Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806011305/kp2007sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806011305/kp2007Isup2.hkl |
CCDC reference: 608433
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.066
- wR factor = 0.142
- Data-to-parameter ratio = 18.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 27.00 Perc. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 17 H2 O
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
C22H27N7·4.5H2O | F(000) = 2024 |
Mr = 470.58 | Dx = 1.022 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 6376 reflections |
a = 7.4815 (5) Å | θ = 2.2–25.2° |
b = 21.5452 (14) Å | µ = 0.07 mm−1 |
c = 37.968 (3) Å | T = 294 K |
β = 91.261 (1)° | Block, yellow |
V = 6118.5 (7) Å3 | 0.30 × 0.26 × 0.24 mm |
Z = 8 |
Bruker SMART APEX CCD area-detector diffractometer | 12024 independent reflections |
Radiation source: sealed tube | 7076 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.064 |
φ annd ω scans | θmax = 26.0°, θmin = 1.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −9→9 |
Tmin = 0.97, Tmax = 0.98 | k = −26→26 |
63905 measured reflections | l = −46→46 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.142 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.05P)2 + 1.22P] where P = (Fo2 + 2Fc2)/3 |
12024 reflections | (Δ/σ)max < 0.001 |
658 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.28 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.1859 (3) | 0.33911 (11) | 0.65638 (6) | 0.0523 (6) | |
H1A | 0.1572 | 0.3824 | 0.6606 | 0.063* | |
H1B | 0.0769 | 0.3151 | 0.6584 | 0.063* | |
C2 | 0.2568 (3) | 0.33196 (10) | 0.61995 (6) | 0.0487 (5) | |
H2A | 0.3490 | 0.3627 | 0.6159 | 0.058* | |
H2B | 0.1613 | 0.3382 | 0.6026 | 0.058* | |
C3 | 0.1928 (3) | 0.21736 (10) | 0.61558 (6) | 0.0520 (6) | |
H3A | 0.1724 | 0.2030 | 0.5916 | 0.062* | |
H3B | 0.0810 | 0.2331 | 0.6244 | 0.062* | |
C4 | 0.2606 (3) | 0.16459 (11) | 0.63855 (6) | 0.0550 (6) | |
H4A | 0.1645 | 0.1351 | 0.6419 | 0.066* | |
H4B | 0.3562 | 0.1433 | 0.6266 | 0.066* | |
C5 | 0.1938 (3) | 0.21461 (10) | 0.69520 (6) | 0.0504 (5) | |
H5A | 0.1702 | 0.1871 | 0.7148 | 0.060* | |
H5B | 0.0828 | 0.2201 | 0.6819 | 0.060* | |
C6 | 0.2559 (3) | 0.27699 (10) | 0.70935 (6) | 0.0495 (5) | |
H6A | 0.1580 | 0.2965 | 0.7215 | 0.059* | |
H6B | 0.3523 | 0.2703 | 0.7264 | 0.059* | |
C7 | 0.4474 (3) | 0.36577 (11) | 0.69455 (6) | 0.0569 (6) | |
H7A | 0.5061 | 0.3823 | 0.6741 | 0.068* | |
H7B | 0.5381 | 0.3459 | 0.7093 | 0.068* | |
C8 | 0.3685 (3) | 0.41820 (10) | 0.71449 (6) | 0.0515 (5) | |
C9 | 0.2640 (3) | 0.51055 (10) | 0.72740 (6) | 0.0466 (5) | |
C10 | 0.1989 (3) | 0.57269 (12) | 0.72770 (7) | 0.0630 (6) | |
H10 | 0.1891 | 0.5963 | 0.7072 | 0.076* | |
C11 | 0.1520 (3) | 0.59554 (11) | 0.75964 (6) | 0.0577 (6) | |
H11 | 0.1162 | 0.6368 | 0.7610 | 0.069* | |
C12 | 0.1551 (3) | 0.56078 (11) | 0.78961 (7) | 0.0581 (6) | |
H12 | 0.1147 | 0.5784 | 0.8103 | 0.070* | |
C13 | 0.2163 (3) | 0.50021 (11) | 0.79030 (6) | 0.0556 (6) | |
H13 | 0.2195 | 0.4772 | 0.8110 | 0.067* | |
C14 | 0.2723 (3) | 0.47548 (10) | 0.75896 (6) | 0.0472 (5) | |
C15 | 0.4561 (3) | 0.14630 (10) | 0.69067 (6) | 0.0480 (5) | |
H15A | 0.5091 | 0.1692 | 0.7103 | 0.058* | |
H15B | 0.5507 | 0.1362 | 0.6746 | 0.058* | |
C16 | 0.3782 (3) | 0.08796 (10) | 0.70411 (6) | 0.0480 (5) | |
C17 | 0.2759 (3) | −0.00859 (11) | 0.70774 (6) | 0.0531 (6) | |
C18 | 0.2172 (3) | −0.06970 (10) | 0.70183 (6) | 0.0510 (5) | |
H18 | 0.2159 | −0.0873 | 0.6795 | 0.061* | |
C19 | 0.1633 (3) | −0.10144 (11) | 0.72998 (6) | 0.0503 (5) | |
H19 | 0.1253 | −0.1423 | 0.7273 | 0.060* | |
C20 | 0.1631 (3) | −0.07392 (11) | 0.76367 (6) | 0.0532 (6) | |
H20 | 0.1251 | −0.0982 | 0.7823 | 0.064* | |
C21 | 0.2130 (3) | −0.01611 (12) | 0.77083 (6) | 0.0580 (6) | |
H21 | 0.2101 | 0.0009 | 0.7933 | 0.070* | |
C22 | 0.2716 (3) | 0.01772 (11) | 0.74090 (6) | 0.0513 (5) | |
C23 | 0.6629 (3) | 0.33514 (10) | 0.40561 (5) | 0.0486 (5) | |
H23A | 0.6329 | 0.3786 | 0.4085 | 0.058* | |
H23B | 0.5556 | 0.3108 | 0.4091 | 0.058* | |
C24 | 0.7323 (3) | 0.32400 (11) | 0.36815 (6) | 0.0580 (6) | |
H24A | 0.6339 | 0.3267 | 0.3512 | 0.070* | |
H24B | 0.8193 | 0.3556 | 0.3625 | 0.070* | |
C25 | 0.6911 (3) | 0.21078 (11) | 0.36742 (6) | 0.0560 (6) | |
H25A | 0.6720 | 0.1948 | 0.3438 | 0.067* | |
H25B | 0.5769 | 0.2252 | 0.3758 | 0.067* | |
C26 | 0.7600 (3) | 0.15799 (11) | 0.39145 (6) | 0.0521 (6) | |
H26A | 0.6651 | 0.1281 | 0.3950 | 0.063* | |
H26B | 0.8581 | 0.1368 | 0.3803 | 0.063* | |
C27 | 0.6860 (3) | 0.21283 (10) | 0.44638 (6) | 0.0511 (5) | |
H27A | 0.6588 | 0.1864 | 0.4662 | 0.061* | |
H27B | 0.5775 | 0.2176 | 0.4322 | 0.061* | |
C28 | 0.7457 (3) | 0.27650 (10) | 0.46004 (5) | 0.0465 (5) | |
H28A | 0.6481 | 0.2957 | 0.4724 | 0.056* | |
H28B | 0.8448 | 0.2712 | 0.4767 | 0.056* | |
C29 | 0.9279 (3) | 0.36555 (11) | 0.44192 (6) | 0.0562 (6) | |
H29A | 0.9738 | 0.3843 | 0.4207 | 0.067* | |
H29B | 1.0279 | 0.3461 | 0.4543 | 0.067* | |
C30 | 0.8569 (3) | 0.41579 (10) | 0.46459 (6) | 0.0487 (5) | |
C31 | 0.7454 (3) | 0.50426 (11) | 0.48498 (6) | 0.0527 (6) | |
C32 | 0.6766 (3) | 0.56253 (11) | 0.48858 (6) | 0.0558 (6) | |
H32 | 0.6518 | 0.5875 | 0.4691 | 0.067* | |
C33 | 0.6457 (3) | 0.58242 (12) | 0.52186 (6) | 0.0545 (6) | |
H33 | 0.5952 | 0.6213 | 0.5253 | 0.065* | |
C34 | 0.6869 (3) | 0.54686 (11) | 0.54981 (6) | 0.0527 (6) | |
H34 | 0.6705 | 0.5629 | 0.5723 | 0.063* | |
C35 | 0.7528 (3) | 0.48724 (11) | 0.54654 (7) | 0.0563 (6) | |
H35 | 0.7731 | 0.4624 | 0.5663 | 0.068* | |
C36 | 0.7866 (3) | 0.46624 (11) | 0.51415 (6) | 0.0555 (6) | |
C37 | 0.9505 (3) | 0.14493 (10) | 0.44515 (6) | 0.0500 (5) | |
H37A | 1.0006 | 0.1692 | 0.4645 | 0.060* | |
H37B | 1.0474 | 0.1343 | 0.4297 | 0.060* | |
C38 | 0.8759 (3) | 0.08725 (10) | 0.45949 (6) | 0.0471 (5) | |
C39 | 0.7794 (3) | −0.00917 (10) | 0.46648 (6) | 0.0496 (5) | |
C40 | 0.7258 (3) | −0.06996 (11) | 0.46196 (7) | 0.0583 (6) | |
H40 | 0.7290 | −0.0898 | 0.4402 | 0.070* | |
C41 | 0.6677 (3) | −0.09922 (11) | 0.49167 (7) | 0.0582 (6) | |
H41 | 0.6312 | −0.1404 | 0.4897 | 0.070* | |
C42 | 0.6599 (3) | −0.07084 (12) | 0.52472 (7) | 0.0613 (7) | |
H42 | 0.6220 | −0.0933 | 0.5441 | 0.074* | |
C43 | 0.7076 (3) | −0.01069 (11) | 0.52834 (6) | 0.0546 (6) | |
H43 | 0.6989 | 0.0096 | 0.5499 | 0.066* | |
C44 | 0.7710 (3) | 0.02040 (11) | 0.49839 (6) | 0.0503 (5) | |
N1 | 0.3164 (2) | 0.31819 (8) | 0.68274 (5) | 0.0514 (5) | |
N2 | 0.3328 (3) | 0.26782 (8) | 0.61641 (5) | 0.0524 (5) | |
H2C | 0.4088 | 0.2608 | 0.6347 | 0.063* | |
N3 | 0.3259 (2) | 0.18573 (8) | 0.67257 (5) | 0.0484 (4) | |
N4 | 0.3261 (2) | 0.47259 (8) | 0.70186 (5) | 0.0492 (4) | |
H4 | 0.3362 | 0.4831 | 0.6801 | 0.059* | |
N5 | 0.3365 (2) | 0.41830 (8) | 0.74922 (5) | 0.0479 (4) | |
N6 | 0.3445 (2) | 0.03607 (9) | 0.68581 (5) | 0.0512 (5) | |
N7 | 0.3354 (3) | 0.07741 (9) | 0.73753 (5) | 0.0553 (5) | |
H7 | 0.3460 | 0.1039 | 0.7544 | 0.066* | |
N8 | 0.8005 (2) | 0.31734 (8) | 0.43163 (5) | 0.0480 (4) | |
N9 | 0.8145 (2) | 0.26305 (8) | 0.36621 (5) | 0.0491 (5) | |
H9A | 0.8943 | 0.2593 | 0.3842 | 0.059* | |
N10 | 0.8209 (2) | 0.18328 (8) | 0.42554 (4) | 0.0428 (4) | |
N11 | 0.7912 (2) | 0.46896 (9) | 0.45497 (5) | 0.0506 (5) | |
H11A | 0.7773 | 0.4811 | 0.4335 | 0.061* | |
N12 | 0.8542 (3) | 0.41055 (9) | 0.50063 (5) | 0.0600 (5) | |
N13 | 0.8444 (2) | 0.03517 (8) | 0.44374 (5) | 0.0481 (4) | |
H13A | 0.8618 | 0.0288 | 0.4217 | 0.058* | |
N14 | 0.8266 (2) | 0.08042 (8) | 0.49383 (4) | 0.0429 (4) | |
O1 | 0.2163 (4) | 0.61291 (15) | 0.88526 (8) | 0.0386 (8) | 0.40 |
H1D | 0.3212 | 0.6171 | 0.8940 | 0.046* | 0.40 |
H1E | 0.1861 | 0.6460 | 0.8745 | 0.046* | 0.40 |
O2 | 0.4792 (5) | 0.72461 (16) | 0.45344 (9) | 0.0464 (9) | 0.40 |
H2E | 0.4984 | 0.7525 | 0.4382 | 0.056* | 0.40 |
H2F | 0.4939 | 0.6890 | 0.4443 | 0.056* | 0.40 |
O3 | 0.7144 (5) | 0.49975 (17) | 0.37789 (10) | 0.0562 (10) | 0.40 |
H3D | 0.6022 | 0.5028 | 0.3744 | 0.067* | 0.40 |
H3E | 0.7641 | 0.5340 | 0.3728 | 0.067* | 0.40 |
O4 | 0.7684 (5) | 0.24306 (14) | 0.23019 (9) | 0.0408 (8) | 0.40 |
H4E | 0.7968 | 0.2277 | 0.2105 | 0.049* | 0.40 |
H4F | 0.6571 | 0.2509 | 0.2300 | 0.049* | 0.40 |
O5 | 0.8409 (5) | 0.47745 (16) | 0.64193 (9) | 0.0482 (9) | 0.40 |
H5E | 0.8885 | 0.4417 | 0.6405 | 0.058* | 0.40 |
H5F | 0.7448 | 0.4783 | 0.6296 | 0.058* | 0.40 |
O6 | 0.8329 (2) | 0.17663 (7) | 0.54300 (4) | 0.0540 (4) | |
H6C | 0.8985 | 0.1449 | 0.5400 | 0.065* | |
H6E | 0.7640 | 0.1702 | 0.5601 | 0.065* | |
O7 | 0.7212 (5) | 0.34956 (17) | 0.61338 (10) | 0.0518 (9) | 0.40 |
H7F | 0.7407 | 0.3181 | 0.6005 | 0.062* | 0.40 |
H7C | 0.7798 | 0.3460 | 0.6327 | 0.062* | 0.40 |
O8 | 0.3772 (4) | 0.18115 (15) | 0.79300 (9) | 0.0440 (8) | 0.40 |
H8D | 0.4138 | 0.1988 | 0.7745 | 0.053* | 0.40 |
H8C | 0.4584 | 0.1572 | 0.8012 | 0.053* | 0.40 |
O9 | 0.47605 (19) | 0.01240 (7) | 0.61949 (4) | 0.0495 (4) | |
H9F | 0.4640 | 0.0313 | 0.6390 | 0.059* | |
H9E | 0.5845 | 0.0145 | 0.6134 | 0.059* | |
O10 | 0.2051 (5) | 0.14010 (17) | 0.86493 (10) | 0.0526 (10) | 0.40 |
H10B | 0.1556 | 0.1103 | 0.8756 | 0.063* | 0.40 |
H10D | 0.2284 | 0.1292 | 0.8440 | 0.063* | 0.40 |
O11 | 0.3473 (2) | 0.33101 (7) | 0.80130 (4) | 0.0558 (4) | |
H11B | 0.3397 | 0.3625 | 0.8147 | 0.067* | |
H11D | 0.2737 | 0.3348 | 0.7841 | 0.067* | |
O12 | 0.9835 (4) | 0.00977 (16) | 0.37816 (9) | 0.0446 (8) | 0.40 |
H12A | 0.9416 | −0.0268 | 0.3762 | 0.053* | 0.40 |
H12B | 0.9403 | 0.0324 | 0.3617 | 0.053* | 0.40 |
O13 | 0.28393 (19) | 0.11084 (6) | 0.37363 (4) | 0.0459 (4) | |
H13B | 0.3835 | 0.0967 | 0.3813 | 0.055* | |
H13C | 0.1998 | 0.0875 | 0.3804 | 0.055* | |
O14 | 1.2258 (5) | 0.24921 (17) | 0.40344 (9) | 0.0489 (9) | 0.40 |
H14A | 1.1819 | 0.2864 | 0.4117 | 0.059* | 0.40 |
H14B | 1.1771 | 0.2396 | 0.3878 | 0.059* | 0.40 |
O15 | 0.9775 (2) | 0.30901 (7) | 0.54434 (4) | 0.0585 (4) | |
H15E | 0.9464 | 0.2713 | 0.5417 | 0.070* | |
H15C | 0.9524 | 0.3292 | 0.5257 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0568 (14) | 0.0444 (12) | 0.0551 (14) | 0.0047 (10) | −0.0095 (11) | −0.0065 (10) |
C2 | 0.0519 (13) | 0.0511 (13) | 0.0427 (12) | −0.0008 (10) | −0.0057 (10) | 0.0005 (10) |
C3 | 0.0574 (14) | 0.0453 (13) | 0.0528 (13) | 0.0014 (10) | −0.0113 (11) | −0.0119 (10) |
C4 | 0.0529 (14) | 0.0527 (14) | 0.0585 (15) | 0.0007 (11) | −0.0186 (11) | −0.0124 (11) |
C5 | 0.0531 (13) | 0.0409 (12) | 0.0575 (14) | 0.0018 (10) | 0.0081 (10) | 0.0058 (10) |
C6 | 0.0573 (13) | 0.0401 (12) | 0.0510 (13) | −0.0008 (10) | 0.0007 (10) | 0.0007 (10) |
C7 | 0.0672 (15) | 0.0509 (14) | 0.0526 (14) | −0.0005 (12) | −0.0002 (12) | −0.0009 (11) |
C8 | 0.0640 (15) | 0.0391 (12) | 0.0514 (13) | −0.0046 (10) | 0.0012 (11) | −0.0059 (10) |
C9 | 0.0516 (13) | 0.0447 (12) | 0.0434 (12) | −0.0060 (10) | 0.0025 (10) | 0.0051 (10) |
C10 | 0.0630 (16) | 0.0567 (15) | 0.0690 (17) | −0.0012 (12) | −0.0068 (12) | 0.0004 (13) |
C11 | 0.0616 (15) | 0.0521 (14) | 0.0598 (15) | 0.0025 (11) | 0.0146 (12) | −0.0145 (12) |
C12 | 0.0558 (14) | 0.0592 (15) | 0.0596 (15) | −0.0049 (11) | 0.0090 (11) | −0.0283 (12) |
C13 | 0.0572 (14) | 0.0586 (15) | 0.0510 (14) | −0.0128 (11) | 0.0015 (11) | −0.0067 (11) |
C14 | 0.0457 (12) | 0.0440 (12) | 0.0517 (13) | −0.0100 (9) | −0.0043 (10) | −0.0033 (10) |
C15 | 0.0470 (12) | 0.0470 (13) | 0.0504 (13) | 0.0118 (10) | 0.0087 (10) | −0.0018 (10) |
C16 | 0.0477 (12) | 0.0482 (13) | 0.0479 (13) | 0.0131 (10) | −0.0034 (10) | −0.0003 (10) |
C17 | 0.0549 (13) | 0.0482 (13) | 0.0559 (14) | 0.0132 (11) | −0.0065 (11) | −0.0006 (11) |
C18 | 0.0508 (13) | 0.0438 (12) | 0.0579 (14) | 0.0049 (10) | −0.0083 (10) | −0.0111 (10) |
C19 | 0.0514 (13) | 0.0474 (13) | 0.0516 (13) | −0.0026 (10) | −0.0112 (10) | 0.0139 (11) |
C20 | 0.0573 (14) | 0.0515 (14) | 0.0509 (14) | 0.0093 (11) | 0.0061 (11) | 0.0139 (11) |
C21 | 0.0601 (14) | 0.0646 (16) | 0.0501 (14) | 0.0113 (12) | 0.0172 (11) | 0.0158 (12) |
C22 | 0.0460 (12) | 0.0515 (13) | 0.0562 (14) | 0.0090 (10) | −0.0021 (10) | −0.0044 (11) |
C23 | 0.0582 (14) | 0.0438 (12) | 0.0435 (12) | 0.0056 (10) | −0.0022 (10) | −0.0084 (9) |
C24 | 0.0563 (14) | 0.0600 (15) | 0.0576 (15) | 0.0042 (12) | 0.0001 (11) | 0.0138 (12) |
C25 | 0.0686 (15) | 0.0499 (13) | 0.0489 (13) | 0.0028 (11) | −0.0133 (11) | −0.0064 (11) |
C26 | 0.0521 (13) | 0.0538 (13) | 0.0498 (13) | −0.0014 (11) | −0.0137 (10) | −0.0050 (10) |
C27 | 0.0554 (13) | 0.0388 (12) | 0.0599 (14) | 0.0080 (10) | 0.0179 (11) | 0.0053 (10) |
C28 | 0.0563 (13) | 0.0442 (12) | 0.0393 (11) | −0.0038 (10) | 0.0069 (10) | 0.0003 (9) |
C29 | 0.0564 (14) | 0.0560 (14) | 0.0567 (14) | −0.0048 (11) | 0.0119 (11) | −0.0069 (11) |
C30 | 0.0507 (13) | 0.0425 (13) | 0.0527 (13) | −0.0131 (10) | −0.0003 (10) | −0.0072 (10) |
C31 | 0.0489 (13) | 0.0498 (14) | 0.0590 (14) | 0.0023 (10) | −0.0040 (10) | −0.0133 (11) |
C32 | 0.0616 (14) | 0.0551 (14) | 0.0508 (14) | 0.0013 (11) | 0.0020 (11) | −0.0270 (11) |
C33 | 0.0510 (13) | 0.0610 (15) | 0.0520 (13) | −0.0115 (11) | 0.0071 (11) | −0.0156 (12) |
C34 | 0.0550 (13) | 0.0539 (14) | 0.0491 (14) | −0.0010 (11) | −0.0009 (11) | −0.0159 (11) |
C35 | 0.0521 (13) | 0.0521 (13) | 0.0642 (15) | −0.0137 (11) | −0.0057 (11) | −0.0303 (12) |
C36 | 0.0566 (14) | 0.0496 (14) | 0.0602 (15) | −0.0095 (11) | −0.0002 (11) | −0.0218 (12) |
C37 | 0.0469 (12) | 0.0521 (13) | 0.0508 (13) | −0.0006 (10) | −0.0015 (10) | −0.0028 (10) |
C38 | 0.0533 (13) | 0.0449 (13) | 0.0430 (12) | 0.0035 (10) | −0.0022 (10) | −0.0040 (10) |
C39 | 0.0415 (12) | 0.0490 (13) | 0.0582 (14) | −0.0026 (10) | 0.0024 (10) | 0.0020 (11) |
C40 | 0.0569 (14) | 0.0569 (15) | 0.0606 (15) | 0.0080 (11) | −0.0112 (11) | −0.0131 (12) |
C41 | 0.0692 (16) | 0.0453 (13) | 0.0601 (16) | −0.0055 (11) | 0.0015 (12) | 0.0160 (12) |
C42 | 0.0530 (14) | 0.0606 (16) | 0.0701 (17) | 0.0119 (12) | −0.0035 (12) | 0.0441 (13) |
C43 | 0.0561 (14) | 0.0576 (15) | 0.0503 (13) | 0.0106 (11) | 0.0073 (11) | 0.0165 (11) |
C44 | 0.0461 (12) | 0.0536 (13) | 0.0509 (13) | 0.0026 (10) | −0.0052 (10) | 0.0084 (11) |
N1 | 0.0524 (11) | 0.0476 (11) | 0.0540 (12) | 0.0004 (9) | −0.0054 (9) | −0.0032 (9) |
N2 | 0.0642 (12) | 0.0514 (11) | 0.0415 (10) | 0.0086 (9) | −0.0010 (9) | −0.0068 (8) |
N3 | 0.0516 (10) | 0.0402 (10) | 0.0531 (11) | 0.0039 (8) | −0.0020 (8) | −0.0028 (8) |
N4 | 0.0505 (10) | 0.0452 (11) | 0.0516 (11) | −0.0013 (8) | −0.0046 (8) | 0.0011 (9) |
N5 | 0.0562 (11) | 0.0428 (10) | 0.0445 (10) | −0.0067 (8) | −0.0063 (8) | −0.0010 (8) |
N6 | 0.0567 (12) | 0.0458 (11) | 0.0508 (11) | 0.0052 (9) | −0.0028 (9) | −0.0056 (9) |
N7 | 0.0664 (13) | 0.0448 (11) | 0.0543 (12) | 0.0185 (9) | −0.0071 (9) | −0.0052 (9) |
N8 | 0.0503 (10) | 0.0405 (10) | 0.0530 (11) | 0.0019 (8) | −0.0021 (8) | −0.0052 (8) |
N9 | 0.0561 (11) | 0.0515 (11) | 0.0396 (10) | 0.0050 (9) | −0.0005 (8) | −0.0108 (8) |
N10 | 0.0458 (10) | 0.0404 (9) | 0.0419 (10) | −0.0011 (8) | −0.0049 (8) | −0.0041 (7) |
N11 | 0.0499 (11) | 0.0509 (11) | 0.0512 (11) | −0.0020 (9) | 0.0059 (9) | −0.0031 (9) |
N12 | 0.0667 (13) | 0.0566 (12) | 0.0566 (12) | −0.0039 (10) | 0.0014 (10) | −0.0115 (10) |
N13 | 0.0651 (12) | 0.0396 (10) | 0.0396 (10) | 0.0050 (8) | 0.0035 (8) | −0.0012 (8) |
N14 | 0.0481 (10) | 0.0417 (10) | 0.0387 (9) | −0.0025 (8) | −0.0013 (7) | 0.0104 (7) |
O1 | 0.0402 (18) | 0.0410 (19) | 0.0350 (18) | 0.0122 (14) | 0.0096 (14) | 0.0107 (14) |
O2 | 0.054 (2) | 0.047 (2) | 0.0386 (19) | −0.0318 (17) | 0.0131 (16) | −0.0083 (16) |
O3 | 0.053 (2) | 0.060 (3) | 0.055 (2) | −0.0087 (19) | −0.0143 (18) | 0.0213 (19) |
O4 | 0.0465 (19) | 0.0344 (18) | 0.0420 (19) | −0.0018 (15) | 0.0077 (15) | −0.0123 (15) |
O5 | 0.055 (2) | 0.043 (2) | 0.047 (2) | −0.0108 (17) | 0.0131 (17) | −0.0051 (16) |
O6 | 0.0515 (9) | 0.0530 (9) | 0.0583 (10) | −0.0001 (7) | 0.0205 (7) | −0.0068 (7) |
O7 | 0.050 (2) | 0.050 (2) | 0.054 (2) | −0.0141 (18) | −0.0149 (17) | 0.0100 (18) |
O8 | 0.050 (2) | 0.0407 (19) | 0.0407 (19) | 0.0180 (16) | −0.0131 (16) | −0.0071 (15) |
O9 | 0.0497 (8) | 0.0495 (8) | 0.0498 (9) | −0.0043 (7) | 0.0140 (7) | −0.0202 (7) |
O10 | 0.051 (2) | 0.056 (2) | 0.050 (2) | 0.0155 (18) | −0.0102 (17) | −0.0134 (18) |
O11 | 0.0553 (9) | 0.0578 (10) | 0.0549 (9) | −0.0011 (7) | 0.0192 (8) | 0.0029 (7) |
O12 | 0.044 (2) | 0.0422 (19) | 0.048 (2) | −0.0029 (15) | 0.0080 (16) | −0.0020 (16) |
O13 | 0.0468 (8) | 0.0456 (8) | 0.0460 (8) | 0.0044 (6) | 0.0141 (6) | 0.0014 (6) |
O14 | 0.047 (2) | 0.053 (2) | 0.046 (2) | −0.0121 (17) | −0.0068 (16) | 0.0098 (17) |
O15 | 0.0539 (9) | 0.0600 (10) | 0.0609 (10) | 0.0109 (8) | −0.0163 (8) | 0.0100 (8) |
C1—N1 | 1.454 (3) | C28—N8 | 1.458 (3) |
C1—C2 | 1.500 (3) | C28—H28A | 0.9700 |
C1—H1A | 0.9700 | C28—H28B | 0.9700 |
C1—H1B | 0.9700 | C29—N8 | 1.458 (3) |
C2—N2 | 1.502 (3) | C29—C30 | 1.488 (3) |
C2—H2A | 0.9700 | C29—H29A | 0.9700 |
C2—H2B | 0.9700 | C29—H29B | 0.9700 |
C3—N2 | 1.509 (3) | C30—N11 | 1.296 (3) |
C3—C4 | 1.514 (3) | C30—N12 | 1.373 (3) |
C3—H3A | 0.9700 | C31—C32 | 1.365 (3) |
C3—H3B | 0.9700 | C31—C36 | 1.406 (3) |
C4—N3 | 1.445 (3) | C31—N11 | 1.418 (3) |
C4—H4A | 0.9700 | C32—C33 | 1.359 (3) |
C4—H4B | 0.9700 | C32—H32 | 0.9300 |
C5—N3 | 1.463 (3) | C33—C34 | 1.339 (3) |
C5—C6 | 1.517 (3) | C33—H33 | 0.9300 |
C5—H5A | 0.9700 | C34—C35 | 1.382 (3) |
C5—H5B | 0.9700 | C34—H34 | 0.9300 |
C6—N1 | 1.426 (3) | C35—C36 | 1.340 (3) |
C6—H6A | 0.9700 | C35—H35 | 0.9300 |
C6—H6B | 0.9700 | C36—N12 | 1.404 (3) |
C7—N1 | 1.481 (3) | C37—N10 | 1.464 (3) |
C7—C8 | 1.489 (3) | C37—C38 | 1.472 (3) |
C7—H7A | 0.9700 | C37—H37A | 0.9700 |
C7—H7B | 0.9700 | C37—H37B | 0.9700 |
C8—N4 | 1.303 (3) | C38—N13 | 1.290 (3) |
C8—N5 | 1.345 (3) | C38—N14 | 1.371 (3) |
C9—N4 | 1.358 (3) | C39—C44 | 1.372 (3) |
C9—C14 | 1.417 (3) | C39—C40 | 1.379 (3) |
C9—C10 | 1.425 (3) | C39—N13 | 1.383 (3) |
C10—C11 | 1.362 (3) | C40—C41 | 1.371 (3) |
C10—H10 | 0.9300 | C40—H40 | 0.9300 |
C11—C12 | 1.362 (3) | C41—C42 | 1.398 (4) |
C11—H11 | 0.9300 | C41—H41 | 0.9300 |
C12—C13 | 1.383 (3) | C42—C43 | 1.351 (3) |
C12—H12 | 0.9300 | C42—H42 | 0.9300 |
C13—C14 | 1.377 (3) | C43—C44 | 1.411 (3) |
C13—H13 | 0.9300 | C43—H43 | 0.9300 |
C14—N5 | 1.376 (3) | C44—N14 | 1.371 (3) |
C15—N3 | 1.454 (3) | N2—H2C | 0.8999 |
C15—C16 | 1.481 (3) | N4—H4 | 0.8600 |
C15—H15A | 0.9700 | N7—H7 | 0.8600 |
C15—H15B | 0.9700 | N9—H9A | 0.9000 |
C16—N7 | 1.335 (3) | N11—H11A | 0.8600 |
C16—N6 | 1.337 (3) | N13—H13A | 0.8600 |
C17—N6 | 1.379 (3) | O1—H1D | 0.8499 |
C17—C22 | 1.382 (3) | O1—H1E | 0.8499 |
C17—C18 | 1.404 (3) | O2—H2E | 0.8501 |
C18—C19 | 1.338 (3) | O2—H2F | 0.8500 |
C18—H18 | 0.9300 | O3—H3D | 0.8500 |
C19—C20 | 1.410 (3) | O3—H3E | 0.8499 |
C19—H19 | 0.9300 | O4—H4E | 0.8499 |
C20—C21 | 1.327 (3) | O4—H4F | 0.8500 |
C20—H20 | 0.9300 | O5—H5E | 0.8501 |
C21—C22 | 1.427 (3) | O5—H5F | 0.8500 |
C21—H21 | 0.9300 | O6—H6C | 0.8500 |
C22—N7 | 1.379 (3) | O6—H6E | 0.8502 |
C23—N8 | 1.462 (3) | O7—H7F | 0.8499 |
C23—C24 | 1.544 (3) | O7—H7C | 0.8501 |
C23—H23A | 0.9700 | O8—H8D | 0.8500 |
C23—H23B | 0.9700 | O8—H8C | 0.8500 |
C24—N9 | 1.453 (3) | O9—H9F | 0.8501 |
C24—H24A | 0.9700 | O9—H9E | 0.8500 |
C24—H24B | 0.9700 | O10—H10B | 0.8501 |
C25—N9 | 1.457 (3) | O10—H10D | 0.8499 |
C25—C26 | 1.540 (3) | O11—H11B | 0.8501 |
C25—H25A | 0.9700 | O11—H11D | 0.8498 |
C25—H25B | 0.9700 | O12—H12A | 0.8500 |
C26—N10 | 1.468 (3) | O12—H12B | 0.8499 |
C26—H26A | 0.9700 | O13—H13B | 0.8501 |
C26—H26B | 0.9700 | O13—H13C | 0.8500 |
C27—N10 | 1.444 (3) | O14—H14A | 0.9235 |
C27—C28 | 1.530 (3) | O14—H14B | 0.7205 |
C27—H27A | 0.9700 | O15—H15E | 0.8500 |
C27—H27B | 0.9700 | O15—H15C | 0.8499 |
N1—C1—C2 | 110.91 (19) | N10—C27—H27A | 109.2 |
N1—C1—H1A | 109.5 | C28—C27—H27A | 109.2 |
C2—C1—H1A | 109.5 | N10—C27—H27B | 109.2 |
N1—C1—H1B | 109.5 | C28—C27—H27B | 109.2 |
C2—C1—H1B | 109.5 | H27A—C27—H27B | 107.9 |
H1A—C1—H1B | 108.0 | N8—C28—C27 | 112.04 (17) |
C1—C2—N2 | 108.62 (18) | N8—C28—H28A | 109.2 |
C1—C2—H2A | 110.0 | C27—C28—H28A | 109.2 |
N2—C2—H2A | 110.0 | N8—C28—H28B | 109.2 |
C1—C2—H2B | 110.0 | C27—C28—H28B | 109.2 |
N2—C2—H2B | 110.0 | H28A—C28—H28B | 107.9 |
H2A—C2—H2B | 108.3 | N8—C29—C30 | 115.68 (19) |
N2—C3—C4 | 107.80 (18) | N8—C29—H29A | 108.4 |
N2—C3—H3A | 110.1 | C30—C29—H29A | 108.4 |
C4—C3—H3A | 110.1 | N8—C29—H29B | 108.4 |
N2—C3—H3B | 110.1 | C30—C29—H29B | 108.4 |
C4—C3—H3B | 110.1 | H29A—C29—H29B | 107.4 |
H3A—C3—H3B | 108.5 | N11—C30—N12 | 109.9 (2) |
N3—C4—C3 | 112.38 (18) | N11—C30—C29 | 128.2 (2) |
N3—C4—H4A | 109.1 | N12—C30—C29 | 122.0 (2) |
C3—C4—H4A | 109.1 | C32—C31—C36 | 122.2 (2) |
N3—C4—H4B | 109.1 | C32—C31—N11 | 132.2 (2) |
C3—C4—H4B | 109.1 | C36—C31—N11 | 105.54 (19) |
H4A—C4—H4B | 107.9 | C33—C32—C31 | 117.1 (3) |
N3—C5—C6 | 112.28 (19) | C33—C32—H32 | 121.5 |
N3—C5—H5A | 109.1 | C31—C32—H32 | 121.5 |
C6—C5—H5A | 109.1 | C34—C33—C32 | 121.0 (2) |
N3—C5—H5B | 109.1 | C34—C33—H33 | 119.5 |
C6—C5—H5B | 109.1 | C32—C33—H33 | 119.5 |
H5A—C5—H5B | 107.9 | C33—C34—C35 | 122.5 (2) |
N1—C6—C5 | 113.58 (19) | C33—C34—H34 | 118.8 |
N1—C6—H6A | 108.8 | C35—C34—H34 | 118.8 |
C5—C6—H6A | 108.8 | C36—C35—C34 | 118.1 (3) |
N1—C6—H6B | 108.8 | C36—C35—H35 | 121.0 |
C5—C6—H6B | 108.8 | C34—C35—H35 | 121.0 |
H6A—C6—H6B | 107.7 | C35—C36—N12 | 134.5 (3) |
N1—C7—C8 | 114.3 (2) | C35—C36—C31 | 118.9 (2) |
N1—C7—H7A | 108.7 | N12—C36—C31 | 106.5 (2) |
C8—C7—H7A | 108.7 | N10—C37—C38 | 114.36 (18) |
N1—C7—H7B | 108.7 | N10—C37—H37A | 108.7 |
C8—C7—H7B | 108.7 | C38—C37—H37A | 108.7 |
H7A—C7—H7B | 107.6 | N10—C37—H37B | 108.7 |
N4—C8—N5 | 108.21 (19) | C38—C37—H37B | 108.7 |
N4—C8—C7 | 126.2 (2) | H37A—C37—H37B | 107.6 |
N5—C8—C7 | 125.5 (2) | N13—C38—N14 | 107.29 (19) |
N4—C9—C14 | 105.87 (19) | N13—C38—C37 | 129.0 (2) |
N4—C9—C10 | 133.9 (2) | N14—C38—C37 | 123.69 (19) |
C14—C9—C10 | 120.2 (2) | C44—C39—C40 | 122.2 (2) |
C11—C10—C9 | 116.2 (2) | C44—C39—N13 | 104.7 (2) |
C11—C10—H10 | 121.9 | C40—C39—N13 | 133.1 (2) |
C9—C10—H10 | 121.9 | C41—C40—C39 | 115.5 (2) |
C10—C11—C12 | 123.0 (2) | C41—C40—H40 | 122.2 |
C10—C11—H11 | 118.5 | C39—C40—H40 | 122.2 |
C12—C11—H11 | 118.5 | C40—C41—C42 | 123.9 (2) |
C11—C12—C13 | 122.3 (2) | C40—C41—H41 | 118.1 |
C11—C12—H12 | 118.9 | C42—C41—H41 | 118.1 |
C13—C12—H12 | 118.9 | C43—C42—C41 | 119.7 (2) |
C14—C13—C12 | 117.1 (2) | C43—C42—H42 | 120.2 |
C14—C13—H13 | 121.4 | C41—C42—H42 | 120.2 |
C12—C13—H13 | 121.4 | C42—C43—C44 | 117.8 (2) |
N5—C14—C13 | 133.9 (2) | C42—C43—H43 | 121.1 |
N5—C14—C9 | 105.02 (19) | C44—C43—H43 | 121.1 |
C13—C14—C9 | 121.1 (2) | N14—C44—C39 | 107.9 (2) |
N3—C15—C16 | 113.23 (18) | N14—C44—C43 | 131.2 (2) |
N3—C15—H15A | 108.9 | C39—C44—C43 | 120.9 (2) |
C16—C15—H15A | 108.9 | C6—N1—C1 | 117.51 (19) |
N3—C15—H15B | 108.9 | C6—N1—C7 | 115.74 (18) |
C16—C15—H15B | 108.9 | C1—N1—C7 | 115.06 (18) |
H15A—C15—H15B | 107.7 | C2—N2—C3 | 113.62 (18) |
N7—C16—N6 | 107.8 (2) | C2—N2—H2C | 108.7 |
N7—C16—C15 | 125.2 (2) | C3—N2—H2C | 108.7 |
N6—C16—C15 | 127.0 (2) | C4—N3—C15 | 116.64 (17) |
N6—C17—C22 | 106.3 (2) | C4—N3—C5 | 116.09 (18) |
N6—C17—C18 | 132.6 (2) | C15—N3—C5 | 115.17 (18) |
C22—C17—C18 | 121.1 (2) | C8—N4—C9 | 111.28 (19) |
C19—C18—C17 | 116.8 (2) | C8—N4—H4 | 124.4 |
C19—C18—H18 | 121.6 | C9—N4—H4 | 124.4 |
C17—C18—H18 | 121.6 | C8—N5—C14 | 109.61 (18) |
C18—C19—C20 | 121.0 (2) | C16—N6—C17 | 109.76 (19) |
C18—C19—H19 | 119.5 | C16—N7—C22 | 109.74 (19) |
C20—C19—H19 | 119.5 | C16—N7—H7 | 125.1 |
C21—C20—C19 | 125.1 (2) | C22—N7—H7 | 125.1 |
C21—C20—H20 | 117.5 | C28—N8—C29 | 115.13 (18) |
C19—C20—H20 | 117.5 | C28—N8—C23 | 116.95 (18) |
C20—C21—C22 | 114.0 (2) | C29—N8—C23 | 116.17 (18) |
C20—C21—H21 | 123.0 | C24—N9—C25 | 115.33 (19) |
C22—C21—H21 | 123.0 | C24—N9—H9A | 108.4 |
N7—C22—C17 | 106.4 (2) | C25—N9—H9A | 108.5 |
N7—C22—C21 | 131.5 (2) | C27—N10—C37 | 115.65 (17) |
C17—C22—C21 | 122.0 (2) | C27—N10—C26 | 116.09 (18) |
N8—C23—C24 | 109.60 (18) | C37—N10—C26 | 115.34 (17) |
N8—C23—H23A | 109.8 | C30—N11—C31 | 110.1 (2) |
C24—C23—H23A | 109.8 | C30—N11—H11A | 124.9 |
N8—C23—H23B | 109.8 | C31—N11—H11A | 124.9 |
C24—C23—H23B | 109.8 | C30—N12—C36 | 107.9 (2) |
H23A—C23—H23B | 108.2 | C38—N13—C39 | 112.00 (19) |
N9—C24—C23 | 109.80 (18) | C38—N13—H13A | 124.0 |
N9—C24—H24A | 109.7 | C39—N13—H13A | 124.0 |
C23—C24—H24A | 109.7 | C44—N14—C38 | 108.07 (18) |
N9—C24—H24B | 109.7 | H1D—O1—H1E | 109.5 |
C23—C24—H24B | 109.7 | H2E—O2—H2F | 109.5 |
H24A—C24—H24B | 108.2 | H3D—O3—H3E | 109.5 |
N9—C25—C26 | 112.68 (19) | H4E—O4—H4F | 109.5 |
N9—C25—H25A | 109.1 | H5E—O5—H5F | 109.5 |
C26—C25—H25A | 109.1 | H6C—O6—H6E | 109.5 |
N9—C25—H25B | 109.1 | H7F—O7—H7C | 109.5 |
C26—C25—H25B | 109.1 | H8D—O8—H8C | 109.5 |
H25A—C25—H25B | 107.8 | H9F—O9—H9E | 109.5 |
N10—C26—C25 | 109.97 (18) | H10B—O10—H10D | 109.8 |
N10—C26—H26A | 109.7 | H11B—O11—H11D | 109.5 |
C25—C26—H26A | 109.7 | H12A—O12—H12B | 109.5 |
N10—C26—H26B | 109.7 | H13B—O13—H13C | 109.5 |
C25—C26—H26B | 109.7 | H14A—O14—H14B | 110.7 |
H26A—C26—H26B | 108.2 | H15E—O15—H15C | 109.6 |
N10—C27—C28 | 112.25 (18) |
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2C···N3 | 0.90 | 2.26 | 2.772 (3) | 116 |
N7—H7···O8 | 0.86 | 2.23 | 3.082 (4) | 173 |
N9—H9A···N10 | 0.90 | 2.34 | 2.833 (2) | 114 |
N9—H9A···O14 | 0.90 | 2.58 | 3.371 (4) | 147 |
N11—H11A···O3 | 0.86 | 2.19 | 3.043 (4) | 171 |
N13—H13A···O12 | 0.86 | 1.95 | 2.774 (4) | 160 |
O5—H5E···O7 | 0.85 | 2.55 | 3.087 (5) | 122 |
O6—H6C···N14 | 0.85 | 2.29 | 2.789 (2) | 118 |
O9—H9F···N6 | 0.85 | 2.01 | 2.771 (2) | 148 |
O10—H10D···O8 | 0.85 | 2.52 | 3.171 (5) | 134 |
O11—H11D···N5 | 0.85 | 2.29 | 2.729 (2) | 113 |
O15—H15E···O6 | 0.85 | 2.21 | 3.051 (2) | 169 |
O15—H15C···N12 | 0.85 | 2.12 | 2.885 (3) | 150 |
N4—H4···O3i | 0.86 | 2.26 | 3.094 (4) | 164 |
O2—H2E···N2i | 0.85 | 2.49 | 3.033 (4) | 123 |
O6—H6E···O1ii | 0.85 | 2.41 | 3.079 (3) | 136 |
O9—H9E···O1ii | 0.85 | 2.59 | 3.168 (3) | 126 |
O11—H11B···O13iii | 0.85 | 2.36 | 3.065 (2) | 141 |
O13—H13B···O9iv | 0.85 | 2.58 | 3.2128 (19) | 133 |
O13—H13C···O12v | 0.85 | 2.33 | 3.137 (4) | 159 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y−1/2, −z+3/2; (iii) x, −y+1/2, z+1/2; (iv) −x+1, −y, −z+1; (v) x−1, y, z. |
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