# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[3]rotaxane_9 _database_code_depnum_ccdc_archive 'CCDC 922154' #TrackingRef '[3]rotaxanes_updated.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H40 N4 O4, 2(C32 H28 N4 O4), 3.5(C2 H6 O)' _chemical_formula_sum 'C110 H117 N12 O15.50' _chemical_formula_weight 1855.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8101(6) _cell_length_b 21.2231(13) _cell_length_c 22.7870(16) _cell_angle_alpha 110.488(8) _cell_angle_beta 97.325(7) _cell_angle_gamma 97.504(7) _cell_volume 4770.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21641 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.4 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1970 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9828 _exptl_absorpt_correction_T_max 0.9983 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_source_power 2.5 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Mitegen _diffrn_detector CCD _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33613 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 16656 _reflns_number_gt 9224 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the crystal structure the two phenyl rings and one uncoordinated ethanol are disordered. Number of geometrical constraints (DFIX/DANG/AFIX 66) was used to preserve reasonable molecular geometry. Additionally, similarity constraints on displacement parameters such as SIMU/DELU as well as EADP and ISOR were applied. All non-hydrogen atoms are refined as anisotropic. One ethanol molecule highly disordered over centre of inversion has been refined as isotropic only. This led structure refinement to satisfactory convergence. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(0.26(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+2.8765*P+(0.0991P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16656 _refine_ls_number_parameters 1316 _refine_ls_number_restraints 405 _refine_ls_R_factor_all 0.1513 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9475(4) 0.3428(2) 0.5759(2) 0.0438(12) Uani 1 1 d . . . H1A H 0.9769 0.3917 0.5838 0.053 Uiso 1 1 calc R A 1 H1B H 1.0113 0.3287 0.6016 0.053 Uiso 1 1 calc R A 1 C8 C 0.8922(5) 0.3316(3) 0.4627(2) 0.0585(14) Uani 1 1 d DU . . H8A H 0.8447 0.3676 0.4832 0.070 Uiso 1 1 calc R B 1 H8B H 0.8333 0.2957 0.4258 0.070 Uiso 1 1 calc R B 1 C2A C 0.8208(8) 0.3342(6) 0.5972(4) 0.045(3) Uani 0.642(5) 1 d PGU C 1 C3A C 0.7683(8) 0.3922(5) 0.6223(4) 0.080(4) Uani 0.642(5) 1 d PGU C 1 H3A H 0.8100 0.4354 0.6244 0.097 Uiso 0.642(5) 1 calc PR C 1 C4A C 0.6546(9) 0.3868(4) 0.6443(4) 0.102(4) Uani 0.642(5) 1 d PGU C 1 H4A H 0.6188 0.4264 0.6614 0.122 Uiso 0.642(5) 1 calc PR C 1 C5A C 0.5935(9) 0.3236(5) 0.6412(4) 0.075(3) Uani 0.642(5) 1 d PGU C 1 H5A H 0.5159 0.3200 0.6562 0.090 Uiso 0.642(5) 1 calc PR C 1 C6A C 0.6460(12) 0.2657(4) 0.6161(5) 0.0586(16) Uani 0.642(5) 1 d PGU C 1 H6A H 0.6042 0.2225 0.6140 0.070 Uiso 0.642(5) 1 calc PR C 1 C7A C 0.7596(12) 0.2710(5) 0.5941(5) 0.046(2) Uani 0.642(5) 1 d PGU C 1 H7A H 0.7955 0.2314 0.5770 0.056 Uiso 0.642(5) 1 calc PR C 1 C2B C 0.8192(16) 0.3411(12) 0.5946(9) 0.050(5) Uani 0.358(5) 1 d PGU C 2 C3B C 0.7441(15) 0.3886(10) 0.5916(6) 0.063(4) Uani 0.358(5) 1 d PGU C 2 H3B H 0.7772 0.4269 0.5821 0.076 Uiso 0.358(5) 1 calc PR C 2 C4B C 0.6204(15) 0.3801(9) 0.6023(6) 0.069(4) Uani 0.358(5) 1 d PGU C 2 H4B H 0.5690 0.4125 0.6002 0.083 Uiso 0.358(5) 1 calc PR C 2 C5B C 0.5718(16) 0.3240(10) 0.6161(7) 0.074(5) Uani 0.358(5) 1 d PGU C 2 H5B H 0.4873 0.3181 0.6235 0.089 Uiso 0.358(5) 1 calc PR C 2 C6B C 0.647(2) 0.2765(9) 0.6192(10) 0.0586(16) Uani 0.358(5) 1 d PGU C 2 H6B H 0.6139 0.2381 0.6287 0.070 Uiso 0.358(5) 1 calc PR C 2 C7B C 0.771(2) 0.2850(10) 0.6085(11) 0.046(2) Uani 0.358(5) 1 d PGU C 2 H7B H 0.8221 0.2525 0.6106 0.056 Uiso 0.358(5) 1 calc PR C 2 C9A C 1.0039(7) 0.3631(5) 0.4390(5) 0.071(3) Uani 0.642(5) 1 d PGDU C 1 C10A C 1.1290(8) 0.3560(5) 0.4533(5) 0.090(3) Uani 0.642(5) 1 d PGU C 1 H10A H 1.1503 0.3312 0.4795 0.108 Uiso 0.642(5) 1 calc PR C 1 C11A C 1.2230(7) 0.3852(5) 0.4292(5) 0.110(4) Uani 0.642(5) 1 d PGU C 1 H11A H 1.3085 0.3803 0.4390 0.132 Uiso 0.642(5) 1 calc PR C 1 C12A C 1.1920(9) 0.4214(6) 0.3908(5) 0.120(4) Uani 0.642(5) 1 d PGU C 1 H12A H 1.2562 0.4413 0.3744 0.144 Uiso 0.642(5) 1 calc PR C 1 C13A C 1.0669(10) 0.4285(5) 0.3765(5) 0.112(4) Uani 0.642(5) 1 d PGU C 1 H13A H 1.0456 0.4532 0.3503 0.134 Uiso 0.642(5) 1 calc PR C 1 C14A C 0.9729(7) 0.3993(5) 0.4006(5) 0.084(3) Uani 0.642(5) 1 d PGU C 1 H14A H 0.8874 0.4041 0.3908 0.101 Uiso 0.642(5) 1 calc PR C 1 C9B C 0.9749(15) 0.3743(9) 0.4413(9) 0.064(4) Uani 0.358(5) 1 d PGDU C 2 C10B C 1.0940(16) 0.3576(8) 0.4355(8) 0.077(5) Uani 0.358(5) 1 d PGU C 2 H10B H 1.1239 0.3280 0.4548 0.093 Uiso 0.358(5) 1 calc PR C 2 C11B C 1.1693(14) 0.3841(9) 0.4013(8) 0.100(6) Uani 0.358(5) 1 d PGU C 2 H11B H 1.2507 0.3726 0.3973 0.120 Uiso 0.358(5) 1 calc PR C 2 C12B C 1.1255(17) 0.4273(10) 0.3730(8) 0.107(6) Uani 0.358(5) 1 d PGU C 2 H12B H 1.1769 0.4455 0.3497 0.129 Uiso 0.358(5) 1 calc PR C 2 C13B C 1.0063(17) 0.4441(10) 0.3789(9) 0.120(7) Uani 0.358(5) 1 d PGU C 2 H13B H 0.9764 0.4736 0.3596 0.145 Uiso 0.358(5) 1 calc PR C 2 C14B C 0.9310(13) 0.4175(10) 0.4130(10) 0.121(8) Uani 0.358(5) 1 d PGU C 2 H14B H 0.8496 0.4290 0.4170 0.145 Uiso 0.358(5) 1 calc PR C 2 C15 C 0.9605(4) 0.2368(2) 0.4904(2) 0.0364(10) Uani 1 1 d . . . C16 C 0.9478(4) 0.1983(2) 0.4212(2) 0.0366(11) Uani 1 1 d . C . H16 H 0.9602 0.2231 0.3941 0.044 Uiso 1 1 calc R . . C17 C 0.9199(4) 0.1312(2) 0.39576(19) 0.0341(10) Uani 1 1 d . . . H17 H 0.9064 0.1059 0.4222 0.041 Uiso 1 1 calc R C . C18 C 0.9092(4) 0.0944(2) 0.32627(19) 0.0311(10) Uani 1 1 d . C . C19 C 0.8874(4) -0.0162(2) 0.2403(2) 0.0374(11) Uani 1 1 d . C . H19A H 0.9336 -0.0540 0.2381 0.045 Uiso 1 1 calc R . . H19B H 0.9307 0.0118 0.2193 0.045 Uiso 1 1 calc R . . C20 C 0.7533(4) -0.0459(2) 0.20440(19) 0.0387(11) Uani 1 1 d . . . H20A H 0.7048 -0.0085 0.2087 0.046 Uiso 1 1 calc R . . H20B H 0.7116 -0.0769 0.2229 0.046 Uiso 1 1 calc R . . C21 C 0.7522(4) -0.0854(2) 0.1339(2) 0.0403(11) Uani 1 1 d . . . H21A H 0.7795 -0.0527 0.1138 0.048 Uiso 1 1 calc R . . H21B H 0.8138 -0.1166 0.1301 0.048 Uiso 1 1 calc R . . C22 C 0.5927(4) -0.1904(2) 0.09202(19) 0.0314(10) Uani 1 1 d . . . C23 C 0.4656(4) -0.2254(2) 0.05308(19) 0.0325(10) Uani 1 1 d . . . H23 H 0.4125 -0.1996 0.0383 0.039 Uiso 1 1 calc R . . C24 C 0.4239(4) -0.2911(2) 0.03836(19) 0.0317(10) Uani 1 1 d . . . H24 H 0.4762 -0.3173 0.0530 0.038 Uiso 1 1 calc R . . C25 C 0.2967(4) -0.3246(2) -0.00069(19) 0.0311(10) Uani 1 1 d . . . C26 C 0.3406(4) -0.4361(2) 0.0020(2) 0.0354(10) Uani 1 1 d . . . H26A H 0.4223 -0.4253 -0.0110 0.042 Uiso 1 1 calc R . . H26B H 0.3019 -0.4842 -0.0252 0.042 Uiso 1 1 calc R . . C27 C 0.3684(4) -0.4310(2) 0.0703(2) 0.0353(10) Uani 1 1 d . . . C28 C 0.4909(4) -0.4306(2) 0.0976(2) 0.0420(11) Uani 1 1 d . . . H28 H 0.5570 -0.4314 0.0737 0.050 Uiso 1 1 calc R . . C29 C 0.5182(4) -0.4291(3) 0.1589(3) 0.0482(13) Uani 1 1 d . . . H29 H 0.6024 -0.4293 0.1769 0.058 Uiso 1 1 calc R . . C30 C 0.4244(5) -0.4273(3) 0.1937(2) 0.0490(13) Uani 1 1 d . . . H30 H 0.4434 -0.4265 0.2359 0.059 Uiso 1 1 calc R . . C31 C 0.3018(4) -0.4267(2) 0.1684(2) 0.0437(12) Uani 1 1 d . . . H31 H 0.2369 -0.4247 0.1931 0.052 Uiso 1 1 calc R . . C32 C 0.2741(4) -0.4290(2) 0.1064(2) 0.0392(11) Uani 1 1 d . . . H32 H 0.1896 -0.4293 0.0886 0.047 Uiso 1 1 calc R . . C33 C 0.1280(4) -0.4247(2) -0.0469(2) 0.0365(10) Uani 1 1 d . . . H33A H 0.0708 -0.3914 -0.0347 0.044 Uiso 1 1 calc R . . H33B H 0.0984 -0.4634 -0.0342 0.044 Uiso 1 1 calc R . . C34 C 0.1170(4) -0.4513(2) -0.1183(2) 0.0349(10) Uani 1 1 d . . . C35 C 0.2208(4) -0.4594(2) -0.1480(2) 0.0393(11) Uani 1 1 d . . . H35 H 0.3037 -0.4472 -0.1228 0.047 Uiso 1 1 calc R . . C36 C 0.2057(5) -0.4849(3) -0.2135(2) 0.0472(12) Uani 1 1 d . . . H36 H 0.2780 -0.4895 -0.2332 0.057 Uiso 1 1 calc R . . C37 C 0.0861(5) -0.5036(3) -0.2504(2) 0.0494(13) Uani 1 1 d . . . H37 H 0.0757 -0.5223 -0.2956 0.059 Uiso 1 1 calc R . . C38 C -0.0191(5) -0.4951(3) -0.2217(2) 0.0490(13) Uani 1 1 d . . . H38 H -0.1017 -0.5068 -0.2471 0.059 Uiso 1 1 calc R . . C39 C -0.0035(4) -0.4697(2) -0.1561(2) 0.0427(11) Uani 1 1 d . . . H39 H -0.0760 -0.4646 -0.1365 0.051 Uiso 1 1 calc R . . O1 O 0.9903(3) 0.21187(16) 0.53004(14) 0.0412(8) Uani 1 1 d . C . O2 O 0.9162(3) 0.12533(16) 0.28929(13) 0.0363(7) Uani 1 1 d . . . O3 O 0.6642(3) -0.22118(15) 0.11491(13) 0.0366(7) Uani 1 1 d . . . O4 O 0.2279(3) -0.29269(15) -0.02263(13) 0.0359(7) Uani 1 1 d . . . N1 N 0.9386(4) 0.3019(2) 0.50813(17) 0.0416(9) Uani 1 1 d . C . N2 N 0.8935(3) 0.02609(19) 0.30659(15) 0.0327(8) Uani 1 1 d . . . H2 H 0.8867 0.0064 0.3345 0.039 Uiso 1 1 calc R C . N3 N 0.6274(3) -0.12492(19) 0.10037(16) 0.0372(9) Uani 1 1 d . . . H3N H 0.5725 -0.1048 0.0850 0.045 Uiso 1 1 calc R . . N4 N 0.2567(3) -0.39165(18) -0.01123(16) 0.0326(8) Uani 1 1 d . . . C40 C 0.0817(4) -0.1252(2) -0.0120(2) 0.0338(10) Uani 1 1 d . . . C41 C 0.0066(4) -0.0881(2) -0.0358(2) 0.0406(11) Uani 1 1 d . . . H41 H -0.0621 -0.0729 -0.0161 0.049 Uiso 1 1 calc R . . C42 C 0.0317(4) -0.0732(3) -0.0879(2) 0.0458(12) Uani 1 1 d . . . H42 H -0.0208 -0.0483 -0.1043 0.055 Uiso 1 1 calc R . . C43 C 0.1316(4) -0.0940(2) -0.1164(2) 0.0397(11) Uani 1 1 d . . . H43 H 0.1474 -0.0838 -0.1525 0.048 Uiso 1 1 calc R . . C44 C 0.2098(4) -0.1301(2) -0.0927(2) 0.0332(10) Uani 1 1 d . . . C45 C 0.1824(4) -0.1462(2) -0.04064(19) 0.0321(10) Uani 1 1 d . . . H45 H 0.2337 -0.1720 -0.0248 0.038 Uiso 1 1 calc R . . C46 C 0.0563(4) -0.1381(2) 0.0462(2) 0.0391(11) Uani 1 1 d . . . C47 C 0.0785(4) -0.2150(3) 0.1056(2) 0.0398(11) Uani 1 1 d . . . H47A H 0.0407 -0.2643 0.0907 0.048 Uiso 1 1 calc R . . H47B H 0.0205 -0.1887 0.1302 0.048 Uiso 1 1 calc R . . C48 C 0.2048(4) -0.2014(2) 0.1489(2) 0.0338(10) Uani 1 1 d . . . C49 C 0.2815(4) -0.1377(2) 0.1741(2) 0.0423(11) Uani 1 1 d . . . H49 H 0.2559 -0.1014 0.1631 0.051 Uiso 1 1 calc R . . C50 C 0.3956(4) -0.1256(2) 0.2151(2) 0.0404(11) Uani 1 1 d . . . H50 H 0.4476 -0.0813 0.2312 0.048 Uiso 1 1 calc R . . C51 C 0.4354(4) -0.1766(2) 0.23307(19) 0.0353(10) Uani 1 1 d . . . C52 C 0.3581(4) -0.2412(3) 0.2068(2) 0.0437(12) Uani 1 1 d . . . H52 H 0.3837 -0.2776 0.2174 0.052 Uiso 1 1 calc R . . C53 C 0.2451(4) -0.2533(2) 0.1657(2) 0.0422(11) Uani 1 1 d . . . H53 H 0.1939 -0.2978 0.1485 0.051 Uiso 1 1 calc R . . C54 C 0.5562(4) -0.1629(3) 0.2796(2) 0.0418(11) Uani 1 1 d . . . H54A H 0.5961 -0.1140 0.2937 0.050 Uiso 1 1 calc R . . H54B H 0.5358 -0.1715 0.3176 0.050 Uiso 1 1 calc R . . C55 C 0.7056(4) -0.2400(3) 0.2832(2) 0.0420(11) Uani 1 1 d . . . C56 C 0.7976(4) -0.2797(2) 0.2502(2) 0.0345(10) Uani 1 1 d . . . C57 C 0.9008(5) -0.2895(3) 0.2864(2) 0.0455(12) Uani 1 1 d . . . H57 H 0.9126 -0.2707 0.3316 0.055 Uiso 1 1 calc R . . C58 C 0.9871(5) -0.3266(3) 0.2568(2) 0.0503(13) Uani 1 1 d . . . H58 H 1.0574 -0.3336 0.2818 0.060 Uiso 1 1 calc R . . C59 C 0.9707(4) -0.3533(2) 0.1910(2) 0.0410(11) Uani 1 1 d . . . H59 H 1.0297 -0.3789 0.1709 0.049 Uiso 1 1 calc R . . C60 C 0.8692(4) -0.3431(2) 0.15430(19) 0.0313(10) Uani 1 1 d . . . C61 C 0.7822(4) -0.3064(2) 0.18414(19) 0.0322(10) Uani 1 1 d . . . H61 H 0.7117 -0.2997 0.1591 0.039 Uiso 1 1 calc R . . C62 C 0.8585(4) -0.3711(2) 0.08336(19) 0.0304(10) Uani 1 1 d . . . C63 C 0.7695(4) -0.3702(3) -0.0197(2) 0.0410(11) Uani 1 1 d . . . H63A H 0.7306 -0.4194 -0.0398 0.049 Uiso 1 1 calc R . . H63B H 0.8560 -0.3646 -0.0295 0.049 Uiso 1 1 calc R . . C64 C 0.6924(4) -0.3305(2) -0.04735(18) 0.0301(9) Uani 1 1 d . . . C65 C 0.5838(4) -0.3636(2) -0.0935(2) 0.0408(11) Uani 1 1 d . . . H65 H 0.5559 -0.4115 -0.1059 0.049 Uiso 1 1 calc R . . C66 C 0.5161(4) -0.3273(3) -0.1215(2) 0.0409(11) Uani 1 1 d . . . H66 H 0.4421 -0.3505 -0.1531 0.049 Uiso 1 1 calc R . . C67 C 0.5553(4) -0.2567(2) -0.1039(2) 0.0337(10) Uani 1 1 d . . . C68 C 0.6618(4) -0.2241(2) -0.05732(19) 0.0339(10) Uani 1 1 d . . . H68 H 0.6889 -0.1760 -0.0444 0.041 Uiso 1 1 calc R . . C69 C 0.7296(4) -0.2596(2) -0.02914(19) 0.0329(10) Uani 1 1 d . . . H69 H 0.8025 -0.2359 0.0030 0.039 Uiso 1 1 calc R . . C70 C 0.4861(4) -0.2184(3) -0.1376(2) 0.0442(12) Uani 1 1 d . . . H70A H 0.5449 -0.1771 -0.1347 0.053 Uiso 1 1 calc R . . H70B H 0.4581 -0.2478 -0.1833 0.053 Uiso 1 1 calc R . . C71 C 0.3220(4) -0.1480(2) -0.12111(19) 0.0347(10) Uani 1 1 d . . . O5 O 0.0083(3) -0.09848(18) 0.08673(17) 0.0547(9) Uani 1 1 d . . . O6 O 0.6882(4) -0.23968(19) 0.33567(15) 0.0577(10) Uani 1 1 d . . . O7 O 0.9221(3) -0.41357(16) 0.05690(14) 0.0424(8) Uani 1 1 d . . . O8 O 0.3665(3) -0.11727(17) -0.15352(14) 0.0444(8) Uani 1 1 d . . . N5 N 0.0887(3) -0.19644(19) 0.05058(16) 0.0344(8) Uani 1 1 d . . . H5 H 0.1170 -0.2241 0.0186 0.041 Uiso 1 1 calc R . . N6 N 0.6465(3) -0.2050(2) 0.25311(17) 0.0393(9) Uani 1 1 d . . . H6N H 0.6631 -0.2077 0.2156 0.047 Uiso 1 1 calc R . . N7 N 0.7781(3) -0.34765(18) 0.04915(15) 0.0324(8) Uani 1 1 d . . . H7N H 0.7311 -0.3188 0.0684 0.039 Uiso 1 1 calc R . . N8 N 0.3756(3) -0.19788(19) -0.11055(16) 0.0350(9) Uani 1 1 d . . . H8 H 0.3435 -0.2184 -0.0869 0.042 Uiso 1 1 calc R . . C300 C 1.3317(10) 0.4248(5) 0.2584(5) 0.155(4) Uani 1 1 d DU . . H30A H 1.2422 0.4022 0.2438 0.232 Uiso 1 1 calc R . . H30B H 1.3634 0.4361 0.2242 0.232 Uiso 1 1 calc R . . H30C H 1.3397 0.4668 0.2958 0.232 Uiso 1 1 calc R . . C301 C 1.4102(8) 0.3761(4) 0.2762(4) 0.123(3) Uani 1 1 d DU . . H30D H 1.3804 0.3653 0.3116 0.147 Uiso 1 1 calc R . . H30E H 1.4004 0.3327 0.2391 0.147 Uiso 1 1 calc R . . O301 O 1.5298(8) 0.4071(5) 0.2938(5) 0.227(4) Uani 1 1 d DU . . H301 H 1.5744 0.3814 0.3036 0.340 Uiso 1 1 calc R . . C07A C 0.3465(11) 0.0271(5) 0.0442(6) 0.094(4) Uani 0.642(5) 1 d PDU C 1 H07A H 0.2596 0.0358 0.0403 0.141 Uiso 0.642(5) 1 calc PR C 1 H07B H 0.3564 -0.0077 0.0043 0.141 Uiso 0.642(5) 1 calc PR C 1 H07C H 0.4065 0.0696 0.0531 0.141 Uiso 0.642(5) 1 calc PR C 1 C08A C 0.3737(9) 0.0012(7) 0.0998(5) 0.080(4) Uani 0.642(5) 1 d PDU C 1 H08A H 0.3617 0.0360 0.1399 0.096 Uiso 0.642(5) 1 calc PR C 1 H08B H 0.3121 -0.0414 0.0910 0.096 Uiso 0.642(5) 1 calc PR C 1 O09A O 0.4928(16) -0.0113(9) 0.1074(7) 0.081(4) Uani 0.642(5) 1 d PDU C 1 H09A H 0.5454 0.0252 0.1166 0.122 Uiso 0.642(5) 1 calc PR C 1 C07B C 0.3112(18) 0.0243(12) 0.0999(13) 0.102(7) Uani 0.358(5) 1 d PDU C 2 H07D H 0.2481 0.0381 0.0743 0.153 Uiso 0.358(5) 1 calc PR C 2 H07E H 0.3515 0.0638 0.1387 0.153 Uiso 0.358(5) 1 calc PR C 2 H07F H 0.2693 -0.0122 0.1116 0.153 Uiso 0.358(5) 1 calc PR C 2 C08B C 0.4124(18) -0.0018(12) 0.0610(11) 0.100(6) Uani 0.358(5) 1 d PDU C 2 H08C H 0.3687 -0.0378 0.0197 0.119 Uiso 0.358(5) 1 calc PR C 2 H08D H 0.4565 0.0365 0.0516 0.119 Uiso 0.358(5) 1 calc PR C 2 O09B O 0.498(3) -0.0269(19) 0.0872(16) 0.081(4) Uani 0.358(5) 1 d PDU C 2 H09B H 0.5415 0.0041 0.1204 0.122 Uiso 0.358(5) 1 calc PR C 2 C01A C 0.7114(18) 0.5489(8) 0.3833(8) 0.155(5) Uani 0.642(5) 1 d PDU C 1 H01A H 0.6848 0.5045 0.3479 0.233 Uiso 0.642(5) 1 calc PR C 1 H01B H 0.6532 0.5531 0.4135 0.233 Uiso 0.642(5) 1 calc PR C 1 H01C H 0.7977 0.5522 0.4051 0.233 Uiso 0.642(5) 1 calc PR C 1 C02A C 0.7093(10) 0.6057(6) 0.3580(6) 0.099(3) Uani 0.642(5) 1 d PDU C 1 H02A H 0.7692 0.6019 0.3280 0.118 Uiso 0.642(5) 1 calc PR C 1 H02B H 0.6231 0.6011 0.3343 0.118 Uiso 0.642(5) 1 calc PR C 1 O03A O 0.7420(8) 0.6672(5) 0.4057(4) 0.120(3) Uani 0.642(5) 1 d PDU C 1 H03A H 0.7372 0.6981 0.3909 0.180 Uiso 0.642(5) 1 calc PR C 1 C01B C 0.696(3) 0.4900(16) 0.4001(13) 0.155(5) Uani 0.358(5) 1 d PDU C 2 H01D H 0.7454 0.5220 0.4414 0.233 Uiso 0.358(5) 1 calc PR C 2 H01E H 0.7533 0.4663 0.3738 0.233 Uiso 0.358(5) 1 calc PR C 2 H01F H 0.6342 0.4563 0.4069 0.233 Uiso 0.358(5) 1 calc PR C 2 C02B C 0.6278(19) 0.5284(12) 0.3671(9) 0.099(3) Uani 0.358(5) 1 d PDU C 2 H02C H 0.5569 0.5371 0.3906 0.118 Uiso 0.358(5) 1 calc PR C 2 H02D H 0.6870 0.5731 0.3835 0.118 Uiso 0.358(5) 1 calc PR C 2 O03B O 0.5774(14) 0.5262(9) 0.3127(6) 0.120(3) Uani 0.358(5) 1 d PDU C 2 H03B H 0.5737 0.5661 0.3145 0.180 Uiso 0.358(5) 1 calc PR C 2 C011 C 0.521(5) 0.484(2) 0.517(2) 0.39(3) Uiso 0.50 1 d PD D -1 H01G H 0.5656 0.5297 0.5447 0.588 Uiso 0.50 1 calc PR D -1 H01H H 0.4964 0.4575 0.5430 0.588 Uiso 0.50 1 calc PR D -1 H01I H 0.4441 0.4868 0.4908 0.588 Uiso 0.50 1 calc PR D -1 C012 C 0.608(3) 0.4470(18) 0.473(2) 0.32(2) Uiso 0.50 1 d PD D -1 H01J H 0.6303 0.4727 0.4460 0.380 Uiso 0.50 1 calc PR D -1 H01K H 0.6874 0.4463 0.4996 0.380 Uiso 0.50 1 calc PR D -1 O04 O 0.553(2) 0.3848(15) 0.4375(12) 0.271(10) Uiso 0.50 1 d PD D -1 H04 H 0.5174 0.3839 0.4021 0.406 Uiso 0.50 1 calc PR D -1 C72 C 0.8861(4) 0.0821(2) 0.55817(19) 0.0294(9) Uani 1 1 d . E -1 H72 H 0.8917 0.0687 0.5144 0.035 Uiso 1 1 calc R E -1 C73 C 0.7696(4) 0.0911(2) 0.57670(19) 0.0308(10) Uani 1 1 d . E -1 C74 C 0.7640(4) 0.1120(2) 0.6409(2) 0.0355(10) Uani 1 1 d . E -1 H74 H 0.6855 0.1190 0.6543 0.043 Uiso 1 1 calc R E -1 C75 C 0.8714(4) 0.1227(3) 0.6857(2) 0.0411(11) Uani 1 1 d . E -1 H75 H 0.8666 0.1371 0.7297 0.049 Uiso 1 1 calc R E -1 C76 C 0.9861(4) 0.1124(2) 0.6664(2) 0.0360(10) Uani 1 1 d . E -1 H76 H 1.0598 0.1191 0.6971 0.043 Uiso 1 1 calc R E -1 C77 C 0.9930(4) 0.0925(2) 0.60270(18) 0.0279(9) Uani 1 1 d . E -1 C78 C 1.1189(4) 0.0837(2) 0.58276(18) 0.0301(10) Uani 1 1 d . E -1 C79 C 1.2739(4) 0.1243(3) 0.52677(19) 0.0355(10) Uani 1 1 d . E -1 H79A H 1.3131 0.0847 0.5270 0.043 Uiso 1 1 calc R E -1 H79B H 1.3302 0.1664 0.5581 0.043 Uiso 1 1 calc R E -1 C80 C 1.2623(3) 0.1276(2) 0.4617(2) 0.0313(10) Uani 1 1 d . E -1 C81 C 1.2883(4) 0.1886(3) 0.4519(2) 0.0440(12) Uani 1 1 d . E -1 H81 H 1.3104 0.2309 0.4873 0.053 Uiso 1 1 calc R E -1 C82 C 1.2820(4) 0.1874(3) 0.3897(2) 0.0454(12) Uani 1 1 d . E -1 H82 H 1.3001 0.2293 0.3834 0.054 Uiso 1 1 calc R E -1 C83 C 1.2500(4) 0.1270(3) 0.3377(2) 0.0394(11) Uani 1 1 d . E -1 C84 C 1.2202(4) 0.0670(3) 0.3473(2) 0.0389(11) Uani 1 1 d . E -1 H84 H 1.1964 0.0248 0.3118 0.047 Uiso 1 1 calc R E -1 C85 C 1.2248(4) 0.0678(3) 0.4083(2) 0.0378(11) Uani 1 1 d . E -1 H85 H 1.2014 0.0258 0.4139 0.045 Uiso 1 1 calc R E -1 C86 C 1.2509(4) 0.1258(3) 0.2711(2) 0.0491(13) Uani 1 1 d . E -1 H86A H 1.3373 0.1455 0.2685 0.059 Uiso 1 1 calc R E -1 H86B H 1.2292 0.0779 0.2403 0.059 Uiso 1 1 calc R E -1 C87 C 1.1875(4) 0.2072(3) 0.2237(2) 0.0490(13) Uani 1 1 d . E -1 C88 C 1.0867(4) 0.2448(2) 0.2113(2) 0.0374(11) Uani 1 1 d . E -1 C89 C 1.0920(4) 0.2709(3) 0.1633(2) 0.0435(12) Uani 1 1 d . E -1 H89 H 1.1595 0.2650 0.1402 0.052 Uiso 1 1 calc R E -1 C90 C 0.9997(4) 0.3052(2) 0.1492(2) 0.0408(11) Uani 1 1 d . E -1 H90 H 1.0037 0.3225 0.1161 0.049 Uiso 1 1 calc R E -1 C91 C 0.9020(4) 0.3145(2) 0.1826(2) 0.0370(10) Uani 1 1 d . E -1 H91 H 0.8399 0.3392 0.1734 0.044 Uiso 1 1 calc R E -1 C92 C 0.8940(4) 0.2876(2) 0.23020(19) 0.0325(10) Uani 1 1 d . E -1 C93 C 0.9878(4) 0.2538(2) 0.24406(19) 0.0343(10) Uani 1 1 d . E -1 H93 H 0.9839 0.2364 0.2770 0.041 Uiso 1 1 calc R E -1 C94 C 0.7824(4) 0.2954(2) 0.2624(2) 0.0366(10) Uani 1 1 d . E -1 C95 C 0.6330(4) 0.2508(3) 0.3166(2) 0.0416(11) Uani 1 1 d . E -1 H95A H 0.5583 0.2448 0.2838 0.050 Uiso 1 1 calc R E -1 H95B H 0.6406 0.2958 0.3514 0.050 Uiso 1 1 calc R E -1 C96 C 0.6133(4) 0.1945(3) 0.3427(2) 0.0356(11) Uani 1 1 d . E -1 C97 C 0.6048(4) 0.2102(3) 0.4060(2) 0.0395(11) Uani 1 1 d . E -1 H97 H 0.6138 0.2567 0.4334 0.047 Uiso 1 1 calc R E -1 C98 C 0.5832(4) 0.1593(2) 0.4306(2) 0.0375(11) Uani 1 1 d . E -1 H98 H 0.5781 0.1712 0.4743 0.045 Uiso 1 1 calc R E -1 C99 C 0.5692(4) 0.0911(2) 0.3913(2) 0.0322(10) Uani 1 1 d . E -1 C100 C 0.5786(4) 0.0756(3) 0.3276(2) 0.0387(11) Uani 1 1 d . E -1 H100 H 0.5710 0.0291 0.3003 0.046 Uiso 1 1 calc R E -1 C101 C 0.5989(4) 0.1267(3) 0.3033(2) 0.0379(11) Uani 1 1 d . E -1 H101 H 0.6030 0.1150 0.2595 0.045 Uiso 1 1 calc R E -1 C102 C 0.5462(4) 0.0358(2) 0.4181(2) 0.0357(10) Uani 1 1 d . E -1 H10C H 0.4663 0.0379 0.4350 0.043 Uiso 1 1 calc R E -1 H10D H 0.5365 -0.0096 0.3836 0.043 Uiso 1 1 calc R E -1 C103 C 0.6497(4) 0.0791(2) 0.5301(2) 0.0308(10) Uani 1 1 d . E -1 O9 O 1.1847(3) 0.04719(15) 0.60058(13) 0.0336(7) Uani 1 1 d . E -1 O10 O 1.2884(4) 0.2129(3) 0.2058(2) 0.0809(14) Uani 1 1 d . E -1 O11 O 0.7209(3) 0.34134(18) 0.26372(16) 0.0515(9) Uani 1 1 d . E -1 O12 O 0.5572(3) 0.10285(16) 0.54862(14) 0.0388(7) Uani 1 1 d . E -1 N9 N 1.1496(3) 0.11752(18) 0.54569(15) 0.0301(8) Uani 1 1 d . E -1 H9 H 1.0918 0.1370 0.5316 0.036 Uiso 1 1 calc R E -1 N10 N 1.1607(3) 0.1647(2) 0.25407(18) 0.0454(10) Uani 1 1 d . E -1 H10N H 1.0850 0.1601 0.2642 0.055 Uiso 1 1 calc R E -1 N11 N 0.7479(3) 0.24958(19) 0.28839(17) 0.0370(9) Uani 1 1 d . E -1 H11N H 0.7945 0.2186 0.2885 0.044 Uiso 1 1 calc R E -1 N12 N 0.6503(3) 0.04336(19) 0.46877(16) 0.0324(8) Uani 1 1 d . E -1 H12N H 0.7156 0.0238 0.4588 0.039 Uiso 1 1 calc R E -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(3) 0.038(3) 0.033(3) 0.010(2) -0.006(2) 0.006(2) C8 0.086(4) 0.046(3) 0.041(3) 0.018(3) -0.011(3) 0.019(3) C2A 0.048(6) 0.042(6) 0.036(6) 0.004(5) 0.002(5) 0.011(4) C3A 0.083(7) 0.045(5) 0.104(9) 0.006(7) 0.043(6) 0.012(5) C4A 0.098(8) 0.058(5) 0.143(10) 0.010(8) 0.070(7) 0.023(6) C5A 0.061(6) 0.067(6) 0.095(9) 0.017(6) 0.036(6) 0.019(5) C6A 0.064(3) 0.050(4) 0.049(3) 0.002(3) 0.018(3) 0.008(3) C7A 0.062(4) 0.043(5) 0.030(6) 0.006(4) 0.007(4) 0.014(4) C2B 0.054(9) 0.047(10) 0.043(11) 0.011(9) -0.002(10) 0.012(7) C3B 0.070(8) 0.055(8) 0.054(9) 0.009(8) -0.005(8) 0.023(7) C4B 0.067(8) 0.071(9) 0.053(9) 0.000(8) -0.001(8) 0.035(8) C5B 0.065(8) 0.080(10) 0.055(10) -0.005(8) 0.013(8) 0.022(7) C6B 0.064(3) 0.050(4) 0.049(3) 0.002(3) 0.018(3) 0.008(3) C7B 0.062(4) 0.043(5) 0.030(6) 0.006(4) 0.007(4) 0.014(4) C9A 0.106(5) 0.044(5) 0.067(5) 0.030(4) -0.003(4) 0.018(5) C10A 0.103(6) 0.081(6) 0.097(7) 0.052(5) 0.018(5) 0.004(5) C11A 0.122(6) 0.102(7) 0.116(7) 0.061(6) 0.023(6) -0.003(6) C12A 0.143(7) 0.102(7) 0.135(7) 0.078(6) 0.028(6) -0.002(6) C13A 0.142(7) 0.096(7) 0.108(7) 0.061(6) 0.016(6) 0.001(6) C14A 0.126(6) 0.054(5) 0.072(5) 0.037(4) -0.007(5) 0.004(5) C9B 0.102(7) 0.047(7) 0.052(7) 0.032(5) 0.004(6) 0.019(6) C10B 0.091(7) 0.069(9) 0.084(9) 0.053(7) 0.006(7) -0.004(7) C11B 0.119(9) 0.096(9) 0.094(9) 0.053(7) 0.024(7) -0.005(7) C12B 0.123(9) 0.097(9) 0.112(9) 0.060(7) 0.015(7) 0.003(7) C13B 0.130(9) 0.118(10) 0.121(10) 0.059(7) 0.020(7) 0.011(7) C14B 0.128(10) 0.119(12) 0.122(11) 0.055(8) 0.019(8) 0.022(8) C15 0.039(2) 0.040(3) 0.034(2) 0.017(2) 0.005(2) 0.010(2) C16 0.036(2) 0.046(3) 0.038(2) 0.024(2) 0.012(2) 0.011(2) C17 0.029(2) 0.045(3) 0.034(2) 0.022(2) 0.0077(18) 0.004(2) C18 0.022(2) 0.041(3) 0.036(2) 0.020(2) 0.0063(17) 0.0056(19) C19 0.036(2) 0.043(3) 0.040(3) 0.022(2) 0.012(2) 0.010(2) C20 0.035(2) 0.044(3) 0.033(2) 0.012(2) 0.0080(19) 0.002(2) C21 0.038(2) 0.039(3) 0.040(3) 0.010(2) 0.011(2) 0.002(2) C22 0.033(2) 0.036(3) 0.025(2) 0.008(2) 0.0134(18) 0.007(2) C23 0.036(2) 0.033(3) 0.030(2) 0.013(2) 0.0085(18) 0.008(2) C24 0.034(2) 0.034(3) 0.032(2) 0.013(2) 0.0126(18) 0.013(2) C25 0.034(2) 0.030(2) 0.032(2) 0.010(2) 0.0141(19) 0.010(2) C26 0.035(2) 0.027(2) 0.047(3) 0.013(2) 0.014(2) 0.0099(19) C27 0.032(2) 0.029(2) 0.050(3) 0.020(2) 0.008(2) 0.0068(19) C28 0.029(2) 0.034(3) 0.070(3) 0.026(3) 0.011(2) 0.010(2) C29 0.036(3) 0.046(3) 0.070(3) 0.034(3) -0.005(2) 0.008(2) C30 0.052(3) 0.045(3) 0.055(3) 0.032(3) -0.002(2) 0.000(2) C31 0.040(3) 0.043(3) 0.048(3) 0.020(2) 0.006(2) 0.000(2) C32 0.029(2) 0.036(3) 0.052(3) 0.018(2) 0.004(2) 0.008(2) C33 0.028(2) 0.036(3) 0.047(3) 0.016(2) 0.011(2) 0.008(2) C34 0.033(2) 0.028(2) 0.045(3) 0.015(2) 0.006(2) 0.0062(19) C35 0.037(2) 0.035(3) 0.044(3) 0.013(2) 0.006(2) 0.006(2) C36 0.047(3) 0.048(3) 0.045(3) 0.015(3) 0.010(2) 0.010(2) C37 0.058(3) 0.043(3) 0.042(3) 0.012(2) 0.002(2) 0.010(3) C38 0.043(3) 0.043(3) 0.052(3) 0.015(3) -0.008(2) 0.003(2) C39 0.038(3) 0.034(3) 0.052(3) 0.012(2) 0.005(2) 0.005(2) O1 0.0464(18) 0.049(2) 0.0389(17) 0.0250(16) 0.0094(14) 0.0178(16) O2 0.0353(16) 0.0454(19) 0.0392(17) 0.0262(16) 0.0129(13) 0.0100(14) O3 0.0340(16) 0.0406(19) 0.0340(16) 0.0115(15) 0.0055(13) 0.0099(14) O4 0.0355(16) 0.0336(17) 0.0405(17) 0.0150(15) 0.0052(13) 0.0113(14) N1 0.051(2) 0.043(2) 0.032(2) 0.0159(19) 0.0012(17) 0.0154(19) N2 0.0315(18) 0.040(2) 0.0298(19) 0.0170(18) 0.0068(15) 0.0074(17) N3 0.039(2) 0.032(2) 0.037(2) 0.0113(18) 0.0062(16) -0.0008(17) N4 0.0264(17) 0.033(2) 0.040(2) 0.0141(18) 0.0102(15) 0.0087(16) C40 0.028(2) 0.031(2) 0.040(2) 0.010(2) 0.0042(19) 0.0047(19) C41 0.033(2) 0.034(3) 0.053(3) 0.012(2) 0.009(2) 0.013(2) C42 0.045(3) 0.043(3) 0.053(3) 0.021(3) 0.003(2) 0.017(2) C43 0.044(3) 0.032(3) 0.040(3) 0.014(2) 0.002(2) 0.005(2) C44 0.031(2) 0.032(2) 0.037(2) 0.012(2) 0.0054(19) 0.0050(19) C45 0.027(2) 0.032(2) 0.034(2) 0.009(2) 0.0030(18) 0.0049(19) C46 0.027(2) 0.042(3) 0.052(3) 0.018(2) 0.014(2) 0.010(2) C47 0.033(2) 0.047(3) 0.044(3) 0.021(2) 0.016(2) 0.005(2) C48 0.033(2) 0.039(3) 0.034(2) 0.014(2) 0.0176(19) 0.010(2) C49 0.051(3) 0.037(3) 0.042(3) 0.016(2) 0.012(2) 0.012(2) C50 0.043(3) 0.035(3) 0.042(3) 0.013(2) 0.012(2) 0.003(2) C51 0.037(2) 0.043(3) 0.030(2) 0.014(2) 0.0184(19) 0.010(2) C52 0.042(3) 0.044(3) 0.052(3) 0.023(3) 0.016(2) 0.011(2) C53 0.036(2) 0.037(3) 0.055(3) 0.019(2) 0.013(2) -0.001(2) C54 0.040(2) 0.050(3) 0.033(2) 0.009(2) 0.014(2) 0.012(2) C55 0.048(3) 0.046(3) 0.031(3) 0.016(2) 0.003(2) 0.006(2) C56 0.042(2) 0.032(3) 0.033(2) 0.015(2) 0.006(2) 0.008(2) C57 0.062(3) 0.041(3) 0.035(3) 0.016(2) 0.001(2) 0.014(3) C58 0.060(3) 0.046(3) 0.046(3) 0.020(3) -0.004(2) 0.019(3) C59 0.049(3) 0.039(3) 0.044(3) 0.023(2) 0.011(2) 0.015(2) C60 0.031(2) 0.029(2) 0.037(2) 0.017(2) 0.0055(19) 0.0036(19) C61 0.031(2) 0.029(2) 0.033(2) 0.012(2) 0.0011(18) 0.0010(19) C62 0.030(2) 0.029(2) 0.035(2) 0.016(2) 0.0072(19) 0.0012(19) C63 0.048(3) 0.049(3) 0.035(2) 0.019(2) 0.019(2) 0.020(2) C64 0.032(2) 0.035(3) 0.028(2) 0.013(2) 0.0133(18) 0.0102(19) C65 0.046(3) 0.037(3) 0.037(3) 0.011(2) 0.014(2) 0.004(2) C66 0.031(2) 0.055(3) 0.036(3) 0.019(2) 0.0036(19) 0.004(2) C67 0.029(2) 0.046(3) 0.033(2) 0.018(2) 0.0158(19) 0.011(2) C68 0.036(2) 0.036(3) 0.035(2) 0.016(2) 0.013(2) 0.010(2) C69 0.028(2) 0.042(3) 0.026(2) 0.009(2) 0.0085(18) 0.005(2) C70 0.035(2) 0.062(3) 0.050(3) 0.033(3) 0.015(2) 0.019(2) C71 0.037(2) 0.037(3) 0.031(2) 0.015(2) 0.0010(19) 0.003(2) O5 0.056(2) 0.056(2) 0.070(2) 0.029(2) 0.0377(18) 0.0294(19) O6 0.083(3) 0.066(3) 0.0312(18) 0.0195(18) 0.0195(17) 0.024(2) O7 0.0507(19) 0.043(2) 0.0467(19) 0.0231(16) 0.0203(15) 0.0251(16) O8 0.0443(18) 0.053(2) 0.0476(19) 0.0323(18) 0.0110(15) 0.0072(16) N5 0.0359(19) 0.034(2) 0.035(2) 0.0113(18) 0.0148(16) 0.0104(17) N6 0.039(2) 0.050(3) 0.032(2) 0.0133(19) 0.0141(16) 0.0152(19) N7 0.0335(18) 0.038(2) 0.0297(19) 0.0122(17) 0.0113(15) 0.0152(17) N8 0.0333(19) 0.045(2) 0.038(2) 0.0253(19) 0.0132(16) 0.0126(17) C300 0.185(9) 0.110(8) 0.159(9) 0.025(7) 0.043(7) 0.057(7) C301 0.127(6) 0.081(6) 0.149(8) 0.020(5) 0.069(6) 0.003(5) O301 0.157(4) 0.221(6) 0.253(6) 0.020(4) 0.028(4) 0.066(4) C07A 0.072(7) 0.056(7) 0.125(10) 0.021(7) -0.035(7) -0.001(6) C08A 0.035(5) 0.107(10) 0.070(7) 0.006(6) 0.019(5) -0.012(5) O09A 0.081(3) 0.045(9) 0.108(11) 0.025(8) -0.010(6) 0.018(4) C07B 0.054(12) 0.082(15) 0.18(2) 0.072(15) 0.004(12) -0.010(9) C08B 0.079(13) 0.080(14) 0.115(16) 0.033(13) -0.041(10) -0.005(10) O09B 0.081(3) 0.045(9) 0.108(11) 0.025(8) -0.010(6) 0.018(4) C01A 0.161(12) 0.174(10) 0.133(11) 0.063(9) 0.006(9) 0.044(11) C02A 0.062(5) 0.105(7) 0.103(7) 0.002(5) 0.000(5) 0.043(5) O03A 0.117(5) 0.158(6) 0.077(4) 0.017(4) 0.011(4) 0.084(5) C01B 0.161(12) 0.174(10) 0.133(11) 0.063(9) 0.006(9) 0.044(11) C02B 0.062(5) 0.105(7) 0.103(7) 0.002(5) 0.000(5) 0.043(5) O03B 0.117(5) 0.158(6) 0.077(4) 0.017(4) 0.011(4) 0.084(5) C72 0.030(2) 0.034(2) 0.031(2) 0.017(2) 0.0123(18) 0.0099(19) C73 0.030(2) 0.039(3) 0.033(2) 0.022(2) 0.0142(18) 0.0117(19) C74 0.036(2) 0.042(3) 0.039(3) 0.019(2) 0.020(2) 0.017(2) C75 0.046(3) 0.052(3) 0.033(2) 0.020(2) 0.019(2) 0.015(2) C76 0.034(2) 0.044(3) 0.033(2) 0.018(2) 0.0048(19) 0.009(2) C77 0.031(2) 0.032(2) 0.027(2) 0.016(2) 0.0113(18) 0.0106(19) C78 0.026(2) 0.041(3) 0.021(2) 0.008(2) 0.0034(17) 0.0080(19) C79 0.023(2) 0.053(3) 0.036(2) 0.022(2) 0.0091(18) 0.009(2) C80 0.0185(19) 0.046(3) 0.041(3) 0.025(2) 0.0133(18) 0.0102(19) C81 0.036(2) 0.049(3) 0.052(3) 0.023(3) 0.009(2) 0.010(2) C82 0.039(3) 0.061(4) 0.059(3) 0.045(3) 0.017(2) 0.016(2) C83 0.025(2) 0.060(3) 0.046(3) 0.032(3) 0.008(2) 0.018(2) C84 0.030(2) 0.055(3) 0.037(2) 0.022(2) 0.0094(19) 0.010(2) C85 0.032(2) 0.055(3) 0.037(3) 0.027(3) 0.0090(19) 0.010(2) C86 0.041(3) 0.082(4) 0.050(3) 0.045(3) 0.020(2) 0.030(3) C87 0.041(3) 0.080(4) 0.050(3) 0.044(3) 0.024(2) 0.023(3) C88 0.035(2) 0.047(3) 0.037(2) 0.024(2) 0.010(2) 0.009(2) C89 0.048(3) 0.053(3) 0.046(3) 0.032(3) 0.023(2) 0.015(2) C90 0.054(3) 0.042(3) 0.037(3) 0.024(2) 0.015(2) 0.011(2) C91 0.040(2) 0.034(3) 0.041(3) 0.019(2) 0.008(2) 0.006(2) C92 0.036(2) 0.029(2) 0.032(2) 0.012(2) 0.0051(19) 0.0013(19) C93 0.033(2) 0.042(3) 0.031(2) 0.021(2) 0.0024(18) 0.000(2) C94 0.037(2) 0.037(3) 0.040(3) 0.018(2) 0.008(2) 0.009(2) C95 0.040(2) 0.054(3) 0.044(3) 0.028(3) 0.015(2) 0.017(2) C96 0.025(2) 0.051(3) 0.039(3) 0.026(2) 0.0092(19) 0.006(2) C97 0.043(3) 0.044(3) 0.044(3) 0.025(2) 0.015(2) 0.018(2) C98 0.040(2) 0.045(3) 0.039(3) 0.022(2) 0.018(2) 0.018(2) C99 0.0200(19) 0.047(3) 0.035(2) 0.023(2) 0.0041(17) 0.0041(19) C100 0.032(2) 0.045(3) 0.039(3) 0.016(2) 0.0037(19) 0.005(2) C101 0.031(2) 0.056(3) 0.032(2) 0.025(2) 0.0068(19) 0.003(2) C102 0.023(2) 0.045(3) 0.044(3) 0.023(2) 0.0073(19) 0.006(2) C103 0.023(2) 0.038(3) 0.045(3) 0.029(2) 0.0177(19) 0.0095(19) O9 0.0322(15) 0.0446(19) 0.0335(16) 0.0227(15) 0.0077(12) 0.0151(14) O10 0.058(2) 0.131(4) 0.114(3) 0.095(3) 0.055(2) 0.045(3) O11 0.053(2) 0.054(2) 0.066(2) 0.0363(19) 0.0248(17) 0.0200(18) O12 0.0290(15) 0.050(2) 0.0512(19) 0.0282(17) 0.0207(14) 0.0166(15) N9 0.0242(17) 0.046(2) 0.0306(18) 0.0225(18) 0.0107(14) 0.0144(16) N10 0.033(2) 0.078(3) 0.052(2) 0.048(2) 0.0181(18) 0.024(2) N11 0.0347(19) 0.043(2) 0.048(2) 0.030(2) 0.0161(17) 0.0119(17) N12 0.0217(17) 0.044(2) 0.040(2) 0.0215(19) 0.0140(15) 0.0113(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.467(6) . ? C1 C2B 1.502(17) . ? C1 C2A 1.521(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C8 C9B 1.437(9) . ? C8 N1 1.460(5) . ? C8 C9A 1.550(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C2A C3A 1.3900 . ? C2A C7A 1.3900 . ? C3A C4A 1.3900 . ? C3A H3A 0.9500 . ? C4A C5A 1.3900 . ? C4A H4A 0.9500 . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A C7A 1.3900 . ? C6A H6A 0.9500 . ? C7A H7A 0.9500 . ? C2B C3B 1.3900 . ? C2B C7B 1.3900 . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B H4B 0.9500 . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B C7B 1.3900 . ? C6B H6B 0.9500 . ? C7B H7B 0.9500 . ? C9A C10A 1.3900 . ? C9A C14A 1.3900 . ? C10A C11A 1.3900 . ? C10A H10A 0.9500 . ? C11A C12A 1.3900 . ? C11A H11A 0.9500 . ? C12A C13A 1.3900 . ? C12A H12A 0.9500 . ? C13A C14A 1.3900 . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? C9B C10B 1.3900 . ? C9B C14B 1.3900 . ? C10B C11B 1.3900 . ? C10B H10B 0.9500 . ? C11B C12B 1.3900 . ? C11B H11B 0.9500 . ? C12B C13B 1.3900 . ? C12B H12B 0.9500 . ? C13B C14B 1.3900 . ? C13B H13B 0.9500 . ? C14B H14B 0.9500 . ? C15 O1 1.227(5) . ? C15 N1 1.358(6) . ? C15 C16 1.480(6) . ? C16 C17 1.312(6) . ? C16 H16 0.9500 . ? C17 C18 1.482(6) . ? C17 H17 0.9500 . ? C18 O2 1.240(5) . ? C18 N2 1.338(5) . ? C19 N2 1.450(5) . ? C19 C20 1.505(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.527(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N3 1.450(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O3 1.250(5) . ? C22 N3 1.331(5) . ? C22 C23 1.479(6) . ? C23 C24 1.316(6) . ? C23 H23 0.9500 . ? C24 C25 1.476(6) . ? C24 H24 0.9500 . ? C25 O4 1.239(5) . ? C25 N4 1.358(5) . ? C26 N4 1.469(5) . ? C26 C27 1.509(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.386(6) . ? C27 C28 1.387(6) . ? C28 C29 1.379(6) . ? C28 H28 0.9500 . ? C29 C30 1.362(7) . ? C29 H29 0.9500 . ? C30 C31 1.380(6) . ? C30 H30 0.9500 . ? C31 C32 1.387(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 N4 1.465(5) . ? C33 C34 1.506(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.381(6) . ? C34 C39 1.392(6) . ? C35 C36 1.378(6) . ? C35 H35 0.9500 . ? C36 C37 1.375(7) . ? C36 H36 0.9500 . ? C37 C38 1.384(7) . ? C37 H37 0.9500 . ? C38 C39 1.378(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? N2 H2 0.8800 . ? N3 H3N 0.8800 . ? C40 C45 1.385(6) . ? C40 C41 1.388(6) . ? C40 C46 1.494(6) . ? C41 C42 1.382(6) . ? C41 H41 0.9500 . ? C42 C43 1.373(6) . ? C42 H42 0.9500 . ? C43 C44 1.392(6) . ? C43 H43 0.9500 . ? C44 C45 1.398(6) . ? C44 C71 1.478(6) . ? C45 H45 0.9500 . ? C46 O5 1.234(5) . ? C46 N5 1.363(6) . ? C47 N5 1.451(5) . ? C47 C48 1.509(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.374(6) . ? C48 C53 1.387(6) . ? C49 C50 1.384(6) . ? C49 H49 0.9500 . ? C50 C51 1.384(6) . ? C50 H50 0.9500 . ? C51 C52 1.390(6) . ? C51 C54 1.498(6) . ? C52 C53 1.376(6) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 N6 1.456(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O6 1.232(5) . ? C55 N6 1.341(6) . ? C55 C56 1.494(6) . ? C56 C57 1.383(6) . ? C56 C61 1.388(6) . ? C57 C58 1.387(7) . ? C57 H57 0.9500 . ? C58 C59 1.383(6) . ? C58 H58 0.9500 . ? C59 C60 1.380(6) . ? C59 H59 0.9500 . ? C60 C61 1.391(6) . ? C60 C62 1.497(6) . ? C61 H61 0.9500 . ? C62 O7 1.239(5) . ? C62 N7 1.350(5) . ? C63 N7 1.458(5) . ? C63 C64 1.490(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.389(6) . ? C64 C69 1.400(6) . ? C65 C66 1.382(6) . ? C65 H65 0.9500 . ? C66 C67 1.399(6) . ? C66 H66 0.9500 . ? C67 C68 1.378(6) . ? C67 C70 1.502(6) . ? C68 C69 1.372(6) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 N8 1.460(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 O8 1.244(5) . ? C71 N8 1.349(5) . ? N5 H5 0.8800 . ? N6 H6N 0.8800 . ? N7 H7N 0.8800 . ? N8 H8 0.8800 . ? C300 C301 1.545(5) . ? C300 H30A 0.9800 . ? C300 H30B 0.9800 . ? C300 H30C 0.9800 . ? C301 O301 1.314(9) . ? C301 H30D 0.9900 . ? C301 H30E 0.9900 . ? O301 H301 0.8400 . ? C07A C08A 1.559(12) . ? C07A H07A 0.9800 . ? C07A H07B 0.9800 . ? C07A H07C 0.9800 . ? C08A O09A 1.350(13) . ? C08A H08A 0.9900 . ? C08A H08B 0.9900 . ? O09A H09A 0.8400 . ? C07B C08B 1.534(15) . ? C07B H07D 0.9800 . ? C07B H07E 0.9800 . ? C07B H07F 0.9800 . ? C08B O09B 1.308(16) . ? C08B H08C 0.9900 . ? C08B H08D 0.9900 . ? O09B H09B 0.8400 . ? C01A C02A 1.510(13) . ? C01A H01A 0.9800 . ? C01A H01B 0.9800 . ? C01A H01C 0.9800 . ? C02A O03A 1.342(10) . ? C02A H02A 0.9900 . ? C02A H02B 0.9900 . ? O03A H03A 0.8400 . ? C01B C02B 1.492(15) . ? C01B H01D 0.9800 . ? C01B H01E 0.9800 . ? C01B H01F 0.9800 . ? C02B O03B 1.270(14) . ? C02B H02C 0.9900 . ? C02B H02D 0.9900 . ? O03B H03B 0.8400 . ? C011 C012 1.541(9) . ? C011 H01G 0.9800 . ? C011 H01H 0.9800 . ? C011 H01I 0.9800 . ? C012 O04 1.296(17) . ? C012 H01J 0.9900 . ? C012 H01K 0.9900 . ? O04 H04 0.8400 . ? C72 C77 1.376(6) . ? C72 C73 1.394(5) . ? C72 H72 0.9500 . ? C73 C74 1.384(5) . ? C73 C103 1.498(6) . ? C74 C75 1.382(6) . ? C74 H74 0.9500 . ? C75 C76 1.387(6) . ? C75 H75 0.9500 . ? C76 C77 1.378(5) . ? C76 H76 0.9500 . ? C77 C78 1.503(5) . ? C78 O9 1.250(5) . ? C78 N9 1.331(5) . ? C79 N9 1.466(5) . ? C79 C80 1.499(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C85 1.383(6) . ? C80 C81 1.388(6) . ? C81 C82 1.403(6) . ? C81 H81 0.9500 . ? C82 C83 1.372(7) . ? C82 H82 0.9500 . ? C83 C84 1.369(6) . ? C83 C86 1.511(6) . ? C84 C85 1.380(6) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 N10 1.456(5) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 O10 1.218(5) . ? C87 N10 1.340(6) . ? C87 C88 1.486(6) . ? C88 C93 1.376(6) . ? C88 C89 1.392(6) . ? C89 C90 1.380(6) . ? C89 H89 0.9500 . ? C90 C91 1.375(6) . ? C90 H90 0.9500 . ? C91 C92 1.397(6) . ? C91 H91 0.9500 . ? C92 C93 1.382(6) . ? C92 C94 1.489(6) . ? C93 H93 0.9500 . ? C94 O11 1.243(5) . ? C94 N11 1.342(5) . ? C95 N11 1.469(5) . ? C95 C96 1.513(6) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C101 1.380(6) . ? C96 C97 1.381(6) . ? C97 C98 1.387(6) . ? C97 H97 0.9500 . ? C98 C99 1.386(6) . ? C98 H98 0.9500 . ? C99 C100 1.392(6) . ? C99 C102 1.509(6) . ? C100 C101 1.386(6) . ? C100 H100 0.9500 . ? C101 H101 0.9500 . ? C102 N12 1.454(5) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 O12 1.233(5) . ? C103 N12 1.339(5) . ? N9 H9 0.8800 . ? N10 H10N 0.8800 . ? N11 H11N 0.8800 . ? N12 H12N 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2B 111.6(8) . . ? N1 C1 C2A 111.9(5) . . ? C2B C1 C2A 6.6(13) . . ? N1 C1 H1A 109.2 . . ? C2B C1 H1A 103.6 . . ? C2A C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2B C1 H1B 115.0 . . ? C2A C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C9B C8 N1 122.8(9) . . ? C9B C8 C9A 15.4(10) . . ? N1 C8 C9A 110.8(5) . . ? C9B C8 H8A 95.1 . . ? N1 C8 H8A 109.5 . . ? C9A C8 H8A 109.5 . . ? C9B C8 H8B 110.3 . . ? N1 C8 H8B 109.5 . . ? C9A C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C3A C2A C7A 120.0 . . ? C3A C2A C1 118.3(8) . . ? C7A C2A C1 121.7(8) . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C7A C6A C5A 120.0 . . ? C7A C6A H6A 120.0 . . ? C5A C6A H6A 120.0 . . ? C6A C7A C2A 120.0 . . ? C6A C7A H7A 120.0 . . ? C2A C7A H7A 120.0 . . ? C3B C2B C7B 120.0 . . ? C3B C2B C1 122.4(15) . . ? C7B C2B C1 117.2(15) . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C6B C7B 120.0 . . ? C5B C6B H6B 120.0 . . ? C7B C6B H6B 120.0 . . ? C6B C7B C2B 120.0 . . ? C6B C7B H7B 120.0 . . ? C2B C7B H7B 120.0 . . ? C10A C9A C14A 120.0 . . ? C10A C9A C8 123.9(5) . . ? C14A C9A C8 116.1(5) . . ? C11A C10A C9A 120.0 . . ? C11A C10A H10A 120.0 . . ? C9A C10A H10A 120.0 . . ? C10A C11A C12A 120.0 . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C13A C14A C9A 120.0 . . ? C13A C14A H14A 120.0 . . ? C9A C14A H14A 120.0 . . ? C10B C9B C14B 120.0 . . ? C10B C9B C8 115.5(12) . . ? C14B C9B C8 122.6(12) . . ? C9B C10B C11B 120.0 . . ? C9B C10B H10B 120.0 . . ? C11B C10B H10B 120.0 . . ? C12B C11B C10B 120.0 . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B H13B 120.0 . . ? C14B C13B H13B 120.0 . . ? C13B C14B C9B 120.0 . . ? C13B C14B H14B 120.0 . . ? C9B C14B H14B 120.0 . . ? O1 C15 N1 121.4(4) . . ? O1 C15 C16 122.1(4) . . ? N1 C15 C16 116.5(4) . . ? C17 C16 C15 122.3(4) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? O2 C18 N2 122.7(4) . . ? O2 C18 C17 121.7(4) . . ? N2 C18 C17 115.6(4) . . ? N2 C19 C20 112.7(3) . . ? N2 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N2 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 110.5(3) . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N3 C21 C20 111.9(3) . . ? N3 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? N3 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O3 C22 N3 122.0(4) . . ? O3 C22 C23 121.7(4) . . ? N3 C22 C23 116.3(4) . . ? C24 C23 C22 121.8(4) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? O4 C25 N4 120.9(4) . . ? O4 C25 C24 121.5(4) . . ? N4 C25 C24 117.6(4) . . ? N4 C26 C27 116.1(3) . . ? N4 C26 H26A 108.3 . . ? C27 C26 H26A 108.3 . . ? N4 C26 H26B 108.3 . . ? C27 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C32 C27 C28 118.3(4) . . ? C32 C27 C26 122.0(4) . . ? C28 C27 C26 119.6(4) . . ? C29 C28 C27 121.0(4) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 119.9(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.6(4) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 119.4(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C27 C32 C31 120.7(4) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? N4 C33 C34 114.3(3) . . ? N4 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? N4 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C35 C34 C39 118.4(4) . . ? C35 C34 C33 123.0(4) . . ? C39 C34 C33 118.5(4) . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 120.1(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.0(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 119.6(4) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C34 120.9(4) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C15 N1 C8 123.3(4) . . ? C15 N1 C1 119.5(4) . . ? C8 N1 C1 116.9(4) . . ? C18 N2 C19 121.4(3) . . ? C18 N2 H2 119.3 . . ? C19 N2 H2 119.3 . . ? C22 N3 C21 122.4(4) . . ? C22 N3 H3N 118.8 . . ? C21 N3 H3N 118.8 . . ? C25 N4 C33 118.4(3) . . ? C25 N4 C26 123.7(3) . . ? C33 N4 C26 117.1(3) . . ? C45 C40 C41 119.2(4) . . ? C45 C40 C46 121.5(4) . . ? C41 C40 C46 119.2(4) . . ? C42 C41 C40 120.1(4) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.7(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 118.8(4) . . ? C43 C44 C71 119.5(4) . . ? C45 C44 C71 121.7(4) . . ? C40 C45 C44 120.9(4) . . ? C40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? O5 C46 N5 123.0(4) . . ? O5 C46 C40 121.6(4) . . ? N5 C46 C40 115.4(4) . . ? N5 C47 C48 113.0(3) . . ? N5 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? N5 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C53 118.1(4) . . ? C49 C48 C47 121.6(4) . . ? C53 C48 C47 120.3(4) . . ? C48 C49 C50 120.9(4) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C49 C50 C51 121.4(4) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C50 C51 C52 117.4(4) . . ? C50 C51 C54 121.5(4) . . ? C52 C51 C54 121.2(4) . . ? C53 C52 C51 121.2(5) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C48 121.0(4) . . ? C52 C53 H53 119.5 . . ? C48 C53 H53 119.5 . . ? N6 C54 C51 113.0(4) . . ? N6 C54 H54A 109.0 . . ? C51 C54 H54A 109.0 . . ? N6 C54 H54B 109.0 . . ? C51 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? O6 C55 N6 123.2(4) . . ? O6 C55 C56 120.3(4) . . ? N6 C55 C56 116.5(4) . . ? C57 C56 C61 119.5(4) . . ? C57 C56 C55 119.0(4) . . ? C61 C56 C55 121.5(4) . . ? C56 C57 C58 120.1(4) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C57 120.0(4) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C60 C59 C58 120.5(4) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 119.3(4) . . ? C59 C60 C62 118.3(4) . . ? C61 C60 C62 122.4(4) . . ? C56 C61 C60 120.6(4) . . ? C56 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? O7 C62 N7 121.0(4) . . ? O7 C62 C60 121.5(4) . . ? N7 C62 C60 117.5(4) . . ? N7 C63 C64 111.7(3) . . ? N7 C63 H63A 109.3 . . ? C64 C63 H63A 109.3 . . ? N7 C63 H63B 109.3 . . ? C64 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? C65 C64 C69 118.4(4) . . ? C65 C64 C63 120.6(4) . . ? C69 C64 C63 121.0(4) . . ? C66 C65 C64 120.5(4) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C65 C66 C67 120.7(4) . . ? C65 C66 H66 119.6 . . ? C67 C66 H66 119.6 . . ? C68 C67 C66 118.4(4) . . ? C68 C67 C70 121.2(4) . . ? C66 C67 C70 120.3(4) . . ? C69 C68 C67 121.3(4) . . ? C69 C68 H68 119.3 . . ? C67 C68 H68 119.3 . . ? C68 C69 C64 120.7(4) . . ? C68 C69 H69 119.7 . . ? C64 C69 H69 119.7 . . ? N8 C70 C67 112.2(3) . . ? N8 C70 H70A 109.2 . . ? C67 C70 H70A 109.2 . . ? N8 C70 H70B 109.2 . . ? C67 C70 H70B 109.2 . . ? H70A C70 H70B 107.9 . . ? O8 C71 N8 120.9(4) . . ? O8 C71 C44 120.8(4) . . ? N8 C71 C44 118.4(4) . . ? C46 N5 C47 123.0(4) . . ? C46 N5 H5 118.5 . . ? C47 N5 H5 118.5 . . ? C55 N6 C54 123.0(4) . . ? C55 N6 H6N 118.5 . . ? C54 N6 H6N 118.5 . . ? C62 N7 C63 119.8(3) . . ? C62 N7 H7N 120.1 . . ? C63 N7 H7N 120.1 . . ? C71 N8 C70 121.2(3) . . ? C71 N8 H8 119.4 . . ? C70 N8 H8 119.4 . . ? C301 C300 H30A 109.5 . . ? C301 C300 H30B 109.5 . . ? H30A C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30A C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? O301 C301 C300 107.8(8) . . ? O301 C301 H30D 110.1 . . ? C300 C301 H30D 110.1 . . ? O301 C301 H30E 110.1 . . ? C300 C301 H30E 110.1 . . ? H30D C301 H30E 108.5 . . ? C301 O301 H301 109.5 . . ? C08A C07A H07A 109.5 . . ? C08A C07A H07B 109.5 . . ? H07A C07A H07B 109.5 . . ? C08A C07A H07C 109.5 . . ? H07A C07A H07C 109.5 . . ? H07B C07A H07C 109.5 . . ? O09A C08A C07A 111.8(13) . . ? O09A C08A H08A 109.3 . . ? C07A C08A H08A 109.3 . . ? O09A C08A H08B 109.3 . . ? C07A C08A H08B 109.3 . . ? H08A C08A H08B 107.9 . . ? C08A O09A H09A 109.5 . . ? C08B C07B H07D 109.5 . . ? C08B C07B H07E 109.5 . . ? H07D C07B H07E 109.5 . . ? C08B C07B H07F 109.5 . . ? H07D C07B H07F 109.5 . . ? H07E C07B H07F 109.5 . . ? O09B C08B C07B 117(2) . . ? O09B C08B H08C 108.1 . . ? C07B C08B H08C 108.1 . . ? O09B C08B H08D 108.1 . . ? C07B C08B H08D 108.1 . . ? H08C C08B H08D 107.3 . . ? C08B O09B H09B 109.5 . . ? C02A C01A H01A 109.5 . . ? C02A C01A H01B 109.5 . . ? H01A C01A H01B 109.5 . . ? C02A C01A H01C 109.5 . . ? H01A C01A H01C 109.5 . . ? H01B C01A H01C 109.5 . . ? O03A C02A C01A 110.8(11) . . ? O03A C02A H02A 109.5 . . ? C01A C02A H02A 109.5 . . ? O03A C02A H02B 109.5 . . ? C01A C02A H02B 109.5 . . ? H02A C02A H02B 108.1 . . ? C02A O03A H03A 109.5 . . ? C02B C01B H01D 109.5 . . ? C02B C01B H01E 109.5 . . ? H01D C01B H01E 109.5 . . ? C02B C01B H01F 109.5 . . ? H01D C01B H01F 109.5 . . ? H01E C01B H01F 109.5 . . ? O03B C02B C01B 143(2) . . ? O03B C02B H02C 101.1 . . ? C01B C02B H02C 101.1 . . ? O03B C02B H02D 101.1 . . ? C01B C02B H02D 101.1 . . ? H02C C02B H02D 104.5 . . ? C02B O03B H03B 109.5 . . ? C012 C011 H01G 109.5 . . ? C012 C011 H01H 109.5 . . ? H01G C011 H01H 109.5 . . ? C012 C011 H01I 109.5 . . ? H01G C011 H01I 109.5 . . ? H01H C011 H01I 109.5 . . ? O04 C012 C011 111(2) . . ? O04 C012 H01J 109.5 . . ? C011 C012 H01J 109.5 . . ? O04 C012 H01K 109.5 . . ? C011 C012 H01K 109.5 . . ? H01J C012 H01K 108.0 . . ? C012 O04 H04 109.5 . . ? C77 C72 C73 120.7(4) . . ? C77 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C74 C73 C72 118.7(4) . . ? C74 C73 C103 118.4(3) . . ? C72 C73 C103 122.9(3) . . ? C75 C74 C73 120.7(4) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C74 C75 C76 119.8(4) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? C77 C76 C75 119.9(4) . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C72 C77 C76 120.1(4) . . ? C72 C77 C78 120.6(3) . . ? C76 C77 C78 119.2(3) . . ? O9 C78 N9 125.6(3) . . ? O9 C78 C77 120.6(3) . . ? N9 C78 C77 113.8(3) . . ? N9 C79 C80 111.4(3) . . ? N9 C79 H79A 109.3 . . ? C80 C79 H79A 109.3 . . ? N9 C79 H79B 109.3 . . ? C80 C79 H79B 109.3 . . ? H79A C79 H79B 108.0 . . ? C85 C80 C81 117.5(4) . . ? C85 C80 C79 119.6(4) . . ? C81 C80 C79 122.9(4) . . ? C80 C81 C82 119.7(5) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C83 C82 C81 121.4(5) . . ? C83 C82 H82 119.3 . . ? C81 C82 H82 119.3 . . ? C84 C83 C82 118.8(4) . . ? C84 C83 C86 120.1(5) . . ? C82 C83 C86 121.0(4) . . ? C83 C84 C85 120.1(5) . . ? C83 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C84 C85 C80 122.3(4) . . ? C84 C85 H85 118.8 . . ? C80 C85 H85 118.8 . . ? N10 C86 C83 111.4(4) . . ? N10 C86 H86A 109.3 . . ? C83 C86 H86A 109.3 . . ? N10 C86 H86B 109.3 . . ? C83 C86 H86B 109.3 . . ? H86A C86 H86B 108.0 . . ? O10 C87 N10 121.2(4) . . ? O10 C87 C88 122.2(4) . . ? N10 C87 C88 116.6(4) . . ? C93 C88 C89 118.7(4) . . ? C93 C88 C87 123.3(4) . . ? C89 C88 C87 118.0(4) . . ? C90 C89 C88 120.4(4) . . ? C90 C89 H89 119.8 . . ? C88 C89 H89 119.8 . . ? C91 C90 C89 120.4(4) . . ? C91 C90 H90 119.8 . . ? C89 C90 H90 119.8 . . ? C90 C91 C92 119.9(4) . . ? C90 C91 H91 120.0 . . ? C92 C91 H91 120.0 . . ? C93 C92 C91 118.8(4) . . ? C93 C92 C94 123.2(4) . . ? C91 C92 C94 118.0(4) . . ? C88 C93 C92 121.7(4) . . ? C88 C93 H93 119.1 . . ? C92 C93 H93 119.1 . . ? O11 C94 N11 121.0(4) . . ? O11 C94 C92 121.5(4) . . ? N11 C94 C92 117.4(4) . . ? N11 C95 C96 111.1(4) . . ? N11 C95 H95A 109.4 . . ? C96 C95 H95A 109.4 . . ? N11 C95 H95B 109.4 . . ? C96 C95 H95B 109.4 . . ? H95A C95 H95B 108.0 . . ? C101 C96 C97 118.9(4) . . ? C101 C96 C95 120.7(4) . . ? C97 C96 C95 120.4(4) . . ? C96 C97 C98 121.4(5) . . ? C96 C97 H97 119.3 . . ? C98 C97 H97 119.3 . . ? C99 C98 C97 120.0(4) . . ? C99 C98 H98 120.0 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 118.4(4) . . ? C98 C99 C102 120.0(4) . . ? C100 C99 C102 121.6(4) . . ? C101 C100 C99 121.2(5) . . ? C101 C100 H100 119.4 . . ? C99 C100 H100 119.4 . . ? C96 C101 C100 120.2(4) . . ? C96 C101 H101 119.9 . . ? C100 C101 H101 119.9 . . ? N12 C102 C99 111.4(3) . . ? N12 C102 H10C 109.3 . . ? C99 C102 H10C 109.3 . . ? N12 C102 H10D 109.3 . . ? C99 C102 H10D 109.3 . . ? H10C C102 H10D 108.0 . . ? O12 C103 N12 122.9(4) . . ? O12 C103 C73 120.3(4) . . ? N12 C103 C73 116.8(3) . . ? C78 N9 C79 124.1(3) . . ? C78 N9 H9 117.9 . . ? C79 N9 H9 117.9 . . ? C87 N10 C86 123.0(4) . . ? C87 N10 H10N 118.5 . . ? C86 N10 H10N 118.5 . . ? C94 N11 C95 120.5(4) . . ? C94 N11 H11N 119.8 . . ? C95 N11 H11N 119.8 . . ? C103 N12 C102 122.0(3) . . ? C103 N12 H12N 119.0 . . ? C102 N12 H12N 119.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O9 0.88 2.31 3.166(4) 165.6 2_756 N5 H5 O4 0.88 2.05 2.877(5) 155.2 . N6 H6N O3 0.88 2.21 3.080(4) 168.8 . N7 H7N O3 0.88 2.23 3.080(5) 161.0 . N9 H9 O1 0.88 2.05 2.889(4) 158.4 . N10 H10N O2 0.88 2.10 2.960(4) 165.2 . N11 H11N O2 0.88 2.52 3.398(5) 176.6 . N12 H12N O9 0.88 2.15 2.977(4) 155.9 2_756 O301 H301 O11 0.84 2.06 2.670(9) 129.3 1_655 O09A H09A O8 0.84 1.90 2.71(2) 163.9 2_655 O09B H09B O8 0.84 2.29 2.97(4) 138.1 2_655 O03A H03A O6 0.84 2.19 3.011(9) 166.4 1_565 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.743 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.062 data_[3]rotaxane_10 _database_code_depnum_ccdc_archive 'CCDC 922155' #TrackingRef '[3]rotaxanes_updated.cif' # start Validation Reply Form _vrf_PLAT029_3rotaxane_10 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.949 RESPONSE: The crystal was the best quality that could be grown, and the best dataset possible was obtained but despite this the diffraction was weak, especially at higher 2Theta angles. This lead to slightly low completeness. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H36 N4 O4, 2(C32 H28 N4 O4), 0.5(C2 H6 O), 0.5(C H4 O), 2(H2 O)' _chemical_formula_sum 'C102.50 H101 N12 O15' _chemical_formula_weight 1740.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.0536(3) _cell_length_b 38.7489(11) _cell_length_c 11.7046(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.610(2) _cell_angle_gamma 90.00 _cell_volume 4555.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7785 _cell_measurement_theta_min 3.781 _cell_measurement_theta_max 70.820 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8671 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details 'SADABS V2.07 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 19955 reflections reduced R(int) from 0.0392 to 0.0282 Ratio of minimum to maximum apparent transmission: 0.886955 The given Tmin and Tmax were generated using the SHELX SIZE command. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 6000' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27608 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 6.35 _diffrn_reflns_theta_max 66.58 _reflns_number_total 13650 _reflns_number_gt 12562 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART V5.626 (Bruker, 1997)' _computing_cell_refinement 'SAINT V6.28A (Bruker, 1997)' _computing_data_reduction 'SAINT V6.28A (Bruker, 1997)' _computing_structure_solution ; Sir2004 (Burla, Caliandro, Camalli, Carrozzini, Cascarano, De Caro, Giacovazzo, Polidori, & Spagna, 2005) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; OLEX2 (Dolomanov, O.V., Bourhis, L.J., Gildea, R.J., Howard, J.A.K, & Puschmann, H., 2009) ; _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains 0.5 ethanol molecules, 0.5 methanol molecules and 2 water molecules per [3]-rotaxane. The ethanol molecule O(301), C(301), C(302) and methanol molecule O(31'), C(31') are present on the same site at 50 % occupancy each. The water molecule O(501), O(51'), O(5'') is disordered over three positions at a percentage occupancy ratio of 60:25:15. O(5'') had to be refined isotropically. It was not possible to refine hydrogen atom positions for this water molecule or for the methanol molecule O(31'), C(31'). As a result of this it was not possible to list all the hydrogen bonding. All hydrogen atoms not belonging to water molecules were fixed as riding models. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+1.0238P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(17) _chemical_absolute_configuration unk _refine_ls_number_reflns 13650 _refine_ls_number_parameters 1191 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6549(3) 0.49436(9) 0.0078(3) 0.0353(7) Uani 1 1 d . . . C2 C 0.6131(3) 0.52588(9) 0.0475(3) 0.0388(7) Uani 1 1 d . . . H2 H 0.5401 0.5270 0.0961 0.047 Uiso 1 1 calc R . . C3 C 0.6781(3) 0.55616(9) 0.0164(3) 0.0394(7) Uani 1 1 d . . . H3 H 0.6492 0.5779 0.0438 0.047 Uiso 1 1 calc R . . C4 C 0.7834(3) 0.55440(8) -0.0535(3) 0.0357(7) Uani 1 1 d . . . H4 H 0.8254 0.5750 -0.0770 0.043 Uiso 1 1 calc R . . C5 C 0.8291(3) 0.52273(9) -0.0901(3) 0.0404(7) Uani 1 1 d . . . H5 H 0.9037 0.5215 -0.1368 0.048 Uiso 1 1 calc R . . C6 C 0.7655(3) 0.49296(9) -0.0581(3) 0.0374(7) Uani 1 1 d . . . H6 H 0.7981 0.4712 -0.0817 0.045 Uiso 1 1 calc R . . C7 C 0.5802(4) 0.46162(10) 0.0341(3) 0.0439(8) Uani 1 1 d . . . H7A H 0.4845 0.4671 0.0398 0.053 Uiso 1 1 calc R . . H7B H 0.5885 0.4452 -0.0299 0.053 Uiso 1 1 calc R . . C8 C 0.5939(3) 0.46097(8) 0.2458(3) 0.0364(7) Uani 1 1 d . . . C9 C 0.4658(4) 0.45739(11) 0.2837(4) 0.0537(9) Uani 1 1 d . . . H9 H 0.4019 0.4440 0.2409 0.064 Uiso 1 1 calc R . . C10 C 0.4318(4) 0.47312(13) 0.3822(4) 0.0656(12) Uani 1 1 d . . . H10 H 0.3441 0.4705 0.4081 0.079 Uiso 1 1 calc R . . C11 C 0.5231(4) 0.49274(11) 0.4447(4) 0.0574(10) Uani 1 1 d . . . H11 H 0.4990 0.5034 0.5139 0.069 Uiso 1 1 calc R . . C12 C 0.6502(4) 0.49689(10) 0.4062(3) 0.0499(9) Uani 1 1 d . . . H12 H 0.7133 0.5106 0.4486 0.060 Uiso 1 1 calc R . . C13 C 0.6852(3) 0.48113(9) 0.3068(3) 0.0412(8) Uani 1 1 d . . . H13 H 0.7723 0.4841 0.2801 0.049 Uiso 1 1 calc R . . C14 C 0.7173(3) 0.41880(9) 0.1366(3) 0.0371(7) Uani 1 1 d . . . C15 C 0.7520(3) 0.40015(8) 0.2435(3) 0.0350(7) Uani 1 1 d . . . H15 H 0.7174 0.4077 0.3134 0.042 Uiso 1 1 calc R . . C16 C 0.8304(3) 0.37310(8) 0.2424(3) 0.0359(7) Uani 1 1 d . . . H16 H 0.8641 0.3656 0.1720 0.043 Uiso 1 1 calc R . . C17 C 0.8672(3) 0.35403(8) 0.3486(3) 0.0323(6) Uani 1 1 d . . . C18 C 1.0209(3) 0.31254(9) 0.4386(3) 0.0433(8) Uani 1 1 d . . . H18A H 1.0003 0.3255 0.5086 0.052 Uiso 1 1 calc R . . H18B H 1.1188 0.3124 0.4329 0.052 Uiso 1 1 calc R . . C19 C 0.9722(3) 0.27547(9) 0.4500(3) 0.0418(8) Uani 1 1 d . . . H19A H 0.9914 0.2627 0.3794 0.050 Uiso 1 1 calc R . . H19B H 1.0230 0.2643 0.5144 0.050 Uiso 1 1 calc R . . C20 C 0.8255(3) 0.27251(8) 0.4702(3) 0.0371(7) Uani 1 1 d . . . H20A H 0.8059 0.2842 0.5427 0.044 Uiso 1 1 calc R . . H20B H 0.7737 0.2841 0.4074 0.044 Uiso 1 1 calc R . . C21 C 0.7232(3) 0.22039(8) 0.3891(3) 0.0317(6) Uani 1 1 d . . . C22 C 0.6995(3) 0.18295(8) 0.4060(2) 0.0303(6) Uani 1 1 d . . . H22 H 0.7282 0.1725 0.4762 0.036 Uiso 1 1 calc R . . C23 C 0.6398(3) 0.16407(8) 0.3262(3) 0.0323(6) Uani 1 1 d . . . H23 H 0.6102 0.1746 0.2563 0.039 Uiso 1 1 calc R . . C24 C 0.6172(3) 0.12656(8) 0.3423(2) 0.0286(6) Uani 1 1 d . . . C25 C 0.4778(3) 0.12599(7) 0.1649(3) 0.0294(6) Uani 1 1 d . . . C26 C 0.3445(3) 0.13434(8) 0.1597(3) 0.0344(7) Uani 1 1 d . . . H26 H 0.2916 0.1301 0.2234 0.041 Uiso 1 1 calc R . . C27 C 0.2883(3) 0.14889(9) 0.0612(3) 0.0430(8) Uani 1 1 d . . . H27 H 0.1963 0.1546 0.0572 0.052 Uiso 1 1 calc R . . C28 C 0.3649(4) 0.15518(9) -0.0314(3) 0.0436(8) Uani 1 1 d . . . H28 H 0.3261 0.1655 -0.0986 0.052 Uiso 1 1 calc R . . C29 C 0.4979(4) 0.14645(9) -0.0262(3) 0.0396(7) Uani 1 1 d . . . H29 H 0.5507 0.1506 -0.0900 0.048 Uiso 1 1 calc R . . C30 C 0.5542(3) 0.13178(8) 0.0716(3) 0.0344(7) Uani 1 1 d . . . H30 H 0.6458 0.1256 0.0749 0.041 Uiso 1 1 calc R . . C31 C 0.5076(3) 0.07340(8) 0.2868(3) 0.0347(7) Uani 1 1 d . . . H31A H 0.4264 0.0668 0.2409 0.042 Uiso 1 1 calc R . . H31B H 0.4892 0.0702 0.3685 0.042 Uiso 1 1 calc R . . C32 C 0.6197(3) 0.04983(8) 0.2568(3) 0.0344(7) Uani 1 1 d . . . C33 C 0.6484(3) 0.04388(8) 0.1442(3) 0.0406(7) Uani 1 1 d . . . H33 H 0.5989 0.0556 0.0850 0.049 Uiso 1 1 calc R . . C34 C 0.7478(4) 0.02121(9) 0.1163(4) 0.0510(9) Uani 1 1 d . . . H34 H 0.7652 0.0171 0.0384 0.061 Uiso 1 1 calc R . . C35 C 0.8222(4) 0.00438(9) 0.2022(4) 0.0506(10) Uani 1 1 d . . . H35 H 0.8900 -0.0114 0.1831 0.061 Uiso 1 1 calc R . . C36 C 0.7978(4) 0.01056(9) 0.3136(4) 0.0501(10) Uani 1 1 d . . . H36 H 0.8504 -0.0004 0.3724 0.060 Uiso 1 1 calc R . . C37 C 0.6963(3) 0.03286(8) 0.3418(3) 0.0404(8) Uani 1 1 d . . . H37 H 0.6788 0.0366 0.4199 0.048 Uiso 1 1 calc R . . N1 N 0.6291(3) 0.44503(7) 0.1409(2) 0.0390(6) Uani 1 1 d . . . N2 N 0.9613(3) 0.33027(7) 0.3400(2) 0.0393(6) Uani 1 1 d . . . H2A H 0.9886 0.3251 0.2717 0.047 Uiso 1 1 calc R . . N3 N 0.7853(3) 0.23631(7) 0.4759(2) 0.0350(6) Uani 1 1 d . . . H3A H 0.8032 0.2247 0.5394 0.042 Uiso 1 1 calc R . . N4 N 0.5366(2) 0.11021(6) 0.2663(2) 0.0294(5) Uani 1 1 d . . . O1 O 0.7643(2) 0.41000(6) 0.04442(19) 0.0435(5) Uani 1 1 d . . . O2 O 0.8151(2) 0.36051(6) 0.43965(18) 0.0378(5) Uani 1 1 d . . . O3 O 0.6852(2) 0.23502(6) 0.29941(18) 0.0396(5) Uani 1 1 d . . . O4 O 0.6695(2) 0.11126(5) 0.42567(17) 0.0331(5) Uani 1 1 d . . . C101 C 1.1265(4) 0.41322(12) -0.0806(3) 0.0543(10) Uani 1 1 d D . . C102 C 1.0608(4) 0.38359(13) -0.1476(3) 0.0575(11) Uani 1 1 d D . . C103 C 1.1421(4) 0.35949(15) -0.1987(4) 0.0670(12) Uani 1 1 d . . . H103 H 1.2359 0.3627 -0.1971 0.080 Uiso 1 1 calc R . . C104 C 1.0853(5) 0.33086(18) -0.2516(4) 0.0833(17) Uani 1 1 d . . . H104 H 1.1409 0.3148 -0.2878 0.100 Uiso 1 1 calc R . . C105 C 0.9487(5) 0.32506(15) -0.2533(4) 0.0702(13) Uani 1 1 d . . . H105 H 0.9116 0.3046 -0.2862 0.084 Uiso 1 1 calc R . . C106 C 0.8659(4) 0.35024(13) -0.2050(3) 0.0550(11) Uani 1 1 d . . . C107 C 0.9240(4) 0.37917(11) -0.1542(3) 0.0489(9) Uani 1 1 d . . . H107 H 0.8687 0.3964 -0.1233 0.059 Uiso 1 1 calc R . . C108 C 0.7207(4) 0.34276(12) -0.2031(3) 0.0530(10) Uani 1 1 d . . . C109 C 0.5176(3) 0.35481(10) -0.1002(3) 0.0437(8) Uani 1 1 d . . . H10A H 0.4824 0.3350 -0.1456 0.052 Uiso 1 1 calc R . . H10B H 0.4638 0.3754 -0.1218 0.052 Uiso 1 1 calc R . . C110 C 0.5060(3) 0.34743(9) 0.0258(3) 0.0355(7) Uani 1 1 d . . . C111 C 0.5738(4) 0.32029(8) 0.0765(3) 0.0423(8) Uani 1 1 d . . . H111 H 0.6285 0.3062 0.0317 0.051 Uiso 1 1 calc R . . C112 C 0.5640(4) 0.31305(8) 0.1914(3) 0.0391(7) Uani 1 1 d . . . H112 H 0.6110 0.2940 0.2244 0.047 Uiso 1 1 calc R . . C113 C 0.4868(3) 0.33335(8) 0.2582(3) 0.0335(7) Uani 1 1 d . . . C114 C 0.4214(3) 0.36125(11) 0.2085(3) 0.0488(9) Uani 1 1 d . . . H114 H 0.3696 0.3759 0.2541 0.059 Uiso 1 1 calc R . . C115 C 0.4300(4) 0.36820(11) 0.0940(3) 0.0485(9) Uani 1 1 d . . . H115 H 0.3835 0.3874 0.0612 0.058 Uiso 1 1 calc R . . C116 C 0.4739(3) 0.32557(9) 0.3838(3) 0.0376(7) Uani 1 1 d . . . H11A H 0.3795 0.3205 0.3980 0.045 Uiso 1 1 calc R . . H11B H 0.5268 0.3047 0.4042 0.045 Uiso 1 1 calc R . . C117 C 0.4439(3) 0.36952(9) 0.5322(3) 0.0384(7) Uani 1 1 d . . . C118 C 0.5077(3) 0.39897(9) 0.5975(3) 0.0360(7) Uani 1 1 d . . . C119 C 0.4293(3) 0.42079(11) 0.6606(3) 0.0453(8) Uani 1 1 d . . . H119 H 0.3368 0.4164 0.6656 0.054 Uiso 1 1 calc R . . C120 C 0.4866(4) 0.44876(11) 0.7157(3) 0.0499(9) Uani 1 1 d . . . H120 H 0.4337 0.4634 0.7602 0.060 Uiso 1 1 calc R . . C121 C 0.6202(4) 0.45569(10) 0.7070(3) 0.0460(8) Uani 1 1 d . . . H121 H 0.6572 0.4758 0.7425 0.055 Uiso 1 1 calc R . . C122 C 0.7015(3) 0.43392(9) 0.6474(3) 0.0370(7) Uani 1 1 d . . . C123 C 0.6423(3) 0.40576(9) 0.5940(3) 0.0428(8) Uani 1 1 d . . . H123 H 0.6964 0.3904 0.5532 0.051 Uiso 1 1 calc R . . C124 C 0.8459(3) 0.44157(9) 0.6421(3) 0.0438(8) Uani 1 1 d . . . C125 C 1.0562(3) 0.42488(10) 0.5564(3) 0.0436(8) Uani 1 1 d . . . H12A H 1.1041 0.4031 0.5753 0.052 Uiso 1 1 calc R . . H12B H 1.0940 0.4433 0.6067 0.052 Uiso 1 1 calc R . . C126 C 1.0758(3) 0.43411(9) 0.4339(3) 0.0443(8) Uani 1 1 d . . . C127 C 1.0385(4) 0.46585(10) 0.3893(4) 0.0518(9) Uani 1 1 d . . . H127 H 1.0056 0.4832 0.4381 0.062 Uiso 1 1 calc R . . C128 C 1.0488(4) 0.47253(10) 0.2745(4) 0.0573(11) Uani 1 1 d . . . H128 H 1.0235 0.4947 0.2464 0.069 Uiso 1 1 calc R . . C129 C 1.0947(3) 0.44829(10) 0.1972(4) 0.0465(9) Uani 1 1 d . . . C130 C 1.1322(3) 0.41685(9) 0.2428(3) 0.0434(8) Uani 1 1 d . . . H130 H 1.1633 0.3994 0.1936 0.052 Uiso 1 1 calc R . . C131 C 1.1259(3) 0.41001(9) 0.3574(3) 0.0400(7) Uani 1 1 d . . . H131 H 1.1564 0.3883 0.3859 0.048 Uiso 1 1 calc R . . C132 C 1.1026(4) 0.45595(11) 0.0723(4) 0.0557(10) Uani 1 1 d . . . H13A H 1.0513 0.4772 0.0546 0.067 Uiso 1 1 calc R . . H13B H 1.1967 0.4606 0.0559 0.067 Uiso 1 1 calc R . . N101 N 1.0535(3) 0.42895(10) -0.0023(3) 0.0551(9) Uani 1 1 d . . . H101 H 0.9705 0.4223 0.0035 0.066 Uiso 1 1 calc R . . N102 N 0.6549(3) 0.36075(9) -0.1254(2) 0.0454(7) Uani 1 1 d . . . H102 H 0.6982 0.3772 -0.0876 0.054 Uiso 1 1 calc R . . N103 N 0.5190(3) 0.35401(7) 0.4557(2) 0.0361(6) Uani 1 1 d . . . H10C H 0.6007 0.3616 0.4488 0.043 Uiso 1 1 calc R . . N104 N 0.9152(3) 0.42064(8) 0.5767(2) 0.0412(6) Uani 1 1 d . . . H10D H 0.8731 0.4031 0.5437 0.049 Uiso 1 1 calc R . . O101 O 1.2444(3) 0.42079(9) -0.0941(3) 0.0711(9) Uani 1 1 d . . . O102 O 0.6687(3) 0.32063(9) -0.2667(2) 0.0669(8) Uani 1 1 d . . . O103 O 0.3287(2) 0.36032(8) 0.5493(2) 0.0540(7) Uani 1 1 d . . . O104 O 0.8968(3) 0.46623(9) 0.6945(3) 0.0787(10) Uani 1 1 d . . . C201 C 0.6908(4) 0.22101(9) -0.0380(3) 0.0426(8) Uani 1 1 d . . . C202 C 0.5508(4) 0.23245(8) -0.0238(3) 0.0399(8) Uani 1 1 d . . . C203 C 0.4774(4) 0.24294(11) -0.1186(3) 0.0544(10) Uani 1 1 d . . . H203 H 0.5159 0.2433 -0.1912 0.065 Uiso 1 1 calc R . . C204 C 0.3471(5) 0.25292(14) -0.1077(3) 0.0721(14) Uani 1 1 d . . . H204 H 0.2956 0.2602 -0.1734 0.087 Uiso 1 1 calc R . . C205 C 0.2906(4) 0.25250(13) -0.0026(3) 0.0620(11) Uani 1 1 d . . . H205 H 0.2000 0.2591 0.0029 0.074 Uiso 1 1 calc R . . C206 C 0.3641(3) 0.24263(9) 0.0950(3) 0.0392(7) Uani 1 1 d . . . C207 C 0.4931(3) 0.23196(7) 0.0821(2) 0.0333(7) Uani 1 1 d . . . H207 H 0.5442 0.2240 0.1472 0.040 Uiso 1 1 calc R . . C208 C 0.3023(3) 0.24452(8) 0.2084(3) 0.0370(7) Uani 1 1 d . . . C209 C 0.3341(3) 0.23899(8) 0.4178(3) 0.0368(7) Uani 1 1 d . . . H20C H 0.2374 0.2439 0.4152 0.044 Uiso 1 1 calc R . . H20D H 0.3800 0.2579 0.4608 0.044 Uiso 1 1 calc R . . C210 C 0.3601(3) 0.20524(8) 0.4796(3) 0.0329(6) Uani 1 1 d . . . C211 C 0.3070(3) 0.17477(8) 0.4361(3) 0.0382(7) Uani 1 1 d . . . H211 H 0.2553 0.1750 0.3661 0.046 Uiso 1 1 calc R . . C212 C 0.3285(3) 0.14384(9) 0.4935(3) 0.0386(7) Uani 1 1 d . . . H212 H 0.2908 0.1232 0.4626 0.046 Uiso 1 1 calc R . . C213 C 0.4042(3) 0.14264(9) 0.5952(3) 0.0393(7) Uani 1 1 d . . . C214 C 0.4593(4) 0.17345(9) 0.6375(3) 0.0435(8) Uani 1 1 d . . . H214 H 0.5133 0.1732 0.7062 0.052 Uiso 1 1 calc R . . C215 C 0.4369(4) 0.20414(9) 0.5813(3) 0.0418(8) Uani 1 1 d . . . H215 H 0.4742 0.2248 0.6122 0.050 Uiso 1 1 calc R . . C216 C 0.4288(4) 0.10893(9) 0.6576(3) 0.0452(8) Uani 1 1 d . . . H21A H 0.4018 0.1112 0.7375 0.054 Uiso 1 1 calc R . . H21B H 0.3743 0.0905 0.6202 0.054 Uiso 1 1 calc R . . C217 C 0.6354(4) 0.08525(8) 0.7460(3) 0.0422(8) Uani 1 1 d . . . C218 C 0.7806(4) 0.07871(8) 0.7322(3) 0.0402(8) Uani 1 1 d . . . C219 C 0.8617(5) 0.07361(12) 0.8296(3) 0.0606(11) Uani 1 1 d . . . H219 H 0.8243 0.0734 0.9026 0.073 Uiso 1 1 calc R . . C220 C 0.9959(5) 0.06886(15) 0.8206(4) 0.0752(14) Uani 1 1 d . . . H220 H 1.0506 0.0655 0.8880 0.090 Uiso 1 1 calc R . . C221 C 1.0530(4) 0.06884(12) 0.7164(4) 0.0599(11) Uani 1 1 d . . . H221 H 1.1463 0.0656 0.7120 0.072 Uiso 1 1 calc R . . C222 C 0.9738(4) 0.07357(9) 0.6176(3) 0.0414(8) Uani 1 1 d . . . C223 C 0.8376(3) 0.07797(8) 0.6272(3) 0.0365(7) Uani 1 1 d . . . H223 H 0.7822 0.0805 0.5598 0.044 Uiso 1 1 calc R . . C224 C 1.0385(3) 0.07377(8) 0.5049(3) 0.0378(7) Uani 1 1 d . . . C225 C 1.0059(3) 0.08384(9) 0.2989(3) 0.0401(7) Uani 1 1 d . . . H22A H 0.9598 0.0648 0.2566 0.048 Uiso 1 1 calc R . . H22B H 1.1026 0.0790 0.3006 0.048 Uiso 1 1 calc R . . C226 C 0.9789(3) 0.11739(9) 0.2361(3) 0.0347(7) Uani 1 1 d . . . C227 C 0.9311(3) 0.11749(9) 0.1230(3) 0.0402(7) Uani 1 1 d . . . H227 H 0.9124 0.0962 0.0853 0.048 Uiso 1 1 calc R . . C228 C 0.9103(3) 0.14800(10) 0.0646(3) 0.0428(8) Uani 1 1 d . . . H228 H 0.8776 0.1475 -0.0129 0.051 Uiso 1 1 calc R . . C229 C 0.9364(3) 0.17944(9) 0.1170(3) 0.0401(7) Uani 1 1 d . . . C230 C 0.9845(3) 0.17951(9) 0.2297(3) 0.0417(7) Uani 1 1 d . . . H230 H 1.0040 0.2008 0.2670 0.050 Uiso 1 1 calc R . . C231 C 1.0044(3) 0.14891(9) 0.2885(3) 0.0389(7) Uani 1 1 d . . . H231 H 1.0362 0.1495 0.3662 0.047 Uiso 1 1 calc R . . C232 C 0.9126(4) 0.21305(10) 0.0544(3) 0.0499(9) Uani 1 1 d . . . H23A H 0.9683 0.2313 0.0914 0.060 Uiso 1 1 calc R . . H23B H 0.9399 0.2105 -0.0254 0.060 Uiso 1 1 calc R . . N201 N 0.7736(3) 0.22340(8) 0.0537(2) 0.0448(7) Uani 1 1 d . . . H201 H 0.7426 0.2317 0.1172 0.054 Uiso 1 1 calc R . . N202 N 0.3806(3) 0.23818(7) 0.3008(2) 0.0354(6) Uani 1 1 d . . . H202 H 0.4647 0.2332 0.2912 0.042 Uiso 1 1 calc R . . N203 N 0.5682(3) 0.09965(8) 0.6569(2) 0.0434(7) Uani 1 1 d . . . H20E H 0.6112 0.1037 0.5944 0.052 Uiso 1 1 calc R . . N204 N 0.9622(3) 0.08459(7) 0.4136(2) 0.0377(6) Uani 1 1 d . . . H20F H 0.8818 0.0925 0.4253 0.045 Uiso 1 1 calc R . . O201 O 0.7259(3) 0.21059(8) -0.1306(2) 0.0610(7) Uani 1 1 d . . . O202 O 0.1829(2) 0.25158(7) 0.2154(2) 0.0507(6) Uani 1 1 d . . . O203 O 0.5831(3) 0.07876(7) 0.8363(2) 0.0557(7) Uani 1 1 d . . . O204 O 1.1547(2) 0.06567(7) 0.4966(2) 0.0541(7) Uani 1 1 d . . . C301 C 0.9490(7) 0.17185(17) 0.6915(6) 0.1008(19) Uani 0.50 1 d PD A 1 H31D H 0.9047 0.1553 0.7419 0.121 Uiso 0.50 1 calc PR A 1 H31E H 0.9533 0.1608 0.6154 0.121 Uiso 0.50 1 calc PR A 1 C302 C 1.0752(9) 0.1767(4) 0.7338(9) 0.095(4) Uani 0.50 1 d PD A 1 H32A H 1.1025 0.1569 0.7815 0.142 Uiso 0.50 1 calc PR A 1 H32B H 1.0793 0.1978 0.7800 0.142 Uiso 0.50 1 calc PR A 1 H32C H 1.1351 0.1789 0.6704 0.142 Uiso 0.50 1 calc PR A 1 O301 O 0.8669(3) 0.20185(10) 0.6795(2) 0.0765(10) Uani 0.50 1 d P A 1 H31C H 0.8304 0.2057 0.7414 0.115 Uiso 0.50 1 calc PR A 1 C31' C 0.9490(7) 0.17185(17) 0.6915(6) 0.1008(19) Uani 0.50 1 d P B 2 O31' O 0.8669(3) 0.20185(10) 0.6795(2) 0.0765(10) Uani 0.50 1 d P B 2 O401 O 0.4126(4) 0.29402(8) 0.6506(2) 0.0722(10) Uani 1 1 d D . . H41B H 0.384(5) 0.3147(8) 0.638(6) 0.108 Uiso 1 1 d D . . H41A H 0.501(2) 0.2905(15) 0.649(6) 0.108 Uiso 1 1 d D . . O501 O 0.0531(5) 0.30771(15) 0.1319(3) 0.0626(15) Uani 0.60 1 d P C 1 O51' O 0.1103(15) 0.3237(3) 0.0687(12) 0.070(4) Uani 0.25 1 d P D 2 O5'' O -0.0342(12) 0.3061(3) 0.0528(10) 0.024(3) Uiso 0.15 1 d P E 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0348(15) 0.0386(17) 0.0315(15) -0.0002(14) -0.0079(13) -0.0009(14) C2 0.0358(16) 0.0466(19) 0.0339(16) 0.0032(15) 0.0016(14) 0.0053(15) C3 0.0445(18) 0.0337(16) 0.0394(17) -0.0003(14) -0.0031(15) 0.0058(15) C4 0.0330(15) 0.0346(16) 0.0387(16) 0.0046(14) -0.0071(13) -0.0028(14) C5 0.0358(16) 0.0438(18) 0.0413(17) 0.0054(15) -0.0011(14) 0.0022(15) C6 0.0396(16) 0.0349(16) 0.0372(16) -0.0034(14) -0.0029(14) 0.0037(14) C7 0.0404(18) 0.0435(18) 0.0467(18) 0.0056(16) -0.0085(15) -0.0050(16) C8 0.0292(15) 0.0328(16) 0.0470(18) 0.0098(15) -0.0009(14) -0.0005(13) C9 0.0321(17) 0.059(2) 0.070(2) -0.003(2) 0.0013(17) -0.0076(17) C10 0.0372(19) 0.082(3) 0.079(3) -0.001(3) 0.017(2) -0.001(2) C11 0.057(2) 0.057(2) 0.059(2) -0.001(2) 0.0110(19) 0.015(2) C12 0.049(2) 0.0442(19) 0.056(2) -0.0005(18) -0.0021(17) 0.0032(17) C13 0.0309(16) 0.0440(18) 0.0483(19) 0.0005(16) -0.0008(15) -0.0078(15) C14 0.0296(15) 0.0385(17) 0.0431(17) 0.0022(15) 0.0014(14) -0.0080(14) C15 0.0290(15) 0.0362(16) 0.0401(16) -0.0002(14) 0.0045(13) -0.0067(13) C16 0.0322(16) 0.0341(16) 0.0419(17) -0.0022(14) 0.0078(14) -0.0060(14) C17 0.0269(14) 0.0278(14) 0.0423(17) -0.0059(13) 0.0038(13) -0.0073(13) C18 0.0314(16) 0.0407(18) 0.058(2) 0.0051(17) 0.0015(15) -0.0030(15) C19 0.0386(18) 0.0358(17) 0.0510(19) 0.0036(16) 0.0016(15) 0.0002(15) C20 0.0399(17) 0.0332(15) 0.0379(16) -0.0053(14) 0.0002(14) -0.0042(14) C21 0.0318(15) 0.0338(15) 0.0295(15) -0.0009(13) 0.0004(12) -0.0021(13) C22 0.0337(15) 0.0313(15) 0.0255(13) 0.0039(13) -0.0014(12) -0.0007(13) C23 0.0355(15) 0.0296(14) 0.0313(15) 0.0059(13) -0.0040(13) 0.0007(13) C24 0.0277(14) 0.0287(14) 0.0295(14) -0.0021(13) 0.0008(12) 0.0005(12) C25 0.0323(15) 0.0237(13) 0.0318(15) -0.0026(12) -0.0035(12) 0.0020(12) C26 0.0326(15) 0.0322(15) 0.0382(16) -0.0047(13) -0.0018(13) -0.0002(13) C27 0.0360(16) 0.0395(17) 0.0520(19) -0.0087(16) -0.0128(15) 0.0058(15) C28 0.059(2) 0.0338(17) 0.0366(17) -0.0008(14) -0.0145(16) 0.0055(16) C29 0.0518(19) 0.0370(16) 0.0300(15) 0.0002(14) 0.0004(14) -0.0026(16) C30 0.0343(15) 0.0342(16) 0.0345(15) -0.0029(13) 0.0000(13) 0.0034(13) C31 0.0349(16) 0.0261(14) 0.0430(16) 0.0039(13) -0.0001(14) -0.0049(13) C32 0.0307(15) 0.0233(14) 0.0485(18) 0.0025(14) -0.0046(14) -0.0044(12) C33 0.0431(18) 0.0294(15) 0.0486(19) -0.0015(15) -0.0049(15) 0.0017(14) C34 0.050(2) 0.0359(18) 0.067(2) -0.0068(18) 0.0059(19) 0.0020(17) C35 0.0343(17) 0.0275(16) 0.090(3) -0.0018(19) 0.0005(19) 0.0008(14) C36 0.0415(18) 0.0261(15) 0.080(3) 0.0092(18) -0.0212(19) -0.0004(14) C37 0.0421(18) 0.0281(15) 0.0500(19) 0.0077(15) -0.0081(15) -0.0052(14) N1 0.0363(14) 0.0411(15) 0.0393(14) 0.0031(13) -0.0018(12) -0.0067(12) N2 0.0398(15) 0.0351(14) 0.0441(15) 0.0001(12) 0.0120(12) 0.0011(12) N3 0.0431(14) 0.0327(13) 0.0289(12) -0.0007(11) -0.0015(11) -0.0084(12) N4 0.0314(12) 0.0237(11) 0.0327(13) 0.0015(10) -0.0034(11) -0.0021(10) O1 0.0443(12) 0.0481(13) 0.0385(12) 0.0004(11) 0.0068(10) -0.0077(11) O2 0.0403(12) 0.0354(11) 0.0384(11) -0.0050(10) 0.0075(10) -0.0035(10) O3 0.0530(14) 0.0306(11) 0.0340(11) 0.0025(9) -0.0095(10) -0.0028(10) O4 0.0353(11) 0.0326(11) 0.0310(11) 0.0051(9) -0.0025(9) 0.0004(9) C101 0.0349(18) 0.071(3) 0.057(2) 0.030(2) 0.0108(17) 0.0072(19) C102 0.0395(19) 0.096(3) 0.0376(18) 0.019(2) 0.0092(16) 0.016(2) C103 0.046(2) 0.104(4) 0.052(2) -0.008(3) 0.0066(19) 0.012(2) C104 0.060(3) 0.135(5) 0.056(3) -0.020(3) 0.004(2) 0.031(3) C105 0.059(3) 0.103(4) 0.048(2) -0.024(2) -0.0027(19) 0.020(3) C106 0.051(2) 0.087(3) 0.0275(16) 0.0031(19) 0.0053(15) 0.013(2) C107 0.0397(19) 0.067(2) 0.0405(18) 0.0196(18) 0.0114(16) 0.0110(18) C108 0.051(2) 0.079(3) 0.0298(16) 0.0037(19) 0.0004(15) 0.008(2) C109 0.0378(17) 0.054(2) 0.0391(17) -0.0034(16) -0.0015(14) -0.0039(16) C110 0.0305(15) 0.0403(17) 0.0354(16) -0.0025(14) -0.0006(13) -0.0087(14) C111 0.054(2) 0.0297(16) 0.0434(18) -0.0090(14) 0.0084(16) 0.0025(15) C112 0.0506(19) 0.0275(15) 0.0393(17) 0.0001(14) 0.0040(15) -0.0035(15) C113 0.0286(15) 0.0376(16) 0.0343(15) -0.0021(14) 0.0033(13) -0.0091(14) C114 0.0345(17) 0.068(2) 0.0442(19) -0.0011(18) 0.0062(15) 0.0149(18) C115 0.0397(18) 0.063(2) 0.0428(18) 0.0105(18) 0.0016(15) 0.0115(17) C116 0.0375(17) 0.0396(17) 0.0359(16) -0.0033(14) 0.0033(14) -0.0089(14) C117 0.0316(16) 0.0463(18) 0.0376(16) -0.0001(15) 0.0037(14) 0.0048(15) C118 0.0333(16) 0.0427(17) 0.0322(15) -0.0022(14) 0.0030(13) 0.0049(14) C119 0.0337(16) 0.065(2) 0.0373(17) -0.0025(17) -0.0017(14) 0.0128(17) C120 0.0439(19) 0.066(2) 0.0390(17) -0.0204(18) -0.0067(15) 0.0228(18) C121 0.0462(19) 0.050(2) 0.0403(17) -0.0136(16) -0.0104(15) 0.0127(17) C122 0.0362(16) 0.0392(17) 0.0355(16) -0.0113(14) -0.0009(13) 0.0046(14) C123 0.0341(17) 0.0464(19) 0.0480(19) -0.0130(16) 0.0042(15) 0.0064(15) C124 0.0400(18) 0.0439(19) 0.0472(19) -0.0159(17) -0.0021(15) 0.0011(16) C125 0.0309(16) 0.0463(19) 0.053(2) -0.0141(17) -0.0084(15) -0.0015(15) C126 0.0208(14) 0.0418(18) 0.070(2) -0.0084(18) -0.0047(15) -0.0079(14) C127 0.0406(19) 0.044(2) 0.070(3) -0.0008(19) -0.0049(18) -0.0037(17) C128 0.0310(17) 0.0398(19) 0.101(3) 0.016(2) -0.006(2) -0.0088(15) C129 0.0245(15) 0.046(2) 0.069(2) 0.0084(19) 0.0036(16) -0.0090(15) C130 0.0238(14) 0.0433(18) 0.063(2) 0.0037(18) 0.0033(15) -0.0034(14) C131 0.0271(15) 0.0384(17) 0.054(2) 0.0012(16) -0.0003(14) -0.0054(14) C132 0.0380(19) 0.050(2) 0.080(3) 0.017(2) 0.0069(19) -0.0046(17) N101 0.0322(15) 0.077(2) 0.0565(18) 0.0193(18) 0.0031(14) -0.0015(15) N102 0.0445(16) 0.0616(19) 0.0303(13) -0.0022(14) 0.0037(12) -0.0002(15) N103 0.0314(13) 0.0431(15) 0.0339(13) -0.0014(12) 0.0035(11) -0.0123(12) N104 0.0328(13) 0.0389(14) 0.0514(16) -0.0144(14) -0.0021(12) -0.0008(12) O101 0.0314(13) 0.078(2) 0.105(2) 0.0289(19) 0.0136(14) 0.0031(13) O102 0.0625(18) 0.088(2) 0.0493(15) -0.0227(16) -0.0031(13) 0.0154(17) O103 0.0318(12) 0.0624(16) 0.0684(16) -0.0095(14) 0.0102(12) -0.0066(12) O104 0.0485(16) 0.081(2) 0.107(2) -0.067(2) 0.0108(16) -0.0168(15) C201 0.064(2) 0.0321(16) 0.0322(16) 0.0060(14) 0.0104(16) 0.0055(16) C202 0.059(2) 0.0280(15) 0.0327(15) 0.0027(13) -0.0033(15) 0.0042(15) C203 0.069(3) 0.064(2) 0.0299(17) 0.0043(17) -0.0002(17) 0.021(2) C204 0.081(3) 0.101(4) 0.0329(19) 0.003(2) -0.0118(19) 0.039(3) C205 0.061(2) 0.085(3) 0.0391(19) 0.000(2) -0.0083(18) 0.026(2) C206 0.0476(18) 0.0361(17) 0.0333(16) 0.0012(14) -0.0056(14) 0.0034(15) C207 0.0485(18) 0.0246(14) 0.0262(14) 0.0048(12) -0.0037(13) -0.0010(14) C208 0.0426(18) 0.0320(16) 0.0360(16) 0.0043(13) -0.0047(14) -0.0038(14) C209 0.0468(18) 0.0319(16) 0.0318(15) -0.0015(13) 0.0023(14) -0.0045(15) C210 0.0331(15) 0.0340(15) 0.0320(15) -0.0021(13) 0.0053(13) -0.0047(14) C211 0.0370(16) 0.0365(17) 0.0406(17) -0.0009(14) -0.0037(14) -0.0040(14) C212 0.0358(16) 0.0344(16) 0.0456(18) -0.0014(15) 0.0020(14) -0.0079(14) C213 0.0386(17) 0.0370(17) 0.0432(17) 0.0042(15) 0.0135(15) -0.0027(15) C214 0.054(2) 0.0450(19) 0.0317(16) 0.0040(15) 0.0000(15) -0.0061(17) C215 0.0530(19) 0.0390(17) 0.0334(16) -0.0003(14) 0.0029(15) -0.0131(16) C216 0.0488(19) 0.0383(18) 0.050(2) 0.0070(16) 0.0171(17) 0.0020(16) C217 0.068(2) 0.0274(15) 0.0310(16) 0.0024(13) 0.0043(16) -0.0013(16) C218 0.061(2) 0.0292(15) 0.0298(15) 0.0046(13) -0.0055(15) -0.0039(16) C219 0.078(3) 0.068(3) 0.0350(18) 0.0081(19) -0.0114(19) -0.015(2) C220 0.074(3) 0.100(4) 0.048(2) 0.021(2) -0.033(2) -0.016(3) C221 0.049(2) 0.070(3) 0.058(2) 0.018(2) -0.0239(19) -0.006(2) C222 0.0467(19) 0.0306(16) 0.0454(18) 0.0100(15) -0.0133(15) -0.0034(15) C223 0.0441(18) 0.0302(15) 0.0339(15) 0.0060(13) -0.0119(14) -0.0019(14) C224 0.0323(16) 0.0286(15) 0.0516(19) 0.0012(15) -0.0081(15) -0.0045(13) C225 0.0343(16) 0.0398(17) 0.0465(18) -0.0004(15) 0.0062(14) -0.0005(14) C226 0.0228(13) 0.0397(17) 0.0418(17) -0.0005(15) 0.0039(13) -0.0027(13) C227 0.0352(16) 0.0426(18) 0.0430(17) -0.0014(16) 0.0027(14) -0.0014(15) C228 0.0389(17) 0.053(2) 0.0372(16) 0.0031(17) 0.0045(14) 0.0020(17) C229 0.0328(16) 0.0455(18) 0.0425(17) 0.0043(16) 0.0081(14) 0.0008(15) C230 0.0405(17) 0.0355(16) 0.0494(19) 0.0019(15) 0.0052(15) -0.0044(15) C231 0.0334(15) 0.0462(18) 0.0372(16) -0.0018(16) 0.0015(13) -0.0024(15) C232 0.0455(19) 0.052(2) 0.053(2) 0.0126(18) 0.0107(17) -0.0008(17) N201 0.0504(17) 0.0452(16) 0.0390(15) 0.0086(13) 0.0061(13) 0.0067(14) N202 0.0381(14) 0.0365(14) 0.0314(13) 0.0014(11) -0.0008(11) -0.0033(12) N203 0.0503(16) 0.0463(16) 0.0342(14) 0.0131(13) 0.0088(13) 0.0034(14) N204 0.0250(12) 0.0423(15) 0.0455(15) 0.0072(13) -0.0011(11) 0.0014(11) O201 0.0796(19) 0.0672(18) 0.0373(13) -0.0005(13) 0.0149(13) 0.0168(16) O202 0.0409(13) 0.0661(17) 0.0449(13) 0.0084(12) 0.0001(11) 0.0054(12) O203 0.0808(19) 0.0494(15) 0.0379(13) 0.0096(12) 0.0156(13) 0.0031(14) O204 0.0364(13) 0.0511(15) 0.0736(18) 0.0052(14) -0.0095(13) 0.0064(11) C301 0.112(5) 0.084(4) 0.106(5) 0.015(4) -0.003(4) 0.029(4) C302 0.051(5) 0.160(12) 0.072(6) -0.026(7) -0.005(5) 0.047(6) O301 0.084(2) 0.099(2) 0.0469(15) 0.0161(17) 0.0127(15) 0.042(2) C31' 0.112(5) 0.084(4) 0.106(5) 0.015(4) -0.003(4) 0.029(4) O31' 0.084(2) 0.099(2) 0.0469(15) 0.0161(17) 0.0127(15) 0.042(2) O401 0.131(3) 0.0427(15) 0.0425(14) 0.0073(13) -0.0042(18) -0.0190(19) O501 0.078(3) 0.091(4) 0.0210(18) 0.012(2) 0.021(2) 0.062(3) O51' 0.097(9) 0.029(5) 0.083(9) -0.015(6) -0.013(8) 0.040(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.379(5) . ? C1 C6 1.383(5) . ? C1 C7 1.513(5) . ? C2 C3 1.399(5) . ? C2 H2 0.9500 . ? C3 C4 1.369(5) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.378(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.470(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.380(5) . ? C8 C9 1.388(5) . ? C8 N1 1.433(4) . ? C9 C10 1.362(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(7) . ? C10 H10 0.9500 . ? C11 C12 1.383(6) . ? C11 H11 0.9500 . ? C12 C13 1.374(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O1 1.244(4) . ? C14 N1 1.352(4) . ? C14 C15 1.473(5) . ? C15 C16 1.312(5) . ? C15 H15 0.9500 . ? C16 C17 1.479(5) . ? C16 H16 0.9500 . ? C17 O2 1.234(4) . ? C17 N2 1.327(4) . ? C18 N2 1.450(5) . ? C18 C19 1.525(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.509(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N3 1.462(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O3 1.238(4) . ? C21 N3 1.321(4) . ? C21 C22 1.485(4) . ? C22 C23 1.310(4) . ? C22 H22 0.9500 . ? C23 C24 1.484(4) . ? C23 H23 0.9500 . ? C24 O4 1.238(4) . ? C24 N4 1.336(4) . ? C25 C26 1.377(4) . ? C25 C30 1.382(4) . ? C25 N4 1.438(4) . ? C26 C27 1.381(5) . ? C26 H26 0.9500 . ? C27 C28 1.380(5) . ? C27 H27 0.9500 . ? C28 C29 1.377(5) . ? C28 H28 0.9500 . ? C29 C30 1.376(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 N4 1.478(4) . ? C31 C32 1.504(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.381(5) . ? C32 C37 1.395(5) . ? C33 C34 1.381(5) . ? C33 H33 0.9500 . ? C34 C35 1.388(6) . ? C34 H34 0.9500 . ? C35 C36 1.359(6) . ? C35 H35 0.9500 . ? C36 C37 1.389(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? N2 H2A 0.8800 . ? N3 H3A 0.8800 . ? C101 O101 1.238(5) . ? C101 N101 1.345(5) . ? C101 C102 1.524(6) . ? C102 C107 1.385(5) . ? C102 C103 1.393(6) . ? C103 C104 1.381(8) . ? C103 H103 0.9500 . ? C104 C105 1.391(7) . ? C104 H104 0.9500 . ? C105 C106 1.417(6) . ? C105 H105 0.9500 . ? C106 C107 1.385(6) . ? C106 C108 1.489(6) . ? C107 H107 0.9500 . ? C108 O102 1.236(5) . ? C108 N102 1.344(5) . ? C109 N102 1.443(4) . ? C109 C110 1.512(5) . ? C109 H10A 0.9900 . ? C109 H10B 0.9900 . ? C110 C111 1.373(5) . ? C110 C115 1.387(5) . ? C111 C112 1.381(5) . ? C111 H111 0.9500 . ? C112 C113 1.374(5) . ? C112 H112 0.9500 . ? C113 C114 1.381(5) . ? C113 C116 1.511(4) . ? C114 C115 1.373(5) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 N103 1.447(4) . ? C116 H11A 0.9900 . ? C116 H11B 0.9900 . ? C117 O103 1.236(4) . ? C117 N103 1.340(4) . ? C117 C118 1.502(5) . ? C118 C123 1.381(5) . ? C118 C119 1.390(5) . ? C119 C120 1.374(6) . ? C119 H119 0.9500 . ? C120 C121 1.377(5) . ? C120 H120 0.9500 . ? C121 C122 1.385(5) . ? C121 H121 0.9500 . ? C122 C123 1.379(5) . ? C122 C124 1.486(5) . ? C123 H123 0.9500 . ? C124 O104 1.234(4) . ? C124 N104 1.333(5) . ? C125 N104 1.458(4) . ? C125 C126 1.499(5) . ? C125 H12A 0.9900 . ? C125 H12B 0.9900 . ? C126 C131 1.403(5) . ? C126 C127 1.381(5) . ? C127 C128 1.378(6) . ? C127 H127 0.9500 . ? C128 C129 1.396(6) . ? C128 H128 0.9500 . ? C129 C130 1.376(5) . ? C129 C132 1.498(6) . ? C130 C131 1.371(5) . ? C130 H130 0.9500 . ? C131 H131 0.9500 . ? C132 N101 1.436(6) . ? C132 H13A 0.9900 . ? C132 H13B 0.9900 . ? N101 H101 0.8800 . ? N102 H102 0.8800 . ? N103 H10C 0.8800 . ? N104 H10D 0.8800 . ? C201 O201 1.223(4) . ? C201 N201 1.331(5) . ? C201 C202 1.492(5) . ? C202 C203 1.366(5) . ? C202 C207 1.393(4) . ? C203 C204 1.377(6) . ? C203 H203 0.9500 . ? C204 C205 1.378(6) . ? C204 H204 0.9500 . ? C205 C206 1.387(5) . ? C205 H205 0.9500 . ? C206 C207 1.376(5) . ? C206 C208 1.492(5) . ? C207 H207 0.9500 . ? C208 O202 1.238(4) . ? C208 N202 1.330(4) . ? C209 N202 1.467(4) . ? C209 C210 1.512(4) . ? C209 H20C 0.9900 . ? C209 H20D 0.9900 . ? C210 C211 1.383(5) . ? C210 C215 1.389(5) . ? C211 C212 1.386(5) . ? C211 H211 0.9500 . ? C212 C213 1.384(5) . ? C212 H212 0.9500 . ? C213 C214 1.398(5) . ? C213 C216 1.511(5) . ? C214 C215 1.372(5) . ? C214 H214 0.9500 . ? C215 H215 0.9500 . ? C216 N203 1.447(5) . ? C216 H21A 0.9900 . ? C216 H21B 0.9900 . ? C217 O203 1.228(4) . ? C217 N203 1.338(5) . ? C217 C218 1.498(5) . ? C218 C223 1.379(5) . ? C218 C219 1.385(5) . ? C219 C220 1.370(7) . ? C219 H219 0.9500 . ? C220 C221 1.371(7) . ? C220 H220 0.9500 . ? C221 C222 1.387(5) . ? C221 H221 0.9500 . ? C222 C223 1.390(5) . ? C222 C224 1.497(5) . ? C223 H223 0.9500 . ? C224 O204 1.218(4) . ? C224 N204 1.353(4) . ? C225 N204 1.433(4) . ? C225 C226 1.511(5) . ? C225 H22A 0.9900 . ? C225 H22B 0.9900 . ? C226 C231 1.385(5) . ? C226 C227 1.388(5) . ? C227 C228 1.377(5) . ? C227 H227 0.9500 . ? C228 C229 1.384(5) . ? C228 H228 0.9500 . ? C229 C230 1.384(5) . ? C229 C232 1.508(5) . ? C230 C231 1.381(5) . ? C230 H230 0.9500 . ? C231 H231 0.9500 . ? C232 N201 1.453(5) . ? C232 H23A 0.9900 . ? C232 H23B 0.9900 . ? N201 H201 0.8800 . ? N202 H202 0.8800 . ? N203 H20E 0.8800 . ? N204 H20F 0.8800 . ? C301 C302 1.354(10) . ? C301 O301 1.429(7) . ? C301 H31D 0.9900 . ? C301 H31E 0.9900 . ? C302 H32A 0.9800 . ? C302 H32B 0.9800 . ? C302 H32C 0.9800 . ? O301 H31C 0.8400 . ? O401 H41B 0.86(2) . ? O401 H41A 0.901(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.2(3) . . ? C2 C1 C7 120.8(3) . . ? C6 C1 C7 120.0(3) . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? N1 C7 C1 112.9(3) . . ? N1 C7 H7A 109.0 . . ? C1 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C1 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C13 C8 C9 119.7(3) . . ? C13 C8 N1 120.3(3) . . ? C9 C8 N1 119.9(3) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.6(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.0(3) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? O1 C14 N1 120.9(3) . . ? O1 C14 C15 121.2(3) . . ? N1 C14 C15 117.8(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? O2 C17 N2 122.6(3) . . ? O2 C17 C16 121.6(3) . . ? N2 C17 C16 115.7(3) . . ? N2 C18 C19 113.2(3) . . ? N2 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? N2 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 113.9(3) . . ? C20 C19 H19A 108.8 . . ? C18 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? C18 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N3 C20 C19 110.7(3) . . ? N3 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? O3 C21 N3 123.7(3) . . ? O3 C21 C22 121.0(3) . . ? N3 C21 C22 115.3(3) . . ? C23 C22 C21 121.4(3) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 121.6(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? O4 C24 N4 121.4(3) . . ? O4 C24 C23 120.5(3) . . ? N4 C24 C23 118.1(3) . . ? C26 C25 C30 120.1(3) . . ? C26 C25 N4 119.9(3) . . ? C30 C25 N4 119.9(3) . . ? C25 C26 C27 119.6(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.1(3) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? N4 C31 C32 113.1(2) . . ? N4 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? N4 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C37 118.0(3) . . ? C33 C32 C31 121.0(3) . . ? C37 C32 C31 120.9(3) . . ? C32 C33 C34 121.1(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C35 120.0(4) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.3(3) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 120.7(4) . . ? C36 C37 H37 119.6 . . ? C32 C37 H37 119.6 . . ? C14 N1 C8 123.0(3) . . ? C14 N1 C7 119.4(3) . . ? C8 N1 C7 117.0(3) . . ? C17 N2 C18 122.5(3) . . ? C17 N2 H2A 118.7 . . ? C18 N2 H2A 118.7 . . ? C21 N3 C20 122.3(3) . . ? C21 N3 H3A 118.8 . . ? C20 N3 H3A 118.8 . . ? C24 N4 C25 124.2(2) . . ? C24 N4 C31 117.9(2) . . ? C25 N4 C31 117.9(2) . . ? O101 C101 N101 122.3(4) . . ? O101 C101 C102 120.5(4) . . ? N101 C101 C102 117.0(3) . . ? C107 C102 C103 119.6(5) . . ? C107 C102 C101 121.9(4) . . ? C103 C102 C101 118.5(4) . . ? C104 C103 C102 119.5(4) . . ? C104 C103 H103 120.3 . . ? C102 C103 H103 120.3 . . ? C103 C104 C105 121.6(5) . . ? C103 C104 H104 119.2 . . ? C105 C104 H104 119.2 . . ? C104 C105 C106 118.7(5) . . ? C104 C105 H105 120.6 . . ? C106 C105 H105 120.6 . . ? C107 C106 C105 119.0(4) . . ? C107 C106 C108 123.1(4) . . ? C105 C106 C108 117.8(4) . . ? C106 C107 C102 121.5(4) . . ? C106 C107 H107 119.2 . . ? C102 C107 H107 119.2 . . ? O102 C108 N102 124.0(4) . . ? O102 C108 C106 121.0(4) . . ? N102 C108 C106 115.0(4) . . ? N102 C109 C110 110.3(3) . . ? N102 C109 H10A 109.6 . . ? C110 C109 H10A 109.6 . . ? N102 C109 H10B 109.6 . . ? C110 C109 H10B 109.6 . . ? H10A C109 H10B 108.1 . . ? C111 C110 C115 118.1(3) . . ? C111 C110 C109 120.5(3) . . ? C115 C110 C109 121.4(3) . . ? C110 C111 C112 121.4(3) . . ? C110 C111 H111 119.3 . . ? C112 C111 H111 119.3 . . ? C113 C112 C111 120.3(3) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C112 C113 C114 118.6(3) . . ? C112 C113 C116 121.0(3) . . ? C114 C113 C116 120.4(3) . . ? C115 C114 C113 121.0(3) . . ? C115 C114 H114 119.5 . . ? C113 C114 H114 119.5 . . ? C114 C115 C110 120.5(3) . . ? C114 C115 H115 119.7 . . ? C110 C115 H115 119.7 . . ? N103 C116 C113 112.0(3) . . ? N103 C116 H11A 109.2 . . ? C113 C116 H11A 109.2 . . ? N103 C116 H11B 109.2 . . ? C113 C116 H11B 109.2 . . ? H11A C116 H11B 107.9 . . ? O103 C117 N103 122.6(3) . . ? O103 C117 C118 121.2(3) . . ? N103 C117 C118 116.1(3) . . ? C123 C118 C119 118.7(3) . . ? C123 C118 C117 121.8(3) . . ? C119 C118 C117 119.5(3) . . ? C120 C119 C118 119.5(3) . . ? C120 C119 H119 120.2 . . ? C118 C119 H119 120.2 . . ? C119 C120 C121 120.5(3) . . ? C119 C120 H120 119.7 . . ? C121 C120 H120 119.7 . . ? C120 C121 C122 121.2(3) . . ? C120 C121 H121 119.4 . . ? C122 C121 H121 119.4 . . ? C123 C122 C121 117.2(3) . . ? C123 C122 C124 122.8(3) . . ? C121 C122 C124 120.0(3) . . ? C122 C123 C118 122.7(3) . . ? C122 C123 H123 118.6 . . ? C118 C123 H123 118.6 . . ? O104 C124 N104 122.7(3) . . ? O104 C124 C122 121.2(3) . . ? N104 C124 C122 116.1(3) . . ? N104 C125 C126 110.7(3) . . ? N104 C125 H12A 109.5 . . ? C126 C125 H12A 109.5 . . ? N104 C125 H12B 109.5 . . ? C126 C125 H12B 109.5 . . ? H12A C125 H12B 108.1 . . ? C127 C126 C131 116.8(4) . . ? C127 C126 C125 121.9(3) . . ? C131 C126 C125 121.2(3) . . ? C128 C127 C126 120.3(4) . . ? C128 C127 H127 119.8 . . ? C126 C127 H127 119.8 . . ? C127 C128 C129 123.2(4) . . ? C127 C128 H128 118.4 . . ? C129 C128 H128 118.4 . . ? C130 C129 C128 115.9(4) . . ? C130 C129 C132 121.9(4) . . ? C128 C129 C132 122.2(4) . . ? C131 C130 C129 121.8(4) . . ? C131 C130 H130 119.1 . . ? C129 C130 H130 119.1 . . ? C130 C131 C126 121.9(3) . . ? C130 C131 H131 119.0 . . ? C126 C131 H131 119.0 . . ? N101 C132 C129 114.7(3) . . ? N101 C132 H13A 108.6 . . ? C129 C132 H13A 108.6 . . ? N101 C132 H13B 108.6 . . ? C129 C132 H13B 108.6 . . ? H13A C132 H13B 107.6 . . ? C101 N101 C132 124.1(3) . . ? C101 N101 H101 117.9 . . ? C132 N101 H101 117.9 . . ? C108 N102 C109 124.1(3) . . ? C108 N102 H102 117.9 . . ? C109 N102 H102 117.9 . . ? C117 N103 C116 124.0(3) . . ? C117 N103 H10C 118.0 . . ? C116 N103 H10C 118.0 . . ? C124 N104 C125 124.3(3) . . ? C124 N104 H10D 117.9 . . ? C125 N104 H10D 117.9 . . ? O201 C201 N201 122.8(4) . . ? O201 C201 C202 120.6(3) . . ? N201 C201 C202 116.6(3) . . ? C203 C202 C207 119.7(3) . . ? C203 C202 C201 118.3(3) . . ? C207 C202 C201 121.9(3) . . ? C202 C203 C204 119.3(3) . . ? C202 C203 H203 120.4 . . ? C204 C203 H203 120.4 . . ? C203 C204 C205 120.8(4) . . ? C203 C204 H204 119.6 . . ? C205 C204 H204 119.6 . . ? C204 C205 C206 120.8(4) . . ? C204 C205 H205 119.6 . . ? C206 C205 H205 119.6 . . ? C207 C206 C205 117.5(3) . . ? C207 C206 C208 123.0(3) . . ? C205 C206 C208 119.5(3) . . ? C206 C207 C202 121.8(3) . . ? C206 C207 H207 119.1 . . ? C202 C207 H207 119.1 . . ? O202 C208 N202 121.8(3) . . ? O202 C208 C206 120.9(3) . . ? N202 C208 C206 117.3(3) . . ? N202 C209 C210 111.9(3) . . ? N202 C209 H20C 109.2 . . ? C210 C209 H20C 109.2 . . ? N202 C209 H20D 109.2 . . ? C210 C209 H20D 109.2 . . ? H20C C209 H20D 107.9 . . ? C211 C210 C215 118.6(3) . . ? C211 C210 C209 120.5(3) . . ? C215 C210 C209 120.9(3) . . ? C210 C211 C212 120.7(3) . . ? C210 C211 H211 119.7 . . ? C212 C211 H211 119.7 . . ? C213 C212 C211 120.9(3) . . ? C213 C212 H212 119.5 . . ? C211 C212 H212 119.5 . . ? C212 C213 C214 118.0(3) . . ? C212 C213 C216 121.1(3) . . ? C214 C213 C216 120.9(3) . . ? C215 C214 C213 121.1(3) . . ? C215 C214 H214 119.4 . . ? C213 C214 H214 119.4 . . ? C214 C215 C210 120.6(3) . . ? C214 C215 H215 119.7 . . ? C210 C215 H215 119.7 . . ? N203 C216 C213 110.4(3) . . ? N203 C216 H21A 109.6 . . ? C213 C216 H21A 109.6 . . ? N203 C216 H21B 109.6 . . ? C213 C216 H21B 109.6 . . ? H21A C216 H21B 108.1 . . ? O203 C217 N203 122.4(4) . . ? O203 C217 C218 121.0(3) . . ? N203 C217 C218 116.5(3) . . ? C223 C218 C219 118.5(4) . . ? C223 C218 C217 123.0(3) . . ? C219 C218 C217 118.4(3) . . ? C220 C219 C218 120.1(4) . . ? C220 C219 H219 120.0 . . ? C218 C219 H219 120.0 . . ? C219 C220 C221 121.4(4) . . ? C219 C220 H220 119.3 . . ? C221 C220 H220 119.3 . . ? C220 C221 C222 119.6(4) . . ? C220 C221 H221 120.2 . . ? C222 C221 H221 120.2 . . ? C221 C222 C223 118.6(4) . . ? C221 C222 C224 118.7(3) . . ? C223 C222 C224 122.7(3) . . ? C218 C223 C222 121.7(3) . . ? C218 C223 H223 119.1 . . ? C222 C223 H223 119.1 . . ? O204 C224 N204 121.9(3) . . ? O204 C224 C222 121.7(3) . . ? N204 C224 C222 116.3(3) . . ? N204 C225 C226 112.5(3) . . ? N204 C225 H22A 109.1 . . ? C226 C225 H22A 109.1 . . ? N204 C225 H22B 109.1 . . ? C226 C225 H22B 109.1 . . ? H22A C225 H22B 107.8 . . ? C231 C226 C227 118.0(3) . . ? C231 C226 C225 121.2(3) . . ? C227 C226 C225 120.8(3) . . ? C228 C227 C226 120.9(3) . . ? C228 C227 H227 119.5 . . ? C226 C227 H227 119.5 . . ? C227 C228 C229 120.9(3) . . ? C227 C228 H228 119.5 . . ? C229 C228 H228 119.5 . . ? C230 C229 C228 118.4(3) . . ? C230 C229 C232 120.2(3) . . ? C228 C229 C232 121.4(3) . . ? C231 C230 C229 120.6(3) . . ? C231 C230 H230 119.7 . . ? C229 C230 H230 119.7 . . ? C230 C231 C226 121.1(3) . . ? C230 C231 H231 119.4 . . ? C226 C231 H231 119.4 . . ? N201 C232 C229 111.9(3) . . ? N201 C232 H23A 109.2 . . ? C229 C232 H23A 109.2 . . ? N201 C232 H23B 109.2 . . ? C229 C232 H23B 109.2 . . ? H23A C232 H23B 107.9 . . ? C201 N201 C232 123.4(3) . . ? C201 N201 H201 118.3 . . ? C232 N201 H201 118.3 . . ? C208 N202 C209 123.6(3) . . ? C208 N202 H202 118.2 . . ? C209 N202 H202 118.2 . . ? C217 N203 C216 123.6(3) . . ? C217 N203 H20E 118.2 . . ? C216 N203 H20E 118.2 . . ? C224 N204 C225 123.2(3) . . ? C224 N204 H20F 118.4 . . ? C225 N204 H20F 118.4 . . ? C302 C301 O301 116.8(8) . . ? C302 C301 H31D 108.1 . . ? O301 C301 H31D 108.1 . . ? C302 C301 H31E 108.1 . . ? O301 C301 H31E 108.1 . . ? H31D C301 H31E 107.3 . . ? C301 C302 H32A 109.5 . . ? C301 C302 H32B 109.5 . . ? H32A C302 H32B 109.5 . . ? C301 C302 H32C 109.5 . . ? H32A C302 H32C 109.5 . . ? H32B C302 H32C 109.5 . . ? H41B O401 H41A 117(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.2(5) . . . . ? C7 C1 C2 C3 -175.9(3) . . . . ? C1 C2 C3 C4 0.0(5) . . . . ? C2 C3 C4 C5 -2.5(5) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C4 C5 C6 C1 1.5(5) . . . . ? C2 C1 C6 C5 -3.9(5) . . . . ? C7 C1 C6 C5 175.2(3) . . . . ? C2 C1 C7 N1 -89.7(4) . . . . ? C6 C1 C7 N1 91.2(4) . . . . ? C13 C8 C9 C10 -1.5(6) . . . . ? N1 C8 C9 C10 -178.7(4) . . . . ? C8 C9 C10 C11 0.3(7) . . . . ? C9 C10 C11 C12 0.8(7) . . . . ? C10 C11 C12 C13 -0.8(6) . . . . ? C11 C12 C13 C8 -0.5(6) . . . . ? C9 C8 C13 C12 1.6(5) . . . . ? N1 C8 C13 C12 178.8(3) . . . . ? O1 C14 C15 C16 -2.1(5) . . . . ? N1 C14 C15 C16 175.6(3) . . . . ? C14 C15 C16 C17 179.7(3) . . . . ? C15 C16 C17 O2 7.7(5) . . . . ? C15 C16 C17 N2 -170.9(3) . . . . ? N2 C18 C19 C20 -63.9(4) . . . . ? C18 C19 C20 N3 177.9(3) . . . . ? O3 C21 C22 C23 1.2(5) . . . . ? N3 C21 C22 C23 -179.5(3) . . . . ? C21 C22 C23 C24 179.3(3) . . . . ? C22 C23 C24 O4 -9.5(5) . . . . ? C22 C23 C24 N4 168.9(3) . . . . ? C30 C25 C26 C27 -0.7(5) . . . . ? N4 C25 C26 C27 -178.8(3) . . . . ? C25 C26 C27 C28 -0.2(5) . . . . ? C26 C27 C28 C29 0.9(5) . . . . ? C27 C28 C29 C30 -0.5(5) . . . . ? C28 C29 C30 C25 -0.5(5) . . . . ? C26 C25 C30 C29 1.1(5) . . . . ? N4 C25 C30 C29 179.1(3) . . . . ? N4 C31 C32 C33 -71.7(4) . . . . ? N4 C31 C32 C37 109.4(3) . . . . ? C37 C32 C33 C34 1.5(5) . . . . ? C31 C32 C33 C34 -177.4(3) . . . . ? C32 C33 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C36 -0.6(5) . . . . ? C34 C35 C36 C37 1.8(5) . . . . ? C35 C36 C37 C32 -1.4(5) . . . . ? C33 C32 C37 C36 -0.3(5) . . . . ? C31 C32 C37 C36 178.6(3) . . . . ? O1 C14 N1 C8 -166.2(3) . . . . ? C15 C14 N1 C8 16.1(4) . . . . ? O1 C14 N1 C7 4.7(5) . . . . ? C15 C14 N1 C7 -172.9(3) . . . . ? C13 C8 N1 C14 69.7(4) . . . . ? C9 C8 N1 C14 -113.1(4) . . . . ? C13 C8 N1 C7 -101.5(4) . . . . ? C9 C8 N1 C7 75.7(4) . . . . ? C1 C7 N1 C14 -97.0(4) . . . . ? C1 C7 N1 C8 74.5(4) . . . . ? O2 C17 N2 C18 -6.8(5) . . . . ? C16 C17 N2 C18 171.8(3) . . . . ? C19 C18 N2 C17 105.1(4) . . . . ? O3 C21 N3 C20 -5.4(5) . . . . ? C22 C21 N3 C20 175.3(3) . . . . ? C19 C20 N3 C21 -101.5(4) . . . . ? O4 C24 N4 C25 -176.9(3) . . . . ? C23 C24 N4 C25 4.8(4) . . . . ? O4 C24 N4 C31 2.2(4) . . . . ? C23 C24 N4 C31 -176.2(3) . . . . ? C26 C25 N4 C24 -105.9(3) . . . . ? C30 C25 N4 C24 76.0(4) . . . . ? C26 C25 N4 C31 75.0(4) . . . . ? C30 C25 N4 C31 -103.0(3) . . . . ? C32 C31 N4 C24 -77.3(3) . . . . ? C32 C31 N4 C25 101.8(3) . . . . ? O101 C101 C102 C107 -165.5(4) . . . . ? N101 C101 C102 C107 18.6(5) . . . . ? O101 C101 C102 C103 17.7(6) . . . . ? N101 C101 C102 C103 -158.3(4) . . . . ? C107 C102 C103 C104 -2.3(7) . . . . ? C101 C102 C103 C104 174.6(4) . . . . ? C102 C103 C104 C105 -1.4(8) . . . . ? C103 C104 C105 C106 3.6(8) . . . . ? C104 C105 C106 C107 -2.2(6) . . . . ? C104 C105 C106 C108 -177.4(4) . . . . ? C105 C106 C107 C102 -1.4(6) . . . . ? C108 C106 C107 C102 173.5(3) . . . . ? C103 C102 C107 C106 3.7(6) . . . . ? C101 C102 C107 C106 -173.1(3) . . . . ? C107 C106 C108 O102 166.1(4) . . . . ? C105 C106 C108 O102 -18.9(6) . . . . ? C107 C106 C108 N102 -16.3(5) . . . . ? C105 C106 C108 N102 158.7(4) . . . . ? N102 C109 C110 C111 -58.2(4) . . . . ? N102 C109 C110 C115 120.1(4) . . . . ? C115 C110 C111 C112 1.9(5) . . . . ? C109 C110 C111 C112 -179.7(3) . . . . ? C110 C111 C112 C113 -0.8(5) . . . . ? C111 C112 C113 C114 -1.0(5) . . . . ? C111 C112 C113 C116 179.3(3) . . . . ? C112 C113 C114 C115 1.7(5) . . . . ? C116 C113 C114 C115 -178.6(3) . . . . ? C113 C114 C115 C110 -0.6(6) . . . . ? C111 C110 C115 C114 -1.1(5) . . . . ? C109 C110 C115 C114 -179.5(3) . . . . ? C112 C113 C116 N103 120.6(3) . . . . ? C114 C113 C116 N103 -59.2(4) . . . . ? O103 C117 C118 C123 168.6(3) . . . . ? N103 C117 C118 C123 -11.0(5) . . . . ? O103 C117 C118 C119 -13.4(5) . . . . ? N103 C117 C118 C119 166.9(3) . . . . ? C123 C118 C119 C120 1.3(5) . . . . ? C117 C118 C119 C120 -176.7(3) . . . . ? C118 C119 C120 C121 1.3(6) . . . . ? C119 C120 C121 C122 -3.1(6) . . . . ? C120 C121 C122 C123 2.2(5) . . . . ? C120 C121 C122 C124 -178.4(3) . . . . ? C121 C122 C123 C118 0.4(5) . . . . ? C124 C122 C123 C118 -178.9(3) . . . . ? C119 C118 C123 C122 -2.2(5) . . . . ? C117 C118 C123 C122 175.8(3) . . . . ? C123 C122 C124 O104 -177.2(4) . . . . ? C121 C122 C124 O104 3.5(6) . . . . ? C123 C122 C124 N104 3.7(5) . . . . ? C121 C122 C124 N104 -175.6(3) . . . . ? C128 C127 C126 C131 1.2(5) . . . . ? C128 C127 C126 C125 -175.2(3) . . . . ? C130 C131 C126 C127 -2.9(5) . . . . ? C130 C131 C126 C125 173.5(3) . . . . ? N104 C125 C126 C127 69.8(4) . . . . ? N104 C125 C126 C131 -106.4(3) . . . . ? C126 C127 C128 C129 0.8(5) . . . . ? C127 C128 C129 C130 -1.2(5) . . . . ? C127 C128 C129 C132 178.8(3) . . . . ? C128 C129 C130 C131 -0.6(5) . . . . ? C132 C129 C130 C131 179.4(3) . . . . ? C129 C130 C131 C126 2.7(5) . . . . ? C130 C129 C132 N101 44.6(5) . . . . ? C128 C129 C132 N101 -135.4(4) . . . . ? O101 C101 N101 C132 0.5(6) . . . . ? C102 C101 N101 C132 176.4(3) . . . . ? C129 C132 N101 C101 -121.8(4) . . . . ? O102 C108 N102 C109 4.8(6) . . . . ? C106 C108 N102 C109 -172.7(3) . . . . ? C110 C109 N102 C108 123.6(4) . . . . ? O103 C117 N103 C116 1.3(5) . . . . ? C118 C117 N103 C116 -179.1(3) . . . . ? C113 C116 N103 C117 123.7(3) . . . . ? O104 C124 N104 C125 -2.1(6) . . . . ? C122 C124 N104 C125 177.0(3) . . . . ? C126 C125 N104 C124 -112.8(4) . . . . ? O201 C201 C202 C203 -23.3(5) . . . . ? N201 C201 C202 C203 155.6(3) . . . . ? O201 C201 C202 C207 155.2(3) . . . . ? N201 C201 C202 C207 -25.9(5) . . . . ? C207 C202 C203 C204 0.1(6) . . . . ? C201 C202 C203 C204 178.7(4) . . . . ? C202 C203 C204 C205 0.1(8) . . . . ? C203 C204 C205 C206 1.2(8) . . . . ? C204 C205 C206 C207 -2.7(7) . . . . ? C204 C205 C206 C208 176.3(4) . . . . ? C205 C206 C207 C202 2.9(5) . . . . ? C208 C206 C207 C202 -176.0(3) . . . . ? C203 C202 C207 C206 -1.7(5) . . . . ? C201 C202 C207 C206 179.8(3) . . . . ? C207 C206 C208 O202 -174.1(3) . . . . ? C205 C206 C208 O202 7.0(5) . . . . ? C207 C206 C208 N202 5.6(5) . . . . ? C205 C206 C208 N202 -173.3(4) . . . . ? N202 C209 C210 C211 -58.5(4) . . . . ? N202 C209 C210 C215 121.8(3) . . . . ? C215 C210 C211 C212 0.9(5) . . . . ? C209 C210 C211 C212 -178.9(3) . . . . ? C210 C211 C212 C213 -0.4(5) . . . . ? C211 C212 C213 C214 -0.7(5) . . . . ? C211 C212 C213 C216 -179.5(3) . . . . ? C212 C213 C214 C215 1.4(5) . . . . ? C216 C213 C214 C215 -179.8(3) . . . . ? C213 C214 C215 C210 -1.0(5) . . . . ? C211 C210 C215 C214 -0.2(5) . . . . ? C209 C210 C215 C214 179.6(3) . . . . ? C212 C213 C216 N203 113.3(4) . . . . ? C214 C213 C216 N203 -65.5(4) . . . . ? O203 C217 C218 C223 164.8(3) . . . . ? N203 C217 C218 C223 -17.9(5) . . . . ? O203 C217 C218 C219 -16.1(5) . . . . ? N203 C217 C218 C219 161.3(3) . . . . ? C223 C218 C219 C220 1.7(6) . . . . ? C217 C218 C219 C220 -177.5(4) . . . . ? C218 C219 C220 C221 -0.3(8) . . . . ? C219 C220 C221 C222 -0.3(8) . . . . ? C220 C221 C222 C223 -0.5(6) . . . . ? C220 C221 C222 C224 179.4(4) . . . . ? C219 C218 C223 C222 -2.5(5) . . . . ? C217 C218 C223 C222 176.7(3) . . . . ? C221 C222 C223 C218 1.9(5) . . . . ? C224 C222 C223 C218 -178.0(3) . . . . ? C221 C222 C224 O204 9.3(5) . . . . ? C223 C222 C224 O204 -170.7(3) . . . . ? C221 C222 C224 N204 -168.5(3) . . . . ? C223 C222 C224 N204 11.5(5) . . . . ? N204 C225 C226 C231 43.6(4) . . . . ? N204 C225 C226 C227 -138.2(3) . . . . ? C231 C226 C227 C228 0.3(5) . . . . ? C225 C226 C227 C228 -178.0(3) . . . . ? C226 C227 C228 C229 0.0(5) . . . . ? C227 C228 C229 C230 0.2(5) . . . . ? C227 C228 C229 C232 -179.3(3) . . . . ? C228 C229 C230 C231 -0.7(5) . . . . ? C232 C229 C230 C231 178.8(3) . . . . ? C229 C230 C231 C226 1.0(5) . . . . ? C227 C226 C231 C230 -0.7(5) . . . . ? C225 C226 C231 C230 177.5(3) . . . . ? C230 C229 C232 N201 -98.0(4) . . . . ? C228 C229 C232 N201 81.5(4) . . . . ? O201 C201 N201 C232 -1.8(5) . . . . ? C202 C201 N201 C232 179.4(3) . . . . ? C229 C232 N201 C201 -105.5(4) . . . . ? O202 C208 N202 C209 -0.1(5) . . . . ? C206 C208 N202 C209 -179.9(3) . . . . ? C210 C209 N202 C208 123.4(3) . . . . ? O203 C217 N203 C216 -0.1(5) . . . . ? C218 C217 N203 C216 -177.5(3) . . . . ? C213 C216 N203 C217 141.4(3) . . . . ? O204 C224 N204 C225 7.1(5) . . . . ? C222 C224 N204 C225 -175.2(3) . . . . ? C226 C225 N204 C224 -132.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O501 0.88 1.91 2.784(5) 172.2 1_655 N3 H3A O301 0.88 1.95 2.820(4) 172.2 . N3 H3A O31' 0.88 1.95 2.820(4) 172.2 . N101 H101 O1 0.88 2.20 3.072(4) 170.8 . N102 H102 O1 0.88 2.09 2.934(4) 161.4 . N103 H10C O2 0.88 2.16 3.002(3) 159.3 . N104 H10D O2 0.88 2.12 2.978(4) 165.5 . N201 H201 O3 0.88 2.24 3.082(4) 160.5 . N202 H202 O3 0.88 2.22 3.066(4) 162.5 . N203 H20E O4 0.88 2.11 2.969(3) 166.4 . N204 H20F O4 0.88 2.26 3.127(3) 171.0 . O301 H31C O201 0.84 1.88 2.711(4) 170.9 1_556 O401 H41B O103 0.86(2) 2.11(3) 2.937(4) 160(6) . O401 H41A O102 0.901(19) 2.24(5) 2.898(5) 129(5) 1_556 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 66.58 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.611 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.052