#------------------------------------------------------------------------------ #$Date: 2020-05-13 02:19:07 +0300 (Wed, 13 May 2020) $ #$Revision: 251996 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038351.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_4038351 loop_ _publ_author_name 'Ruggeri, Michele' 'Dombrowski, Amanda W.' 'Djuric, Stevan W.' 'Baxendale, Ian R.' _publ_section_title ; A rearrangement of 3-hydroxyazetidines into 2-oxazolines. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00656 _journal_year 2020 _chemical_formula_moiety 'C37 H40 N4 O6 S2, 0.316(C H4 O)' _chemical_formula_sum 'C37.32 H41.26 N4 O6.32 S2' _chemical_formula_weight 710.98 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2020-02-09 _audit_creation_method ; Olex2 1.3-alpha (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020) ; _cell_angle_alpha 90 _cell_angle_beta 96.410(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.8945(9) _cell_length_b 21.4091(15) _cell_length_c 28.158(2) _cell_measurement_reflns_used 9324 _cell_measurement_temperature 120 _cell_measurement_theta_max 29.57 _cell_measurement_theta_min 2.38 _cell_volume 7125.6(9) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_collection 'APEX3 v.2019.1-0 (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _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, 2015a)' _diffrn_ambient_temperature 120 _diffrn_detector 'Bruker PHOTON 100 CMOS' _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 139564 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.000 _diffrn_reflns_theta_min 1.944 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker, 2016) was used for absorption correction. wR2(int) was 0.1338 before and 0.0432 after correction. The Ratio of minimum to maximum transmission is 0.9593. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_description tablet _exptl_crystal_F_000 3006 _exptl_crystal_size_max 0.475 _exptl_crystal_size_mid 0.246 _exptl_crystal_size_min 0.138 _refine_diff_density_max 0.522 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.062 _refine_ls_extinction_coef 0.00100(16) _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, 2015a)' _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 962 _refine_ls_number_reflns 19071 _refine_ls_number_restraints 162 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0522 _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^)+(0.0455P)^2^+6.0690P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1222 _refine_ls_wR_factor_ref 0.1309 _reflns_Friedel_coverage 0.000 _reflns_number_gt 15076 _reflns_number_total 19071 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 20srv039.cif _cod_data_source_block 20srv039 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 7125.5(9) _cod_database_code 4038351 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.9863(3) 0.0137(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.3 times of: All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 3. Restrained distances N1B-C8 \\sim N1A-C8 with sigma of 0.02 S1B-O1B \\sim S1A-O1A with sigma of 0.02 S1B-N1B \\sim S1A-N1A with sigma of 0.02 S1A-O2A \\sim S1B-O2B with sigma of 0.02 S1B-C1B \\sim S1A-C1A with sigma of 0.02 S2A-N2 \\sim S2B-N2 with sigma of 0.02 S2A-O4A \\sim S2B-O4B \\sim S2A-O3A \\sim S2B-O3B with sigma of 0.02 4. Uiso/Uaniso restraints and constraints Uanis(N1A) = Uanis(N1B) Uanis(C1B) = Uanis(C1A) Uanis(C7A) = Uanis(C7B) Uanis(C4A) = Uanis(C4B) Uanis(C3A) = Uanis(C3B) Uanis(C6A) = Uanis(C6B) Uanis(C5A) = Uanis(C5B) Uanis(C2A) = Uanis(C2B) Uanis(S2B) = Uanis(S2A) Uanis(O4B) = Uanis(O4A) Uanis(O3B) = Uanis(O3A) Uanis(O2B) = Uanis(O2A) 5. Rigid body (RIGU) restrains N1A, S1A, O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A, C7A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1B, S1B, O1B, O2B, C1B, C6B, C5B, C4B, C3B, C2B, C7B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(H8A)=Sof(H8B)=Sof(S1B)=Sof(S2B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)= Sof(N1B)=Sof(H1B)=Sof(C1B)=Sof(C6B)=Sof(H6B)=Sof(C5B)=Sof(H5B)=Sof(C4B)= Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=1- FVAR(1) Sof(H8AA)=Sof(H8AB)=Sof(S1A)=Sof(S2A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)= Sof(N1A)=Sof(H1A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)= Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)= Sof(O1S)=Sof(H1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(1) 7.a Riding coordinates: N1A(H1A), C7A(H7AA,H7AB,H7AC), N1B(H1B), C7B(H7BA,H7BB,H7BC), O1S(H1S) 7.b Secondary CH2 refined with riding coordinates: C8'(H8'A,H8'B), C10'(H10A,H10B), C18'(H18A,H18B), C19'(H19A,H19B), C20'(H20A, H20B), C23'(H23A,H23B), C24'(H24A,H24B), C8(H8AA,H8AB), C8(H8A,H8B), C10(H10C, H10D), C18(H18C,H18D), C19(H19C,H19D), C20(H20C,H20D), C23(H23C,H23D), C24(H24C,H24D) 7.c Aromatic/amide H refined with riding coordinates: C2'(H2'A), C3'(H3'), C5'(H5'), C6'(H6'), C12'(H12'), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'), C32'(H32'), C33'(H33'), C35'(H35'), C36'(H36'), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C6B(H6B), C5B(H5B), C3B(H3B), C2B(H2B) 7.d Fitted hexagon refined as free rotating group: C1B(C6B,C5B,C4B,C3B,C2B) 7.e Idealised Me refined as rotating group: C7'(H7'A,H7'B,H7'C), C37'(H37A,H37B,H37C), C37(H37D,H37E,H37F), C1S(H1SA,H1SB, H1SC) ; _oslims_operator_name 'Dr A Batsanov' _oslims_operator_uuid 642c0cab-15e1-4db6-aabf-d1e3f44b6814 _oslims_submitter_name 'Mr Michele Ruggeri' _oslims_submitter_uuid 1a56f251-525c-414f-9d37-3e740585b168 _shelx_estimated_absorpt_t_min 0.910 _shelx_estimated_absorpt_t_max 0.973 _shelx_res_checksum 35473 _shelx_res_file ; TITL 20srv039_a.res in P2(1)/c 20srv039.res created by SHELXL-2018/3 at 21:15:38 on 09-Feb-2020 REM Old TITL 20srv039 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.213, Rweak 0.017, Alpha 0.040 REM 1.688 for 416 systematic absences, Orientation as input REM Formula found by SHELXT: C75 N8 O12 S4 CELL 0.71073 11.8945 21.4091 28.1577 90 96.41 90 ZERR 8 0.0009 0.0015 0.002 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 298.53 330.12 32 50.53 16 SADI N1B C8 N1A C8 SADI S1B O1B S1A O1A SADI S1B N1B S1A N1A EADP N1A N1B SADI S1A O2A S1B O2B SADI S1B C1B S1A C1A EADP C1B C1A EADP C7A C7B EADP C4A C4B EADP C3A C3B EADP C6A C6B EADP C5A C5B EADP C2A C2B RIGU N1A S1A O1A O2A C1A > C7A RIGU N1B S1B O1B O2B C1B > C7B SADI S2A N2 S2B N2 SADI S2A O4A S2B O4B S2A O3A S2B O3B EADP S2B S2A EADP O4B O4A EADP O3B O3A EADP O2B O2A L.S. 7 PLAN 10 SIZE 0.138 0.246 0.475 TEMP -153.15 CONF HTAB O1S O3A HTAB N2' N3' HTAB N2 N3 HTAB N1A O1S HTAB N1' O3' HTAB N1B O3B BOND list 4 MORE -1 BOND $H fmap 2 53 acta TWIN -1 0 0 0 -1 0 0.5 0 1 2 OMIT -3 58 OMIT -1 3 2 OMIT 0 2 0 OMIT 1 1 0 OMIT 0 20 1 OMIT 1 4 1 OMIT 3 7 7 REM REM REM WGHT 0.045500 6.069000 EXTI 0.001003 BASF 0.01366 FVAR 0.27717 0.63279 S1' 5 0.576898 0.349212 -0.023110 11.00000 0.02630 0.03236 = 0.02101 0.00037 0.00093 0.00170 S2' 5 0.784905 0.449638 0.142088 11.00000 0.01515 0.01756 = 0.01951 0.00200 0.00176 0.00158 O1' 4 0.653321 0.395687 -0.037109 11.00000 0.03182 0.04955 = 0.02949 0.01112 0.00516 -0.00293 O2' 4 0.571712 0.289412 -0.045939 11.00000 0.04097 0.04449 = 0.03359 -0.01398 0.00083 0.00672 O3' 4 0.782423 0.424751 0.094512 11.00000 0.02452 0.02314 = 0.02051 0.00053 0.00407 0.00321 O4' 4 0.877810 0.488541 0.160689 11.00000 0.01695 0.02578 = 0.02916 0.00071 0.00114 -0.00330 O5' 4 0.766416 0.207599 0.071820 11.00000 0.02304 0.02374 = 0.03804 -0.00524 0.00689 0.00051 O6' 4 0.990871 0.298775 0.232310 11.00000 0.01645 0.02599 = 0.04389 -0.00096 -0.00100 0.00252 N1' 3 0.611613 0.339206 0.033653 11.00000 0.02350 0.02593 = 0.02321 0.00310 -0.00141 -0.00327 H1' 2 0.652059 0.366117 0.045479 11.00000 0.04461 N2' 3 0.779065 0.389609 0.176195 11.00000 0.02127 0.01807 = 0.02065 0.00320 0.00014 0.00344 H2' 2 0.746396 0.359131 0.161395 11.00000 0.03540 N3' 3 0.702537 0.282500 0.118238 11.00000 0.01850 0.01839 = 0.02685 0.00212 -0.00108 0.00153 N4' 3 0.803446 0.285261 0.235477 11.00000 0.01816 0.02218 = 0.02652 0.00706 -0.00361 -0.00269 C1' 1 0.437308 0.378355 -0.028659 11.00000 0.02668 0.03101 = 0.02076 0.00749 0.00062 0.00113 C2' 1 0.352920 0.348339 -0.057937 11.00000 0.03351 0.05456 = 0.02409 -0.00677 -0.00143 0.00137 AFIX 43 H2'A 2 0.369361 0.311632 -0.074817 11.00000 -1.20000 AFIX 0 C3' 1 0.244133 0.372478 -0.062336 11.00000 0.03132 0.06988 = 0.02681 0.00272 -0.00419 -0.00099 AFIX 43 H3' 2 0.186203 0.352031 -0.082539 11.00000 -1.20000 AFIX 0 C4' 1 0.218310 0.425250 -0.038149 11.00000 0.02983 0.04631 = 0.03649 0.02476 0.00495 0.00486 C5' 1 0.303418 0.454765 -0.008524 11.00000 0.04144 0.02457 = 0.05871 0.00996 0.01144 0.00542 AFIX 43 H5' 2 0.286508 0.491346 0.008408 11.00000 -1.20000 AFIX 0 C6' 1 0.412963 0.431294 -0.003433 11.00000 0.03315 0.02391 = 0.04477 0.00342 0.00046 -0.00198 AFIX 43 H6' 2 0.470648 0.451357 0.017155 11.00000 -1.20000 AFIX 0 C7' 1 0.099496 0.451445 -0.043243 11.00000 0.03441 0.07175 = 0.06124 0.03739 0.01084 0.01357 AFIX 137 H7'A 2 0.058472 0.434947 -0.017657 11.00000 -1.50000 H7'B 2 0.060211 0.439258 -0.074310 11.00000 -1.50000 H7'C 2 0.102811 0.497106 -0.041063 11.00000 -1.50000 AFIX 0 C8' 1 0.536377 0.306345 0.062394 11.00000 0.01891 0.02057 = 0.02614 0.00322 -0.00106 -0.00021 AFIX 23 H8'A 2 0.473602 0.287450 0.041121 11.00000 -1.20000 H8'B 2 0.503363 0.336503 0.083604 11.00000 -1.20000 AFIX 0 C9' 1 0.599013 0.254841 0.092906 11.00000 0.01957 0.01646 = 0.02371 0.00050 -0.00142 0.00096 C10' 1 0.644476 0.204283 0.060716 11.00000 0.02439 0.02061 = 0.03077 -0.00144 0.00018 0.00259 AFIX 23 H10A 2 0.615907 0.162416 0.068256 11.00000 -1.20000 H10B 2 0.621828 0.213402 0.026516 11.00000 -1.20000 AFIX 0 C11' 1 0.520324 0.229494 0.127254 11.00000 0.02028 0.01517 = 0.02596 0.00195 0.00059 0.00249 C12' 1 0.418636 0.201431 0.108455 11.00000 0.02561 0.02301 = 0.02792 -0.00029 -0.00088 -0.00222 AFIX 43 H12' 2 0.402697 0.196106 0.074883 11.00000 -1.20000 AFIX 0 C13' 1 0.341257 0.181411 0.138314 11.00000 0.02544 0.02373 = 0.03920 -0.00163 0.00248 -0.00540 AFIX 43 H13' 2 0.271507 0.163575 0.125173 11.00000 -1.20000 AFIX 0 C14' 1 0.365303 0.187328 0.187334 11.00000 0.03212 0.02514 = 0.03730 0.00155 0.01149 -0.00166 AFIX 43 H14' 2 0.311957 0.173762 0.207849 11.00000 -1.20000 AFIX 0 C15' 1 0.467296 0.213067 0.206444 11.00000 0.03358 0.02465 = 0.02811 0.00306 0.00339 0.00136 AFIX 43 H15' 2 0.484548 0.216207 0.240123 11.00000 -1.20000 AFIX 0 C16' 1 0.544901 0.234432 0.176369 11.00000 0.02378 0.01899 = 0.02852 0.00274 -0.00098 0.00120 AFIX 43 H16' 2 0.614508 0.252340 0.189606 11.00000 -1.20000 AFIX 0 C17' 1 0.786909 0.254877 0.103578 11.00000 0.02378 0.01837 = 0.02636 0.00334 0.00284 0.00213 C18' 1 0.909006 0.268336 0.118248 11.00000 0.01969 0.02557 = 0.03639 -0.00095 0.00578 0.00157 AFIX 23 H18A 2 0.915772 0.308591 0.135635 11.00000 -1.20000 H18B 2 0.948614 0.272612 0.089308 11.00000 -1.20000 AFIX 0 C19' 1 0.966609 0.216873 0.150285 11.00000 0.02241 0.02737 = 0.04848 -0.00385 -0.00196 0.00817 AFIX 23 H19A 2 0.965982 0.177502 0.131818 11.00000 -1.20000 H19B 2 1.046550 0.228603 0.159576 11.00000 -1.20000 AFIX 0 C20' 1 0.909237 0.205686 0.195371 11.00000 0.03075 0.02028 = 0.04437 0.00631 -0.00654 0.00585 AFIX 23 H20A 2 0.834027 0.186635 0.186386 11.00000 -1.20000 H20B 2 0.955020 0.175763 0.216216 11.00000 -1.20000 AFIX 0 C21' 1 0.895033 0.264282 0.222522 11.00000 0.02060 0.02184 = 0.03032 0.00936 -0.00581 0.00095 C22' 1 0.828470 0.346916 0.257594 11.00000 0.01327 0.02162 = 0.02371 0.00637 -0.00161 -0.00279 C23' 1 0.957373 0.354460 0.255981 11.00000 0.01456 0.02534 = 0.02903 0.00338 -0.00114 -0.00052 AFIX 23 H23A 2 0.973916 0.392290 0.237771 11.00000 -1.20000 H23B 2 0.997439 0.357561 0.288656 11.00000 -1.20000 AFIX 0 C24' 1 0.761450 0.396765 0.226566 11.00000 0.01608 0.02612 = 0.02124 0.00397 0.00131 0.00359 AFIX 23 H24A 2 0.679852 0.392684 0.230014 11.00000 -1.20000 H24B 2 0.786267 0.438922 0.237749 11.00000 -1.20000 AFIX 0 C25' 1 0.790809 0.350794 0.307352 11.00000 0.01643 0.03249 = 0.02514 0.01091 -0.00275 0.00058 C26' 1 0.709187 0.310173 0.321372 11.00000 0.02019 0.04342 = 0.03225 0.01236 -0.00137 -0.00609 AFIX 43 H26' 2 0.679239 0.278204 0.300226 11.00000 -1.20000 AFIX 0 C27' 1 0.671356 0.316082 0.365979 11.00000 0.02290 0.06930 = 0.03566 0.01993 0.00317 -0.00831 AFIX 43 H27' 2 0.616892 0.287674 0.375618 11.00000 -1.20000 AFIX 0 C28' 1 0.713100 0.363446 0.396427 11.00000 0.03353 0.08787 = 0.02467 0.01334 0.00536 -0.00348 AFIX 43 H28' 2 0.686313 0.367964 0.426787 11.00000 -1.20000 AFIX 0 C29' 1 0.793749 0.404227 0.382751 11.00000 0.04191 0.06465 = 0.02607 0.00119 0.00077 -0.00976 AFIX 43 H29' 2 0.822534 0.436665 0.403704 11.00000 -1.20000 AFIX 0 C30' 1 0.832392 0.397622 0.338427 11.00000 0.02885 0.04142 = 0.02590 0.00629 -0.00004 -0.00670 AFIX 43 H30' 2 0.888114 0.425551 0.329213 11.00000 -1.20000 AFIX 0 C31' 1 0.661166 0.493849 0.145421 11.00000 0.01801 0.01750 = 0.01832 0.00460 0.00290 0.00287 C32' 1 0.667887 0.552733 0.165455 11.00000 0.02545 0.02111 = 0.03962 -0.00353 -0.00039 0.00201 AFIX 43 H32' 2 0.739332 0.569871 0.177130 11.00000 -1.20000 AFIX 0 C33' 1 0.569586 0.586781 0.168444 11.00000 0.03587 0.02228 = 0.04311 -0.00332 0.00653 0.00829 AFIX 43 H33' 2 0.574465 0.627442 0.182028 11.00000 -1.20000 AFIX 0 C34' 1 0.464609 0.562491 0.151970 11.00000 0.02718 0.03149 = 0.02679 0.01136 0.00976 0.01362 C35' 1 0.459819 0.503615 0.131426 11.00000 0.01819 0.03832 = 0.04282 0.00287 0.00450 0.00352 AFIX 43 H35' 2 0.388522 0.486552 0.119448 11.00000 -1.20000 AFIX 0 C36' 1 0.556924 0.469316 0.128065 11.00000 0.02074 0.02611 = 0.03878 -0.00404 0.00198 0.00028 AFIX 43 H36' 2 0.552218 0.429001 0.113885 11.00000 -1.20000 AFIX 0 C37' 1 0.358261 0.599096 0.156178 11.00000 0.03505 0.04983 = 0.04325 0.01125 0.01351 0.02387 AFIX 137 H37A 2 0.316442 0.579894 0.180473 11.00000 -1.50000 H37B 2 0.311081 0.599069 0.125333 11.00000 -1.50000 H37C 2 0.377960 0.642179 0.165469 11.00000 -1.50000 AFIX 0 O5 4 0.646833 1.051708 0.095227 11.00000 0.02688 0.02581 = 0.03790 0.00790 -0.00141 0.00629 O6 4 0.497190 0.942275 0.245864 11.00000 0.01736 0.03569 = 0.03468 0.00684 0.00534 0.00632 N2 3 0.685351 0.857786 0.191675 11.00000 0.02465 0.01781 = 0.02109 -0.00351 0.00031 0.00443 H2 2 0.707617 0.888965 0.175446 11.00000 0.02950 N3 3 0.730458 0.968750 0.133510 11.00000 0.01978 0.02395 = 0.02473 0.00397 0.00263 0.00113 N4 3 0.684854 0.961708 0.252777 11.00000 0.02202 0.01697 = 0.02161 -0.00293 0.00473 -0.00050 C8 1 0.866126 0.957051 0.075570 11.00000 0.02746 0.02779 = 0.02608 -0.00438 0.00343 -0.00183 PART 1 AFIX 23 H8AA 2 0.934900 0.974997 0.064101 21.00000 -1.20000 H8AB 2 0.886795 0.916370 0.090834 21.00000 -1.20000 AFIX 23 PART 2 H8A 2 0.916525 0.979820 0.055837 -21.00000 -1.20000 H8B 2 0.909168 0.922053 0.091800 -21.00000 -1.20000 AFIX 0 PART 0 C9 1 0.823450 1.001042 0.112493 11.00000 0.02316 0.01918 = 0.02095 0.00367 0.00270 0.00191 C10 1 0.764955 1.059478 0.088960 11.00000 0.02778 0.02195 = 0.03720 0.00760 -0.00190 0.00073 AFIX 23 H10C 2 0.795688 1.098056 0.104878 11.00000 -1.20000 H10D 2 0.775516 1.061576 0.054616 11.00000 -1.20000 AFIX 0 C11 1 0.921336 1.018448 0.149726 11.00000 0.02140 0.01799 = 0.02342 0.00129 0.00265 0.00310 C12 1 1.019366 1.043862 0.134897 11.00000 0.02804 0.02661 = 0.02289 0.00136 0.00459 -0.00069 AFIX 43 H12 2 1.024241 1.050118 0.101788 11.00000 -1.20000 AFIX 0 C13 1 1.109899 1.060133 0.167882 11.00000 0.02647 0.02905 = 0.03720 0.00015 0.00404 -0.00404 AFIX 43 H13 2 1.176679 1.076995 0.157318 11.00000 -1.20000 AFIX 0 C14 1 1.103054 1.051844 0.216066 11.00000 0.02968 0.02726 = 0.03295 -0.00329 -0.00553 -0.00029 AFIX 43 H14 2 1.165135 1.062879 0.238710 11.00000 -1.20000 AFIX 0 C15 1 1.005638 1.027443 0.231312 11.00000 0.03366 0.02819 = 0.02230 -0.00078 0.00063 0.00406 AFIX 43 H15 2 1.000700 1.022087 0.264506 11.00000 -1.20000 AFIX 0 C16 1 0.914683 1.010665 0.198277 11.00000 0.02604 0.02211 = 0.02315 0.00057 0.00457 0.00193 AFIX 43 H16 2 0.848007 0.993874 0.208985 11.00000 -1.20000 AFIX 0 C17 1 0.639945 0.998883 0.121227 11.00000 0.02608 0.02295 = 0.02184 0.00041 0.00084 0.00303 C18 1 0.524338 0.982716 0.132883 11.00000 0.02045 0.04059 = 0.03086 0.00254 -0.00023 0.00471 AFIX 23 H18C 2 0.526386 0.940899 0.147963 11.00000 -1.20000 H18D 2 0.472500 0.980476 0.102875 11.00000 -1.20000 AFIX 0 C19 1 0.477660 1.029991 0.166520 11.00000 0.03160 0.04283 = 0.03837 0.01011 0.00752 0.02120 AFIX 23 H19C 2 0.402628 1.015508 0.174065 11.00000 -1.20000 H19D 2 0.466817 1.070597 0.149816 11.00000 -1.20000 AFIX 0 C20 1 0.554533 1.039689 0.213346 11.00000 0.04390 0.02427 = 0.03477 0.00123 0.01136 0.01539 AFIX 23 H20C 2 0.624451 1.061244 0.206342 11.00000 -1.20000 H20D 2 0.515499 1.067083 0.234610 11.00000 -1.20000 AFIX 0 C21 1 0.585671 0.980112 0.238731 11.00000 0.02684 0.02232 = 0.02379 -0.00346 0.00833 0.00636 C22 1 0.675748 0.898494 0.273108 11.00000 0.01347 0.01868 = 0.02164 -0.00133 0.00342 -0.00083 C23 1 0.546382 0.887432 0.269746 11.00000 0.01591 0.02645 = 0.02694 0.00099 0.00288 -0.00026 AFIX 23 H23C 2 0.524786 0.849281 0.251048 11.00000 -1.20000 H23D 2 0.521435 0.883104 0.301971 11.00000 -1.20000 AFIX 0 C24 1 0.732532 0.852313 0.241657 11.00000 0.01784 0.01966 = 0.02154 -0.00212 0.00100 0.00429 AFIX 23 H24C 2 0.814868 0.860671 0.244469 11.00000 -1.20000 H24D 2 0.721384 0.809187 0.252924 11.00000 -1.20000 AFIX 0 C25 1 0.737549 0.894379 0.323356 11.00000 0.01547 0.02312 = 0.02027 -0.00508 0.00349 -0.00041 C26 1 0.827745 0.933745 0.337393 11.00000 0.02347 0.03404 = 0.02869 0.00017 0.00337 -0.01164 AFIX 43 H26 2 0.848305 0.965220 0.316202 11.00000 -1.20000 AFIX 0 C27 1 0.888230 0.927404 0.382296 11.00000 0.02496 0.04911 = 0.03132 -0.00725 -0.00113 -0.01649 AFIX 43 H27 2 0.949777 0.954636 0.391685 11.00000 -1.20000 AFIX 0 C28 1 0.859218 0.881627 0.413370 11.00000 0.02853 0.05073 = 0.02373 -0.00195 -0.00294 -0.00736 AFIX 43 H28 2 0.900439 0.877447 0.444103 11.00000 -1.20000 AFIX 0 C29 1 0.770096 0.842098 0.399463 11.00000 0.03305 0.04278 = 0.02602 0.00644 -0.00181 -0.00898 AFIX 43 H29 2 0.749920 0.810573 0.420693 11.00000 -1.20000 AFIX 0 C30 1 0.709786 0.848136 0.354649 11.00000 0.02349 0.02967 = 0.02672 0.00133 -0.00095 -0.00873 AFIX 43 H30 2 0.648967 0.820426 0.345254 11.00000 -1.20000 AFIX 0 C31 1 0.793137 0.757063 0.159083 11.00000 0.02138 0.02073 = 0.02025 -0.00831 -0.00035 0.00382 C32 1 0.815289 0.703860 0.186332 11.00000 0.02532 0.02581 = 0.02948 0.00021 0.00418 0.00045 AFIX 43 H32 2 0.760116 0.687684 0.204957 11.00000 -1.20000 AFIX 0 C33 1 0.919125 0.674369 0.186144 11.00000 0.02997 0.02654 = 0.03287 0.00173 -0.00299 0.00737 AFIX 43 H33 2 0.933928 0.637225 0.204223 11.00000 -1.20000 AFIX 0 C34 1 1.001365 0.698005 0.160164 11.00000 0.02130 0.03214 = 0.03191 -0.01187 -0.00013 0.00539 C35 1 0.977773 0.751830 0.133420 11.00000 0.03129 0.03504 = 0.03461 -0.00664 0.01469 -0.00238 AFIX 43 H35 2 1.033812 0.768779 0.115598 11.00000 -1.20000 AFIX 0 C36 1 0.874085 0.781112 0.132328 11.00000 0.03788 0.02387 = 0.02540 0.00073 0.00749 0.00359 AFIX 43 H36 2 0.858344 0.817455 0.113390 11.00000 -1.20000 AFIX 0 C37 1 1.113944 0.665559 0.161090 11.00000 0.02656 0.05444 = 0.06400 -0.01791 0.00077 0.01538 AFIX 137 H37D 2 1.101751 0.620859 0.155035 11.00000 -1.50000 H37E 2 1.157198 0.671361 0.192492 11.00000 -1.50000 H37F 2 1.156134 0.683345 0.136344 11.00000 -1.50000 AFIX 0 PART 1 S1A 5 0.818558 0.934662 -0.018556 21.00000 0.05179 0.04274 = 0.01508 -0.00328 0.00476 -0.01080 S2A 5 0.658491 0.793395 0.163013 21.00000 0.01774 0.02194 = 0.01510 -0.00386 0.00253 0.00301 O1A 4 0.719487 0.922308 -0.050762 21.00000 0.06894 0.04756 = 0.02109 -0.00302 -0.00881 -0.00516 O2A 4 0.892536 0.985446 -0.027816 21.00000 0.07138 0.04506 = 0.02812 0.00411 0.01542 -0.02098 O3A 4 0.617270 0.812346 0.115092 21.00000 0.02921 0.03319 = 0.02206 -0.00434 -0.00382 0.00809 O4A 4 0.589941 0.752436 0.188168 21.00000 0.02138 0.02320 = 0.03411 -0.00365 0.01197 -0.00529 N1A 3 0.777210 0.946903 0.033529 21.00000 0.03450 0.03399 = 0.01931 -0.00102 0.00599 -0.01021 AFIX 3 H1A 2 0.734740 0.922873 0.048279 21.00000 -1.30000 AFIX 0 C1A 1 0.900242 0.866057 -0.012336 21.00000 0.04741 0.04672 = 0.00941 -0.00674 0.00631 -0.00654 C2A 1 1.016026 0.870846 -0.003860 21.00000 0.04734 0.05228 = 0.02408 -0.01018 0.02328 -0.01254 AFIX 43 H2A 2 1.051989 0.910434 -0.004247 21.00000 -1.20000 AFIX 0 C3A 1 1.078845 0.817468 0.005173 21.00000 0.03572 0.06681 = 0.02924 -0.01512 0.01553 -0.00745 AFIX 43 H3A 2 1.158882 0.821053 0.010366 21.00000 -1.20000 AFIX 0 C4A 1 1.031083 0.758741 0.007066 21.00000 0.04365 0.05959 = 0.02030 -0.00889 0.00621 0.00139 C5A 1 0.912879 0.754962 -0.000861 21.00000 0.04438 0.04325 = 0.03167 -0.00413 -0.00065 -0.00779 AFIX 43 H5A 2 0.876874 0.715482 0.000407 21.00000 -1.20000 AFIX 0 C6A 1 0.847835 0.808135 -0.010532 21.00000 0.03724 0.04766 = 0.02887 -0.00681 -0.00559 -0.00527 AFIX 43 H6A 2 0.767750 0.805038 -0.015910 21.00000 -1.20000 AFIX 0 C7A 1 1.110487 0.703633 0.016976 21.00000 0.04847 0.06606 = 0.03664 0.00579 0.01379 0.00067 AFIX 3 H7AA 2 1.180647 0.716543 0.034406 21.00000 -1.50000 H7AB 2 1.073297 0.674363 0.035796 21.00000 -1.50000 H7AC 2 1.125207 0.684243 -0.012434 21.00000 -1.50000 AFIX 0 PART 2 S1B 5 0.788586 0.916593 -0.007566 -21.00000 0.04856 0.04149 = 0.02165 -0.00907 -0.00092 -0.00051 S2B 5 0.669111 0.800327 0.153678 -21.00000 0.01774 0.02194 = 0.01510 -0.00386 0.00253 0.00301 O1B 4 0.681263 0.895168 -0.029430 -21.00000 0.05625 0.05075 = 0.03301 -0.01297 -0.01337 0.00169 O2B 4 0.848895 0.969552 -0.027098 -21.00000 0.07138 0.04506 = 0.02812 0.00411 0.01542 -0.02098 O3B 4 0.645082 0.826678 0.106913 -21.00000 0.02921 0.03319 = 0.02206 -0.00434 -0.00382 0.00809 O4B 4 0.592663 0.760260 0.173118 -21.00000 0.02138 0.02320 = 0.03411 -0.00365 0.01197 -0.00529 N1B 3 0.769447 0.933891 0.046259 -21.00000 0.03450 0.03399 = 0.01931 -0.00102 0.00599 -0.01021 AFIX 3 H1B 2 0.731867 0.901761 0.058589 -21.00000 -1.30000 AFIX 66 C1B 1 0.883937 0.853025 -0.002488 -21.00000 0.04741 0.04672 = 0.00941 -0.00674 0.00631 -0.00654 C6B 1 0.841097 0.792740 -0.000974 -21.00000 0.03724 0.04766 = 0.02887 -0.00681 -0.00559 -0.00527 AFIX 43 H6B 2 0.761671 0.785993 -0.005284 -21.00000 -1.20000 AFIX 65 C5B 1 0.914468 0.742327 0.006848 -21.00000 0.04438 0.04325 = 0.03167 -0.00413 -0.00065 -0.00779 AFIX 43 H5B 2 0.885188 0.701125 0.007883 -21.00000 -1.20000 AFIX 65 C4B 1 1.030679 0.752199 0.013155 -21.00000 0.04365 0.05959 = 0.02030 -0.00889 0.00621 0.00139 C3B 1 1.073521 0.812483 0.011641 -21.00000 0.03572 0.06681 = 0.02924 -0.01512 0.01553 -0.00745 AFIX 43 H3B 2 1.152946 0.819230 0.015951 -21.00000 -1.20000 AFIX 65 C2B 1 1.000151 0.862897 0.003819 -21.00000 0.04734 0.05228 = 0.02408 -0.01018 0.02328 -0.01254 AFIX 43 H2B 2 1.029431 0.904098 0.002784 -21.00000 -1.20000 AFIX 0 C7B 1 1.093014 0.693663 0.023233 -21.00000 0.04847 0.06606 = 0.03664 0.00579 0.01379 0.00067 AFIX 3 H7BA 2 1.103764 0.674703 -0.006827 -21.00000 -1.50000 H7BB 2 1.165294 0.701983 0.040823 -21.00000 -1.50000 H7BC 2 1.050814 0.665823 0.041273 -21.00000 -1.50000 AFIX 0 PART 1 O1S 4 0.586684 0.859847 0.023265 21.00000 0.05797 0.08972 = 0.05399 0.03832 -0.00713 -0.01082 AFIX 3 H1S 2 0.588224 0.851857 0.052545 21.00000 -1.50000 AFIX 0 C1S 1 0.504290 0.906483 0.010279 21.00000 0.07847 0.11091 = 0.05559 -0.01662 -0.01372 -0.02896 AFIX 137 H1SA 2 0.520797 0.943534 0.030285 21.00000 -1.50000 H1SB 2 0.429138 0.890457 0.014957 21.00000 -1.50000 H1SC 2 0.505996 0.917685 -0.023378 21.00000 -1.50000 AFIX 0 HKLF 4 REM 20srv039_a.res in P2(1)/c REM wR2 = 0.1309, GooF = S = 1.102, Restrained GooF = 1.099 for all data REM R1 = 0.0522 for 15076 Fo > 4sig(Fo) and 0.0717 for all 19071 data REM 962 parameters refined using 162 restraints END WGHT 0.0455 6.0589 REM Highest difference peak 0.522, deepest hole -0.351, 1-sigma level 0.062 Q1 1 0.4394 0.9639 0.0066 11.00000 0.05 0.52 Q2 1 0.3869 0.9407 0.0144 11.00000 0.05 0.44 Q3 1 0.7200 0.4785 0.1407 11.00000 0.05 0.36 Q4 1 0.8669 0.9017 -0.0126 11.00000 0.05 0.34 Q5 1 0.7128 0.8984 0.3024 11.00000 0.05 0.32 Q6 1 0.8019 0.3556 0.2803 11.00000 0.05 0.30 Q7 1 0.5684 0.2799 0.0793 11.00000 0.05 0.30 Q8 1 0.7770 0.4173 0.1616 11.00000 0.05 0.30 Q9 1 0.8156 0.8578 0.4022 11.00000 0.05 0.30 Q10 1 0.9703 0.9571 -0.0193 11.00000 0.05 0.30 ; _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 S1' S 0.57690(4) 0.34921(2) -0.02311(2) 0.02668(11) Uani 1 1 d . . . . . S2' S 0.78491(4) 0.44964(2) 0.14209(2) 0.01742(9) Uani 1 1 d . . . . . O1' O 0.65332(13) 0.39569(8) -0.03711(5) 0.0368(4) Uani 1 1 d . . . . . O2' O 0.57171(14) 0.28941(8) -0.04594(6) 0.0399(4) Uani 1 1 d . . . . . O3' O 0.78242(11) 0.42475(6) 0.09451(5) 0.0226(3) Uani 1 1 d . . . . . O4' O 0.87781(11) 0.48854(6) 0.16069(5) 0.0241(3) Uani 1 1 d . . . . . O5' O 0.76642(12) 0.20760(7) 0.07182(5) 0.0280(3) Uani 1 1 d . . . . . O6' O 0.99087(11) 0.29877(7) 0.23231(6) 0.0291(3) Uani 1 1 d . . . . . N1' N 0.61161(14) 0.33921(8) 0.03365(6) 0.0245(3) Uani 1 1 d . . . . . H1' H 0.652(2) 0.3661(14) 0.0455(10) 0.045(8) Uiso 1 1 d . . . . . N2' N 0.77907(13) 0.38961(7) 0.17620(6) 0.0202(3) Uani 1 1 d . . . . . H2' H 0.746(2) 0.3591(13) 0.1614(9) 0.035(7) Uiso 1 1 d . . . . . N3' N 0.70254(13) 0.28250(7) 0.11824(6) 0.0215(3) Uani 1 1 d . . . . . N4' N 0.80345(13) 0.28526(7) 0.23548(6) 0.0227(3) Uani 1 1 d . . . . . C1' C 0.43731(17) 0.37835(10) -0.02866(7) 0.0263(4) Uani 1 1 d . . . . . C2' C 0.3529(2) 0.34834(13) -0.05794(8) 0.0377(5) Uani 1 1 d . . . . . H2'A H 0.369361 0.311632 -0.074817 0.045 Uiso 1 1 calc R U . . . C3' C 0.2441(2) 0.37248(14) -0.06234(8) 0.0432(6) Uani 1 1 d . . . . . H3' H 0.186203 0.352031 -0.082539 0.052 Uiso 1 1 calc R U . . . C4' C 0.21831(19) 0.42525(12) -0.03815(8) 0.0374(5) Uani 1 1 d . . . . . C5' C 0.3034(2) 0.45476(11) -0.00852(10) 0.0411(6) Uani 1 1 d . . . . . H5' H 0.286508 0.491346 0.008408 0.049 Uiso 1 1 calc R U . . . C6' C 0.41296(19) 0.43129(10) -0.00343(9) 0.0342(5) Uani 1 1 d . . . . . H6' H 0.470648 0.451357 0.017155 0.041 Uiso 1 1 calc R U . . . C7' C 0.0995(2) 0.45145(15) -0.04324(11) 0.0554(8) Uani 1 1 d . . . . . H7'A H 0.058472 0.434947 -0.017657 0.083 Uiso 1 1 calc R U . . . H7'B H 0.060211 0.439258 -0.074310 0.083 Uiso 1 1 calc R U . . . H7'C H 0.102811 0.497106 -0.041063 0.083 Uiso 1 1 calc R U . . . C8' C 0.53638(16) 0.30635(9) 0.06239(7) 0.0221(4) Uani 1 1 d . . . . . H8'A H 0.473602 0.287450 0.041121 0.027 Uiso 1 1 calc R U . . . H8'B H 0.503363 0.336503 0.083604 0.027 Uiso 1 1 calc R U . . . C9' C 0.59901(15) 0.25484(8) 0.09291(7) 0.0202(4) Uani 1 1 d . . . . . C10' C 0.64448(17) 0.20428(9) 0.06072(7) 0.0255(4) Uani 1 1 d . . . . . H10A H 0.615907 0.162416 0.068256 0.031 Uiso 1 1 calc R U . . . H10B H 0.621828 0.213402 0.026516 0.031 Uiso 1 1 calc R U . . . C11' C 0.52032(15) 0.22949(8) 0.12725(7) 0.0206(4) Uani 1 1 d . . . . . C12' C 0.41864(17) 0.20143(9) 0.10845(7) 0.0258(4) Uani 1 1 d . . . . . H12' H 0.402697 0.196106 0.074883 0.031 Uiso 1 1 calc R U . . . C13' C 0.34126(18) 0.18141(10) 0.13831(8) 0.0295(4) Uani 1 1 d . . . . . H13' H 0.271507 0.163575 0.125173 0.035 Uiso 1 1 calc R U . . . C14' C 0.36530(19) 0.18733(10) 0.18733(8) 0.0309(4) Uani 1 1 d . . . . . H14' H 0.311957 0.173762 0.207849 0.037 Uiso 1 1 calc R U . . . C15' C 0.46730(18) 0.21307(10) 0.20644(8) 0.0288(4) Uani 1 1 d . . . . . H15' H 0.484548 0.216207 0.240123 0.035 Uiso 1 1 calc R U . . . C16' C 0.54490(17) 0.23443(9) 0.17637(7) 0.0241(4) Uani 1 1 d . . . . . H16' H 0.614508 0.252340 0.189606 0.029 Uiso 1 1 calc R U . . . C17' C 0.78691(16) 0.25488(9) 0.10358(7) 0.0228(4) Uani 1 1 d . . . . . C18' C 0.90901(16) 0.26834(10) 0.11825(8) 0.0270(4) Uani 1 1 d . . . . . H18A H 0.915772 0.308591 0.135635 0.032 Uiso 1 1 calc R U . . . H18B H 0.948614 0.272612 0.089308 0.032 Uiso 1 1 calc R U . . . C19' C 0.96661(18) 0.21687(10) 0.15029(9) 0.0332(5) Uani 1 1 d . . . . . H19A H 0.965982 0.177502 0.131818 0.040 Uiso 1 1 calc R U . . . H19B H 1.046550 0.228603 0.159576 0.040 Uiso 1 1 calc R U . . . C20' C 0.90924(19) 0.20569(10) 0.19537(8) 0.0326(5) Uani 1 1 d . . . . . H20A H 0.834027 0.186635 0.186386 0.039 Uiso 1 1 calc R U . . . H20B H 0.955020 0.175763 0.216216 0.039 Uiso 1 1 calc R U . . . C21' C 0.89503(16) 0.26428(9) 0.22252(7) 0.0249(4) Uani 1 1 d . . . . . C22' C 0.82847(14) 0.34692(9) 0.25759(7) 0.0198(4) Uani 1 1 d . . . . . C23' C 0.95737(15) 0.35446(9) 0.25598(7) 0.0232(4) Uani 1 1 d . . . . . H23A H 0.973916 0.392290 0.237771 0.028 Uiso 1 1 calc R U . . . H23B H 0.997439 0.357561 0.288656 0.028 Uiso 1 1 calc R U . . . C24' C 0.76145(15) 0.39677(9) 0.22657(6) 0.0212(4) Uani 1 1 d . . . . . H24A H 0.679852 0.392684 0.230014 0.025 Uiso 1 1 calc R U . . . H24B H 0.786267 0.438922 0.237749 0.025 Uiso 1 1 calc R U . . . C25' C 0.79081(16) 0.35079(10) 0.30735(7) 0.0251(4) Uani 1 1 d . . . . . C26' C 0.70919(17) 0.31017(11) 0.32137(8) 0.0323(5) Uani 1 1 d . . . . . H26' H 0.679239 0.278204 0.300226 0.039 Uiso 1 1 calc R U . . . C27' C 0.67136(19) 0.31608(14) 0.36598(9) 0.0426(6) Uani 1 1 d . . . . . H27' H 0.616892 0.287674 0.375618 0.051 Uiso 1 1 calc R U . . . C28' C 0.7131(2) 0.36345(15) 0.39643(9) 0.0485(7) Uani 1 1 d . . . . . H28' H 0.686313 0.367964 0.426787 0.058 Uiso 1 1 calc R U . . . C29' C 0.7937(2) 0.40423(14) 0.38275(8) 0.0444(6) Uani 1 1 d . . . . . H29' H 0.822534 0.436665 0.403704 0.053 Uiso 1 1 calc R U . . . C30' C 0.83239(18) 0.39762(11) 0.33843(7) 0.0323(5) Uani 1 1 d . . . . . H30' H 0.888114 0.425551 0.329213 0.039 Uiso 1 1 calc R U . . . C31' C 0.66117(15) 0.49385(8) 0.14542(6) 0.0179(3) Uani 1 1 d . . . . . C32' C 0.66789(18) 0.55273(9) 0.16545(8) 0.0290(4) Uani 1 1 d . . . . . H32' H 0.739332 0.569871 0.177130 0.035 Uiso 1 1 calc R U . . . C33' C 0.56959(19) 0.58678(10) 0.16844(8) 0.0336(5) Uani 1 1 d . . . . . H33' H 0.574465 0.627442 0.182028 0.040 Uiso 1 1 calc R U . . . C34' C 0.46461(17) 0.56249(10) 0.15197(7) 0.0280(4) Uani 1 1 d . . . . . C35' C 0.45982(17) 0.50361(11) 0.13143(8) 0.0330(5) Uani 1 1 d . . . . . H35' H 0.388522 0.486552 0.119448 0.040 Uiso 1 1 calc R U . . . C36' C 0.55692(17) 0.46932(10) 0.12807(8) 0.0286(4) Uani 1 1 d . . . . . H36' H 0.552218 0.429001 0.113885 0.034 Uiso 1 1 calc R U . . . C37' C 0.3583(2) 0.59910(13) 0.15618(9) 0.0420(6) Uani 1 1 d . . . . . H37A H 0.316442 0.579894 0.180473 0.063 Uiso 1 1 calc R U . . . H37B H 0.311081 0.599069 0.125333 0.063 Uiso 1 1 calc R U . . . H37C H 0.377960 0.642179 0.165469 0.063 Uiso 1 1 calc R U . . . O5 O 0.64683(12) 1.05171(7) 0.09523(5) 0.0306(3) Uani 1 1 d . . . . . O6 O 0.49719(11) 0.94227(7) 0.24586(5) 0.0291(3) Uani 1 1 d . . . . . N2 N 0.68535(14) 0.85779(8) 0.19167(6) 0.0214(3) Uani 1 1 d D . . . . H2 H 0.708(2) 0.8890(12) 0.1754(9) 0.029(6) Uiso 1 1 d . . . . . N3 N 0.73046(13) 0.96875(8) 0.13351(6) 0.0228(3) Uani 1 1 d . . . . . N4 N 0.68485(13) 0.96171(7) 0.25278(5) 0.0200(3) Uani 1 1 d . . . . . C8 C 0.86613(17) 0.95705(10) 0.07557(7) 0.0271(4) Uani 1 1 d D . . . . H8AA H 0.934900 0.974997 0.064101 0.032 Uiso 0.633(3) 1 calc R U P A 1 H8AB H 0.886795 0.916370 0.090834 0.032 Uiso 0.633(3) 1 calc R U P A 1 H8A H 0.916525 0.979820 0.055837 0.032 Uiso 0.367(3) 1 calc R U P A 2 H8B H 0.909168 0.922053 0.091800 0.032 Uiso 0.367(3) 1 calc R U P A 2 C9 C 0.82345(16) 1.00104(9) 0.11249(7) 0.0211(4) Uani 1 1 d . . . . . C10 C 0.76496(18) 1.05948(10) 0.08896(8) 0.0294(4) Uani 1 1 d . . . . . H10C H 0.795688 1.098056 0.104878 0.035 Uiso 1 1 calc R U . . . H10D H 0.775516 1.061576 0.054616 0.035 Uiso 1 1 calc R U . . . C11 C 0.92134(16) 1.01845(8) 0.14973(7) 0.0209(4) Uani 1 1 d . . . . . C12 C 1.01937(17) 1.04386(9) 0.13490(7) 0.0257(4) Uani 1 1 d . . . . . H12 H 1.024241 1.050118 0.101788 0.031 Uiso 1 1 calc R U . . . C13 C 1.10990(18) 1.06013(10) 0.16788(8) 0.0309(4) Uani 1 1 d . . . . . H13 H 1.176679 1.076995 0.157318 0.037 Uiso 1 1 calc R U . . . C14 C 1.10305(18) 1.05184(10) 0.21607(8) 0.0306(4) Uani 1 1 d . . . . . H14 H 1.165135 1.062879 0.238710 0.037 Uiso 1 1 calc R U . . . C15 C 1.00564(18) 1.02744(10) 0.23131(7) 0.0282(4) Uani 1 1 d . . . . . H15 H 1.000700 1.022087 0.264506 0.034 Uiso 1 1 calc R U . . . C16 C 0.91468(17) 1.01067(9) 0.19828(7) 0.0236(4) Uani 1 1 d . . . . . H16 H 0.848007 0.993874 0.208985 0.028 Uiso 1 1 calc R U . . . C17 C 0.63995(17) 0.99888(9) 0.12123(7) 0.0238(4) Uani 1 1 d . . . . . C18 C 0.52434(17) 0.98272(11) 0.13288(8) 0.0309(4) Uani 1 1 d . . . . . H18C H 0.526386 0.940899 0.147963 0.037 Uiso 1 1 calc R U . . . H18D H 0.472500 0.980476 0.102875 0.037 Uiso 1 1 calc R U . . . C19 C 0.4777(2) 1.02999(12) 0.16652(8) 0.0373(5) Uani 1 1 d . . . . . H19C H 0.402628 1.015508 0.174065 0.045 Uiso 1 1 calc R U . . . H19D H 0.466817 1.070597 0.149816 0.045 Uiso 1 1 calc R U . . . C20 C 0.5545(2) 1.03969(10) 0.21335(8) 0.0338(5) Uani 1 1 d . . . . . H20C H 0.624451 1.061244 0.206342 0.041 Uiso 1 1 calc R U . . . H20D H 0.515499 1.067083 0.234610 0.041 Uiso 1 1 calc R U . . . C21 C 0.58567(17) 0.98011(9) 0.23873(7) 0.0239(4) Uani 1 1 d . . . . . C22 C 0.67575(14) 0.89849(8) 0.27311(6) 0.0178(3) Uani 1 1 d . . . . . C23 C 0.54638(15) 0.88743(9) 0.26975(7) 0.0231(4) Uani 1 1 d . . . . . H23C H 0.524786 0.849281 0.251048 0.028 Uiso 1 1 calc R U . . . H23D H 0.521435 0.883104 0.301971 0.028 Uiso 1 1 calc R U . . . C24 C 0.73253(15) 0.85231(9) 0.24166(6) 0.0198(3) Uani 1 1 d . . . . . H24C H 0.814868 0.860671 0.244469 0.024 Uiso 1 1 calc R U . . . H24D H 0.721384 0.809187 0.252924 0.024 Uiso 1 1 calc R U . . . C25 C 0.73755(15) 0.89438(9) 0.32336(6) 0.0195(3) Uani 1 1 d . . . . . C26 C 0.82775(17) 0.93375(10) 0.33739(7) 0.0287(4) Uani 1 1 d . . . . . H26 H 0.848305 0.965220 0.316202 0.034 Uiso 1 1 calc R U . . . C27 C 0.88823(18) 0.92740(12) 0.38230(8) 0.0355(5) Uani 1 1 d . . . . . H27 H 0.949777 0.954636 0.391685 0.043 Uiso 1 1 calc R U . . . C28 C 0.85922(19) 0.88163(12) 0.41337(8) 0.0348(5) Uani 1 1 d . . . . . H28 H 0.900439 0.877447 0.444103 0.042 Uiso 1 1 calc R U . . . C29 C 0.77010(19) 0.84210(11) 0.39946(8) 0.0343(5) Uani 1 1 d . . . . . H29 H 0.749920 0.810573 0.420693 0.041 Uiso 1 1 calc R U . . . C30 C 0.70979(17) 0.84814(10) 0.35465(7) 0.0269(4) Uani 1 1 d . . . . . H30 H 0.648967 0.820426 0.345254 0.032 Uiso 1 1 calc R U . . . C31 C 0.79314(16) 0.75706(9) 0.15908(7) 0.0210(4) Uani 1 1 d . . . . . C32 C 0.81529(17) 0.70386(9) 0.18633(7) 0.0268(4) Uani 1 1 d . . . . . H32 H 0.760116 0.687684 0.204957 0.032 Uiso 1 1 calc R U . . . C33 C 0.91913(18) 0.67437(10) 0.18614(8) 0.0303(4) Uani 1 1 d . . . . . H33 H 0.933928 0.637225 0.204223 0.036 Uiso 1 1 calc R U . . . C34 C 1.00137(17) 0.69800(10) 0.16016(8) 0.0287(4) Uani 1 1 d . . . . . C35 C 0.97777(19) 0.75183(11) 0.13342(8) 0.0328(5) Uani 1 1 d . . . . . H35 H 1.033812 0.768779 0.115598 0.039 Uiso 1 1 calc R U . . . C36 C 0.87408(19) 0.78111(10) 0.13233(7) 0.0288(4) Uani 1 1 d . . . . . H36 H 0.858344 0.817455 0.113390 0.035 Uiso 1 1 calc R U . . . C37 C 1.1139(2) 0.66556(14) 0.16109(11) 0.0487(7) Uani 1 1 d . . . . . H37D H 1.101751 0.620859 0.155035 0.073 Uiso 1 1 calc R U . . . H37E H 1.157198 0.671361 0.192492 0.073 Uiso 1 1 calc R U . . . H37F H 1.156134 0.683345 0.136344 0.073 Uiso 1 1 calc R U . . . S1A S 0.81856(15) 0.93466(8) -0.01856(5) 0.0365(3) Uani 0.633(3) 1 d D . P A 1 S2A S 0.6585(2) 0.79339(13) 0.16301(8) 0.0182(3) Uani 0.633(3) 1 d D . P A 1 O1A O 0.7195(3) 0.92231(15) -0.05076(10) 0.0469(8) Uani 0.633(3) 1 d D . P A 1 O2A O 0.8925(4) 0.98545(18) -0.02782(12) 0.0474(8) Uani 0.633(3) 1 d D . P A 1 O3A O 0.6173(3) 0.8123(2) 0.11509(14) 0.0287(8) Uani 0.633(3) 1 d D . P A 1 O4A O 0.5899(4) 0.7524(2) 0.18817(13) 0.0256(8) Uani 0.633(3) 1 d D . P A 1 N1A N 0.7772(4) 0.9469(2) 0.03353(13) 0.0290(8) Uani 0.633(3) 1 d D . P A 1 H1A H 0.734740 0.922873 0.048279 0.038 Uiso 0.633(3) 1 d R U P A 1 C1A C 0.9002(5) 0.8661(3) -0.01234(19) 0.0343(10) Uani 0.633(3) 1 d D . P A 1 C2A C 1.0160(6) 0.8708(4) -0.0039(3) 0.0398(11) Uani 0.633(3) 1 d . . P A 1 H2A H 1.051989 0.910434 -0.004247 0.048 Uiso 0.633(3) 1 calc R U P A 1 C3A C 1.0788(6) 0.8175(6) 0.0052(4) 0.0430(13) Uani 0.633(3) 1 d . . P A 1 H3A H 1.158882 0.821053 0.010366 0.052 Uiso 0.633(3) 1 calc R U P A 1 C4A C 1.0311(9) 0.7587(5) 0.0071(5) 0.0410(13) Uani 0.633(3) 1 d . . P A 1 C5A C 0.9129(9) 0.7550(3) -0.0009(4) 0.0401(12) Uani 0.633(3) 1 d . . P A 1 H5A H 0.876874 0.715482 0.000407 0.048 Uiso 0.633(3) 1 calc R U P A 1 C6A C 0.8478(6) 0.8081(3) -0.0105(2) 0.0386(11) Uani 0.633(3) 1 d . . P A 1 H6A H 0.767750 0.805038 -0.015910 0.046 Uiso 0.633(3) 1 calc R U P A 1 C7A C 1.1105(13) 0.7036(7) 0.0170(6) 0.0497(18) Uani 0.633(3) 1 d . . P A 1 H7AA H 1.180647 0.716543 0.034406 0.075 Uiso 0.633(3) 1 d R U P A 1 H7AB H 1.073297 0.674363 0.035796 0.075 Uiso 0.633(3) 1 d R U P A 1 H7AC H 1.125207 0.684243 -0.012434 0.075 Uiso 0.633(3) 1 d R U P A 1 S1B S 0.7886(2) 0.91659(14) -0.00757(9) 0.0376(5) Uani 0.367(3) 1 d D . P A 2 S2B S 0.6691(5) 0.8003(3) 0.15368(15) 0.0182(3) Uani 0.367(3) 1 d D . P A 2 O1B O 0.6813(5) 0.8952(3) -0.02943(19) 0.0481(14) Uani 0.367(3) 1 d D . P A 2 O2B O 0.8489(7) 0.9696(4) -0.0271(2) 0.0474(8) Uani 0.367(3) 1 d D . P A 2 O3B O 0.6451(7) 0.8267(4) 0.1069(3) 0.0287(8) Uani 0.367(3) 1 d D . P A 2 O4B O 0.5927(9) 0.7603(5) 0.1731(3) 0.0256(8) Uani 0.367(3) 1 d D . P A 2 N1B N 0.7694(8) 0.9339(4) 0.0463(3) 0.0290(8) Uani 0.367(3) 1 d D . P A 2 H1B H 0.731867 0.901761 0.058589 0.038 Uiso 0.367(3) 1 d R U P A 2 C1B C 0.8839(9) 0.8530(4) -0.0025(4) 0.0343(10) Uani 0.367(3) 1 d DG . P A 2 C6B C 0.8411(10) 0.7927(5) -0.0010(4) 0.0386(11) Uani 0.367(3) 1 d G . P A 2 H6B H 0.761671 0.785993 -0.005284 0.046 Uiso 0.367(3) 1 calc R U P A 2 C5B C 0.9145(17) 0.7423(4) 0.0068(7) 0.0401(12) Uani 0.367(3) 1 d G . P A 2 H5B H 0.885188 0.701125 0.007883 0.048 Uiso 0.367(3) 1 calc R U P A 2 C4B C 1.0307(15) 0.7522(8) 0.0132(9) 0.0410(13) Uani 0.367(3) 1 d G . P A 2 C3B C 1.0735(9) 0.8125(10) 0.0116(8) 0.0430(13) Uani 0.367(3) 1 d G . P A 2 H3B H 1.152946 0.819230 0.015951 0.052 Uiso 0.367(3) 1 calc R U P A 2 C2B C 1.0002(10) 0.8629(7) 0.0038(5) 0.0398(11) Uani 0.367(3) 1 d G . P A 2 H2B H 1.029431 0.904098 0.002784 0.048 Uiso 0.367(3) 1 calc R U P A 2 C7B C 1.093(2) 0.6937(13) 0.0232(11) 0.0497(18) Uani 0.367(3) 1 d . . P A 2 H7BA H 1.103764 0.674703 -0.006827 0.075 Uiso 0.367(3) 1 d R U P A 2 H7BB H 1.165294 0.701983 0.040823 0.075 Uiso 0.367(3) 1 d R U P A 2 H7BC H 1.050814 0.665823 0.041273 0.075 Uiso 0.367(3) 1 d R U P A 2 O1S O 0.5867(3) 0.85985(18) 0.02327(12) 0.0682(11) Uani 0.633(3) 1 d . . P A 1 H1S H 0.588224 0.851857 0.052545 0.102 Uiso 0.633(3) 1 d R U P A 1 C1S C 0.5043(5) 0.9065(3) 0.0103(2) 0.083(2) Uani 0.633(3) 1 d . . P A 1 H1SA H 0.520797 0.943534 0.030285 0.125 Uiso 0.633(3) 1 calc R U P A 1 H1SB H 0.429138 0.890457 0.014957 0.125 Uiso 0.633(3) 1 calc R U P A 1 H1SC H 0.505996 0.917685 -0.023378 0.125 Uiso 0.633(3) 1 calc R U P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1' 0.0263(2) 0.0324(3) 0.0210(2) 0.00037(19) 0.00093(18) 0.0017(2) S2' 0.01515(19) 0.0176(2) 0.0195(2) 0.00200(16) 0.00176(15) 0.00158(15) O1' 0.0318(8) 0.0495(10) 0.0295(8) 0.0111(7) 0.0052(6) -0.0029(7) O2' 0.0410(9) 0.0445(10) 0.0336(8) -0.0140(7) 0.0008(7) 0.0067(8) O3' 0.0245(7) 0.0231(7) 0.0205(6) 0.0005(5) 0.0041(5) 0.0032(5) O4' 0.0169(6) 0.0258(7) 0.0292(7) 0.0007(6) 0.0011(5) -0.0033(5) O5' 0.0230(7) 0.0237(7) 0.0380(8) -0.0052(6) 0.0069(6) 0.0005(6) O6' 0.0164(6) 0.0260(7) 0.0439(9) -0.0010(6) -0.0010(6) 0.0025(5) N1' 0.0235(8) 0.0259(9) 0.0232(8) 0.0031(7) -0.0014(6) -0.0033(7) N2' 0.0213(8) 0.0181(7) 0.0207(8) 0.0032(6) 0.0001(6) 0.0034(6) N3' 0.0185(7) 0.0184(7) 0.0269(8) 0.0021(6) -0.0011(6) 0.0015(6) N4' 0.0182(7) 0.0222(8) 0.0265(8) 0.0071(6) -0.0036(6) -0.0027(6) C1' 0.0267(10) 0.0310(10) 0.0208(9) 0.0075(8) 0.0006(7) 0.0011(8) C2' 0.0335(12) 0.0546(15) 0.0241(10) -0.0068(10) -0.0014(9) 0.0014(11) C3' 0.0313(12) 0.0699(18) 0.0268(11) 0.0027(11) -0.0042(9) -0.0010(12) C4' 0.0298(11) 0.0463(13) 0.0365(12) 0.0248(10) 0.0049(9) 0.0049(10) C5' 0.0414(13) 0.0246(11) 0.0587(16) 0.0100(10) 0.0114(11) 0.0054(10) C6' 0.0331(11) 0.0239(10) 0.0448(13) 0.0034(9) 0.0005(9) -0.0020(9) C7' 0.0344(13) 0.072(2) 0.0612(17) 0.0374(15) 0.0108(12) 0.0136(13) C8' 0.0189(8) 0.0206(9) 0.0261(9) 0.0032(7) -0.0011(7) -0.0002(7) C9' 0.0196(8) 0.0165(8) 0.0237(9) 0.0005(7) -0.0014(7) 0.0010(7) C10' 0.0244(9) 0.0206(9) 0.0308(10) -0.0014(8) 0.0002(8) 0.0026(7) C11' 0.0203(9) 0.0152(8) 0.0260(9) 0.0019(7) 0.0006(7) 0.0025(7) C12' 0.0256(10) 0.0230(9) 0.0279(10) -0.0003(8) -0.0009(8) -0.0022(8) C13' 0.0254(10) 0.0237(10) 0.0392(12) -0.0016(8) 0.0025(8) -0.0054(8) C14' 0.0321(11) 0.0251(10) 0.0373(11) 0.0015(9) 0.0115(9) -0.0017(8) C15' 0.0336(11) 0.0246(10) 0.0281(10) 0.0031(8) 0.0034(8) 0.0014(8) C16' 0.0238(9) 0.0190(9) 0.0285(10) 0.0027(7) -0.0010(7) 0.0012(7) C17' 0.0238(9) 0.0184(9) 0.0264(9) 0.0033(7) 0.0028(7) 0.0021(7) C18' 0.0197(9) 0.0256(10) 0.0364(11) -0.0010(8) 0.0058(8) 0.0016(8) C19' 0.0224(10) 0.0274(11) 0.0485(13) -0.0039(9) -0.0020(9) 0.0082(8) C20' 0.0307(11) 0.0203(9) 0.0444(13) 0.0063(9) -0.0065(9) 0.0059(8) C21' 0.0206(9) 0.0218(9) 0.0303(10) 0.0094(8) -0.0058(7) 0.0009(7) C22' 0.0133(8) 0.0216(9) 0.0237(9) 0.0064(7) -0.0016(6) -0.0028(7) C23' 0.0146(8) 0.0253(9) 0.0290(10) 0.0034(8) -0.0011(7) -0.0005(7) C24' 0.0161(8) 0.0261(9) 0.0212(9) 0.0040(7) 0.0013(7) 0.0036(7) C25' 0.0164(8) 0.0325(10) 0.0251(9) 0.0109(8) -0.0028(7) 0.0006(7) C26' 0.0202(9) 0.0434(12) 0.0323(11) 0.0124(9) -0.0014(8) -0.0061(9) C27' 0.0229(10) 0.0693(17) 0.0357(12) 0.0199(12) 0.0032(9) -0.0083(11) C28' 0.0335(12) 0.088(2) 0.0247(11) 0.0133(12) 0.0054(9) -0.0035(13) C29' 0.0419(14) 0.0647(17) 0.0261(11) 0.0012(11) 0.0008(10) -0.0098(12) C30' 0.0289(11) 0.0414(12) 0.0259(10) 0.0063(9) 0.0000(8) -0.0067(9) C31' 0.0180(8) 0.0175(8) 0.0183(8) 0.0046(6) 0.0029(6) 0.0029(6) C32' 0.0254(10) 0.0211(9) 0.0396(12) -0.0035(8) -0.0004(8) 0.0020(8) C33' 0.0359(12) 0.0223(10) 0.0431(13) -0.0033(9) 0.0065(10) 0.0083(9) C34' 0.0272(10) 0.0315(11) 0.0268(10) 0.0114(8) 0.0098(8) 0.0136(8) C35' 0.0182(9) 0.0383(12) 0.0428(12) 0.0029(10) 0.0045(8) 0.0035(8) C36' 0.0207(9) 0.0261(10) 0.0388(11) -0.0040(8) 0.0020(8) 0.0003(8) C37' 0.0351(12) 0.0498(15) 0.0432(13) 0.0113(11) 0.0135(10) 0.0239(11) O5 0.0269(7) 0.0258(7) 0.0379(8) 0.0079(6) -0.0014(6) 0.0063(6) O6 0.0174(6) 0.0357(8) 0.0347(8) 0.0068(6) 0.0053(5) 0.0063(6) N2 0.0247(8) 0.0178(7) 0.0211(8) -0.0035(6) 0.0003(6) 0.0044(6) N3 0.0198(8) 0.0240(8) 0.0247(8) 0.0040(6) 0.0026(6) 0.0011(6) N4 0.0220(8) 0.0170(7) 0.0216(7) -0.0029(6) 0.0047(6) -0.0005(6) C8 0.0275(10) 0.0278(10) 0.0261(10) -0.0044(8) 0.0034(8) -0.0018(8) C9 0.0232(9) 0.0192(8) 0.0210(9) 0.0037(7) 0.0027(7) 0.0019(7) C10 0.0278(10) 0.0220(9) 0.0372(11) 0.0076(8) -0.0019(8) 0.0007(8) C11 0.0214(9) 0.0180(8) 0.0234(9) 0.0013(7) 0.0026(7) 0.0031(7) C12 0.0280(10) 0.0266(10) 0.0229(9) 0.0014(8) 0.0046(8) -0.0007(8) C13 0.0265(10) 0.0290(11) 0.0372(11) 0.0001(9) 0.0040(8) -0.0040(8) C14 0.0297(11) 0.0273(10) 0.0330(11) -0.0033(9) -0.0055(8) -0.0003(8) C15 0.0337(11) 0.0282(10) 0.0223(9) -0.0008(8) 0.0006(8) 0.0041(8) C16 0.0260(9) 0.0221(9) 0.0232(9) 0.0006(7) 0.0046(7) 0.0019(7) C17 0.0261(10) 0.0229(9) 0.0218(9) 0.0004(7) 0.0008(7) 0.0030(7) C18 0.0205(9) 0.0406(12) 0.0309(11) 0.0025(9) -0.0002(8) 0.0047(8) C19 0.0316(11) 0.0428(13) 0.0384(12) 0.0101(10) 0.0075(9) 0.0212(10) C20 0.0439(13) 0.0243(10) 0.0348(11) 0.0012(8) 0.0114(10) 0.0154(9) C21 0.0268(10) 0.0223(9) 0.0238(9) -0.0035(7) 0.0083(7) 0.0064(7) C22 0.0135(8) 0.0187(8) 0.0216(8) -0.0013(7) 0.0034(6) -0.0008(6) C23 0.0159(8) 0.0264(9) 0.0269(9) 0.0010(8) 0.0029(7) -0.0003(7) C24 0.0178(8) 0.0197(8) 0.0215(9) -0.0021(7) 0.0010(7) 0.0043(7) C25 0.0155(8) 0.0231(9) 0.0203(8) -0.0051(7) 0.0035(6) -0.0004(7) C26 0.0235(10) 0.0340(11) 0.0287(10) 0.0002(8) 0.0034(8) -0.0116(8) C27 0.0250(10) 0.0491(14) 0.0313(11) -0.0073(10) -0.0011(8) -0.0165(10) C28 0.0285(11) 0.0507(14) 0.0237(10) -0.0020(9) -0.0029(8) -0.0074(10) C29 0.0331(11) 0.0428(13) 0.0260(10) 0.0064(9) -0.0018(8) -0.0090(10) C30 0.0235(9) 0.0297(10) 0.0267(10) 0.0013(8) -0.0009(7) -0.0087(8) C31 0.0214(9) 0.0207(9) 0.0203(8) -0.0083(7) -0.0004(7) 0.0038(7) C32 0.0253(10) 0.0258(10) 0.0295(10) 0.0002(8) 0.0042(8) 0.0004(8) C33 0.0300(11) 0.0265(10) 0.0329(11) 0.0017(8) -0.0030(8) 0.0074(8) C34 0.0213(9) 0.0321(11) 0.0319(10) -0.0119(9) -0.0001(8) 0.0054(8) C35 0.0313(11) 0.0350(12) 0.0346(11) -0.0066(9) 0.0147(9) -0.0024(9) C36 0.0379(11) 0.0239(10) 0.0254(10) 0.0007(8) 0.0075(8) 0.0036(8) C37 0.0266(12) 0.0544(16) 0.0640(17) -0.0179(13) 0.0008(11) 0.0154(11) S1A 0.0518(8) 0.0427(8) 0.0151(5) -0.0033(4) 0.0048(4) -0.0108(6) S2A 0.0177(6) 0.0219(7) 0.0151(9) -0.0039(6) 0.0025(6) 0.0030(5) O1A 0.069(2) 0.0476(18) 0.0211(13) -0.0030(12) -0.0088(13) -0.0052(15) O2A 0.071(3) 0.045(2) 0.0281(10) 0.0041(12) 0.0154(16) -0.0210(15) O3A 0.029(2) 0.033(2) 0.0221(16) -0.0043(12) -0.0038(12) 0.0081(14) O4A 0.0214(8) 0.0232(15) 0.034(3) -0.0037(17) 0.0120(18) -0.0053(9) N1A 0.0345(13) 0.034(2) 0.019(2) -0.0010(15) 0.0060(16) -0.0102(14) C1A 0.047(2) 0.047(2) 0.009(2) -0.0067(16) 0.0063(14) -0.0065(19) C2A 0.047(2) 0.052(2) 0.024(3) -0.0102(19) 0.0233(17) -0.0125(17) C3A 0.0357(14) 0.067(2) 0.029(3) -0.015(2) 0.0155(13) -0.0075(14) C4A 0.0436(13) 0.060(2) 0.020(4) -0.0089(19) 0.0062(15) 0.0014(15) C5A 0.0444(14) 0.043(3) 0.032(4) -0.004(2) -0.001(2) -0.008(2) C6A 0.0372(16) 0.048(3) 0.029(3) -0.007(2) -0.0056(17) -0.0053(19) C7A 0.048(5) 0.066(5) 0.037(4) 0.006(3) 0.014(3) 0.001(3) S1B 0.0486(13) 0.0415(13) 0.0216(10) -0.0091(9) -0.0009(8) -0.0005(10) S2B 0.0177(6) 0.0219(7) 0.0151(9) -0.0039(6) 0.0025(6) 0.0030(5) O1B 0.056(3) 0.051(3) 0.033(3) -0.013(2) -0.013(2) 0.002(2) O2B 0.071(3) 0.045(2) 0.0281(10) 0.0041(12) 0.0154(16) -0.0210(15) O3B 0.029(2) 0.033(2) 0.0221(16) -0.0043(12) -0.0038(12) 0.0081(14) O4B 0.0214(8) 0.0232(15) 0.034(3) -0.0037(17) 0.0120(18) -0.0053(9) N1B 0.0345(13) 0.034(2) 0.019(2) -0.0010(15) 0.0060(16) -0.0102(14) C1B 0.047(2) 0.047(2) 0.009(2) -0.0067(16) 0.0063(14) -0.0065(19) C6B 0.0372(16) 0.048(3) 0.029(3) -0.007(2) -0.0056(17) -0.0053(19) C5B 0.0444(14) 0.043(3) 0.032(4) -0.004(2) -0.001(2) -0.008(2) C4B 0.0436(13) 0.060(2) 0.020(4) -0.0089(19) 0.0062(15) 0.0014(15) C3B 0.0357(14) 0.067(2) 0.029(3) -0.015(2) 0.0155(13) -0.0075(14) C2B 0.047(2) 0.052(2) 0.024(3) -0.0102(19) 0.0233(17) -0.0125(17) C7B 0.048(5) 0.066(5) 0.037(4) 0.006(3) 0.014(3) 0.001(3) O1S 0.058(2) 0.090(3) 0.054(2) 0.0383(19) -0.0071(16) -0.0108(19) C1S 0.078(4) 0.111(5) 0.056(3) -0.017(3) -0.014(3) -0.029(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0990 0.00 -1.00 0.00 0.1230 0.00 1.00 -1.00 0.0910 0.00 0.00 -1.00 0.0690 0.00 0.00 1.00 0.0690 -1.00 0.00 -1.00 0.1970 1.00 -1.00 0.00 0.1660 0.00 1.00 1.00 0.1040 -1.00 0.00 1.00 0.1960 -1.00 -1.00 1.00 0.1830 1.00 1.00 -1.00 0.2310 -1.00 -2.00 2.00 0.1530 0.00 -2.00 -1.00 0.0980 0.00 -1.00 1.00 0.1270 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 O1' S1' N1' 105.29(9) . . ? O1' S1' C1' 110.48(10) . . ? O2' S1' O1' 119.65(10) . . ? O2' S1' N1' 108.57(10) . . ? O2' S1' C1' 106.48(10) . . ? N1' S1' C1' 105.54(9) . . ? O3' S2' N2' 105.18(8) . . ? O3' S2' C31' 108.55(8) . . ? O4' S2' O3' 119.31(8) . . ? O4' S2' N2' 109.16(8) . . ? O4' S2' C31' 106.42(8) . . ? N2' S2' C31' 107.77(8) . . ? C17' O5' C10' 106.30(14) . . ? C21' O6' C23' 105.88(14) . . ? S1' N1' H1' 113(2) . . ? C8' N1' S1' 120.56(14) . . ? C8' N1' H1' 120(2) . . ? S2' N2' H2' 111.7(18) . . ? C24' N2' S2' 120.95(13) . . ? C24' N2' H2' 116.8(18) . . ? C17' N3' C9' 107.59(16) . . ? C21' N4' C22' 107.38(15) . . ? C2' C1' S1' 120.09(17) . . ? C2' C1' C6' 120.4(2) . . ? C6' C1' S1' 119.50(16) . . ? C1' C2' H2'A 120.4 . . ? C1' C2' C3' 119.2(2) . . ? C3' C2' H2'A 120.4 . . ? C2' C3' H3' 119.3 . . ? C4' C3' C2' 121.4(2) . . ? C4' C3' H3' 119.3 . . ? C3' C4' C5' 119.0(2) . . ? C3' C4' C7' 121.1(3) . . ? C5' C4' C7' 119.9(3) . . ? C4' C5' H5' 119.7 . . ? C6' C5' C4' 120.6(2) . . ? C6' C5' H5' 119.7 . . ? C1' C6' C5' 119.4(2) . . ? C1' C6' H6' 120.3 . . ? C5' C6' H6' 120.3 . . ? C4' C7' H7'A 109.5 . . ? C4' C7' H7'B 109.5 . . ? C4' C7' H7'C 109.5 . . ? H7'A C7' H7'B 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? N1' C8' H8'A 109.3 . . ? N1' C8' H8'B 109.3 . . ? N1' C8' C9' 111.60(15) . . ? H8'A C8' H8'B 108.0 . . ? C9' C8' H8'A 109.3 . . ? C9' C8' H8'B 109.3 . . ? N3' C9' C8' 107.95(14) . . ? N3' C9' C10' 103.67(15) . . ? N3' C9' C11' 112.06(15) . . ? C8' C9' C10' 110.69(16) . . ? C11' C9' C8' 108.49(15) . . ? C11' C9' C10' 113.79(15) . . ? O5' C10' C9' 104.23(15) . . ? O5' C10' H10A 110.9 . . ? O5' C10' H10B 110.9 . . ? C9' C10' H10A 110.9 . . ? C9' C10' H10B 110.9 . . ? H10A C10' H10B 108.9 . . ? C12' C11' C9' 118.69(17) . . ? C16' C11' C9' 122.14(17) . . ? C16' C11' C12' 119.16(18) . . ? C11' C12' H12' 119.7 . . ? C13' C12' C11' 120.58(19) . . ? C13' C12' H12' 119.7 . . ? C12' C13' H13' 120.0 . . ? C12' C13' C14' 120.06(19) . . ? C14' C13' H13' 120.0 . . ? C13' C14' H14' 120.1 . . ? C13' C14' C15' 119.9(2) . . ? C15' C14' H14' 120.1 . . ? C14' C15' H15' 119.9 . . ? C14' C15' C16' 120.3(2) . . ? C16' C15' H15' 119.9 . . ? C11' C16' C15' 120.00(18) . . ? C11' C16' H16' 120.0 . . ? C15' C16' H16' 120.0 . . ? O5' C17' C18' 115.13(16) . . ? N3' C17' O5' 118.10(17) . . ? N3' C17' C18' 126.76(18) . . ? C17' C18' H18A 109.1 . . ? C17' C18' H18B 109.1 . . ? C17' C18' C19' 112.36(17) . . ? H18A C18' H18B 107.9 . . ? C19' C18' H18A 109.1 . . ? C19' C18' H18B 109.1 . . ? C18' C19' H19A 109.0 . . ? C18' C19' H19B 109.0 . . ? H19A C19' H19B 107.8 . . ? C20' C19' C18' 112.93(17) . . ? C20' C19' H19A 109.0 . . ? C20' C19' H19B 109.0 . . ? C19' C20' H20A 109.1 . . ? C19' C20' H20B 109.1 . . ? H20A C20' H20B 107.8 . . ? C21' C20' C19' 112.46(18) . . ? C21' C20' H20A 109.1 . . ? C21' C20' H20B 109.1 . . ? O6' C21' C20' 114.90(18) . . ? N4' C21' O6' 118.46(18) . . ? N4' C21' C20' 126.60(19) . . ? N4' C22' C23' 103.58(15) . . ? N4' C22' C24' 108.21(14) . . ? N4' C22' C25' 111.81(15) . . ? C24' C22' C23' 111.23(15) . . ? C25' C22' C23' 114.60(15) . . ? C25' C22' C24' 107.29(15) . . ? O6' C23' C22' 104.65(15) . . ? O6' C23' H23A 110.8 . . ? O6' C23' H23B 110.8 . . ? C22' C23' H23A 110.8 . . ? C22' C23' H23B 110.8 . . ? H23A C23' H23B 108.9 . . ? N2' C24' C22' 110.80(15) . . ? N2' C24' H24A 109.5 . . ? N2' C24' H24B 109.5 . . ? C22' C24' H24A 109.5 . . ? C22' C24' H24B 109.5 . . ? H24A C24' H24B 108.1 . . ? C26' C25' C22' 120.90(19) . . ? C30' C25' C22' 120.04(17) . . ? C30' C25' C26' 118.9(2) . . ? C25' C26' H26' 119.8 . . ? C27' C26' C25' 120.4(2) . . ? C27' C26' H26' 119.8 . . ? C26' C27' H27' 120.1 . . ? C28' C27' C26' 119.9(2) . . ? C28' C27' H27' 120.1 . . ? C27' C28' H28' 119.9 . . ? C29' C28' C27' 120.1(2) . . ? C29' C28' H28' 119.9 . . ? C28' C29' H29' 120.1 . . ? C28' C29' C30' 119.8(2) . . ? C30' C29' H29' 120.1 . . ? C25' C30' H30' 119.6 . . ? C29' C30' C25' 120.8(2) . . ? C29' C30' H30' 119.6 . . ? C32' C31' S2' 120.15(15) . . ? C32' C31' C36' 119.98(18) . . ? C36' C31' S2' 119.88(14) . . ? C31' C32' H32' 120.2 . . ? C31' C32' C33' 119.59(19) . . ? C33' C32' H32' 120.2 . . ? C32' C33' H33' 119.4 . . ? C34' C33' C32' 121.1(2) . . ? C34' C33' H33' 119.4 . . ? C33' C34' C35' 118.38(18) . . ? C33' C34' C37' 120.9(2) . . ? C35' C34' C37' 120.7(2) . . ? C34' C35' H35' 119.4 . . ? C36' C35' C34' 121.1(2) . . ? C36' C35' H35' 119.4 . . ? C31' C36' H36' 120.1 . . ? C35' C36' C31' 119.81(19) . . ? C35' C36' H36' 120.1 . . ? C34' C37' H37A 109.5 . . ? C34' C37' H37B 109.5 . . ? C34' C37' H37C 109.5 . . ? H37A C37' H37B 109.5 . . ? H37A C37' H37C 109.5 . . ? H37B C37' H37C 109.5 . . ? C17 O5 C10 106.28(15) . . ? C21 O6 C23 105.84(14) . . ? C24 N2 H2 117.6(16) . . ? C24 N2 S2A 116.58(16) . . ? C24 N2 S2B 125.3(2) . . ? S2A N2 H2 116.7(16) . . ? S2B N2 H2 104.8(16) . . ? C17 N3 C9 107.58(16) . . ? C21 N4 C22 107.47(15) . . ? H8AA C8 H8AB 108.0 . . ? H8A C8 H8B 108.5 . . ? C9 C8 H8AA 109.4 . . ? C9 C8 H8AB 109.4 . . ? C9 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? N1A C8 H8AA 109.4 . . ? N1A C8 H8AB 109.4 . . ? N1A C8 C9 111.3(2) . . ? N1B C8 H8A 110.2 . . ? N1B C8 H8B 110.2 . . ? N1B C8 C9 107.4(4) . . ? N3 C9 C8 107.64(15) . . ? N3 C9 C10 103.21(15) . . ? N3 C9 C11 112.73(15) . . ? C8 C9 C10 112.00(16) . . ? C11 C9 C8 109.39(15) . . ? C11 C9 C10 111.73(16) . . ? O5 C10 C9 104.59(15) . . ? O5 C10 H10C 110.8 . . ? O5 C10 H10D 110.8 . . ? C9 C10 H10C 110.8 . . ? C9 C10 H10D 110.8 . . ? H10C C10 H10D 108.9 . . ? C12 C11 C9 119.37(17) . . ? C16 C11 C9 121.68(17) . . ? C16 C11 C12 118.94(18) . . ? C11 C12 H12 119.6 . . ? C13 C12 C11 120.75(19) . . ? C13 C12 H12 119.6 . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.0(2) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.84(19) . . ? C15 C14 H14 120.1 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.37(19) . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.09(18) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? O5 C17 C18 115.22(17) . . ? N3 C17 O5 118.09(18) . . ? N3 C17 C18 126.69(18) . . ? C17 C18 H18C 109.0 . . ? C17 C18 H18D 109.0 . . ? C17 C18 C19 112.95(19) . . ? H18C C18 H18D 107.8 . . ? C19 C18 H18C 109.0 . . ? C19 C18 H18D 109.0 . . ? C18 C19 H19C 108.9 . . ? C18 C19 H19D 108.9 . . ? C18 C19 C20 113.50(17) . . ? H19C C19 H19D 107.7 . . ? C20 C19 H19C 108.9 . . ? C20 C19 H19D 108.9 . . ? C19 C20 H20C 109.0 . . ? C19 C20 H20D 109.0 . . ? H20C C20 H20D 107.8 . . ? C21 C20 C19 112.93(19) . . ? C21 C20 H20C 109.0 . . ? C21 C20 H20D 109.0 . . ? O6 C21 C20 115.21(18) . . ? N4 C21 O6 118.57(17) . . ? N4 C21 C20 126.20(19) . . ? N4 C22 C23 103.39(14) . . ? N4 C22 C24 108.10(14) . . ? N4 C22 C25 111.36(14) . . ? C24 C22 C23 111.39(15) . . ? C25 C22 C23 114.91(15) . . ? C25 C22 C24 107.54(14) . . ? O6 C23 C22 104.61(15) . . ? O6 C23 H23C 110.8 . . ? O6 C23 H23D 110.8 . . ? C22 C23 H23C 110.8 . . ? C22 C23 H23D 110.8 . . ? H23C C23 H23D 108.9 . . ? N2 C24 C22 110.99(14) . . ? N2 C24 H24C 109.4 . . ? N2 C24 H24D 109.4 . . ? C22 C24 H24C 109.4 . . ? C22 C24 H24D 109.4 . . ? H24C C24 H24D 108.0 . . ? C26 C25 C22 120.51(17) . . ? C26 C25 C30 118.91(18) . . ? C30 C25 C22 120.42(16) . . ? C25 C26 H26 119.8 . . ? C25 C26 C27 120.36(19) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.29(19) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.6(2) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 119.8 . . ? C28 C29 C30 120.3(2) . . ? C30 C29 H29 119.8 . . ? C25 C30 H30 119.7 . . ? C29 C30 C25 120.55(19) . . ? C29 C30 H30 119.7 . . ? C32 C31 C36 120.45(18) . . ? C32 C31 S2A 116.04(16) . . ? C32 C31 S2B 126.6(2) . . ? C36 C31 S2A 123.45(17) . . ? C36 C31 S2B 112.9(2) . . ? C31 C32 H32 120.4 . . ? C31 C32 C33 119.17(19) . . ? C33 C32 H32 120.4 . . ? C32 C33 H33 119.4 . . ? C34 C33 C32 121.2(2) . . ? C34 C33 H33 119.4 . . ? C33 C34 C35 118.64(19) . . ? C33 C34 C37 120.2(2) . . ? C35 C34 C37 121.2(2) . . ? C34 C35 H35 119.5 . . ? C36 C35 C34 121.0(2) . . ? C36 C35 H35 119.5 . . ? C31 C36 H36 120.3 . . ? C35 C36 C31 119.48(19) . . ? C35 C36 H36 120.3 . . ? C34 C37 H37D 109.5 . . ? C34 C37 H37E 109.5 . . ? C34 C37 H37F 109.5 . . ? H37D C37 H37E 109.5 . . ? H37D C37 H37F 109.5 . . ? H37E C37 H37F 109.5 . . ? O1A S1A O2A 120.1(2) . . ? O1A S1A N1A 107.0(2) . . ? O1A S1A C1A 108.4(3) . . ? O2A S1A N1A 107.2(2) . . ? O2A S1A C1A 107.8(3) . . ? N1A S1A C1A 105.4(2) . . ? N2 S2A C31 105.86(18) . . ? O3A S2A N2 104.8(2) . . ? O3A S2A C31 106.1(2) . . ? O4A S2A N2 111.5(2) . . ? O4A S2A C31 109.0(3) . . ? O4A S2A O3A 118.7(3) . . ? C8 N1A S1A 118.4(3) . . ? C8 N1A H1A 96.0 . . ? S1A N1A H1A 126.5 . . ? C2A C1A S1A 119.1(5) . . ? C2A C1A C6A 120.3(4) . . ? C6A C1A S1A 120.2(4) . . ? C1A C2A H2A 120.5 . . ? C3A C2A C1A 118.9(4) . . ? C3A C2A H2A 120.5 . . ? C2A C3A H3A 118.4 . . ? C2A C3A C4A 123.1(4) . . ? C4A C3A H3A 118.4 . . ? C3A C4A C5A 117.1(4) . . ? C3A C4A C7A 117.6(10) . . ? C5A C4A C7A 125.3(10) . . ? C4A C5A H5A 119.6 . . ? C6A C5A C4A 120.8(4) . . ? C6A C5A H5A 119.6 . . ? C1A C6A H6A 120.1 . . ? C5A C6A C1A 119.8(4) . . ? C5A C6A H6A 120.1 . . ? C4A C7A H7AA 111.0 . . ? C4A C7A H7AB 107.1 . . ? C4A C7A H7AC 110.3 . . ? H7AA C7A H7AB 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? O1B S1B O2B 122.2(4) . . ? O1B S1B N1B 105.5(4) . . ? O1B S1B C1B 108.8(5) . . ? O2B S1B N1B 107.5(4) . . ? O2B S1B C1B 106.7(4) . . ? N1B S1B C1B 105.0(5) . . ? N2 S2B C31 108.0(3) . . ? O3B S2B N2 107.7(5) . . ? O3B S2B C31 111.8(4) . . ? O4B S2B N2 103.9(5) . . ? O4B S2B C31 102.8(5) . . ? O4B S2B O3B 121.8(6) . . ? C8 N1B S1B 115.9(6) . . ? C8 N1B H1B 116.1 . . ? S1B N1B H1B 108.3 . . ? C6B C1B S1B 118.9(7) . . ? C6B C1B C2B 120.0 . . ? C2B C1B S1B 120.9(8) . . ? C1B C6B H6B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B H6B 120.0 . . ? C6B C5B H5B 120.0 . . ? C4B C5B C6B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C4B C7B 111.6(17) . . ? C3B C4B C5B 120.0 . . ? C3B C4B C7B 128.3(18) . . ? C4B C3B H3B 120.0 . . ? C4B C3B C2B 120.0 . . ? C2B C3B H3B 120.0 . . ? C1B C2B H2B 120.0 . . ? C3B C2B C1B 120.0 . . ? C3B C2B H2B 120.0 . . ? C4B C7B H7BA 107.7 . . ? C4B C7B H7BB 110.2 . . ? C4B C7B H7BC 110.5 . . ? H7BA C7B H7BB 109.5 . . ? H7BA C7B H7BC 109.4 . . ? H7BB C7B H7BC 109.5 . . ? C1S O1S H1S 109.6 . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 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 S1' O1' 1.4324(17) . ? S1' O2' 1.4308(17) . ? S1' N1' 1.6198(17) . ? S1' C1' 1.764(2) . ? S2' O3' 1.4389(14) . ? S2' O4' 1.4352(14) . ? S2' N2' 1.6105(16) . ? S2' C31' 1.7612(18) . ? O5' C10' 1.451(2) . ? O5' C17' 1.355(2) . ? O6' C21' 1.360(2) . ? O6' C23' 1.443(2) . ? N1' H1' 0.80(3) . ? N1' C8' 1.453(2) . ? N2' H2' 0.85(3) . ? N2' C24' 1.465(2) . ? N3' C9' 1.476(2) . ? N3' C17' 1.273(2) . ? N4' C21' 1.269(3) . ? N4' C22' 1.476(2) . ? C1' C2' 1.384(3) . ? C1' C6' 1.385(3) . ? C2' H2'A 0.9500 . ? C2' C3' 1.386(3) . ? C3' H3' 0.9500 . ? C3' C4' 1.372(4) . ? C4' C5' 1.390(4) . ? C4' C7' 1.512(3) . ? C5' H5' 0.9500 . ? C5' C6' 1.389(3) . ? C6' H6' 0.9500 . ? C7' H7'A 0.9800 . ? C7' H7'B 0.9800 . ? C7' H7'C 0.9800 . ? C8' H8'A 0.9900 . ? C8' H8'B 0.9900 . ? C8' C9' 1.538(2) . ? C9' C10' 1.548(3) . ? C9' C11' 1.519(3) . ? C10' H10A 0.9900 . ? C10' H10B 0.9900 . ? C11' C12' 1.400(3) . ? C11' C16' 1.385(3) . ? C12' H12' 0.9500 . ? C12' C13' 1.382(3) . ? C13' H13' 0.9500 . ? C13' C14' 1.384(3) . ? C14' H14' 0.9500 . ? C14' C15' 1.385(3) . ? C15' H15' 0.9500 . ? C15' C16' 1.397(3) . ? C16' H16' 0.9500 . ? C17' C18' 1.493(3) . ? C18' H18A 0.9900 . ? C18' H18B 0.9900 . ? C18' C19' 1.536(3) . ? C19' H19A 0.9900 . ? C19' H19B 0.9900 . ? C19' C20' 1.526(3) . ? C20' H20A 0.9900 . ? C20' H20B 0.9900 . ? C20' C21' 1.488(3) . ? C22' C23' 1.547(2) . ? C22' C24' 1.543(2) . ? C22' C25' 1.520(3) . ? C23' H23A 0.9900 . ? C23' H23B 0.9900 . ? C24' H24A 0.9900 . ? C24' H24B 0.9900 . ? C25' C26' 1.393(3) . ? C25' C30' 1.385(3) . ? C26' H26' 0.9500 . ? C26' C27' 1.386(3) . ? C27' H27' 0.9500 . ? C27' C28' 1.384(4) . ? C28' H28' 0.9500 . ? C28' C29' 1.383(4) . ? C29' H29' 0.9500 . ? C29' C30' 1.385(3) . ? C30' H30' 0.9500 . ? C31' C32' 1.380(3) . ? C31' C36' 1.384(3) . ? C32' H32' 0.9500 . ? C32' C33' 1.388(3) . ? C33' H33' 0.9500 . ? C33' C34' 1.384(3) . ? C34' C35' 1.385(3) . ? C34' C37' 1.504(3) . ? C35' H35' 0.9500 . ? C35' C36' 1.381(3) . ? C36' H36' 0.9500 . ? C37' H37A 0.9800 . ? C37' H37B 0.9800 . ? C37' H37C 0.9800 . ? O5 C10 1.445(3) . ? O5 C17 1.355(2) . ? O6 C21 1.361(2) . ? O6 C23 1.444(2) . ? N2 H2 0.87(3) . ? N2 C24 1.460(2) . ? N2 S2A 1.611(3) . ? N2 S2B 1.628(6) . ? N3 C9 1.482(2) . ? N3 C17 1.270(2) . ? N4 C21 1.265(2) . ? N4 C22 1.478(2) . ? C8 H8AA 0.9900 . ? C8 H8AB 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.531(3) . ? C8 N1A 1.512(5) . ? C8 N1B 1.427(9) . ? C9 C10 1.544(3) . ? C9 C11 1.523(3) . ? C10 H10C 0.9900 . ? C10 H10D 0.9900 . ? C11 C12 1.392(3) . ? C11 C16 1.388(3) . ? C12 H12 0.9500 . ? C12 C13 1.386(3) . ? C13 H13 0.9500 . ? C13 C14 1.380(3) . ? C14 H14 0.9500 . ? C14 C15 1.382(3) . ? C15 H15 0.9500 . ? C15 C16 1.393(3) . ? C16 H16 0.9500 . ? C17 C18 1.490(3) . ? C18 H18C 0.9900 . ? C18 H18D 0.9900 . ? C18 C19 1.532(3) . ? C19 H19C 0.9900 . ? C19 H19D 0.9900 . ? C19 C20 1.532(3) . ? C20 H20C 0.9900 . ? C20 H20D 0.9900 . ? C20 C21 1.489(3) . ? C22 C23 1.549(2) . ? C22 C24 1.533(2) . ? C22 C25 1.522(2) . ? C23 H23C 0.9900 . ? C23 H23D 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C25 C26 1.387(3) . ? C25 C30 1.389(3) . ? C26 H26 0.9500 . ? C26 C27 1.390(3) . ? C27 H27 0.9500 . ? C27 C28 1.383(3) . ? C28 H28 0.9500 . ? C28 C29 1.379(3) . ? C29 H29 0.9500 . ? C29 C30 1.386(3) . ? C30 H30 0.9500 . ? C31 C32 1.382(3) . ? C31 C36 1.386(3) . ? C31 S2A 1.795(3) . ? C31 S2B 1.734(6) . ? C32 H32 0.9500 . ? C32 C33 1.388(3) . ? C33 H33 0.9500 . ? C33 C34 1.381(3) . ? C34 C35 1.388(3) . ? C34 C37 1.506(3) . ? C35 H35 0.9500 . ? C35 C36 1.381(3) . ? C36 H36 0.9500 . ? C37 H37D 0.9800 . ? C37 H37E 0.9800 . ? C37 H37F 0.9800 . ? S1A O1A 1.429(3) . ? S1A O2A 1.441(3) . ? S1A N1A 1.619(4) . ? S1A C1A 1.759(5) . ? S2A O3A 1.442(4) . ? S2A O4A 1.437(3) . ? N1A H1A 0.8598 . ? C1A C2A 1.375(6) . ? C1A C6A 1.391(6) . ? C2A H2A 0.9500 . ? C2A C3A 1.374(7) . ? C3A H3A 0.9500 . ? C3A C4A 1.383(6) . ? C4A C5A 1.401(6) . ? C4A C7A 1.518(16) . ? C5A H5A 0.9500 . ? C5A C6A 1.386(6) . ? C6A H6A 0.9500 . ? C7A H7AA 0.9603 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9598 . ? S1B O1B 1.429(5) . ? S1B O2B 1.480(6) . ? S1B N1B 1.601(8) . ? S1B C1B 1.767(9) . ? S2B O3B 1.432(7) . ? S2B O4B 1.405(7) . ? N1B H1B 0.9100 . ? C1B C6B 1.3900 . ? C1B C2B 1.3900 . ? C6B H6B 0.9500 . ? C6B C5B 1.3900 . ? C5B H5B 0.9500 . ? C5B C4B 1.3900 . ? C4B C3B 1.3900 . ? C4B C7B 1.47(3) . ? C3B H3B 0.9500 . ? C3B C2B 1.3900 . ? C2B H2B 0.9500 . ? C7B H7BA 0.9601 . ? C7B H7BB 0.9597 . ? C7B H7BC 0.9603 . ? O1S H1S 0.8402 . ? O1S C1S 1.418(8) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? 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 _geom_hbond_publ_flag N1' H1' O3' 0.80(3) 2.33(3) 3.105(2) 165(3) . yes N2' H2' N3' 0.85(3) 2.07(3) 2.901(2) 166(2) . yes N2 H2 N3 0.87(3) 2.11(3) 2.968(2) 170(2) . yes N1A H1A O1S 0.86 2.27 2.923(5) 133.1 . yes N1B H1B O3B 0.91 2.41 3.307(10) 168.1 . yes O1S H1S O3A 0.84 1.95 2.764(5) 163.1 . yes 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 S1' N1' C8' C9' 129.85(15) . . . . ? S1' C1' C2' C3' -179.10(18) . . . . ? S1' C1' C6' C5' 178.87(17) . . . . ? S2' N2' C24' C22' -144.51(13) . . . . ? S2' C31' C32' C33' -179.15(17) . . . . ? S2' C31' C36' C35' 178.92(17) . . . . ? O1' S1' N1' C8' 165.60(15) . . . . ? O1' S1' C1' C2' 121.50(18) . . . . ? O1' S1' C1' C6' -58.65(19) . . . . ? O2' S1' N1' C8' -65.14(17) . . . . ? O2' S1' C1' C2' -9.9(2) . . . . ? O2' S1' C1' C6' 169.95(17) . . . . ? O3' S2' N2' C24' -170.06(13) . . . . ? O3' S2' C31' C32' -132.45(16) . . . . ? O3' S2' C31' C36' 47.81(18) . . . . ? O4' S2' N2' C24' 60.79(16) . . . . ? O4' S2' C31' C32' -2.87(18) . . . . ? O4' S2' C31' C36' 177.40(16) . . . . ? O5' C17' C18' C19' -70.9(2) . . . . ? N1' S1' C1' C2' -125.17(18) . . . . ? N1' S1' C1' C6' 54.67(19) . . . . ? N1' C8' C9' N3' 49.8(2) . . . . ? N1' C8' C9' C10' -63.0(2) . . . . ? N1' C8' C9' C11' 171.46(15) . . . . ? N2' S2' C31' C32' 114.11(16) . . . . ? N2' S2' C31' C36' -65.62(18) . . . . ? N3' C9' C10' O5' 1.26(19) . . . . ? N3' C9' C11' C12' -179.64(16) . . . . ? N3' C9' C11' C16' 1.7(2) . . . . ? N3' C17' C18' C19' 108.2(2) . . . . ? N4' C22' C23' O6' 1.81(18) . . . . ? N4' C22' C24' N2' -50.13(19) . . . . ? N4' C22' C25' C26' -21.0(2) . . . . ? N4' C22' C25' C30' 163.10(17) . . . . ? C1' S1' N1' C8' 48.70(18) . . . . ? C1' C2' C3' C4' -0.3(4) . . . . ? C2' C1' C6' C5' -1.3(3) . . . . ? C2' C3' C4' C5' -0.2(4) . . . . ? C2' C3' C4' C7' 179.8(2) . . . . ? C3' C4' C5' C6' 0.0(3) . . . . ? C4' C5' C6' C1' 0.7(3) . . . . ? C6' C1' C2' C3' 1.1(3) . . . . ? C7' C4' C5' C6' 180.0(2) . . . . ? C8' C9' C10' O5' 116.78(16) . . . . ? C8' C9' C11' C12' 61.3(2) . . . . ? C8' C9' C11' C16' -117.37(19) . . . . ? C9' N3' C17' O5' -2.7(2) . . . . ? C9' N3' C17' C18' 178.30(18) . . . . ? C9' C11' C12' C13' -175.78(18) . . . . ? C9' C11' C16' C15' 176.93(17) . . . . ? C10' O5' C17' N3' 3.5(2) . . . . ? C10' O5' C17' C18' -177.32(16) . . . . ? C10' C9' C11' C12' -62.4(2) . . . . ? C10' C9' C11' C16' 118.94(19) . . . . ? C11' C9' C10' O5' -120.73(16) . . . . ? C11' C12' C13' C14' -1.9(3) . . . . ? C12' C11' C16' C15' -1.7(3) . . . . ? C12' C13' C14' C15' -0.3(3) . . . . ? C13' C14' C15' C16' 1.5(3) . . . . ? C14' C15' C16' C11' -0.5(3) . . . . ? C16' C11' C12' C13' 2.9(3) . . . . ? C17' O5' C10' C9' -2.63(19) . . . . ? C17' N3' C9' C8' -116.81(17) . . . . ? C17' N3' C9' C10' 0.64(19) . . . . ? C17' N3' C9' C11' 123.77(17) . . . . ? C17' C18' C19' C20' -57.3(2) . . . . ? C18' C19' C20' C21' -52.3(2) . . . . ? C19' C20' C21' O6' -51.7(2) . . . . ? C19' C20' C21' N4' 125.8(2) . . . . ? C21' O6' C23' C22' -0.71(19) . . . . ? C21' N4' C22' C23' -2.35(19) . . . . ? C21' N4' C22' C24' 115.79(17) . . . . ? C21' N4' C22' C25' -126.26(17) . . . . ? C22' N4' C21' O6' 2.2(2) . . . . ? C22' N4' C21' C20' -175.19(18) . . . . ? C22' C25' C26' C27' -176.8(2) . . . . ? C22' C25' C30' C29' 176.0(2) . . . . ? C23' O6' C21' N4' -0.9(2) . . . . ? C23' O6' C21' C20' 176.75(16) . . . . ? C23' C22' C24' N2' 63.0(2) . . . . ? C23' C22' C25' C26' -138.46(19) . . . . ? C23' C22' C25' C30' 45.6(2) . . . . ? C24' C22' C23' O6' -114.22(17) . . . . ? C24' C22' C25' C26' 97.5(2) . . . . ? C24' C22' C25' C30' -78.4(2) . . . . ? C25' C22' C23' O6' 123.88(17) . . . . ? C25' C22' C24' N2' -170.93(15) . . . . ? C25' C26' C27' C28' 1.4(4) . . . . ? C26' C25' C30' C29' 0.0(3) . . . . ? C26' C27' C28' C29' -1.0(4) . . . . ? C27' C28' C29' C30' 0.2(4) . . . . ? C28' C29' C30' C25' 0.4(4) . . . . ? C30' C25' C26' C27' -0.8(3) . . . . ? C31' S2' N2' C24' -54.39(16) . . . . ? C31' C32' C33' C34' 0.5(3) . . . . ? C32' C31' C36' C35' -0.8(3) . . . . ? C32' C33' C34' C35' -1.3(3) . . . . ? C32' C33' C34' C37' 178.8(2) . . . . ? C33' C34' C35' C36' 1.1(3) . . . . ? C34' C35' C36' C31' 0.0(3) . . . . ? C36' C31' C32' C33' 0.6(3) . . . . ? C37' C34' C35' C36' -179.0(2) . . . . ? O5 C17 C18 C19 -66.2(2) . . . . ? N3 C9 C10 O5 -4.7(2) . . . . ? N3 C9 C11 C12 174.12(17) . . . . ? N3 C9 C11 C16 -7.0(2) . . . . ? N3 C17 C18 C19 113.1(2) . . . . ? N4 C22 C23 O6 3.34(18) . . . . ? N4 C22 C24 N2 -54.05(19) . . . . ? N4 C22 C25 C26 -26.4(2) . . . . ? N4 C22 C25 C30 158.35(17) . . . . ? C8 C9 C10 O5 110.78(18) . . . . ? C8 C9 C11 C12 54.4(2) . . . . ? C8 C9 C11 C16 -126.75(19) . . . . ? C9 N3 C17 O5 -2.6(2) . . . . ? C9 N3 C17 C18 178.12(19) . . . . ? C9 C8 N1A S1A 148.5(3) . . . . ? C9 C8 N1B S1B 150.6(5) . . . . ? C9 C11 C12 C13 -179.95(18) . . . . ? C9 C11 C16 C15 -179.62(18) . . . . ? C10 O5 C17 N3 -0.7(2) . . . . ? C10 O5 C17 C18 178.67(17) . . . . ? C10 C9 C11 C12 -70.2(2) . . . . ? C10 C9 C11 C16 108.7(2) . . . . ? C11 C9 C10 O5 -126.10(17) . . . . ? C11 C12 C13 C14 -0.7(3) . . . . ? C12 C11 C16 C15 -0.8(3) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? C13 C14 C15 C16 0.6(3) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? C16 C11 C12 C13 1.2(3) . . . . ? C17 O5 C10 C9 3.5(2) . . . . ? C17 N3 C9 C8 -114.14(18) . . . . ? C17 N3 C9 C10 4.4(2) . . . . ? C17 N3 C9 C11 125.15(17) . . . . ? C17 C18 C19 C20 -55.8(3) . . . . ? C18 C19 C20 C21 -52.6(3) . . . . ? C19 C20 C21 O6 -51.7(2) . . . . ? C19 C20 C21 N4 126.6(2) . . . . ? C21 O6 C23 C22 -2.37(19) . . . . ? C21 N4 C22 C23 -3.21(19) . . . . ? C21 N4 C22 C24 114.96(16) . . . . ? C21 N4 C22 C25 -127.12(16) . . . . ? C22 N4 C21 O6 2.0(2) . . . . ? C22 N4 C21 C20 -176.25(18) . . . . ? C22 C25 C26 C27 -176.17(19) . . . . ? C22 C25 C30 C29 176.38(19) . . . . ? C23 O6 C21 N4 0.4(2) . . . . ? C23 O6 C21 C20 178.77(16) . . . . ? C23 C22 C24 N2 58.9(2) . . . . ? C23 C22 C25 C26 -143.49(18) . . . . ? C23 C22 C25 C30 41.2(2) . . . . ? C24 N2 S2A C31 -66.21(18) . . . . ? C24 N2 S2A O3A -178.1(2) . . . . ? C24 N2 S2A O4A 52.2(3) . . . . ? C24 N2 S2B C31 -46.2(3) . . . . ? C24 N2 S2B O3B -167.1(4) . . . . ? C24 N2 S2B O4B 62.4(6) . . . . ? C24 C22 C23 O6 -112.51(16) . . . . ? C24 C22 C25 C26 91.9(2) . . . . ? C24 C22 C25 C30 -83.4(2) . . . . ? C25 C22 C23 O6 124.90(16) . . . . ? C25 C22 C24 N2 -174.39(15) . . . . ? C25 C26 C27 C28 0.2(4) . . . . ? C26 C25 C30 C29 1.0(3) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? C27 C28 C29 C30 0.0(4) . . . . ? C28 C29 C30 C25 -0.6(4) . . . . ? C30 C25 C26 C27 -0.8(3) . . . . ? C31 C32 C33 C34 1.5(3) . . . . ? C32 C31 C36 C35 -0.6(3) . . . . ? C32 C31 S2A N2 109.76(18) . . . . ? C32 C31 S2A O3A -139.2(2) . . . . ? C32 C31 S2A O4A -10.3(3) . . . . ? C32 C31 S2B N2 95.5(3) . . . . ? C32 C31 S2B O3B -146.3(4) . . . . ? C32 C31 S2B O4B -13.9(6) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? C32 C33 C34 C37 179.2(2) . . . . ? C33 C34 C35 C36 -0.5(3) . . . . ? C34 C35 C36 C31 1.3(3) . . . . ? C36 C31 C32 C33 -0.8(3) . . . . ? C36 C31 S2A N2 -67.5(2) . . . . ? C36 C31 S2A O3A 43.5(3) . . . . ? C36 C31 S2A O4A 172.4(3) . . . . ? C36 C31 S2B N2 -84.6(2) . . . . ? C36 C31 S2B O3B 33.7(5) . . . . ? C36 C31 S2B O4B 166.0(4) . . . . ? C37 C34 C35 C36 179.4(2) . . . . ? S1A C1A C2A C3A 174.3(5) . . . . ? S1A C1A C6A C5A -173.6(5) . . . . ? S2A N2 C24 C22 -136.45(17) . . . . ? S2A C31 C32 C33 -178.10(19) . . . . ? S2A C31 C36 C35 176.53(19) . . . . ? O1A S1A N1A C8 176.0(3) . . . . ? O1A S1A C1A C2A 148.8(4) . . . . ? O1A S1A C1A C6A -38.5(4) . . . . ? O2A S1A N1A C8 -53.9(4) . . . . ? O2A S1A C1A C2A 17.3(4) . . . . ? O2A S1A C1A C6A -170.0(4) . . . . ? N1A C8 C9 N3 66.6(2) . . . . ? N1A C8 C9 C10 -46.2(3) . . . . ? N1A C8 C9 C11 -170.6(2) . . . . ? N1A S1A C1A C2A -96.9(4) . . . . ? N1A S1A C1A C6A 75.8(4) . . . . ? C1A S1A N1A C8 60.8(4) . . . . ? C1A C2A C3A C4A -1.2(6) . . . . ? C2A C1A C6A C5A -1.0(6) . . . . ? C2A C3A C4A C5A 0.2(6) . . . . ? C2A C3A C4A C7A 179.5(12) . . . . ? C3A C4A C5A C6A 0.5(6) . . . . ? C4A C5A C6A C1A -0.1(6) . . . . ? C6A C1A C2A C3A 1.6(6) . . . . ? C7A C4A C5A C6A -178.8(12) . . . . ? S1B C1B C6B C5B -174.8(10) . . . . ? S1B C1B C2B C3B 174.7(10) . . . . ? S2B N2 C24 C22 -146.1(3) . . . . ? S2B C31 C32 C33 179.2(3) . . . . ? S2B C31 C36 C35 179.4(3) . . . . ? O1B S1B N1B C8 -179.7(6) . . . . ? O1B S1B C1B C6B -24.7(8) . . . . ? O1B S1B C1B C2B 160.5(7) . . . . ? O2B S1B N1B C8 -47.9(8) . . . . ? O2B S1B C1B C6B -158.2(7) . . . . ? O2B S1B C1B C2B 27.0(8) . . . . ? N1B C8 C9 N3 47.8(4) . . . . ? N1B C8 C9 C10 -65.0(4) . . . . ? N1B C8 C9 C11 170.6(3) . . . . ? N1B S1B C1B C6B 87.9(7) . . . . ? N1B S1B C1B C2B -86.9(8) . . . . ? C1B S1B N1B C8 65.4(7) . . . . ? C1B C6B C5B C4B 0.0 . . . . ? C6B C1B C2B C3B 0.0 . . . . ? C6B C5B C4B C3B 0.0 . . . . ? C6B C5B C4B C7B 177(2) . . . . ? C5B C4B C3B C2B 0.0 . . . . ? C4B C3B C2B C1B 0.0 . . . . ? C2B C1B C6B C5B 0.0 . . . . ? C7B C4B C3B C2B -177(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.9863(3) ref 1 0 0 0 1 0 0 0 1 2 0.0137(3) mt_II -1 0 0 0 -1 0 0.5 0 1