Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802011558/ob6144sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802011558/ob6144Isup2.hkl |
CCDC reference: 193739
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.006 Å
- R factor = 0.056
- wR factor = 0.141
- Data-to-parameter ratio = 16.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.814 0.997 Tmin' and Tmax expected: 0.941 0.997 RR' = 0.865 Please check that your absorption correction is appropriate. General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.27 From the CIF: _reflns_number_total 8394 Count of symmetry unique reflns 5336 Completeness (_total/calc) 157.31% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3058 Fraction of Friedel pairs measured 0.573 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1998); program(s) used to solve structure: SHELXD (Sheldrick & Gould, 1996); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: RASTER3D (Merritt & Bacon, 1997); software used to prepare material for publication: PARST (Nardelli, 1995).
C41H49N7O6S·(H2O) | F(000) = 836 |
Mr = 785.95 | Dx = 1.264 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.037 (3) Å | Cell parameters from 15361 reflections |
b = 13.239 (3) Å | θ = 2.2–19.9° |
c = 14.158 (3) Å | µ = 0.14 mm−1 |
β = 113.728 (4)° | T = 100 K |
V = 2065.5 (8) Å3 | Needle, colourless |
Z = 2 | 0.45 × 0.03 × 0.03 mm |
Bruker SMART APEX CCD diffractometer | 8394 independent reflections |
Radiation source: MacScience M18XCE rotating-anode | 5679 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 8.366 pixels mm-1 | θmax = 28.3°, θmin = 1.6° |
ω scans | h = −15→12 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −17→16 |
Tmin = 0.814, Tmax = 0.997 | l = −18→18 |
13044 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.141 | w = 1/[σ2(Fo2) + (0.0509P)2 + 0.3572P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.003 |
8394 reflections | Δρmax = 0.37 e Å−3 |
513 parameters | Δρmin = −0.43 e Å−3 |
1 restraint | Absolute structure: (Flack, 1983), 3058 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (10) |
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. Data collection was performed on a CCD camera (Bruker AXS, SMART APEX). The structure was solved by a dual-space recycling method using SHELXD (Sheldrick & Gould, 1996) and refined by SHELXL97 (Sheldrick, 1997). A single peak was found in the differential Fourier map and was included in the refinement as a water molecule. 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 | ||
N_1 | 1.3544 (3) | 1.0192 (2) | 1.3187 (2) | 0.0212 (7) | |
H1_1 | 1.3733 | 0.9676 | 1.3616 | 0.025* | |
CA_1 | 1.4163 (3) | 1.0337 (3) | 1.2500 (2) | 0.0193 (8) | |
H2_1 | 1.3967 | 1.1042 | 1.2233 | 0.023* | |
CB_1 | 1.5568 (3) | 1.0300 (3) | 1.3077 (3) | 0.0252 (9) | |
H3_1 | 1.5919 | 1.0492 | 1.2572 | 0.030* | |
CG2_1 | 1.5953 (4) | 1.1110 (4) | 1.3923 (3) | 0.0342 (11) | |
H4_1 | 1.5613 | 1.1764 | 1.3619 | 0.051* | |
H5_1 | 1.6840 | 1.1155 | 1.4242 | 0.051* | |
H6_1 | 1.5651 | 1.0928 | 1.4449 | 0.051* | |
CG1_1 | 1.6101 (4) | 0.9283 (3) | 1.3530 (3) | 0.0302 (10) | |
H7_1 | 1.5642 | 0.9018 | 1.3921 | 0.036* | |
H8_1 | 1.6949 | 0.9390 | 1.4029 | 0.036* | |
CD_1 | 1.6103 (4) | 0.8483 (4) | 1.2766 (4) | 0.0390 (11) | |
H9_1 | 1.6456 | 0.7858 | 1.3136 | 0.058* | |
H10_1 | 1.6585 | 0.8719 | 1.2393 | 0.058* | |
H11_1 | 1.5268 | 0.8354 | 1.2274 | 0.058* | |
C3_2 | 1.3610 (3) | 0.9668 (3) | 1.1578 (3) | 0.0190 (8) | |
N_2 | 1.2805 (3) | 0.8993 (2) | 1.1451 (2) | 0.0206 (7) | |
CA_2 | 1.2467 (3) | 0.8599 (3) | 1.0400 (3) | 0.0189 (8) | |
H12_2 | 1.1595 | 0.8766 | 0.9984 | 0.023* | |
CB_2 | 1.3252 (4) | 0.9190 (3) | 0.9947 (3) | 0.0213 (8) | |
H13_2 | 1.3789 | 0.8716 | 0.9773 | 0.026* | |
OG1_2 | 1.3981 (2) | 0.9848 (2) | 1.08080 (19) | 0.0244 (6) | |
CG2_2 | 1.2533 (4) | 0.9847 (3) | 0.9023 (3) | 0.0301 (10) | |
H14_2 | 1.3092 | 1.0188 | 0.8779 | 0.045* | |
H15_2 | 1.2075 | 1.0353 | 0.9223 | 0.045* | |
H16_2 | 1.1970 | 0.9424 | 0.8468 | 0.045* | |
C_2 | 1.2627 (3) | 0.7469 (3) | 1.0350 (3) | 0.0221 (9) | |
O_2 | 1.2332 (3) | 0.7045 (2) | 0.9509 (2) | 0.0318 (7) | |
N_3 | 1.3107 (3) | 0.6982 (2) | 1.1262 (2) | 0.0208 (7) | |
H17_3 | 1.3320 | 0.7329 | 1.1838 | 0.025* | |
CA_3 | 1.3279 (3) | 0.5893 (3) | 1.1310 (3) | 0.0219 (9) | |
H18_3 | 1.2557 | 0.5572 | 1.0757 | 0.026* | |
CB_3 | 1.4421 (3) | 0.5594 (3) | 1.1149 (3) | 0.0243 (9) | |
H19_3 | 1.4414 | 0.5934 | 1.0524 | 0.029* | |
H20_3 | 1.5147 | 0.5828 | 1.1746 | 0.029* | |
CG_3 | 1.4504 (3) | 0.4465 (3) | 1.1033 (3) | 0.0223 (9) | |
CD1_3 | 1.5339 (4) | 0.3880 (3) | 1.1808 (3) | 0.0283 (10) | |
H21_3 | 1.5870 | 0.4193 | 1.2430 | 0.034* | |
CE1_3 | 1.5408 (4) | 0.2845 (3) | 1.1686 (3) | 0.0349 (11) | |
H22_3 | 1.5989 | 0.2458 | 1.2223 | 0.042* | |
CZ_3 | 1.4646 (4) | 0.2379 (4) | 1.0800 (4) | 0.0372 (11) | |
H23_3 | 1.4709 | 0.1672 | 1.0719 | 0.045* | |
CE2_3 | 1.3772 (4) | 0.2944 (4) | 1.0012 (4) | 0.0381 (11) | |
H24_3 | 1.3221 | 0.2621 | 0.9405 | 0.046* | |
CD2_3 | 1.3722 (4) | 0.3976 (3) | 1.0130 (3) | 0.0314 (10) | |
H25_3 | 1.3146 | 0.4363 | 0.9590 | 0.038* | |
C_3 | 1.3350 (3) | 0.5544 (3) | 1.2353 (3) | 0.0222 (8) | |
O_3 | 1.4137 (2) | 0.5903 (2) | 1.31432 (19) | 0.0281 (7) | |
N_4 | 1.2556 (3) | 0.4842 (2) | 1.2384 (2) | 0.0201 (7) | |
CA_4 | 1.1467 (3) | 0.4499 (3) | 1.1495 (3) | 0.0205 (8) | |
H26_4 | 1.1702 | 0.4141 | 1.0981 | 0.025* | |
CB_4 | 1.0886 (4) | 0.3759 (3) | 1.2002 (3) | 0.0263 (9) | |
H27_4 | 0.9994 | 0.3733 | 1.1615 | 0.032* | |
H28_4 | 1.1221 | 0.3070 | 1.2038 | 0.032* | |
CG_4 | 1.1223 (4) | 0.4198 (3) | 1.3085 (3) | 0.0291 (10) | |
H29_4 | 1.0692 | 0.4773 | 1.3071 | 0.035* | |
H30_4 | 1.1172 | 0.3678 | 1.3569 | 0.035* | |
CD_4 | 1.2525 (4) | 0.4540 (4) | 1.3377 (3) | 0.0314 (10) | |
H31_4 | 1.2728 | 0.5117 | 1.3863 | 0.038* | |
H32_4 | 1.3101 | 0.3982 | 1.3699 | 0.038* | |
C3_5 | 1.0659 (3) | 0.5395 (3) | 1.1000 (3) | 0.0180 (8) | |
N_5 | 1.0649 (3) | 0.6206 (2) | 1.1513 (2) | 0.0200 (7) | |
CA_5 | 0.9871 (3) | 0.6926 (3) | 1.0881 (3) | 0.0193 (8) | |
CB_5 | 0.9285 (3) | 0.6641 (3) | 0.9874 (3) | 0.0208 (8) | |
H33_5 | 0.8709 | 0.7043 | 0.9348 | 0.025* | |
SG_5 | 0.97326 (9) | 0.54599 (7) | 0.96903 (7) | 0.0211 (2) | |
C_5 | 0.9775 (3) | 0.7929 (3) | 1.1296 (3) | 0.0196 (8) | |
O_5 | 0.9156 (2) | 0.8611 (2) | 1.07613 (19) | 0.0256 (6) | |
N_6 | 1.0440 (3) | 0.8014 (2) | 1.2318 (2) | 0.0209 (7) | |
H34_6 | 1.0845 | 0.7484 | 1.2661 | 0.025* | |
CA_6 | 1.0509 (3) | 0.8945 (3) | 1.2868 (3) | 0.0197 (8) | |
H35_6 | 1.0633 | 0.9530 | 1.2473 | 0.024* | |
CB_6 | 0.9316 (4) | 0.9087 (3) | 1.3048 (3) | 0.0246 (9) | |
H36_6 | 0.8609 | 0.8937 | 1.2397 | 0.029* | |
H37_6 | 0.9312 | 0.8597 | 1.3574 | 0.029* | |
CG_6 | 0.9184 (3) | 1.0132 (3) | 1.3395 (3) | 0.0237 (9) | |
CD1_6 | 0.9493 (3) | 1.0364 (3) | 1.4424 (3) | 0.0262 (9) | |
H38_6 | 0.9740 | 0.9838 | 1.4923 | 0.031* | |
CE1_6 | 0.9449 (4) | 1.1347 (3) | 1.4739 (3) | 0.0309 (10) | |
H39_6 | 0.9659 | 1.1490 | 1.5448 | 0.037* | |
CZ_6 | 0.9098 (4) | 1.2120 (4) | 1.4024 (3) | 0.0331 (10) | |
H40_6 | 0.9079 | 1.2796 | 1.4240 | 0.040* | |
CE2_6 | 0.8775 (4) | 1.1904 (3) | 1.2987 (3) | 0.0302 (10) | |
H41_6 | 0.8532 | 1.2433 | 1.2492 | 0.036* | |
CD2_6 | 0.8808 (4) | 1.0913 (3) | 1.2676 (3) | 0.0276 (10) | |
H42_6 | 0.8571 | 1.0767 | 1.1964 | 0.033* | |
C_6 | 1.1589 (3) | 0.8842 (3) | 1.3914 (3) | 0.0197 (8) | |
O_6 | 1.1813 (2) | 0.8006 (2) | 1.43262 (19) | 0.0244 (6) | |
N_7 | 1.2239 (3) | 0.9667 (2) | 1.4356 (2) | 0.0197 (7) | |
CA_7 | 1.2105 (3) | 1.0695 (3) | 1.3926 (3) | 0.0220 (9) | |
H43_7 | 1.1226 | 1.0881 | 1.3598 | 0.026* | |
CB_7 | 1.2765 (4) | 1.1365 (3) | 1.4889 (3) | 0.0294 (10) | |
H44_7 | 1.3564 | 1.1588 | 1.4919 | 0.035* | |
H45_7 | 1.2274 | 1.1969 | 1.4875 | 0.035* | |
CG_7 | 1.2920 (4) | 1.0699 (3) | 1.5804 (3) | 0.0287 (10) | |
H46_7 | 1.2190 | 1.0723 | 1.5961 | 0.034* | |
H47_7 | 1.3635 | 1.0908 | 1.6424 | 0.034* | |
CD_7 | 1.3099 (4) | 0.9650 (3) | 1.5450 (3) | 0.0272 (10) | |
H48_7 | 1.3944 | 0.9548 | 1.5521 | 0.033* | |
H49_7 | 1.2886 | 0.9116 | 1.5839 | 0.033* | |
C_7 | 1.2682 (3) | 1.0849 (3) | 1.3165 (3) | 0.0222 (9) | |
O_7 | 1.2399 (3) | 1.1594 (2) | 1.2606 (2) | 0.0333 (7) | |
O_8 | 1.4041 (3) | 0.7863 (3) | 1.4053 (3) | 0.0465 (9) | |
H50_8 | 1.432 (6) | 0.716 (5) | 1.381 (5) | 0.10 (2)* | |
H51_8 | 1.317 (8) | 0.785 (7) | 1.421 (6) | 0.16 (3)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
N_1 | 0.0217 (17) | 0.0230 (19) | 0.0155 (16) | 0.0004 (13) | 0.0039 (13) | −0.0002 (13) |
CA_1 | 0.0217 (19) | 0.019 (2) | 0.0149 (17) | 0.0017 (16) | 0.0054 (15) | 0.0008 (16) |
CB_1 | 0.020 (2) | 0.034 (3) | 0.0179 (18) | −0.0028 (18) | 0.0033 (16) | −0.0011 (18) |
CG2_1 | 0.030 (2) | 0.045 (3) | 0.023 (2) | −0.012 (2) | 0.0057 (19) | −0.002 (2) |
CG1_1 | 0.022 (2) | 0.035 (2) | 0.030 (2) | 0.0009 (19) | 0.0064 (19) | 0.0080 (19) |
CD_1 | 0.029 (2) | 0.034 (3) | 0.045 (3) | 0.007 (2) | 0.006 (2) | 0.005 (2) |
C3_2 | 0.0159 (19) | 0.024 (2) | 0.0138 (18) | 0.0053 (16) | 0.0021 (15) | 0.0043 (16) |
N_2 | 0.0199 (17) | 0.0223 (18) | 0.0161 (15) | 0.0026 (14) | 0.0038 (13) | 0.0014 (13) |
CA_2 | 0.0152 (19) | 0.021 (2) | 0.0161 (19) | 0.0049 (16) | 0.0022 (15) | 0.0024 (16) |
CB_2 | 0.022 (2) | 0.022 (2) | 0.0158 (18) | 0.0020 (16) | 0.0029 (16) | −0.0017 (16) |
OG1_2 | 0.0290 (15) | 0.0261 (15) | 0.0196 (14) | −0.0061 (12) | 0.0114 (12) | −0.0033 (12) |
CG2_2 | 0.026 (2) | 0.043 (3) | 0.018 (2) | 0.0064 (19) | 0.0045 (17) | 0.0059 (19) |
C_2 | 0.0135 (19) | 0.030 (2) | 0.018 (2) | −0.0022 (17) | 0.0008 (16) | −0.0022 (17) |
O_2 | 0.0417 (18) | 0.0282 (16) | 0.0188 (15) | −0.0028 (14) | 0.0054 (13) | −0.0032 (13) |
N_3 | 0.0203 (17) | 0.0234 (18) | 0.0155 (16) | 0.0021 (14) | 0.0039 (14) | −0.0013 (13) |
CA_3 | 0.0168 (19) | 0.027 (2) | 0.0168 (19) | −0.0018 (16) | 0.0011 (16) | −0.0010 (16) |
CB_3 | 0.0207 (19) | 0.026 (2) | 0.0253 (19) | −0.0033 (18) | 0.0084 (16) | −0.0021 (18) |
CG_3 | 0.022 (2) | 0.026 (2) | 0.022 (2) | −0.0008 (17) | 0.0120 (17) | −0.0012 (17) |
CD1_3 | 0.032 (2) | 0.031 (3) | 0.020 (2) | 0.0044 (19) | 0.0079 (18) | 0.0014 (18) |
CE1_3 | 0.044 (3) | 0.033 (3) | 0.035 (2) | 0.009 (2) | 0.023 (2) | 0.010 (2) |
CZ_3 | 0.044 (3) | 0.026 (2) | 0.054 (3) | −0.001 (2) | 0.033 (3) | 0.000 (2) |
CE2_3 | 0.026 (3) | 0.036 (3) | 0.052 (3) | −0.012 (2) | 0.015 (2) | −0.018 (2) |
CD2_3 | 0.023 (2) | 0.036 (3) | 0.029 (2) | −0.0001 (19) | 0.0034 (18) | −0.005 (2) |
C_3 | 0.0212 (19) | 0.023 (2) | 0.0209 (19) | 0.0024 (18) | 0.0068 (16) | −0.0010 (17) |
O_3 | 0.0218 (15) | 0.0351 (17) | 0.0185 (14) | −0.0049 (12) | −0.0013 (12) | −0.0053 (12) |
N_4 | 0.0188 (16) | 0.0221 (17) | 0.0128 (15) | 0.0003 (13) | −0.0006 (13) | 0.0018 (13) |
CA_4 | 0.0163 (19) | 0.020 (2) | 0.0193 (19) | −0.0005 (15) | 0.0007 (15) | −0.0033 (16) |
CB_4 | 0.025 (2) | 0.024 (2) | 0.024 (2) | −0.0013 (17) | 0.0039 (17) | 0.0014 (17) |
CG_4 | 0.031 (2) | 0.030 (2) | 0.023 (2) | −0.0053 (19) | 0.0066 (18) | 0.0010 (18) |
CD_4 | 0.028 (2) | 0.044 (3) | 0.017 (2) | −0.005 (2) | 0.0051 (17) | 0.0038 (19) |
C3_5 | 0.0155 (17) | 0.018 (2) | 0.0162 (17) | −0.0012 (16) | 0.0023 (14) | 0.0017 (17) |
N_5 | 0.0179 (16) | 0.0182 (17) | 0.0170 (16) | −0.0009 (13) | −0.0002 (13) | −0.0001 (13) |
CA_5 | 0.0170 (19) | 0.018 (2) | 0.0180 (19) | −0.0033 (16) | 0.0024 (15) | −0.0014 (16) |
CB_5 | 0.0185 (19) | 0.022 (2) | 0.0162 (19) | −0.0027 (16) | 0.0010 (15) | 0.0029 (16) |
SG_5 | 0.0210 (5) | 0.0212 (5) | 0.0138 (4) | −0.0015 (4) | −0.0005 (4) | −0.0011 (4) |
C_5 | 0.0158 (19) | 0.021 (2) | 0.0187 (18) | −0.0020 (16) | 0.0030 (16) | 0.0018 (16) |
O_5 | 0.0247 (15) | 0.0214 (15) | 0.0189 (14) | 0.0031 (12) | −0.0034 (12) | 0.0039 (12) |
N_6 | 0.0228 (18) | 0.0195 (17) | 0.0115 (15) | 0.0023 (14) | −0.0025 (13) | 0.0004 (13) |
CA_6 | 0.0139 (19) | 0.023 (2) | 0.0158 (18) | −0.0011 (16) | −0.0005 (15) | −0.0017 (16) |
CB_6 | 0.020 (2) | 0.026 (2) | 0.024 (2) | −0.0023 (17) | 0.0045 (17) | −0.0005 (17) |
CG_6 | 0.0095 (18) | 0.032 (2) | 0.026 (2) | 0.0017 (16) | 0.0043 (16) | −0.0019 (17) |
CD1_6 | 0.022 (2) | 0.036 (3) | 0.0198 (19) | 0.0048 (19) | 0.0076 (16) | 0.0020 (19) |
CE1_6 | 0.025 (2) | 0.047 (3) | 0.021 (2) | 0.006 (2) | 0.0097 (18) | −0.003 (2) |
CZ_6 | 0.031 (2) | 0.035 (3) | 0.034 (2) | 0.004 (2) | 0.014 (2) | −0.009 (2) |
CE2_6 | 0.027 (2) | 0.033 (3) | 0.028 (2) | 0.0097 (19) | 0.0083 (19) | 0.0023 (19) |
CD2_6 | 0.018 (2) | 0.037 (3) | 0.022 (2) | 0.0025 (18) | 0.0025 (17) | −0.0023 (19) |
C_6 | 0.0151 (19) | 0.027 (2) | 0.0156 (18) | 0.0032 (16) | 0.0045 (15) | 0.0027 (17) |
O_6 | 0.0244 (15) | 0.0259 (16) | 0.0169 (13) | 0.0010 (12) | 0.0020 (12) | 0.0036 (12) |
N_7 | 0.0163 (16) | 0.0226 (18) | 0.0126 (15) | −0.0001 (13) | −0.0023 (13) | 0.0001 (13) |
CA_7 | 0.0159 (18) | 0.026 (2) | 0.0183 (19) | 0.0008 (16) | 0.0009 (15) | 0.0009 (16) |
CB_7 | 0.024 (2) | 0.035 (3) | 0.022 (2) | −0.0008 (19) | 0.0016 (17) | −0.0066 (18) |
CG_7 | 0.022 (2) | 0.042 (3) | 0.0151 (19) | −0.0034 (19) | −0.0005 (16) | −0.0048 (18) |
CD_7 | 0.025 (2) | 0.035 (3) | 0.0137 (19) | −0.0042 (19) | −0.0002 (16) | −0.0016 (17) |
C_7 | 0.019 (2) | 0.023 (2) | 0.0178 (19) | 0.0048 (17) | 0.0006 (16) | −0.0007 (17) |
O_7 | 0.0339 (17) | 0.0353 (18) | 0.0318 (16) | 0.0124 (14) | 0.0142 (14) | 0.0137 (14) |
O_8 | 0.044 (2) | 0.042 (2) | 0.055 (2) | 0.0048 (17) | 0.0214 (18) | 0.0074 (17) |
N_1—C_7 | 1.344 (5) | CA_4—CB_4 | 1.539 (5) |
N_1—CA_1 | 1.457 (5) | CB_4—CG_4 | 1.534 (5) |
CA_1—C3_2 | 1.494 (5) | CG_4—CD_4 | 1.520 (6) |
CA_1—CB_1 | 1.555 (5) | C3_5—N_5 | 1.299 (5) |
CB_1—CG1_1 | 1.518 (6) | C3_5—SG_5 | 1.739 (3) |
CB_1—CG2_1 | 1.534 (6) | N_5—CA_5 | 1.382 (5) |
CG1_1—CD_1 | 1.515 (6) | CA_5—CB_5 | 1.365 (5) |
C3_2—N_2 | 1.276 (5) | CA_5—C_5 | 1.476 (5) |
C3_2—OG1_2 | 1.355 (4) | CB_5—SG_5 | 1.707 (4) |
N_2—CA_2 | 1.472 (5) | C_5—O_5 | 1.221 (4) |
CA_2—C_2 | 1.514 (5) | C_5—N_6 | 1.347 (4) |
CA_2—CB_2 | 1.550 (5) | N_6—CA_6 | 1.442 (5) |
CB_2—OG1_2 | 1.467 (4) | CA_6—C_6 | 1.534 (5) |
CB_2—CG2_2 | 1.519 (5) | CA_6—CB_6 | 1.568 (5) |
C_2—O_2 | 1.232 (4) | CB_6—CG_6 | 1.497 (6) |
C_2—N_3 | 1.347 (5) | CG_6—CD1_6 | 1.385 (5) |
N_3—CA_3 | 1.454 (5) | CG_6—CD2_6 | 1.393 (5) |
CA_3—C_3 | 1.517 (5) | CD1_6—CE1_6 | 1.383 (6) |
CA_3—CB_3 | 1.533 (5) | CE1_6—CZ_6 | 1.381 (6) |
CB_3—CG_3 | 1.511 (6) | CZ_6—CE2_6 | 1.388 (6) |
CG_3—CD1_3 | 1.388 (5) | CE2_6—CD2_6 | 1.389 (6) |
CG_3—CD2_3 | 1.403 (5) | C_6—O_6 | 1.229 (4) |
CD1_3—CE1_3 | 1.388 (6) | C_6—N_7 | 1.344 (5) |
CE1_3—CZ_3 | 1.367 (6) | N_7—CA_7 | 1.472 (5) |
CZ_3—CE2_3 | 1.402 (7) | N_7—CD_7 | 1.476 (4) |
CE2_3—CD2_3 | 1.381 (6) | CA_7—C_7 | 1.513 (5) |
C_3—O_3 | 1.233 (4) | CA_7—CB_7 | 1.551 (5) |
C_3—N_4 | 1.346 (5) | CB_7—CG_7 | 1.515 (6) |
N_4—CA_4 | 1.476 (4) | CG_7—CD_7 | 1.521 (6) |
N_4—CD_4 | 1.477 (5) | C_7—O_7 | 1.224 (4) |
CA_4—C3_5 | 1.516 (5) | ||
C_7—N_1—CA_1 | 119.7 (3) | CG_4—CB_4—CA_4 | 103.7 (3) |
N_1—CA_1—C3_2 | 109.7 (3) | CD_4—CG_4—CB_4 | 102.4 (3) |
N_1—CA_1—CB_1 | 112.7 (3) | N_4—CD_4—CG_4 | 103.9 (3) |
C3_2—CA_1—CB_1 | 116.7 (3) | N_5—C3_5—CA_4 | 122.5 (3) |
CG1_1—CB_1—CG2_1 | 110.3 (3) | N_5—C3_5—SG_5 | 114.2 (3) |
CG1_1—CB_1—CA_1 | 115.8 (3) | CA_4—C3_5—SG_5 | 123.3 (3) |
CG2_1—CB_1—CA_1 | 108.2 (3) | C3_5—N_5—CA_5 | 111.3 (3) |
CB_1—CG1_1—CD_1 | 116.1 (3) | CB_5—CA_5—N_5 | 114.7 (3) |
N_2—C3_2—OG1_2 | 119.1 (3) | CB_5—CA_5—C_5 | 125.1 (3) |
N_2—C3_2—CA_1 | 125.8 (3) | N_5—CA_5—C_5 | 120.2 (3) |
OG1_2—C3_2—CA_1 | 115.1 (3) | CA_5—CB_5—SG_5 | 110.5 (3) |
C3_2—N_2—CA_2 | 106.0 (3) | CB_5—SG_5—C3_5 | 89.39 (18) |
N_2—CA_2—C_2 | 114.1 (3) | O_5—C_5—N_6 | 123.7 (4) |
N_2—CA_2—CB_2 | 105.8 (3) | O_5—C_5—CA_5 | 123.0 (3) |
C_2—CA_2—CB_2 | 111.7 (3) | N_6—C_5—CA_5 | 113.3 (3) |
OG1_2—CB_2—CG2_2 | 108.6 (3) | C_5—N_6—CA_6 | 122.1 (3) |
OG1_2—CB_2—CA_2 | 102.5 (3) | N_6—CA_6—C_6 | 106.7 (3) |
CG2_2—CB_2—CA_2 | 114.5 (3) | N_6—CA_6—CB_6 | 109.4 (3) |
C3_2—OG1_2—CB_2 | 106.5 (3) | C_6—CA_6—CB_6 | 109.2 (3) |
O_2—C_2—N_3 | 123.6 (4) | CG_6—CB_6—CA_6 | 113.0 (3) |
O_2—C_2—CA_2 | 120.1 (3) | CD1_6—CG_6—CD2_6 | 118.3 (4) |
N_3—C_2—CA_2 | 116.2 (3) | CD1_6—CG_6—CB_6 | 122.1 (4) |
C_2—N_3—CA_3 | 121.1 (3) | CD2_6—CG_6—CB_6 | 119.5 (3) |
N_3—CA_3—C_3 | 107.4 (3) | CE1_6—CD1_6—CG_6 | 121.3 (4) |
N_3—CA_3—CB_3 | 111.6 (3) | CZ_6—CE1_6—CD1_6 | 120.0 (4) |
C_3—CA_3—CB_3 | 111.3 (3) | CE1_6—CZ_6—CE2_6 | 119.7 (4) |
CG_3—CB_3—CA_3 | 112.0 (3) | CD2_6—CE2_6—CZ_6 | 119.9 (4) |
CD1_3—CG_3—CD2_3 | 118.0 (4) | CE2_6—CD2_6—CG_6 | 120.8 (4) |
CD1_3—CG_3—CB_3 | 121.6 (4) | O_6—C_6—N_7 | 122.4 (3) |
CD2_3—CG_3—CB_3 | 120.4 (4) | O_6—C_6—CA_6 | 118.5 (3) |
CE1_3—CD1_3—CG_3 | 120.9 (4) | N_7—C_6—CA_6 | 119.1 (3) |
CZ_3—CE1_3—CD1_3 | 120.5 (4) | C_6—N_7—CA_7 | 127.8 (3) |
CE1_3—CZ_3—CE2_3 | 120.1 (5) | C_6—N_7—CD_7 | 120.4 (3) |
CD2_3—CE2_3—CZ_3 | 119.1 (4) | CA_7—N_7—CD_7 | 111.3 (3) |
CE2_3—CD2_3—CG_3 | 121.4 (4) | N_7—CA_7—C_7 | 114.5 (3) |
O_3—C_3—N_4 | 122.2 (3) | N_7—CA_7—CB_7 | 103.5 (3) |
O_3—C_3—CA_3 | 119.2 (3) | C_7—CA_7—CB_7 | 109.2 (3) |
N_4—C_3—CA_3 | 118.6 (3) | CG_7—CB_7—CA_7 | 105.2 (3) |
C_3—N_4—CA_4 | 125.7 (3) | CB_7—CG_7—CD_7 | 103.6 (3) |
C_3—N_4—CD_4 | 120.5 (3) | N_7—CD_7—CG_7 | 101.5 (3) |
CA_4—N_4—CD_4 | 112.0 (3) | O_7—C_7—N_1 | 123.2 (4) |
N_4—CA_4—C3_5 | 109.8 (3) | O_7—C_7—CA_7 | 118.8 (3) |
N_4—CA_4—CB_4 | 102.3 (3) | N_1—C_7—CA_7 | 117.8 (3) |
C3_5—CA_4—CB_4 | 112.7 (3) | ||
C_7—N_1—Ca_1—Cb_1 | 129.3 (4) | N_4—Ca_4—Cb_4—Cg_4 | 31.9 (4) |
C_7—N_1—Ca_1—C3_2 | −99.0 (4) | C3_5—Ca_4—Cb_4—Cg_4 | −85.9 (4) |
Ca_1—N_1—C_7—Ca_7 | −177.2 (3) | N_4—Ca_4—C3_5—N_5 | −27.0 (5) |
Ca_1—N_1—C_7—O_7 | −1.9 (6) | N_4—Ca_4—C3_5—Sg_5 | 149.3 (3) |
N_1—Ca_1—Cb_1—Cg2_1 | −57.2 (4) | Cb_4—Ca_4—C3_5—N_5 | 86.3 (5) |
N_1—Ca_1—Cb_1—Cg1_1 | 67.0 (4) | Cb_4—Ca_4—C3_5—Sg_5 | −97.4 (4) |
C3_2—Ca_1—Cb_1—Cg2_1 | 174.5 (3) | Ca_4—Cb_4—Cg_4—Cd_4 | −40.1 (4) |
C3_2—Ca_1—Cb_1—Cg1_1 | −61.2 (5) | Cb_4—Cg_4—Cd_4—N_4 | 32.2 (4) |
N_1—Ca_1—C3_2—N_2 | −6.8 (5) | Ca_4—C3_5—N_5—Ca_5 | 177.8 (4) |
N_1—Ca_1—C3_2—Og1_2 | 170.2 (3) | Sg_5—C3_5—N_5—Ca_5 | 1.2 (4) |
Cb_1—Ca_1—C3_2—N_2 | 122.8 (4) | Ca_4—C3_5—Sg_5—Cb_5 | −178.3 (4) |
Cb_1—Ca_1—C3_2—Og1_2 | −60.2 (4) | N_5—C3_5—Sg_5—Cb_5 | −1.7 (3) |
Ca_1—Cb_1—Cg1_1—Cd_1 | 73.4 (5) | C3_5—N_5—Ca_5—Cb_5 | 0.2 (5) |
Cg2_1—Cb_1—Cg1_1—Cd_1 | −163.4 (4) | C3_5—N_5—Ca_5—C_5 | −176.5 (4) |
Ca_1—C3_2—N_2—Ca_2 | 175.1 (4) | N_5—Ca_5—Cb_5—Sg_5 | −1.5 (5) |
Og1_2—C3_2—N_2—Ca_2 | −1.8 (5) | C_5—Ca_5—Cb_5—Sg_5 | 175.0 (3) |
Ca_1—C3_2—Og1_2—Cb_2 | −174.5 (3) | N_5—Ca_5—C_5—O_5 | 175.8 (4) |
N_2—C3_2—Og1_2—Cb_2 | 2.7 (5) | N_5—Ca_5—C_5—N_6 | −4.0 (5) |
C3_2—N_2—Ca_2—Cb_2 | 0.1 (4) | Cb_5—Ca_5—C_5—O_5 | −0.6 (6) |
C3_2—N_2—Ca_2—C_2 | 123.3 (4) | Cb_5—Ca_5—C_5—N_6 | 179.6 (4) |
N_2—Ca_2—Cb_2—Og1_2 | 1.3 (4) | Ca_5—Cb_5—Sg_5—C3_5 | 1.8 (3) |
N_2—Ca_2—Cb_2—Cg2_2 | −116.1 (4) | Ca_5—C_5—N_6—Ca_6 | 177.6 (3) |
C_2—Ca_2—Cb_2—Og1_2 | −123.5 (3) | O_5—C_5—N_6—Ca_6 | −2.2 (6) |
C_2—Ca_2—Cb_2—Cg2_2 | 119.2 (4) | C_5—N_6—Ca_6—Cb_6 | 77.0 (4) |
N_2—Ca_2—C_2—O_2 | 177.3 (4) | C_5—N_6—Ca_6—C_6 | −164.9 (3) |
N_2—Ca_2—C_2—N_3 | −3.1 (5) | N_6—Ca_6—Cb_6—Cg_6 | −166.9 (3) |
Cb_2—Ca_2—C_2—O_2 | −62.7 (5) | C_6—Ca_6—Cb_6—Cg_6 | 76.6 (4) |
Cb_2—Ca_2—C_2—N_3 | 116.9 (4) | N_6—Ca_6—C_6—O_6 | −34.2 (5) |
Ca_2—Cb_2—Og1_2—C3_2 | −2.1 (4) | N_6—Ca_6—C_6—N_7 | 147.1 (3) |
Cg2_2—Cb_2—Og1_2—C3_2 | 119.3 (4) | Cb_6—Ca_6—C_6—O_6 | 84.0 (4) |
Ca_2—C_2—N_3—Ca_3 | 178.6 (3) | Cb_6—Ca_6—C_6—N_7 | −94.6 (4) |
O_2—C_2—N_3—Ca_3 | −1.8 (6) | Ca_6—Cb_6—Cg_6—Cd1_6 | −98.5 (5) |
C_2—N_3—Ca_3—Cb_3 | 79.5 (4) | Ca_6—Cb_6—Cg_6—Cd2_6 | 77.6 (5) |
C_2—N_3—Ca_3—C_3 | −158.2 (3) | Cb_6—Cg_6—Cd1_6—Ce1_6 | 175.2 (4) |
N_3—Ca_3—Cb_3—Cg_3 | −171.2 (3) | Cd2_6—Cg_6—Cd1_6—Ce1_6 | −0.9 (6) |
C_3—Ca_3—Cb_3—Cg_3 | 68.8 (4) | Cb_6—Cg_6—Cd2_6—Ce2_6 | −174.6 (4) |
N_3—Ca_3—C_3—O_3 | −57.9 (5) | Cd1_6—Cg_6—Cd2_6—Ce2_6 | 1.7 (6) |
N_3—Ca_3—C_3—N_4 | 122.8 (4) | Cg_6—Cd1_6—Ce1_6—Cz_6 | −0.3 (7) |
Cb_3—Ca_3—C_3—O_3 | 64.5 (5) | Cd1_6—Ce1_6—Cz_6—Ce2_6 | 0.8 (7) |
Cb_3—Ca_3—C_3—N_4 | −114.8 (4) | Ce1_6—Cz_6—Ce2_6—Cd2_6 | −0.1 (7) |
Ca_3—Cb_3—Cg_3—Cd1_3 | −107.5 (4) | Cz_6—Ce2_6—Cd2_6—Cg_6 | −1.2 (7) |
Ca_3—Cb_3—Cg_3—Cd2_3 | 72.0 (5) | Ca_6—C_6—N_7—Ca_7 | −4.6 (6) |
Cb_3—Cg_3—Cd1_3—Ce1_3 | −179.6 (4) | Ca_6—C_6—N_7—Cd_7 | 166.3 (3) |
Cd2_3—Cg_3—Cd1_3—Ce1_3 | 0.9 (6) | O_6—C_6—N_7—Ca_7 | 176.8 (4) |
Cb_3—Cg_3—Cd2_3—Ce2_3 | −179.2 (4) | O_6—C_6—N_7—Cd_7 | −12.3 (6) |
Cd1_3—Cg_3—Cd2_3—Ce2_3 | 0.3 (6) | C_6—N_7—Ca_7—Cb_7 | 161.4 (4) |
Cg_3—Cd1_3—Ce1_3—Cz_3 | −0.5 (7) | C_6—N_7—Ca_7—C_7 | −79.8 (5) |
Cd1_3—Ce1_3—Cz_3—Ce2_3 | −1.1 (7) | Cd_7—N_7—Ca_7—Cb_7 | −10.2 (4) |
Ce1_3—Cz_3—Ce2_3—Cd2_3 | 2.2 (8) | Cd_7—N_7—Ca_7—C_7 | 108.6 (4) |
Cz_3—Ce2_3—Cd2_3—Cg_3 | −1.8 (7) | C_6—N_7—Cd_7—Cg_7 | −141.6 (4) |
Ca_3—C_3—N_4—Ca_4 | −11.6 (6) | Ca_7—N_7—Cd_7—Cg_7 | 30.7 (4) |
Ca_3—C_3—N_4—Cd_4 | −175.0 (4) | N_7—Ca_7—Cb_7—Cg_7 | −14.8 (4) |
O_3—C_3—N_4—Ca_4 | 169.1 (4) | C_7—Ca_7—Cb_7—Cg_7 | −137.1 (4) |
O_3—C_3—N_4—Cd_4 | 5.7 (6) | N_7—Ca_7—C_7—N_1 | −20.1 (5) |
C_3—N_4—Ca_4—Cb_4 | −176.5 (4) | N_7—Ca_7—C_7—O_7 | 164.3 (4) |
C_3—N_4—Ca_4—C3_5 | −56.7 (5) | Cb_7—Ca_7—C_7—N_1 | 95.4 (4) |
Cd_4—N_4—Ca_4—Cb_4 | −12.0 (4) | Cb_7—Ca_7—C_7—O_7 | −80.2 (5) |
Cd_4—N_4—Ca_4—C3_5 | 107.9 (4) | Ca_7—Cb_7—Cg_7—Cd_7 | 33.4 (4) |
C_3—N_4—Cd_4—Cg_4 | 152.6 (4) | Cb_7—Cg_7—Cd_7—N_7 | −38.5 (4) |
Ca_4—N_4—Cd_4—Cg_4 | −12.8 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O_8—H50_8···O_3 | 1.09 (7) | 1.88 (7) | 2.920 (5) | 158 (5) |
O_8—H51_8···O_6 | 1.16 (11) | 1.72 (11) | 2.866 (5) | 171 (8) |
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