#------------------------------------------------------------------------------ #$Date: 2020-06-05 14:32:12 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252929 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157500.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_7157500 loop_ _publ_author_name 'Peng, Xiaogang' 'Duan, Fangfang' 'He, Yangzhou' 'Gao, Ying' 'Chen, Juan' 'Chang, Jinling' 'Ruan, Hanli' _publ_section_title ; Ergocytochalasin A, a polycyclic merocytochalasan from an endophytic fungus Phoma multirostrata XJ-2-1. ; _journal_issue 21 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4056 _journal_page_last 4062 _journal_paper_doi 10.1039/d0ob00701c _journal_volume 18 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C57 H77 N O6' _chemical_formula_sum 'C57 H77 N O6' _chemical_formula_weight 872.19 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-05-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-14 deposited with the CCDC. 2020-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0080(10) _cell_length_b 13.0066(10) _cell_length_c 34.139(2) _cell_measurement_reflns_used 45737 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.5460 _cell_measurement_theta_min 3.6210 _cell_volume 5331.9(7) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 -17.00 9.00 0.50 0.50 -- 0.00 -82.00 120.00 52 2 \w -89.00 -37.00 0.50 0.50 -- 0.00 -38.00 90.00 104 3 \w -32.00 30.00 0.50 0.50 -- 0.00 -82.00-180.00 124 4 \w -31.00 30.00 0.50 0.50 -- 0.00 -82.00 60.00 122 5 \w -43.00 1.00 0.50 0.50 -- 0.00 -77.00 -90.00 88 6 \w -45.00 -13.00 0.50 0.50 -- 0.00 -77.00 -30.00 64 7 \w -13.00 12.00 0.50 0.50 -- 0.00 -38.00 90.00 50 8 \w 55.00 105.00 0.50 1.00 -- 94.60 -82.00 -30.00 100 9 \w 71.00 175.00 0.50 1.00 -- 94.60 15.00 -30.00 208 10 \w 67.00 111.00 0.50 1.00 -- 94.60 -30.00 -30.00 88 11 \w 47.00 118.00 0.50 1.00 -- 94.60 -61.00 90.00 142 12 \w 7.00 117.00 0.50 1.00 -- 94.60 -61.00-120.00 220 13 \w 18.00 44.00 0.50 1.00 -- 94.60 -61.00 90.00 52 14 \w 13.00 107.00 0.50 1.00 -- 94.60 -61.00 30.00 188 15 \w 5.00 31.00 0.50 1.00 -- 94.60 -82.00 90.00 52 16 \w 9.00 51.00 0.50 1.00 -- 94.60 -45.00-180.00 84 17 \w 6.00 94.00 0.50 1.00 -- 94.60 -15.00 60.00 176 18 \w 82.00 126.00 0.50 1.00 -- 94.60 -82.00 90.00 88 19 \w 19.00 121.00 0.50 1.00 -- 94.60 -82.00 30.00 204 20 \w 8.00 126.00 0.50 1.00 -- 94.60 -82.00-120.00 236 21 \w 84.00 174.00 0.50 1.00 -- 94.60 30.00 0.00 180 22 \w 70.00 105.00 0.50 1.00 -- 94.60 -82.00-150.00 70 23 \w 13.00 38.00 0.50 1.00 -- 94.60 -82.00 -60.00 50 24 \w 95.00 121.00 0.50 1.00 -- 94.60 -82.00 -60.00 52 25 \w 76.00 101.00 0.50 1.00 -- 94.60 -82.00 0.00 50 26 \w 16.00 41.00 0.50 1.00 -- 94.60 -30.00 -30.00 50 27 \w 84.00 110.00 0.50 1.00 -- 94.60 -82.00 150.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0138122000 _diffrn_orient_matrix_UB_12 -0.0515967000 _diffrn_orient_matrix_UB_13 0.0403243000 _diffrn_orient_matrix_UB_21 -0.0897576000 _diffrn_orient_matrix_UB_22 0.0717499000 _diffrn_orient_matrix_UB_23 0.0171203000 _diffrn_orient_matrix_UB_31 -0.0906395000 _diffrn_orient_matrix_UB_32 -0.0788553000 _diffrn_orient_matrix_UB_33 -0.0108158000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_unetI/netI 0.0122 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 56478 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 64.978 _diffrn_reflns_theta_max 64.978 _diffrn_reflns_theta_min 3.637 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (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 1.087 _exptl_crystal_description block _exptl_crystal_F_000 1896 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.332 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.033 _refine_ls_abs_structure_details ; Flack x determined using 3878 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.18(2) _refine_ls_extinction_coef 0.00076(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 587 _refine_ls_number_reflns 9055 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0362 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+1.8393P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.0958 _reflns_Friedel_coverage 0.792 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 8920 _reflns_number_total 9055 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 20190524_pms-41.res created by SHELXL-2014/7 TITL 20190524_pms-41_a.res in P2(1)2(1)2(1) REM Old TITL 20190524_PMS-41 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.132, Rweak 0.032, Alpha 0.001, Orientation as input REM Flack x = 0.144 ( 0.025 ) from Parsons' quotients REM Formula found by SHELXT: C60 N2 O7 CELL 1.54184 12.008 13.0066 34.1392 90 90 90 ZERR 4 0.001 0.001 0.002 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 228 308 4 24 EQIV $1 2-X,0.5+Y,1.5-Z EQIV $2 -1+X,+Y,+Z ISOR 0.01 0.02 C27 C28 L.S. 4 PLAN 20 SIZE 0.12 0.1 0.1 HTAB O1' O1_$1 HTAB O2 O1'_$2 BOND $H CONF BOND $H HTAB CONF list 4 ABIN fmap 2 53 acta OMIT -3 130 OMIT 4 0 7 OMIT 0 2 0 OMIT 1 9 0 OMIT 1 0 1 OMIT 5 0 23 OMIT 0 0 2 OMIT 0 0 12 OMIT 5 0 19 OMIT 4 0 3 OMIT 0 1 2 OMIT 1 0 5 REM REM REM WGHT 0.048500 1.839300 EXTI 0.000761 FVAR 0.49475 C1 1 0.699939 0.555154 0.749443 11.00000 0.03181 0.03402 = 0.02308 0.00580 0.00044 -0.00214 C1' 1 1.095288 0.808396 0.643965 11.00000 0.04049 0.03043 = 0.03025 0.00235 -0.00552 -0.00263 AFIX 23 H1'A 2 1.096303 0.853709 0.621401 11.00000 -1.20000 H1'B 2 1.028257 0.823436 0.658750 11.00000 -1.20000 AFIX 0 C2' 1 1.195984 0.832902 0.669545 11.00000 0.04326 0.03240 = 0.03474 0.00117 -0.00715 -0.00290 AFIX 23 H2'A 2 1.263529 0.826054 0.654181 11.00000 -1.20000 H2'B 2 1.191163 0.903389 0.678670 11.00000 -1.20000 AFIX 0 C3 1 0.804478 0.697640 0.772371 11.00000 0.03747 0.03166 = 0.01513 -0.00193 0.00244 -0.00182 AFIX 13 H3 2 0.769502 0.760680 0.782161 11.00000 -1.20000 AFIX 0 C3' 1 1.201065 0.761295 0.704226 11.00000 0.02980 0.03738 = 0.02368 -0.00128 -0.00163 0.00223 AFIX 13 H3' 2 1.133389 0.769051 0.719995 11.00000 -1.20000 AFIX 0 C4 1 0.810861 0.701135 0.726739 11.00000 0.02955 0.03073 = 0.01764 -0.00362 -0.00001 -0.00158 AFIX 13 H4 2 0.886243 0.681447 0.718693 11.00000 -1.20000 AFIX 0 C4' 1 1.210095 0.651715 0.689924 11.00000 0.03177 0.03462 = 0.02991 -0.00003 -0.00053 0.00426 AFIX 23 H4'A 2 1.280987 0.643007 0.676713 11.00000 -1.20000 H4'B 2 1.209266 0.605926 0.712349 11.00000 -1.20000 AFIX 0 C5 1 0.785281 0.808925 0.710056 11.00000 0.03390 0.02691 = 0.01575 -0.00367 0.00444 -0.00267 AFIX 13 H5 2 0.791138 0.803756 0.681492 11.00000 -1.20000 AFIX 0 C5' 1 1.118138 0.621206 0.662419 11.00000 0.03348 0.02849 = 0.02521 -0.00137 0.00108 0.00636 C6 1 0.667242 0.839703 0.719122 11.00000 0.03419 0.03199 = 0.01804 -0.00260 0.00224 -0.00239 C6' 1 1.070801 0.529237 0.665081 11.00000 0.03968 0.02898 = 0.02695 0.00226 -0.00045 0.00575 AFIX 43 H6' 2 1.090175 0.488708 0.686464 11.00000 -1.20000 AFIX 0 C7 1 0.578836 0.756866 0.712943 11.00000 0.03310 0.03358 = 0.01792 -0.00208 0.00123 -0.00365 AFIX 13 H7 2 0.548587 0.736804 0.738485 11.00000 -1.20000 AFIX 0 C7' 1 0.988926 0.485224 0.636609 11.00000 0.03913 0.02583 = 0.02528 -0.00064 0.00397 0.00132 AFIX 13 H7' 2 1.030573 0.435888 0.620605 11.00000 -1.20000 AFIX 0 C8 1 0.623348 0.660818 0.692252 11.00000 0.03368 0.02818 = 0.01686 0.00168 0.00086 -0.00529 AFIX 13 H8 2 0.645976 0.682305 0.665914 11.00000 -1.20000 AFIX 0 C8' 1 0.943130 0.563805 0.608615 11.00000 0.03864 0.02677 = 0.02187 -0.00032 0.00642 0.00071 C9 1 0.728960 0.617731 0.712602 11.00000 0.03335 0.02855 = 0.01599 -0.00301 0.00399 -0.00311 C9' 1 0.967601 0.675959 0.616069 11.00000 0.03715 0.02738 = 0.02253 0.00131 -0.00081 -0.00376 AFIX 13 H9' 2 0.920988 0.695129 0.638472 11.00000 -1.20000 AFIX 0 C10 1 0.919607 0.685197 0.790696 11.00000 0.03968 0.03935 = 0.02001 -0.00385 -0.00066 -0.00270 AFIX 23 H10A 2 0.952259 0.621750 0.781152 11.00000 -1.20000 H10B 2 0.966490 0.741345 0.781877 11.00000 -1.20000 AFIX 0 C10' 1 1.088903 0.696158 0.629321 11.00000 0.03910 0.02739 = 0.02099 0.00140 0.00060 -0.00227 C11 1 0.871659 0.887986 0.723239 11.00000 0.03592 0.03199 = 0.02943 -0.00662 0.00131 -0.00423 AFIX 137 H11A 2 0.862676 0.901358 0.750712 11.00000 -1.50000 H11B 2 0.861459 0.950628 0.708806 11.00000 -1.50000 H11C 2 0.945099 0.861632 0.718477 11.00000 -1.50000 AFIX 0 C11' 1 0.925525 0.741107 0.581874 11.00000 0.05016 0.03079 = 0.02993 0.00629 -0.00771 -0.01053 AFIX 23 H11D 2 0.976964 0.734983 0.560091 11.00000 -1.20000 H11E 2 0.923429 0.812741 0.589743 11.00000 -1.20000 AFIX 0 C12 1 0.635769 0.931767 0.731075 11.00000 0.03460 0.03349 = 0.03258 -0.00880 0.00198 -0.00226 AFIX 93 H12A 2 0.688379 0.983476 0.734474 11.00000 -1.20000 H12B 2 0.560989 0.944906 0.736095 11.00000 -1.20000 AFIX 0 C12' 1 0.808690 0.707768 0.568467 11.00000 0.05407 0.02659 = 0.03193 0.00734 -0.01328 -0.00933 AFIX 23 H12C 2 0.783226 0.753716 0.547957 11.00000 -1.20000 H12D 2 0.757401 0.713521 0.590308 11.00000 -1.20000 AFIX 0 C13 1 0.533643 0.581557 0.687104 11.00000 0.03530 0.03242 = 0.02231 0.00529 0.00005 -0.00686 AFIX 43 H13 2 0.493588 0.561778 0.709168 11.00000 -1.20000 AFIX 0 C13' 1 0.807310 0.595967 0.552960 11.00000 0.04580 0.03386 = 0.01806 0.00159 -0.00164 -0.00982 C14 1 0.507815 0.538103 0.653425 11.00000 0.04132 0.03510 = 0.02425 0.00185 0.00054 -0.00863 AFIX 43 H14 2 0.541960 0.564831 0.631195 11.00000 -1.20000 AFIX 0 C14' 1 0.872425 0.529928 0.581682 11.00000 0.04224 0.02755 = 0.02001 0.00029 0.00515 -0.00255 C15 1 0.428846 0.449757 0.647190 11.00000 0.04457 0.03536 = 0.02721 0.00143 -0.00211 -0.01218 AFIX 23 H15A 2 0.381749 0.463794 0.624734 11.00000 -1.20000 H15B 2 0.381384 0.442066 0.669994 11.00000 -1.20000 AFIX 0 C15' 1 0.827474 0.421326 0.583376 11.00000 0.04737 0.02539 = 0.02180 -0.00477 0.00307 -0.00371 AFIX 13 H15' 2 0.881569 0.372315 0.572730 11.00000 -1.20000 AFIX 0 C16 1 0.494785 0.348723 0.640215 11.00000 0.04318 0.03413 = 0.02846 -0.00055 -0.00156 -0.01238 AFIX 13 H16 2 0.565804 0.367947 0.628116 11.00000 -1.20000 AFIX 0 C16' 1 0.722535 0.426416 0.557427 11.00000 0.05067 0.02890 = 0.02000 -0.00421 0.00215 -0.00776 AFIX 23 H16A 2 0.662213 0.387441 0.569116 11.00000 -1.20000 H16B 2 0.737829 0.398698 0.531604 11.00000 -1.20000 AFIX 0 C17 1 0.521991 0.298086 0.679200 11.00000 0.06797 0.03611 = 0.02714 0.00120 0.00700 -0.00720 AFIX 23 H17A 2 0.453829 0.269535 0.689885 11.00000 -1.20000 H17B 2 0.547393 0.350922 0.697152 11.00000 -1.20000 AFIX 0 C17' 1 0.691682 0.541338 0.554739 11.00000 0.04658 0.02790 = 0.01817 0.00047 -0.00132 -0.00998 AFIX 13 H17' 2 0.658334 0.559950 0.579961 11.00000 -1.20000 AFIX 0 C18 1 0.609996 0.212594 0.677997 11.00000 0.06952 0.02735 = 0.02677 0.00388 0.00250 -0.01009 AFIX 23 H18A 2 0.604482 0.172381 0.701847 11.00000 -1.20000 H18B 2 0.593616 0.167275 0.656180 11.00000 -1.20000 AFIX 0 C18' 1 0.859054 0.590080 0.511829 11.00000 0.05612 0.05764 = 0.02197 0.00542 0.00200 -0.02248 AFIX 137 H18C 2 0.813541 0.627736 0.493700 11.00000 -1.50000 H18D 2 0.863481 0.519524 0.503721 11.00000 -1.50000 H18E 2 0.932450 0.619304 0.512383 11.00000 -1.50000 AFIX 0 C19 1 0.729008 0.251534 0.673862 11.00000 0.06786 0.03068 = 0.02643 0.00230 -0.00038 -0.00867 AFIX 23 H19A 2 0.779557 0.197745 0.682301 11.00000 -1.20000 H19B 2 0.739100 0.309705 0.691284 11.00000 -1.20000 AFIX 0 C19' 1 1.172856 0.677553 0.595961 11.00000 0.04441 0.05780 = 0.02894 -0.00547 0.00626 -0.00531 AFIX 137 H19C 2 1.162571 0.728546 0.575955 11.00000 -1.50000 H19D 2 1.161053 0.610411 0.585046 11.00000 -1.50000 H19E 2 1.247276 0.682106 0.606087 11.00000 -1.50000 AFIX 0 C20 1 0.760881 0.284313 0.632321 11.00000 0.05901 0.02704 = 0.02814 0.00044 0.00403 -0.00615 C20' 1 0.603676 0.564578 0.523232 11.00000 0.05713 0.03848 = 0.02314 0.00693 -0.00722 -0.01489 AFIX 13 H20' 2 0.633173 0.542451 0.497829 11.00000 -1.20000 AFIX 0 C21 1 0.798872 0.395172 0.626644 11.00000 0.04627 0.02490 = 0.02150 -0.00297 0.00146 -0.00422 AFIX 13 H21 2 0.734996 0.438381 0.633589 11.00000 -1.20000 AFIX 0 C21' 1 0.574111 0.679523 0.520396 11.00000 0.06632 0.04019 = 0.05135 0.01847 -0.02896 -0.01213 AFIX 137 H21A 2 0.555012 0.705012 0.545917 11.00000 -1.50000 H21B 2 0.511924 0.688277 0.503042 11.00000 -1.50000 H21C 2 0.636962 0.716951 0.510462 11.00000 -1.50000 AFIX 0 C22 1 0.893279 0.422817 0.656501 11.00000 0.04292 0.02292 = 0.02376 0.00006 0.00138 0.00095 AFIX 13 H22 2 0.925428 0.357993 0.665788 11.00000 -1.20000 AFIX 0 C22' 1 0.497717 0.505215 0.531182 11.00000 0.04928 0.03259 = 0.02045 0.00205 -0.00245 -0.00439 AFIX 43 H22' 2 0.470450 0.506654 0.556673 11.00000 -1.20000 AFIX 0 C23 1 0.853303 0.481397 0.692127 11.00000 0.03569 0.02637 = 0.02320 0.00015 0.00110 -0.00422 C23' 1 0.440673 0.451837 0.505419 11.00000 0.04562 0.03699 = 0.02231 -0.00230 0.00462 -0.00593 AFIX 43 H23' 2 0.470075 0.448506 0.480249 11.00000 -1.20000 AFIX 0 C24 1 0.435813 0.277013 0.611774 11.00000 0.05941 0.04428 = 0.05240 -0.01219 -0.01090 -0.01148 AFIX 137 H24A 2 0.367599 0.253210 0.623299 11.00000 -1.50000 H24B 2 0.482961 0.219282 0.606122 11.00000 -1.50000 H24C 2 0.419663 0.313293 0.587954 11.00000 -1.50000 AFIX 0 C24' 1 0.332693 0.395353 0.512194 11.00000 0.04709 0.03589 = 0.01924 -0.00411 0.00146 -0.00661 AFIX 13 H24' 2 0.309280 0.407647 0.539292 11.00000 -1.20000 AFIX 0 C25 1 0.920515 0.683253 0.835026 11.00000 0.04191 0.04829 = 0.02185 -0.00310 -0.00573 -0.00414 C25' 1 0.239999 0.435444 0.484669 11.00000 0.04934 0.03939 = 0.02451 -0.00112 0.00336 -0.00250 AFIX 13 H25' 2 0.266560 0.427428 0.457698 11.00000 -1.20000 AFIX 0 C26 1 0.986475 0.613047 0.854516 11.00000 0.08331 0.08193 = 0.02729 -0.00244 -0.00468 0.03695 AFIX 43 H26 2 1.025153 0.563502 0.840349 11.00000 -1.20000 AFIX 0 C26' 1 0.217205 0.549349 0.491256 11.00000 0.07196 0.04142 = 0.04752 0.00242 -0.00409 -0.00019 AFIX 137 H26A 2 0.188261 0.559378 0.517188 11.00000 -1.50000 H26B 2 0.163784 0.573052 0.472384 11.00000 -1.50000 H26C 2 0.285205 0.587403 0.488345 11.00000 -1.50000 AFIX 0 C27 1 0.995834 0.615573 0.895441 11.00000 0.11672 0.10780 = 0.02876 0.00036 -0.01023 0.05637 AFIX 43 H27 2 1.042543 0.569310 0.908150 11.00000 -1.20000 AFIX 0 C27' 1 0.131604 0.376449 0.488215 11.00000 0.04855 0.05213 = 0.05593 0.00469 -0.00422 -0.00315 AFIX 137 H27A 2 0.144426 0.305298 0.482248 11.00000 -1.50000 H27B 2 0.078102 0.404169 0.470185 11.00000 -1.50000 H27C 2 0.103635 0.382514 0.514456 11.00000 -1.50000 AFIX 0 C28 1 0.936337 0.686047 0.916817 11.00000 0.09450 0.08426 = 0.02219 -0.00320 -0.00742 0.02497 AFIX 43 H28 2 0.941678 0.686734 0.943992 11.00000 -1.20000 AFIX 0 C28' 1 0.350722 0.279223 0.506896 11.00000 0.05285 0.03688 = 0.03789 -0.00916 0.00064 -0.00592 AFIX 137 H28A 2 0.361279 0.264166 0.479618 11.00000 -1.50000 H28B 2 0.286720 0.242732 0.516418 11.00000 -1.50000 H28C 2 0.415432 0.258217 0.521340 11.00000 -1.50000 AFIX 0 C29 1 0.868564 0.755899 0.897907 11.00000 0.05919 0.04739 = 0.02251 -0.00458 -0.00076 -0.00115 AFIX 43 H29 2 0.827499 0.803366 0.912274 11.00000 -1.20000 AFIX 0 C30 1 0.862043 0.754881 0.857224 11.00000 0.04801 0.02912 = 0.02226 0.00027 -0.00148 -0.00663 AFIX 43 H30 2 0.817612 0.803150 0.844588 11.00000 -1.20000 AFIX 0 N2 3 0.733194 0.610095 0.780637 11.00000 0.03990 0.03729 = 0.01415 0.00357 0.00313 -0.00364 AFIX 43 H2 2 0.713454 0.594369 0.804099 11.00000 -1.20000 AFIX 0 O1 4 0.650131 0.473818 0.749729 11.00000 0.04020 0.03453 = 0.02926 0.00962 -0.00216 -0.00855 O1' 4 1.297199 0.780485 0.728267 11.00000 0.03834 0.03693 = 0.02945 -0.00517 -0.00773 0.00466 AFIX 3 H1' 2 1.293279 0.849185 0.738467 11.00000 -1.20000 AFIX 0 O2 4 0.490914 0.798069 0.689603 11.00000 0.03493 0.04007 = 0.03580 -0.00036 -0.00583 -0.00204 AFIX 147 H2A 2 0.430998 0.786771 0.700292 11.00000 -1.50000 AFIX 0 O3 4 0.776903 0.552999 0.682264 11.00000 0.03582 0.02390 = 0.01942 -0.00273 0.00074 -0.00143 O4 4 0.888221 0.469322 0.724914 11.00000 0.04384 0.03560 = 0.02343 0.00066 -0.00268 0.00178 O5 4 0.754452 0.224684 0.605255 11.00000 0.08919 0.02746 = 0.03002 -0.00660 0.00497 -0.01372 HKLF 4 REM 20190524_pms-41_a.res in P2(1)2(1)2(1) REM R1 = 0.0362 for 8920 Fo > 4sig(Fo) and 0.0366 for all 9055 data REM 587 parameters refined using 12 restraints END WGHT 0.0485 1.8436 REM Instructions for potential hydrogen bonds HTAB C21 O3 HTAB O1' O1_$1 HTAB O2 O1'_$2 REM Highest difference peak 0.332, deepest hole -0.205, 1-sigma level 0.033 Q1 1 0.9296 0.5821 0.8977 11.00000 0.05 0.33 Q2 1 0.9238 0.5788 0.8611 11.00000 0.05 0.27 Q3 1 0.5230 0.8955 0.6589 11.00000 0.05 0.27 Q4 1 0.8732 0.6519 0.9206 11.00000 0.05 0.26 Q5 1 0.6547 0.5453 0.8586 11.00000 0.05 0.24 Q6 1 0.5505 0.9444 0.6428 11.00000 0.05 0.19 Q7 1 0.8369 0.2238 0.6002 11.00000 0.05 0.13 Q8 1 1.3602 0.9871 0.6182 11.00000 0.05 0.13 Q9 1 0.6961 0.8795 0.6420 11.00000 0.05 0.13 Q10 1 0.6074 0.4974 0.8402 11.00000 0.05 0.12 Q11 1 0.8506 0.3981 0.6392 11.00000 0.05 0.12 Q12 1 0.5030 0.4350 0.5209 11.00000 0.05 0.12 Q13 1 1.0962 0.6532 0.6422 11.00000 0.05 0.12 Q14 1 0.8374 0.7813 0.4626 11.00000 0.05 0.12 Q15 1 1.0945 0.7418 0.6421 11.00000 0.05 0.12 Q16 1 1.3753 0.7651 0.7252 11.00000 0.05 0.12 Q17 1 0.9147 0.4781 0.6443 11.00000 0.05 0.12 Q18 1 0.5198 0.3317 0.6599 11.00000 0.05 0.11 Q19 1 0.9950 0.6516 0.8961 11.00000 0.05 0.11 Q20 1 0.6007 0.7143 0.7003 11.00000 0.05 0.11 REM The information below was added by Olex2. REM REM R1 = 0.0362 for 8920 Fo > 4sig(Fo) and 0.0366 for all 61102 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.33, deepest hole -0.20 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0366 REM R1_gt = 0.0362 REM wR_ref = 0.0958 REM GOOF = 1.050 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 61102 REM Reflections_gt = 8920 REM Parameters = n/a REM Hole = -0.20 REM Peak = 0.33 REM Flack = 0.18(2) ; _cod_data_source_file d0ob00701c2.cif _cod_data_source_block 20190524_pms-41 _cod_depositor_comments 'Adding full bibliography for 7157500.cif.' _cod_original_cell_volume 5332.0(7) _cod_database_code 7157500 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_max 0.948 _shelx_estimated_absorpt_t_min 0.938 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H1' of O1', All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, H2A of O2 2. Uiso/Uaniso restraints and constraints Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3.a Riding coordinates: O1'(H1') 3.b Ternary CH refined with riding coordinates: C3(H3), C3'(H3'), C4(H4), C5(H5), C7(H7), C7'(H7'), C8(H8), C9'(H9'), C15'(H15'), C16(H16), C17'(H17'), C20'(H20'), C21(H21), C22(H22), C24'(H24'), C25'(H25') 3.c Secondary CH2 refined with riding coordinates: C1'(H1'A,H1'B), C2'(H2'A,H2'B), C4'(H4'A,H4'B), C10(H10A,H10B), C11'(H11D, H11E), C12'(H12C,H12D), C15(H15A,H15B), C16'(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B) 3.d Aromatic/amide H refined with riding coordinates: C6'(H6'), C13(H13), C14(H14), C22'(H22'), C23'(H23'), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), N2(H2) 3.e X=CH2 refined with riding coordinates: C12(H12A,H12B) 3.f Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C18'(H18C,H18D,H18E), C19'(H19C,H19D,H19E), C21'(H21A, H21B,H21C), C24(H24A,H24B,H24C), C26'(H26A,H26B,H26C), C27'(H27A,H27B,H27C), C28'(H28A,H28B,H28C) 3.g Idealised tetrahedral OH refined as rotating group: O2(H2A) ; _shelx_fab_file ; -14 -5 -6 0.7725 0.2256 -14 -5 -5 -0.0138 -0.4922 -14 -5 -4 0.4098 -0.0876 -14 -5 -3 -0.1587 -0.9909 -14 -5 -2 -0.2768 -0.1649 -14 -5 -1 -0.2740 0.8069 -14 -4 -10 0.3642 -0.2020 -14 -4 -9 0.7386 0.0668 -14 -4 -8 0.1124 -0.8459 -14 -4 -7 -0.4727 -0.1868 -14 -4 -6 -0.1163 0.2095 -14 -4 -5 -1.1248 0.3498 -14 -4 -4 -0.0974 0.5374 -14 -4 -3 0.8495 0.6870 -14 -4 -2 -0.1423 -0.4224 -14 -4 -1 1.1257 -0.8306 -14 -3 -12 -0.0522 -0.3247 -14 -3 -11 0.5890 -0.5061 -14 -3 -10 -0.6319 -0.1482 -14 -3 -9 -0.3672 0.4142 -14 -3 -8 0.4443 0.2359 -14 -3 -7 -0.3537 1.1239 -14 -3 -6 0.5922 0.1658 -14 -3 -5 0.7708 -0.5759 -14 -3 -4 -1.0192 0.2564 -14 -3 -3 -0.3234 -1.1972 -14 -3 -2 -0.2116 0.3640 -14 -3 -1 -0.8911 0.7693 -14 -2 -14 -0.2402 -0.0293 -14 -2 -13 -0.2568 -0.8557 -14 -2 -12 -0.1323 0.3520 -14 -2 -11 0.3795 0.3900 -14 -2 -10 0.4635 -0.2335 -14 -2 -9 0.7918 0.9524 -14 -2 -8 0.1239 -0.5049 -14 -2 -7 -0.6905 -0.9239 -14 -2 -6 -0.1097 0.8440 -14 -2 -5 -1.3661 -0.5584 -14 -2 -4 0.2308 0.3490 -14 -2 -3 0.3376 1.0553 -14 -2 -2 -0.0689 -1.2892 -14 -2 -1 0.7724 -0.3638 -14 -1 -14 -0.2504 0.0079 -14 -1 -13 0.5344 -0.0951 -14 -1 -12 -0.0679 -0.3787 -14 -1 -11 1.6362 -0.1720 -14 -1 -10 -0.0275 0.1134 -14 -1 -9 -0.8268 0.6675 -14 -1 -8 0.4818 0.2695 -14 -1 -7 -1.3167 0.8096 -14 -1 -6 0.1789 -0.6140 -14 -1 -5 1.3207 -0.4747 -14 -1 -4 -0.8103 -0.2997 -14 -1 -3 0.6034 -0.8460 -14 -1 -2 -0.0476 0.6732 -14 -1 -1 -0.6466 0.2701 -13 -7 -9 -0.2617 -0.2709 -13 -7 -8 0.5510 0.2746 -13 -7 -7 -0.4513 -0.2374 -13 -7 -6 -0.5227 -0.7094 -13 -7 -5 0.1119 0.1768 -13 -7 -4 -0.5985 -0.1343 -13 -7 -3 0.3459 0.5674 -13 -7 -2 -0.0253 0.3598 -13 -7 -1 0.0215 0.3265 -13 -6 -12 0.3015 -0.7189 -13 -6 -11 -0.4483 0.1939 -13 -6 -10 0.1970 -1.6256 -13 -6 -9 -0.7275 0.1014 -13 -6 -8 -0.8435 0.9733 -13 -6 -7 0.2828 -0.5381 -13 -6 -6 -0.4564 1.0873 -13 -6 -5 0.9523 -0.4099 -13 -6 -4 0.5190 -1.0086 -13 -6 -3 0.2527 0.2299 -13 -6 -2 -0.2076 -0.5668 -13 -6 -1 -0.7915 0.1788 -13 -5 -16 1.7212 0.6142 -13 -5 -15 -0.0600 -0.3511 -13 -5 -14 -1.0188 0.1737 -13 -5 -13 0.0546 0.3718 -13 -5 -12 -2.2967 -0.2135 -13 -5 -11 0.1903 0.8393 -13 -5 -10 1.4581 0.2848 -13 -5 -9 -0.5828 -0.6098 -13 -5 -8 1.8754 0.1901 -13 -5 -7 -0.5145 -1.2448 -13 -5 -6 -1.7550 -0.4198 -13 -5 -5 0.5009 -0.0129 -13 -5 -4 -1.1199 0.4450 -13 -5 -3 0.3377 0.7106 -13 -5 -2 1.5029 0.0011 -13 -5 -1 -0.1585 0.3246 -13 -4 -18 0.4433 -1.2429 -13 -4 -17 -0.3600 0.0902 -13 -4 -16 -0.2687 0.4380 -13 -4 -15 -0.1367 -0.1743 -13 -4 -14 -0.6393 2.0828 -13 -4 -13 0.5435 -0.1522 -13 -4 -12 0.1568 -1.1878 -13 -4 -11 -0.5466 0.7087 -13 -4 -10 0.3067 -1.9558 -13 -4 -9 -0.9273 0.5582 -13 -4 -8 -0.4304 1.9671 -13 -4 -7 0.4476 -0.8798 -13 -4 -6 0.2099 1.2557 -13 -4 -5 0.2304 -0.4508 -13 -4 -4 0.2276 -2.2616 -13 -4 -3 -0.3842 0.6418 -13 -4 -2 -1.3693 -0.4433 -13 -4 -1 0.5990 0.3696 -13 -3 -19 -0.0082 0.2752 -13 -3 -18 -0.0038 0.5581 -13 -3 -17 -0.3093 0.0750 -13 -3 -16 1.6565 0.6748 -13 -3 -15 0.1821 -0.4749 -13 -3 -14 -0.5467 -0.5253 -13 -3 -13 0.6845 0.4379 -13 -3 -12 -1.9188 -0.5834 -13 -3 -11 0.1105 0.9215 -13 -3 -10 1.3265 0.8673 -13 -3 -9 -1.0647 -0.6665 -13 -3 -8 1.2399 0.3442 -13 -3 -7 -0.0888 -0.3751 -13 -3 -6 -2.1802 -0.9983 -13 -3 -5 1.2387 0.6788 -13 -3 -4 -0.7639 0.2818 -13 -3 -3 0.1767 -0.9373 -13 -3 -2 2.0786 0.3543 -13 -3 -1 -0.9582 -1.1759 -13 -2 -20 0.5605 0.2396 -13 -2 -19 0.3107 0.6243 -13 -2 -18 0.5937 -0.7531 -13 -2 -17 -0.2229 -0.3241 -13 -2 -16 -0.6116 0.2414 -13 -2 -15 -0.0115 -0.8664 -13 -2 -14 -0.7691 1.4564 -13 -2 -13 0.4158 0.0346 -13 -2 -12 0.8971 -0.6825 -13 -2 -11 -0.7695 0.8878 -13 -2 -10 0.5118 -0.9596 -13 -2 -9 -0.7468 -0.1296 -13 -2 -8 -1.5100 1.7472 -13 -2 -7 0.6750 -1.1086 -13 -2 -6 -0.3052 0.7375 -13 -2 -5 -0.3088 0.3850 -13 -2 -4 1.2675 -1.9380 -13 -2 -3 -0.8877 1.2564 -13 -2 -2 -0.0519 -0.4448 -13 -2 -1 1.2546 0.4286 -13 -1 -20 -0.0938 0.2061 -13 -1 -19 -0.5318 0.4220 -13 -1 -18 -0.0489 1.0726 -13 -1 -17 -1.2243 0.7488 -13 -1 -16 0.5642 0.4030 -13 -1 -15 0.4539 0.1709 -13 -1 -14 -0.1303 -1.5223 -13 -1 -13 1.4414 0.0811 -13 -1 -12 -0.3059 -0.9551 -13 -1 -11 -0.1037 0.0903 -13 -1 -10 0.8907 1.6087 -13 -1 -9 -1.3791 -0.5653 -13 -1 -8 0.0810 0.5249 -13 -1 -7 0.4418 -0.1363 -13 -1 -6 -1.5329 -1.9825 -13 -1 -5 1.6600 0.3900 -13 -1 -4 -0.2580 -0.3667 -13 -1 -3 -0.0248 -0.7348 -13 -1 -2 1.3200 1.1358 -13 -1 -1 -1.2480 -0.8051 -12 -9 -6 -0.3656 0.1017 -12 -9 -5 1.1858 0.3107 -12 -9 -4 0.2922 0.0204 -12 -9 -3 0.3353 -0.0947 -12 -9 -2 0.1666 0.0328 -12 -9 -1 -0.5943 -0.4342 -12 -8 -14 0.2675 0.0795 -12 -8 -13 -0.8555 -0.2213 -12 -8 -12 -0.2464 -0.9976 -12 -8 -11 -0.4216 0.8269 -12 -8 -10 0.0472 -0.5043 -12 -8 -9 0.8338 0.4032 -12 -8 -8 0.2764 0.8681 -12 -8 -7 0.2951 -1.7290 -12 -8 -6 0.0887 -0.0615 -12 -8 -5 -0.9096 -0.6455 -12 -8 -4 -0.2046 -0.5626 -12 -8 -3 -0.6703 1.6316 -12 -8 -2 -0.2323 0.5513 -12 -8 -1 -0.0666 -0.0403 -12 -7 -17 -0.0934 -0.6369 -12 -7 -16 -0.2160 -0.6306 -12 -7 -15 -0.4221 1.4629 -12 -7 -14 -0.9750 0.5000 -12 -7 -13 0.7104 1.3274 -12 -7 -12 -0.5653 0.4832 -12 -7 -11 0.6027 -1.1444 -12 -7 -10 1.1154 -0.3105 -12 -7 -9 -1.4869 -0.5888 -12 -7 -8 0.4136 -0.4220 -12 -7 -7 -0.7733 1.5273 -12 -7 -6 -0.7510 0.1129 -12 -7 -5 2.0769 0.3987 -12 -7 -4 0.6826 0.6299 -12 -7 -3 0.4252 -1.1562 -12 -7 -2 0.3819 0.2413 -12 -7 -1 -1.0906 -0.2769 -12 -6 -20 -0.5445 0.0440 -12 -6 -19 -0.6669 -0.5445 -12 -6 -18 -0.7554 0.3349 -12 -6 -17 1.7901 0.3755 -12 -6 -16 0.6892 0.5226 -12 -6 -15 1.6933 0.1443 -12 -6 -14 0.6548 0.0870 -12 -6 -13 -2.1231 -0.4381 -12 -6 -12 -0.7585 -0.9306 -12 -6 -11 -1.5678 0.5003 -12 -6 -10 -0.9593 -0.3976 -12 -6 -9 2.3225 0.4997 -12 -6 -8 -0.0310 0.7739 -12 -6 -7 0.8927 -1.3611 -12 -6 -6 1.1133 -0.7119 -12 -6 -5 -2.2170 -0.3227 -12 -6 -4 0.6461 -0.9087 -12 -6 -3 -0.5797 1.6331 -12 -6 -2 -0.4268 1.1960 -12 -6 -1 0.6929 -0.7000 -12 -5 -21 -0.8002 0.6659 -12 -5 -20 0.4465 0.6573 -12 -5 -19 0.0850 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12 8 2 -0.2323 -0.5513 12 8 3 -0.6703 -1.6316 12 8 4 -0.2046 0.5626 12 8 5 -0.9096 0.6455 12 8 6 0.0887 0.0615 12 8 7 0.2951 1.7290 12 8 8 0.2764 -0.8681 12 8 9 0.8338 -0.4032 12 8 10 0.0472 0.5043 12 8 11 -0.4216 -0.8269 12 8 12 -0.2464 0.9976 12 8 13 -0.8555 0.2213 12 8 14 0.2675 -0.0795 12 9 0 -0.3435 -0.0280 12 9 1 -0.5943 0.4342 12 9 2 0.1666 -0.0328 12 9 3 0.3353 0.0947 12 9 4 0.2922 -0.0204 12 9 5 1.1858 -0.3107 12 9 6 -0.3656 -0.1017 12 9 7 -0.3879 -0.3623 12 9 8 0.0280 -0.1161 12 9 9 -0.6292 -0.0029 13 0 1 0.0079 -0.9279 13 0 2 0.9227 -0.0040 13 0 3 0.0051 -2.0843 13 0 4 2.1773 -0.0078 13 0 5 -0.0139 -0.3431 13 0 6 -0.3903 0.0171 13 0 7 -0.0040 1.9904 13 0 8 -1.9892 0.0054 13 0 9 0.0131 0.3349 13 0 10 1.0829 -0.0046 13 0 11 -0.0097 -1.8450 13 0 12 2.0942 0.0046 13 0 13 -0.0134 -0.4660 13 0 14 -0.7719 -0.0066 13 0 15 0.0107 1.6838 13 0 16 -2.0386 0.0052 13 0 17 -0.0026 0.8601 13 0 18 -0.5749 0.0120 13 0 19 -0.0057 -0.9827 13 0 20 0.8335 -0.0087 13 0 21 0.0116 -0.3057 13 1 0 0.0041 -0.6491 13 1 1 -1.2480 0.8051 13 1 2 1.3200 -1.1358 13 1 3 -0.0248 0.7348 13 1 4 -0.2580 0.3667 13 1 5 1.6600 -0.3900 13 1 6 -1.5329 1.9825 13 1 7 0.4418 0.1363 13 1 8 0.0810 -0.5249 13 1 9 -1.3791 0.5653 13 1 10 0.8907 -1.6087 13 1 11 -0.1037 -0.0903 13 1 12 -0.3059 0.9551 13 1 13 1.4414 -0.0811 13 1 14 -0.1303 1.5223 13 1 15 0.4539 -0.1709 13 1 16 0.5642 -0.4030 13 1 17 -1.2243 -0.7488 13 1 18 -0.0489 -1.0726 13 1 19 -0.5318 -0.4220 13 1 20 -0.0938 -0.2061 13 2 0 0.0244 -1.5407 13 2 1 1.2546 -0.4286 13 2 2 -0.0519 0.4448 13 2 3 -0.8877 -1.2564 13 2 4 1.2675 1.9380 13 2 5 -0.3088 -0.3850 13 2 6 -0.3052 -0.7375 13 2 7 0.6750 1.1086 13 2 8 -1.5100 -1.7472 13 2 9 -0.7468 0.1296 13 2 10 0.5118 0.9596 13 2 11 -0.7695 -0.8878 13 2 12 0.8971 0.6825 13 2 13 0.4158 -0.0346 13 2 14 -0.7691 -1.4564 13 2 15 -0.0115 0.8664 13 2 16 -0.6116 -0.2414 13 2 17 -0.2229 0.3241 13 2 18 0.5937 0.7531 13 2 19 0.3107 -0.6243 13 2 20 0.5605 -0.2396 13 3 0 -0.0081 0.9220 13 3 1 -0.9582 1.1759 13 3 2 2.0786 -0.3543 13 3 3 0.1767 0.9373 13 3 4 -0.7639 -0.2818 13 3 5 1.2387 -0.6788 13 3 6 -2.1802 0.9983 13 3 7 -0.0888 0.3751 13 3 8 1.2399 -0.3442 13 3 9 -1.0647 0.6665 13 3 10 1.3265 -0.8673 13 3 11 0.1105 -0.9215 13 3 12 -1.9188 0.5834 13 3 13 0.6845 -0.4379 13 3 14 -0.5467 0.5253 13 3 15 0.1821 0.4749 13 3 16 1.6565 -0.6748 13 3 17 -0.3093 -0.0750 13 3 18 -0.0038 -0.5581 13 3 19 -0.0082 -0.2752 13 4 0 0.0340 -2.1819 13 4 1 0.5990 -0.3696 13 4 2 -1.3693 0.4433 13 4 3 -0.3842 -0.6418 13 4 4 0.2276 2.2616 13 4 5 0.2304 0.4508 13 4 6 0.2099 -1.2557 13 4 7 0.4476 0.8798 13 4 8 -0.4304 -1.9671 13 4 9 -0.9273 -0.5582 13 4 10 0.3067 1.9558 13 4 11 -0.5466 -0.7087 13 4 12 0.1568 1.1878 13 4 13 0.5435 0.1522 13 4 14 -0.6393 -2.0828 13 4 15 -0.1367 0.1743 13 4 16 -0.2687 -0.4380 13 4 17 -0.3600 -0.0902 13 4 18 0.4433 1.2429 13 5 0 -0.0019 1.3417 13 5 1 -0.1585 -0.3246 13 5 2 1.5029 -0.0011 13 5 3 0.3377 -0.7106 13 5 4 -1.1199 -0.4450 13 5 5 0.5009 0.0129 13 5 6 -1.7550 0.4198 13 5 7 -0.5145 1.2448 13 5 8 1.8754 -0.1901 13 5 9 -0.5828 0.6098 13 5 10 1.4581 -0.2848 13 5 11 0.1903 -0.8393 13 5 12 -2.2967 0.2135 13 5 13 0.0546 -0.3718 13 5 14 -1.0188 -0.1737 13 5 15 -0.0600 0.3511 13 6 0 0.0424 -0.5720 13 6 1 -0.7915 -0.1788 13 6 2 -0.2076 0.5668 13 6 3 0.2527 -0.2299 13 6 4 0.5190 1.0086 13 6 5 0.9523 0.4099 13 6 6 -0.4564 -1.0873 13 6 7 0.2828 0.5381 13 6 8 -0.8435 -0.9733 13 6 9 -0.7275 -0.1014 13 6 10 0.1970 1.6256 13 6 11 -0.4483 -0.1939 13 6 12 0.3015 0.7189 13 6 13 0.4246 -0.2039 13 7 0 -0.0045 0.0968 13 7 1 0.0215 -0.3265 13 7 2 -0.0253 -0.3598 13 7 3 0.3459 -0.5674 13 7 4 -0.5985 0.1343 13 7 5 0.1119 -0.1768 13 7 6 -0.5227 0.7094 13 7 7 -0.4513 0.2374 13 7 8 0.5510 -0.2746 13 7 9 -0.2617 0.2709 13 7 10 0.2452 -0.4654 14 0 0 -0.8079 -0.0116 14 0 1 -0.0083 -0.2790 14 0 2 0.3351 0.0082 14 0 3 -0.0003 -1.1544 14 0 4 1.0802 0.0088 14 0 5 0.0164 1.3406 14 0 6 -0.2546 -0.0115 14 0 7 -0.0087 1.2269 14 0 8 -0.6799 0.0017 14 0 9 -0.0043 -1.9523 14 0 10 0.1789 0.0042 14 0 11 0.0098 -0.7831 14 0 12 0.0639 -0.0048 14 0 13 -0.0125 1.9722 14 0 14 -0.2558 0.0037 14 1 0 0.9864 -0.0079 14 1 1 -0.6466 -0.2701 14 1 2 -0.0476 -0.6732 14 1 3 0.6034 0.8460 14 1 4 -0.8103 0.2997 14 1 5 1.3207 0.4747 14 1 6 0.1789 0.6140 14 1 7 -1.3167 -0.8096 14 1 8 0.4818 -0.2695 14 1 9 -0.8268 -0.6675 14 1 10 -0.0275 -0.1134 14 1 11 1.6362 0.1720 14 1 12 -0.0679 0.3787 14 1 13 0.5344 0.0951 14 1 14 -0.2504 -0.0079 14 2 0 -0.5157 -0.0103 14 2 1 0.7724 0.3638 14 2 2 -0.0689 1.2892 14 2 3 0.3376 -1.0553 14 2 4 0.2308 -0.3490 14 2 5 -1.3661 0.5584 14 2 6 -0.1097 -0.8440 14 2 7 -0.6905 0.9239 14 2 8 0.1239 0.5049 14 2 9 0.7918 -0.9524 14 2 10 0.4635 0.2335 14 2 11 0.3795 -0.3900 14 2 12 -0.1323 -0.3520 14 3 0 1.2833 0.0142 14 3 1 -0.8911 -0.7693 14 3 2 -0.2116 -0.3640 14 3 3 -0.3234 1.1972 14 3 4 -1.0192 -0.2564 14 3 5 0.7708 0.5759 14 3 6 0.5922 -0.1658 14 3 7 -0.3537 -1.1239 14 3 8 0.4443 -0.2359 14 3 9 -0.3672 -0.4142 14 3 10 -0.6319 0.1482 14 3 11 0.5890 0.5061 14 3 12 -0.0522 0.3247 14 4 0 -0.1855 -0.0197 14 4 1 1.1257 0.8306 14 4 2 -0.1423 0.4224 14 4 3 0.8495 -0.6870 14 4 4 -0.0974 -0.5374 14 4 5 -1.1248 -0.3498 14 4 6 -0.1163 -0.2095 14 4 7 -0.4727 0.1868 14 4 8 0.1124 0.8459 14 4 9 0.7386 -0.0668 14 4 10 0.3642 0.2020 14 5 0 -0.3952 0.0170 14 5 1 -0.2740 -0.8069 14 5 2 -0.2768 0.1649 14 5 3 -0.1587 0.9909 14 5 4 0.4098 0.0876 14 5 5 -0.0138 0.4922 14 5 6 0.7725 -0.2256 14 5 7 -0.1510 -0.7906 0 0 0 0.0 0.0 ; _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 1.616 _oxdiff_exptl_absorpt_empirical_full_min 0.762 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 C1 C 0.6999(2) 0.55515(19) 0.74944(7) 0.0296(5) Uani 1 1 d . . . . . C1' C 1.0953(2) 0.80840(19) 0.64396(7) 0.0337(5) Uani 1 1 d . . . . . H1'A H 1.0963 0.8537 0.6214 0.040 Uiso 1 1 calc R . . . . H1'B H 1.0283 0.8234 0.6587 0.040 Uiso 1 1 calc R . . . . C2' C 1.1960(2) 0.8329(2) 0.66955(8) 0.0368(6) Uani 1 1 d . . . . . H2'A H 1.2635 0.8261 0.6542 0.044 Uiso 1 1 calc R . . . . H2'B H 1.1912 0.9034 0.6787 0.044 Uiso 1 1 calc R . . . . C3 C 0.8045(2) 0.69764(18) 0.77237(6) 0.0281(5) Uani 1 1 d . . . . . H3 H 0.7695 0.7607 0.7822 0.034 Uiso 1 1 calc R . . . . C3' C 1.2011(2) 0.76129(19) 0.70423(7) 0.0303(5) Uani 1 1 d . . . . . H3' H 1.1334 0.7691 0.7200 0.036 Uiso 1 1 calc R . . . . C4 C 0.81086(19) 0.70113(18) 0.72674(6) 0.0260(5) Uani 1 1 d . . . . . H4 H 0.8862 0.6814 0.7187 0.031 Uiso 1 1 calc R . . . . C4' C 1.2101(2) 0.65172(19) 0.68992(7) 0.0321(5) Uani 1 1 d . . . . . H4'A H 1.2810 0.6430 0.6767 0.039 Uiso 1 1 calc R . . . . H4'B H 1.2093 0.6059 0.7123 0.039 Uiso 1 1 calc R . . . . C5 C 0.78528(19) 0.80892(17) 0.71006(6) 0.0255(5) Uani 1 1 d . . . . . H5 H 0.7911 0.8038 0.6815 0.031 Uiso 1 1 calc R . . . . C5' C 1.1181(2) 0.62121(18) 0.66242(7) 0.0291(5) Uani 1 1 d . . . . . C6 C 0.6672(2) 0.83970(18) 0.71912(6) 0.0281(5) Uani 1 1 d . . . . . C6' C 1.0708(2) 0.52924(19) 0.66508(7) 0.0319(5) Uani 1 1 d . . . . . H6' H 1.0902 0.4887 0.6865 0.038 Uiso 1 1 calc R . . . . C7 C 0.5788(2) 0.75687(18) 0.71294(7) 0.0282(5) Uani 1 1 d . . . . . H7 H 0.5486 0.7368 0.7385 0.034 Uiso 1 1 calc R . . . . C7' C 0.9889(2) 0.48522(18) 0.63661(7) 0.0301(5) Uani 1 1 d . . . . . H7' H 1.0306 0.4359 0.6206 0.036 Uiso 1 1 calc R . . . . C8 C 0.6233(2) 0.66082(18) 0.69225(6) 0.0262(5) Uani 1 1 d . . . . . H8 H 0.6460 0.6823 0.6659 0.031 Uiso 1 1 calc R . . . . C8' C 0.9431(2) 0.56381(18) 0.60862(7) 0.0291(5) Uani 1 1 d . . . . . C9 C 0.7290(2) 0.61773(17) 0.71260(6) 0.0260(5) Uani 1 1 d . . . . . C9' C 0.9676(2) 0.67596(18) 0.61607(7) 0.0290(5) Uani 1 1 d . . . . . H9' H 0.9210 0.6951 0.6385 0.035 Uiso 1 1 calc R . . . . C10 C 0.9196(2) 0.6852(2) 0.79070(7) 0.0330(5) Uani 1 1 d . . . . . H10A H 0.9523 0.6218 0.7812 0.040 Uiso 1 1 calc R . . . . H10B H 0.9665 0.7413 0.7819 0.040 Uiso 1 1 calc R . . . . C10' C 1.0889(2) 0.69616(18) 0.62932(7) 0.0292(5) Uani 1 1 d . . . . . C11 C 0.8717(2) 0.88799(19) 0.72324(7) 0.0324(5) Uani 1 1 d . . . . . H11A H 0.8627 0.9014 0.7507 0.049 Uiso 1 1 calc GR . . . . H11B H 0.8615 0.9506 0.7088 0.049 Uiso 1 1 calc GR . . . . H11C H 0.9451 0.8616 0.7185 0.049 Uiso 1 1 calc GR . . . . C11' C 0.9255(2) 0.7411(2) 0.58187(8) 0.0370(6) Uani 1 1 d . . . . . H11D H 0.9770 0.7350 0.5601 0.044 Uiso 1 1 calc R . . . . H11E H 0.9234 0.8127 0.5897 0.044 Uiso 1 1 calc R . . . . C12 C 0.6358(2) 0.9318(2) 0.73107(7) 0.0336(5) Uani 1 1 d . . . . . H12A H 0.6884 0.9835 0.7345 0.040 Uiso 1 1 calc R . . . . H12B H 0.5610 0.9449 0.7361 0.040 Uiso 1 1 calc R . . . . C12' C 0.8087(2) 0.70777(19) 0.56847(8) 0.0375(6) Uani 1 1 d . . . . . H12C H 0.7832 0.7537 0.5480 0.045 Uiso 1 1 calc R . . . . H12D H 0.7574 0.7135 0.5903 0.045 Uiso 1 1 calc R . . . . C13 C 0.5336(2) 0.58156(19) 0.68710(7) 0.0300(5) Uani 1 1 d . . . . . H13 H 0.4936 0.5618 0.7092 0.036 Uiso 1 1 calc R . . . . C13' C 0.8073(2) 0.59597(19) 0.55296(7) 0.0326(5) Uani 1 1 d . . . . . C14 C 0.5078(2) 0.53810(19) 0.65343(7) 0.0336(6) Uani 1 1 d . . . . . H14 H 0.5420 0.5648 0.6312 0.040 Uiso 1 1 calc R . . . . C14' C 0.8724(2) 0.52993(18) 0.58168(6) 0.0299(5) Uani 1 1 d . . . . . C15 C 0.4288(2) 0.4498(2) 0.64719(7) 0.0357(6) Uani 1 1 d . . . . . H15A H 0.3817 0.4638 0.6247 0.043 Uiso 1 1 calc R . . . . H15B H 0.3814 0.4421 0.6700 0.043 Uiso 1 1 calc R . . . . C15' C 0.8275(2) 0.42133(18) 0.58338(7) 0.0315(5) Uani 1 1 d . . . . . H15' H 0.8816 0.3723 0.5727 0.038 Uiso 1 1 calc R . . . . C16 C 0.4948(2) 0.34872(19) 0.64022(7) 0.0353(6) Uani 1 1 d . . . . . H16 H 0.5658 0.3679 0.6281 0.042 Uiso 1 1 calc R . . . . C16' C 0.7225(2) 0.42642(18) 0.55743(7) 0.0332(6) Uani 1 1 d . . . . . H16A H 0.6622 0.3874 0.5691 0.040 Uiso 1 1 calc R . . . . H16B H 0.7378 0.3987 0.5316 0.040 Uiso 1 1 calc R . . . . C17 C 0.5220(3) 0.2981(2) 0.67920(8) 0.0437(7) Uani 1 1 d . . . . . H17A H 0.4538 0.2695 0.6899 0.052 Uiso 1 1 calc R . . . . H17B H 0.5474 0.3509 0.6972 0.052 Uiso 1 1 calc R . . . . C17' C 0.6917(2) 0.54134(18) 0.55474(7) 0.0309(5) Uani 1 1 d . . . . . H17' H 0.6583 0.5600 0.5800 0.037 Uiso 1 1 calc R . . . . C18 C 0.6100(3) 0.2126(2) 0.67800(8) 0.0412(6) Uani 1 1 d . . . . . H18A H 0.6045 0.1724 0.7018 0.049 Uiso 1 1 calc R . . . . H18B H 0.5936 0.1673 0.6562 0.049 Uiso 1 1 calc R . . . . C18' C 0.8591(3) 0.5901(2) 0.51183(7) 0.0452(7) Uani 1 1 d . . . . . H18C H 0.8135 0.6277 0.4937 0.068 Uiso 1 1 calc GR . . . . H18D H 0.8635 0.5195 0.5037 0.068 Uiso 1 1 calc GR . . . . H18E H 0.9325 0.6193 0.5124 0.068 Uiso 1 1 calc GR . . . . C19 C 0.7290(3) 0.2515(2) 0.67386(8) 0.0417(7) Uani 1 1 d . . . . . H19A H 0.7796 0.1977 0.6823 0.050 Uiso 1 1 calc R . . . . H19B H 0.7391 0.3097 0.6913 0.050 Uiso 1 1 calc R . . . . C19' C 1.1729(2) 0.6776(2) 0.59596(8) 0.0437(7) Uani 1 1 d . . . . . H19C H 1.1626 0.7285 0.5760 0.066 Uiso 1 1 calc GR . . . . H19D H 1.1611 0.6104 0.5850 0.066 Uiso 1 1 calc GR . . . . H19E H 1.2473 0.6821 0.6061 0.066 Uiso 1 1 calc GR . . . . C20 C 0.7609(3) 0.28431(19) 0.63232(7) 0.0381(6) Uani 1 1 d . . . . . C20' C 0.6037(2) 0.5646(2) 0.52323(7) 0.0396(6) Uani 1 1 d . . . . . H20' H 0.6332 0.5425 0.4978 0.047 Uiso 1 1 calc R . . . . C21 C 0.7989(2) 0.39517(18) 0.62664(7) 0.0309(5) Uani 1 1 d . . . . . H21 H 0.7350 0.4384 0.6336 0.037 Uiso 1 1 calc R . . . . C21' C 0.5741(3) 0.6795(2) 0.52040(9) 0.0526(8) Uani 1 1 d . . . . . H21A H 0.5550 0.7050 0.5459 0.079 Uiso 1 1 calc GR . . . . H21B H 0.5119 0.6883 0.5030 0.079 Uiso 1 1 calc GR . . . . H21C H 0.6370 0.7170 0.5105 0.079 Uiso 1 1 calc GR . . . . C22 C 0.8933(2) 0.42282(18) 0.65650(7) 0.0299(5) Uani 1 1 d . . . . . H22 H 0.9254 0.3580 0.6658 0.036 Uiso 1 1 calc R . . . . C22' C 0.4977(2) 0.50521(19) 0.53118(7) 0.0341(6) Uani 1 1 d . . . . . H22' H 0.4705 0.5067 0.5567 0.041 Uiso 1 1 calc R . . . . C23 C 0.8533(2) 0.48140(18) 0.69213(7) 0.0284(5) Uani 1 1 d . . . . . C23' C 0.4407(2) 0.4518(2) 0.50542(7) 0.0350(6) Uani 1 1 d . . . . . H23' H 0.4701 0.4485 0.4802 0.042 Uiso 1 1 calc R . . . . C24 C 0.4358(3) 0.2770(2) 0.61177(10) 0.0520(8) Uani 1 1 d . . . . . H24A H 0.3676 0.2532 0.6233 0.078 Uiso 1 1 calc GR . . . . H24B H 0.4830 0.2193 0.6061 0.078 Uiso 1 1 calc GR . . . . H24C H 0.4197 0.3133 0.5880 0.078 Uiso 1 1 calc GR . . . . C24' C 0.3327(2) 0.3954(2) 0.51219(7) 0.0341(6) Uani 1 1 d . . . . . H24' H 0.3093 0.4076 0.5393 0.041 Uiso 1 1 calc R . . . . C25 C 0.9205(2) 0.6833(2) 0.83503(7) 0.0374(6) Uani 1 1 d . . . . . C25' C 0.2400(2) 0.4354(2) 0.48467(7) 0.0377(6) Uani 1 1 d . . . . . H25' H 0.2666 0.4274 0.4577 0.045 Uiso 1 1 calc R . . . . C26 C 0.9865(3) 0.6130(3) 0.85452(9) 0.0642(10) Uani 1 1 d . . . . . H26 H 1.0252 0.5635 0.8403 0.077 Uiso 1 1 calc R . . . . C26' C 0.2172(3) 0.5493(2) 0.49126(10) 0.0536(8) Uani 1 1 d . . . . . H26A H 0.1883 0.5594 0.5172 0.080 Uiso 1 1 calc GR . . . . H26B H 0.1638 0.5731 0.4724 0.080 Uiso 1 1 calc GR . . . . H26C H 0.2852 0.5874 0.4883 0.080 Uiso 1 1 calc GR . . . . C27 C 0.9958(4) 0.6156(4) 0.89544(10) 0.0844(14) Uani 1 1 d . U . . . H27 H 1.0425 0.5693 0.9081 0.101 Uiso 1 1 calc R . . . . C27' C 0.1316(3) 0.3764(3) 0.48821(10) 0.0522(7) Uani 1 1 d . . . . . H27A H 0.1444 0.3053 0.4822 0.078 Uiso 1 1 calc GR . . . . H27B H 0.0781 0.4042 0.4702 0.078 Uiso 1 1 calc GR . . . . H27C H 0.1036 0.3825 0.5145 0.078 Uiso 1 1 calc GR . . . . C28 C 0.9363(3) 0.6860(3) 0.91682(9) 0.0670(10) Uani 1 1 d . U . . . H28 H 0.9417 0.6867 0.9440 0.080 Uiso 1 1 calc R . . . . C28' C 0.3507(3) 0.2792(2) 0.50690(8) 0.0425(6) Uani 1 1 d . . . . . H28A H 0.3613 0.2642 0.4796 0.064 Uiso 1 1 calc GR . . . . H28B H 0.2867 0.2427 0.5164 0.064 Uiso 1 1 calc GR . . . . H28C H 0.4154 0.2582 0.5213 0.064 Uiso 1 1 calc GR . . . . C29 C 0.8686(3) 0.7559(2) 0.89791(8) 0.0430(7) Uani 1 1 d . . . . . H29 H 0.8275 0.8034 0.9123 0.052 Uiso 1 1 calc R . . . . C30 C 0.8620(2) 0.75488(19) 0.85722(7) 0.0331(5) Uani 1 1 d . . . . . H30 H 0.8176 0.8032 0.8446 0.040 Uiso 1 1 calc R . . . . N2 N 0.73319(17) 0.61010(16) 0.78064(5) 0.0304(4) Uani 1 1 d . . . . . H2 H 0.7135 0.5944 0.8041 0.037 Uiso 1 1 calc R . . . . O1 O 0.65013(15) 0.47382(13) 0.74973(5) 0.0347(4) Uani 1 1 d . . . . . O1' O 1.29720(14) 0.78049(14) 0.72827(5) 0.0349(4) Uani 1 1 d . . . . . H1' H 1.2933 0.8492 0.7385 0.042 Uiso 1 1 d R . . . . O2 O 0.49091(15) 0.79807(15) 0.68960(5) 0.0369(4) Uani 1 1 d . . . . . H2A H 0.4310 0.7868 0.7003 0.055 Uiso 1 1 calc GR . . . . O3 O 0.77690(13) 0.55300(12) 0.68226(4) 0.0264(3) Uani 1 1 d . . . . . O4 O 0.88822(15) 0.46932(13) 0.72491(5) 0.0343(4) Uani 1 1 d . . . . . O5 O 0.7545(2) 0.22468(14) 0.60526(5) 0.0489(5) 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 0.0318(12) 0.0340(12) 0.0231(11) 0.0058(10) 0.0004(10) -0.0021(11) C1' 0.0405(14) 0.0304(13) 0.0303(12) 0.0024(10) -0.0055(11) -0.0026(11) C2' 0.0433(14) 0.0324(13) 0.0347(13) 0.0012(11) -0.0072(11) -0.0029(11) C3 0.0375(13) 0.0317(12) 0.0151(10) -0.0019(9) 0.0024(9) -0.0018(10) C3' 0.0298(12) 0.0374(13) 0.0237(11) -0.0013(10) -0.0016(9) 0.0022(10) C4 0.0296(12) 0.0307(12) 0.0176(10) -0.0036(9) 0.0000(9) -0.0016(9) C4' 0.0318(12) 0.0346(13) 0.0299(12) 0.0000(10) -0.0005(10) 0.0043(10) C5 0.0339(12) 0.0269(11) 0.0157(10) -0.0037(9) 0.0044(9) -0.0027(10) C5' 0.0335(12) 0.0285(12) 0.0252(11) -0.0014(9) 0.0011(10) 0.0064(10) C6 0.0342(12) 0.0320(12) 0.0180(10) -0.0026(9) 0.0022(9) -0.0024(10) C6' 0.0397(13) 0.0290(12) 0.0270(12) 0.0023(10) -0.0005(10) 0.0058(11) C7 0.0331(12) 0.0336(12) 0.0179(11) -0.0021(9) 0.0012(9) -0.0037(10) C7' 0.0391(13) 0.0258(11) 0.0253(11) -0.0006(9) 0.0040(10) 0.0013(10) C8 0.0337(12) 0.0282(11) 0.0169(10) 0.0017(9) 0.0009(9) -0.0053(10) C8' 0.0386(13) 0.0268(12) 0.0219(11) -0.0003(9) 0.0064(10) 0.0007(10) C9 0.0334(12) 0.0286(11) 0.0160(10) -0.0030(9) 0.0040(9) -0.0031(10) C9' 0.0371(13) 0.0274(12) 0.0225(11) 0.0013(9) -0.0008(9) -0.0038(10) C10 0.0397(13) 0.0394(13) 0.0200(11) -0.0039(10) -0.0007(10) -0.0027(11) C10' 0.0391(13) 0.0274(12) 0.0210(11) 0.0014(9) 0.0006(10) -0.0023(10) C11 0.0359(13) 0.0320(12) 0.0294(12) -0.0066(10) 0.0013(10) -0.0042(10) C11' 0.0502(15) 0.0308(12) 0.0299(13) 0.0063(10) -0.0077(12) -0.0105(11) C12 0.0346(13) 0.0335(13) 0.0326(13) -0.0088(10) 0.0020(10) -0.0023(10) C12' 0.0541(16) 0.0266(12) 0.0319(13) 0.0073(10) -0.0133(12) -0.0093(11) C13 0.0353(12) 0.0324(13) 0.0223(11) 0.0053(10) 0.0000(10) -0.0069(10) C13' 0.0458(14) 0.0339(13) 0.0181(11) 0.0016(9) -0.0016(10) -0.0098(11) C14 0.0413(14) 0.0351(13) 0.0242(12) 0.0018(10) 0.0005(10) -0.0086(11) C14' 0.0422(14) 0.0276(12) 0.0200(11) 0.0003(9) 0.0052(10) -0.0026(10) C15 0.0446(14) 0.0354(13) 0.0272(12) 0.0014(10) -0.0021(11) -0.0122(12) C15' 0.0474(14) 0.0254(12) 0.0218(11) -0.0048(9) 0.0031(10) -0.0037(10) C16 0.0432(14) 0.0341(13) 0.0285(12) -0.0005(10) -0.0016(11) -0.0124(11) C16' 0.0507(15) 0.0289(12) 0.0200(11) -0.0042(9) 0.0021(10) -0.0078(11) C17 0.0680(19) 0.0361(14) 0.0271(13) 0.0012(11) 0.0070(13) -0.0072(14) C17' 0.0466(14) 0.0279(12) 0.0182(11) 0.0005(9) -0.0013(10) -0.0100(11) C18 0.0695(19) 0.0273(12) 0.0268(12) 0.0039(10) 0.0025(12) -0.0101(13) C18' 0.0561(17) 0.0576(18) 0.0220(12) 0.0054(12) 0.0020(12) -0.0225(15) C19 0.0679(18) 0.0307(13) 0.0264(13) 0.0023(10) -0.0004(13) -0.0087(13) C19' 0.0444(15) 0.0578(17) 0.0289(13) -0.0055(12) 0.0063(11) -0.0053(13) C20 0.0590(17) 0.0270(12) 0.0281(13) 0.0004(10) 0.0040(12) -0.0062(12) C20' 0.0571(17) 0.0385(14) 0.0231(12) 0.0069(10) -0.0072(11) -0.0149(13) C21 0.0463(14) 0.0249(11) 0.0215(11) -0.0030(9) 0.0015(10) -0.0042(11) C21' 0.066(2) 0.0402(16) 0.0513(17) 0.0185(13) -0.0290(16) -0.0121(15) C22 0.0429(13) 0.0229(11) 0.0238(11) 0.0001(9) 0.0014(10) 0.0010(10) C22' 0.0493(15) 0.0326(13) 0.0204(11) 0.0020(10) -0.0024(11) -0.0044(12) C23 0.0357(12) 0.0264(11) 0.0232(11) 0.0001(9) 0.0011(10) -0.0042(10) C23' 0.0456(15) 0.0370(13) 0.0223(11) -0.0023(10) 0.0046(11) -0.0059(12) C24 0.0594(19) 0.0443(17) 0.0524(18) -0.0122(14) -0.0109(15) -0.0115(15) C24' 0.0471(14) 0.0359(13) 0.0192(11) -0.0041(10) 0.0015(10) -0.0066(11) C25 0.0419(14) 0.0483(15) 0.0219(12) -0.0031(11) -0.0057(10) -0.0041(12) C25' 0.0493(15) 0.0394(14) 0.0245(12) -0.0011(10) 0.0034(11) -0.0025(12) C26 0.083(2) 0.082(2) 0.0273(14) -0.0024(15) -0.0047(15) 0.037(2) C26' 0.072(2) 0.0414(16) 0.0475(17) 0.0024(13) -0.0041(16) -0.0002(15) C27 0.117(3) 0.108(3) 0.0288(16) 0.0004(18) -0.0102(19) 0.056(3) C27' 0.0485(17) 0.0521(18) 0.0559(18) 0.0047(15) -0.0042(14) -0.0031(14) C28 0.095(3) 0.084(2) 0.0222(14) -0.0032(15) -0.0074(15) 0.025(2) C28' 0.0529(17) 0.0369(14) 0.0379(14) -0.0092(11) 0.0006(13) -0.0059(13) C29 0.0592(17) 0.0474(16) 0.0225(13) -0.0046(11) -0.0008(12) -0.0012(14) C30 0.0480(15) 0.0291(12) 0.0223(12) 0.0003(9) -0.0015(11) -0.0066(11) N2 0.0399(11) 0.0373(11) 0.0142(9) 0.0036(8) 0.0031(8) -0.0036(9) O1 0.0402(9) 0.0345(9) 0.0293(9) 0.0096(7) -0.0022(7) -0.0086(8) O1' 0.0383(9) 0.0369(9) 0.0294(9) -0.0052(7) -0.0077(8) 0.0047(8) O2 0.0349(9) 0.0401(10) 0.0358(10) -0.0004(8) -0.0058(8) -0.0020(8) O3 0.0358(9) 0.0239(8) 0.0194(7) -0.0027(6) 0.0007(6) -0.0014(7) O4 0.0438(10) 0.0356(9) 0.0234(8) 0.0007(7) -0.0027(7) 0.0018(8) O5 0.0892(16) 0.0275(9) 0.0300(9) -0.0066(8) 0.0050(10) -0.0137(10) 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 N2 C1 C9 107.42(19) . . ? O1 C1 C9 125.4(2) . . ? O1 C1 N2 127.1(2) . . ? H1'A C1' H1'B 107.5 . . ? C2' C1' H1'A 108.5 . . ? C2' C1' H1'B 108.5 . . ? C2' C1' C10' 115.0(2) . . ? C10' C1' H1'A 108.5 . . ? C10' C1' H1'B 108.5 . . ? C1' C2' H2'A 109.5 . . ? C1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 108.1 . . ? C3' C2' C1' 110.6(2) . . ? C3' C2' H2'A 109.5 . . ? C3' C2' H2'B 109.5 . . ? C4 C3 H3 109.7 . . ? C10 C3 H3 109.7 . . ? C10 C3 C4 111.58(19) . . ? N2 C3 H3 109.7 . . ? N2 C3 C4 104.23(18) . . ? N2 C3 C10 111.79(19) . . ? C2' C3' H3' 109.5 . . ? C2' C3' C4' 109.4(2) . . ? C4' C3' H3' 109.5 . . ? O1' C3' C2' 111.9(2) . . ? O1' C3' H3' 109.5 . . ? O1' C3' C4' 106.89(19) . . ? C3 C4 H4 108.5 . . ? C5 C4 C3 112.64(18) . . ? C5 C4 H4 108.5 . . ? C9 C4 C3 105.11(18) . . ? C9 C4 H4 108.5 . . ? C9 C4 C5 113.36(18) . . ? C3' C4' H4'A 108.9 . . ? C3' C4' H4'B 108.9 . . ? H4'A C4' H4'B 107.7 . . ? C5' C4' C3' 113.5(2) . . ? C5' C4' H4'A 108.9 . . ? C5' C4' H4'B 108.9 . . ? C4 C5 H5 106.9 . . ? C6 C5 C4 110.67(19) . . ? C6 C5 H5 106.9 . . ? C6 C5 C11 113.56(19) . . ? C11 C5 C4 111.55(19) . . ? C11 C5 H5 106.9 . . ? C4' C5' C10' 117.4(2) . . ? C6' C5' C4' 120.6(2) . . ? C6' C5' C10' 121.7(2) . . ? C5 C6 C7 116.01(19) . . ? C12 C6 C5 125.1(2) . . ? C12 C6 C7 118.9(2) . . ? C5' C6' H6' 117.2 . . ? C5' C6' C7' 125.6(2) . . ? C7' C6' H6' 117.2 . . ? C6 C7 H7 108.8 . . ? C6 C7 C8 113.37(19) . . ? C8 C7 H7 108.8 . . ? O2 C7 C6 109.05(19) . . ? O2 C7 H7 108.8 . . ? O2 C7 C8 107.88(18) . . ? C6' C7' H7' 106.1 . . ? C6' C7' C8' 113.2(2) . . ? C6' C7' C22 113.55(19) . . ? C8' C7' H7' 106.1 . . ? C8' C7' C22 111.1(2) . . ? C22 C7' H7' 106.1 . . ? C7 C8 H8 106.7 . . ? C7 C8 C9 111.94(18) . . ? C9 C8 H8 106.7 . . ? C13 C8 C7 111.3(2) . . ? C13 C8 H8 106.7 . . ? C13 C8 C9 113.02(19) . . ? C7' C8' C9' 118.6(2) . . ? C14' C8' C7' 116.7(2) . . ? C14' C8' C9' 124.2(2) . . ? C1 C9 C4 105.12(17) . . ? C1 C9 C8 111.86(19) . . ? C4 C9 C8 114.05(19) . . ? O3 C9 C1 111.46(18) . . ? O3 C9 C4 112.21(18) . . ? O3 C9 C8 102.36(16) . . ? C8' C9' H9' 105.4 . . ? C8' C9' C10' 113.4(2) . . ? C8' C9' C11' 110.0(2) . . ? C10' C9' H9' 105.4 . . ? C11' C9' H9' 105.4 . . ? C11' C9' C10' 116.1(2) . . ? C3 C10 H10A 108.6 . . ? C3 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C25 C10 C3 114.7(2) . . ? C25 C10 H10A 108.6 . . ? C25 C10 H10B 108.6 . . ? C1' C10' C9' 107.6(2) . . ? C5' C10' C1' 110.55(19) . . ? C5' C10' C9' 108.84(19) . . ? C5' C10' C19' 107.2(2) . . ? C19' C10' C1' 110.8(2) . . ? C19' C10' C9' 111.9(2) . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9' C11' H11D 109.2 . . ? C9' C11' H11E 109.2 . . ? C9' C11' C12' 111.9(2) . . ? H11D C11' H11E 107.9 . . ? C12' C11' H11D 109.2 . . ? C12' C11' H11E 109.2 . . ? C6 C12 H12A 120.0 . . ? C6 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? C11' C12' H12C 109.2 . . ? C11' C12' H12D 109.2 . . ? C11' C12' C13' 112.1(2) . . ? H12C C12' H12D 107.9 . . ? C13' C12' H12C 109.2 . . ? C13' C12' H12D 109.2 . . ? C8 C13 H13 117.8 . . ? C14 C13 C8 124.4(2) . . ? C14 C13 H13 117.8 . . ? C12' C13' C17' 115.1(2) . . ? C14' C13' C12' 107.75(19) . . ? C14' C13' C17' 100.09(19) . . ? C14' C13' C18' 110.7(2) . . ? C18' C13' C12' 110.8(2) . . ? C18' C13' C17' 111.9(2) . . ? C13 C14 H14 116.6 . . ? C13 C14 C15 126.8(2) . . ? C15 C14 H14 116.6 . . ? C8' C14' C13' 126.1(2) . . ? C8' C14' C15' 120.8(2) . . ? C15' C14' C13' 111.6(2) . . ? C14 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C14 C15 C16 110.3(2) . . ? H15A C15 H15B 108.1 . . ? C16 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14' C15' H15' 110.9 . . ? C14' C15' C16' 103.27(19) . . ? C14' C15' C21 108.63(18) . . ? C16' C15' H15' 110.9 . . ? C16' C15' C21 112.0(2) . . ? C21 C15' H15' 110.9 . . ? C15 C16 H16 107.0 . . ? C17 C16 C15 110.0(2) . . ? C17 C16 H16 107.0 . . ? C17 C16 C24 113.1(2) . . ? C24 C16 C15 112.3(2) . . ? C24 C16 H16 107.0 . . ? C15' C16' H16A 110.6 . . ? C15' C16' H16B 110.6 . . ? C15' C16' C17' 105.79(19) . . ? H16A C16' H16B 108.7 . . ? C17' C16' H16A 110.6 . . ? C17' C16' H16B 110.6 . . ? C16 C17 H17A 108.3 . . ? C16 C17 H17B 108.3 . . ? C16 C17 C18 116.0(2) . . ? H17A C17 H17B 107.4 . . ? C18 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C13' C17' H17' 106.6 . . ? C16' C17' C13' 103.3(2) . . ? C16' C17' H17' 106.6 . . ? C20' C17' C13' 119.6(2) . . ? C20' C17' C16' 113.4(2) . . ? C20' C17' H17' 106.6 . . ? C17 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C19 C18 C17 114.1(2) . . ? C19 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C13' C18' H18C 109.5 . . ? C13' C18' H18D 109.5 . . ? C13' C18' H18E 109.5 . . ? H18C C18' H18D 109.5 . . ? H18C C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C18 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C18 C19 C20 114.4(2) . . ? H19A C19 H19B 107.6 . . ? C20 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? C10' C19' H19C 109.5 . . ? C10' C19' H19D 109.5 . . ? C10' C19' H19E 109.5 . . ? H19C C19' H19D 109.5 . . ? H19C C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C21 C20 C19 117.2(2) . . ? O5 C20 C19 120.9(2) . . ? O5 C20 C21 121.9(2) . . ? C17' C20' H20' 108.2 . . ? C17' C20' C21' 113.2(2) . . ? C21' C20' H20' 108.2 . . ? C22' C20' C17' 110.6(2) . . ? C22' C20' H20' 108.2 . . ? C22' C20' C21' 108.2(3) . . ? C15' C21 H21 106.1 . . ? C15' C21 C22 114.1(2) . . ? C20 C21 C15' 113.20(19) . . ? C20 C21 H21 106.1 . . ? C20 C21 C22 110.5(2) . . ? C22 C21 H21 106.1 . . ? C20' C21' H21A 109.5 . . ? C20' C21' H21B 109.5 . . ? C20' C21' H21C 109.5 . . ? H21A C21' H21B 109.5 . . ? H21A C21' H21C 109.5 . . ? H21B C21' H21C 109.5 . . ? C7' C22 C21 111.63(19) . . ? C7' C22 H22 107.3 . . ? C21 C22 H22 107.3 . . ? C23 C22 C7' 108.73(19) . . ? C23 C22 C21 114.1(2) . . ? C23 C22 H22 107.3 . . ? C20' C22' H22' 117.0 . . ? C23' C22' C20' 126.0(2) . . ? C23' C22' H22' 117.0 . . ? O3 C23 C22 111.25(19) . . ? O4 C23 C22 124.8(2) . . ? O4 C23 O3 123.9(2) . . ? C22' C23' H23' 116.4 . . ? C22' C23' C24' 127.1(2) . . ? C24' C23' H23' 116.4 . . ? C16 C24 H24A 109.5 . . ? C16 C24 H24B 109.5 . . ? C16 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23' C24' H24' 108.2 . . ? C23' C24' C25' 111.2(2) . . ? C23' C24' C28' 109.9(2) . . ? C25' C24' H24' 108.2 . . ? C28' C24' H24' 108.2 . . ? C28' C24' C25' 111.2(2) . . ? C26 C25 C10 119.8(3) . . ? C26 C25 C30 118.1(2) . . ? C30 C25 C10 122.0(2) . . ? C24' C25' H25' 107.5 . . ? C26' C25' C24' 111.6(2) . . ? C26' C25' H25' 107.5 . . ? C27' C25' C24' 113.5(2) . . ? C27' C25' H25' 107.5 . . ? C27' C25' C26' 109.0(3) . . ? C25 C26 H26 119.6 . . ? C25 C26 C27 120.7(3) . . ? C27 C26 H26 119.6 . . ? C25' C26' H26A 109.5 . . ? C25' C26' H26B 109.5 . . ? C25' C26' H26C 109.5 . . ? H26A C26' H26B 109.5 . . ? H26A C26' H26C 109.5 . . ? H26B C26' H26C 109.5 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.9 . . ? C25' C27' H27A 109.5 . . ? C25' C27' H27B 109.5 . . ? C25' C27' H27C 109.5 . . ? H27A C27' H27B 109.5 . . ? H27A C27' H27C 109.5 . . ? H27B C27' H27C 109.5 . . ? C27 C28 H28 120.1 . . ? C27 C28 C29 119.9(3) . . ? C29 C28 H28 120.1 . . ? C24' C28' H28A 109.5 . . ? C24' C28' H28B 109.5 . . ? C24' C28' H28C 109.5 . . ? H28A C28' H28B 109.5 . . ? H28A C28' H28C 109.5 . . ? H28B C28' H28C 109.5 . . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.6(3) . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 121.5(3) . . ? C25 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C1 N2 C3 116.00(18) . . ? C1 N2 H2 122.0 . . ? C3 N2 H2 122.0 . . ? C3' O1' H1' 109.2 . . ? C7 O2 H2A 109.5 . . ? C23 O3 C9 119.41(17) . . ? 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 C9 1.538(3) . ? C1 N2 1.343(3) . ? C1 O1 1.215(3) . ? C1' H1'A 0.9700 . ? C1' H1'B 0.9700 . ? C1' C2' 1.525(4) . ? C1' C10' 1.545(3) . ? C2' H2'A 0.9700 . ? C2' H2'B 0.9700 . ? C2' C3' 1.508(3) . ? C3 H3 0.9800 . ? C3 C4 1.560(3) . ? C3 C10 1.526(3) . ? C3 N2 1.452(3) . ? C3' H3' 0.9800 . ? C3' C4' 1.510(3) . ? C3' O1' 1.438(3) . ? C4 H4 0.9800 . ? C4 C5 1.544(3) . ? C4 C9 1.542(3) . ? C4' H4'A 0.9700 . ? C4' H4'B 0.9700 . ? C4' C5' 1.503(3) . ? C5 H5 0.9800 . ? C5 C6 1.505(3) . ? C5 C11 1.528(3) . ? C5' C6' 1.328(4) . ? C5' C10' 1.533(3) . ? C6 C7 1.527(3) . ? C6 C12 1.320(3) . ? C6' H6' 0.9300 . ? C6' C7' 1.496(4) . ? C7 H7 0.9800 . ? C7 C8 1.531(3) . ? C7 O2 1.427(3) . ? C7' H7' 0.9800 . ? C7' C8' 1.503(3) . ? C7' C22 1.562(3) . ? C8 H8 0.9800 . ? C8 C9 1.551(3) . ? C8 C13 1.501(3) . ? C8' C9' 1.510(3) . ? C8' C14' 1.327(4) . ? C9 O3 1.454(3) . ? C9' H9' 0.9800 . ? C9' C10' 1.548(3) . ? C9' C11' 1.528(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C25 1.514(3) . ? C10' C19' 1.540(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11' H11D 0.9700 . ? C11' H11E 0.9700 . ? C11' C12' 1.538(4) . ? C12 H12A 0.9300 . ? C12 H12B 0.9300 . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C12' C13' 1.548(4) . ? C13 H13 0.9300 . ? C13 C14 1.318(3) . ? C13' C14' 1.520(3) . ? C13' C17' 1.561(3) . ? C13' C18' 1.537(3) . ? C14 H14 0.9300 . ? C14 C15 1.505(3) . ? C14' C15' 1.513(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.553(4) . ? C15' H15' 0.9800 . ? C15' C16' 1.542(4) . ? C15' C21 1.554(3) . ? C16 H16 0.9800 . ? C16 C17 1.520(4) . ? C16 C24 1.521(4) . ? C16' H16A 0.9700 . ? C16' H16B 0.9700 . ? C16' C17' 1.543(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.535(4) . ? C17' H17' 0.9800 . ? C17' C20' 1.538(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.523(4) . ? C18' H18C 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.530(3) . ? C19' H19C 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C20 C21 1.525(3) . ? C20 O5 1.209(3) . ? C20' H20' 0.9800 . ? C20' C21' 1.540(4) . ? C20' C22' 1.513(4) . ? C21 H21 0.9800 . ? C21 C22 1.566(3) . ? C21' H21A 0.9600 . ? C21' H21B 0.9600 . ? C21' H21C 0.9600 . ? C22 H22 0.9800 . ? C22 C23 1.513(3) . ? C22' H22' 0.9300 . ? C22' C23' 1.313(4) . ? C23 O3 1.350(3) . ? C23 O4 1.206(3) . ? C23' H23' 0.9300 . ? C23' C24' 1.508(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24' H24' 0.9800 . ? C24' C25' 1.547(4) . ? C24' C28' 1.537(4) . ? C25 C26 1.380(4) . ? C25 C30 1.391(4) . ? C25' H25' 0.9800 . ? C25' C26' 1.523(4) . ? C25' C27' 1.516(4) . ? C26 H26 0.9300 . ? C26 C27 1.402(4) . ? C26' H26A 0.9600 . ? C26' H26B 0.9600 . ? C26' H26C 0.9600 . ? C27 H27 0.9300 . ? C27 C28 1.372(5) . ? C27' H27A 0.9600 . ? C27' H27B 0.9600 . ? C27' H27C 0.9600 . ? C28 H28 0.9300 . ? C28 C29 1.380(5) . ? C28' H28A 0.9600 . ? C28' H28B 0.9600 . ? C28' H28C 0.9600 . ? C29 H29 0.9300 . ? C29 C30 1.391(4) . ? C30 H30 0.9300 . ? N2 H2 0.8600 . ? O1' H1' 0.9602 . ? O2 H2A 0.8200 . ? 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 O1' H1' O1 0.96 1.80 2.700(2) 154.0 3_756 O2 H2A O1' 0.82 1.87 2.684(3) 171.3 1_455 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 C1 C9 O3 C23 -42.8(3) . . . . ? C1' C2' C3' C4' 59.9(3) . . . . ? C1' C2' C3' O1' 178.2(2) . . . . ? C2' C1' C10' C5' 43.2(3) . . . . ? C2' C1' C10' C9' 161.9(2) . . . . ? C2' C1' C10' C19' -75.5(3) . . . . ? C2' C3' C4' C5' -55.5(3) . . . . ? C3 C4 C5 C6 -63.9(2) . . . . ? C3 C4 C5 C11 63.5(2) . . . . ? C3 C4 C9 C1 -12.2(2) . . . . ? C3 C4 C9 C8 110.7(2) . . . . ? C3 C4 C9 O3 -133.51(19) . . . . ? C3 C10 C25 C26 137.4(3) . . . . ? C3 C10 C25 C30 -46.9(4) . . . . ? C3' C4' C5' C6' -138.9(2) . . . . ? C3' C4' C5' C10' 46.4(3) . . . . ? C4 C3 C10 C25 178.9(2) . . . . ? C4 C3 N2 C1 4.0(3) . . . . ? C4 C5 C6 C7 -43.9(2) . . . . ? C4 C5 C6 C12 137.4(2) . . . . ? C4 C9 O3 C23 74.8(2) . . . . ? C4' C5' C6' C7' -172.1(2) . . . . ? C4' C5' C10' C1' -38.6(3) . . . . ? C4' C5' C10' C9' -156.5(2) . . . . ? C4' C5' C10' C19' 82.3(3) . . . . ? C5 C4 C9 C1 -135.63(19) . . . . ? C5 C4 C9 C8 -12.8(3) . . . . ? C5 C4 C9 O3 103.1(2) . . . . ? C5 C6 C7 C8 -9.1(3) . . . . ? C5 C6 C7 O2 -129.3(2) . . . . ? C5' C6' C7' C8' -13.2(3) . . . . ? C5' C6' C7' C22 -141.1(2) . . . . ? C6 C7 C8 C9 52.1(2) . . . . ? C6 C7 C8 C13 179.64(19) . . . . ? C6' C5' C10' C1' 146.7(2) . . . . ? C6' C5' C10' C9' 28.8(3) . . . . ? C6' C5' C10' C19' -92.4(3) . . . . ? C6' C7' C8' C9' -10.0(3) . . . . ? C6' C7' C8' C14' 178.0(2) . . . . ? C6' C7' C22 C21 169.8(2) . . . . ? C6' C7' C22 C23 43.0(3) . . . . ? C7 C8 C9 C1 79.0(2) . . . . ? C7 C8 C9 C4 -40.1(2) . . . . ? C7 C8 C9 O3 -161.52(17) . . . . ? C7 C8 C13 C14 127.2(3) . . . . ? C7' C8' C9' C10' 41.4(3) . . . . ? C7' C8' C9' C11' 173.3(2) . . . . ? C7' C8' C14' C13' 173.8(2) . . . . ? C7' C8' C14' C15' 9.1(3) . . . . ? C7' C22 C23 O3 84.6(2) . . . . ? C7' C22 C23 O4 -92.4(3) . . . . ? C8 C9 O3 C23 -162.53(18) . . . . ? C8 C13 C14 C15 172.1(2) . . . . ? C8' C7' C22 C21 40.9(3) . . . . ? C8' C7' C22 C23 -85.9(2) . . . . ? C8' C9' C10' C1' -168.48(19) . . . . ? C8' C9' C10' C5' -48.7(3) . . . . ? C8' C9' C10' C19' 69.6(3) . . . . ? C8' C9' C11' C12' 43.9(3) . . . . ? C8' C14' C15' C16' 160.8(2) . . . . ? C8' C14' C15' C21 41.7(3) . . . . ? C9 C1 N2 C3 -12.1(3) . . . . ? C9 C4 C5 C6 55.3(2) . . . . ? C9 C4 C5 C11 -177.26(18) . . . . ? C9 C8 C13 C14 -105.8(3) . . . . ? C9' C8' C14' C13' 2.2(4) . . . . ? C9' C8' C14' C15' -162.4(2) . . . . ? C9' C11' C12' C13' -62.5(3) . . . . ? C10 C3 C4 C5 -109.5(2) . . . . ? C10 C3 C4 C9 126.6(2) . . . . ? C10 C3 N2 C1 -116.7(2) . . . . ? C10 C25 C26 C27 174.6(4) . . . . ? C10 C25 C30 C29 -176.3(3) . . . . ? C10' C1' C2' C3' -55.8(3) . . . . ? C10' C5' C6' C7' 2.5(4) . . . . ? C10' C9' C11' C12' 174.4(2) . . . . ? C11 C5 C6 C7 -170.22(19) . . . . ? C11 C5 C6 C12 11.0(3) . . . . ? C11' C9' C10' C1' 62.7(3) . . . . ? C11' C9' C10' C5' -177.5(2) . . . . ? C11' C9' C10' C19' -59.3(3) . . . . ? C11' C12' C13' C14' 45.7(3) . . . . ? C11' C12' C13' C17' 156.3(2) . . . . ? C11' C12' C13' C18' -75.5(3) . . . . ? C12 C6 C7 C8 169.7(2) . . . . ? C12 C6 C7 O2 49.5(3) . . . . ? C12' C13' C14' C8' -17.3(3) . . . . ? C12' C13' C14' C15' 148.6(2) . . . . ? C12' C13' C17' C16' -153.68(19) . . . . ? C12' C13' C17' C20' 79.2(3) . . . . ? C13 C8 C9 C1 -47.6(3) . . . . ? C13 C8 C9 C4 -166.76(18) . . . . ? C13 C8 C9 O3 71.8(2) . . . . ? C13 C14 C15 C16 -103.0(3) . . . . ? C13' C14' C15' C16' -5.9(2) . . . . ? C13' C14' C15' C21 -125.0(2) . . . . ? C13' C17' C20' C21' -57.1(3) . . . . ? C13' C17' C20' C22' -178.8(2) . . . . ? C14 C15 C16 C17 86.9(3) . . . . ? C14 C15 C16 C24 -146.1(2) . . . . ? C14' C8' C9' C10' -147.2(2) . . . . ? C14' C8' C9' C11' -15.3(3) . . . . ? C14' C13' C17' C16' -38.5(2) . . . . ? C14' C13' C17' C20' -165.7(2) . . . . ? C14' C15' C16' C17' -19.4(2) . . . . ? C14' C15' C21 C20 -175.7(2) . . . . ? C14' C15' C21 C22 -48.1(3) . . . . ? C15 C16 C17 C18 -165.8(2) . . . . ? C15' C16' C17' C13' 37.0(2) . . . . ? C15' C16' C17' C20' 168.0(2) . . . . ? C15' C21 C22 C7' 8.1(3) . . . . ? C15' C21 C22 C23 131.9(2) . . . . ? C16 C17 C18 C19 75.7(3) . . . . ? C16' C15' C21 C20 70.9(3) . . . . ? C16' C15' C21 C22 -161.50(19) . . . . ? C16' C17' C20' C21' -179.4(2) . . . . ? C16' C17' C20' C22' 59.0(3) . . . . ? C17 C18 C19 C20 -78.0(3) . . . . ? C17' C13' C14' C8' -137.9(2) . . . . ? C17' C13' C14' C15' 28.0(2) . . . . ? C17' C20' C22' C23' -133.0(3) . . . . ? C18 C19 C20 C21 121.1(3) . . . . ? C18 C19 C20 O5 -57.9(4) . . . . ? C18' C13' C14' C8' 104.0(3) . . . . ? C18' C13' C14' C15' -90.2(2) . . . . ? C18' C13' C17' C16' 78.7(2) . . . . ? C18' C13' C17' C20' -48.4(3) . . . . ? C19 C20 C21 C15' -179.1(2) . . . . ? C19 C20 C21 C22 51.5(3) . . . . ? C20 C21 C22 C7' 137.1(2) . . . . ? C20 C21 C22 C23 -99.1(2) . . . . ? C20' C22' C23' C24' -177.5(3) . . . . ? C21 C15' C16' C17' 97.3(2) . . . . ? C21 C22 C23 O3 -40.8(3) . . . . ? C21 C22 C23 O4 142.3(2) . . . . ? C21' C20' C22' C23' 102.5(3) . . . . ? C22 C7' C8' C9' 119.2(2) . . . . ? C22 C7' C8' C14' -52.8(3) . . . . ? C22 C23 O3 C9 -179.65(18) . . . . ? C22' C23' C24' C25' 121.3(3) . . . . ? C22' C23' C24' C28' -115.3(3) . . . . ? C23' C24' C25' C26' -60.3(3) . . . . ? C23' C24' C25' C27' 176.0(2) . . . . ? C24 C16 C17 C18 67.7(3) . . . . ? C25 C26 C27 C28 2.2(8) . . . . ? C26 C25 C30 C29 -0.5(4) . . . . ? C26 C27 C28 C29 -1.2(7) . . . . ? C27 C28 C29 C30 -0.6(6) . . . . ? C28 C29 C30 C25 1.5(5) . . . . ? C28' C24' C25' C26' 176.9(2) . . . . ? C28' C24' C25' C27' 53.3(3) . . . . ? C30 C25 C26 C27 -1.3(6) . . . . ? N2 C1 C9 C4 14.9(3) . . . . ? N2 C1 C9 C8 -109.4(2) . . . . ? N2 C1 C9 O3 136.7(2) . . . . ? N2 C3 C4 C5 129.7(2) . . . . ? N2 C3 C4 C9 5.8(2) . . . . ? N2 C3 C10 C25 -64.9(3) . . . . ? O1 C1 C9 C4 -169.0(2) . . . . ? O1 C1 C9 C8 66.7(3) . . . . ? O1 C1 C9 O3 -47.2(3) . . . . ? O1 C1 N2 C3 171.9(2) . . . . ? O1' C3' C4' C5' -176.92(19) . . . . ? O2 C7 C8 C9 172.93(18) . . . . ? O2 C7 C8 C13 -59.5(2) . . . . ? O4 C23 O3 C9 -2.7(3) . . . . ? O5 C20 C21 C15' -0.1(4) . . . . ? O5 C20 C21 C22 -129.5(3) . . . . ? 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 0.015 0.049 0.105 194.5 42.8 ? 2 -0.015 0.549 0.395 194.5 42.7 ? 3 0.515 0.451 0.895 194.5 42.7 ? 4 0.485 -0.049 0.605 194.5 42.8 ?