#------------------------------------------------------------------------------ #$Date: 2025-01-16 01:15:09 +0200 (Thu, 16 Jan 2025) $ #$Revision: 297334 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573690.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_1573690 loop_ _publ_author_name 'Seo, Seung Mo' 'Kim, Dongwook' 'Kim, Taewan' 'Han, Sunkyu' _publ_section_title ; Total synthesis of (-)-flueggenine A and (-)-15'-epi-flueggenine D. ; _journal_issue 3 _journal_name_full 'Chemical science' _journal_page_first 1216 _journal_page_last 1221 _journal_paper_doi 10.1039/d4sc07525k _journal_volume 16 _journal_year 2024 _chemical_formula_moiety 'C21 H34 I N O5 Si' _chemical_formula_sum 'C21 H34 I N O5 Si' _chemical_formula_weight 535.48 _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 direct _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2024-09-23 deposited with the CCDC. 2024-12-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9672(4) _cell_length_b 14.2728(6) _cell_length_c 19.4271(9) _cell_measurement_reflns_used 9936 _cell_measurement_temperature 2035(2) _cell_measurement_theta_max 27.54 _cell_measurement_theta_min 2.54 _cell_volume 2486.42(19) _computing_cell_refinement 'Bruker APEX4' _computing_data_collection 'Bruker APEX4' _computing_data_reduction 'Bruker APEX4' _computing_molecular_graphics ORTEP _computing_publication_material CIFTAB _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 2035(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'PHOTON II 14' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 34500 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.591 _diffrn_reflns_theta_min 2.536 _diffrn_source 'I\/Y\`iS 3.0 Microfocus' _exptl_absorpt_coefficient_mu 1.365 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.430 _exptl_crystal_description block _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.269 _exptl_crystal_size_min 0.117 _refine_diff_density_max 0.178 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details ; Flack x determined using 1980 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.020(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 5717 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0256 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.0427P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.0569 _reflns_Friedel_coverage 0.773 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 5072 _reflns_number_total 5717 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07525k2.cif _cod_data_source_block A23255O_019 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 1573690 _shelx_shelxl_version_number 2019/3 _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. ; _shelx_estimated_absorpt_t_min 0.699 _shelx_estimated_absorpt_t_max 0.857 _shelx_res_file ; TITL A23255O_019 in P2(1)2(1)2(1) A23255O_019.res created by SHELXL-2019/3 at 12:40:00 on 16-Aug-2023 CELL 0.71073 8.96720 14.27280 19.42710 90.0000 90.0000 90.0000 ZERR 4.00 0.00040 0.00060 0.00090 0.0000 0.0000 0.0000 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 SI I UNIT 84 136 4 20 4 4 OMIT 0 0 6 TEMP 1761.850 SIZE 0.117 0.269 0.283 L.S. 7 BOND $H ACTA LIST 4 MERG 2 CONF FMAP 2 PLAN 5 WGHT 0.023800 0.042700 FVAR 0.14954 0.65547 O1 4 0.733949 0.675159 0.677074 11.00000 0.07235 0.03994 = 0.05690 -0.00088 -0.03060 -0.00160 C2 1 0.640436 0.690410 0.633742 11.00000 0.04264 0.03434 = 0.02730 0.00005 -0.00045 -0.00079 C3 1 0.591226 0.786722 0.615837 11.00000 0.04818 0.02925 = 0.03093 -0.00193 0.00345 -0.00233 I4 6 0.684957 0.895013 0.674526 11.00000 0.08362 0.03658 = 0.04634 -0.00989 -0.00479 -0.00515 C5 1 0.494614 0.804901 0.565763 11.00000 0.04916 0.02872 = 0.03430 0.00706 0.00547 0.00252 AFIX 43 H5 2 0.467036 0.866666 0.557367 11.00000 -1.20000 AFIX 0 C6 1 0.428895 0.728454 0.522445 11.00000 0.04275 0.03642 = 0.02870 0.00974 -0.00064 0.00164 AFIX 13 H6 2 0.420877 0.751568 0.475089 11.00000 -1.20000 AFIX 0 C7 1 0.526310 0.641346 0.521886 11.00000 0.03815 0.03308 = 0.02829 0.00038 0.00194 -0.00043 AFIX 23 H7A 2 0.475497 0.591381 0.497485 11.00000 -1.20000 H7B 2 0.618813 0.654640 0.497916 11.00000 -1.20000 AFIX 0 C8 1 0.560193 0.610124 0.594925 11.00000 0.03015 0.03081 = 0.02526 0.00295 0.00204 0.00163 O9 4 0.423414 0.594118 0.631993 11.00000 0.03019 0.03734 = 0.03085 0.00978 0.00397 0.00643 O10 4 0.280874 0.708241 0.547002 11.00000 0.03872 0.04163 = 0.04036 0.01237 -0.00299 0.00565 SI11 5 0.259840 0.643096 0.616791 11.00000 0.03554 0.04293 = 0.03688 0.01110 0.00480 0.01153 PART 1 C12 1 0.225904 0.726751 0.693717 21.00000 0.04132 0.03677 = 0.04378 -0.00426 0.00850 0.00131 AFIX 13 H12 2 0.305103 0.773999 0.691880 21.00000 -1.20000 AFIX 0 C13 1 0.248106 0.673176 0.760601 21.00000 0.06116 0.06592 = 0.03338 0.00006 0.00203 0.00467 AFIX 137 H13A 2 0.235104 0.714953 0.798862 21.00000 -1.50000 H13B 2 0.346911 0.647327 0.761716 21.00000 -1.50000 H13C 2 0.176317 0.623430 0.763448 21.00000 -1.50000 AFIX 0 C14 1 0.081029 0.778855 0.686260 21.00000 0.05903 0.05920 = 0.06479 -0.01026 0.00291 0.01941 AFIX 137 H14A 2 0.072182 0.824116 0.722585 21.00000 -1.50000 H14B 2 -0.000497 0.735403 0.688846 21.00000 -1.50000 H14C 2 0.078924 0.810306 0.642591 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C12B 1 0.172158 0.695136 0.690429 -21.00000 0.03735 0.02109 = 0.04863 -0.00298 0.00197 -0.01062 AFIX 13 H12B 2 0.069581 0.672167 0.694691 -21.00000 -1.20000 AFIX 0 C13B 1 0.253547 0.688888 0.762319 -21.00000 0.07813 0.08445 = 0.10677 -0.00928 -0.03438 0.01987 AFIX 137 H13D 2 0.198239 0.723891 0.795917 -21.00000 -1.50000 H13E 2 0.352209 0.714428 0.758334 -21.00000 -1.50000 H13F 2 0.259698 0.624545 0.776433 -21.00000 -1.50000 AFIX 0 C14B 1 0.171957 0.804666 0.682114 -21.00000 0.07912 0.04336 = 0.05002 -0.00963 0.00484 0.00391 AFIX 137 H14D 2 0.125699 0.832729 0.721622 -21.00000 -1.50000 H14E 2 0.117314 0.821447 0.641447 -21.00000 -1.50000 H14F 2 0.272734 0.826727 0.678193 -21.00000 -1.50000 AFIX 0 PART 0 C15 1 0.119109 0.552346 0.594903 11.00000 0.03054 0.06209 = 0.06813 0.02556 -0.00114 0.00361 AFIX 13 H15 2 0.029005 0.585888 0.580491 11.00000 -1.20000 AFIX 0 C16 1 0.167643 0.492254 0.533450 11.00000 0.05721 0.06547 = 0.06042 0.01310 -0.01573 -0.01285 AFIX 137 H16A 2 0.089327 0.449203 0.521843 11.00000 -1.50000 H16B 2 0.256025 0.457899 0.545303 11.00000 -1.50000 H16C 2 0.187967 0.532033 0.494722 11.00000 -1.50000 AFIX 0 C17 1 0.073758 0.490011 0.655799 11.00000 0.04411 0.07627 = 0.08309 0.02968 0.01066 -0.00213 AFIX 137 H17A 2 0.004868 0.443049 0.640295 11.00000 -1.50000 H17B 2 0.027275 0.527729 0.690637 11.00000 -1.50000 H17C 2 0.160768 0.460273 0.674548 11.00000 -1.50000 AFIX 0 C18 1 0.659439 0.521656 0.600054 11.00000 0.03056 0.03020 = 0.03397 -0.00044 -0.00152 -0.00120 H18 2 0.768174 0.545528 0.594056 11.00000 -1.50000 C19 1 0.639752 0.466353 0.667012 11.00000 0.03719 0.03674 = 0.03763 0.00550 -0.00365 0.00561 AFIX 23 H19A 2 0.733574 0.439008 0.681639 11.00000 -1.20000 H19B 2 0.602238 0.506392 0.703452 11.00000 -1.20000 AFIX 0 C20 1 0.526450 0.389984 0.649004 11.00000 0.04477 0.03617 = 0.03695 0.01013 0.00407 0.00262 AFIX 23 H20A 2 0.537349 0.336314 0.679220 11.00000 -1.20000 H20B 2 0.425297 0.413565 0.652595 11.00000 -1.20000 AFIX 0 C21 1 0.563436 0.364101 0.575306 11.00000 0.04485 0.02989 = 0.04130 0.00354 0.00613 -0.00382 AFIX 23 H21A 2 0.635859 0.313672 0.573606 11.00000 -1.20000 H21B 2 0.474648 0.345209 0.550391 11.00000 -1.20000 AFIX 0 N22 3 0.625922 0.451318 0.546808 11.00000 0.03745 0.02633 = 0.03508 0.00175 0.00613 -0.00214 C23 1 0.700505 0.453141 0.486190 11.00000 0.04010 0.02889 = 0.03970 -0.00040 0.00865 0.00259 O24 4 0.779593 0.517649 0.467201 11.00000 0.05161 0.03652 = 0.04867 0.00022 0.02040 -0.00474 O25 4 0.673575 0.374510 0.450246 11.00000 0.06368 0.03268 = 0.03534 -0.00347 0.01416 -0.00367 C26 1 0.717962 0.366848 0.377210 11.00000 0.06475 0.04053 = 0.03938 -0.00211 0.01365 0.01048 C27 1 0.641574 0.442864 0.335854 11.00000 0.10339 0.06019 = 0.04614 0.00709 -0.00050 0.01757 AFIX 137 H27A 2 0.660933 0.433349 0.287759 11.00000 -1.50000 H27B 2 0.679305 0.502965 0.349596 11.00000 -1.50000 H27C 2 0.536043 0.440481 0.343982 11.00000 -1.50000 AFIX 0 C28 1 0.886912 0.369713 0.370586 11.00000 0.06640 0.06237 = 0.07629 -0.01037 0.03210 0.01299 AFIX 137 H28A 2 0.915160 0.350806 0.324991 11.00000 -1.50000 H28B 2 0.930610 0.327838 0.403579 11.00000 -1.50000 H28C 2 0.921599 0.432305 0.379007 11.00000 -1.50000 AFIX 0 C29 1 0.659600 0.270528 0.358798 11.00000 0.09404 0.05255 = 0.04578 -0.01444 0.00661 -0.00157 AFIX 137 H29A 2 0.682356 0.257138 0.311525 11.00000 -1.50000 H29B 2 0.553533 0.268872 0.365391 11.00000 -1.50000 H29C 2 0.705901 0.224493 0.387803 11.00000 -1.50000 AFIX 0 HKLF 4 REM A23255O_019 in P2(1)2(1)2(1) REM wR2 = 0.0569, GooF = S = 1.070, Restrained GooF = 1.070 for all data REM R1 = 0.0256 for 5072 Fo > 4sig(Fo) and 0.0333 for all 5717 data REM 302 parameters refined using 0 restraints END WGHT 0.0238 0.0427 REM Highest difference peak 0.178, deepest hole -0.476, 1-sigma level 0.053 Q1 1 0.0396 0.9035 0.7759 11.00000 0.05 0.18 Q2 1 0.0081 0.8992 0.7310 11.00000 0.05 0.17 Q3 1 0.7942 0.5714 0.4885 11.00000 0.05 0.16 Q4 1 0.0305 0.7020 0.6535 11.00000 0.05 0.16 Q5 1 0.6346 0.5016 0.7705 11.00000 0.05 0.16 ; _shelx_res_checksum 42410 _shelx_hkl_file ; 2 0 0 850.79 47.23 2 0 0 835.95 50.60 3 0 0 3.95 2.68 -3 0 0 0.97 0.16 3 0 0 1.60 1.44 -4 0 0 2.51 0.28 4 0 0 2.52 0.48 4 0 0 1.34 2.99 4 0 0 9.42 5.94 4 0 0 2.91 0.34 -4 0 0 2.51 0.52 -4 0 0 2.60 0.46 -5 0 0 0.00 0.25 5 0 0 2.57 5.51 5 0 0 -2.33 5.05 -5 0 0 0.18 0.16 -5 0 0 -0.05 0.16 5 0 0 0.10 0.17 5 0 0 -0.22 0.22 -5 0 0 0.33 0.34 -6 0 0 3.56 0.75 -6 0 0 2.95 0.37 6 0 0 2.59 0.63 6 0 0 2.87 0.42 -6 0 0 4.07 0.51 -6 0 0 2.73 0.66 -7 0 0 0.17 0.45 -7 0 0 0.08 0.20 -7 0 0 0.16 0.41 7 0 0 -0.29 1.15 7 0 0 0.92 1.01 7 0 0 0.06 0.42 -8 0 0 6.83 1.20 -8 0 0 9.93 0.91 -8 0 0 8.13 0.69 8 0 0 8.74 1.24 -9 0 0 -0.30 0.39 -9 0 0 -0.07 0.49 9 0 0 -0.46 0.49 -9 0 0 0.00 0.25 -10 0 0 1.32 0.73 -10 0 0 0.93 0.37 -11 0 0 -0.14 0.51 -1 -1 0 53.42 7.79 -1 1 0 38.30 6.06 -1 1 0 50.47 1.87 1 1 0 47.57 2.06 1 1 0 44.15 6.87 1 -1 0 49.27 1.88 -1 -1 0 48.73 1.91 1 -1 0 48.75 6.01 1 1 0 52.00 2.16 1 1 0 44.65 1.96 2 1 0 66.50 2.87 -2 -1 0 66.11 2.85 -2 1 0 65.38 10.10 -2 1 0 66.33 2.45 2 -1 0 69.03 2.73 -2 -1 0 66.34 2.65 -2 -1 0 68.38 2.85 2 -1 0 57.52 9.47 -2 1 0 68.58 2.78 2 1 0 69.16 2.69 2 1 0 59.44 10.28 2 -1 0 68.77 2.45 -2 -1 0 59.25 10.45 2 1 0 72.21 2.90 2 -1 0 68.51 2.76 3 1 0 57.50 12.05 3 1 0 59.99 2.48 3 1 0 59.83 13.09 -3 1 0 59.15 2.69 -3 1 0 57.78 2.65 3 1 0 58.02 2.74 -3 -1 0 59.45 2.72 3 1 0 57.66 2.73 -3 -1 0 61.82 2.78 -3 1 0 58.75 2.21 3 -1 0 67.71 12.34 3 -1 0 59.93 2.24 -3 -1 0 57.52 2.40 3 -1 0 58.67 2.60 3 -1 0 59.11 2.67 4 -1 0 54.96 13.65 4 1 0 43.40 2.29 4 -1 0 32.77 10.73 4 1 0 25.53 11.01 -4 1 0 40.61 2.23 4 1 0 43.43 1.96 -4 1 0 40.22 1.66 -4 -1 0 44.51 2.30 4 1 0 41.57 2.29 4 -1 0 40.68 1.70 4 1 0 26.52 10.54 -4 -1 0 41.97 2.27 4 -1 0 42.48 2.20 -4 1 0 41.99 2.24 -4 -1 0 41.50 1.85 5 -1 0 -4.63 4.65 -5 -1 0 0.13 0.16 -5 1 0 0.31 0.17 -5 1 0 0.20 0.27 -5 1 0 -0.14 0.26 5 -1 0 0.26 0.16 5 -1 0 -0.12 0.23 5 1 0 1.30 5.40 5 1 0 0.08 0.29 -5 -1 0 0.36 0.35 -5 1 0 0.23 0.13 5 -1 0 -1.05 2.78 5 1 0 -5.73 3.69 -5 -1 0 -0.03 0.27 6 1 0 1.08 1.02 6 -1 0 0.56 0.20 6 1 0 0.36 0.68 -6 1 0 0.37 0.18 6 -1 0 0.59 0.37 -6 1 0 0.28 0.40 -6 -1 0 0.59 0.34 -6 1 0 -0.16 0.32 6 -1 0 1.10 0.77 -6 -1 0 0.51 0.24 -6 -1 0 0.47 0.38 6 -1 0 -0.07 0.68 6 1 0 0.07 0.23 6 1 0 -0.21 0.29 -6 1 0 0.40 0.21 -6 -1 0 -0.01 0.37 -7 1 0 2.85 0.42 7 1 0 3.69 0.56 -7 -1 0 3.44 0.80 -7 1 0 3.27 0.38 7 1 0 2.61 0.78 7 -1 0 1.07 1.16 -7 -1 0 3.19 0.59 -7 1 0 3.72 0.86 -7 1 0 3.84 0.84 7 -1 0 2.08 0.69 -8 1 0 2.95 0.43 -8 1 0 1.39 0.81 8 1 0 2.89 0.81 -8 1 0 2.56 0.35 -8 -1 0 2.52 0.45 -8 -1 0 1.80 0.81 8 -1 0 1.68 0.67 9 1 0 9.99 1.38 -9 -1 0 9.83 1.39 -9 1 0 7.17 1.32 -9 1 0 9.00 0.64 -9 1 0 9.47 0.61 -9 -1 0 9.36 0.84 9 -1 0 5.30 1.24 -10 -1 0 1.16 0.44 10 1 0 1.73 0.96 -10 -1 0 0.82 0.71 -11 1 0 1.46 0.77 0 2 0 49.39 1.86 0 -2 0 50.52 1.85 0 2 0 46.37 5.86 0 -2 0 49.18 1.99 0 2 0 50.02 1.91 0 -2 0 48.97 1.87 0 2 0 52.27 2.02 0 -2 0 51.40 5.82 1 -2 0 159.37 5.61 1 2 0 165.91 14.79 1 -2 0 160.12 5.60 -1 2 0 151.24 5.64 1 2 0 156.03 5.85 -1 2 0 156.15 5.66 1 2 0 158.37 5.78 1 2 0 157.10 5.85 1 -2 0 156.79 5.69 -1 -2 0 163.31 5.75 -1 2 0 152.91 11.86 1 -2 0 150.71 5.65 -1 -2 0 156.20 5.83 1 -2 0 146.37 14.10 -1 -2 0 160.21 5.83 -1 2 0 150.92 5.67 -1 -2 0 147.14 13.97 -2 2 0 13.15 0.78 -2 2 0 6.63 3.43 2 -2 0 13.67 0.56 2 -2 0 14.04 0.69 -2 -2 0 14.70 0.92 2 -2 0 13.04 0.74 2 -2 0 14.41 4.25 -2 -2 0 13.15 0.78 2 -2 0 13.64 0.54 2 2 0 5.20 4.37 -2 2 0 13.30 0.76 2 2 0 13.16 0.90 -2 -2 0 10.13 5.12 2 2 0 13.74 0.83 2 2 0 13.77 0.90 -2 -2 0 14.66 0.88 -3 -2 0 522.08 42.26 3 2 0 529.03 18.65 3 2 0 489.97 18.34 3 2 0 455.80 40.25 3 -2 0 529.22 38.21 -3 2 0 536.90 38.49 3 -2 0 500.72 18.35 3 2 0 509.92 18.64 -3 -2 0 502.44 18.60 3 -2 0 497.01 18.25 -4 -2 0 75.56 3.21 4 -2 0 81.09 3.46 -4 -2 0 81.83 3.63 4 2 0 78.37 3.34 4 2 0 75.63 3.65 4 2 0 76.31 16.56 -4 2 0 76.41 3.51 4 2 0 74.68 3.64 -4 2 0 73.16 3.46 4 -2 0 71.55 15.66 -4 -2 0 77.26 3.62 -5 -2 0 206.97 7.86 5 2 0 217.86 8.04 5 2 0 202.36 8.49 -5 -2 0 220.66 8.59 -5 2 0 197.01 7.36 5 -2 0 205.31 28.73 5 2 0 139.34 25.40 5 2 0 217.78 33.29 5 -2 0 228.12 30.39 -5 2 0 210.74 8.34 -5 -2 0 204.76 8.41 -5 2 0 208.05 8.39 -5 2 0 197.86 7.37 5 -2 0 205.66 8.24 6 2 0 26.20 1.99 -6 2 0 27.05 1.90 -6 2 0 25.08 1.00 6 -2 0 23.73 1.73 -6 2 0 22.09 1.81 -6 -2 0 22.95 1.39 -6 2 0 23.80 0.99 7 2 0 -0.39 1.10 7 2 0 -0.22 1.22 -7 2 0 1.96 0.68 -7 2 0 2.64 0.73 7 -2 0 0.90 1.06 7 -2 0 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3.23 1 -4 0 83.51 3.20 -1 4 0 68.99 9.03 -1 -4 0 85.40 3.36 1 4 0 75.62 3.28 -1 4 0 77.44 3.09 1 -4 0 78.32 10.83 -1 -4 0 80.42 3.04 -1 4 0 79.07 3.02 2 4 0 92.98 14.88 -2 4 0 73.18 2.93 -2 -4 0 74.61 3.00 2 4 0 71.31 3.24 -2 -4 0 67.93 13.34 -2 -4 0 74.30 3.20 2 -4 0 72.81 2.86 -2 4 0 74.69 10.59 -2 -4 0 72.14 3.16 2 -4 0 73.47 2.95 2 -4 0 76.18 10.57 2 4 0 70.90 3.12 2 4 0 72.81 3.23 -2 4 0 73.08 2.92 -2 4 0 73.53 2.89 3 4 0 357.18 13.62 -3 -4 0 347.89 13.44 3 -4 0 358.91 12.90 3 -4 0 380.07 13.03 -3 -4 0 370.95 13.44 -3 -4 0 383.09 37.25 3 -4 0 352.97 12.98 -3 4 0 356.81 13.29 -3 4 0 296.15 36.60 3 4 0 366.42 34.78 3 -4 0 346.30 13.06 3 4 0 355.98 13.69 3 -4 0 354.22 30.12 -3 -4 0 393.93 13.71 3 4 0 371.44 13.58 -3 4 0 364.83 13.25 -4 -4 0 42.13 2.33 -4 -4 0 47.66 14.11 4 -4 0 50.71 12.15 -4 4 0 43.04 11.61 -4 4 0 44.69 2.28 -4 4 0 44.00 2.28 4 4 0 48.07 2.59 4 4 0 31.12 13.00 4 -4 0 47.27 2.15 -4 -4 0 48.36 2.32 -5 4 0 26.33 10.45 -5 -4 0 45.44 2.32 -5 4 0 43.60 2.44 5 -4 0 39.48 13.57 5 -4 0 43.94 2.23 5 4 0 44.59 2.73 5 4 0 52.58 16.10 -5 -4 0 42.40 2.48 -6 -4 0 7.51 1.02 -6 4 0 5.89 0.90 6 4 0 7.11 1.09 6 -4 0 7.24 0.83 -6 -4 0 6.73 0.78 -6 4 0 8.65 1.06 -7 -4 0 0.24 0.45 7 -4 0 1.35 0.50 -7 4 0 1.09 0.49 -7 4 0 0.61 0.49 7 4 0 1.07 0.63 -7 -4 0 0.11 0.33 8 4 0 8.05 1.27 -8 -4 0 7.06 0.89 -8 -4 0 7.62 1.18 -8 4 0 6.32 1.15 -8 4 0 6.84 1.22 -9 4 0 6.90 1.37 -9 -4 0 2.18 0.61 -9 -4 0 3.45 0.94 9 -4 0 1.70 0.85 9 4 0 3.63 0.99 -10 -4 0 -0.09 0.59 -10 -4 0 0.19 0.40 -10 4 0 0.03 0.47 10 4 0 0.14 0.73 -11 -4 0 0.94 0.62 -11 4 0 1.63 0.79 -11 -4 0 1.23 0.89 0 5 0 0.11 0.13 0 5 0 -2.95 1.77 0 -5 0 0.07 0.06 0 -5 0 0.11 0.11 0 -5 0 0.43 1.77 0 5 0 -0.02 0.07 0 5 0 -0.01 0.10 -1 -5 0 359.14 13.37 1 5 0 371.47 29.42 -1 -5 0 397.06 30.84 -1 -5 0 371.25 13.60 1 -5 0 377.72 13.58 -1 5 0 360.02 13.30 -1 5 0 366.85 26.67 -1 5 0 344.32 13.46 1 5 0 355.59 13.66 1 5 0 382.85 13.57 1 -5 0 388.67 28.45 2 -5 0 94.87 3.81 2 5 0 95.87 3.91 2 -5 0 77.64 11.96 -2 5 0 92.11 12.47 -2 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138.89 21.94 3 -6 0 105.04 15.81 -3 6 0 106.41 4.35 3 6 0 111.54 19.68 3 6 0 114.46 4.83 -4 -6 0 40.31 2.10 -4 -6 0 29.59 12.91 -4 -6 0 36.08 2.13 4 6 0 38.36 2.45 4 6 0 45.58 14.45 -4 6 0 39.99 2.03 -4 6 0 61.24 12.80 4 -6 0 39.13 1.75 -4 6 0 40.19 2.06 4 -6 0 40.56 11.40 4 -6 0 37.57 1.60 4 6 0 37.26 2.36 5 6 0 83.83 4.38 5 6 0 81.15 4.31 -5 -6 0 79.64 3.88 -5 6 0 79.53 3.82 -5 -6 0 88.26 3.95 -5 6 0 87.87 3.93 -6 -6 0 19.44 1.59 -6 6 0 16.66 1.75 6 6 0 18.17 1.84 -6 -6 0 19.59 1.48 -7 6 0 5.91 0.96 -7 -6 0 5.50 0.91 -7 -6 0 5.16 0.82 -7 6 0 5.73 0.97 7 6 0 6.94 1.20 -8 -6 0 22.99 2.00 8 6 0 21.48 2.23 -8 6 0 27.82 2.17 -8 6 0 23.58 2.10 -8 -6 0 21.30 1.74 9 6 0 10.21 1.59 -9 -6 0 8.39 1.07 -9 -6 0 8.11 1.25 -9 6 0 6.23 1.25 10 6 0 1.53 0.84 -10 -6 0 3.23 0.75 -10 -6 0 0.51 0.69 -10 6 0 1.33 0.77 -11 -6 0 0.52 0.66 -11 6 0 2.03 0.88 -11 -6 0 1.38 0.69 0 -7 0 -0.01 0.17 0 7 0 0.21 0.13 0 7 0 3.61 2.98 0 -7 0 -3.49 2.91 -1 7 0 23.84 1.50 1 -7 0 16.46 7.09 1 -7 0 24.50 1.58 -1 7 0 23.19 1.15 1 7 0 22.52 8.44 -1 -7 0 28.30 9.91 1 7 0 22.81 1.44 1 -7 0 21.62 1.36 -1 7 0 21.49 8.29 -1 -7 0 25.42 1.15 1 7 0 22.01 1.23 -2 7 0 106.72 4.70 2 7 0 110.08 18.86 2 7 0 118.53 5.03 2 -7 0 109.69 17.56 -2 7 0 123.43 15.47 -2 -7 0 115.96 4.94 2 -7 0 115.10 4.60 2 7 0 113.26 4.72 -2 -7 0 104.98 18.98 2 -7 0 113.59 4.82 -2 7 0 112.44 4.44 -2 -7 0 108.74 4.37 -2 7 0 117.10 4.58 3 7 0 12.83 1.12 -3 7 0 11.56 0.84 -3 7 0 7.29 8.01 3 -7 0 12.11 0.79 -3 7 0 10.98 0.81 -3 -7 0 10.54 0.80 3 -7 0 12.58 6.05 -3 -7 0 10.53 1.00 3 7 0 12.21 1.19 -3 -7 0 12.01 7.53 -4 -7 0 193.01 31.51 -4 -7 0 182.05 7.21 -4 7 0 184.59 7.21 4 -7 0 191.11 24.58 4 -7 0 183.21 7.01 4 7 0 189.34 7.82 4 7 0 176.65 7.84 4 -7 0 179.66 6.79 -4 7 0 192.57 24.83 4 7 0 168.65 28.65 -4 -7 0 187.55 7.53 -4 7 0 176.60 7.14 5 7 0 -0.06 0.40 -5 7 0 0.42 0.69 -5 -7 0 1.12 0.88 -5 7 0 0.14 0.29 -5 -7 0 -0.16 0.31 5 -7 0 0.56 0.13 -5 7 0 0.58 0.35 -5 -7 0 0.14 0.27 5 -7 0 -0.82 0.52 5 7 0 -0.09 0.75 5 7 0 0.27 0.46 5 -7 0 0.35 0.14 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3 -6 -23 1.78 0.98 0 -7 -23 8.30 1.70 0 7 -23 6.98 1.21 0 7 -23 11.23 1.98 0 -7 -23 6.73 1.41 1 7 -23 0.29 0.59 -1 -7 -23 -0.04 0.83 -1 -7 -23 -0.54 0.50 1 7 -23 0.81 0.94 1 -7 -23 -0.42 0.47 -1 7 -23 -0.43 0.77 1 -7 -23 1.31 0.79 -1 7 -23 0.70 0.55 2 7 -23 1.38 0.73 -2 -7 -23 2.91 0.94 -2 -7 -23 2.77 1.20 2 7 -23 0.97 0.73 -2 7 -23 1.25 0.61 2 -7 -23 1.26 0.92 -2 7 -23 1.71 1.01 2 -7 -23 1.06 0.89 0 0 -24 0.98 0.68 0 0 -24 1.27 0.95 -1 0 -24 15.93 2.34 -1 0 -24 14.53 1.77 1 0 -24 16.42 2.44 1 0 -24 16.19 1.99 2 0 -24 4.56 1.68 -2 0 -24 6.56 1.13 -2 0 -24 5.87 1.55 2 0 -24 7.35 1.83 -3 0 -24 3.29 0.90 3 0 -24 6.66 1.79 3 0 -24 3.05 1.08 -3 0 -24 7.20 1.69 0 1 -24 1.78 0.86 0 -1 -24 3.92 1.03 0 -1 -24 6.30 1.69 0 1 -24 3.65 1.44 1 1 -24 2.26 0.94 1 1 -24 1.24 1.16 -1 -1 -24 0.98 0.87 -1 -1 -24 2.51 0.87 -1 1 -24 2.91 0.98 -1 1 -24 1.46 0.75 1 -1 -24 3.27 1.37 1 -1 -24 1.24 0.90 2 1 -24 4.30 1.20 -2 -1 -24 2.64 1.38 -2 -1 -24 4.18 1.05 -2 1 -24 2.32 1.08 -2 1 -24 5.41 1.05 2 -1 -24 6.78 1.57 -3 -1 -24 5.54 1.09 -3 -1 -24 5.06 1.61 3 1 -24 3.95 1.41 3 1 -24 4.69 1.29 -3 1 -24 2.96 1.29 -3 1 -24 3.70 0.94 3 -1 -24 4.99 1.53 0 -2 -24 1.02 1.01 0 2 -24 3.26 1.00 0 2 -24 1.12 0.90 1 2 -24 0.87 0.66 -1 -2 -24 2.53 1.02 1 2 -24 1.51 1.13 -1 -2 -24 1.86 1.03 -1 2 -24 2.06 0.84 1 -2 -24 1.03 0.74 1 -2 -24 3.35 1.31 -1 2 -24 -0.46 0.82 -2 -2 -24 1.03 0.68 -2 -2 -24 2.93 1.48 2 2 -24 1.49 0.77 2 2 -24 0.78 0.79 2 -2 -24 0.57 0.50 -2 2 -24 1.18 0.99 2 -2 -24 2.44 0.97 -2 2 -24 1.66 0.77 -3 -2 -24 1.53 1.14 3 2 -24 0.73 0.86 -3 -2 -24 0.47 0.61 3 2 -24 0.96 0.72 3 -2 -24 1.40 0.81 -3 2 -24 1.83 1.00 3 -2 -24 0.27 0.84 -3 2 -24 1.33 0.61 0 3 -24 3.64 0.98 0 -3 -24 4.09 1.48 0 -3 -24 1.98 0.96 0 3 -24 3.42 1.29 1 3 -24 3.24 1.10 -1 -3 -24 5.09 1.33 1 3 -24 7.31 1.51 1 -3 -24 2.72 1.07 -1 3 -24 3.56 1.44 -1 3 -24 5.24 1.11 1 -3 -24 5.44 1.70 -2 -3 -24 0.61 0.62 2 3 -24 2.03 0.96 2 3 -24 2.07 1.05 -2 -3 -24 2.83 1.29 2 -3 -24 0.41 0.89 -2 3 -24 0.29 0.86 2 -3 -24 2.17 1.04 -2 3 -24 2.03 0.72 -3 -3 -24 3.54 0.91 3 3 -24 2.31 1.17 3 3 -24 2.48 1.03 -3 -3 -24 2.49 1.09 -3 3 -24 2.32 0.77 3 -3 -24 2.62 1.01 3 -3 -24 2.51 1.18 -3 3 -24 3.70 1.43 0 4 -24 1.62 0.86 0 -4 -24 1.57 0.86 0 -4 -24 1.12 0.91 0 4 -24 2.92 1.29 -1 -4 -24 6.95 1.38 1 4 -24 8.21 1.39 -1 -4 -24 6.32 1.85 1 4 -24 9.02 1.76 -1 4 -24 7.34 1.22 1 -4 -24 6.73 1.64 -1 4 -24 7.66 1.70 1 -4 -24 9.86 1.58 -2 -4 -24 5.44 1.12 2 4 -24 5.49 1.30 -2 -4 -24 3.72 1.41 2 4 -24 5.86 1.27 -2 4 -24 2.52 1.20 -2 4 -24 4.41 0.99 2 -4 -24 4.75 1.27 2 -4 -24 2.91 1.25 0 5 -24 18.93 1.98 0 -5 -24 17.24 2.50 0 5 -24 17.94 2.54 0 -5 -24 16.45 2.04 -1 -5 -24 1.18 0.81 1 5 -24 1.03 0.74 -1 -5 -24 0.54 0.94 1 5 -24 0.99 0.64 -1 5 -24 0.57 0.55 -1 5 -24 1.66 0.94 1 -5 -24 1.54 1.13 1 -5 -24 0.54 0.82 -2 -5 -24 9.27 1.86 0 0 -25 0.34 0.57 -1 0 -25 1.54 0.76 -1 0 -25 0.54 0.76 1 0 -25 2.64 1.24 1 0 -25 -0.58 0.65 0 1 -25 5.40 1.64 0 -1 -25 2.46 1.02 0 1 -25 3.01 0.98 0 -1 -25 2.70 1.28 1 1 -25 2.38 1.40 1 1 -25 2.52 1.02 -1 -1 -25 8.53 1.73 -1 -1 -25 4.14 1.04 1 -1 -25 5.02 1.47 1 -1 -25 4.44 1.22 -1 1 -25 5.52 1.43 -1 1 -25 3.45 1.05 0 -2 -25 0.48 0.85 0 2 -25 0.09 0.69 0 2 -25 0.10 0.80 0 -2 -25 1.09 0.80 1 2 -25 1.17 0.67 1 2 -25 1.77 1.04 -1 -2 -25 0.12 0.54 -1 -2 -25 1.39 0.88 -1 2 -25 0.23 0.57 1 -2 -25 -1.24 0.71 1 -2 -25 0.89 0.73 -1 2 -25 -0.88 0.50 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 51495 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 O1 O 0.7339(3) 0.67516(16) 0.67707(15) 0.0564(7) Uani 1 1 d . . . . . C2 C 0.6404(4) 0.6904(2) 0.63374(16) 0.0348(7) Uani 1 1 d . . . . . C3 C 0.5912(4) 0.7867(2) 0.61584(16) 0.0361(7) Uani 1 1 d . . . . . I4 I 0.68496(3) 0.89501(2) 0.67453(2) 0.05551(9) Uani 1 1 d . . . . . C5 C 0.4946(4) 0.8049(2) 0.56576(17) 0.0374(7) Uani 1 1 d . . . . . H5 H 0.467036 0.866666 0.557367 0.045 Uiso 1 1 calc R U . . . C6 C 0.4289(4) 0.7285(2) 0.52245(16) 0.0360(7) Uani 1 1 d . . . . . H6 H 0.420877 0.751568 0.475089 0.043 Uiso 1 1 calc R U . . . C7 C 0.5263(4) 0.6413(2) 0.52189(16) 0.0332(6) Uani 1 1 d . . . . . H7A H 0.475497 0.591381 0.497485 0.040 Uiso 1 1 calc R U . . . H7B H 0.618813 0.654640 0.497916 0.040 Uiso 1 1 calc R U . . . C8 C 0.5602(3) 0.6101(2) 0.59492(14) 0.0287(6) Uani 1 1 d . . . . . O9 O 0.4234(2) 0.59412(15) 0.63199(10) 0.0328(4) Uani 1 1 d . . . . . O10 O 0.2809(2) 0.70824(16) 0.54700(12) 0.0402(5) Uani 1 1 d . . . . . Si11 Si 0.25984(10) 0.64310(7) 0.61679(5) 0.0385(2) Uani 1 1 d . . . . . C12 C 0.2259(12) 0.7268(7) 0.6937(3) 0.0406(19) Uani 0.655(19) 1 d . . P A 1 H12 H 0.305103 0.773999 0.691880 0.049 Uiso 0.655(19) 1 calc R U P A 1 C13 C 0.248(2) 0.6732(18) 0.7606(7) 0.053(3) Uani 0.655(19) 1 d . . P A 1 H13A H 0.235104 0.714953 0.798862 0.080 Uiso 0.655(19) 1 calc R U P A 1 H13B H 0.346911 0.647327 0.761716 0.080 Uiso 0.655(19) 1 calc R U P A 1 H13C H 0.176317 0.623430 0.763448 0.080 Uiso 0.655(19) 1 calc R U P A 1 C14 C 0.0810(13) 0.7789(7) 0.6863(4) 0.061(3) Uani 0.655(19) 1 d . . P A 1 H14A H 0.072182 0.824116 0.722585 0.092 Uiso 0.655(19) 1 calc R U P A 1 H14B H -0.000497 0.735403 0.688846 0.092 Uiso 0.655(19) 1 calc R U P A 1 H14C H 0.078924 0.810306 0.642591 0.092 Uiso 0.655(19) 1 calc R U P A 1 C12B C 0.1722(19) 0.6951(10) 0.6904(6) 0.036(3) Uani 0.345(19) 1 d . . P A 2 H12B H 0.069581 0.672167 0.694691 0.043 Uiso 0.345(19) 1 calc R U P A 2 C13B C 0.254(5) 0.689(4) 0.762(2) 0.090(16) Uani 0.345(19) 1 d . . P A 2 H13D H 0.198239 0.723891 0.795917 0.135 Uiso 0.345(19) 1 calc R U P A 2 H13E H 0.352209 0.714428 0.758334 0.135 Uiso 0.345(19) 1 calc R U P A 2 H13F H 0.259698 0.624545 0.776433 0.135 Uiso 0.345(19) 1 calc R U P A 2 C14B C 0.172(3) 0.8047(9) 0.6821(7) 0.058(5) Uani 0.345(19) 1 d . . P A 2 H14D H 0.125699 0.832729 0.721622 0.086 Uiso 0.345(19) 1 calc R U P A 2 H14E H 0.117314 0.821447 0.641447 0.086 Uiso 0.345(19) 1 calc R U P A 2 H14F H 0.272734 0.826727 0.678193 0.086 Uiso 0.345(19) 1 calc R U P A 2 C15 C 0.1191(4) 0.5523(3) 0.5949(2) 0.0536(10) Uani 1 1 d . . . . . H15 H 0.029005 0.585888 0.580491 0.064 Uiso 1 1 calc R U . . . C16 C 0.1676(5) 0.4923(3) 0.5334(2) 0.0610(10) Uani 1 1 d . . . . . H16A H 0.089327 0.449203 0.521843 0.092 Uiso 1 1 calc R U . . . H16B H 0.256025 0.457899 0.545303 0.092 Uiso 1 1 calc R U . . . H16C H 0.187967 0.532033 0.494722 0.092 Uiso 1 1 calc R U . . . C17 C 0.0738(5) 0.4900(3) 0.6558(3) 0.0678(13) Uani 1 1 d . . . . . H17A H 0.004868 0.443049 0.640295 0.102 Uiso 1 1 calc R U . . . H17B H 0.027275 0.527729 0.690637 0.102 Uiso 1 1 calc R U . . . H17C H 0.160768 0.460273 0.674548 0.102 Uiso 1 1 calc R U . . . C18 C 0.6594(3) 0.5217(2) 0.60005(16) 0.0316(6) Uani 1 1 d . . . . . H18 H 0.768(4) 0.546(3) 0.594(2) 0.047 Uiso 1 1 d . U . . . C19 C 0.6398(3) 0.4664(2) 0.66701(18) 0.0372(7) Uani 1 1 d . . . . . H19A H 0.733574 0.439008 0.681639 0.045 Uiso 1 1 calc R U . . . H19B H 0.602238 0.506392 0.703452 0.045 Uiso 1 1 calc R U . . . C20 C 0.5264(4) 0.3900(2) 0.64900(16) 0.0393(7) Uani 1 1 d . . . . . H20A H 0.537349 0.336314 0.679220 0.047 Uiso 1 1 calc R U . . . H20B H 0.425297 0.413565 0.652595 0.047 Uiso 1 1 calc R U . . . C21 C 0.5634(4) 0.3641(2) 0.57531(17) 0.0387(7) Uani 1 1 d . . . . . H21A H 0.635859 0.313672 0.573606 0.046 Uiso 1 1 calc R U . . . H21B H 0.474648 0.345209 0.550391 0.046 Uiso 1 1 calc R U . . . N22 N 0.6259(3) 0.45132(17) 0.54681(13) 0.0330(6) Uani 1 1 d . . . . . C23 C 0.7005(4) 0.4531(2) 0.48619(16) 0.0362(7) Uani 1 1 d . . . . . O24 O 0.7796(3) 0.51765(15) 0.46720(13) 0.0456(6) Uani 1 1 d . . . . . O25 O 0.6736(3) 0.37451(14) 0.45025(11) 0.0439(5) Uani 1 1 d . . . . . C26 C 0.7180(5) 0.3668(2) 0.3772(2) 0.0482(9) Uani 1 1 d . . . . . C27 C 0.6416(6) 0.4429(3) 0.3359(2) 0.0699(13) Uani 1 1 d . . . . . H27A H 0.660933 0.433349 0.287759 0.105 Uiso 1 1 calc R U . . . H27B H 0.679305 0.502965 0.349596 0.105 Uiso 1 1 calc R U . . . H27C H 0.536043 0.440481 0.343982 0.105 Uiso 1 1 calc R U . . . C28 C 0.8869(5) 0.3697(3) 0.3706(3) 0.0684(13) Uani 1 1 d . . . . . H28A H 0.915160 0.350806 0.324991 0.103 Uiso 1 1 calc R U . . . H28B H 0.930610 0.327838 0.403579 0.103 Uiso 1 1 calc R U . . . H28C H 0.921599 0.432305 0.379007 0.103 Uiso 1 1 calc R U . . . C29 C 0.6596(6) 0.2705(3) 0.3588(2) 0.0641(12) Uani 1 1 d . . . . . H29A H 0.682356 0.257138 0.311525 0.096 Uiso 1 1 calc R U . . . H29B H 0.553533 0.268872 0.365391 0.096 Uiso 1 1 calc R U . . . H29C H 0.705901 0.224493 0.387803 0.096 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0723(17) 0.0399(12) 0.0569(16) -0.0009(12) -0.0306(15) -0.0016(11) C2 0.0426(19) 0.0343(15) 0.0273(16) 0.0001(12) -0.0004(13) -0.0008(13) C3 0.0482(19) 0.0293(14) 0.0309(16) -0.0019(12) 0.0034(14) -0.0023(13) I4 0.08362(18) 0.03658(11) 0.04634(13) -0.00989(10) -0.00479(13) -0.00515(12) C5 0.049(2) 0.0287(14) 0.0343(17) 0.0071(12) 0.0055(14) 0.0025(13) C6 0.0428(19) 0.0364(15) 0.0287(16) 0.0097(12) -0.0006(13) 0.0016(13) C7 0.0381(17) 0.0331(14) 0.0283(15) 0.0004(12) 0.0019(13) -0.0004(12) C8 0.0302(14) 0.0308(13) 0.0253(13) 0.0029(12) 0.0020(11) 0.0016(13) O9 0.0302(10) 0.0373(11) 0.0309(11) 0.0098(9) 0.0040(8) 0.0064(9) O10 0.0387(14) 0.0416(12) 0.0404(13) 0.0124(9) -0.0030(10) 0.0057(10) Si11 0.0355(5) 0.0429(5) 0.0369(5) 0.0111(4) 0.0048(4) 0.0115(4) C12 0.041(4) 0.037(4) 0.044(3) -0.004(3) 0.008(3) 0.001(3) C13 0.061(8) 0.066(7) 0.033(5) 0.000(4) 0.002(5) 0.005(5) C14 0.059(6) 0.059(4) 0.065(5) -0.010(4) 0.003(4) 0.019(4) C12B 0.037(7) 0.021(5) 0.049(6) -0.003(4) 0.002(5) -0.011(5) C13B 0.08(2) 0.08(2) 0.11(3) -0.009(15) -0.034(17) 0.020(15) C14B 0.079(13) 0.043(6) 0.050(7) -0.010(5) 0.005(9) 0.004(7) C15 0.0305(18) 0.062(2) 0.068(3) 0.026(2) -0.0011(17) 0.0036(17) C16 0.057(2) 0.065(2) 0.060(2) 0.0131(19) -0.016(2) -0.013(2) C17 0.044(2) 0.076(3) 0.083(3) 0.030(2) 0.011(2) -0.002(2) C18 0.0306(17) 0.0302(13) 0.0340(16) -0.0004(11) -0.0015(13) -0.0012(12) C19 0.0372(17) 0.0367(15) 0.0376(17) 0.0055(13) -0.0037(14) 0.0056(12) C20 0.0448(18) 0.0362(15) 0.0369(16) 0.0101(14) 0.0041(13) 0.0026(15) C21 0.0448(19) 0.0299(14) 0.0413(18) 0.0035(12) 0.0061(15) -0.0038(13) N22 0.0375(14) 0.0263(11) 0.0351(14) 0.0017(10) 0.0061(11) -0.0021(10) C23 0.0401(18) 0.0289(14) 0.0397(17) -0.0004(11) 0.0087(15) 0.0026(14) O24 0.0516(16) 0.0365(11) 0.0487(14) 0.0002(10) 0.0204(12) -0.0047(10) O25 0.0637(15) 0.0327(11) 0.0353(11) -0.0035(8) 0.0142(12) -0.0037(11) C26 0.065(3) 0.0405(18) 0.0394(18) -0.0021(14) 0.0137(17) 0.0105(16) C27 0.103(4) 0.060(2) 0.046(2) 0.0071(19) 0.000(2) 0.018(2) C28 0.066(3) 0.062(3) 0.076(3) -0.010(2) 0.032(2) 0.013(2) C29 0.094(3) 0.053(2) 0.046(2) -0.0144(17) 0.007(2) -0.002(2) 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 O1 C2 C3 122.4(3) . . ? O1 C2 C8 121.9(3) . . ? C3 C2 C8 115.6(3) . . ? C5 C3 C2 123.1(3) . . ? C5 C3 I4 121.0(2) . . ? C2 C3 I4 115.8(2) . . ? C3 C5 C6 121.7(3) . . ? C3 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? O10 C6 C5 108.8(3) . . ? O10 C6 C7 111.6(2) . . ? C5 C6 C7 111.9(3) . . ? O10 C6 H6 108.1 . . ? C5 C6 H6 108.1 . . ? C7 C6 H6 108.1 . . ? C8 C7 C6 110.4(3) . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O9 C8 C7 110.1(2) . . ? O9 C8 C18 109.1(2) . . ? C7 C8 C18 114.5(2) . . ? O9 C8 C2 105.6(2) . . ? C7 C8 C2 109.3(2) . . ? C18 C8 C2 107.8(2) . . ? C8 O9 Si11 126.85(17) . . ? C6 O10 Si11 119.29(18) . . ? O9 Si11 O10 106.45(11) . . ? O9 Si11 C12B 115.0(5) . . ? O10 Si11 C12B 118.1(4) . . ? O9 Si11 C15 110.44(15) . . ? O10 Si11 C15 106.36(16) . . ? C12B Si11 C15 100.0(6) . . ? O9 Si11 C12 105.2(3) . . ? O10 Si11 C12 107.7(3) . . ? C15 Si11 C12 120.0(4) . . ? C14 C12 C13 116.4(10) . . ? C14 C12 Si11 111.5(7) . . ? C13 C12 Si11 109.2(10) . . ? C14 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? Si11 C12 H12 106.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C14B C12B C13B 98(3) . . ? C14B C12B Si11 109.3(12) . . ? C13B C12B Si11 118.7(19) . . ? C14B C12B H12B 109.9 . . ? C13B C12B H12B 109.9 . . ? Si11 C12B H12B 109.9 . . ? C12B C13B H13D 109.5 . . ? C12B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C16 C15 C17 110.6(4) . . ? C16 C15 Si11 112.1(3) . . ? C17 C15 Si11 114.1(3) . . ? C16 C15 H15 106.6 . . ? C17 C15 H15 106.6 . . ? Si11 C15 H15 106.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N22 C18 C19 102.8(2) . . ? N22 C18 C8 113.2(2) . . ? C19 C18 C8 114.1(2) . . ? N22 C18 H18 110(2) . . ? C19 C18 H18 112(2) . . ? C8 C18 H18 105(2) . . ? C20 C19 C18 104.4(3) . . ? C20 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? C20 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C19 104.1(3) . . ? C21 C20 H20A 110.9 . . ? C19 C20 H20A 110.9 . . ? C21 C20 H20B 110.9 . . ? C19 C20 H20B 110.9 . . ? H20A C20 H20B 108.9 . . ? N22 C21 C20 103.4(2) . . ? N22 C21 H21A 111.1 . . ? C20 C21 H21A 111.1 . . ? N22 C21 H21B 111.1 . . ? C20 C21 H21B 111.1 . . ? H21A C21 H21B 109.0 . . ? C23 N22 C18 119.8(3) . . ? C23 N22 C21 122.1(2) . . ? C18 N22 C21 112.9(2) . . ? O24 C23 O25 125.3(3) . . ? O24 C23 N22 124.4(3) . . ? O25 C23 N22 110.3(3) . . ? C23 O25 C26 120.8(2) . . ? O25 C26 C29 101.6(3) . . ? O25 C26 C27 109.6(3) . . ? C29 C26 C27 111.7(4) . . ? O25 C26 C28 110.3(4) . . ? C29 C26 C28 110.4(3) . . ? C27 C26 C28 112.7(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.208(4) . ? C2 C3 1.485(4) . ? C2 C8 1.549(4) . ? C3 C5 1.328(5) . ? C3 I4 2.097(3) . ? C5 C6 1.499(5) . ? C5 H5 0.9300 . ? C6 O10 1.440(4) . ? C6 C7 1.520(4) . ? C6 H6 0.9800 . ? C7 C8 1.518(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O9 1.441(3) . ? C8 C18 1.548(4) . ? O9 Si11 1.651(2) . ? O10 Si11 1.655(2) . ? Si11 C12B 1.793(12) . ? Si11 C15 1.858(4) . ? Si11 C12 1.937(7) . ? C12 C14 1.504(12) . ? C12 C13 1.521(19) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C12B C14B 1.57(2) . ? C12B C13B 1.58(4) . ? C12B H12B 0.9800 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15 C16 1.533(6) . ? C15 C17 1.535(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N22 1.472(4) . ? C18 C19 1.532(4) . ? C18 H18 1.04(4) . ? C19 C20 1.531(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.515(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N22 1.473(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N22 C23 1.355(4) . ? C23 O24 1.219(4) . ? C23 O25 1.344(4) . ? O25 C26 1.478(4) . ? C26 C29 1.514(5) . ? C26 C27 1.514(6) . ? C26 C28 1.521(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C5 176.2(3) . . . . ? C8 C2 C3 C5 -5.8(5) . . . . ? O1 C2 C3 I4 -3.5(4) . . . . ? C8 C2 C3 I4 174.6(2) . . . . ? C2 C3 C5 C6 -0.9(5) . . . . ? I4 C3 C5 C6 178.8(2) . . . . ? C3 C5 C6 O10 100.7(4) . . . . ? C3 C5 C6 C7 -23.1(4) . . . . ? O10 C6 C7 C8 -69.0(3) . . . . ? C5 C6 C7 C8 53.3(3) . . . . ? C6 C7 C8 O9 56.7(3) . . . . ? C6 C7 C8 C18 -179.9(2) . . . . ? C6 C7 C8 C2 -58.9(3) . . . . ? O1 C2 C8 O9 95.0(3) . . . . ? C3 C2 C8 O9 -83.0(3) . . . . ? O1 C2 C8 C7 -146.5(3) . . . . ? C3 C2 C8 C7 35.4(4) . . . . ? O1 C2 C8 C18 -21.5(4) . . . . ? C3 C2 C8 C18 160.4(3) . . . . ? C7 C8 O9 Si11 -26.1(3) . . . . ? C18 C8 O9 Si11 -152.5(2) . . . . ? C2 C8 O9 Si11 91.9(3) . . . . ? C5 C6 O10 Si11 -78.6(3) . . . . ? C7 C6 O10 Si11 45.5(3) . . . . ? C8 O9 Si11 O10 4.1(3) . . . . ? C8 O9 Si11 C12B -128.7(6) . . . . ? C8 O9 Si11 C15 119.1(3) . . . . ? C8 O9 Si11 C12 -110.0(4) . . . . ? C6 O10 Si11 O9 -13.5(3) . . . . ? C6 O10 Si11 C12B 117.5(7) . . . . ? C6 O10 Si11 C15 -131.3(3) . . . . ? C6 O10 Si11 C12 98.9(4) . . . . ? O9 Si11 C12B C14B 110.6(14) . . . . ? O10 Si11 C12B C14B -16.4(18) . . . . ? C15 Si11 C12B C14B -131.2(15) . . . . ? O9 Si11 C12B C13B -1(3) . . . . ? O10 Si11 C12B C13B -128(3) . . . . ? C15 Si11 C12B C13B 117(3) . . . . ? O9 Si11 C15 C16 -56.4(3) . . . . ? O10 Si11 C15 C16 58.7(3) . . . . ? C12B Si11 C15 C16 -177.9(5) . . . . ? C12 Si11 C15 C16 -179.0(3) . . . . ? O9 Si11 C15 C17 70.2(3) . . . . ? O10 Si11 C15 C17 -174.7(3) . . . . ? C12B Si11 C15 C17 -51.4(5) . . . . ? C12 Si11 C15 C17 -52.4(4) . . . . ? O9 C8 C18 N22 86.1(3) . . . . ? C7 C8 C18 N22 -37.8(4) . . . . ? C2 C8 C18 N22 -159.7(2) . . . . ? O9 C8 C18 C19 -31.1(3) . . . . ? C7 C8 C18 C19 -155.0(3) . . . . ? C2 C8 C18 C19 83.2(3) . . . . ? N22 C18 C19 C20 -27.6(3) . . . . ? C8 C18 C19 C20 95.4(3) . . . . ? C18 C19 C20 C21 35.7(3) . . . . ? C19 C20 C21 N22 -29.0(3) . . . . ? C19 C18 N22 C23 -145.2(3) . . . . ? C8 C18 N22 C23 91.2(3) . . . . ? C19 C18 N22 C21 9.8(3) . . . . ? C8 C18 N22 C21 -113.8(3) . . . . ? C20 C21 N22 C23 166.5(3) . . . . ? C20 C21 N22 C18 12.1(3) . . . . ? C18 N22 C23 O24 -11.6(5) . . . . ? C21 N22 C23 O24 -164.3(3) . . . . ? C18 N22 C23 O25 168.9(3) . . . . ? C21 N22 C23 O25 16.3(4) . . . . ? O24 C23 O25 C26 -11.2(5) . . . . ? N22 C23 O25 C26 168.3(3) . . . . ? C23 O25 C26 C29 -177.5(3) . . . . ? C23 O25 C26 C27 -59.3(5) . . . . ? C23 O25 C26 C28 65.4(4) . . . . ?