data_global _journal_coden_Cambridge 177 loop_ _publ_author_name 'Philip Gale' _publ_contact_author_name 'Philip Gale' _publ_contact_author_email PHILIP.GALE@SOTON.AC.UK _publ_section_title ; Fluorescent carbazolylurea anion receptors ; # Attachment '08jh4_08jh3_combined.cif' data_2008jh0004 _database_code_depnum_ccdc_archive 'CCDC 715669' _chemical_compound_source ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H57 N5 O3' _chemical_formula_weight 691.94 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0933(2) _cell_length_b 26.7833(6) _cell_length_c 13.2013(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.0560(10) _cell_angle_gamma 90.00 _cell_volume 3883.60(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 32663 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9826 _exptl_absorpt_correction_T_max 0.9926 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 23894 reflections reduced R(int) from 0.1372 to 0.0597 Ratio of minimum to maximum apparent transmission: 0.869588 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40088 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8914 _reflns_number_gt 5380 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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. ; _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^)+(0.0529P)^2^+2.5142P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8914 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1274 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1613 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C26 C 0.6302(2) 0.12556(9) 0.32971(18) 0.0252(5) Uani 1 1 d . . . C27 C 0.7470(2) 0.10892(10) 0.2939(2) 0.0361(6) Uani 1 1 d . . . H27A H 0.8033 0.1363 0.2987 0.054 Uiso 1 1 calc R . . H27B H 0.7303 0.0979 0.2242 0.054 Uiso 1 1 calc R . . H27C H 0.7817 0.0819 0.3362 0.054 Uiso 1 1 calc R . . C28 C 0.6301(2) 0.17892(9) 0.77934(18) 0.0284(6) Uani 1 1 d . . . H28A H 0.6021 0.1488 0.8096 0.034 Uiso 1 1 calc R . . H28B H 0.7029 0.1900 0.8228 0.034 Uiso 1 1 calc R . . C29 C 0.6912(2) 0.21227(9) 0.61601(18) 0.0247(5) Uani 1 1 d . . . H29A H 0.7037 0.2024 0.5475 0.030 Uiso 1 1 calc R . . H29B H 0.6198 0.2336 0.6095 0.030 Uiso 1 1 calc R . . C30 C 0.7759(2) 0.13209(9) 0.69360(19) 0.0299(6) Uani 1 1 d . . . H30A H 0.8397 0.1499 0.7368 0.036 Uiso 1 1 calc R . . H30B H 0.7553 0.1029 0.7313 0.036 Uiso 1 1 calc R . . C31 C 0.5592(2) 0.13968(9) 0.60924(18) 0.0279(5) Uani 1 1 d . . . H31A H 0.4900 0.1622 0.6020 0.033 Uiso 1 1 calc R . . H31B H 0.5817 0.1349 0.5415 0.033 Uiso 1 1 calc R . . C33 C 0.5333(2) 0.21870(10) 0.77984(18) 0.0300(6) Uani 1 1 d . . . H33A H 0.4623 0.2098 0.7316 0.036 Uiso 1 1 calc R . . H33B H 0.5641 0.2504 0.7588 0.036 Uiso 1 1 calc R . . C34 C 0.8264(2) 0.11457(10) 0.5987(2) 0.0362(6) Uani 1 1 d . . . H34A H 0.8452 0.1432 0.5587 0.043 Uiso 1 1 calc R . . H34B H 0.7660 0.0944 0.5568 0.043 Uiso 1 1 calc R . . C35 C 0.8000(2) 0.24270(9) 0.66255(18) 0.0282(5) Uani 1 1 d . . . H35A H 0.8745 0.2252 0.6539 0.034 Uiso 1 1 calc R . . H35B H 0.7979 0.2470 0.7352 0.034 Uiso 1 1 calc R . . C36 C 0.5175(2) 0.08984(10) 0.6457(2) 0.0367(6) Uani 1 1 d . . . H36A H 0.4950 0.0933 0.7138 0.044 Uiso 1 1 calc R . . H36B H 0.5831 0.0657 0.6489 0.044 Uiso 1 1 calc R . . C37 C 0.4978(2) 0.22365(10) 0.88640(19) 0.0308(6) Uani 1 1 d . . . H37A H 0.5708 0.2271 0.9357 0.037 Uiso 1 1 calc R . . H37B H 0.4561 0.1935 0.9029 0.037 Uiso 1 1 calc R . . C38 C 0.7983(2) 0.29359(9) 0.61098(19) 0.0297(6) Uani 1 1 d . . . H38A H 0.7758 0.2894 0.5378 0.036 Uiso 1 1 calc R . . H38B H 0.7368 0.3143 0.6356 0.036 Uiso 1 1 calc R . . C39 C 0.9418(3) 0.08373(12) 0.6299(2) 0.0514(8) Uani 1 1 d . . . H39A H 0.9967 0.1023 0.6798 0.062 Uiso 1 1 calc R . . H39B H 0.9203 0.0530 0.6620 0.062 Uiso 1 1 calc R . . C40 C 0.4082(3) 0.07174(10) 0.5717(2) 0.0426(7) Uani 1 1 d . . . H40A H 0.3436 0.0963 0.5692 0.051 Uiso 1 1 calc R . . H40B H 0.4315 0.0693 0.5037 0.051 Uiso 1 1 calc R . . C41 C 1.0061(3) 0.07120(14) 0.5396(3) 0.0704(11) Uani 1 1 d . . . H41A H 0.9526 0.0522 0.4906 0.106 Uiso 1 1 calc R . . H41B H 1.0777 0.0519 0.5625 0.106 Uiso 1 1 calc R . . H41C H 1.0290 0.1015 0.5084 0.106 Uiso 1 1 calc R . . C42 C 0.9205(2) 0.32013(10) 0.6311(2) 0.0376(6) Uani 1 1 d . . . H42A H 0.9456 0.3226 0.7035 0.056 Uiso 1 1 calc R . . H42B H 0.9130 0.3530 0.6019 0.056 Uiso 1 1 calc R . . H42C H 0.9800 0.3015 0.6005 0.056 Uiso 1 1 calc R . . C43 C 0.4151(2) 0.26856(10) 0.8947(2) 0.0374(6) Uani 1 1 d . . . H43A H 0.4551 0.2983 0.8763 0.056 Uiso 1 1 calc R . . H43B H 0.3980 0.2715 0.9638 0.056 Uiso 1 1 calc R . . H43C H 0.3403 0.2641 0.8494 0.056 Uiso 1 1 calc R . . C44 C 0.3600(3) 0.02191(11) 0.6003(3) 0.0615(10) Uani 1 1 d . . . H44A H 0.4238 -0.0025 0.6044 0.092 Uiso 1 1 calc R . . H44B H 0.2941 0.0119 0.5493 0.092 Uiso 1 1 calc R . . H44C H 0.3314 0.0245 0.6654 0.092 Uiso 1 1 calc R . . C1 C 1.1815(2) 0.16987(10) -0.1828(2) 0.0333(6) Uani 1 1 d . . . H1A H 1.2083 0.1894 -0.2335 0.040 Uiso 1 1 calc R . . C2 C 1.2287(2) 0.12273(10) -0.1600(2) 0.0376(7) Uani 1 1 d . . . H2A H 1.2881 0.1103 -0.1964 0.045 Uiso 1 1 calc R . . C3 C 1.1891(2) 0.09330(10) -0.0836(2) 0.0386(7) Uani 1 1 d . . . H3A H 1.2231 0.0619 -0.0697 0.046 Uiso 1 1 calc R . . C4 C 1.1007(2) 0.11016(9) -0.0286(2) 0.0338(6) Uani 1 1 d . . . H4A H 1.0747 0.0905 0.0222 0.041 Uiso 1 1 calc R . . C5 C 1.0505(2) 0.15765(9) -0.05082(19) 0.0275(5) Uani 1 1 d . . . C6 C 1.0926(2) 0.18697(9) -0.12712(19) 0.0285(6) Uani 1 1 d . . . C7 C 0.9603(2) 0.18724(9) -0.00844(19) 0.0271(5) Uani 1 1 d . . . C8 C 0.9529(2) 0.23315(8) -0.06164(17) 0.0241(5) Uani 1 1 d . . . C9 C 0.8871(2) 0.17931(9) 0.06794(19) 0.0292(6) Uani 1 1 d . . . H9 H 0.8922 0.1497 0.1050 0.035 Uiso 1 1 calc R . . C10 C 0.8068(2) 0.21643(9) 0.08731(19) 0.0311(6) Uani 1 1 d . . . H10 H 0.7566 0.2112 0.1372 0.037 Uiso 1 1 calc R . . C11 C 0.7992(2) 0.26172(9) 0.03353(18) 0.0271(5) Uani 1 1 d . . . H11 H 0.7443 0.2860 0.0483 0.032 Uiso 1 1 calc R . . C12 C 0.8724(2) 0.27086(8) -0.04140(18) 0.0243(5) Uani 1 1 d . . . C13 C 0.7685(2) 0.34280(9) -0.13268(18) 0.0262(5) Uani 1 1 d . . . C14 C 0.7139(2) 0.41991(8) -0.23492(18) 0.0256(5) Uani 1 1 d . . . C15 C 0.7627(2) 0.45771(8) -0.29084(18) 0.0241(5) Uani 1 1 d . . . C16 C 0.6892(2) 0.49367(8) -0.34748(18) 0.0258(5) Uani 1 1 d . . . C17 C 0.5627(2) 0.49221(9) -0.3493(2) 0.0305(6) Uani 1 1 d . . . H17 H 0.5125 0.5155 -0.3866 0.037 Uiso 1 1 calc R . . C18 C 0.5147(2) 0.45525(9) -0.2942(2) 0.0317(6) Uani 1 1 d . . . H18 H 0.4310 0.4541 -0.2942 0.038 Uiso 1 1 calc R . . C19 C 0.5882(2) 0.41937(9) -0.23802(19) 0.0296(6) Uani 1 1 d . . . H19 H 0.5522 0.3949 -0.2023 0.036 Uiso 1 1 calc R . . C20 C 0.7705(2) 0.52573(8) -0.39425(18) 0.0247(5) Uani 1 1 d . . . C21 C 0.8897(2) 0.50770(8) -0.36326(18) 0.0242(5) Uani 1 1 d . . . C22 C 0.7541(2) 0.56748(9) -0.45837(19) 0.0288(6) Uani 1 1 d . . . H22 H 0.6764 0.5798 -0.4800 0.035 Uiso 1 1 calc R . . C23 C 0.8544(2) 0.59010(9) -0.48914(19) 0.0304(6) Uani 1 1 d . . . H23 H 0.8441 0.6179 -0.5318 0.037 Uiso 1 1 calc R . . C24 C 0.9716(2) 0.57185(9) -0.45701(18) 0.0289(6) Uani 1 1 d . . . H24 H 1.0380 0.5879 -0.4784 0.035 Uiso 1 1 calc R . . C25 C 0.9912(2) 0.53041(9) -0.39399(18) 0.0273(5) Uani 1 1 d . . . H25 H 1.0693 0.5183 -0.3731 0.033 Uiso 1 1 calc R . . N1 N 0.88371(17) 0.46651(7) -0.30122(15) 0.0256(4) Uani 1 1 d . . . H1 H 0.9449 0.4492 -0.2736 0.031 Uiso 1 1 calc R . . N2 N 0.79526(17) 0.38585(7) -0.18099(15) 0.0263(5) Uani 1 1 d . . . H2 H 0.8713 0.3929 -0.1779 0.032 Uiso 1 1 calc R . . N3 N 0.87224(17) 0.31643(7) -0.09594(15) 0.0252(4) Uani 1 1 d . . . H3 H 0.9412 0.3284 -0.1068 0.030 Uiso 1 1 calc R . . N4 N 1.03276(17) 0.23248(7) -0.13341(15) 0.0264(4) Uani 1 1 d . . . H4 H 1.0434 0.2563 -0.1749 0.032 Uiso 1 1 calc R . . O1 O 0.66617(15) 0.32903(6) -0.12309(14) 0.0367(4) Uani 1 1 d . . . O2 O 0.54460(15) 0.09412(6) 0.32422(14) 0.0353(4) Uani 1 1 d . . . O3 O 0.62243(15) 0.16909(6) 0.36329(13) 0.0318(4) Uani 1 1 d . . . N5 N 0.66448(16) 0.16561(7) 0.67449(14) 0.0251(4) Uani 1 1 d . . . 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 C26 0.0253(12) 0.0269(13) 0.0227(13) 0.0005(10) 0.0010(9) 0.0024(10) C27 0.0329(14) 0.0369(15) 0.0405(16) -0.0046(13) 0.0125(12) 0.0023(12) C28 0.0261(12) 0.0367(14) 0.0221(13) 0.0041(11) 0.0023(10) 0.0004(10) C29 0.0253(12) 0.0297(13) 0.0194(12) 0.0057(10) 0.0039(9) 0.0037(10) C30 0.0275(12) 0.0332(14) 0.0287(14) 0.0077(11) 0.0027(10) 0.0072(11) C31 0.0283(12) 0.0313(13) 0.0236(13) 0.0023(11) 0.0024(10) 0.0002(10) C33 0.0294(13) 0.0355(14) 0.0253(13) 0.0027(11) 0.0044(10) 0.0043(11) C34 0.0389(15) 0.0381(15) 0.0325(15) 0.0065(12) 0.0075(12) 0.0098(12) C35 0.0282(12) 0.0330(14) 0.0227(13) 0.0022(11) 0.0007(10) 0.0005(10) C36 0.0405(15) 0.0336(14) 0.0352(16) 0.0069(12) 0.0032(12) -0.0023(12) C37 0.0244(12) 0.0395(15) 0.0287(14) -0.0020(12) 0.0048(10) -0.0038(11) C38 0.0346(13) 0.0309(13) 0.0228(13) 0.0028(11) 0.0013(10) 0.0007(11) C39 0.0488(18) 0.059(2) 0.0483(19) 0.0075(16) 0.0128(14) 0.0203(15) C40 0.0469(17) 0.0348(15) 0.0439(17) 0.0041(13) -0.0011(13) -0.0036(13) C41 0.059(2) 0.081(3) 0.075(3) 0.000(2) 0.0208(18) 0.034(2) C42 0.0460(16) 0.0391(15) 0.0277(15) 0.0026(12) 0.0049(12) -0.0115(13) C43 0.0328(14) 0.0398(15) 0.0418(16) -0.0025(13) 0.0129(12) -0.0014(12) C44 0.061(2) 0.0431(19) 0.076(3) 0.0094(17) -0.0055(18) -0.0139(16) C1 0.0274(13) 0.0336(14) 0.0384(16) -0.0008(12) 0.0032(11) -0.0025(11) C2 0.0258(13) 0.0357(15) 0.0511(18) -0.0090(13) 0.0046(12) 0.0003(11) C3 0.0276(13) 0.0273(14) 0.0593(19) 0.0002(13) 0.0011(12) 0.0001(11) C4 0.0288(13) 0.0257(13) 0.0441(16) 0.0048(12) -0.0046(11) -0.0045(10) C5 0.0240(12) 0.0251(12) 0.0316(14) -0.0002(11) -0.0029(10) -0.0057(10) C6 0.0227(12) 0.0266(13) 0.0340(15) -0.0015(11) -0.0041(10) -0.0040(10) C7 0.0273(12) 0.0239(12) 0.0281(14) 0.0000(10) -0.0029(10) -0.0080(10) C8 0.0242(11) 0.0240(12) 0.0225(13) -0.0007(10) -0.0020(9) -0.0072(10) C9 0.0341(13) 0.0227(12) 0.0291(14) 0.0039(11) -0.0011(11) -0.0068(10) C10 0.0364(14) 0.0306(14) 0.0263(14) 0.0001(11) 0.0043(11) -0.0106(11) C11 0.0275(12) 0.0256(13) 0.0275(14) -0.0015(11) 0.0016(10) -0.0037(10) C12 0.0262(12) 0.0231(12) 0.0223(13) 0.0002(10) -0.0010(9) -0.0058(10) C13 0.0302(13) 0.0249(12) 0.0233(13) 0.0012(10) 0.0032(10) -0.0037(10) C14 0.0291(12) 0.0227(12) 0.0252(13) -0.0003(10) 0.0046(10) -0.0011(10) C15 0.0244(12) 0.0217(12) 0.0266(13) -0.0023(10) 0.0052(9) -0.0010(9) C16 0.0285(12) 0.0212(12) 0.0279(13) -0.0004(10) 0.0047(10) 0.0013(10) C17 0.0286(13) 0.0267(13) 0.0357(15) 0.0008(11) 0.0022(11) 0.0052(10) C18 0.0229(12) 0.0331(14) 0.0395(16) 0.0008(12) 0.0059(11) 0.0002(10) C19 0.0289(13) 0.0286(13) 0.0327(14) 0.0024(11) 0.0089(10) -0.0023(10) C20 0.0301(12) 0.0196(12) 0.0244(13) -0.0045(10) 0.0037(10) -0.0018(10) C21 0.0307(13) 0.0185(11) 0.0234(13) -0.0014(10) 0.0037(10) -0.0008(10) C22 0.0316(13) 0.0255(13) 0.0285(14) 0.0018(11) 0.0016(10) 0.0020(10) C23 0.0390(14) 0.0228(12) 0.0289(14) 0.0015(11) 0.0031(11) -0.0010(11) C24 0.0347(13) 0.0259(13) 0.0272(14) -0.0012(11) 0.0080(11) -0.0064(10) C25 0.0270(12) 0.0259(13) 0.0293(14) -0.0041(11) 0.0049(10) -0.0010(10) N1 0.0223(10) 0.0239(10) 0.0309(12) 0.0045(9) 0.0043(8) 0.0022(8) N2 0.0225(10) 0.0245(10) 0.0318(12) 0.0053(9) 0.0038(8) -0.0014(8) N3 0.0214(10) 0.0240(10) 0.0299(12) 0.0055(9) 0.0031(8) -0.0029(8) N4 0.0272(10) 0.0251(10) 0.0264(11) 0.0060(9) 0.0024(8) -0.0004(8) O1 0.0251(9) 0.0358(10) 0.0493(12) 0.0141(9) 0.0056(8) -0.0035(8) O2 0.0269(9) 0.0291(9) 0.0495(12) -0.0074(8) 0.0042(8) -0.0021(8) O3 0.0285(9) 0.0267(9) 0.0401(11) -0.0069(8) 0.0049(7) 0.0026(7) N5 0.0237(10) 0.0294(11) 0.0219(11) 0.0040(9) 0.0020(8) 0.0037(8) _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 C26 O3 1.255(3) . ? C26 O2 1.263(3) . ? C26 C27 1.507(3) . ? C28 C33 1.513(3) . ? C28 N5 1.529(3) . ? C29 C35 1.514(3) . ? C29 N5 1.520(3) . ? C30 C34 1.516(4) . ? C30 N5 1.520(3) . ? C31 C36 1.514(3) . ? C31 N5 1.519(3) . ? C33 C37 1.519(3) . ? C34 C39 1.531(4) . ? C35 C38 1.523(3) . ? C36 C40 1.525(4) . ? C37 C43 1.526(3) . ? C38 C42 1.521(3) . ? C39 C41 1.510(4) . ? C40 C44 1.505(4) . ? C1 C2 1.384(4) . ? C1 C6 1.387(4) . ? C2 C3 1.399(4) . ? C3 C4 1.376(4) . ? C4 C5 1.403(3) . ? C5 C6 1.408(3) . ? C5 C7 1.449(3) . ? C6 N4 1.385(3) . ? C7 C9 1.397(4) . ? C7 C8 1.413(3) . ? C8 N4 1.385(3) . ? C8 C12 1.399(3) . ? C9 C10 1.383(4) . ? C10 C11 1.402(3) . ? C11 C12 1.387(3) . ? C12 N3 1.417(3) . ? C13 O1 1.217(3) . ? C13 N2 1.370(3) . ? C13 N3 1.379(3) . ? C14 C19 1.390(3) . ? C14 N2 1.405(3) . ? C14 C15 1.405(3) . ? C15 N1 1.389(3) . ? C15 C16 1.407(3) . ? C16 C17 1.401(3) . ? C16 C20 1.445(3) . ? C17 C18 1.378(3) . ? C18 C19 1.403(3) . ? C20 C22 1.399(3) . ? C20 C21 1.414(3) . ? C21 N1 1.381(3) . ? C21 C25 1.389(3) . ? C22 C23 1.378(3) . ? C23 C24 1.398(3) . ? C24 C25 1.386(3) . ? 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 O3 C26 O2 123.5(2) . . ? O3 C26 C27 119.3(2) . . ? O2 C26 C27 117.2(2) . . ? C33 C28 N5 115.80(19) . . ? C35 C29 N5 115.95(18) . . ? C34 C30 N5 115.55(19) . . ? C36 C31 N5 117.9(2) . . ? C28 C33 C37 110.0(2) . . ? C30 C34 C39 109.7(2) . . ? C29 C35 C38 109.97(19) . . ? C31 C36 C40 109.1(2) . . ? C33 C37 C43 111.9(2) . . ? C42 C38 C35 112.7(2) . . ? C41 C39 C34 112.2(3) . . ? C44 C40 C36 113.6(2) . . ? C2 C1 C6 117.5(2) . . ? C1 C2 C3 121.5(3) . . ? C4 C3 C2 121.0(2) . . ? C3 C4 C5 118.6(2) . . ? C4 C5 C6 119.6(2) . . ? C4 C5 C7 133.7(2) . . ? C6 C5 C7 106.7(2) . . ? N4 C6 C1 129.0(2) . . ? N4 C6 C5 109.2(2) . . ? C1 C6 C5 121.8(2) . . ? C9 C7 C8 119.5(2) . . ? C9 C7 C5 134.3(2) . . ? C8 C7 C5 106.2(2) . . ? N4 C8 C12 128.8(2) . . ? N4 C8 C7 109.3(2) . . ? C12 C8 C7 121.9(2) . . ? C10 C9 C7 118.6(2) . . ? C9 C10 C11 121.5(2) . . ? C12 C11 C10 121.0(2) . . ? C11 C12 C8 117.5(2) . . ? C11 C12 N3 123.7(2) . . ? C8 C12 N3 118.7(2) . . ? O1 C13 N2 124.7(2) . . ? O1 C13 N3 123.6(2) . . ? N2 C13 N3 111.7(2) . . ? C19 C14 N2 125.4(2) . . ? C19 C14 C15 116.8(2) . . ? N2 C14 C15 117.8(2) . . ? N1 C15 C14 128.5(2) . . ? N1 C15 C16 109.1(2) . . ? C14 C15 C16 122.4(2) . . ? C17 C16 C15 119.6(2) . . ? C17 C16 C20 133.9(2) . . ? C15 C16 C20 106.5(2) . . ? C18 C17 C16 118.1(2) . . ? C17 C18 C19 122.2(2) . . ? C14 C19 C18 121.0(2) . . ? C22 C20 C21 119.0(2) . . ? C22 C20 C16 134.3(2) . . ? C21 C20 C16 106.7(2) . . ? N1 C21 C25 129.1(2) . . ? N1 C21 C20 108.9(2) . . ? C25 C21 C20 122.0(2) . . ? C23 C22 C20 119.2(2) . . ? C22 C23 C24 120.8(2) . . ? C25 C24 C23 121.5(2) . . ? C24 C25 C21 117.4(2) . . ? C21 N1 C15 108.77(18) . . ? C13 N2 C14 128.1(2) . . ? C13 N3 C12 124.15(19) . . ? C8 N4 C6 108.52(19) . . ? C31 N5 C29 106.08(17) . . ? C31 N5 C30 111.53(18) . . ? C29 N5 C30 110.99(18) . . ? C31 N5 C28 110.53(18) . . ? C29 N5 C28 111.06(18) . . ? C30 N5 C28 106.72(17) . . ? 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 N5 C28 C33 C37 173.29(19) . . . . ? N5 C30 C34 C39 176.9(2) . . . . ? N5 C29 C35 C38 -166.8(2) . . . . ? N5 C31 C36 C40 177.6(2) . . . . ? C28 C33 C37 C43 171.2(2) . . . . ? C29 C35 C38 C42 -163.5(2) . . . . ? C30 C34 C39 C41 -172.1(3) . . . . ? C31 C36 C40 C44 179.3(3) . . . . ? C6 C1 C2 C3 -0.3(4) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C3 C4 C5 C7 -178.4(2) . . . . ? C2 C1 C6 N4 178.8(2) . . . . ? C2 C1 C6 C5 -0.6(3) . . . . ? C4 C5 C6 N4 -178.3(2) . . . . ? C7 C5 C6 N4 -0.2(2) . . . . ? C4 C5 C6 C1 1.2(3) . . . . ? C7 C5 C6 C1 179.3(2) . . . . ? C4 C5 C7 C9 -2.2(5) . . . . ? C6 C5 C7 C9 -180.0(2) . . . . ? C4 C5 C7 C8 177.7(2) . . . . ? C6 C5 C7 C8 -0.1(2) . . . . ? C9 C7 C8 N4 -179.8(2) . . . . ? C5 C7 C8 N4 0.3(2) . . . . ? C9 C7 C8 C12 -1.2(3) . . . . ? C5 C7 C8 C12 178.9(2) . . . . ? C8 C7 C9 C10 1.7(3) . . . . ? C5 C7 C9 C10 -178.4(2) . . . . ? C7 C9 C10 C11 -1.2(3) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 C8 0.5(3) . . . . ? C10 C11 C12 N3 -177.7(2) . . . . ? N4 C8 C12 C11 178.4(2) . . . . ? C7 C8 C12 C11 0.1(3) . . . . ? N4 C8 C12 N3 -3.3(3) . . . . ? C7 C8 C12 N3 178.4(2) . . . . ? C19 C14 C15 N1 -179.6(2) . . . . ? N2 C14 C15 N1 0.2(4) . . . . ? C19 C14 C15 C16 0.2(3) . . . . ? N2 C14 C15 C16 180.0(2) . . . . ? N1 C15 C16 C17 179.6(2) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? N1 C15 C16 C20 0.0(3) . . . . ? C14 C15 C16 C20 -179.8(2) . . . . ? C15 C16 C17 C18 0.4(4) . . . . ? C20 C16 C17 C18 179.9(3) . . . . ? C16 C17 C18 C19 -0.6(4) . . . . ? N2 C14 C19 C18 179.9(2) . . . . ? C15 C14 C19 C18 -0.3(4) . . . . ? C17 C18 C19 C14 0.6(4) . . . . ? C17 C16 C20 C22 0.4(5) . . . . ? C15 C16 C20 C22 179.9(3) . . . . ? C17 C16 C20 C21 -179.7(3) . . . . ? C15 C16 C20 C21 -0.2(3) . . . . ? C22 C20 C21 N1 -179.7(2) . . . . ? C16 C20 C21 N1 0.4(3) . . . . ? C22 C20 C21 C25 0.5(3) . . . . ? C16 C20 C21 C25 -179.4(2) . . . . ? C21 C20 C22 C23 -0.4(3) . . . . ? C16 C20 C22 C23 179.5(3) . . . . ? C20 C22 C23 C24 -0.1(4) . . . . ? C22 C23 C24 C25 0.4(4) . . . . ? C23 C24 C25 C21 -0.4(4) . . . . ? N1 C21 C25 C24 -179.8(2) . . . . ? C20 C21 C25 C24 -0.1(3) . . . . ? C25 C21 N1 C15 179.4(2) . . . . ? C20 C21 N1 C15 -0.4(3) . . . . ? C14 C15 N1 C21 -180.0(2) . . . . ? C16 C15 N1 C21 0.3(3) . . . . ? O1 C13 N2 C14 -5.5(4) . . . . ? N3 C13 N2 C14 174.3(2) . . . . ? C19 C14 N2 C13 8.9(4) . . . . ? C15 C14 N2 C13 -170.9(2) . . . . ? O1 C13 N3 C12 -1.1(4) . . . . ? N2 C13 N3 C12 179.1(2) . . . . ? C11 C12 N3 C13 -41.7(3) . . . . ? C8 C12 N3 C13 140.1(2) . . . . ? C12 C8 N4 C6 -178.9(2) . . . . ? C7 C8 N4 C6 -0.4(2) . . . . ? C1 C6 N4 C8 -179.1(2) . . . . ? C5 C6 N4 C8 0.4(2) . . . . ? C36 C31 N5 C29 176.3(2) . . . . ? C36 C31 N5 C30 55.3(3) . . . . ? C36 C31 N5 C28 -63.2(3) . . . . ? C35 C29 N5 C31 -175.6(2) . . . . ? C35 C29 N5 C30 -54.3(3) . . . . ? C35 C29 N5 C28 64.3(2) . . . . ? C34 C30 N5 C31 59.6(3) . . . . ? C34 C30 N5 C29 -58.5(3) . . . . ? C34 C30 N5 C28 -179.6(2) . . . . ? C33 C28 N5 C31 -67.8(3) . . . . ? C33 C28 N5 C29 49.6(3) . . . . ? C33 C28 N5 C30 170.7(2) . . . . ? 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 N1 H1 O2 0.86 1.96 2.781(2) 159.8 4_665 N2 H2 O2 0.86 1.95 2.809(2) 177.0 4_665 N3 H3 O3 0.86 2.10 2.926(2) 159.9 4_665 N3 H3 O2 0.86 2.60 3.327(3) 143.5 4_665 N4 H4 O3 0.86 2.21 2.820(2) 127.6 4_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.251 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.057 #==END data_2008jh0003 _database_code_depnum_ccdc_archive 'CCDC 715670' _chemical_compound_source ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H59 N5 O3' _chemical_formula_weight 754.00 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 0.0000 '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 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.980(5) _cell_length_b 13.774(5) _cell_length_c 15.173(5) _cell_angle_alpha 68.760(5) _cell_angle_beta 85.232(5) _cell_angle_gamma 81.541(5) _cell_volume 2114.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 32733 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9609 _exptl_absorpt_correction_T_max 0.9963 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44837 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.59 _reflns_number_total 9728 _reflns_number_gt 6254 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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. ; _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^)+(0.0766P)^2^+0.2090P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9728 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.7182(4) 0.5291(4) 0.3155(4) 0.0310(11) Uani 1 1 d . . . C2 C 0.7370(5) 0.6240(4) 0.2439(4) 0.0371(12) Uani 1 1 d . . . H2 H 0.6974 0.6473 0.1867 0.045 Uiso 1 1 calc R . . C3 C 0.8192(5) 0.6822(4) 0.2631(4) 0.0438(14) Uani 1 1 d . . . H3 H 0.8333 0.7467 0.2179 0.053 Uiso 1 1 calc R . . C4 C 0.8805(5) 0.6457(5) 0.3486(4) 0.0473(15) Uani 1 1 d . . . H4A H 0.9368 0.6853 0.3575 0.057 Uiso 1 1 calc R . . C5 C 0.8598(4) 0.5535(4) 0.4194(4) 0.0360(12) Uani 1 1 d . . . H5A H 0.9002 0.5306 0.4762 0.043 Uiso 1 1 calc R . . C6 C 0.7752(4) 0.4944(4) 0.4033(3) 0.0287(10) Uani 1 1 d . . . C7 C 0.7300(4) 0.3961(4) 0.4615(3) 0.0263(10) Uani 1 1 d . . . C8 C 0.7444(4) 0.3295(4) 0.5556(4) 0.0314(11) Uani 1 1 d . . . H8A H 0.7950 0.3432 0.5948 0.038 Uiso 1 1 calc R . . C9 C 0.6818(4) 0.2428(4) 0.5888(3) 0.0297(10) Uani 1 1 d . . . H9 H 0.6880 0.1994 0.6520 0.036 Uiso 1 1 calc R . . C10 C 0.6093(4) 0.2185(4) 0.5301(3) 0.0310(11) Uani 1 1 d . . . H10 H 0.5692 0.1588 0.5546 0.037 Uiso 1 1 calc R . . C11 C 0.5963(4) 0.2827(3) 0.4350(3) 0.0248(10) Uani 1 1 d . . . C12 C 0.6527(4) 0.3753(3) 0.4028(3) 0.0249(10) Uani 1 1 d . . . C13 C 0.5281(4) 0.1603(3) 0.3697(3) 0.0241(10) Uani 1 1 d . . . C14 C 0.3645(4) 0.0981(3) 0.1953(3) 0.0226(9) Uani 1 1 d . . . C15 C 0.4475(4) 0.0789(3) 0.2679(3) 0.0235(9) Uani 1 1 d . . . C16 C 0.5191(4) -0.0181(4) 0.2984(3) 0.0284(10) Uani 1 1 d . . . H16 H 0.5761 -0.0326 0.3450 0.034 Uiso 1 1 calc R . . C17 C 0.5071(4) -0.0951(3) 0.2600(3) 0.0301(11) Uani 1 1 d . . . H17 H 0.5550 -0.1601 0.2829 0.036 Uiso 1 1 calc R . . C18 C 0.4260(4) -0.0765(4) 0.1894(3) 0.0299(11) Uani 1 1 d . . . H18 H 0.4196 -0.1277 0.1641 0.036 Uiso 1 1 calc R . . C19 C 0.3535(4) 0.0216(3) 0.1566(3) 0.0246(9) Uani 1 1 d . . . C20 C 0.2686(4) 0.0717(3) 0.0799(3) 0.0252(10) Uani 1 1 d . . . C21 C 0.2221(5) 0.0397(4) 0.0139(3) 0.0352(11) Uani 1 1 d . . . H21 H 0.2432 -0.0288 0.0153 0.042 Uiso 1 1 calc R . . C22 C 0.1444(5) 0.1102(4) -0.0540(4) 0.0363(12) Uani 1 1 d . . . H22 H 0.1143 0.0895 -0.0991 0.044 Uiso 1 1 calc R . . C23 C 0.1108(4) 0.2130(4) -0.0552(3) 0.0342(11) Uani 1 1 d . . . H23 H 0.0581 0.2594 -0.1013 0.041 Uiso 1 1 calc R . . C24 C 0.1537(4) 0.2472(4) 0.0102(3) 0.0298(11) Uani 1 1 d . . . H24 H 0.1313 0.3154 0.0092 0.036 Uiso 1 1 calc R . . C25 C 0.2322(4) 0.1748(4) 0.0777(3) 0.0264(10) Uani 1 1 d . . . C26 C 0.3559(4) 0.4378(3) 0.1889(3) 0.0276(10) Uani 1 1 d . . . C27 C 0.2847(4) 0.5451(3) 0.1466(3) 0.0252(10) Uani 1 1 d . . . C28 C 0.3463(4) 0.6321(3) 0.1058(3) 0.0297(10) Uani 1 1 d . . . H28 H 0.4320 0.6241 0.1047 0.036 Uiso 1 1 calc R . . C29 C 0.2813(5) 0.7316(4) 0.0663(4) 0.0391(12) Uani 1 1 d . . . H29 H 0.3231 0.7899 0.0387 0.047 Uiso 1 1 calc R . . C30 C 0.1533(5) 0.7430(4) 0.0684(4) 0.0382(12) Uani 1 1 d . . . H30 H 0.1095 0.8093 0.0415 0.046 Uiso 1 1 calc R . . C31 C 0.0909(5) 0.6576(4) 0.1097(4) 0.0370(12) Uani 1 1 d . . . H31 H 0.0053 0.6659 0.1122 0.044 Uiso 1 1 calc R . . C32 C 0.1570(4) 0.5584(4) 0.1480(3) 0.0306(11) Uani 1 1 d . . . H32 H 0.1149 0.5001 0.1749 0.037 Uiso 1 1 calc R . . C33 C -0.2902(4) -0.6340(4) 0.9241(3) 0.0292(11) Uani 1 1 d . . . C34 C -0.3674(4) -0.6240(4) 0.9986(3) 0.0334(11) Uani 1 1 d . . . H909 H -0.3889 -0.5593 1.0057 0.040 Uiso 1 1 calc R . . C35 C -0.4108(5) -0.7131(4) 1.0616(4) 0.0376(12) Uani 1 1 d . . . H35 H -0.4625 -0.7082 1.1120 0.045 Uiso 1 1 calc R . . C36 C -0.3792(5) -0.8111(4) 1.0518(4) 0.0386(12) Uani 1 1 d . . . H36 H -0.4095 -0.8701 1.0958 0.046 Uiso 1 1 calc R . . C37 C -0.3037(4) -0.8209(4) 0.9777(3) 0.0334(11) Uani 1 1 d . . . H37 H -0.2834 -0.8860 0.9713 0.040 Uiso 1 1 calc R . . C38 C -0.2579(4) -0.7325(4) 0.9125(3) 0.0266(10) Uani 1 1 d . . . C39 C -0.1738(4) -0.7150(3) 0.8320(3) 0.0256(10) Uani 1 1 d . . . C40 C -0.1059(4) -0.7826(4) 0.7895(3) 0.0298(11) Uani 1 1 d . . . H40 H -0.1170 -0.8530 0.8092 0.036 Uiso 1 1 calc R . . C41 C -0.0216(4) -0.7400(4) 0.7170(3) 0.0292(10) Uani 1 1 d . . . H41 H 0.0236 -0.7831 0.6877 0.035 Uiso 1 1 calc R . . C42 C -0.0026(4) -0.6351(4) 0.6870(3) 0.0294(10) Uani 1 1 d . . . H42 H 0.0566 -0.6104 0.6396 0.035 Uiso 1 1 calc R . . C43 C -0.0707(4) -0.5662(3) 0.7265(3) 0.0245(10) Uani 1 1 d . . . C44 C -0.1579(4) -0.6079(4) 0.7994(3) 0.0264(10) Uani 1 1 d . . . C45 C 0.0220(4) -0.4027(3) 0.6331(3) 0.0250(10) Uani 1 1 d . . . C46 C 0.1710(4) -0.1825(3) 0.6217(3) 0.0290(10) Uani 1 1 d . . . C47 C 0.1092(4) -0.2356(3) 0.5789(3) 0.0277(10) Uani 1 1 d . . . C48 C 0.1323(4) -0.2161(4) 0.4834(3) 0.0305(11) Uani 1 1 d . . . H48 H 0.0903 -0.2480 0.4527 0.037 Uiso 1 1 calc R . . C49 C 0.2183(4) -0.1489(4) 0.4323(3) 0.0324(11) Uani 1 1 d . . . H49 H 0.2314 -0.1364 0.3680 0.039 Uiso 1 1 calc R . . C50 C 0.2842(4) -0.1007(4) 0.4748(3) 0.0337(11) Uani 1 1 d . . . H50 H 0.3429 -0.0581 0.4404 0.040 Uiso 1 1 calc R . . C51 C 0.2607(4) -0.1174(3) 0.5703(3) 0.0313(11) Uani 1 1 d . . . C52 C 0.3087(4) -0.0818(4) 0.6378(3) 0.0314(11) Uani 1 1 d . . . C53 C 0.4023(5) -0.0188(4) 0.6322(4) 0.0445(13) Uani 1 1 d . . . H53 H 0.4476 0.0082 0.5761 0.053 Uiso 1 1 calc R . . C54 C 0.4247(6) 0.0015(5) 0.7112(5) 0.0556(16) Uani 1 1 d . . . H54 H 0.4872 0.0413 0.7089 0.067 Uiso 1 1 calc R . . C55 C 0.3542(6) -0.0370(5) 0.7958(4) 0.0569(17) Uani 1 1 d . . . H55 H 0.3686 -0.0200 0.8477 0.068 Uiso 1 1 calc R . . C56 C 0.2636(6) -0.0999(4) 0.8024(4) 0.0469(14) Uani 1 1 d . . . H56 H 0.2178 -0.1265 0.8584 0.056 Uiso 1 1 calc R . . C57 C 0.2436(5) -0.1217(4) 0.7233(4) 0.0340(11) Uani 1 1 d . . . C58 C -0.1542(4) -0.2883(4) 0.8333(3) 0.0321(11) Uani 1 1 d . . . C59 C -0.2121(4) -0.2300(3) 0.8968(3) 0.0297(10) Uani 1 1 d . . . C60 C -0.1417(5) -0.1734(4) 0.9266(4) 0.0394(12) Uani 1 1 d . . . H60 H -0.0590 -0.1719 0.9078 0.047 Uiso 1 1 calc R . . C61 C -0.1932(5) -0.1179(4) 0.9851(4) 0.0471(14) Uani 1 1 d . . . H61 H -0.1452 -0.0787 1.0036 0.057 Uiso 1 1 calc R . . C62 C -0.3123(6) -0.1215(5) 1.0144(5) 0.0575(17) Uani 1 1 d . . . H62 H -0.3464 -0.0849 1.0533 0.069 Uiso 1 1 calc R . . C63 C -0.3843(6) -0.1794(5) 0.9869(6) 0.071(2) Uani 1 1 d . . . H63 H -0.4660 -0.1831 1.0081 0.085 Uiso 1 1 calc R . . C64 C -0.3328(6) -0.2322(5) 0.9270(5) 0.0556(16) Uani 1 1 d . . . H64 H -0.3816 -0.2698 0.9073 0.067 Uiso 1 1 calc R . . C65 C 0.3902(4) -0.4042(4) 0.7046(3) 0.0314(11) Uani 1 1 d . . . H65A H 0.3856 -0.3285 0.6751 0.038 Uiso 1 1 calc R . . H65B H 0.3066 -0.4218 0.7147 0.038 Uiso 1 1 calc R . . C66 C 0.4478(5) -0.4373(4) 0.7998(3) 0.0381(12) Uani 1 1 d . . . H66A H 0.5260 -0.4098 0.7915 0.046 Uiso 1 1 calc R . . H66B H 0.4639 -0.5134 0.8260 0.046 Uiso 1 1 calc R . . C67 C 0.3648(5) -0.3983(4) 0.8694(4) 0.0402(12) Uani 1 1 d . . . H67A H 0.4111 -0.4118 0.9253 0.048 Uiso 1 1 calc R . . H67B H 0.3438 -0.3229 0.8405 0.048 Uiso 1 1 calc R . . C68 C 0.2470(6) -0.4476(6) 0.9000(5) 0.0642(18) Uani 1 1 d . . . H68A H 0.1969 -0.4297 0.8461 0.096 Uiso 1 1 calc R . . H68B H 0.2030 -0.4219 0.9461 0.096 Uiso 1 1 calc R . . H68C H 0.2662 -0.5225 0.9272 0.096 Uiso 1 1 calc R . . C69 C 0.4707(4) -0.5730(4) 0.6778(4) 0.0332(11) Uani 1 1 d . . . H69A H 0.5081 -0.6001 0.6298 0.040 Uiso 1 1 calc R . . H69B H 0.5265 -0.5971 0.7299 0.040 Uiso 1 1 calc R . . C70 C 0.3507(5) -0.6194(4) 0.7134(4) 0.0387(12) Uani 1 1 d . . . H70A H 0.3149 -0.5969 0.7646 0.046 Uiso 1 1 calc R . . H70B H 0.2927 -0.5940 0.6627 0.046 Uiso 1 1 calc R . . C71 C 0.3734(5) -0.7387(4) 0.7483(4) 0.0420(13) Uani 1 1 d . . . H71A H 0.2945 -0.7657 0.7616 0.050 Uiso 1 1 calc R . . H71B H 0.4151 -0.7600 0.6981 0.050 Uiso 1 1 calc R . . C72 C 0.4495(6) -0.7879(5) 0.8361(4) 0.0548(16) Uani 1 1 d . . . H72A H 0.5315 -0.7691 0.8214 0.082 Uiso 1 1 calc R . . H72B H 0.4527 -0.8629 0.8577 0.082 Uiso 1 1 calc R . . H72C H 0.4125 -0.7630 0.8848 0.082 Uiso 1 1 calc R . . C73 C 0.3844(4) -0.4117(4) 0.5456(4) 0.0336(11) Uani 1 1 d . . . H73A H 0.3024 -0.4325 0.5615 0.040 Uiso 1 1 calc R . . H73B H 0.3757 -0.3356 0.5227 0.040 Uiso 1 1 calc R . . C74 C 0.4393(5) -0.4480(5) 0.4652(4) 0.0448(14) Uani 1 1 d . . . H74A H 0.4290 -0.5212 0.4810 0.054 Uiso 1 1 calc R . . H74B H 0.5269 -0.4424 0.4582 0.054 Uiso 1 1 calc R . . C75 C 0.3768(5) -0.3812(5) 0.3692(4) 0.0487(14) Uani 1 1 d . . . H75A H 0.3705 -0.3073 0.3605 0.058 Uiso 1 1 calc R . . H75B H 0.4280 -0.3924 0.3177 0.058 Uiso 1 1 calc R . . C76 C 0.2505(6) -0.4093(6) 0.3658(5) 0.0638(18) Uani 1 1 d . . . H76A H 0.2575 -0.4792 0.3649 0.096 Uiso 1 1 calc R . . H76B H 0.2112 -0.3608 0.3096 0.096 Uiso 1 1 calc R . . H76C H 0.2023 -0.4057 0.4205 0.096 Uiso 1 1 calc R . . C77 C 0.5877(4) -0.4223(3) 0.6144(3) 0.0273(10) Uani 1 1 d . . . H77A H 0.6279 -0.4400 0.6738 0.033 Uiso 1 1 calc R . . H77B H 0.6335 -0.4643 0.5804 0.033 Uiso 1 1 calc R . . C78 C 0.5958(4) -0.3077(4) 0.5570(4) 0.0329(11) Uani 1 1 d . . . H78A H 0.5390 -0.2638 0.5836 0.039 Uiso 1 1 calc R . . H78B H 0.5734 -0.2921 0.4924 0.039 Uiso 1 1 calc R . . C79 C 0.7273(4) -0.2845(4) 0.5584(4) 0.0321(11) Uani 1 1 d . . . H79A H 0.7845 -0.3408 0.5486 0.038 Uiso 1 1 calc R . . H79B H 0.7415 -0.2832 0.6202 0.038 Uiso 1 1 calc R . . C80 C 0.7530(5) -0.1799(4) 0.4826(4) 0.0409(13) Uani 1 1 d . . . H80A H 0.7411 -0.1814 0.4211 0.061 Uiso 1 1 calc R . . H80B H 0.8365 -0.1690 0.4865 0.061 Uiso 1 1 calc R . . H80C H 0.6977 -0.1238 0.4925 0.061 Uiso 1 1 calc R . . C81 C -0.1106(4) 0.1217(4) 0.4376(3) 0.0309(11) Uani 1 1 d . . . H81A H -0.1219 0.1704 0.4713 0.037 Uiso 1 1 calc R . . H81B H -0.1914 0.1150 0.4206 0.037 Uiso 1 1 calc R . . C82 C -0.0549(5) 0.0158(4) 0.5035(4) 0.0461(14) Uani 1 1 d . . . H82A H 0.0289 0.0199 0.5165 0.055 Uiso 1 1 calc R . . H82B H -0.0520 -0.0357 0.4733 0.055 Uiso 1 1 calc R . . C83 C -0.1304(6) -0.0189(4) 0.5962(4) 0.0491(14) Uani 1 1 d . . . H83A H -0.2171 0.0040 0.5834 0.059 Uiso 1 1 calc R . . H83B H -0.1193 -0.0950 0.6240 0.059 Uiso 1 1 calc R . . C84 C -0.0942(6) 0.0241(5) 0.6633(5) 0.0582(16) Uani 1 1 d . . . H84A H -0.0111 -0.0046 0.6815 0.087 Uiso 1 1 calc R . . H84B H -0.1483 0.0062 0.7183 0.087 Uiso 1 1 calc R . . H84C H -0.0993 0.0991 0.6344 0.087 Uiso 1 1 calc R . . C85 C -0.0129(5) 0.0928(4) 0.2927(4) 0.0369(12) Uani 1 1 d . . . H85A H 0.0397 0.1225 0.2377 0.044 Uiso 1 1 calc R . . H85B H 0.0314 0.0273 0.3325 0.044 Uiso 1 1 calc R . . C86 C -0.1281(5) 0.0685(4) 0.2597(5) 0.0483(14) Uani 1 1 d . . . H86A H -0.1806 0.1334 0.2286 0.058 Uiso 1 1 calc R . . H86B H -0.1738 0.0257 0.3138 0.058 Uiso 1 1 calc R . . C87 C -0.0909(8) 0.0083(6) 0.1889(7) 0.093(3) Uani 1 1 d . . . H87A H -0.1652 -0.0113 0.1730 0.112 Uiso 1 1 calc R . . H87B H -0.0578 0.0567 0.1310 0.112 Uiso 1 1 calc R . . C88 C -0.0033(8) -0.0841(7) 0.2208(7) 0.095(3) Uani 1 1 d . . . H88A H 0.0762 -0.0645 0.2239 0.143 Uiso 1 1 calc R . . H88B H 0.0013 -0.1210 0.1775 0.143 Uiso 1 1 calc R . . H88C H -0.0286 -0.1288 0.2825 0.143 Uiso 1 1 calc R . . C89 C -0.1050(4) 0.2711(4) 0.2890(3) 0.0291(10) Uani 1 1 d . . . H89A H -0.1061 0.3202 0.3217 0.035 Uiso 1 1 calc R . . H89B H -0.1895 0.2600 0.2861 0.035 Uiso 1 1 calc R . . C90 C -0.0551(4) 0.3215(3) 0.1885(3) 0.0292(10) Uani 1 1 d . . . H90A H 0.0312 0.3290 0.1899 0.035 Uiso 1 1 calc R . . H90B H -0.0610 0.2764 0.1529 0.035 Uiso 1 1 calc R . . C91 C -0.1269(5) 0.4287(4) 0.1398(3) 0.0359(11) Uani 1 1 d . . . H91A H -0.2138 0.4213 0.1422 0.043 Uiso 1 1 calc R . . H91B H -0.1173 0.4744 0.1740 0.043 Uiso 1 1 calc R . . C92 C -0.0855(5) 0.4788(4) 0.0386(4) 0.0427(13) Uani 1 1 d . . . H92A H -0.0006 0.4897 0.0359 0.064 Uiso 1 1 calc R . . H92B H -0.1350 0.5451 0.0106 0.064 Uiso 1 1 calc R . . H92C H -0.0942 0.4337 0.0045 0.064 Uiso 1 1 calc R . . C93 C 0.0920(4) 0.1826(4) 0.3702(3) 0.0338(11) Uani 1 1 d . . . H93A H 0.1399 0.1140 0.3952 0.041 Uiso 1 1 calc R . . H93B H 0.1327 0.2220 0.3116 0.041 Uiso 1 1 calc R . . C94 C 0.0947(5) 0.2380(5) 0.4398(4) 0.0417(13) Uani 1 1 d . . . H94A H 0.0591 0.1980 0.5004 0.050 Uiso 1 1 calc R . . H94B H 0.0473 0.3070 0.4166 0.050 Uiso 1 1 calc R . . C95 C 0.2287(5) 0.2482(5) 0.4506(4) 0.0448(14) Uani 1 1 d . . . H95A H 0.2770 0.1797 0.4654 0.054 Uiso 1 1 calc R . . H95B H 0.2604 0.2942 0.3909 0.054 Uiso 1 1 calc R . . C96 C 0.2445(5) 0.2905(6) 0.5260(5) 0.0575(17) Uani 1 1 d . . . H96A H 0.1917 0.3555 0.5148 0.086 Uiso 1 1 calc R . . H96B H 0.3287 0.3022 0.5253 0.086 Uiso 1 1 calc R . . H96C H 0.2233 0.2408 0.5866 0.086 Uiso 1 1 calc R . . N1 N 0.6464(3) 0.4549(3) 0.3154(3) 0.0276(9) Uani 1 1 d . . . H901 H 0.6048 0.4577 0.2687 0.033 Uiso 1 1 calc R . . N2 N 0.5296(3) 0.2603(3) 0.3704(3) 0.0270(8) Uani 1 1 d . . . H902 H 0.4875 0.3118 0.3291 0.032 Uiso 1 1 calc R . . N3 N 0.4544(3) 0.1624(3) 0.3005(3) 0.0240(8) Uani 1 1 d . . . H903 H 0.4075 0.2201 0.2742 0.029 Uiso 1 1 calc R . . N4 N 0.2893(3) 0.1894(3) 0.1495(2) 0.0221(8) Uani 1 1 d . . . H904 H 0.2795 0.2455 0.1631 0.027 Uiso 1 1 calc R . . N5 N 0.1614(3) -0.1848(3) 0.7140(3) 0.0288(9) Uani 1 1 d . . . H905 H 0.1130 -0.2194 0.7580 0.035 Uiso 1 1 calc R . . N6 N 0.0275(3) -0.3063(3) 0.6372(3) 0.0286(9) Uani 1 1 d . . . H906 H -0.0209 -0.2870 0.6771 0.034 Uiso 1 1 calc R . . N7 N -0.0548(3) -0.4594(3) 0.7032(3) 0.0286(9) Uani 1 1 d . . . H907 H -0.0975 -0.4266 0.7363 0.034 Uiso 1 1 calc R . . N8 N -0.2310(3) -0.5592(3) 0.8531(3) 0.0282(9) Uani 1 1 d . . . H908 H -0.2387 -0.4933 0.8441 0.034 Uiso 1 1 calc R . . N9 N 0.4576(3) -0.4534(3) 0.6364(3) 0.0284(9) Uani 1 1 d . . . N10 N -0.0342(3) 0.1677(3) 0.3473(3) 0.0293(9) Uani 1 1 d . . . O1 O 0.5854(3) 0.0813(2) 0.4237(2) 0.0300(7) Uani 1 1 d . . . O2 O 0.0799(3) -0.4354(3) 0.5745(2) 0.0335(8) Uani 1 1 d . . . O3 O 0.2983(3) 0.3589(2) 0.2083(2) 0.0297(7) Uani 1 1 d . . . O4 O 0.4687(3) 0.4321(2) 0.2037(2) 0.0332(8) Uani 1 1 d . . . O5 O -0.2178(3) -0.3453(3) 0.8123(2) 0.0364(8) Uani 1 1 d . . . O6 O -0.0444(3) -0.2770(3) 0.8055(3) 0.0404(8) Uani 1 1 d . . . 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 0.025(2) 0.037(3) 0.039(3) -0.024(2) 0.003(2) -0.003(2) C2 0.038(3) 0.035(3) 0.040(3) -0.017(2) 0.007(2) -0.005(2) C3 0.046(3) 0.031(3) 0.060(4) -0.022(3) 0.007(3) -0.012(2) C4 0.037(3) 0.053(4) 0.069(4) -0.039(3) 0.006(3) -0.018(3) C5 0.028(3) 0.044(3) 0.046(3) -0.028(3) 0.002(2) -0.008(2) C6 0.017(2) 0.041(3) 0.033(3) -0.021(2) 0.002(2) 0.0007(19) C7 0.021(2) 0.031(2) 0.036(3) -0.023(2) -0.003(2) 0.0001(19) C8 0.021(2) 0.041(3) 0.039(3) -0.024(2) -0.007(2) 0.006(2) C9 0.028(2) 0.034(3) 0.028(3) -0.015(2) -0.003(2) 0.004(2) C10 0.026(2) 0.036(3) 0.033(3) -0.015(2) 0.000(2) -0.001(2) C11 0.019(2) 0.031(2) 0.027(3) -0.014(2) 0.0000(19) -0.0022(19) C12 0.023(2) 0.027(2) 0.026(3) -0.013(2) -0.0013(19) 0.0036(18) C13 0.020(2) 0.029(2) 0.024(2) -0.009(2) -0.0007(19) -0.0034(19) C14 0.019(2) 0.022(2) 0.024(2) -0.0058(18) 0.0053(18) -0.0037(17) C15 0.023(2) 0.022(2) 0.027(2) -0.0093(19) 0.0020(19) -0.0055(18) C16 0.025(2) 0.033(3) 0.025(2) -0.008(2) -0.0020(19) -0.003(2) C17 0.032(3) 0.023(2) 0.032(3) -0.009(2) -0.002(2) 0.004(2) C18 0.037(3) 0.022(2) 0.032(3) -0.012(2) 0.001(2) -0.001(2) C19 0.024(2) 0.023(2) 0.024(2) -0.0075(19) 0.0014(19) -0.0019(18) C20 0.026(2) 0.023(2) 0.025(2) -0.0065(19) -0.0012(19) -0.0037(18) C21 0.047(3) 0.031(3) 0.032(3) -0.014(2) -0.010(2) -0.003(2) C22 0.040(3) 0.039(3) 0.035(3) -0.019(2) -0.013(2) 0.001(2) C23 0.036(3) 0.032(3) 0.033(3) -0.008(2) -0.014(2) 0.001(2) C24 0.032(3) 0.026(2) 0.032(3) -0.013(2) -0.007(2) 0.000(2) C25 0.028(2) 0.029(2) 0.024(2) -0.011(2) -0.001(2) -0.010(2) C26 0.037(3) 0.025(2) 0.019(2) -0.0046(19) -0.007(2) -0.005(2) C27 0.032(2) 0.026(2) 0.020(2) -0.0101(19) -0.0022(19) -0.0043(19) C28 0.031(3) 0.029(2) 0.030(3) -0.011(2) -0.002(2) -0.004(2) C29 0.042(3) 0.024(2) 0.049(3) -0.009(2) -0.009(3) -0.006(2) C30 0.043(3) 0.025(3) 0.040(3) -0.008(2) 0.000(2) 0.004(2) C31 0.032(3) 0.037(3) 0.039(3) -0.012(2) 0.003(2) -0.001(2) C32 0.035(3) 0.026(2) 0.029(3) -0.009(2) 0.003(2) -0.005(2) C33 0.020(2) 0.031(3) 0.031(3) -0.003(2) -0.004(2) -0.0052(19) C34 0.029(3) 0.036(3) 0.034(3) -0.011(2) 0.002(2) -0.003(2) C35 0.032(3) 0.044(3) 0.034(3) -0.010(2) 0.008(2) -0.012(2) C36 0.041(3) 0.034(3) 0.035(3) -0.004(2) 0.007(2) -0.012(2) C37 0.034(3) 0.029(3) 0.035(3) -0.008(2) 0.001(2) -0.010(2) C38 0.024(2) 0.034(3) 0.023(2) -0.010(2) 0.0041(19) -0.009(2) C39 0.022(2) 0.027(2) 0.027(2) -0.0078(19) -0.0075(19) -0.0024(18) C40 0.032(3) 0.031(2) 0.028(3) -0.010(2) -0.007(2) -0.007(2) C41 0.028(2) 0.033(3) 0.027(3) -0.011(2) -0.008(2) -0.001(2) C42 0.024(2) 0.042(3) 0.021(2) -0.010(2) -0.0022(19) -0.001(2) C43 0.022(2) 0.030(2) 0.020(2) -0.0045(19) -0.0023(19) -0.0057(19) C44 0.021(2) 0.031(2) 0.025(2) -0.008(2) -0.0053(19) 0.0010(19) C45 0.019(2) 0.028(2) 0.025(2) -0.006(2) -0.0030(19) -0.0024(19) C46 0.022(2) 0.025(2) 0.033(3) -0.004(2) 0.003(2) 0.0000(19) C47 0.023(2) 0.026(2) 0.027(3) -0.004(2) 0.0045(19) 0.0016(19) C48 0.028(2) 0.033(3) 0.027(3) -0.008(2) -0.001(2) 0.004(2) C49 0.033(3) 0.030(3) 0.024(3) -0.001(2) 0.005(2) 0.003(2) C50 0.031(3) 0.025(2) 0.033(3) -0.001(2) 0.012(2) 0.001(2) C51 0.029(2) 0.019(2) 0.038(3) -0.002(2) 0.000(2) 0.0002(19) C52 0.031(3) 0.024(2) 0.034(3) -0.006(2) 0.004(2) -0.001(2) C53 0.049(3) 0.035(3) 0.048(3) -0.012(3) 0.008(3) -0.013(3) C54 0.065(4) 0.053(4) 0.056(4) -0.023(3) 0.012(3) -0.028(3) C55 0.076(4) 0.055(4) 0.051(4) -0.025(3) -0.002(3) -0.027(3) C56 0.061(4) 0.040(3) 0.043(3) -0.015(3) 0.003(3) -0.019(3) C57 0.033(3) 0.027(2) 0.038(3) -0.007(2) 0.001(2) -0.006(2) C58 0.033(3) 0.028(3) 0.028(3) -0.002(2) 0.000(2) -0.002(2) C59 0.026(2) 0.022(2) 0.033(3) -0.003(2) 0.005(2) 0.0004(19) C60 0.032(3) 0.047(3) 0.038(3) -0.018(3) 0.004(2) 0.001(2) C61 0.050(4) 0.045(3) 0.050(4) -0.022(3) 0.005(3) -0.008(3) C62 0.063(4) 0.049(4) 0.063(4) -0.029(3) 0.020(3) -0.003(3) C63 0.049(4) 0.065(4) 0.108(6) -0.049(4) 0.035(4) -0.012(3) C64 0.048(4) 0.050(4) 0.081(5) -0.038(3) 0.019(3) -0.018(3) C65 0.030(3) 0.029(2) 0.036(3) -0.017(2) 0.001(2) 0.005(2) C66 0.039(3) 0.048(3) 0.026(3) -0.016(2) -0.004(2) 0.004(2) C67 0.041(3) 0.052(3) 0.029(3) -0.020(3) -0.003(2) 0.006(3) C68 0.061(4) 0.086(5) 0.051(4) -0.033(4) 0.021(3) -0.015(4) C69 0.033(3) 0.030(3) 0.036(3) -0.013(2) 0.000(2) -0.001(2) C70 0.032(3) 0.041(3) 0.046(3) -0.019(3) 0.005(2) -0.007(2) C71 0.044(3) 0.039(3) 0.044(3) -0.012(3) -0.006(3) -0.010(2) C72 0.068(4) 0.048(3) 0.045(4) -0.005(3) -0.016(3) -0.021(3) C73 0.029(3) 0.040(3) 0.036(3) -0.021(2) -0.010(2) 0.005(2) C74 0.034(3) 0.068(4) 0.037(3) -0.030(3) -0.006(2) 0.010(3) C75 0.037(3) 0.070(4) 0.046(3) -0.034(3) -0.006(3) 0.010(3) C76 0.065(4) 0.089(5) 0.046(4) -0.032(4) -0.004(3) -0.010(4) C77 0.020(2) 0.031(2) 0.030(3) -0.013(2) -0.0002(19) 0.0034(19) C78 0.026(2) 0.033(3) 0.039(3) -0.013(2) -0.003(2) 0.000(2) C79 0.028(3) 0.027(2) 0.040(3) -0.012(2) -0.005(2) 0.000(2) C80 0.037(3) 0.031(3) 0.051(3) -0.009(2) -0.007(3) -0.006(2) C81 0.022(2) 0.027(2) 0.034(3) -0.001(2) 0.000(2) -0.0004(19) C82 0.034(3) 0.037(3) 0.054(4) -0.005(3) 0.008(3) -0.001(2) C83 0.053(4) 0.034(3) 0.046(3) 0.000(3) -0.001(3) 0.000(3) C84 0.055(4) 0.048(4) 0.060(4) -0.007(3) -0.005(3) -0.003(3) C85 0.040(3) 0.028(2) 0.043(3) -0.017(2) 0.000(2) 0.009(2) C86 0.051(3) 0.040(3) 0.063(4) -0.026(3) -0.003(3) -0.010(3) C87 0.091(6) 0.069(5) 0.147(8) -0.066(5) -0.063(6) 0.015(4) C88 0.091(6) 0.095(6) 0.131(8) -0.081(6) 0.015(6) -0.013(5) C89 0.027(2) 0.027(2) 0.036(3) -0.014(2) -0.003(2) 0.0021(19) C90 0.030(2) 0.025(2) 0.033(3) -0.012(2) 0.004(2) -0.002(2) C91 0.043(3) 0.033(3) 0.029(3) -0.010(2) -0.008(2) 0.002(2) C92 0.043(3) 0.044(3) 0.033(3) -0.006(2) -0.001(2) 0.002(2) C93 0.023(2) 0.047(3) 0.030(3) -0.012(2) -0.003(2) -0.003(2) C94 0.033(3) 0.058(3) 0.041(3) -0.021(3) -0.001(2) -0.016(3) C95 0.036(3) 0.065(4) 0.039(3) -0.022(3) 0.002(2) -0.016(3) C96 0.036(3) 0.095(5) 0.059(4) -0.043(4) 0.005(3) -0.027(3) N1 0.030(2) 0.026(2) 0.031(2) -0.0134(17) -0.0039(17) -0.0061(16) N2 0.0236(19) 0.028(2) 0.027(2) -0.0063(17) -0.0105(17) -0.0003(16) N3 0.0257(19) 0.0225(19) 0.024(2) -0.0091(16) -0.0054(16) 0.0003(15) N4 0.0250(19) 0.0184(18) 0.025(2) -0.0093(15) -0.0038(16) -0.0027(15) N5 0.029(2) 0.028(2) 0.025(2) -0.0035(17) 0.0043(17) -0.0079(17) N6 0.027(2) 0.036(2) 0.023(2) -0.0119(18) 0.0071(17) -0.0053(17) N7 0.030(2) 0.026(2) 0.027(2) -0.0069(17) 0.0016(17) -0.0016(16) N8 0.0239(19) 0.027(2) 0.029(2) -0.0044(17) 0.0016(17) -0.0036(16) N9 0.0238(19) 0.031(2) 0.032(2) -0.0159(18) -0.0040(17) 0.0025(16) N10 0.023(2) 0.031(2) 0.033(2) -0.0104(18) 0.0016(17) -0.0016(17) O1 0.0294(17) 0.0307(17) 0.0298(18) -0.0109(14) -0.0108(14) 0.0025(14) O2 0.0299(18) 0.0390(19) 0.0318(19) -0.0139(16) 0.0089(15) -0.0069(15) O3 0.0341(18) 0.0220(16) 0.0327(18) -0.0089(14) -0.0038(15) -0.0034(14) O4 0.0316(18) 0.0310(18) 0.035(2) -0.0085(15) -0.0122(15) -0.0003(14) O5 0.0352(19) 0.0320(18) 0.041(2) -0.0119(16) 0.0006(16) -0.0041(15) O6 0.035(2) 0.050(2) 0.041(2) -0.0214(18) 0.0121(16) -0.0116(17) _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 1.381(6) . ? C1 C2 1.395(7) . ? C1 C6 1.408(7) . ? C2 C3 1.403(7) . ? C3 C4 1.400(8) . ? C4 C5 1.369(8) . ? C5 C6 1.411(6) . ? C6 C7 1.455(7) . ? C7 C8 1.397(7) . ? C7 C12 1.407(6) . ? C8 C9 1.378(7) . ? C9 C10 1.398(6) . ? C10 C11 1.399(7) . ? C11 C12 1.407(6) . ? C11 N2 1.413(5) . ? C12 N1 1.380(6) . ? C13 O1 1.220(5) . ? C13 N3 1.367(5) . ? C13 N2 1.383(6) . ? C14 N4 1.379(6) . ? C14 C19 1.402(6) . ? C14 C15 1.413(6) . ? C15 C16 1.386(6) . ? C15 N3 1.422(5) . ? C16 C17 1.408(6) . ? C17 C18 1.378(7) . ? C18 C19 1.404(6) . ? C19 C20 1.452(6) . ? C20 C21 1.389(6) . ? C20 C25 1.406(6) . ? C21 C22 1.382(7) . ? C22 C23 1.404(7) . ? C23 C24 1.383(6) . ? C24 C25 1.393(6) . ? C25 N4 1.390(5) . ? C26 O4 1.263(6) . ? C26 O3 1.269(5) . ? C26 C27 1.504(6) . ? C27 C28 1.382(6) . ? C27 C32 1.387(7) . ? C28 C29 1.391(7) . ? C29 C30 1.390(7) . ? C30 C31 1.369(7) . ? C31 C32 1.391(7) . ? C33 N8 1.386(6) . ? C33 C34 1.391(7) . ? C33 C38 1.421(6) . ? C34 C35 1.377(7) . ? C35 C36 1.401(7) . ? C36 C37 1.375(7) . ? C37 C38 1.392(6) . ? C38 C39 1.438(6) . ? C39 C44 1.409(6) . ? C39 C40 1.410(7) . ? C40 C41 1.390(7) . ? C41 C42 1.390(6) . ? C42 C43 1.396(7) . ? C43 C44 1.413(6) . ? C43 N7 1.418(6) . ? C44 N8 1.374(6) . ? C45 O2 1.229(5) . ? C45 N6 1.362(6) . ? C45 N7 1.377(6) . ? C46 N5 1.385(6) . ? C46 C47 1.407(6) . ? C46 C51 1.416(6) . ? C47 C48 1.383(7) . ? C47 N6 1.428(6) . ? C48 C49 1.402(7) . ? C49 C50 1.381(7) . ? C50 C51 1.390(7) . ? C51 C52 1.449(7) . ? C52 C57 1.393(7) . ? C52 C53 1.417(7) . ? C53 C54 1.375(8) . ? C54 C55 1.411(9) . ? C55 C56 1.387(8) . ? C56 C57 1.380(7) . ? C57 N5 1.390(6) . ? C58 O6 1.256(6) . ? C58 O5 1.259(6) . ? C58 C59 1.512(7) . ? C59 C64 1.366(7) . ? C59 C60 1.379(7) . ? C60 C61 1.404(7) . ? C61 C62 1.349(8) . ? C62 C63 1.384(9) . ? C63 C64 1.395(9) . ? C65 C66 1.511(7) . ? C65 N9 1.521(6) . ? C66 C67 1.531(7) . ? C67 C68 1.510(8) . ? C69 C70 1.521(7) . ? C69 N9 1.524(6) . ? C70 C71 1.520(7) . ? C71 C72 1.515(8) . ? C73 C74 1.528(7) . ? C73 N9 1.531(6) . ? C74 C75 1.565(8) . ? C75 C76 1.503(8) . ? C77 C78 1.514(6) . ? C77 N9 1.527(6) . ? C78 C79 1.526(6) . ? C79 C80 1.531(7) . ? C81 C82 1.511(7) . ? C81 N10 1.523(6) . ? C82 C83 1.527(8) . ? C83 C84 1.455(9) . ? C85 C86 1.521(7) . ? C85 N10 1.523(6) . ? C86 C87 1.577(10) . ? C87 C88 1.432(11) . ? C89 N10 1.513(6) . ? C89 C90 1.522(7) . ? C90 C91 1.521(7) . ? C91 C92 1.500(7) . ? C93 C94 1.514(7) . ? C93 N10 1.516(6) . ? C94 C95 1.525(7) . ? C95 C96 1.491(7) . ? 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 C2 128.8(4) . . ? N1 C1 C6 108.8(4) . . ? C2 C1 C6 122.4(4) . . ? C1 C2 C3 116.1(5) . . ? C4 C3 C2 121.7(5) . . ? C5 C4 C3 121.9(5) . . ? C4 C5 C6 117.8(5) . . ? C1 C6 C5 120.0(5) . . ? C1 C6 C7 107.3(4) . . ? C5 C6 C7 132.7(4) . . ? C8 C7 C12 120.6(4) . . ? C8 C7 C6 134.3(4) . . ? C12 C7 C6 105.1(4) . . ? C9 C8 C7 118.2(4) . . ? C8 C9 C10 121.8(5) . . ? C9 C10 C11 120.8(4) . . ? C10 C11 C12 117.4(4) . . ? C10 C11 N2 123.9(4) . . ? C12 C11 N2 118.6(4) . . ? N1 C12 C11 128.9(4) . . ? N1 C12 C7 110.3(4) . . ? C11 C12 C7 120.8(4) . . ? O1 C13 N3 125.0(4) . . ? O1 C13 N2 124.1(4) . . ? N3 C13 N2 110.9(4) . . ? N4 C14 C19 110.2(4) . . ? N4 C14 C15 128.3(4) . . ? C19 C14 C15 121.4(4) . . ? C16 C15 C14 117.4(4) . . ? C16 C15 N3 125.3(4) . . ? C14 C15 N3 117.2(4) . . ? C15 C16 C17 121.0(4) . . ? C18 C17 C16 121.6(4) . . ? C17 C18 C19 118.3(4) . . ? C14 C19 C18 120.2(4) . . ? C14 C19 C20 105.8(4) . . ? C18 C19 C20 133.7(4) . . ? C21 C20 C25 118.9(4) . . ? C21 C20 C19 134.3(4) . . ? C25 C20 C19 106.8(4) . . ? C22 C21 C20 119.6(4) . . ? C21 C22 C23 120.3(4) . . ? C24 C23 C22 121.7(4) . . ? C23 C24 C25 116.9(4) . . ? N4 C25 C24 128.4(4) . . ? N4 C25 C20 109.0(4) . . ? C24 C25 C20 122.6(4) . . ? O4 C26 O3 124.2(4) . . ? O4 C26 C27 118.0(4) . . ? O3 C26 C27 117.7(4) . . ? C28 C27 C32 119.0(4) . . ? C28 C27 C26 120.1(4) . . ? C32 C27 C26 120.9(4) . . ? C27 C28 C29 120.5(4) . . ? C30 C29 C28 119.4(5) . . ? C31 C30 C29 120.7(5) . . ? C30 C31 C32 119.4(5) . . ? C27 C32 C31 121.0(4) . . ? N8 C33 C34 129.9(4) . . ? N8 C33 C38 108.7(4) . . ? C34 C33 C38 121.3(4) . . ? C35 C34 C33 117.8(5) . . ? C34 C35 C36 121.7(5) . . ? C37 C36 C35 120.5(5) . . ? C36 C37 C38 119.5(5) . . ? C37 C38 C33 119.2(4) . . ? C37 C38 C39 134.3(4) . . ? C33 C38 C39 106.4(4) . . ? C44 C39 C40 120.3(4) . . ? C44 C39 C38 106.5(4) . . ? C40 C39 C38 133.0(4) . . ? C41 C40 C39 117.6(4) . . ? C42 C41 C40 122.2(4) . . ? C41 C42 C43 121.3(4) . . ? C42 C43 C44 117.2(4) . . ? C42 C43 N7 125.4(4) . . ? C44 C43 N7 117.3(4) . . ? N8 C44 C39 109.6(4) . . ? N8 C44 C43 128.9(4) . . ? C39 C44 C43 121.3(4) . . ? O2 C45 N6 123.9(4) . . ? O2 C45 N7 124.2(4) . . ? N6 C45 N7 111.8(4) . . ? N5 C46 C47 129.4(4) . . ? N5 C46 C51 109.6(4) . . ? C47 C46 C51 121.0(4) . . ? C48 C47 C46 117.8(4) . . ? C48 C47 N6 124.5(4) . . ? C46 C47 N6 117.6(4) . . ? C47 C48 C49 120.7(4) . . ? C50 C49 C48 121.9(4) . . ? C49 C50 C51 118.3(4) . . ? C50 C51 C46 120.1(4) . . ? C50 C51 C52 134.5(4) . . ? C46 C51 C52 105.4(4) . . ? C57 C52 C53 118.9(5) . . ? C57 C52 C51 107.6(4) . . ? C53 C52 C51 133.5(5) . . ? C54 C53 C52 118.7(5) . . ? C53 C54 C55 120.9(5) . . ? C56 C55 C54 120.8(5) . . ? C57 C56 C55 117.8(5) . . ? C56 C57 N5 128.0(5) . . ? C56 C57 C52 122.8(5) . . ? N5 C57 C52 109.2(4) . . ? O6 C58 O5 124.3(4) . . ? O6 C58 C59 117.2(4) . . ? O5 C58 C59 118.5(4) . . ? C64 C59 C60 118.3(5) . . ? C64 C59 C58 122.1(5) . . ? C60 C59 C58 119.6(4) . . ? C59 C60 C61 120.9(5) . . ? C62 C61 C60 119.8(5) . . ? C61 C62 C63 120.4(6) . . ? C62 C63 C64 119.2(6) . . ? C59 C64 C63 121.4(6) . . ? C66 C65 N9 115.3(4) . . ? C65 C66 C67 112.0(4) . . ? C68 C67 C66 114.9(5) . . ? C70 C69 N9 115.0(4) . . ? C71 C70 C69 110.6(4) . . ? C72 C71 C70 114.2(4) . . ? C74 C73 N9 116.0(4) . . ? C73 C74 C75 111.8(4) . . ? C76 C75 C74 112.0(5) . . ? C78 C77 N9 115.6(4) . . ? C77 C78 C79 109.2(4) . . ? C78 C79 C80 112.7(4) . . ? C82 C81 N10 114.4(4) . . ? C81 C82 C83 110.7(4) . . ? C84 C83 C82 111.7(5) . . ? C86 C85 N10 115.8(4) . . ? C85 C86 C87 109.8(5) . . ? C88 C87 C86 116.7(7) . . ? N10 C89 C90 115.6(4) . . ? C91 C90 C89 110.8(4) . . ? C92 C91 C90 112.7(4) . . ? C94 C93 N10 116.4(4) . . ? C93 C94 C95 108.2(4) . . ? C96 C95 C94 113.0(5) . . ? C12 N1 C1 108.4(4) . . ? C13 N2 C11 123.9(4) . . ? C13 N3 C15 126.5(4) . . ? C14 N4 C25 108.1(3) . . ? C46 N5 C57 108.2(4) . . ? C45 N6 C47 123.4(4) . . ? C45 N7 C43 126.7(4) . . ? C44 N8 C33 108.6(4) . . ? C65 N9 C69 112.0(4) . . ? C65 N9 C77 109.9(3) . . ? C69 N9 C77 107.0(3) . . ? C65 N9 C73 107.2(3) . . ? C69 N9 C73 110.8(3) . . ? C77 N9 C73 109.9(4) . . ? C89 N10 C93 111.4(3) . . ? C89 N10 C81 107.2(3) . . ? C93 N10 C81 110.7(4) . . ? C89 N10 C85 110.6(4) . . ? C93 N10 C85 106.6(4) . . ? C81 N10 C85 110.4(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 N1 C1 C2 C3 -177.8(5) . . . . ? C6 C1 C2 C3 1.7(7) . . . . ? C1 C2 C3 C4 1.3(7) . . . . ? C2 C3 C4 C5 -2.7(8) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? N1 C1 C6 C5 176.1(4) . . . . ? C2 C1 C6 C5 -3.5(7) . . . . ? N1 C1 C6 C7 -3.2(5) . . . . ? C2 C1 C6 C7 177.2(4) . . . . ? C4 C5 C6 C1 2.1(7) . . . . ? C4 C5 C6 C7 -178.8(5) . . . . ? C1 C6 C7 C8 -174.2(5) . . . . ? C5 C6 C7 C8 6.6(9) . . . . ? C1 C6 C7 C12 2.8(5) . . . . ? C5 C6 C7 C12 -176.4(5) . . . . ? C12 C7 C8 C9 0.5(6) . . . . ? C6 C7 C8 C9 177.1(5) . . . . ? C7 C8 C9 C10 2.6(7) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C9 C10 C11 C12 -3.8(6) . . . . ? C9 C10 C11 N2 176.7(4) . . . . ? C10 C11 C12 N1 -174.8(4) . . . . ? N2 C11 C12 N1 4.7(7) . . . . ? C10 C11 C12 C7 6.8(6) . . . . ? N2 C11 C12 C7 -173.7(4) . . . . ? C8 C7 C12 N1 176.0(4) . . . . ? C6 C7 C12 N1 -1.5(5) . . . . ? C8 C7 C12 C11 -5.3(6) . . . . ? C6 C7 C12 C11 177.2(4) . . . . ? N4 C14 C15 C16 -175.9(4) . . . . ? C19 C14 C15 C16 1.0(6) . . . . ? N4 C14 C15 N3 1.4(7) . . . . ? C19 C14 C15 N3 178.2(4) . . . . ? C14 C15 C16 C17 -1.5(6) . . . . ? N3 C15 C16 C17 -178.6(4) . . . . ? C15 C16 C17 C18 1.5(7) . . . . ? C16 C17 C18 C19 -0.8(7) . . . . ? N4 C14 C19 C18 177.0(4) . . . . ? C15 C14 C19 C18 -0.3(6) . . . . ? N4 C14 C19 C20 2.0(5) . . . . ? C15 C14 C19 C20 -175.4(4) . . . . ? C17 C18 C19 C14 0.2(7) . . . . ? C17 C18 C19 C20 173.6(5) . . . . ? C14 C19 C20 C21 178.5(5) . . . . ? C18 C19 C20 C21 4.5(9) . . . . ? C14 C19 C20 C25 -0.8(5) . . . . ? C18 C19 C20 C25 -174.9(5) . . . . ? C25 C20 C21 C22 1.9(7) . . . . ? C19 C20 C21 C22 -177.4(5) . . . . ? C20 C21 C22 C23 -1.2(8) . . . . ? C21 C22 C23 C24 0.2(8) . . . . ? C22 C23 C24 C25 0.0(7) . . . . ? C23 C24 C25 N4 178.8(4) . . . . ? C23 C24 C25 C20 0.8(7) . . . . ? C21 C20 C25 N4 179.9(4) . . . . ? C19 C20 C25 N4 -0.6(5) . . . . ? C21 C20 C25 C24 -1.8(7) . . . . ? C19 C20 C25 C24 177.7(4) . . . . ? O4 C26 C27 C28 14.3(6) . . . . ? O3 C26 C27 C28 -166.2(4) . . . . ? O4 C26 C27 C32 -165.4(4) . . . . ? O3 C26 C27 C32 14.0(6) . . . . ? C32 C27 C28 C29 -0.3(7) . . . . ? C26 C27 C28 C29 179.9(4) . . . . ? C27 C28 C29 C30 0.2(7) . . . . ? C28 C29 C30 C31 0.6(8) . . . . ? C29 C30 C31 C32 -1.4(8) . . . . ? C28 C27 C32 C31 -0.5(7) . . . . ? C26 C27 C32 C31 179.3(4) . . . . ? C30 C31 C32 C27 1.3(7) . . . . ? N8 C33 C34 C35 -177.8(4) . . . . ? C38 C33 C34 C35 0.5(7) . . . . ? C33 C34 C35 C36 0.0(7) . . . . ? C34 C35 C36 C37 -0.5(8) . . . . ? C35 C36 C37 C38 0.4(7) . . . . ? C36 C37 C38 C33 0.1(7) . . . . ? C36 C37 C38 C39 175.9(5) . . . . ? N8 C33 C38 C37 178.1(4) . . . . ? C34 C33 C38 C37 -0.6(7) . . . . ? N8 C33 C38 C39 1.2(5) . . . . ? C34 C33 C38 C39 -177.5(4) . . . . ? C37 C38 C39 C44 -175.6(5) . . . . ? C33 C38 C39 C44 0.7(5) . . . . ? C37 C38 C39 C40 -0.2(9) . . . . ? C33 C38 C39 C40 176.0(5) . . . . ? C44 C39 C40 C41 1.8(6) . . . . ? C38 C39 C40 C41 -173.1(4) . . . . ? C39 C40 C41 C42 0.6(6) . . . . ? C40 C41 C42 C43 -2.0(6) . . . . ? C41 C42 C43 C44 1.1(6) . . . . ? C41 C42 C43 N7 177.4(4) . . . . ? C40 C39 C44 N8 -178.4(4) . . . . ? C38 C39 C44 N8 -2.3(5) . . . . ? C40 C39 C44 C43 -2.7(6) . . . . ? C38 C39 C44 C43 173.4(4) . . . . ? C42 C43 C44 N8 176.0(4) . . . . ? N7 C43 C44 N8 -0.6(7) . . . . ? C42 C43 C44 C39 1.3(6) . . . . ? N7 C43 C44 C39 -175.4(4) . . . . ? N5 C46 C47 C48 177.5(4) . . . . ? C51 C46 C47 C48 -4.7(6) . . . . ? N5 C46 C47 N6 -2.8(7) . . . . ? C51 C46 C47 N6 175.1(4) . . . . ? C46 C47 C48 C49 2.6(6) . . . . ? N6 C47 C48 C49 -177.1(4) . . . . ? C47 C48 C49 C50 0.8(7) . . . . ? C48 C49 C50 C51 -2.1(7) . . . . ? C49 C50 C51 C46 0.0(7) . . . . ? C49 C50 C51 C52 -179.8(5) . . . . ? N5 C46 C51 C50 -178.3(4) . . . . ? C47 C46 C51 C50 3.4(7) . . . . ? N5 C46 C51 C52 1.5(5) . . . . ? C47 C46 C51 C52 -176.7(4) . . . . ? C50 C51 C52 C57 177.1(5) . . . . ? C46 C51 C52 C57 -2.7(5) . . . . ? C50 C51 C52 C53 -2.9(9) . . . . ? C46 C51 C52 C53 177.3(5) . . . . ? C57 C52 C53 C54 -0.7(8) . . . . ? C51 C52 C53 C54 179.4(5) . . . . ? C52 C53 C54 C55 -1.6(9) . . . . ? C53 C54 C55 C56 2.6(10) . . . . ? C54 C55 C56 C57 -1.1(10) . . . . ? C55 C56 C57 N5 177.8(5) . . . . ? C55 C56 C57 C52 -1.2(8) . . . . ? C53 C52 C57 C56 2.1(8) . . . . ? C51 C52 C57 C56 -177.9(5) . . . . ? C53 C52 C57 N5 -177.1(4) . . . . ? C51 C52 C57 N5 2.9(5) . . . . ? O6 C58 C59 C64 176.5(5) . . . . ? O5 C58 C59 C64 -4.2(7) . . . . ? O6 C58 C59 C60 -4.2(7) . . . . ? O5 C58 C59 C60 175.1(5) . . . . ? C64 C59 C60 C61 -1.1(8) . . . . ? C58 C59 C60 C61 179.5(5) . . . . ? C59 C60 C61 C62 1.4(9) . . . . ? C60 C61 C62 C63 -0.2(10) . . . . ? C61 C62 C63 C64 -1.3(11) . . . . ? C60 C59 C64 C63 -0.3(9) . . . . ? C58 C59 C64 C63 179.0(6) . . . . ? C62 C63 C64 C59 1.5(11) . . . . ? N9 C65 C66 C67 -171.1(4) . . . . ? C65 C66 C67 C68 67.3(6) . . . . ? N9 C69 C70 C71 177.0(4) . . . . ? C69 C70 C71 C72 66.8(6) . . . . ? N9 C73 C74 C75 -166.2(4) . . . . ? C73 C74 C75 C76 -75.0(6) . . . . ? N9 C77 C78 C79 168.5(4) . . . . ? C77 C78 C79 C80 165.0(4) . . . . ? N10 C81 C82 C83 174.1(4) . . . . ? C81 C82 C83 C84 -85.2(6) . . . . ? N10 C85 C86 C87 169.4(5) . . . . ? C85 C86 C87 C88 53.3(10) . . . . ? N10 C89 C90 C91 -175.3(4) . . . . ? C89 C90 C91 C92 -176.8(4) . . . . ? N10 C93 C94 C95 -178.2(4) . . . . ? C93 C94 C95 C96 -173.3(5) . . . . ? C11 C12 N1 C1 -179.0(4) . . . . ? C7 C12 N1 C1 -0.5(5) . . . . ? C2 C1 N1 C12 -178.1(5) . . . . ? C6 C1 N1 C12 2.3(5) . . . . ? O1 C13 N2 C11 -1.0(7) . . . . ? N3 C13 N2 C11 179.0(4) . . . . ? C10 C11 N2 C13 -37.6(6) . . . . ? C12 C11 N2 C13 142.9(4) . . . . ? O1 C13 N3 C15 -11.8(7) . . . . ? N2 C13 N3 C15 168.1(4) . . . . ? C16 C15 N3 C13 -3.0(7) . . . . ? C14 C15 N3 C13 180.0(4) . . . . ? C19 C14 N4 C25 -2.4(5) . . . . ? C15 C14 N4 C25 174.7(4) . . . . ? C24 C25 N4 C14 -176.3(4) . . . . ? C20 C25 N4 C14 1.9(5) . . . . ? C47 C46 N5 C57 178.2(5) . . . . ? C51 C46 N5 C57 0.2(5) . . . . ? C56 C57 N5 C46 178.9(5) . . . . ? C52 C57 N5 C46 -1.9(5) . . . . ? O2 C45 N6 C47 -5.5(7) . . . . ? N7 C45 N6 C47 173.6(4) . . . . ? C48 C47 N6 C45 42.6(7) . . . . ? C46 C47 N6 C45 -137.1(4) . . . . ? O2 C45 N7 C43 7.0(7) . . . . ? N6 C45 N7 C43 -172.1(4) . . . . ? C42 C43 N7 C45 5.8(7) . . . . ? C44 C43 N7 C45 -177.8(4) . . . . ? C39 C44 N8 C33 3.1(5) . . . . ? C43 C44 N8 C33 -172.2(4) . . . . ? C34 C33 N8 C44 175.9(5) . . . . ? C38 C33 N8 C44 -2.6(5) . . . . ? C66 C65 N9 C69 57.4(5) . . . . ? C66 C65 N9 C77 -61.4(5) . . . . ? C66 C65 N9 C73 179.2(4) . . . . ? C70 C69 N9 C65 53.8(5) . . . . ? C70 C69 N9 C77 174.3(4) . . . . ? C70 C69 N9 C73 -65.9(5) . . . . ? C78 C77 N9 C65 -68.4(5) . . . . ? C78 C77 N9 C69 169.8(4) . . . . ? C78 C77 N9 C73 49.5(5) . . . . ? C74 C73 N9 C65 177.5(4) . . . . ? C74 C73 N9 C69 -60.0(5) . . . . ? C74 C73 N9 C77 58.0(5) . . . . ? C90 C89 N10 C93 68.6(5) . . . . ? C90 C89 N10 C81 -170.2(4) . . . . ? C90 C89 N10 C85 -49.7(5) . . . . ? C94 C93 N10 C89 70.2(5) . . . . ? C94 C93 N10 C81 -49.1(5) . . . . ? C94 C93 N10 C85 -169.1(4) . . . . ? C82 C81 N10 C89 178.3(4) . . . . ? C82 C81 N10 C93 -60.0(5) . . . . ? C82 C81 N10 C85 57.7(5) . . . . ? C86 C85 N10 C89 -57.2(5) . . . . ? C86 C85 N10 C93 -178.4(4) . . . . ? C86 C85 N10 C81 61.3(5) . . . . ? 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 N1 H901 O4 0.86 2.00 2.809(5) 157.3 . N2 H902 O4 0.86 2.02 2.816(5) 152.9 . N3 H903 O3 0.86 2.06 2.917(5) 178.6 . N4 H904 O3 0.86 1.96 2.801(4) 165.4 . N5 H905 O6 0.86 1.98 2.773(5) 153.0 . N6 H906 O6 0.86 2.00 2.762(5) 147.7 . N7 H907 O5 0.86 2.14 2.996(5) 174.9 . N8 H908 O5 0.86 1.96 2.806(5) 167.0 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.527 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.060