
CB_210.072 (3)0.069 (3)0.065 (3)0.011 (2)0.001 (2)0.003 (2)
CG_210.066 (3)0.082 (4)0.092 (4)0.015 (3)0.002 (3)0.008 (3)
CD1_210.064 (3)0.083 (5)0.131 (6)0.005 (3)0.008 (3)0.011 (4)
NE1_210.065 (3)0.078 (4)0.222 (11)0.010 (2)0.020 (4)0.002 (5)
CE2_210.065 (3)0.081 (5)0.146 (7)0.008 (3)0.005 (4)0.011 (5)
CZ2_210.066 (4)0.137 (10)0.28 (2)0.010 (5)0.026 (7)0.120 (13)
CH2_210.087 (6)0.195 (15)0.188 (13)0.035 (7)0.031 (8)0.101 (13)
CZ3_210.096 (5)0.198 (13)0.136 (8)0.048 (7)0.023 (5)0.060 (9)
CE3_210.083 (4)0.148 (8)0.077 (4)0.036 (4)0.009 (3)0.013 (4)
CD2_210.063 (3)0.092 (5)0.116 (5)0.013 (3)0.013 (3)0.031 (4)
C_210.0458 (17)0.066 (3)0.0482 (19)0.0022 (16)0.0003 (14)0.0006 (16)
O_210.0611 (16)0.0631 (19)0.0483 (14)0.0009 (13)0.0028 (12)0.0035 (12)
N_220.0558 (17)0.065 (2)0.0436 (16)0.0015 (15)0.0011 (13)0.0038 (14)
CA_220.0505 (19)0.060 (2)0.0483 (19)0.0011 (16)0.0006 (15)0.0049 (16)
CB_220.0546 (19)0.071 (3)0.0460 (19)0.0020 (18)0.0005 (16)0.0009 (17)
CG_220.058 (2)0.064 (3)0.0466 (19)0.0028 (18)0.0027 (16)0.0037 (16)
OD1_220.0590 (15)0.067 (2)0.0494 (14)0.0074 (13)0.0001 (12)0.0052 (12)
OD2_220.090 (2)0.070 (2)0.0510 (16)0.0110 (18)0.0030 (16)0.0031 (14)
C_220.053 (2)0.067 (3)0.0421 (17)0.0037 (17)0.0017 (15)0.0056 (16)
O_220.0506 (13)0.0631 (18)0.0463 (13)0.0021 (12)0.0012 (11)0.0032 (11)
N_230.0530 (17)0.058 (2)0.0509 (17)0.0024 (14)0.0023 (14)0.0029 (14)
CA_230.055 (2)0.065 (3)0.0485 (19)0.0010 (17)0.0013 (16)0.0026 (16)
CB_230.062 (2)0.064 (3)0.057 (2)0.0021 (19)0.0028 (18)0.0011 (18)
CG_230.066 (2)0.070 (3)0.064 (2)0.000 (2)0.006 (2)0.002 (2)
CD_230.061 (2)0.056 (3)0.070 (3)0.0014 (18)0.010 (2)0.0040 (19)
C_230.0469 (18)0.071 (3)0.0461 (19)0.0066 (16)0.0020 (15)0.0072 (17)
O_230.0577 (15)0.072 (2)0.0514 (15)0.0058 (14)0.0030 (12)0.0100 (13)
N_240.0558 (17)0.064 (2)0.0525 (17)0.0000 (15)0.0003 (14)0.0008 (15)
CA_240.057 (2)0.070 (3)0.0448 (18)0.0035 (18)0.0029 (16)0.0028 (17)
CB_240.060 (2)0.080 (3)0.055 (2)0.006 (2)0.0007 (18)0.002 (2)
CG1_240.058 (2)0.101 (4)0.066 (3)0.001 (2)0.003 (2)0.003 (3)
CG2_240.062 (3)0.098 (4)0.081 (3)0.016 (3)0.005 (2)0.014 (3)
C_240.057 (2)0.062 (2)0.0435 (18)0.0054 (17)0.0024 (15)0.0037 (15)
O_240.0559 (15)0.0670 (19)0.0472 (14)0.0009 (13)0.0018 (12)0.0011 (12)
N_250.0590 (18)0.073 (2)0.0431 (16)0.0029 (16)0.0014 (14)0.0044 (15)
CA_250.060 (2)0.066 (3)0.0453 (18)0.0004 (18)0.0027 (16)0.0000 (17)
CB_250.076 (3)0.067 (3)0.059 (2)0.005 (2)0.009 (2)0.004 (2)
CG_250.083 (3)0.072 (4)0.086 (4)0.010 (3)0.018 (3)0.007 (3)
CD1_250.093 (4)0.072 (4)0.106 (5)0.005 (3)0.029 (4)0.016 (3)
CD2_250.136 (7)0.080 (5)0.123 (6)0.032 (5)0.031 (6)0.032 (4)
C_250.064 (2)0.059 (3)0.0416 (17)0.0005 (17)0.0012 (16)0.0028 (15)
O_250.0587 (15)0.068 (2)0.0465 (13)0.0023 (13)0.0009 (12)0.0056 (12)
N_310.0519 (16)0.061 (2)0.0526 (18)0.0030 (14)0.0006 (14)0.0065 (15)
CA_310.0503 (18)0.064 (3)0.054 (2)0.0009 (16)0.0003 (16)0.0038 (17)
CB_310.066 (2)0.064 (3)0.051 (2)0.0027 (19)0.0021 (18)0.0078 (18)
CG_310.072 (3)0.068 (3)0.052 (2)0.006 (2)0.0005 (19)0.0037 (18)
CD1_310.078 (3)0.078 (4)0.056 (2)0.010 (2)0.001 (2)0.003 (2)
NE1_310.092 (3)0.074 (3)0.061 (2)0.002 (2)0.004 (2)0.0023 (19)
CE2_310.079 (3)0.076 (3)0.055 (2)0.010 (2)0.000 (2)0.003 (2)
CZ2_310.101 (4)0.086 (4)0.066 (3)0.016 (3)0.009 (3)0.005 (3)
CH2_310.094 (4)0.102 (5)0.096 (5)0.017 (4)0.032 (4)0.007 (4)
CZ3_310.079 (3)0.101 (5)0.090 (4)0.001 (3)0.015 (3)0.008 (3)
CE3_310.076 (3)0.085 (4)0.076 (3)0.003 (3)0.014 (3)0.001 (3)
CD2_310.073 (3)0.078 (3)0.055 (2)0.007 (2)0.000 (2)0.002 (2)
C_310.0505 (18)0.071 (3)0.0443 (17)0.0037 (17)0.0005 (15)0.0030 (16)
O_310.0545 (15)0.0633 (19)0.0550 (15)0.0111 (12)0.0061 (12)0.0006 (12)
N_320.0474 (15)0.066 (2)0.0500 (17)0.0035 (14)0.0016 (13)0.0040 (15)
CA_320.0447 (17)0.072 (3)0.052 (2)0.0059 (16)0.0026 (15)0.0056 (18)
CB_320.056 (2)0.062 (3)0.061 (2)0.0031 (17)0.0054 (18)0.0034 (18)
CG_320.056 (2)0.084 (4)0.064 (3)0.001 (2)0.0050 (19)0.012 (2)
OD1_320.0580 (16)0.084 (3)0.0678 (19)0.0122 (16)0.0019 (15)0.0072 (17)
OD2_320.071 (2)0.081 (3)0.211 (8)0.003 (2)0.057 (4)0.007 (4)
C_320.0449 (17)0.053 (2)0.054 (2)0.0025 (14)0.0023 (14)0.0009 (16)
O_320.0524 (14)0.0575 (19)0.0578 (15)0.0031 (12)0.0015 (12)0.0004 (12)
N_330.0512 (16)0.0490 (19)0.0560 (18)0.0035 (13)0.0022 (14)0.0046 (13)
CA_330.0457 (17)0.068 (3)0.053 (2)0.0033 (16)0.0002 (15)0.0057 (18)
CB_330.056 (2)0.071 (3)0.055 (2)0.0058 (18)0.0028 (17)0.0080 (19)
CG_330.065 (2)0.064 (3)0.062 (2)0.0052 (19)0.002 (2)0.011 (2)
CD_330.058 (2)0.054 (2)0.059 (2)0.0036 (16)0.0010 (17)0.0027 (17)
C_330.0498 (19)0.064 (3)0.054 (2)0.0053 (17)0.0011 (16)0.0023 (17)
O_330.0483 (13)0.0685 (19)0.0546 (15)0.0041 (12)0.0001 (11)0.0034 (13)
N_340.0513 (16)0.066 (2)0.0503 (17)0.0029 (14)0.0001 (14)0.0027 (15)
CA_340.0473 (18)0.064 (3)0.056 (2)0.0051 (16)0.0022 (16)0.0011 (18)
CB_340.062 (2)0.063 (3)0.054 (2)0.0094 (18)0.0019 (17)0.0017 (18)
CG1_340.071 (3)0.084 (3)0.049 (2)0.012 (2)0.0040 (19)0.002 (2)
CG2_340.094 (4)0.073 (4)0.069 (3)0.007 (3)0.008 (3)0.011 (2)
C_340.0513 (19)0.059 (2)0.053 (2)0.0037 (16)0.0011 (16)0.0059 (16)
O_340.0480 (13)0.0628 (18)0.0549 (15)0.0075 (12)0.0014 (11)0.0010 (12)
N_350.0452 (15)0.061 (2)0.0548 (18)0.0032 (13)0.0002 (13)0.0002 (14)
CA_350.0452 (17)0.062 (3)0.058 (2)0.0006 (16)0.0037 (16)0.0017 (17)
CB_350.0475 (18)0.067 (3)0.064 (2)0.0028 (17)0.0059 (17)0.0060 (19)
CG_350.059 (2)0.064 (3)0.080 (3)0.0017 (19)0.012 (2)0.007 (2)
CD1_350.068 (3)0.072 (4)0.112 (5)0.006 (2)0.008 (3)0.020 (3)
CD2_350.056 (2)0.068 (3)0.103 (4)0.002 (2)0.007 (3)0.003 (3)
C_350.0427 (16)0.062 (2)0.054 (2)0.0013 (15)0.0017 (15)0.0011 (17)
O_350.0522 (14)0.0587 (18)0.0547 (15)0.0037 (12)0.0014 (12)0.0032 (12)
N_410.0613 (19)0.060 (2)0.058 (2)0.0099 (15)0.0029 (16)0.0056 (15)
CA_410.058 (2)0.063 (3)0.056 (2)0.0050 (18)0.0017 (18)0.0019 (18)
CB_410.077 (3)0.063 (3)0.062 (2)0.008 (2)0.005 (2)0.004 (2)
CG_410.088 (3)0.071 (3)0.061 (3)0.012 (3)0.006 (2)0.008 (2)
CD1_410.098 (4)0.077 (4)0.066 (3)0.011 (3)0.011 (3)0.003 (2)
NE1_410.128 (5)0.076 (3)0.056 (2)0.016 (3)0.006 (3)0.002 (2)
CE2_410.104 (4)0.077 (4)0.059 (3)0.003 (3)0.003 (3)0.002 (2)
CZ2_410.132 (6)0.084 (5)0.072 (3)0.025 (4)0.020 (4)0.005 (3)
CH2_410.114 (6)0.111 (6)0.105 (6)0.008 (5)0.039 (5)0.011 (5)
CZ3_410.095 (4)0.103 (5)0.098 (5)0.010 (4)0.021 (4)0.022 (4)
CE3_410.092 (4)0.083 (4)0.076 (3)0.001 (3)0.004 (3)0.015 (3)
CD2_410.095 (4)0.080 (4)0.060 (3)0.019 (3)0.004 (3)0.009 (2)
C_410.053 (2)0.065 (3)0.0452 (18)0.0112 (17)0.0023 (15)0.0003 (16)
O_410.0541 (15)0.069 (2)0.0664 (18)0.0059 (13)0.0006 (14)0.0055 (15)
N_420.0537 (18)0.065 (2)0.0547 (18)0.0118 (15)0.0045 (15)0.0026 (15)
CA_420.0483 (19)0.068 (3)0.052 (2)0.0111 (17)0.0010 (16)0.0010 (17)
CB_420.056 (2)0.069 (3)0.052 (2)0.0058 (18)0.0023 (17)0.0047 (18)
CG_420.0525 (19)0.064 (3)0.0482 (19)0.0006 (17)0.0036 (15)0.0016 (16)
OD1_420.0546 (15)0.079 (2)0.0690 (19)0.0080 (15)0.0064 (14)0.0199 (17)
OD2_420.0552 (16)0.072 (2)0.076 (2)0.0061 (14)0.0085 (15)0.0086 (17)
C_420.0442 (17)0.065 (3)0.051 (2)0.0073 (15)0.0011 (14)0.0040 (16)
O_420.0502 (13)0.0605 (18)0.0536 (15)0.0048 (12)0.0010 (11)0.0011 (12)
N_430.0504 (16)0.062 (2)0.0507 (17)0.0009 (14)0.0024 (13)0.0025 (14)
CA_430.0477 (17)0.060 (2)0.052 (2)0.0033 (15)0.0037 (15)0.0024 (16)
CB_430.055 (2)0.064 (3)0.062 (2)0.0028 (17)0.0041 (18)0.0045 (19)
CG_430.066 (2)0.066 (3)0.060 (2)0.007 (2)0.004 (2)0.0002 (19)
CD_430.056 (2)0.063 (3)0.058 (2)0.0033 (17)0.0013 (17)0.0063 (18)
C_430.0490 (18)0.066 (3)0.0508 (19)0.0053 (16)0.0026 (15)0.0024 (17)
O_430.0498 (14)0.0651 (19)0.0558 (15)0.0067 (12)0.0022 (12)0.0038 (13)
N_440.0487 (16)0.063 (2)0.0517 (17)0.0075 (14)0.0015 (13)0.0028 (15)
CA_440.0505 (18)0.068 (3)0.054 (2)0.0056 (17)0.0048 (16)0.0030 (18)
CB_440.056 (2)0.073 (3)0.059 (2)0.0117 (19)0.0038 (18)0.003 (2)
CG1_440.087 (3)0.087 (4)0.062 (3)0.003 (3)0.001 (3)0.015 (2)
CG2_440.075 (3)0.085 (4)0.051 (2)0.015 (2)0.003 (2)0.008 (2)
C_440.0505 (19)0.063 (3)0.055 (2)0.0010 (16)0.0028 (16)0.0129 (17)
O_440.0484 (13)0.071 (2)0.0545 (15)0.0049 (12)0.0033 (12)0.0047 (13)
N_450.0495 (16)0.069 (2)0.0558 (18)0.0088 (15)0.0021 (14)0.0121 (16)
CA_450.0496 (18)0.070 (3)0.060 (2)0.0033 (17)0.0018 (17)0.0093 (19)
CB_450.049 (2)0.075 (3)0.078 (3)0.0027 (19)0.002 (2)0.009 (2)
CG_450.064 (2)0.079 (4)0.080 (3)0.001 (2)0.007 (2)0.019 (3)
CD1_450.063 (3)0.076 (4)0.100 (4)0.005 (2)0.014 (3)0.020 (3)
CD2_450.097 (4)0.097 (5)0.110 (5)0.006 (4)0.007 (4)0.038 (4)
C_450.0510 (19)0.065 (3)0.057 (2)0.0007 (17)0.0040 (17)0.0004 (18)
O_450.077 (2)0.101 (3)0.0564 (17)0.036 (2)0.0008 (16)0.0009 (18)
O1_510.0617 (16)0.067 (2)0.0519 (15)0.0056 (13)0.0033 (13)0.0035 (13)
O1_520.0654 (16)0.067 (2)0.0503 (15)0.0026 (14)0.0026 (13)0.0001 (13)
O1_530.0448 (13)0.074 (2)0.0626 (17)0.0026 (12)0.0024 (12)0.0011 (14)
O1_540.0709 (18)0.071 (2)0.0550 (16)0.0111 (15)0.0016 (14)0.0024 (14)
O1_550.114 (3)0.086 (3)0.0567 (18)0.034 (2)0.022 (2)0.0144 (17)
O1_560.0588 (16)0.072 (2)0.0544 (15)0.0094 (14)0.0035 (13)0.0024 (14)
O1_570.0509 (14)0.077 (2)0.0620 (17)0.0049 (13)0.0010 (13)0.0080 (15)
O1_580.0653 (17)0.089 (3)0.0516 (16)0.0115 (17)0.0007 (14)0.0062 (15)
O1_610.093 (3)0.090 (3)0.0517 (17)0.021 (2)0.0005 (17)0.0029 (16)
C1_610.100 (4)0.088 (4)0.065 (3)0.011 (3)0.003 (3)0.010 (3)
C2_610.165 (9)0.121 (7)0.073 (4)0.035 (7)0.011 (5)0.018 (4)
C3_610.090 (4)0.118 (6)0.090 (4)0.017 (4)0.009 (4)0.018 (4)
O1_620.164 (6)0.078 (3)0.102 (4)0.014 (3)0.053 (4)0.005 (3)
C1_620.185 (11)0.119 (8)0.094 (5)0.005 (7)0.044 (7)0.007 (5)
C2_620.26 (2)0.218 (19)0.118 (9)0.074 (18)0.056 (12)0.002 (11)
C3_620.223 (15)0.120 (9)0.129 (8)0.058 (10)0.043 (10)0.015 (6)
O1_630.097 (4)0.089 (4)0.215 (8)0.011 (3)0.065 (5)0.033 (4)
C1_630.101 (6)0.129 (9)0.195 (12)0.012 (6)0.046 (7)0.047 (9)
C2_630.102 (5)0.106 (7)0.180 (11)0.006 (5)0.054 (7)0.007 (7)
C3_630.115 (7)0.110 (8)0.227 (16)0.018 (6)0.034 (9)0.041 (9)
O1_640.087 (3)0.103 (5)0.246 (11)0.003 (3)0.043 (5)0.016 (6)
C1_640.082 (5)0.225 (18)0.242 (19)0.044 (8)0.013 (8)0.055 (15)
C2_640.100 (7)0.165 (14)0.31 (3)0.004 (7)0.021 (11)0.073 (16)
C3_640.37 (4)0.150 (18)0.23 (2)0.07 (2)0.03 (3)0.035 (16)
O1_650.159 (9)0.221 (15)0.30 (2)0.006 (9)0.032 (12)0.040 (14)
C1_650.32 (4)1.8 (3)0.30 (4)0.54 (11)0.21 (4)0.46 (10)
C2_650.33 (3)0.25 (2)0.130 (11)0.12 (2)0.082 (16)0.041 (13)
C3_650.32 (3)0.24 (3)0.179 (19)0.05 (3)0.01 (2)0.014 (18)
O1_660.195 (13)0.180 (13)0.100 (7)0.095 (11)0.029 (8)0.026 (8)
C1_660.46 (7)0.41 (6)0.130 (18)0.37 (6)0.08 (3)0.05 (3)
C2_660.091 (8)0.149 (17)0.163 (17)0.011 (9)0.018 (10)0.021 (13)
C3_660.144 (19)0.32 (5)0.27 (4)0.06 (3)0.04 (2)0.14 (4)
Geometric parameters (Å, º) top
Na_1—O_222.263 (3)CB_25—CG_251.537 (8)
Na_1—O_122.280 (4)CG_25—CD1_251.521 (11)
Na_1—OD1_122.375 (4)CG_25—CD2_251.547 (10)
Na_1—OD1_222.375 (4)C_25—O_251.241 (6)
Na_1—O_242.459 (4)N_31—C_351.339 (6)
Na_1—O_142.471 (4)N_31—CA_311.448 (6)
Na_1—C_223.109 (5)CA_31—C_311.507 (7)
Na_2—O_322.247 (4)CA_31—CB_311.544 (6)
Na_2—O_422.288 (3)CB_31—CG_311.481 (7)
Na_2—OD1_422.338 (4)CG_31—CD1_311.350 (8)
Na_2—OD1_322.387 (5)CG_31—CD2_311.452 (8)
Na_2—O_442.502 (4)CD1_31—NE1_311.340 (8)
Na_2—O_342.519 (4)NE1_31—CE2_311.406 (9)
Na_2—C_423.112 (5)CE2_31—CZ2_311.368 (9)
Na_3—O_11i2.277 (4)CE2_31—CD2_311.405 (8)
Na_3—O1_512.292 (4)CZ2_31—CH2_311.349 (12)
Na_3—O1_542.330 (4)CH2_31—CZ3_311.441 (13)
Na_3—O1_522.340 (4)CZ3_31—CE3_311.388 (9)
Na_3—O_15i2.384 (4)CE3_31—CD2_311.392 (9)
Na_3—Na_43.606 (3)C_31—O_311.249 (6)
Na_4—O1_552.243 (4)C_31—N_321.343 (6)
Na_4—O_33ii2.354 (3)N_32—CA_321.452 (6)
Na_4—O_35ii2.373 (4)CA_32—C_321.514 (6)
Na_4—O1_532.376 (4)CA_32—CB_321.533 (6)
Na_4—O1_512.383 (4)CB_32—CG_321.529 (7)
Na_4—O1_542.847 (4)CG_32—OD1_321.220 (8)
N_11—C_151.333 (6)CG_32—OD2_321.258 (8)
N_11—CA_111.458 (6)C_32—O_321.238 (6)
CA_11—C_111.534 (7)C_32—N_331.343 (6)
CA_11—CB_111.553 (6)N_33—CA_331.457 (6)
CB_11—CG_111.492 (7)N_33—CD_331.474 (6)
CG_11—CD1_111.353 (8)CA_33—CB_331.531 (7)
CG_11—CD2_111.428 (8)CA_33—C_331.548 (7)
CD1_11—NE1_111.387 (8)CB_33—CG_331.517 (7)
NE1_11—CE2_111.383 (9)CG_33—CD_331.515 (6)
CE2_11—CD2_111.400 (8)C_33—O_331.223 (5)
CE2_11—CZ2_111.419 (9)C_33—N_341.347 (6)
CZ2_11—CH2_111.347 (13)O_33—Na_4iv2.355 (3)
CH2_11—CZ3_111.424 (12)N_34—CA_341.454 (6)
CZ3_11—CE3_111.352 (9)CA_34—CB_341.544 (6)
CE3_11—CD2_111.416 (9)CA_34—C_341.542 (6)
C_11—O_111.215 (6)CB_34—CG1_341.519 (7)
C_11—N_121.338 (6)CB_34—CG2_341.538 (8)
O_11—Na_3iii2.277 (4)C_34—O_341.240 (5)
N_12—CA_121.445 (6)C_34—N_351.331 (6)
CA_12—CB_121.535 (6)N_35—CA_351.452 (6)
CA_12—C_121.548 (6)CA_35—C_351.525 (6)
CB_12—CG_121.536 (6)CA_35—CB_351.542 (6)
CG_12—OD1_121.240 (6)CB_35—CG_351.517 (7)
CG_12—OD2_121.261 (6)CG_35—CD2_351.524 (8)
C_12—O_121.232 (6)CG_35—CD1_351.534 (8)
C_12—N_131.322 (6)C_35—O_351.242 (6)
N_13—CD_131.474 (7)O_35—Na_4iv2.373 (4)
N_13—CA_131.480 (5)N_41—C_451.333 (6)
CA_13—C_131.518 (7)N_41—CA_411.449 (6)
CA_13—CB_131.536 (7)CA_41—CB_411.542 (7)
CB_13—CG_131.524 (7)CA_41—C_411.542 (7)
CG_13—CD_131.520 (7)CB_41—CG_411.490 (8)
C_13—O_131.223 (6)CG_41—CD1_411.392 (10)
C_13—N_141.357 (6)CG_41—CD2_411.448 (9)
N_14—CA_141.451 (6)CD1_41—NE1_411.376 (9)
CA_14—CB_141.538 (6)NE1_41—CE2_411.360 (10)
CA_14—C_141.551 (6)CE2_41—CD2_411.407 (9)
CB_14—CG1_141.526 (7)CE2_41—CZ2_411.428 (10)
CB_14—CG2_141.538 (7)CZ2_41—CH2_411.406 (15)
C_14—O_141.238 (5)CH2_41—CZ3_411.348 (15)
C_14—N_151.318 (6)CZ3_41—CE3_411.409 (10)
N_15—CA_151.470 (6)CE3_41—CD2_411.405 (11)
CA_15—CB_151.528 (6)C_41—O_411.226 (6)
CA_15—C_151.531 (6)C_41—N_421.345 (6)
CB_15—CG_151.530 (7)N_42—CA_421.426 (7)
CG_15—CD2_151.498 (7)CA_42—CB_421.532 (6)
CG_15—CD1_151.538 (8)CA_42—C_421.550 (6)
C_15—O_151.231 (6)CB_42—CG_421.535 (6)
O_15—Na_3iii2.384 (4)CG_42—OD1_421.228 (6)
N_21—C_251.331 (6)CG_42—OD2_421.262 (6)
N_21—CA_211.448 (6)C_42—O_421.226 (6)
CA_21—C_211.527 (7)C_42—N_431.348 (6)
CA_21—CB_211.542 (7)N_43—CD_431.468 (6)
CB_21—CG_211.510 (9)N_43—CA_431.479 (5)
CG_21—CD1_211.338 (11)CA_43—CB_431.533 (7)
CG_21—CD2_211.462 (10)CA_43—C_431.549 (6)
CD1_21—NE1_211.385 (13)CB_43—CG_431.527 (7)
NE1_21—CE2_211.324 (15)CG_43—CD_431.535 (7)
CE2_21—CD2_211.375 (12)C_43—O_431.224 (5)
CE2_21—CZ2_211.404 (17)C_43—N_441.356 (6)
CZ2_21—CH2_211.34 (3)N_44—CA_441.460 (6)
CH2_21—CZ3_211.51 (2)CA_44—CB_441.518 (6)
CZ3_21—CE3_211.338 (13)CA_44—C_441.541 (7)
CE3_21—CD2_211.384 (14)CB_44—CG2_441.513 (8)
C_21—O_211.232 (6)CB_44—CG1_441.536 (9)
C_21—N_221.349 (6)C_44—O_441.244 (6)
N_22—CA_221.442 (6)C_44—N_451.337 (6)
CA_22—CB_221.537 (6)N_45—CA_451.460 (7)
CA_22—C_221.538 (6)CA_45—CB_451.527 (7)
CB_22—CG_221.527 (6)CA_45—C_451.538 (6)
CG_22—OD1_221.246 (6)CB_45—CG_451.518 (7)
CG_22—OD2_221.265 (6)CG_45—CD1_451.515 (9)
C_22—O_221.247 (6)CG_45—CD2_451.539 (9)
C_22—N_231.339 (6)C_45—O_451.212 (6)
N_23—CD_231.464 (7)O1_61—C1_611.433 (8)
N_23—CA_231.478 (6)C1_61—C3_611.505 (10)
CA_23—CB_231.497 (7)C1_61—C2_611.523 (9)
CA_23—C_231.557 (6)O1_62—C1_621.384 (10)
CB_23—CG_231.533 (7)C1_62—C2_621.460 (14)
CG_23—CD_231.532 (7)C1_62—C3_621.467 (13)
C_23—O_231.211 (5)O1_63—C1_631.360 (11)
C_23—N_241.348 (6)C1_63—C2_631.453 (12)
N_24—CA_241.454 (6)C1_63—C3_631.478 (12)
CA_24—C_241.521 (7)O1_64—C1_641.379 (11)
CA_24—CB_241.547 (6)C1_64—C2_641.459 (15)
CB_24—CG1_241.516 (8)C1_64—C3_641.514 (16)
CB_24—CG2_241.531 (8)O1_65—C1_651.475 (17)
C_24—O_241.239 (5)C1_65—C2_651.55 (2)
C_24—N_251.336 (6)C1_65—C3_651.560 (18)
N_25—CA_251.475 (6)O1_66—C1_661.4384
CA_25—CB_251.512 (7)C1_66—C3_661.503 (16)
CA_25—C_251.523 (6)C1_66—C2_661.540 (15)
O_22—Na_1—O_12168.77 (14)CB_23—CA_23—C_23112.5 (4)
O_22—Na_1—OD1_12101.17 (13)CA_23—CB_23—CG_23104.7 (4)
O_12—Na_1—OD1_1281.82 (13)CB_23—CG_23—CD_23102.1 (4)
O_22—Na_1—OD1_2279.79 (12)N_23—CD_23—CG_23103.5 (4)
O_12—Na_1—OD1_22111.26 (13)O_23—C_23—N_24123.1 (5)
OD1_12—Na_1—OD1_2287.78 (14)O_23—C_23—CA_23120.5 (4)
O_22—Na_1—O_2481.70 (12)N_24—C_23—CA_23116.4 (4)
O_12—Na_1—O_2487.13 (13)C_23—N_24—CA_24120.6 (4)
OD1_12—Na_1—O_2499.93 (13)N_24—CA_24—C_24106.0 (3)
OD1_22—Na_1—O_24161.01 (14)N_24—CA_24—CB_24111.9 (4)
O_22—Na_1—O_1495.23 (12)C_24—CA_24—CB_24112.4 (4)
O_12—Na_1—O_1481.89 (12)CG1_24—CB_24—CG2_24111.6 (5)
OD1_12—Na_1—O_14163.58 (13)CG1_24—CB_24—CA_24110.9 (5)
OD1_22—Na_1—O_1496.17 (13)CG2_24—CB_24—CA_24109.1 (4)
O_24—Na_1—O_1481.34 (12)O_24—C_24—N_25124.1 (4)
O_22—Na_1—C_2219.89 (11)O_24—C_24—CA_24119.8 (4)
O_12—Na_1—C_22169.42 (14)N_25—C_24—CA_24116.1 (4)
OD1_12—Na_1—C_22103.64 (13)C_24—O_24—Na_1120.9 (3)
OD1_22—Na_1—C_2260.51 (11)C_24—N_25—CA_25122.2 (4)
O_24—Na_1—C_22100.65 (12)N_25—CA_25—CB_25112.0 (4)
O_14—Na_1—C_2292.12 (13)N_25—CA_25—C_25108.4 (4)
O_32—Na_2—O_42175.50 (15)CB_25—CA_25—C_25109.1 (4)
O_32—Na_2—OD1_42101.21 (14)CA_25—CB_25—CG_25114.7 (4)
O_42—Na_2—OD1_4280.30 (13)CD1_25—CG_25—CB_25113.0 (6)
O_32—Na_2—OD1_3279.35 (14)CD1_25—CG_25—CD2_25108.3 (7)
O_42—Na_2—OD1_32105.11 (14)CB_25—CG_25—CD2_25108.0 (5)
OD1_42—Na_2—OD1_3281.42 (16)O_25—C_25—N_21121.9 (4)
O_32—Na_2—O_4491.93 (13)O_25—C_25—CA_25122.7 (4)
O_42—Na_2—O_4486.60 (12)N_21—C_25—CA_25115.4 (4)
OD1_42—Na_2—O_44166.86 (14)C_35—N_31—CA_31121.6 (4)
OD1_32—Na_2—O_44101.11 (15)N_31—CA_31—C_31111.3 (4)
O_32—Na_2—O_3482.65 (12)N_31—CA_31—CB_31109.2 (4)
O_42—Na_2—O_3492.90 (13)C_31—CA_31—CB_31110.8 (4)
OD1_42—Na_2—O_34101.91 (15)CG_31—CB_31—CA_31112.5 (4)
OD1_32—Na_2—O_34161.99 (14)CD1_31—CG_31—CD2_31105.4 (5)
O_44—Na_2—O_3479.73 (12)CD1_31—CG_31—CB_31129.3 (5)
O_32—Na_2—C_42159.55 (14)CD2_31—CG_31—CB_31125.3 (5)
O_42—Na_2—C_4219.59 (11)NE1_31—CD1_31—CG_31112.4 (5)
OD1_42—Na_2—C_4262.74 (13)CD1_31—NE1_31—CE2_31108.4 (5)
OD1_32—Na_2—C_42108.67 (14)CZ2_31—CE2_31—CD2_31123.7 (6)
O_44—Na_2—C_42104.48 (12)CZ2_31—CE2_31—NE1_31129.7 (6)
O_34—Na_2—C_4288.27 (12)CD2_31—CE2_31—NE1_31106.5 (5)
O_11i—Na_3—O1_51109.36 (14)CH2_31—CZ2_31—CE2_31117.7 (7)
O_11i—Na_3—O1_5488.67 (15)CZ2_31—CH2_31—CZ3_31121.6 (6)
O1_51—Na_3—O1_5488.67 (15)CE3_31—CZ3_31—CH2_31119.1 (7)
O_11i—Na_3—O1_52147.22 (15)CZ3_31—CE3_31—CD2_31119.6 (7)
O1_51—Na_3—O1_52102.21 (14)CE3_31—CD2_31—CE2_31118.2 (5)
O1_54—Na_3—O1_52100.89 (14)CE3_31—CD2_31—CG_31134.5 (6)
O_11i—Na_3—O_15i87.47 (13)CE2_31—CD2_31—CG_31107.2 (5)
O1_51—Na_3—O_15i91.30 (13)O_31—C_31—N_32121.7 (4)
O1_54—Na_3—O_15i175.89 (14)O_31—C_31—CA_31120.6 (4)
O1_52—Na_3—O_15i83.13 (13)N_32—C_31—CA_31117.6 (4)
O_11i—Na_3—Na_4118.29 (12)C_31—N_32—CA_32121.4 (4)
O1_51—Na_3—Na_440.46 (10)N_32—CA_32—C_32107.7 (4)
O1_54—Na_3—Na_452.09 (11)N_32—CA_32—CB_32112.4 (4)
O1_52—Na_3—Na_491.51 (11)C_32—CA_32—CB_32113.1 (4)
O_15i—Na_3—Na_4129.11 (10)CG_32—CB_32—CA_32116.4 (4)
O1_55—Na_4—O_33ii119.56 (19)OD1_32—CG_32—OD2_32124.9 (6)
O1_55—Na_4—O_35ii85.48 (15)OD1_32—CG_32—CB_32120.2 (5)
O_33ii—Na_4—O_35ii103.46 (13)OD2_32—CG_32—CB_32114.9 (6)
O1_55—Na_4—O1_53154.23 (19)CG_32—OD1_32—Na_2159.4 (4)
O_33ii—Na_4—O1_5385.55 (13)O_32—C_32—N_33119.6 (4)
O_35ii—Na_4—O1_5382.75 (14)O_32—C_32—CA_32121.2 (4)
O1_55—Na_4—O1_5181.50 (16)N_33—C_32—CA_32119.2 (4)
O_33ii—Na_4—O1_5183.47 (13)C_32—O_32—Na_2126.0 (3)
O_35ii—Na_4—O1_51166.98 (14)C_32—N_33—CA_33119.6 (4)
O1_53—Na_4—O1_51109.03 (14)C_32—N_33—CD_33128.2 (4)
O1_55—Na_4—O1_5480.72 (16)CA_33—N_33—CD_33111.8 (4)
O_33ii—Na_4—O1_54148.51 (13)N_33—CA_33—CB_33104.2 (4)
O_35ii—Na_4—O1_54101.87 (12)N_33—CA_33—C_33110.6 (3)
O1_53—Na_4—O1_5479.39 (12)CB_33—CA_33—C_33113.2 (4)
O1_51—Na_4—O1_5475.70 (12)CG_33—CB_33—CA_33104.6 (4)
O1_55—Na_4—Na_366.79 (12)CD_33—CG_33—CB_33103.8 (4)
O_33ii—Na_4—Na_3121.97 (11)N_33—CD_33—CG_33101.8 (4)
O_35ii—Na_4—Na_3133.94 (10)O_33—C_33—N_34124.6 (4)
O1_53—Na_4—Na_3106.33 (10)O_33—C_33—CA_33120.9 (4)
O1_51—Na_4—Na_338.62 (9)N_34—C_33—CA_33114.5 (4)
O1_54—Na_4—Na_340.22 (9)C_33—O_33—Na_4iv152.9 (3)
C_15—N_11—CA_11122.1 (4)C_33—N_34—CA_34118.4 (4)
N_11—CA_11—C_11109.1 (3)N_34—CA_34—CB_34112.6 (4)
N_11—CA_11—CB_11109.3 (4)N_34—CA_34—C_34105.4 (4)
C_11—CA_11—CB_11114.0 (4)CB_34—CA_34—C_34110.7 (4)
CG_11—CB_11—CA_11112.6 (4)CG1_34—CB_34—CG2_34111.9 (5)
CD1_11—CG_11—CD2_11106.8 (5)CG1_34—CB_34—CA_34111.2 (4)
CD1_11—CG_11—CB_11126.9 (5)CG2_34—CB_34—CA_34109.3 (4)
CD2_11—CG_11—CB_11126.1 (5)O_34—C_34—N_35124.2 (4)
CG_11—CD1_11—NE1_11110.1 (6)O_34—C_34—CA_34120.3 (4)
CE2_11—NE1_11—CD1_11108.1 (5)N_35—C_34—CA_34115.4 (4)
NE1_11—CE2_11—CD2_11107.4 (5)C_34—O_34—Na_2118.6 (3)
NE1_11—CE2_11—CZ2_11130.3 (6)C_34—N_35—CA_35122.7 (4)
CD2_11—CE2_11—CZ2_11122.3 (6)N_35—CA_35—C_35109.5 (4)
CH2_11—CZ2_11—CE2_11116.9 (6)N_35—CA_35—CB_35111.1 (4)
CZ2_11—CH2_11—CZ3_11122.3 (6)C_35—CA_35—CB_35110.8 (3)
CE3_11—CZ3_11—CH2_11120.4 (7)CG_35—CB_35—CA_35113.2 (4)
CZ3_11—CE3_11—CD2_11119.9 (6)CB_35—CG_35—CD2_35112.0 (5)
CE2_11—CD2_11—CE3_11118.1 (5)CB_35—CG_35—CD1_35110.1 (4)
CE2_11—CD2_11—CG_11107.6 (5)CD2_35—CG_35—CD1_35109.4 (5)
CE3_11—CD2_11—CG_11134.3 (5)O_35—C_35—N_31123.0 (4)
O_11—C_11—N_12123.5 (5)O_35—C_35—CA_35121.8 (4)
O_11—C_11—CA_11121.1 (4)N_31—C_35—CA_35115.2 (4)
N_12—C_11—CA_11115.3 (4)C_35—O_35—Na_4iv150.1 (3)
C_11—O_11—Na_3iii125.3 (3)C_45—N_41—CA_41121.9 (4)
C_11—N_12—CA_12121.5 (4)N_41—CA_41—CB_41108.7 (4)
N_12—CA_12—CB_12110.1 (4)N_41—CA_41—C_41110.0 (4)
N_12—CA_12—C_12109.3 (4)CB_41—CA_41—C_41111.6 (4)
CB_12—CA_12—C_12111.7 (3)CG_41—CB_41—CA_41113.5 (5)
CA_12—CB_12—CG_12114.7 (4)CD1_41—CG_41—CD2_41105.6 (6)
OD1_12—CG_12—OD2_12124.9 (5)CD1_41—CG_41—CB_41127.2 (6)
OD1_12—CG_12—CB_12119.6 (4)CD2_41—CG_41—CB_41127.2 (6)
OD2_12—CG_12—CB_12115.5 (4)NE1_41—CD1_41—CG_41109.4 (7)
CG_12—OD1_12—Na_1144.6 (3)CE2_41—NE1_41—CD1_41109.7 (6)
O_12—C_12—N_13121.6 (4)NE1_41—CE2_41—CD2_41108.2 (6)
O_12—C_12—CA_12120.0 (4)NE1_41—CE2_41—CZ2_41130.0 (7)
N_13—C_12—CA_12118.4 (4)CD2_41—CE2_41—CZ2_41121.7 (7)
C_12—O_12—Na_1125.7 (3)CH2_41—CZ2_41—CE2_41116.4 (7)
C_12—N_13—CD_13128.2 (4)CZ3_41—CH2_41—CZ2_41121.6 (8)
C_12—N_13—CA_13120.5 (4)CH2_41—CZ3_41—CE3_41123.2 (9)
CD_13—N_13—CA_13111.2 (4)CD2_41—CE3_41—CZ3_41117.3 (7)
N_13—CA_13—C_13110.7 (4)CE3_41—CD2_41—CE2_41119.7 (6)
N_13—CA_13—CB_13102.8 (4)CE3_41—CD2_41—CG_41133.1 (6)
C_13—CA_13—CB_13111.9 (4)CE2_41—CD2_41—CG_41107.1 (6)
CG_13—CB_13—CA_13106.2 (4)O_41—C_41—N_42123.0 (5)
CD_13—CG_13—CB_13101.6 (4)O_41—C_41—CA_41121.0 (4)
N_13—CD_13—CG_13103.0 (4)N_42—C_41—CA_41116.0 (4)
O_13—C_13—N_14123.2 (5)C_41—N_42—CA_42122.3 (4)
O_13—C_13—CA_13121.8 (5)N_42—CA_42—CB_42112.4 (4)
N_14—C_13—CA_13114.9 (4)N_42—CA_42—C_42107.4 (4)
C_13—N_14—CA_14119.8 (4)CB_42—CA_42—C_42111.5 (4)
N_14—CA_14—CB_14112.6 (4)CA_42—CB_42—CG_42115.5 (4)
N_14—CA_14—C_14105.1 (3)OD1_42—CG_42—OD2_42124.3 (4)
CB_14—CA_14—C_14110.5 (4)OD1_42—CG_42—CB_42118.7 (4)
CG1_14—CB_14—CA_14110.5 (4)OD2_42—CG_42—CB_42117.0 (4)
CG1_14—CB_14—CG2_14110.4 (4)CG_42—OD1_42—Na_2149.5 (4)
CA_14—CB_14—CG2_14110.1 (4)O_42—C_42—N_43121.4 (4)
O_14—C_14—N_15124.7 (4)O_42—C_42—CA_42120.8 (4)
O_14—C_14—CA_14119.0 (4)N_43—C_42—CA_42117.8 (4)
N_15—C_14—CA_14116.3 (3)O_42—C_42—Na_238.73 (19)
C_14—O_14—Na_1122.8 (3)N_43—C_42—Na_2119.1 (3)
C_14—N_15—CA_15122.2 (3)CA_42—C_42—Na_2108.4 (3)
N_15—CA_15—CB_15112.1 (4)C_42—O_42—Na_2121.7 (3)
N_15—CA_15—C_15108.6 (4)C_42—N_43—CD_43129.6 (4)
CB_15—CA_15—C_15109.9 (3)C_42—N_43—CA_43119.6 (4)
CA_15—CB_15—CG_15115.8 (4)CD_43—N_43—CA_43110.6 (4)
CD2_15—CG_15—CB_15111.5 (4)N_43—CA_43—CB_43104.0 (4)
CD2_15—CG_15—CD1_15109.7 (5)N_43—CA_43—C_43110.3 (4)
CB_15—CG_15—CD1_15111.6 (4)CB_43—CA_43—C_43113.6 (4)
O_15—C_15—N_11123.7 (4)CG_43—CB_43—CA_43105.8 (4)
O_15—C_15—CA_15120.3 (4)CB_43—CG_43—CD_43102.1 (4)
N_11—C_15—CA_15116.0 (4)N_43—CD_43—CG_43102.5 (4)
C_15—O_15—Na_3iii138.1 (3)O_43—C_43—N_44124.7 (4)
C_25—N_21—CA_21121.6 (4)O_43—C_43—CA_43121.3 (4)
N_21—CA_21—C_21111.7 (4)N_44—C_43—CA_43113.7 (4)
N_21—CA_21—CB_21108.5 (4)C_43—N_44—CA_44120.6 (4)
C_21—CA_21—CB_21111.6 (4)N_44—CA_44—CB_44112.8 (4)
CG_21—CB_21—CA_21112.7 (5)N_44—CA_44—C_44104.7 (3)
CD1_21—CG_21—CD2_21104.9 (7)CB_44—CA_44—C_44111.6 (4)
CD1_21—CG_21—CB_21128.4 (7)CG2_44—CB_44—CA_44112.3 (4)
CD2_21—CG_21—CB_21126.7 (7)CG2_44—CB_44—CG1_44111.1 (5)
CG_21—CD1_21—NE1_21111.0 (9)CA_44—CB_44—CG1_44109.3 (4)
CE2_21—NE1_21—CD1_21107.7 (8)O_44—C_44—N_45123.2 (5)
NE1_21—CE2_21—CD2_21110.2 (8)O_44—C_44—CA_44119.7 (4)
NE1_21—CE2_21—CZ2_21127.5 (13)N_45—C_44—CA_44117.1 (4)
CD2_21—CE2_21—CZ2_21122.2 (13)C_44—O_44—Na_2115.1 (3)
CH2_21—CZ2_21—CE2_21117.8 (14)C_44—N_45—CA_45121.8 (4)
CZ2_21—CH2_21—CZ3_21121.3 (12)N_45—CA_45—CB_45112.9 (4)
CE3_21—CZ3_21—CH2_21116.4 (15)N_45—CA_45—C_45106.7 (4)
CZ3_21—CE3_21—CD2_21122.7 (11)CB_45—CA_45—C_45110.6 (4)
CE2_21—CD2_21—CE3_21119.2 (8)CG_45—CB_45—CA_45113.2 (4)
CE2_21—CD2_21—CG_21106.1 (8)CD1_45—CG_45—CB_45111.6 (5)
CE3_21—CD2_21—CG_21134.6 (8)CD1_45—CG_45—CD2_45109.2 (6)
O_21—C_21—N_22122.9 (4)CB_45—CG_45—CD2_45109.3 (5)
O_21—C_21—CA_21120.7 (4)O_45—C_45—N_41123.4 (4)
N_22—C_21—CA_21116.4 (4)O_45—C_45—CA_45120.7 (4)
C_21—N_22—CA_22122.0 (4)N_41—C_45—CA_45115.8 (4)
N_22—CA_22—CB_22113.0 (4)Na_3—O1_51—Na_4100.92 (14)
N_22—CA_22—C_22107.6 (4)Na_3—O1_54—Na_487.69 (13)
CB_22—CA_22—C_22112.7 (4)O1_61—C1_61—C3_61113.6 (6)
CG_22—CB_22—CA_22117.6 (4)O1_61—C1_61—C2_61106.0 (6)
OD1_22—CG_22—OD2_22124.1 (4)C3_61—C1_61—C2_61111.4 (8)
OD1_22—CG_22—CB_22119.4 (4)O1_62—C1_62—C2_62121.2 (11)
OD2_22—CG_22—CB_22116.5 (4)O1_62—C1_62—C3_62110.4 (9)
CG_22—OD1_22—Na_1157.4 (3)C2_62—C1_62—C3_62115.5 (12)
O_22—C_22—N_23120.2 (4)O1_63—C1_63—C2_63122.0 (10)
O_22—C_22—CA_22120.2 (4)O1_63—C1_63—C3_63112.5 (10)
N_23—C_22—CA_22119.5 (4)C2_63—C1_63—C3_63117.2 (9)
O_22—C_22—Na_138.16 (19)O1_64—C1_64—C2_64117.2 (12)
N_23—C_22—Na_1117.2 (3)O1_64—C1_64—C3_64114.6 (17)
CA_22—C_22—Na_1108.6 (3)C2_64—C1_64—C3_64114.4 (16)
C_22—O_22—Na_1121.9 (3)O1_65—C1_65—C2_65101.2 (19)
C_22—N_23—CD_23128.5 (4)O1_65—C1_65—C3_65103.1 (14)
C_22—N_23—CA_23120.3 (4)C2_65—C1_65—C3_65102.8 (16)
CD_23—N_23—CA_23111.0 (4)O1_66—C1_66—C3_66116.2 (16)
N_23—CA_23—CB_23104.6 (4)O1_66—C1_66—C2_66110.6 (9)
N_23—CA_23—C_23109.2 (4)C3_66—C1_66—C2_66107.7 (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, z1/2; (iv) x1/2, y+3/2, z+1.

Experimental details

Crystal data
Chemical formula4(C31H41N6O7Na)·8(H2O)·5.63(C3H7OH)
Mr3013.12
Crystal system, space groupOrthorhombic, P212121
Temperature (K)100
a, b, c (Å)25.3930 (4), 34.7193 (3), 25.7201 (4)
V3)22675.5 (5)
Z4
Radiation typeSynchrotron, λ = 0.83400 Å
µ (mm1)0.07
Crystal size (mm)0.08 × 0.04 × 0.04
Data collection
DiffractometerRigaku RAXIS-IV
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
83268, 22865, 22861
Rint0.034
(sin θ/λ)max1)0.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.164, 1.07
No. of reflections22865
No. of parameters1904
No. of restraints36
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
(Δ/σ)max0.656
Δρmax, Δρmin (e Å3)0.56, 0.26
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0 (10)

Computer programs: RIgaku PROCESS, MOSFLM 6.01 (Leslie, 1999), LODEM (Shiono, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-III (Burnett & Johnson,1996), PARST (Nardelli, 1983).

 

Follow Acta Cryst. D
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds