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
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) |