#------------------------------------------------------------------------------ #$Date: 2020-10-25 02:04:22 +0300 (Sun, 25 Oct 2020) $ #$Revision: 258596 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/94/1559409.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1559409 loop_ _publ_author_name 'Zhang, Wei-Yang' 'Zhong, Yue' 'Yu, Yang' 'Shi, Dan-Feng' 'Huang, Hui-Yun' 'Tang, Xiao-Long' 'Wang, Yong-Heng' 'Chen, Guo-Dong' 'Zhang, Hui-Ping' 'Liu, Chen-Li' 'Hu, Dan' 'Gao, Hao' 'Yao, Xin-Sheng' _publ_section_title ; 4-Hydroxy Pyridones from Heterologous Expression and Cultivation of the Native Host. ; _journal_name_full 'Journal of natural products' _journal_paper_doi 10.1021/acs.jnatprod.0c00675 _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_moiety 'C21 H25 N O4' _chemical_formula_sum 'C21 H25 N O4' _chemical_formula_weight 355.42 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-01-08 _audit_creation_method ; Olex2 1.3-alpha (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _cell_angle_alpha 90 _cell_angle_beta 92.297(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.8720(7) _cell_length_b 7.8414(5) _cell_length_c 35.3848(17) _cell_measurement_reflns_used 2333 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 54.0690 _cell_measurement_theta_min 2.4650 _cell_volume 4123.2(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -53.00 33.00 1.00 2.00 -- -41.23 38.00-120.00 86 2 \w 34.00 92.00 1.00 2.00 -- 41.23-125.00 -60.00 58 3 \w 104.00 132.00 1.00 3.50 -- 106.95 -61.00 60.00 28 4 \w 77.00 105.00 1.00 3.50 -- 106.95-125.00 30.00 28 5 \w 46.00 75.00 1.00 3.50 -- 106.95-125.00 30.00 29 6 \w 35.00 99.00 1.00 3.50 -- 106.95 -45.00 60.00 64 7 \w 35.00 135.00 1.00 3.50 -- 106.95 -30.00-150.00 100 8 \w 78.00 178.00 1.00 3.50 -- 106.95 61.00-150.00 100 9 \w 100.00 178.00 1.00 3.50 -- 106.95 125.00 150.00 78 10 \w -113.00 -14.00 1.00 2.00 -- -41.23 -57.00 90.00 99 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0726901000 _diffrn_orient_matrix_UB_12 -0.0690696000 _diffrn_orient_matrix_UB_13 -0.0257737000 _diffrn_orient_matrix_UB_21 0.0730065000 _diffrn_orient_matrix_UB_22 0.0405014000 _diffrn_orient_matrix_UB_23 0.0308123000 _diffrn_orient_matrix_UB_31 -0.0115098000 _diffrn_orient_matrix_UB_32 -0.1793959000 _diffrn_orient_matrix_UB_33 0.0168928000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_unetI/netI 0.0752 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 16490 _diffrn_reflns_point_group_measured_fraction_full 0.694 _diffrn_reflns_point_group_measured_fraction_max 0.662 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.068 _diffrn_reflns_theta_min 2.499 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.145 _exptl_crystal_description block _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.215 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_extinction_coef 0.00024(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 940 _refine_ls_number_reflns 11071 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0667 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1580 _refine_ls_wR_factor_ref 0.1912 _reflns_Friedel_coverage 0.272 _reflns_Friedel_fraction_full 0.337 _reflns_Friedel_fraction_max 0.307 _reflns_number_gt 6460 _reflns_number_total 11071 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np0c00675_si_002.cif _cod_data_source_block 3g6 _cod_database_code 1559409 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Rigid bond restraints C33, C34 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C34, C35 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C71, C72 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints C33 \\sim C34: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A C34 \\sim C35: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A C71 \\sim C72: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A Uanis(C22) = Uanis(C74) Uanis(C68) = Uanis(C69) Uanis(C70) = Uanis(C71) 4.a Ternary CH refined with riding coordinates: C23(H23), C4(H4A), C26(H26), C39(H39), C6(H6), C65(H65), C36(H36), C68(H68) 4.b Secondary CH2 refined with riding coordinates: C5(H5A,H5B), C40(H40A,H40B), C24(H24A,H24B), C70(H70A,H70B), C67(H67A,H67B), C28(H28A,H28B), C7(H7A,H7B), C35(H35A,H35B) 4.c Aromatic/amide H refined with riding coordinates: N2(H2), N1(H1), N3(H3A), N4(H4B), C20(H20), C45(H45), C60(H60), C49(H49), C48(H48), C5'(H5'), C9'(H9'), C54(H54), C51(H51), C58(H58), C52(H52), C6'(H6'), C2'(H2'), C14(H14), C15(H15), C57(H57), C8'(H8'), C55(H55), C18(H18), C8(H8), C17(H17), C29(H29), C71(H71), C9(H9), C72(H72), C34(H34), C30(H30), C33(H33) 4.d Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C38(H38A,H38B, H38C), C10(H10A,H10B,H10C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C73(H73A, H73B,H73C), C69(H69A,H69B,H69C), C66(H66A,H66B,H66C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C) 4.e Idealised tetrahedral OH refined as rotating group: O7(H7), O13(H13), O3(H3), O16(H16), O12(H12), O15(H15A), O6(H6A), O4(H4) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 3g6_a.res in P2(1) 3g6.res created by SHELXL-2018/3 at 13:17:56 on 08-Jan-2020 REM Old TITL 3G6 in P2(1)/m REM SHELXT solution in P2(1): R1 0.217, Rweak 0.065, Alpha 0.009 REM 0.374 for 5 systematic absences, Orientation as input REM Flack x = 0.050 ( 0.248 ) from 1255 Parsons' quotients REM Formula found by SHELXT: C85 O21 CELL 1.54184 14.872 7.8414 35.3848 90 92.297 90 ZERR 8 0.0007 0.0005 0.0017 0 0.004 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 168 200 8 32 SIMU 0.002 0.004 2 C33 C34 DELU C33 C34 SIMU 0.002 0.004 2 C34 C35 DELU C34 C35 SIMU 0.002 0.004 2 C71 C72 DELU C71 C72 EADP C22 C74 EADP C68 C69 EADP C70 C71 L.S. 20 PLAN 10 CONF BOND list 4 MORE -1 BOND $H ABIN fmap 2 53 acta OMIT 0 -1 3 OMIT 7 0 2 REM REM REM WGHT 0.072000 EXTI 0.000238 FVAR 0.33003 O1 4 0.528917 0.369814 0.638389 11.00000 0.06273 0.08217 = 0.05867 -0.01925 0.00706 -0.00326 O7 4 -0.150366 1.253656 0.976031 11.00000 0.05686 0.10722 = 0.05285 0.01990 0.00167 0.00493 AFIX 147 H7 2 -0.198009 1.302917 0.979417 11.00000 -1.50000 AFIX 0 O13 4 0.672428 0.266755 0.377995 11.00000 0.07090 0.10489 = 0.06440 0.01065 0.02638 -0.00206 AFIX 147 H13 2 0.662994 0.357207 0.366903 11.00000 -1.50000 AFIX 0 O2 4 0.655239 0.715808 0.713406 11.00000 0.05707 0.09760 = 0.08483 -0.02622 -0.00388 -0.00766 O3 4 0.510905 0.731738 0.745024 11.00000 0.06157 0.09341 = 0.07347 -0.02804 -0.00049 -0.00819 AFIX 147 H3 2 0.561109 0.761881 0.738949 11.00000 -1.50000 AFIX 0 O18 4 1.022121 0.969313 0.146772 11.00000 0.05430 0.12901 = 0.05772 0.02699 0.00747 0.00618 N2 3 -0.049586 1.056024 1.073865 11.00000 0.06064 0.08201 = 0.04864 0.01209 0.00235 0.01841 AFIX 43 H2 2 -0.024155 1.020451 1.094652 11.00000 -1.20000 AFIX 0 N1 3 0.397073 0.427455 0.664409 11.00000 0.05198 0.07281 = 0.05447 -0.01129 0.00212 -0.01039 AFIX 43 H1 2 0.369870 0.366233 0.647333 11.00000 -1.20000 AFIX 0 O10 4 0.318944 0.228338 0.603164 11.00000 0.07324 0.10594 = 0.04586 -0.00694 0.01403 -0.01967 O8 4 -0.176384 1.091447 1.104732 11.00000 0.06548 0.13061 = 0.05364 0.02419 0.01176 0.01605 O16 4 0.984093 0.651235 0.259540 11.00000 0.07293 0.14564 = 0.07944 0.05264 0.01276 0.03416 AFIX 147 H16 2 1.038244 0.634360 0.258030 11.00000 -1.50000 AFIX 0 O12 4 0.332137 0.107549 0.471329 11.00000 0.08239 0.12726 = 0.04947 -0.01611 0.01054 -0.03130 AFIX 147 H12 2 0.277583 0.095386 0.472619 11.00000 -1.50000 AFIX 0 N3 3 0.445052 0.264429 0.570877 11.00000 0.06041 0.07823 = 0.04470 -0.00224 0.00470 -0.01066 AFIX 43 H3A 2 0.472053 0.295298 0.591711 11.00000 -1.20000 AFIX 0 O15 4 0.607353 0.496996 0.325345 11.00000 0.08354 0.10161 = 0.07911 0.02606 0.02699 0.01126 AFIX 147 H15A 2 0.562656 0.557988 0.326007 11.00000 -1.50000 AFIX 0 O9 4 -0.291997 1.312364 1.005912 11.00000 0.06002 0.12408 = 0.06909 0.03041 0.00083 0.01217 O6 4 0.202568 1.079485 0.887553 11.00000 0.08229 0.13185 = 0.07944 -0.03087 0.03745 -0.01681 AFIX 147 H6A 2 0.188660 0.998973 0.873733 11.00000 -1.50000 AFIX 0 O11 4 0.192521 0.039885 0.502481 11.00000 0.08081 0.16202 = 0.06772 -0.01664 0.00845 -0.04522 C50 1 0.618237 0.255233 0.407605 11.00000 0.05508 0.05799 = 0.05222 -0.00083 0.01479 -0.01142 O4 4 0.151106 0.865300 0.828664 11.00000 0.10005 0.12136 = 0.08740 -0.03580 0.03795 -0.01166 AFIX 147 H4 2 0.135603 0.793059 0.843842 11.00000 -1.50000 AFIX 0 C44 1 0.456381 0.219787 0.504706 11.00000 0.05410 0.05532 = 0.04785 -0.00107 0.00660 0.00065 N4 3 0.886254 0.913246 0.168896 11.00000 0.05917 0.10549 = 0.04792 0.02208 0.00599 0.01827 AFIX 43 H4B 2 0.862702 0.963109 0.149244 11.00000 -1.20000 AFIX 0 C3 1 0.621172 0.627836 0.687159 11.00000 0.05155 0.05967 = 0.07297 0.00228 -0.00043 -0.00202 C2 1 0.527437 0.569329 0.689134 11.00000 0.05519 0.05185 = 0.05123 -0.00011 0.00543 -0.00278 C20 1 0.000336 1.058961 1.042811 11.00000 0.04822 0.07908 = 0.05246 0.00913 0.00877 0.00824 AFIX 43 H20 2 0.058768 1.016749 1.044845 11.00000 -1.20000 AFIX 0 C61 1 0.977123 0.902978 0.172265 11.00000 0.06064 0.08438 = 0.04786 0.01816 0.00796 0.01269 C75 1 -0.120019 1.182885 1.008526 11.00000 0.05113 0.06400 = 0.04845 0.00581 -0.00256 0.00147 C19 1 -0.030149 1.120071 1.008884 11.00000 0.04689 0.06628 = 0.04957 -0.00030 0.00486 -0.00196 C1' 1 0.475084 0.631536 0.718667 11.00000 0.06447 0.05809 = 0.04878 -0.00461 0.00021 -0.00026 C46 1 0.357760 0.215419 0.572297 11.00000 0.06206 0.06013 = 0.04624 -0.00356 0.00230 -0.00368 C1 1 0.488316 0.450847 0.662202 11.00000 0.05580 0.06406 = 0.04866 -0.00719 0.00765 0.00428 C4' 1 0.322643 0.664293 0.749422 11.00000 0.06227 0.05996 = 0.05401 -0.00501 0.01287 -0.00641 C47 1 0.510581 0.228138 0.470748 11.00000 0.05827 0.05582 = 0.04472 0.00255 0.00671 -0.00764 C45 1 0.492647 0.268361 0.539240 11.00000 0.05630 0.06275 = 0.04751 -0.00249 0.01119 -0.00510 AFIX 43 H45 2 0.552096 0.305298 0.540926 11.00000 -1.20000 AFIX 0 C60 1 0.830584 0.849879 0.194545 11.00000 0.05050 0.07467 = 0.05398 0.01453 0.01161 0.01162 AFIX 43 H60 2 0.769037 0.865393 0.190211 11.00000 -1.20000 AFIX 0 C49 1 0.531416 0.316406 0.406123 11.00000 0.06821 0.09152 = 0.04184 0.00647 0.00529 -0.00586 AFIX 43 H49 2 0.508331 0.367265 0.384061 11.00000 -1.20000 AFIX 0 O17 4 1.137054 0.720075 0.242344 11.00000 0.06728 0.21093 = 0.08887 0.05926 -0.00230 0.03751 C48 1 0.477974 0.302843 0.437292 11.00000 0.05695 0.09004 = 0.05402 0.00484 0.00569 -0.00100 AFIX 43 H48 2 0.419381 0.344441 0.435759 11.00000 -1.20000 AFIX 0 C53 1 0.666478 0.565454 0.301321 11.00000 0.07068 0.07021 = 0.06163 0.01856 0.02134 0.00390 C16 1 0.027010 1.118366 0.975838 11.00000 0.05147 0.06437 = 0.04850 0.00087 0.00702 0.00020 C21 1 -0.137705 1.105579 1.074622 11.00000 0.05705 0.07525 = 0.04518 0.00786 0.00976 0.01342 C42 1 0.315501 0.154116 0.537230 11.00000 0.06517 0.05550 = 0.04646 -0.00634 0.00992 -0.01100 C22 1 -0.267887 1.238437 1.035662 11.00000 0.05562 0.06774 = 0.05277 0.00838 0.00571 0.00194 C5' 1 0.235208 0.716033 0.739114 11.00000 0.05450 0.06914 = 0.06800 -0.00756 0.00424 -0.00910 AFIX 43 H5' 2 0.215175 0.709097 0.713925 11.00000 -1.20000 AFIX 0 C43 1 0.366529 0.162590 0.504580 11.00000 0.05943 0.06999 = 0.05141 -0.00632 0.00298 -0.00476 C9' 1 0.350178 0.678580 0.787481 11.00000 0.05977 0.10255 = 0.05377 -0.00651 0.00583 -0.00087 AFIX 43 H9' 2 0.408013 0.645407 0.795298 11.00000 -1.20000 AFIX 0 C74 1 -0.175083 1.173659 1.039462 11.00000 0.05562 0.06774 = 0.05277 0.00838 0.00571 0.00194 C59 1 0.858640 0.764653 0.226379 11.00000 0.06690 0.05955 = 0.04965 0.00832 0.00807 0.01439 C54 1 0.643564 0.591324 0.263299 11.00000 0.06856 0.08352 = 0.06685 0.00519 0.00029 -0.00602 AFIX 43 H54 2 0.585848 0.566121 0.253836 11.00000 -1.20000 AFIX 0 C23 1 -0.337044 1.201651 1.063899 11.00000 0.05221 0.08071 = 0.06301 -0.00833 0.00930 0.01135 AFIX 13 H23 2 -0.307510 1.185784 1.088908 11.00000 -1.20000 AFIX 0 C3' 1 0.381915 0.595709 0.720617 11.00000 0.05553 0.05953 = 0.05622 -0.00430 0.00858 -0.00495 C51 1 0.651492 0.179925 0.440624 11.00000 0.05811 0.06102 = 0.06799 0.00690 0.00703 0.00472 AFIX 43 H51 2 0.710096 0.138361 0.442080 11.00000 -1.20000 AFIX 0 C56 1 0.793207 0.698185 0.252524 11.00000 0.06491 0.05960 = 0.04588 0.00752 0.00701 0.01988 C63 1 0.954471 0.743607 0.230205 11.00000 0.06309 0.09009 = 0.04763 0.01351 0.00304 0.01091 C4 1 0.677473 0.592168 0.653035 11.00000 0.05103 0.05940 = 0.07629 0.00237 0.00938 -0.00463 AFIX 13 H4A 2 0.637148 0.564137 0.631340 11.00000 -1.20000 AFIX 0 C58 1 0.750696 0.608509 0.314956 11.00000 0.07678 0.08829 = 0.04645 0.01648 0.01118 0.02525 AFIX 43 H58 2 0.765961 0.592981 0.340469 11.00000 -1.20000 AFIX 0 C52 1 0.597943 0.166353 0.471378 11.00000 0.05971 0.07114 = 0.05463 0.00895 0.00089 -0.00384 AFIX 43 H52 2 0.621166 0.114073 0.493250 11.00000 -1.20000 AFIX 0 C6' 1 0.178101 0.777289 0.765741 11.00000 0.05608 0.06745 = 0.08792 -0.01064 0.02022 -0.00415 AFIX 43 H6' 2 0.119870 0.810011 0.758424 11.00000 -1.20000 AFIX 0 C2' 1 0.348101 0.494827 0.691721 11.00000 0.05022 0.06960 = 0.05602 -0.01202 0.00913 -0.00789 AFIX 43 H2' 2 0.286750 0.471446 0.691018 11.00000 -1.20000 AFIX 0 C5 1 0.736344 0.435661 0.662918 11.00000 0.05137 0.06678 = 0.07246 0.00066 0.00195 0.00399 AFIX 23 H5A 2 0.776120 0.465565 0.684289 11.00000 -1.20000 H5B 2 0.697172 0.345313 0.671202 11.00000 -1.20000 AFIX 0 C26 1 -0.445643 0.945785 1.076963 11.00000 0.05867 0.08975 = 0.07536 0.00573 0.00888 0.00382 AFIX 13 H26 2 -0.492440 1.027442 1.083478 11.00000 -1.20000 AFIX 0 C14 1 0.173229 1.157613 0.949775 11.00000 0.05047 0.08001 = 0.08364 -0.00938 0.01360 -0.01330 AFIX 43 H14 2 0.232522 1.194325 0.952906 11.00000 -1.20000 AFIX 0 C40 1 0.103785 -0.097439 0.560056 11.00000 0.05880 0.08185 = 0.08373 0.00001 0.01445 -0.01402 AFIX 23 H40A 2 0.141551 -0.194674 0.554723 11.00000 -1.20000 H40B 2 0.067093 -0.074588 0.537338 11.00000 -1.20000 AFIX 0 C24 1 -0.380620 1.031897 1.050562 11.00000 0.06685 0.08388 = 0.06488 0.00571 0.01178 0.00701 AFIX 23 H24A 2 -0.412670 1.052641 1.026587 11.00000 -1.20000 H24B 2 -0.332649 0.951850 1.045807 11.00000 -1.20000 AFIX 0 C62 1 1.012182 0.816187 0.205071 11.00000 0.05859 0.09778 = 0.05559 0.02386 0.00514 0.01571 C15 1 0.116358 1.169431 0.979557 11.00000 0.06313 0.07968 = 0.05560 0.00216 0.00036 -0.00614 AFIX 43 H15 2 0.138345 1.212513 1.002606 11.00000 -1.20000 AFIX 0 C39 1 0.165029 0.055876 0.567281 11.00000 0.05826 0.07911 = 0.06184 -0.00758 0.01204 -0.00990 AFIX 13 H39 2 0.203368 0.031541 0.589806 11.00000 -1.20000 AFIX 0 C41 1 0.225214 0.082209 0.534597 11.00000 0.06556 0.07289 = 0.06549 -0.01134 0.00487 -0.01351 C13 1 0.142989 1.091975 0.915473 11.00000 0.06955 0.08671 = 0.05674 -0.00128 0.01791 -0.00499 C57 1 0.813679 0.675184 0.291110 11.00000 0.06468 0.08427 = 0.04770 0.01289 0.00933 0.01371 AFIX 43 H57 2 0.870431 0.705060 0.300950 11.00000 -1.20000 AFIX 0 C8' 1 0.292570 0.741158 0.813409 11.00000 0.09732 0.09533 = 0.04915 -0.01144 0.02043 -0.01079 AFIX 43 H8' 2 0.311703 0.750849 0.838663 11.00000 -1.20000 AFIX 0 C6 1 0.793648 0.363958 0.632035 11.00000 0.05886 0.07641 = 0.08832 0.00222 0.00674 0.00544 AFIX 13 H6 2 0.828606 0.457200 0.621463 11.00000 -1.20000 AFIX 0 C55 1 0.706468 0.653994 0.239991 11.00000 0.07683 0.07689 = 0.04783 0.00825 0.00698 0.00849 AFIX 43 H55 2 0.690623 0.667867 0.214485 11.00000 -1.20000 AFIX 0 C18 1 0.054695 1.044003 0.911350 11.00000 0.06830 0.11040 = 0.05404 -0.00755 0.00240 -0.00191 AFIX 43 H18 2 0.032821 1.004673 0.887950 11.00000 -1.20000 AFIX 0 C7' 1 0.206289 0.789898 0.802254 11.00000 0.07369 0.09070 = 0.07387 -0.01358 0.03005 -0.00767 C65 1 1.179596 0.897071 0.191166 11.00000 0.06258 0.15850 = 0.05564 0.00451 0.00134 0.00183 AFIX 13 H65 2 1.152874 0.998869 0.179218 11.00000 -1.20000 AFIX 0 C8 1 0.781200 0.227246 0.566232 11.00000 0.10679 0.09750 = 0.08071 0.01567 0.01406 0.02664 AFIX 43 H8 2 0.815009 0.308895 0.554082 11.00000 -1.20000 AFIX 0 C64 1 1.111117 0.811293 0.214165 11.00000 0.07289 0.13941 = 0.05943 0.03191 0.00604 0.01789 C36 1 0.041022 -0.149410 0.591093 11.00000 0.05917 0.09306 = 0.09597 0.01605 0.00533 -0.01204 AFIX 13 H36 2 0.000831 -0.053442 0.595882 11.00000 -1.20000 AFIX 0 C17 1 -0.002635 1.052326 0.940856 11.00000 0.06421 0.08793 = 0.05372 -0.00713 0.00409 -0.00734 AFIX 43 H17 2 -0.061538 1.013713 0.937488 11.00000 -1.20000 AFIX 0 C70 1 1.215046 0.983444 0.107562 11.00000 0.08905 0.14861 = 0.09468 0.04046 0.01545 -0.00428 AFIX 23 H70A 2 1.161870 0.934342 0.095074 11.00000 -1.20000 H70B 2 1.194695 1.068096 0.125289 11.00000 -1.20000 AFIX 0 C68 1 1.262828 0.843863 0.129951 11.00000 0.06711 0.19145 = 0.07242 -0.00217 0.00778 0.02725 AFIX 13 H68 2 1.317881 0.890527 0.142085 11.00000 -1.20000 AFIX 0 C29 1 -0.453576 0.805725 1.141144 11.00000 0.08149 0.13629 = 0.08182 0.02443 0.01001 0.00013 AFIX 43 H29 2 -0.492092 0.879885 1.153107 11.00000 -1.20000 AFIX 0 C27 1 -0.489934 0.793373 1.055348 11.00000 0.09272 0.11644 = 0.10792 0.02676 -0.00494 -0.02794 AFIX 137 H27A 2 -0.527130 0.835361 1.034585 11.00000 -1.50000 H27B 2 -0.526162 0.729551 1.072189 11.00000 -1.50000 H27C 2 -0.443918 0.720893 1.045895 11.00000 -1.50000 AFIX 0 C12 1 0.732903 0.748926 0.643350 11.00000 0.09604 0.07223 = 0.12261 0.01255 0.02923 -0.01489 AFIX 137 H12A 2 0.693246 0.841843 0.636790 11.00000 -1.50000 H12B 2 0.769489 0.723313 0.622338 11.00000 -1.50000 H12C 2 0.770830 0.780197 0.664829 11.00000 -1.50000 AFIX 0 C67 1 1.203312 0.769596 0.160590 11.00000 0.06550 0.15025 = 0.06188 0.01026 0.00386 0.00425 AFIX 23 H67A 2 1.148033 0.727033 0.148542 11.00000 -1.20000 H67B 2 1.234332 0.673547 0.172458 11.00000 -1.20000 AFIX 0 C71 1 1.267532 1.073796 0.078195 11.00000 0.08905 0.14861 = 0.09468 0.04046 0.01545 -0.00428 AFIX 43 H71 2 1.296904 1.001395 0.061921 11.00000 -1.20000 AFIX 0 C9 1 0.781654 0.073227 0.552168 11.00000 0.10010 0.10080 = 0.08532 -0.01425 0.00168 0.02641 AFIX 43 H9 2 0.748908 -0.011354 0.563878 11.00000 -1.20000 AFIX 0 C28 1 -0.397307 0.881387 1.113592 11.00000 0.07540 0.10655 = 0.08122 0.01111 0.00622 -0.01018 AFIX 23 H28A 2 -0.352618 0.797926 1.106782 11.00000 -1.20000 H28B 2 -0.365443 0.976624 1.125398 11.00000 -1.20000 AFIX 0 C72 1 1.278203 1.220637 0.072056 11.00000 0.09256 0.14752 = 0.09857 0.03826 0.01316 -0.00562 AFIX 43 H72 2 1.250293 1.292119 0.088977 11.00000 -1.20000 AFIX 0 C7 1 0.732035 0.285375 0.599751 11.00000 0.07644 0.11706 = 0.07659 -0.01687 0.00225 0.01230 AFIX 23 H7A 2 0.699893 0.189051 0.609869 11.00000 -1.20000 H7B 2 0.687730 0.369799 0.591571 11.00000 -1.20000 AFIX 0 C11 1 0.857272 0.230484 0.646976 11.00000 0.10938 0.15244 = 0.11418 -0.04781 -0.03716 0.05819 AFIX 137 H11A 2 0.892891 0.276084 0.667829 11.00000 -1.50000 H11B 2 0.896031 0.195682 0.627340 11.00000 -1.50000 H11C 2 0.823793 0.133883 0.655362 11.00000 -1.50000 AFIX 0 C34 1 0.033904 -0.222182 0.661191 11.00000 0.09516 0.23451 = 0.11039 0.06069 -0.01965 -0.07904 AFIX 43 H34 2 0.000438 -0.125087 0.666130 11.00000 -1.20000 AFIX 0 C38 1 0.114621 0.219005 0.574340 11.00000 0.11234 0.08089 = 0.12809 0.00122 0.04298 0.00345 AFIX 137 H38A 2 0.076988 0.246304 0.552500 11.00000 -1.50000 H38B 2 0.156793 0.309870 0.579166 11.00000 -1.50000 H38C 2 0.078002 0.204653 0.595847 11.00000 -1.50000 AFIX 0 C35 1 0.091717 -0.196822 0.628761 11.00000 0.09111 0.23277 = 0.10700 0.06065 -0.01782 -0.07967 AFIX 23 H35A 2 0.125511 -0.300759 0.624909 11.00000 -1.20000 H35B 2 0.134681 -0.107180 0.635080 11.00000 -1.20000 AFIX 0 C10 1 0.832931 0.026853 0.517814 11.00000 0.13493 0.14787 = 0.08801 -0.01460 0.01544 0.05707 AFIX 137 H10A 2 0.797728 -0.050466 0.502258 11.00000 -1.50000 H10B 2 0.888682 -0.026709 0.525609 11.00000 -1.50000 H10C 2 0.845087 0.128158 0.503666 11.00000 -1.50000 AFIX 0 C30 1 -0.457389 0.649459 1.151289 11.00000 0.10035 0.17663 = 0.09830 0.05334 -0.01656 -0.01232 AFIX 43 H30 2 -0.414823 0.578199 1.140967 11.00000 -1.20000 AFIX 0 C37 1 -0.017223 -0.303566 0.577668 11.00000 0.09013 0.11563 = 0.12545 0.02205 -0.01591 -0.03878 AFIX 137 H37A 2 -0.042294 -0.281579 0.552721 11.00000 -1.50000 H37B 2 -0.064999 -0.320467 0.594737 11.00000 -1.50000 H37C 2 0.019562 -0.404095 0.577233 11.00000 -1.50000 AFIX 0 C25 1 -0.405469 1.343412 1.065708 11.00000 0.08300 0.09498 = 0.10686 -0.01245 0.01628 0.02045 AFIX 137 H25A 2 -0.375201 1.449193 1.071216 11.00000 -1.50000 H25B 2 -0.446583 1.318982 1.085230 11.00000 -1.50000 H25C 2 -0.438120 1.352178 1.041828 11.00000 -1.50000 AFIX 0 C73 1 1.328026 1.314400 0.042271 11.00000 0.11211 0.17318 = 0.11806 0.02788 0.01315 -0.02727 AFIX 137 H73A 2 1.289387 1.399398 0.030760 11.00000 -1.50000 H73B 2 1.346209 1.235250 0.023340 11.00000 -1.50000 H73C 2 1.380277 1.368388 0.053707 11.00000 -1.50000 AFIX 0 C69 1 1.288079 0.695441 0.103618 11.00000 0.06711 0.19145 = 0.07242 -0.00217 0.00778 0.02725 AFIX 137 H69A 2 1.234279 0.646399 0.092345 11.00000 -1.50000 H69B 2 1.320450 0.610010 0.118050 11.00000 -1.50000 H69C 2 1.325183 0.737783 0.084113 11.00000 -1.50000 AFIX 0 C66 1 1.262980 0.950572 0.216637 11.00000 0.09114 0.26199 = 0.08843 -0.01712 -0.00779 -0.03945 AFIX 137 H66A 2 1.244197 1.026535 0.236081 11.00000 -1.50000 H66B 2 1.305999 1.007159 0.201475 11.00000 -1.50000 H66C 2 1.290024 0.850925 0.228022 11.00000 -1.50000 AFIX 0 C33 1 0.019318 -0.330835 0.682027 11.00000 0.09827 0.23696 = 0.11262 0.05968 -0.02439 -0.07723 AFIX 43 H33 2 0.052229 -0.428624 0.677092 11.00000 -1.20000 AFIX 0 C32 1 -0.039386 -0.353765 0.715046 11.00000 0.15108 0.30773 = 0.10473 0.05801 -0.02799 -0.12770 AFIX 137 H32A 2 -0.100645 -0.328584 0.707449 11.00000 -1.50000 H32B 2 -0.019955 -0.277950 0.735050 11.00000 -1.50000 H32C 2 -0.035202 -0.469464 0.723810 11.00000 -1.50000 AFIX 0 C31 1 -0.521628 0.562763 1.177875 11.00000 0.13495 0.31650 = 0.15483 0.14535 -0.03172 -0.05969 AFIX 137 H31A 2 -0.565144 0.497150 1.163333 11.00000 -1.50000 H31B 2 -0.551964 0.647840 1.192140 11.00000 -1.50000 H31C 2 -0.488162 0.488797 1.194866 11.00000 -1.50000 AFIX 0 HKLF 4 REM 3g6_a.res in P2(1) REM wR2 = 0.1912, GooF = S = 0.985, Restrained GooF = 0.985 for all data REM R1 = 0.0667 for 6460 Fo > 4sig(Fo) and 0.1051 for all 11071 data REM 940 parameters refined using 22 restraints END WGHT 0.0752 0.0000 REM Highest difference peak 0.215, deepest hole -0.210, 1-sigma level 0.042 Q1 1 0.4277 0.5602 0.3193 11.00000 0.05 0.21 Q2 1 0.0346 1.0007 0.9794 11.00000 0.05 0.19 Q3 1 0.8904 0.7679 0.1591 11.00000 0.05 0.17 Q4 1 0.7442 0.7427 0.3187 11.00000 0.05 0.17 Q5 1 -0.1472 1.0463 1.0212 11.00000 0.05 0.16 Q6 1 -0.0123 0.8225 0.8262 11.00000 0.05 0.16 Q7 1 -0.1735 1.0748 1.0370 11.00000 0.05 0.16 Q8 1 0.3787 0.7448 0.7226 11.00000 0.05 0.16 Q9 1 0.3753 0.3232 0.7031 11.00000 0.05 0.16 Q10 1 0.2643 -0.1544 0.5214 11.00000 0.05 0.16 ; _shelx_res_checksum 18834 _shelx_hkl_file ; 0 0 2 4.73 0.59 0 0 3 139.29 3.73 0 0 4 363.04 6.94 0 0 -4 363.55 6.76 0 0 5 34.28 2.46 0 0 -5 41.27 2.58 0 0 6 58.64 3.45 0 0 -6 62.91 3.47 0 0 7 63.21 3.88 0 0 -7 63.89 3.80 0 0 -8 1094.71 16.73 0 0 8 1105.12 17.25 0 0 -9 6.02 1.51 0 0 -10 143.95 6.97 0 0 -11 13.39 2.35 0 0 -12 510.14 14.41 0 0 -13 50.48 4.73 0 0 -14 47.66 4.87 0 0 -15 26.00 3.68 0 0 -16 67.75 6.25 0 0 -17 0.27 1.32 0 0 -18 0.86 1.11 0 0 -19 35.56 5.10 0 0 -20 -0.09 1.54 0 0 -21 6.10 2.30 0 0 -22 30.46 5.10 0 0 -23 3.65 2.46 0 0 -24 1.04 1.66 0 0 25 0.11 1.24 0 0 -25 11.18 4.48 0 0 -26 0.76 2.07 0 0 26 3.45 1.68 0 0 -27 1.57 1.78 0 0 27 -2.53 1.90 0 0 28 82.82 8.03 0 0 -28 97.01 10.93 0 0 -29 20.95 5.59 0 0 29 18.34 3.84 0 0 30 33.69 5.27 0 0 -30 35.14 6.87 0 0 31 79.58 8.23 0 0 32 25.08 4.75 0 0 33 74.61 8.10 0 0 34 6.68 2.73 0 0 35 9.80 2.92 0 0 36 4.31 2.21 0 0 37 2.42 1.55 0 0 38 -1.09 0.97 0 0 39 2.83 1.69 0 0 40 -1.65 1.21 0 0 41 -0.72 1.03 0 0 42 8.29 1.94 0 0 43 1.60 0.97 0 -1 0 0.05 0.46 0 -1 1 546.82 4.73 0 -1 -1 582.79 8.65 0 -1 -2 460.23 7.51 0 -1 -2 447.81 4.41 0 -1 -3 24.83 1.30 0 -1 3 24.70 1.68 0 -1 4 1052.25 12.13 0 -1 -4 1048.16 9.30 0 -1 4 1027.60 13.31 0 -1 5 619.75 10.87 0 -1 -5 628.57 8.35 0 -1 5 631.75 10.48 0 -1 6 286.95 7.84 0 -1 -6 283.99 6.45 0 -1 6 288.84 7.67 0 -1 7 124.70 5.53 0 -1 -7 124.85 4.65 0 -1 7 117.23 5.03 0 -1 -8 204.92 6.53 0 -1 8 198.26 6.65 0 1 -8 192.61 7.74 0 -1 8 202.75 7.54 0 -1 -9 138.72 5.75 0 1 -9 131.42 6.75 0 1 -10 865.12 18.06 0 -1 -10 886.27 15.53 0 -1 -11 26.43 2.94 0 1 -11 28.74 3.59 0 1 -12 14.65 2.72 0 -1 -12 16.93 2.42 0 -1 -13 194.84 8.57 0 1 -13 187.90 9.57 0 -1 -14 74.73 5.61 0 1 -14 74.13 6.26 0 1 -15 169.68 9.94 0 -1 -15 174.72 8.90 0 1 -16 3.60 1.72 0 -1 -16 3.35 1.50 0 -1 -17 33.91 4.35 0 1 -17 33.21 4.84 0 1 -18 16.34 3.61 0 -1 -18 14.84 2.89 0 -1 -19 11.51 2.79 0 1 -19 10.07 2.99 0 1 -20 1.69 1.56 0 -1 -20 2.41 1.57 0 -1 -21 26.36 4.45 0 1 -21 25.25 4.70 0 1 -22 16.80 4.19 0 -1 -22 15.15 3.61 0 1 -23 31.25 5.57 0 -1 -23 26.46 4.79 0 1 -24 -1.38 1.36 0 -1 -24 2.79 2.28 0 -1 -25 24.30 5.07 0 -1 25 25.81 4.51 0 1 -25 25.09 5.32 0 1 -26 -0.96 2.19 0 1 26 0.26 1.59 0 -1 -26 -2.28 2.44 0 -1 26 -1.00 1.86 0 -1 27 -0.45 1.63 0 1 27 0.78 1.41 0 -1 -27 3.83 2.19 0 1 -27 -0.49 2.23 0 -1 28 30.09 5.15 0 -1 -28 32.94 6.73 0 1 28 32.13 4.96 0 1 -28 34.13 6.70 0 1 29 21.21 4.13 0 1 -29 17.91 4.83 0 -1 -29 11.88 4.12 0 -1 29 16.28 3.94 0 -1 -30 338.99 21.05 0 -1 30 310.23 16.38 0 1 -30 347.83 22.04 0 -1 31 44.75 6.41 0 1 31 29.55 4.95 0 1 32 138.30 10.39 0 -1 32 138.68 11.11 0 1 33 34.53 5.26 0 -1 33 28.10 5.14 0 1 34 20.64 4.09 0 -1 34 24.10 4.71 0 1 35 44.75 5.78 0 -1 35 53.17 6.83 0 -1 36 2.40 2.00 0 1 36 1.46 1.06 0 -1 37 3.07 1.58 0 1 37 4.19 1.71 0 1 38 5.54 2.02 0 -1 38 7.35 2.63 0 -1 39 3.38 1.94 0 1 39 1.40 1.43 0 1 40 2.58 1.16 0 -1 40 2.16 1.37 0 1 41 -1.27 0.99 0 -1 41 0.57 0.91 0 1 42 2.18 1.02 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5.47 1.32 18 1 -11 0.78 0.69 18 1 -10 1.53 0.93 18 1 -9 15.69 2.19 18 -1 -8 0.26 0.77 18 1 -8 -0.32 0.71 18 -1 -7 3.40 1.17 18 1 -7 0.87 0.77 18 -1 -6 2.19 1.00 18 1 -6 0.40 0.64 18 -1 -5 0.33 0.81 18 1 -5 -0.57 0.87 18 -1 -4 7.16 1.51 18 1 -4 5.58 1.37 18 -1 -3 1.51 0.86 18 1 -3 -0.07 0.65 18 -1 -2 3.92 1.25 18 1 -2 2.17 1.09 18 -1 -1 1.44 0.95 18 1 -1 0.76 0.93 18 -1 0 2.94 1.21 18 1 0 1.73 0.80 18 -1 1 0.22 0.68 18 1 1 0.96 0.89 18 -1 2 0.55 0.78 18 1 2 0.89 0.71 18 -1 3 0.08 0.62 18 1 3 -1.12 0.99 18 -1 4 1.85 0.88 18 1 4 2.10 0.97 18 -1 5 0.73 0.58 18 1 5 0.27 0.60 18 -1 6 0.77 0.75 18 -1 7 1.56 0.82 0 0 0 0.00 0.00 TITL 3G6 in P2(1)/m REM P2(1)/m (#11 in standard setting) CELL 1.54184 14.871988 7.841440 35.384835 90.0000 92.2974 90.0000 ZERR 18.00 0.000717 0.000524 0.001733 0.0000 0.0043 0.0000 LATT 1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 198.00 180.00 18.00 18.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 66386 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0 9 -0.4952 0.0107 15 0 10 -0.7594 -0.0038 15 0 11 0.0376 -0.0074 15 0 12 -0.4311 -0.0014 15 0 13 0.0245 -0.0042 15 0 14 0.5270 -0.0018 15 0 15 0.0157 0.0133 15 0 16 0.0261 0.0063 15 0 17 0.0191 -0.0096 15 0 18 -0.2063 -0.0040 15 0 19 0.1248 -0.0040 15 0 20 0.0022 -0.0043 15 0 21 -0.4623 0.0133 15 0 22 -0.0545 0.0096 15 1 0 -0.2904 1.0616 15 1 1 -0.1109 0.8658 15 1 2 0.6304 -0.9070 15 1 3 -0.4908 -0.1953 15 1 4 -1.0466 0.7489 15 1 5 0.5028 -0.4075 15 1 6 0.9130 -0.3357 15 1 7 0.1304 0.4211 15 1 8 -0.0807 -0.3325 15 1 9 -0.4868 -0.1376 15 1 10 -0.6037 0.5082 15 1 11 0.1842 -0.2788 15 1 12 0.4572 -0.1233 15 1 13 0.1229 0.6440 15 1 14 -0.0465 -0.0703 15 1 15 -0.1616 -0.5443 15 1 16 -0.0685 -0.1477 15 1 17 0.2092 0.0436 15 1 18 0.1754 0.2956 15 1 19 -0.2387 0.2402 15 1 20 -0.4722 -0.1544 15 2 0 -0.6016 -0.1208 15 2 1 0.3848 1.2768 15 2 2 0.7090 0.2141 15 2 3 0.4046 -1.4946 15 2 4 0.2121 -0.1776 15 2 5 -0.0324 0.9127 15 2 6 -0.5183 0.0988 15 2 7 -0.4735 -0.1365 15 2 8 -0.0806 -0.0962 15 2 9 0.2878 -0.2212 15 2 10 0.6703 0.1390 15 2 11 0.0583 0.0955 15 2 12 -0.8681 -0.1652 15 2 13 -0.2378 0.0883 15 2 14 0.5782 0.1458 15 3 0 0.9531 0.1494 15 3 1 0.6409 0.0310 15 3 2 0.4540 0.1710 15 3 3 -0.4698 0.0318 15 3 4 -1.1354 0.1985 15 3 5 -0.5250 0.2743 16 -4 -14 0.5003 -0.0060 16 -4 -13 0.0830 0.2627 16 -4 -12 -0.0724 0.2706 16 -4 -11 -0.0166 0.1919 16 -4 -10 -0.6115 -0.3906 16 -4 -9 -0.3498 -0.5395 16 -4 -8 0.8511 0.3241 16 -4 -7 0.1474 0.4704 16 -4 -6 -1.1436 -0.4827 16 -4 -5 0.1482 -0.5338 16 -4 -4 1.3676 0.5303 16 -4 -3 0.2084 0.8642 16 -4 -2 -0.7434 0.0542 16 -4 -1 -0.5959 -0.6563 16 -3 -18 -0.1266 0.2316 16 -3 -17 0.0731 -0.0406 16 -3 -16 -0.0912 -0.2532 16 -3 -15 -0.4158 0.1814 16 -3 -14 0.5113 0.3693 16 -3 -13 0.6035 0.1056 16 -3 -12 -0.8103 -0.1457 16 -3 -11 -0.3282 -0.6541 16 -3 -10 1.0541 -0.5726 16 -3 -9 -0.0289 0.7696 16 -3 -8 -1.1272 0.8430 16 -3 -7 0.0133 -0.7251 16 -3 -6 0.7106 -0.4555 16 -3 -5 0.1330 0.8207 16 -3 -4 -0.1015 0.2200 16 -3 -3 -0.2264 -0.4418 16 -3 -2 -0.2982 -0.1583 16 -3 -1 0.2923 -0.2963 16 -2 -21 0.3562 0.1370 16 -2 -20 0.0016 0.1457 16 -2 -19 -0.3945 -0.3590 16 -2 -18 -0.3374 0.0065 16 -2 -17 0.0609 0.3177 16 -2 -16 0.2615 -0.4280 16 -2 -15 0.0628 0.1035 16 -2 -14 0.2117 0.9265 16 -2 -13 0.4735 -0.4930 16 -2 -12 0.0188 -0.9950 16 -2 -11 -0.3833 0.5249 16 -2 -10 -0.4748 0.3126 16 -2 -9 -0.5668 -0.5578 16 -2 -8 0.0730 0.3985 16 -2 -7 0.5943 0.6123 16 -2 -6 0.1363 -0.4276 16 -2 -5 0.2364 -0.2931 16 -2 -4 0.5709 0.1741 16 -2 -3 -0.2238 0.0960 16 -2 -2 -0.7971 0.2174 16 -2 -1 -0.3212 -0.4053 16 -1 -20 -0.0460 0.2410 16 -1 -19 0.0459 -0.2345 16 -1 -18 0.0170 -0.6873 16 -1 -17 0.6457 0.2576 16 -1 -16 0.3585 0.8419 16 -1 -15 -0.8497 0.0873 16 -1 -14 -0.2479 -0.2779 16 -1 -13 0.8486 -0.5308 16 -1 -12 -0.0218 -0.5363 16 -1 -11 -0.7786 0.5452 16 -1 -10 -0.3766 0.5444 16 -1 -9 -0.2226 -0.4223 16 -1 -8 0.3255 0.1197 16 -1 -7 1.1085 0.5826 16 -1 -6 0.5139 -0.2205 16 -1 -5 -0.2747 -0.3637 16 -1 -4 -0.3527 -0.1579 16 -1 -3 -0.9045 -0.4477 16 -1 -2 -0.7419 0.0343 16 -1 -1 0.7763 0.7087 16 0 0 0.6202 0.0103 16 0 1 -0.4468 -0.0023 16 0 2 -0.5585 -0.0055 16 0 3 0.6475 0.0119 16 0 4 -0.2803 -0.0036 16 0 5 -1.1045 -0.0185 16 0 6 0.6249 0.0042 16 0 7 0.7704 0.0154 16 0 8 -0.4309 -0.0005 16 0 9 0.3723 -0.0050 16 0 10 0.3593 0.0057 16 0 11 -1.0978 0.0004 16 0 12 -0.5333 -0.0165 16 0 13 0.7733 -0.0037 16 0 14 0.6879 0.0203 16 0 15 0.1330 0.0063 16 0 16 -0.4893 -0.0124 16 0 17 -0.7593 -0.0029 16 0 18 -0.1823 0.0008 16 0 19 0.4412 -0.0025 16 1 0 -0.8787 0.0569 16 1 1 0.2642 -0.2172 16 1 2 0.1399 0.6414 16 1 3 -0.1680 0.0138 16 1 4 0.0527 -1.2092 16 1 5 -0.1879 -0.1113 16 1 6 0.1131 0.8120 16 1 7 0.7976 -0.0255 16 1 8 0.1685 0.0754 16 1 9 -0.6760 0.2327 16 1 10 -0.4190 -0.7433 16 1 11 0.0140 -0.3270 16 1 12 0.1285 0.7693 16 1 13 0.2160 0.3513 16 1 14 0.2195 -0.2352 16 1 15 -0.0697 -0.2162 16 1 16 -0.3912 -0.1763 16 1 17 -0.1041 0.0437 16 2 0 0.1990 0.9548 16 2 1 0.3040 -0.4850 16 2 2 0.0011 -1.2732 16 2 3 -0.2690 0.1026 16 2 4 0.0024 0.6286 16 2 5 0.4966 0.1532 16 2 6 0.4962 0.2730 16 2 7 -0.2224 -0.0402 16 2 8 -0.5425 -0.6573 16 2 9 -0.0337 -0.3002 16 2 10 -0.2106 0.3739 16 2 11 -0.5953 0.4587 16 2 12 0.3432 0.0958 16 3 0 -0.5385 -0.1010 16 3 1 0.0410 0.3897 16 3 2 0.4247 0.2192 16 3 3 0.3093 0.2676 17 -3 -12 0.1256 -0.6683 17 -3 -11 0.2277 -0.4600 17 -3 -10 -0.3467 0.6737 17 -3 -9 -0.2875 0.7420 17 -3 -8 0.3459 -0.2843 17 -3 -7 0.2428 -0.1488 17 -3 -6 -0.3775 0.3423 17 -3 -5 -0.4820 -0.1112 17 -3 -4 0.0623 -0.2539 17 -3 -3 0.7421 -0.1564 17 -3 -2 0.8488 -0.2278 17 -3 -1 0.0079 0.2609 17 -2 -16 0.0768 0.1116 17 -2 -15 0.3698 0.4433 17 -2 -14 0.1108 -0.5537 17 -2 -13 -0.4151 -0.7447 17 -2 -12 -0.1183 0.1554 17 -2 -11 0.0430 0.2982 17 -2 -10 -0.3831 0.2838 17 -2 -9 -0.0035 0.4899 17 -2 -8 0.3991 0.0203 17 -2 -7 -0.0532 -0.3309 17 -2 -6 0.0421 -0.1437 17 -2 -5 0.4701 -0.3421 17 -2 -4 0.2212 -0.2987 17 -2 -3 -0.2289 0.4185 17 -2 -2 -0.6522 0.3989 17 -2 -1 -0.6225 -0.1228 17 -1 -18 0.3026 0.4430 17 -1 -17 -0.0895 0.1297 17 -1 -16 -0.6020 -0.3206 17 -1 -15 0.1784 -0.0041 17 -1 -14 0.5665 -0.2855 17 -1 -13 -0.2361 -0.3810 17 -1 -12 -0.3414 0.5216 17 -1 -11 0.0015 0.3242 17 -1 -10 -0.1713 -0.1896 17 -1 -9 0.0398 0.4851 17 -1 -8 0.4119 0.2315 17 -1 -7 0.2628 -0.8725 17 -1 -6 0.3187 -0.6385 17 -1 -5 0.0818 0.2112 17 -1 -4 -1.0606 0.4955 17 -1 -3 -1.0748 0.4225 17 -1 -2 0.5686 -0.0042 17 -1 -1 1.2599 -0.4596 17 0 0 -1.2374 -0.0040 17 0 1 -1.3011 0.0018 17 0 2 0.4633 0.0060 17 0 3 0.6837 -0.0110 17 0 4 0.0902 -0.0094 17 0 5 0.2180 0.0094 17 0 6 -0.5023 0.0052 17 0 7 -0.6352 -0.0069 17 0 8 1.0077 0.0030 17 0 9 0.7719 0.0137 17 0 10 -1.0504 -0.0040 17 0 11 -0.7114 -0.0207 17 0 12 0.5013 0.0004 17 0 13 0.4168 0.0186 17 0 14 0.0077 0.0003 17 1 0 -0.4466 -0.1170 17 1 1 0.3267 0.4398 17 1 2 0.7212 -0.0930 17 1 3 0.3250 -0.5141 17 1 4 -0.5574 0.3815 17 1 5 -0.2422 0.3963 17 1 6 0.6431 -0.5323 17 1 7 0.3034 0.0064 17 1 8 -0.4398 0.3675 17 1 9 -0.4372 -0.6069 17 1 10 -0.1770 -0.2635 17 1 11 0.0151 0.8677 17 1 12 0.2955 0.4778 17 2 0 0.0926 -0.0136 17 2 1 0.4635 0.0713 17 2 2 0.3961 0.3534 17 2 3 0.4116 -0.2029 17 2 4 0.2290 -0.3726 17 2 5 -0.1904 0.3001 17 2 6 -0.6138 0.1596 17 2 7 -0.5221 -0.4048 17 2 8 0.1111 -0.0436 18 -1 -8 0.0666 -0.4054 18 -1 -7 -0.0820 -0.3045 18 -1 -6 0.0085 0.1104 18 -1 -5 -0.4671 0.4376 18 -1 -4 -0.5741 0.2660 18 -1 -3 0.2905 -0.1869 18 -1 -2 0.8240 -0.3568 18 -1 -1 0.3073 -0.1966 18 0 0 -0.8165 -0.0025 18 0 1 0.3973 -0.0032 18 0 2 0.7345 -0.0051 18 0 3 0.2316 0.0008 18 0 4 -0.0851 0.0032 18 0 5 -0.7460 -0.0020 18 0 6 -0.5045 -0.0017 18 0 7 0.9373 0.0064 18 0 8 0.6219 0.0077 18 1 0 0.4734 0.1848 18 1 1 0.7046 0.2812 18 1 2 0.0696 0.1468 18 1 3 -0.6224 0.2451 18 1 4 -0.3075 -0.3141 18 1 5 0.2778 -0.8542 0 0 0 0.0 0.0 ; _shelx_fab_checksum 59467 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.350 _oxdiff_exptl_absorpt_empirical_full_min 0.614 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.52892(15) 0.3698(3) 0.63839(6) 0.0677(7) Uani 1 1 d . . . . . O7 O -0.15037(14) 1.2537(4) 0.97603(6) 0.0723(8) Uani 1 1 d . . . . . H7 H -0.198009 1.302917 0.979417 0.108 Uiso 1 1 calc R U . . . O13 O 0.67243(15) 0.2668(4) 0.37800(6) 0.0794(8) Uani 1 1 d . . . . . H13 H 0.662994 0.357207 0.366903 0.119 Uiso 1 1 calc R U . . . O2 O 0.65524(15) 0.7158(4) 0.71341(7) 0.0800(8) Uani 1 1 d . . . . . O3 O 0.51091(15) 0.7317(4) 0.74502(6) 0.0762(8) Uani 1 1 d . . . . . H3 H 0.561109 0.761881 0.738949 0.114 Uiso 1 1 calc R U . . . O18 O 1.02212(15) 0.9693(4) 0.14677(6) 0.0802(9) Uani 1 1 d . . . . . N2 N -0.04959(18) 1.0560(4) 1.07386(7) 0.0638(8) Uani 1 1 d . . . . . H2 H -0.024155 1.020451 1.094652 0.077 Uiso 1 1 calc R U . . . N1 N 0.39707(17) 0.4275(4) 0.66441(7) 0.0598(8) Uani 1 1 d . . . . . H1 H 0.369870 0.366233 0.647333 0.072 Uiso 1 1 calc R U . . . O10 O 0.31894(15) 0.2283(4) 0.60316(6) 0.0747(8) Uani 1 1 d . . . . . O8 O -0.17638(16) 1.0914(4) 1.10473(6) 0.0830(9) Uani 1 1 d . . . . . O16 O 0.98409(17) 0.6512(4) 0.25954(7) 0.0991(10) Uani 1 1 d . . . . . H16 H 1.038244 0.634360 0.258030 0.149 Uiso 1 1 calc R U . . . O12 O 0.33214(17) 0.1075(4) 0.47133(6) 0.0862(9) Uani 1 1 d . . . . . H12 H 0.277583 0.095386 0.472619 0.129 Uiso 1 1 calc R U . . . N3 N 0.44505(17) 0.2644(4) 0.57088(7) 0.0610(8) Uani 1 1 d . . . . . H3A H 0.472053 0.295298 0.591711 0.073 Uiso 1 1 calc R U . . . O15 O 0.60735(18) 0.4970(4) 0.32534(7) 0.0875(9) Uani 1 1 d . . . . . H15A H 0.562656 0.557988 0.326007 0.131 Uiso 1 1 calc R U . . . O9 O -0.29200(16) 1.3124(4) 1.00591(7) 0.0844(9) Uani 1 1 d . . . . . O6 O 0.20257(17) 1.0795(4) 0.88755(7) 0.0969(10) Uani 1 1 d . . . . . H6A H 0.188660 0.998973 0.873733 0.145 Uiso 1 1 calc R U . . . O11 O 0.19252(18) 0.0399(5) 0.50248(7) 0.1034(11) Uani 1 1 d . . . . . C50 C 0.6182(2) 0.2552(4) 0.40761(8) 0.0548(8) Uani 1 1 d . . . . . O4 O 0.15111(19) 0.8653(4) 0.82866(7) 0.1020(10) Uani 1 1 d . . . . . H4 H 0.135603 0.793059 0.843842 0.153 Uiso 1 1 calc R U . . . C44 C 0.4564(2) 0.2198(4) 0.50471(8) 0.0523(8) Uani 1 1 d . . . . . N4 N 0.88625(18) 0.9132(4) 0.16890(7) 0.0708(9) Uani 1 1 d . . . . . H4B H 0.862702 0.963109 0.149244 0.085 Uiso 1 1 calc R U . . . C3 C 0.6212(2) 0.6278(5) 0.68716(9) 0.0615(10) Uani 1 1 d . . . . . C2 C 0.5274(2) 0.5693(4) 0.68913(8) 0.0527(8) Uani 1 1 d . . . . . C20 C 0.0003(2) 1.0590(5) 1.04281(8) 0.0597(10) Uani 1 1 d . . . . . H20 H 0.058768 1.016749 1.044845 0.072 Uiso 1 1 calc R U . . . C61 C 0.9771(2) 0.9030(5) 0.17226(8) 0.0641(10) Uani 1 1 d . . . . . C75 C -0.1200(2) 1.1829(4) 1.00853(8) 0.0546(9) Uani 1 1 d . . . . . C19 C -0.0301(2) 1.1201(4) 1.00888(8) 0.0542(9) Uani 1 1 d . . . . . C1' C 0.4751(2) 0.6315(4) 0.71867(8) 0.0572(9) Uani 1 1 d . . . . . C46 C 0.3578(2) 0.2154(4) 0.57230(8) 0.0561(9) Uani 1 1 d . . . . . C1 C 0.4883(2) 0.4508(4) 0.66220(8) 0.0560(9) Uani 1 1 d . . . . . C4' C 0.3226(2) 0.6643(4) 0.74942(8) 0.0585(9) Uani 1 1 d . . . . . C47 C 0.5106(2) 0.2281(4) 0.47075(8) 0.0528(8) Uani 1 1 d . . . . . C45 C 0.4926(2) 0.2684(4) 0.53924(8) 0.0553(9) Uani 1 1 d . . . . . H45 H 0.552096 0.305298 0.540926 0.066 Uiso 1 1 calc R U . . . C60 C 0.8306(2) 0.8499(5) 0.19455(8) 0.0595(9) Uani 1 1 d . . . . . H60 H 0.769037 0.865393 0.190211 0.071 Uiso 1 1 calc R U . . . C49 C 0.5314(2) 0.3164(5) 0.40612(8) 0.0671(11) Uani 1 1 d . . . . . H49 H 0.508331 0.367265 0.384061 0.081 Uiso 1 1 calc R U . . . O17 O 1.13705(17) 0.7201(5) 0.24234(7) 0.1225(12) Uani 1 1 d . . . . . C48 C 0.4780(2) 0.3028(5) 0.43729(9) 0.0669(11) Uani 1 1 d . . . . . H48 H 0.419381 0.344441 0.435759 0.080 Uiso 1 1 calc R U . . . C53 C 0.6665(2) 0.5655(5) 0.30132(9) 0.0670(10) Uani 1 1 d . . . . . C16 C 0.0270(2) 1.1184(4) 0.97584(8) 0.0546(9) Uani 1 1 d . . . . . C21 C -0.1377(2) 1.1056(5) 1.07462(8) 0.0590(9) Uani 1 1 d . . . . . C42 C 0.3155(2) 0.1541(4) 0.53723(8) 0.0555(9) Uani 1 1 d . . . . . C22 C -0.2679(2) 1.2384(5) 1.03566(8) 0.0586(7) Uani 1 1 d . . . . . C5' C 0.2352(2) 0.7160(5) 0.73911(9) 0.0638(10) Uani 1 1 d . . . . . H5' H 0.215175 0.709097 0.713925 0.077 Uiso 1 1 calc R U . . . C43 C 0.3665(2) 0.1626(5) 0.50458(8) 0.0603(10) Uani 1 1 d . . . . . C9' C 0.3502(2) 0.6786(5) 0.78748(9) 0.0719(12) Uani 1 1 d . . . . . H9' H 0.408013 0.645407 0.795298 0.086 Uiso 1 1 calc R U . . . C74 C -0.1751(2) 1.1737(5) 1.03946(8) 0.0586(7) Uani 1 1 d . . . . . C59 C 0.8586(2) 0.7647(4) 0.22638(8) 0.0585(9) Uani 1 1 d . . . . . C54 C 0.6436(2) 0.5913(5) 0.26330(10) 0.0730(12) Uani 1 1 d . . . . . H54 H 0.585848 0.566121 0.253836 0.088 Uiso 1 1 calc R U . . . C23 C -0.3370(2) 1.2017(5) 1.06390(9) 0.0651(10) Uani 1 1 d . . . . . H23 H -0.307510 1.185784 1.088908 0.078 Uiso 1 1 calc R U . . . C3' C 0.3819(2) 0.5957(4) 0.72062(8) 0.0569(9) Uani 1 1 d . . . . . C51 C 0.6515(2) 0.1799(4) 0.44062(9) 0.0623(10) Uani 1 1 d . . . . . H51 H 0.710096 0.138361 0.442080 0.075 Uiso 1 1 calc R U . . . C56 C 0.7932(2) 0.6982(4) 0.25252(8) 0.0567(9) Uani 1 1 d . . . . . C63 C 0.9545(2) 0.7436(5) 0.23020(8) 0.0669(11) Uani 1 1 d . . . . . C4 C 0.6775(2) 0.5922(4) 0.65304(9) 0.0621(10) Uani 1 1 d . . . . . H4A H 0.637148 0.564137 0.631340 0.074 Uiso 1 1 calc R U . . . C58 C 0.7507(2) 0.6085(5) 0.31496(9) 0.0703(11) Uani 1 1 d . . . . . H58 H 0.765961 0.592981 0.340469 0.084 Uiso 1 1 calc R U . . . C52 C 0.5979(2) 0.1664(5) 0.47138(9) 0.0619(10) Uani 1 1 d . . . . . H52 H 0.621166 0.114073 0.493250 0.074 Uiso 1 1 calc R U . . . C6' C 0.1781(2) 0.7773(5) 0.76574(10) 0.0700(11) Uani 1 1 d . . . . . H6' H 0.119870 0.810011 0.758424 0.084 Uiso 1 1 calc R U . . . C2' C 0.3481(2) 0.4948(4) 0.69172(8) 0.0584(9) Uani 1 1 d . . . . . H2' H 0.286750 0.471446 0.691018 0.070 Uiso 1 1 calc R U . . . C5 C 0.7363(2) 0.4357(5) 0.66292(9) 0.0636(10) Uani 1 1 d . . . . . H5A H 0.776120 0.465565 0.684289 0.076 Uiso 1 1 calc R U . . . H5B H 0.697172 0.345313 0.671202 0.076 Uiso 1 1 calc R U . . . C26 C -0.4456(2) 0.9458(5) 1.07696(10) 0.0744(12) Uani 1 1 d . . . . . H26 H -0.492440 1.027442 1.083478 0.089 Uiso 1 1 calc R U . . . C14 C 0.1732(2) 1.1576(5) 0.94977(10) 0.0711(11) Uani 1 1 d . . . . . H14 H 0.232522 1.194325 0.952906 0.085 Uiso 1 1 calc R U . . . C40 C 0.1038(2) -0.0974(5) 0.56006(10) 0.0745(12) Uani 1 1 d . . . . . H40A H 0.141551 -0.194674 0.554723 0.089 Uiso 1 1 calc R U . . . H40B H 0.067093 -0.074588 0.537338 0.089 Uiso 1 1 calc R U . . . C24 C -0.3806(2) 1.0319(5) 1.05056(9) 0.0716(11) Uani 1 1 d . . . . . H24A H -0.412670 1.052641 1.026587 0.086 Uiso 1 1 calc R U . . . H24B H -0.332649 0.951850 1.045807 0.086 Uiso 1 1 calc R U . . . C62 C 1.0122(2) 0.8162(5) 0.20507(9) 0.0706(11) Uani 1 1 d . . . . . C15 C 0.1164(2) 1.1694(5) 0.97956(9) 0.0662(10) Uani 1 1 d . . . . . H15 H 0.138345 1.212513 1.002606 0.079 Uiso 1 1 calc R U . . . C39 C 0.1650(2) 0.0559(5) 0.56728(9) 0.0661(10) Uani 1 1 d . . . . . H39 H 0.203368 0.031541 0.589806 0.079 Uiso 1 1 calc R U . . . C41 C 0.2252(2) 0.0822(5) 0.53460(9) 0.0679(11) Uani 1 1 d . . . . . C13 C 0.1430(2) 1.0920(5) 0.91547(9) 0.0706(11) Uani 1 1 d . . . . . C57 C 0.8137(2) 0.6752(5) 0.29111(8) 0.0654(10) Uani 1 1 d . . . . . H57 H 0.870431 0.705060 0.300950 0.078 Uiso 1 1 calc R U . . . C8' C 0.2926(3) 0.7412(5) 0.81341(9) 0.0801(12) Uani 1 1 d . . . . . H8' H 0.311703 0.750849 0.838663 0.096 Uiso 1 1 calc R U . . . C6 C 0.7936(2) 0.3640(5) 0.63204(10) 0.0744(12) Uani 1 1 d . . . . . H6 H 0.828606 0.457200 0.621463 0.089 Uiso 1 1 calc R U . . . C55 C 0.7065(2) 0.6540(5) 0.23999(9) 0.0671(11) Uani 1 1 d . . . . . H55 H 0.690623 0.667867 0.214485 0.080 Uiso 1 1 calc R U . . . C18 C 0.0547(2) 1.0440(6) 0.91135(10) 0.0776(13) Uani 1 1 d . . . . . H18 H 0.032821 1.004673 0.887950 0.093 Uiso 1 1 calc R U . . . C7' C 0.2063(2) 0.7899(5) 0.80225(10) 0.0787(12) Uani 1 1 d . . . . . C65 C 1.1796(2) 0.8971(7) 0.19117(10) 0.0923(16) Uani 1 1 d . . . . . H65 H 1.152874 0.998869 0.179218 0.111 Uiso 1 1 calc R U . . . C8 C 0.7812(3) 0.2272(6) 0.56623(11) 0.0947(15) Uani 1 1 d . . . . . H8 H 0.815009 0.308895 0.554082 0.114 Uiso 1 1 calc R U . . . C64 C 1.1111(3) 0.8113(7) 0.21417(10) 0.0905(15) Uani 1 1 d . . . . . C36 C 0.0410(2) -0.1494(6) 0.59109(11) 0.0827(13) Uani 1 1 d . . . . . H36 H 0.000831 -0.053442 0.595882 0.099 Uiso 1 1 calc R U . . . C17 C -0.0026(2) 1.0523(5) 0.94086(9) 0.0686(11) Uani 1 1 d . . . . . H17 H -0.061538 1.013713 0.937488 0.082 Uiso 1 1 calc R U . . . C70 C 1.2150(3) 0.9834(7) 0.10756(12) 0.1105(7) Uani 1 1 d . . . . . H70A H 1.161870 0.934342 0.095074 0.133 Uiso 1 1 calc R U . . . H70B H 1.194695 1.068096 0.125289 0.133 Uiso 1 1 calc R U . . . C68 C 1.2628(3) 0.8439(8) 0.12995(11) 0.1102(14) Uani 1 1 d . . . . . H68 H 1.317881 0.890527 0.142085 0.132 Uiso 1 1 calc R U . . . C29 C -0.4536(3) 0.8057(7) 1.14114(11) 0.0997(17) Uani 1 1 d . . . . . H29 H -0.492092 0.879885 1.153107 0.120 Uiso 1 1 calc R U . . . C27 C -0.4899(3) 0.7934(6) 1.05535(12) 0.1059(17) Uani 1 1 d . . . . . H27A H -0.527130 0.835361 1.034585 0.159 Uiso 1 1 calc R U . . . H27B H -0.526162 0.729551 1.072189 0.159 Uiso 1 1 calc R U . . . H27C H -0.443918 0.720893 1.045895 0.159 Uiso 1 1 calc R U . . . C12 C 0.7329(3) 0.7489(5) 0.64335(12) 0.0963(15) Uani 1 1 d . . . . . H12A H 0.693246 0.841843 0.636790 0.144 Uiso 1 1 calc R U . . . H12B H 0.769489 0.723313 0.622338 0.144 Uiso 1 1 calc R U . . . H12C H 0.770830 0.780197 0.664829 0.144 Uiso 1 1 calc R U . . . C67 C 1.2033(2) 0.7696(7) 0.16059(10) 0.0925(16) Uani 1 1 d . . . . . H67A H 1.148033 0.727033 0.148542 0.111 Uiso 1 1 calc R U . . . H67B H 1.234332 0.673547 0.172458 0.111 Uiso 1 1 calc R U . . . C71 C 1.2675(3) 1.0738(7) 0.07819(12) 0.1105(7) Uani 1 1 d . U . . . H71 H 1.296904 1.001395 0.061921 0.133 Uiso 1 1 calc R U . . . C9 C 0.7817(3) 0.0732(6) 0.55217(11) 0.0955(15) Uani 1 1 d . . . . . H9 H 0.748908 -0.011354 0.563878 0.115 Uiso 1 1 calc R U . . . C28 C -0.3973(3) 0.8814(6) 1.11359(10) 0.0876(14) Uani 1 1 d . . . . . H28A H -0.352618 0.797926 1.106782 0.105 Uiso 1 1 calc R U . . . H28B H -0.365443 0.976624 1.125398 0.105 Uiso 1 1 calc R U . . . C72 C 1.2782(3) 1.2206(8) 0.07206(12) 0.1126(7) Uani 1 1 d . U . . . H72 H 1.250293 1.292119 0.088977 0.135 Uiso 1 1 calc R U . . . C7 C 0.7320(3) 0.2854(6) 0.59975(10) 0.0901(15) Uani 1 1 d . . . . . H7A H 0.699893 0.189051 0.609869 0.108 Uiso 1 1 calc R U . . . H7B H 0.687730 0.369799 0.591571 0.108 Uiso 1 1 calc R U . . . C11 C 0.8573(3) 0.2305(7) 0.64698(13) 0.1264(19) Uani 1 1 d . . . . . H11A H 0.892891 0.276084 0.667829 0.190 Uiso 1 1 calc R U . . . H11B H 0.896031 0.195682 0.627340 0.190 Uiso 1 1 calc R U . . . H11C H 0.823793 0.133883 0.655362 0.190 Uiso 1 1 calc R U . . . C34 C 0.0339(3) -0.2222(9) 0.66119(13) 0.1473(6) Uani 1 1 d . U . . . H34 H 0.000438 -0.125087 0.666130 0.177 Uiso 1 1 calc R U . . . C38 C 0.1146(3) 0.2190(6) 0.57434(12) 0.1061(16) Uani 1 1 d . . . . . H38A H 0.076988 0.246304 0.552500 0.159 Uiso 1 1 calc R U . . . H38B H 0.156793 0.309870 0.579166 0.159 Uiso 1 1 calc R U . . . H38C H 0.078002 0.204653 0.595847 0.159 Uiso 1 1 calc R U . . . C35 C 0.0917(3) -0.1968(9) 0.62876(12) 0.1442(7) Uani 1 1 d . U . . . H35A H 0.125511 -0.300759 0.624909 0.173 Uiso 1 1 calc R U . . . H35B H 0.134681 -0.107180 0.635080 0.173 Uiso 1 1 calc R U . . . C10 C 0.8329(3) 0.0269(7) 0.51781(12) 0.123(2) Uani 1 1 d . . . . . H10A H 0.797728 -0.050466 0.502258 0.185 Uiso 1 1 calc R U . . . H10B H 0.888682 -0.026709 0.525609 0.185 Uiso 1 1 calc R U . . . H10C H 0.845087 0.128158 0.503666 0.185 Uiso 1 1 calc R U . . . C30 C -0.4574(3) 0.6495(8) 1.15129(13) 0.126(2) Uani 1 1 d . . . . . H30 H -0.414823 0.578199 1.140967 0.151 Uiso 1 1 calc R U . . . C37 C -0.0172(3) -0.3036(6) 0.57767(13) 0.1109(17) Uani 1 1 d . . . . . H37A H -0.042294 -0.281579 0.552721 0.166 Uiso 1 1 calc R U . . . H37B H -0.064999 -0.320467 0.594737 0.166 Uiso 1 1 calc R U . . . H37C H 0.019562 -0.404095 0.577233 0.166 Uiso 1 1 calc R U . . . C25 C -0.4055(3) 1.3434(6) 1.06571(12) 0.0946(15) Uani 1 1 d . . . . . H25A H -0.375201 1.449193 1.071216 0.142 Uiso 1 1 calc R U . . . H25B H -0.446583 1.318982 1.085230 0.142 Uiso 1 1 calc R U . . . H25C H -0.438120 1.352178 1.041828 0.142 Uiso 1 1 calc R U . . . C73 C 1.3280(3) 1.3144(8) 0.04227(13) 0.134(2) Uani 1 1 d . . . . . H73A H 1.289387 1.399398 0.030760 0.201 Uiso 1 1 calc R U . . . H73B H 1.346209 1.235250 0.023340 0.201 Uiso 1 1 calc R U . . . H73C H 1.380277 1.368388 0.053707 0.201 Uiso 1 1 calc R U . . . C69 C 1.2881(3) 0.6954(8) 0.10362(10) 0.1102(14) Uani 1 1 d . . . . . H69A H 1.234279 0.646399 0.092345 0.165 Uiso 1 1 calc R U . . . H69B H 1.320450 0.610010 0.118050 0.165 Uiso 1 1 calc R U . . . H69C H 1.325183 0.737783 0.084113 0.165 Uiso 1 1 calc R U . . . C66 C 1.2630(3) 0.9506(9) 0.21664(13) 0.147(3) Uani 1 1 d . . . . . H66A H 1.244197 1.026535 0.236081 0.221 Uiso 1 1 calc R U . . . H66B H 1.305999 1.007159 0.201475 0.221 Uiso 1 1 calc R U . . . H66C H 1.290024 0.850925 0.228022 0.221 Uiso 1 1 calc R U . . . C33 C 0.0193(3) -0.3308(9) 0.68203(13) 0.1500(8) Uani 1 1 d . U . . . H33 H 0.052229 -0.428624 0.677092 0.180 Uiso 1 1 calc R U . . . C32 C -0.0394(4) -0.3538(10) 0.71505(13) 0.189(3) Uani 1 1 d . . . . . H32A H -0.100645 -0.328584 0.707449 0.283 Uiso 1 1 calc R U . . . H32B H -0.019955 -0.277950 0.735050 0.283 Uiso 1 1 calc R U . . . H32C H -0.035202 -0.469464 0.723810 0.283 Uiso 1 1 calc R U . . . C31 C -0.5216(4) 0.5628(10) 1.17788(15) 0.203(3) Uani 1 1 d . . . . . H31A H -0.565144 0.497150 1.163333 0.305 Uiso 1 1 calc R U . . . H31B H -0.551964 0.647840 1.192140 0.305 Uiso 1 1 calc R U . . . H31C H -0.488162 0.488797 1.194866 0.305 Uiso 1 1 calc R U . . . 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 O1 0.0627(13) 0.0822(16) 0.0587(12) -0.0192(12) 0.0071(10) -0.0033(13) O7 0.0569(12) 0.1072(19) 0.0529(11) 0.0199(13) 0.0017(10) 0.0049(14) O13 0.0709(13) 0.105(2) 0.0644(12) 0.0106(14) 0.0264(11) -0.0021(15) O2 0.0571(13) 0.0976(18) 0.0848(15) -0.0262(15) -0.0039(12) -0.0077(14) O3 0.0616(13) 0.0934(17) 0.0735(13) -0.0280(14) -0.0005(11) -0.0082(14) O18 0.0543(12) 0.129(2) 0.0577(12) 0.0270(14) 0.0075(10) 0.0062(15) N2 0.0606(15) 0.0820(19) 0.0486(13) 0.0121(14) 0.0024(12) 0.0184(15) N1 0.0520(13) 0.0728(17) 0.0545(14) -0.0113(14) 0.0021(11) -0.0104(14) O10 0.0732(13) 0.1059(19) 0.0459(10) -0.0069(13) 0.0140(10) -0.0197(15) O8 0.0655(13) 0.131(2) 0.0536(12) 0.0242(14) 0.0118(10) 0.0160(16) O16 0.0729(15) 0.146(2) 0.0794(14) 0.0526(15) 0.0128(12) 0.0342(17) O12 0.0824(15) 0.127(2) 0.0495(12) -0.0161(14) 0.0105(11) -0.0313(17) N3 0.0604(14) 0.0782(19) 0.0447(12) -0.0022(14) 0.0047(11) -0.0107(15) O15 0.0835(16) 0.102(2) 0.0791(15) 0.0261(15) 0.0270(12) 0.0113(16) O9 0.0600(13) 0.124(2) 0.0691(14) 0.0304(15) 0.0008(11) 0.0122(15) O6 0.0823(15) 0.132(2) 0.0794(14) -0.0309(16) 0.0374(12) -0.0168(18) O11 0.0808(16) 0.162(3) 0.0677(15) -0.0166(18) 0.0084(13) -0.0452(18) C50 0.0551(15) 0.0580(18) 0.0522(15) -0.0008(15) 0.0148(13) -0.0114(16) O4 0.1000(18) 0.121(2) 0.0874(16) -0.0358(16) 0.0379(13) -0.0117(19) C44 0.0541(15) 0.0553(17) 0.0478(15) -0.0011(15) 0.0066(13) 0.0006(16) N4 0.0592(15) 0.105(2) 0.0479(13) 0.0221(15) 0.0060(12) 0.0183(16) C3 0.0516(17) 0.060(2) 0.073(2) 0.0023(18) -0.0004(15) -0.0020(17) C2 0.0552(16) 0.0519(17) 0.0512(15) -0.0001(15) 0.0054(13) -0.0028(16) C20 0.0482(15) 0.079(2) 0.0525(16) 0.0091(17) 0.0088(13) 0.0082(17) C61 0.0606(18) 0.084(2) 0.0479(15) 0.0182(17) 0.0080(14) 0.0127(18) C75 0.0511(15) 0.0640(19) 0.0485(15) 0.0058(15) -0.0026(13) 0.0015(16) C19 0.0469(15) 0.066(2) 0.0496(15) -0.0003(16) 0.0049(13) -0.0020(16) C1' 0.0645(18) 0.0581(19) 0.0488(15) -0.0046(15) 0.0002(14) -0.0003(17) C46 0.0621(17) 0.0601(19) 0.0462(14) -0.0036(15) 0.0023(13) -0.0037(17) C1 0.0558(16) 0.064(2) 0.0487(15) -0.0072(15) 0.0077(13) 0.0043(17) C4' 0.0623(17) 0.0600(19) 0.0540(16) -0.0050(16) 0.0129(14) -0.0064(17) C47 0.0583(16) 0.0558(17) 0.0447(14) 0.0026(15) 0.0067(13) -0.0076(16) C45 0.0563(16) 0.0628(19) 0.0475(15) -0.0025(15) 0.0112(13) -0.0051(17) C60 0.0505(16) 0.075(2) 0.0540(16) 0.0145(17) 0.0116(13) 0.0116(17) C49 0.0682(19) 0.092(3) 0.0418(15) 0.0065(17) 0.0053(14) -0.006(2) O17 0.0673(15) 0.211(3) 0.0889(17) 0.059(2) -0.0023(13) 0.038(2) C48 0.0569(18) 0.090(3) 0.0540(17) 0.0048(18) 0.0057(15) -0.0010(19) C53 0.0707(19) 0.070(2) 0.0616(17) 0.0186(17) 0.0213(15) 0.004(2) C16 0.0515(15) 0.064(2) 0.0485(15) 0.0009(15) 0.0070(13) 0.0002(16) C21 0.0570(16) 0.075(2) 0.0452(14) 0.0079(16) 0.0098(13) 0.0134(17) C42 0.0652(17) 0.0555(17) 0.0465(14) -0.0063(15) 0.0099(13) -0.0110(16) C22 0.0556(12) 0.0677(15) 0.0528(11) 0.0084(12) 0.0057(10) 0.0019(12) C5' 0.0545(17) 0.069(2) 0.0680(18) -0.0076(19) 0.0042(15) -0.0091(18) C43 0.0594(17) 0.070(2) 0.0514(16) -0.0063(16) 0.0030(14) -0.0048(18) C9' 0.0598(18) 0.103(3) 0.0538(17) -0.007(2) 0.0058(15) -0.001(2) C74 0.0556(12) 0.0677(15) 0.0528(11) 0.0084(12) 0.0057(10) 0.0019(12) C59 0.0669(18) 0.0596(19) 0.0496(15) 0.0083(15) 0.0081(14) 0.0144(17) C54 0.069(2) 0.084(3) 0.067(2) 0.005(2) 0.0003(17) -0.006(2) C23 0.0522(16) 0.081(2) 0.0630(18) -0.0083(18) 0.0093(14) 0.0113(18) C3' 0.0555(16) 0.0595(19) 0.0562(16) -0.0043(16) 0.0086(14) -0.0049(17) C51 0.0581(17) 0.061(2) 0.0680(19) 0.0069(17) 0.0070(15) 0.0047(18) C56 0.0649(17) 0.0596(18) 0.0459(15) 0.0075(15) 0.0070(13) 0.0199(16) C63 0.0631(18) 0.090(3) 0.0476(15) 0.0135(18) 0.0030(14) 0.011(2) C4 0.0510(16) 0.059(2) 0.076(2) 0.0024(18) 0.0094(15) -0.0046(17) C58 0.077(2) 0.088(2) 0.0464(15) 0.0165(17) 0.0112(15) 0.025(2) C52 0.0597(17) 0.071(2) 0.0546(16) 0.0089(17) 0.0009(14) -0.0038(18) C6' 0.0561(17) 0.067(2) 0.088(2) -0.011(2) 0.0202(16) -0.0042(18) C2' 0.0502(16) 0.070(2) 0.0560(16) -0.0120(16) 0.0091(14) -0.0079(17) C5 0.0514(16) 0.067(2) 0.072(2) 0.0007(18) 0.0019(15) 0.0040(17) C26 0.0587(19) 0.090(3) 0.075(2) 0.006(2) 0.0089(17) 0.004(2) C14 0.0505(16) 0.080(2) 0.084(2) -0.009(2) 0.0136(16) -0.0133(18) C40 0.0588(18) 0.082(3) 0.084(2) 0.000(2) 0.0145(17) -0.0140(19) C24 0.067(2) 0.084(3) 0.0649(19) 0.006(2) 0.0118(16) 0.007(2) C62 0.0586(18) 0.098(3) 0.0556(17) 0.0239(18) 0.0051(15) 0.0157(19) C15 0.0631(19) 0.080(2) 0.0556(17) 0.0022(18) 0.0004(15) -0.006(2) C39 0.0583(17) 0.079(2) 0.0618(18) -0.0076(18) 0.0120(15) -0.0099(19) C41 0.0656(19) 0.073(2) 0.0655(19) -0.0113(18) 0.0049(16) -0.0135(19) C13 0.0696(19) 0.087(3) 0.0567(17) -0.0013(19) 0.0179(15) -0.005(2) C57 0.0647(18) 0.084(2) 0.0477(15) 0.0129(17) 0.0093(14) 0.0137(19) C8' 0.097(2) 0.095(3) 0.0491(16) -0.011(2) 0.0204(17) -0.011(3) C6 0.0589(19) 0.076(2) 0.088(2) 0.002(2) 0.0067(18) 0.005(2) C55 0.077(2) 0.077(2) 0.0478(16) 0.0083(17) 0.0070(15) 0.008(2) C18 0.068(2) 0.110(3) 0.0540(18) -0.008(2) 0.0024(16) -0.002(2) C7' 0.074(2) 0.091(3) 0.074(2) -0.014(2) 0.0301(16) -0.008(2) C65 0.063(2) 0.158(4) 0.0556(19) 0.005(3) 0.0013(17) 0.002(3) C8 0.107(3) 0.097(3) 0.081(2) 0.016(2) 0.014(2) 0.027(3) C64 0.073(2) 0.139(4) 0.0594(19) 0.032(2) 0.0060(17) 0.018(3) C36 0.059(2) 0.093(3) 0.096(3) 0.016(2) 0.0053(19) -0.012(2) C17 0.0642(19) 0.088(3) 0.0537(17) -0.0071(19) 0.0041(15) -0.007(2) C70 0.0891(12) 0.1486(13) 0.0947(12) 0.0405(12) 0.0154(11) -0.0043(12) C68 0.0671(16) 0.191(4) 0.0724(17) -0.002(2) 0.0078(14) 0.027(2) C29 0.081(3) 0.136(4) 0.082(2) 0.024(3) 0.010(2) 0.000(3) C27 0.093(3) 0.116(4) 0.108(3) 0.027(3) -0.005(3) -0.028(3) C12 0.096(3) 0.072(3) 0.123(3) 0.013(3) 0.029(2) -0.015(2) C67 0.065(2) 0.150(4) 0.062(2) 0.010(3) 0.0039(17) 0.004(3) C71 0.0891(12) 0.1486(13) 0.0947(12) 0.0405(12) 0.0154(11) -0.0043(12) C9 0.100(3) 0.101(3) 0.085(3) -0.014(3) 0.002(2) 0.026(3) C28 0.075(2) 0.107(3) 0.081(2) 0.011(2) 0.006(2) -0.010(2) C72 0.0926(13) 0.1475(14) 0.0986(13) 0.0383(13) 0.0132(12) -0.0056(13) C7 0.076(2) 0.117(4) 0.077(2) -0.017(2) 0.002(2) 0.012(3) C11 0.109(3) 0.152(4) 0.114(3) -0.048(3) -0.037(3) 0.058(3) C34 0.0952(10) 0.2345(10) 0.1104(10) 0.0607(10) -0.0197(9) -0.0790(10) C38 0.112(3) 0.081(3) 0.128(3) 0.001(3) 0.043(3) 0.003(3) C35 0.0911(12) 0.2328(14) 0.1070(13) 0.0606(13) -0.0178(12) -0.0797(13) C10 0.135(4) 0.148(4) 0.088(3) -0.015(3) 0.015(3) 0.057(3) C30 0.100(3) 0.177(5) 0.098(3) 0.053(3) -0.017(3) -0.012(4) C37 0.090(3) 0.116(4) 0.125(3) 0.022(3) -0.016(3) -0.039(3) C25 0.083(3) 0.095(3) 0.107(3) -0.012(3) 0.016(2) 0.020(3) C73 0.112(4) 0.173(6) 0.118(4) 0.028(4) 0.013(3) -0.027(4) C69 0.0671(16) 0.191(4) 0.0724(17) -0.002(2) 0.0078(14) 0.027(2) C66 0.091(3) 0.262(8) 0.088(3) -0.017(4) -0.008(3) -0.039(4) C33 0.0983(13) 0.2370(14) 0.1126(13) 0.0597(13) -0.0244(12) -0.0772(13) C32 0.151(4) 0.308(8) 0.105(4) 0.058(4) -0.028(3) -0.128(4) C31 0.135(5) 0.317(8) 0.155(4) 0.145(4) -0.032(4) -0.060(5) 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' 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 C75 O7 H7 109.5 . . ? C50 O13 H13 109.5 . . ? C1' O3 H3 109.5 . . ? C20 N2 H2 117.7 . . ? C20 N2 C21 124.7(3) . . ? C21 N2 H2 117.7 . . ? C1 N1 H1 118.2 . . ? C2' N1 H1 118.2 . . ? C2' N1 C1 123.6(3) . . ? C63 O16 H16 109.5 . . ? C43 O12 H12 109.5 . . ? C46 N3 H3A 117.6 . . ? C45 N3 H3A 117.6 . . ? C45 N3 C46 124.9(3) . . ? C53 O15 H15A 109.5 . . ? C13 O6 H6A 109.5 . . ? O13 C50 C49 122.4(3) . . ? O13 C50 C51 118.7(3) . . ? C49 C50 C51 119.0(3) . . ? C7' O4 H4 109.5 . . ? C45 C44 C47 120.4(3) . . ? C45 C44 C43 115.5(3) . . ? C43 C44 C47 124.1(3) . . ? C61 N4 H4B 118.1 . . ? C60 N4 H4B 118.1 . . ? C60 N4 C61 123.8(3) . . ? O2 C3 C2 119.6(3) . . ? O2 C3 C4 118.2(3) . . ? C2 C3 C4 122.2(3) . . ? C1' C2 C3 118.6(3) . . ? C1' C2 C1 119.5(3) . . ? C1 C2 C3 121.9(3) . . ? N2 C20 H20 118.2 . . ? N2 C20 C19 123.5(3) . . ? C19 C20 H20 118.2 . . ? O18 C61 N4 118.0(3) . . ? O18 C61 C62 126.4(3) . . ? N4 C61 C62 115.5(3) . . ? O7 C75 C19 115.8(3) . . ? O7 C75 C74 120.5(3) . . ? C74 C75 C19 123.7(3) . . ? C20 C19 C75 114.3(3) . . ? C20 C19 C16 121.2(3) . . ? C75 C19 C16 124.6(3) . . ? O3 C1' C2 120.7(3) . . ? O3 C1' C3' 116.9(3) . . ? C2 C1' C3' 122.4(3) . . ? O10 C46 N3 118.8(3) . . ? O10 C46 C42 124.8(3) . . ? N3 C46 C42 116.4(3) . . ? O1 C1 N1 118.8(3) . . ? O1 C1 C2 126.2(3) . . ? N1 C1 C2 115.0(3) . . ? C5' C4' C9' 117.6(3) . . ? C5' C4' C3' 120.1(3) . . ? C9' C4' C3' 122.4(3) . . ? C48 C47 C44 121.9(3) . . ? C52 C47 C44 120.9(3) . . ? C52 C47 C48 117.1(3) . . ? N3 C45 C44 122.2(3) . . ? N3 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? N4 C60 H60 117.9 . . ? N4 C60 C59 124.2(3) . . ? C59 C60 H60 117.9 . . ? C50 C49 H49 119.7 . . ? C50 C49 C48 120.6(3) . . ? C48 C49 H49 119.7 . . ? C47 C48 C49 121.1(3) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? O15 C53 C54 121.6(3) . . ? O15 C53 C58 118.9(3) . . ? C58 C53 C54 119.4(3) . . ? C15 C16 C19 120.2(3) . . ? C15 C16 C17 117.2(3) . . ? C17 C16 C19 122.4(3) . . ? N2 C21 C74 115.1(3) . . ? O8 C21 N2 118.1(3) . . ? O8 C21 C74 126.8(3) . . ? C43 C42 C46 117.2(3) . . ? C43 C42 C41 119.4(3) . . ? C41 C42 C46 123.4(3) . . ? O9 C22 C74 118.4(3) . . ? O9 C22 C23 118.4(3) . . ? C74 C22 C23 122.8(3) . . ? C4' C5' H5' 119.5 . . ? C6' C5' C4' 121.0(3) . . ? C6' C5' H5' 119.5 . . ? O12 C43 C44 115.8(3) . . ? O12 C43 C42 120.5(3) . . ? C44 C43 C42 123.7(3) . . ? C4' C9' H9' 119.8 . . ? C8' C9' C4' 120.5(3) . . ? C8' C9' H9' 119.8 . . ? C75 C74 C21 118.5(3) . . ? C75 C74 C22 119.2(3) . . ? C21 C74 C22 122.2(3) . . ? C60 C59 C56 120.5(3) . . ? C60 C59 C63 113.9(3) . . ? C63 C59 C56 125.6(3) . . ? C53 C54 H54 120.3 . . ? C55 C54 C53 119.4(3) . . ? C55 C54 H54 120.3 . . ? C22 C23 H23 109.5 . . ? C22 C23 C24 104.7(3) . . ? C22 C23 C25 111.7(3) . . ? C24 C23 H23 109.5 . . ? C25 C23 H23 109.5 . . ? C25 C23 C24 111.8(3) . . ? C1' C3' C4' 125.0(3) . . ? C2' C3' C1' 114.1(3) . . ? C2' C3' C4' 120.9(3) . . ? C50 C51 H51 119.9 . . ? C52 C51 C50 120.1(3) . . ? C52 C51 H51 119.9 . . ? C57 C56 C59 122.6(3) . . ? C55 C56 C59 121.2(3) . . ? C55 C56 C57 116.2(3) . . ? O16 C63 C59 115.7(3) . . ? O16 C63 C62 122.2(3) . . ? C62 C63 C59 122.1(3) . . ? C3 C4 H4A 108.9 . . ? C3 C4 C5 107.0(3) . . ? C3 C4 C12 110.4(3) . . ? C5 C4 H4A 108.9 . . ? C12 C4 H4A 108.9 . . ? C12 C4 C5 112.7(3) . . ? C53 C58 H58 119.7 . . ? C53 C58 C57 120.7(3) . . ? C57 C58 H58 119.7 . . ? C47 C52 H52 119.0 . . ? C51 C52 C47 122.1(3) . . ? C51 C52 H52 119.0 . . ? C5' C6' H6' 119.8 . . ? C7' C6' C5' 120.3(3) . . ? C7' C6' H6' 119.9 . . ? N1 C2' C3' 124.8(3) . . ? N1 C2' H2' 117.6 . . ? C3' C2' H2' 117.6 . . ? C4 C5 H5A 107.9 . . ? C4 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C6 C5 C4 117.5(3) . . ? C6 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C24 C26 H26 109.1 . . ? C24 C26 C27 107.8(3) . . ? C24 C26 C28 111.9(3) . . ? C27 C26 H26 109.1 . . ? C28 C26 H26 109.1 . . ? C28 C26 C27 109.7(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C13 C14 C15 120.6(3) . . ? H40A C40 H40B 107.2 . . ? C39 C40 H40A 107.8 . . ? C39 C40 H40B 107.8 . . ? C39 C40 C36 118.0(3) . . ? C36 C40 H40A 107.8 . . ? C36 C40 H40B 107.8 . . ? C23 C24 H24A 107.9 . . ? C23 C24 H24B 107.9 . . ? C26 C24 C23 117.5(3) . . ? C26 C24 H24A 107.9 . . ? C26 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? C61 C62 C64 120.8(3) . . ? C63 C62 C61 120.2(3) . . ? C63 C62 C64 118.8(3) . . ? C16 C15 H15 119.3 . . ? C14 C15 C16 121.4(3) . . ? C14 C15 H15 119.3 . . ? C40 C39 H39 107.9 . . ? C41 C39 C40 110.4(3) . . ? C41 C39 H39 107.9 . . ? C41 C39 C38 109.0(3) . . ? C38 C39 C40 113.5(3) . . ? C38 C39 H39 107.9 . . ? O11 C41 C42 118.7(3) . . ? O11 C41 C39 115.9(3) . . ? C42 C41 C39 125.4(3) . . ? O6 C13 C14 118.0(3) . . ? O6 C13 C18 123.7(3) . . ? C18 C13 C14 118.4(3) . . ? C56 C57 H57 119.5 . . ? C58 C57 C56 121.1(3) . . ? C58 C57 H57 119.5 . . ? C9' C8' H8' 119.8 . . ? C9' C8' C7' 120.4(3) . . ? C7' C8' H8' 119.8 . . ? C5 C6 H6 108.6 . . ? C5 C6 C7 110.0(3) . . ? C7 C6 H6 108.6 . . ? C11 C6 C5 111.7(3) . . ? C11 C6 H6 108.6 . . ? C11 C6 C7 109.1(4) . . ? C54 C55 C56 123.2(3) . . ? C54 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C13 C18 H18 119.1 . . ? C13 C18 C17 121.8(3) . . ? C17 C18 H18 119.1 . . ? C6' C7' O4 120.2(3) . . ? C6' C7' C8' 120.3(3) . . ? C8' C7' O4 119.3(3) . . ? C64 C65 H65 109.2 . . ? C64 C65 C67 105.9(4) . . ? C64 C65 C66 110.5(3) . . ? C67 C65 H65 109.2 . . ? C67 C65 C66 112.6(4) . . ? C66 C65 H65 109.2 . . ? C9 C8 H8 116.7 . . ? C9 C8 C7 126.6(4) . . ? C7 C8 H8 116.7 . . ? O17 C64 C62 116.6(4) . . ? O17 C64 C65 119.3(3) . . ? C65 C64 C62 124.0(3) . . ? C40 C36 H36 108.3 . . ? C40 C36 C35 113.1(3) . . ? C40 C36 C37 109.8(3) . . ? C35 C36 H36 108.3 . . ? C35 C36 C37 108.8(4) . . ? C37 C36 H36 108.3 . . ? C16 C17 H17 119.8 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? H70A C70 H70B 107.2 . . ? C68 C70 H70A 108.0 . . ? C68 C70 H70B 108.0 . . ? C71 C70 H70A 108.0 . . ? C71 C70 H70B 108.0 . . ? C71 C70 C68 117.2(4) . . ? C70 C68 H68 109.0 . . ? C70 C68 C67 111.8(4) . . ? C70 C68 C69 110.5(3) . . ? C67 C68 H68 109.0 . . ? C67 C68 C69 107.4(4) . . ? C69 C68 H68 109.0 . . ? C28 C29 H29 115.9 . . ? C30 C29 H29 115.9 . . ? C30 C29 C28 128.3(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C65 C67 C68 114.0(4) . . ? C65 C67 H67A 108.7 . . ? C65 C67 H67B 108.7 . . ? C68 C67 H67A 108.7 . . ? C68 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? C70 C71 H71 114.2 . . ? C72 C71 C70 131.5(5) . . ? C72 C71 H71 114.2 . . ? C8 C9 H9 118.6 . . ? C8 C9 C10 122.8(5) . . ? C10 C9 H9 118.6 . . ? C26 C28 H28A 108.3 . . ? C26 C28 H28B 108.2 . . ? C29 C28 C26 116.1(3) . . ? C29 C28 H28A 108.3 . . ? C29 C28 H28B 108.2 . . ? H28A C28 H28B 107.4 . . ? C71 C72 H72 113.7 . . ? C71 C72 C73 132.6(5) . . ? C73 C72 H72 113.7 . . ? C6 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 C6 114.3(3) . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C35 C34 H34 111.7 . . ? C33 C34 H34 111.6 . . ? C33 C34 C35 136.7(7) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? C34 C35 C36 115.0(4) . . ? C34 C35 H35A 108.5 . . ? C34 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C29 C30 H30 115.3 . . ? C29 C30 C31 129.5(6) . . ? C31 C30 H30 115.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66B 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C34 C33 H33 112.0 . . ? C34 C33 C32 135.9(7) . . ? C32 C33 H33 112.0 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 O1 C1 1.233(4) . ? O7 H7 0.8200 . ? O7 C75 1.339(4) . ? O13 H13 0.8200 . ? O13 C50 1.350(3) . ? O2 C3 1.248(4) . ? O3 H3 0.8200 . ? O3 C1' 1.316(4) . ? O18 C61 1.257(4) . ? N2 H2 0.8600 . ? N2 C20 1.351(4) . ? N2 C21 1.368(4) . ? N1 H1 0.8600 . ? N1 C1 1.375(4) . ? N1 C2' 1.342(4) . ? O10 C46 1.260(4) . ? O8 C21 1.236(4) . ? O16 H16 0.8200 . ? O16 C63 1.326(4) . ? O12 H12 0.8200 . ? O12 C43 1.336(4) . ? N3 H3A 0.8600 . ? N3 C46 1.357(4) . ? N3 C45 1.349(4) . ? O15 H15A 0.8200 . ? O15 C53 1.358(4) . ? O9 C22 1.242(4) . ? O6 H6A 0.8200 . ? O6 C13 1.357(4) . ? O11 C41 1.262(4) . ? C50 C49 1.376(5) . ? C50 C51 1.383(4) . ? O4 H4 0.8200 . ? O4 C7' 1.399(4) . ? C44 C47 1.475(4) . ? C44 C45 1.370(4) . ? C44 C43 1.409(4) . ? N4 H4B 0.8600 . ? N4 C61 1.354(4) . ? N4 C60 1.348(4) . ? C3 C2 1.472(4) . ? C3 C4 1.523(5) . ? C2 C1' 1.415(4) . ? C2 C1 1.437(4) . ? C20 H20 0.9300 . ? C20 C19 1.354(4) . ? C61 C62 1.426(5) . ? C75 C19 1.424(4) . ? C75 C74 1.395(4) . ? C19 C16 1.473(4) . ? C1' C3' 1.418(4) . ? C46 C42 1.450(4) . ? C4' C5' 1.397(4) . ? C4' C9' 1.396(4) . ? C4' C3' 1.476(4) . ? C47 C48 1.391(4) . ? C47 C52 1.386(4) . ? C45 H45 0.9300 . ? C60 H60 0.9300 . ? C60 C59 1.361(4) . ? C49 H49 0.9300 . ? C49 C48 1.389(4) . ? O17 C64 1.274(5) . ? C48 H48 0.9300 . ? C53 C54 1.389(5) . ? C53 C58 1.366(5) . ? C16 C15 1.389(4) . ? C16 C17 1.397(4) . ? C21 C74 1.444(4) . ? C42 C43 1.409(4) . ? C42 C41 1.456(5) . ? C22 C74 1.472(4) . ? C22 C23 1.491(4) . ? C5' H5' 0.9300 . ? C5' C6' 1.380(5) . ? C9' H9' 0.9300 . ? C9' C8' 1.371(5) . ? C59 C56 1.465(4) . ? C59 C63 1.436(5) . ? C54 H54 0.9300 . ? C54 C55 1.363(5) . ? C23 H23 0.9800 . ? C23 C24 1.546(5) . ? C23 C25 1.510(5) . ? C3' C2' 1.372(4) . ? C51 H51 0.9300 . ? C51 C52 1.378(4) . ? C56 C57 1.399(4) . ? C56 C55 1.391(5) . ? C63 C62 1.383(5) . ? C4 H4A 0.9800 . ? C4 C5 1.540(5) . ? C4 C12 1.527(5) . ? C58 H58 0.9300 . ? C58 C57 1.388(5) . ? C52 H52 0.9300 . ? C6' H6' 0.9300 . ? C6' C7' 1.346(5) . ? C2' H2' 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.520(5) . ? C26 H26 0.9800 . ? C26 C24 1.528(5) . ? C26 C27 1.551(6) . ? C26 C28 1.542(5) . ? C14 H14 0.9300 . ? C14 C15 1.381(5) . ? C14 C13 1.377(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 C39 1.524(5) . ? C40 C36 1.525(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C62 C64 1.494(5) . ? C15 H15 0.9300 . ? C39 H39 0.9800 . ? C39 C41 1.505(5) . ? C39 C38 1.509(6) . ? C13 C18 1.368(5) . ? C57 H57 0.9300 . ? C8' H8' 0.9300 . ? C8' C7' 1.381(5) . ? C6 H6 0.9800 . ? C6 C7 1.562(5) . ? C6 C11 1.493(6) . ? C55 H55 0.9300 . ? C18 H18 0.9300 . ? C18 C17 1.376(5) . ? C65 H65 0.9800 . ? C65 C64 1.489(6) . ? C65 C67 1.525(6) . ? C65 C66 1.561(6) . ? C8 H8 0.9300 . ? C8 C9 1.306(7) . ? C8 C7 1.489(5) . ? C36 H36 0.9800 . ? C36 C35 1.550(6) . ? C36 C37 1.551(6) . ? C17 H17 0.9300 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 C68 1.512(7) . ? C70 C71 1.502(6) . ? C68 H68 0.9800 . ? C68 C67 1.541(6) . ? C68 C69 1.547(7) . ? C29 H29 0.9300 . ? C29 C28 1.438(6) . ? C29 C30 1.279(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C71 H71 0.9300 . ? C71 C72 1.184(8) . ? C9 H9 0.9300 . ? C9 C10 1.505(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C72 H72 0.9300 . ? C72 C73 1.504(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C34 H34 0.9300 . ? C34 C35 1.475(6) . ? C34 C33 1.153(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C30 H30 0.9300 . ? C30 C31 1.527(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C33 H33 0.9300 . ? C33 C32 1.497(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 O7 C75 C19 C20 176.1(3) . . . . ? O7 C75 C19 C16 -4.2(5) . . . . ? O7 C75 C74 C21 -176.3(3) . . . . ? O7 C75 C74 C22 1.7(5) . . . . ? O13 C50 C49 C48 -179.7(3) . . . . ? O13 C50 C51 C52 179.9(3) . . . . ? O2 C3 C2 C1' 7.4(5) . . . . ? O2 C3 C2 C1 -172.2(3) . . . . ? O2 C3 C4 C5 84.8(4) . . . . ? O2 C3 C4 C12 -38.2(4) . . . . ? O3 C1' C3' C4' 1.0(5) . . . . ? O3 C1' C3' C2' 178.1(3) . . . . ? O18 C61 C62 C63 -177.6(4) . . . . ? O18 C61 C62 C64 6.2(6) . . . . ? N2 C20 C19 C75 0.4(5) . . . . ? N2 C20 C19 C16 -179.3(3) . . . . ? N2 C21 C74 C75 0.1(5) . . . . ? N2 C21 C74 C22 -177.8(3) . . . . ? O10 C46 C42 C43 174.4(3) . . . . ? O10 C46 C42 C41 -7.0(6) . . . . ? O8 C21 C74 C75 178.6(4) . . . . ? O8 C21 C74 C22 0.6(6) . . . . ? O16 C63 C62 C61 175.0(4) . . . . ? O16 C63 C62 C64 -8.8(6) . . . . ? N3 C46 C42 C43 -4.4(5) . . . . ? N3 C46 C42 C41 174.2(3) . . . . ? O15 C53 C54 C55 -177.3(4) . . . . ? O15 C53 C58 C57 178.5(3) . . . . ? O9 C22 C74 C75 -5.9(5) . . . . ? O9 C22 C74 C21 172.0(3) . . . . ? O9 C22 C23 C24 84.6(4) . . . . ? O9 C22 C23 C25 -36.7(5) . . . . ? O6 C13 C18 C17 177.3(4) . . . . ? C50 C49 C48 C47 0.3(6) . . . . ? C50 C51 C52 C47 -0.8(5) . . . . ? C44 C47 C48 C49 177.1(3) . . . . ? C44 C47 C52 C51 -176.8(3) . . . . ? N4 C61 C62 C63 2.4(5) . . . . ? N4 C61 C62 C64 -173.8(4) . . . . ? N4 C60 C59 C56 -179.2(3) . . . . ? N4 C60 C59 C63 -1.3(5) . . . . ? C3 C2 C1' O3 -3.8(5) . . . . ? C3 C2 C1' C3' 173.6(3) . . . . ? C3 C2 C1 O1 9.9(5) . . . . ? C3 C2 C1 N1 -171.0(3) . . . . ? C3 C4 C5 C6 174.9(3) . . . . ? C2 C3 C4 C5 -98.3(4) . . . . ? C2 C3 C4 C12 138.8(3) . . . . ? C2 C1' C3' C4' -176.5(3) . . . . ? C2 C1' C3' C2' 0.6(5) . . . . ? C20 N2 C21 O8 177.8(3) . . . . ? C20 N2 C21 C74 -3.6(5) . . . . ? C20 C19 C16 C15 -44.6(5) . . . . ? C20 C19 C16 C17 129.6(4) . . . . ? C61 N4 C60 C59 -1.6(6) . . . . ? C61 C62 C64 O17 -174.8(4) . . . . ? C61 C62 C64 C65 1.5(7) . . . . ? C75 C19 C16 C15 135.8(4) . . . . ? C75 C19 C16 C17 -50.1(5) . . . . ? C19 C75 C74 C21 3.7(5) . . . . ? C19 C75 C74 C22 -178.3(3) . . . . ? C19 C16 C15 C14 175.3(3) . . . . ? C19 C16 C17 C18 -176.1(4) . . . . ? C1' C2 C1 O1 -169.7(3) . . . . ? C1' C2 C1 N1 9.4(4) . . . . ? C1' C3' C2' N1 2.7(5) . . . . ? C46 N3 C45 C44 -0.8(5) . . . . ? C46 C42 C43 O12 179.6(3) . . . . ? C46 C42 C43 C44 2.8(5) . . . . ? C46 C42 C41 O11 176.6(4) . . . . ? C46 C42 C41 C39 -2.2(6) . . . . ? C1 N1 C2' C3' 0.4(5) . . . . ? C1 C2 C1' O3 175.8(3) . . . . ? C1 C2 C1' C3' -6.8(5) . . . . ? C4' C5' C6' C7' 0.7(6) . . . . ? C4' C9' C8' C7' 0.4(6) . . . . ? C4' C3' C2' N1 180.0(3) . . . . ? C47 C44 C45 N3 179.2(3) . . . . ? C47 C44 C43 O12 2.7(5) . . . . ? C47 C44 C43 C42 179.6(3) . . . . ? C45 N3 C46 O10 -175.2(3) . . . . ? C45 N3 C46 C42 3.7(5) . . . . ? C45 C44 C47 C48 -131.6(4) . . . . ? C45 C44 C47 C52 46.2(5) . . . . ? C45 C44 C43 O12 -177.0(3) . . . . ? C45 C44 C43 C42 -0.1(5) . . . . ? C60 N4 C61 O18 -178.9(3) . . . . ? C60 N4 C61 C62 1.1(5) . . . . ? C60 C59 C56 C57 -152.8(3) . . . . ? C60 C59 C56 C55 27.3(5) . . . . ? C60 C59 C63 O16 -175.6(3) . . . . ? C60 C59 C63 C62 4.9(5) . . . . ? C49 C50 C51 C52 0.2(5) . . . . ? C48 C47 C52 C51 1.0(5) . . . . ? C53 C54 C55 C56 -1.6(6) . . . . ? C53 C58 C57 C56 -0.8(6) . . . . ? C21 N2 C20 C19 3.5(6) . . . . ? C22 C23 C24 C26 171.4(3) . . . . ? C5' C4' C9' C8' 0.1(6) . . . . ? C5' C4' C3' C1' 140.1(4) . . . . ? C5' C4' C3' C2' -36.8(5) . . . . ? C5' C6' C7' O4 174.6(3) . . . . ? C5' C6' C7' C8' -0.2(6) . . . . ? C43 C44 C47 C48 48.7(5) . . . . ? C43 C44 C47 C52 -133.5(4) . . . . ? C43 C44 C45 N3 -1.1(5) . . . . ? C43 C42 C41 O11 -4.8(5) . . . . ? C43 C42 C41 C39 176.4(4) . . . . ? C9' C4' C5' C6' -0.6(5) . . . . ? C9' C4' C3' C1' -40.6(5) . . . . ? C9' C4' C3' C2' 142.4(4) . . . . ? C9' C8' C7' O4 -175.2(4) . . . . ? C9' C8' C7' C6' -0.4(7) . . . . ? C74 C75 C19 C20 -3.9(5) . . . . ? C74 C75 C19 C16 175.8(3) . . . . ? C74 C22 C23 C24 -88.1(4) . . . . ? C74 C22 C23 C25 150.7(3) . . . . ? C59 C56 C57 C58 -178.6(3) . . . . ? C59 C56 C55 C54 179.8(3) . . . . ? C59 C63 C62 C61 -5.6(6) . . . . ? C59 C63 C62 C64 170.7(4) . . . . ? C54 C53 C58 C57 -1.0(6) . . . . ? C23 C22 C74 C75 166.8(3) . . . . ? C23 C22 C74 C21 -15.3(5) . . . . ? C3' C4' C5' C6' 178.7(3) . . . . ? C3' C4' C9' C8' -179.2(4) . . . . ? C51 C50 C49 C48 0.0(5) . . . . ? C56 C59 C63 O16 2.1(5) . . . . ? C56 C59 C63 C62 -177.4(3) . . . . ? C63 C59 C56 C57 29.6(5) . . . . ? C63 C59 C56 C55 -150.3(4) . . . . ? C63 C62 C64 O17 9.0(6) . . . . ? C63 C62 C64 C65 -174.7(4) . . . . ? C4 C3 C2 C1' -169.5(3) . . . . ? C4 C3 C2 C1 10.9(5) . . . . ? C4 C5 C6 C7 -67.3(4) . . . . ? C4 C5 C6 C11 171.3(3) . . . . ? C58 C53 C54 C55 2.1(6) . . . . ? C52 C47 C48 C49 -0.8(5) . . . . ? C2' N1 C1 O1 172.6(3) . . . . ? C2' N1 C1 C2 -6.5(5) . . . . ? C5 C6 C7 C8 174.1(4) . . . . ? C14 C13 C18 C17 -3.1(7) . . . . ? C40 C39 C41 O11 31.8(5) . . . . ? C40 C39 C41 C42 -149.4(4) . . . . ? C40 C36 C35 C34 171.0(5) . . . . ? C24 C26 C28 C29 177.1(4) . . . . ? C15 C16 C17 C18 -1.8(6) . . . . ? C15 C14 C13 O6 -178.3(4) . . . . ? C15 C14 C13 C18 2.0(6) . . . . ? C39 C40 C36 C35 -60.0(5) . . . . ? C39 C40 C36 C37 178.2(3) . . . . ? C41 C42 C43 O12 1.0(5) . . . . ? C41 C42 C43 C44 -175.8(3) . . . . ? C13 C14 C15 C16 -1.0(6) . . . . ? C13 C18 C17 C16 3.0(6) . . . . ? C57 C56 C55 C54 -0.1(5) . . . . ? C55 C56 C57 C58 1.3(5) . . . . ? C64 C65 C67 C68 171.2(3) . . . . ? C36 C40 C39 C41 177.0(3) . . . . ? C36 C40 C39 C38 -60.2(4) . . . . ? C17 C16 C15 C14 0.9(6) . . . . ? C70 C68 C67 C65 -64.0(5) . . . . ? C70 C71 C72 C73 -177.9(5) . . . . ? C68 C70 C71 C72 -130.6(6) . . . . ? C27 C26 C24 C23 172.4(3) . . . . ? C27 C26 C28 C29 -63.4(5) . . . . ? C12 C4 C5 C6 -63.5(4) . . . . ? C67 C65 C64 O17 88.8(5) . . . . ? C67 C65 C64 C62 -87.4(5) . . . . ? C71 C70 C68 C67 176.6(4) . . . . ? C71 C70 C68 C69 -63.8(6) . . . . ? C9 C8 C7 C6 121.9(5) . . . . ? C28 C26 C24 C23 -66.9(4) . . . . ? C28 C29 C30 C31 -174.2(5) . . . . ? C7 C8 C9 C10 179.4(4) . . . . ? C11 C6 C7 C8 -63.0(5) . . . . ? C38 C39 C41 O11 -93.6(4) . . . . ? C38 C39 C41 C42 85.2(4) . . . . ? C35 C34 C33 C32 179.5(6) . . . . ? C30 C29 C28 C26 111.0(6) . . . . ? C37 C36 C35 C34 -66.7(6) . . . . ? C25 C23 C24 C26 -67.4(4) . . . . ? C69 C68 C67 C65 174.6(3) . . . . ? C66 C65 C64 O17 -33.5(7) . . . . ? C66 C65 C64 C62 150.3(5) . . . . ? C66 C65 C67 C68 -67.9(5) . . . . ? C33 C34 C35 C36 121.2(7) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.283 -0.015 0.791 210.4 37.3 ? 2 0.283 0.101 0.209 210.4 37.3 ? 3 0.173 0.425 0.642 9.5 0.0 ? 4 0.827 0.925 0.358 9.5 0.0 ?