#------------------------------------------------------------------------------ #$Date: 2024-01-06 10:21:30 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288816 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247573.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_7247573 loop_ _publ_author_name 'Zhou, Hai-Jie' 'Yao, Yi-Ping' 'Zhang, Tonghui' 'Chen, Biao' 'Wang, Xu' 'Zhao, Hang' 'Zeng, Jie' 'Chen, Jian-Ai' 'Xiao, Xiao' 'Chen, Fen-Er' _publ_section_title ; New conformationally flexible and recyclable aryl iodine catalysts from an inexpensive chiral source for asymmetric oxidations ; _journal_issue 24 _journal_name_full 'Green Chemistry' _journal_page_first 10447 _journal_page_last 10457 _journal_paper_doi 10.1039/D3GC02429F _journal_volume 25 _journal_year 2023 _chemical_absolute_configuration ad _chemical_formula_moiety 'C76 H81 I N4 O10 Si2' _chemical_formula_sum 'C76 H81 I N4 O10 Si2' _chemical_formula_weight 1393.52 _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_Hall 'P 2 2ab' _space_group_name_H-M_alt 'P 21 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-01-04 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-01-14 deposited with the CCDC. 2023-10-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.3936(3) _cell_length_b 27.4740(6) _cell_length_c 9.5840(2) _cell_measurement_reflns_used 9985 _cell_measurement_temperature 170.00 _cell_measurement_theta_max 27.46 _cell_measurement_theta_min 2.59 _cell_volume 3526.68(13) _computing_cell_refinement 'SAINT V8.40B (Bruker Nano, Inc., 2019)' _computing_data_collection 'Bruker Instrument Service vV6.2.14' _computing_data_reduction 'SAINT V8.40B (Bruker Nano, Inc., 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 170.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'zju Bruker D8 VENTURE' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 54725 _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 27.495 _diffrn_reflns_theta_min 2.124 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0868 before and 0.0619 after correction. The Ratio of minimum to maximum transmission is 0.9103. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.312 _exptl_crystal_description block _exptl_crystal_F_000 1452 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.434 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Flack x determined using 3146 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.014(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 470 _refine_ls_number_reflns 8123 _refine_ls_number_restraints 111 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0245 _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^)+(0.0255P)^2^+0.5841P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.0584 _reflns_Friedel_coverage 0.784 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 7539 _reflns_number_total 8123 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3gc02429f2.cif _cod_data_source_block mo_230104_zhj_mes _cod_depositor_comments 'Adding full bibliography for 7247573--7247574.cif.' _cod_database_code 7247573 _shelx_shelxl_version_number 2019/2 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.853 _shelx_estimated_absorpt_t_min 0.779 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Si1-C34 \\sim Si1-C34A with sigma of 0.02 C38-C36 \\sim C38A-C36A with sigma of 0.04 C39-C34 \\sim C39A-C34A with sigma of 0.02 C34-C38 \\sim C34A-C38A with sigma of 0.04 C39-C38 \\sim C39A-C38A with sigma of 0.02 C34-C35 \\sim C34A-C35A with sigma of 0.02 C38-C37 \\sim C38A-C37A with sigma of 0.02 C37-C35 \\sim C37A-C35A with sigma of 0.04 C37-C36 \\sim C37A-C36A with sigma of 0.02 C34-C36 \\sim C34A-C36A with sigma of 0.04 C35-C36 \\sim C35A-C36A with sigma of 0.02 Si1-C39 \\sim Si1-C39A with sigma of 0.04 Si1-C35 \\sim Si1-C35A with sigma of 0.04 C39-C37 \\sim C39A-C37A with sigma of 0.04 C39-C35 \\sim C39A-C35A with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Si1 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C34A \\sim C39A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A 4. Others Sof(C34A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=Sof(H38A)=Sof(C37A)=Sof(H37A)= Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=1-FVAR(1) Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)= Sof(H38)=Sof(C39)=Sof(H39)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C5(H5), C12(H12) 5.b Secondary CH2 refined with riding coordinates: C23(H23A,H23B) 5.c Aromatic/amide H refined with riding coordinates: N1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C16(H16), C18(H18), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C39A(H39A), C38A(H38A), C37A(H37A), C36A(H36A), C35A(H35A) 5.d Fitted hexagon refined as free rotating group: C34A(C39A,C38A,C37A,C36A,C35A) 5.e Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C25(H25A,H25B, H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C) ; _shelx_res_file ; TITL mo_230104_zhj_mes_a.res in P2(1)2(1)2 mo_230104_zhj_mes.res created by SHELXL-2019/2 at 14:08:35 on 04-Jan-2023 REM Old TITL mo_230104_ZHJ_Mes_0ma in P2(1)2(1)2 REM SHELXT solution in P2(1)2(1)2: R1 0.137, Rweak 0.025, Alpha 0.004 REM 1.993 for 23 systematic absences, Orientation as input REM Flack x = 0.018 ( 0.005 ) from 2882 Parsons' quotients REM Formula found by SHELXT: C70 I N10 O10 Si2 CELL 0.71073 13.3936 27.474 9.584 90 90 90 ZERR 2 0.0003 0.0006 0.0002 0 0 0 LATT -1 SYMM -X,-Y,+Z SYMM 0.5-X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H I N O Si UNIT 152 162 2 8 20 4 SADI Si1 C34 Si1 C34A SADI 0.04 C38 C36 C38A C36A SADI C39 C34 C39A C34A SADI 0.04 C34 C38 C34A C38A SADI C39 C38 C39A C38A SADI C34 C35 C34A C35A SADI C38 C37 C38A C37A SADI 0.04 C37 C35 C37A C35A SIMU 0.02 0.04 2 Si1 C34 > C39A SADI C37 C36 C37A C36A SADI 0.04 C34 C36 C34A C36A SADI C35 C36 C35A C36A SADI 0.04 Si1 C39 Si1 C39A SADI 0.04 Si1 C35 Si1 C35A SADI 0.04 C39 C37 C39A C37A SADI 0.04 C39 C35 C39A C35A L.S. 20 PLAN 6 SIZE 0.3 0.32 0.48 TEMP -103.15 CONF BOND list 4 fmap 2 53 MORE -1 HTAB BOND $H ACTA OMIT 1 1 1 OMIT 1 4 0 OMIT 4 4 0 REM REM REM WGHT 0.025500 0.584100 FVAR 0.33944 0.59242 I1 3 0.500000 0.500000 1.034289 10.50000 0.06143 0.02970 = 0.03023 0.00000 0.00000 0.00499 SI1 6 0.834002 0.408275 0.692080 11.00000 0.04631 0.02931 = 0.04648 -0.00325 0.00953 -0.00189 O1 5 0.517817 0.415049 0.825412 11.00000 0.04782 0.01801 = 0.03270 -0.00123 0.00210 0.00351 O2 5 0.616353 0.261654 1.046074 11.00000 0.08582 0.03837 = 0.03943 0.00764 0.01195 0.01073 O3 5 0.767806 0.366226 0.772132 11.00000 0.04147 0.03368 = 0.04054 -0.00754 0.00471 -0.00443 O4 5 0.232837 0.238891 0.433803 11.00000 0.09561 0.05893 = 0.05779 -0.00813 -0.02369 -0.02490 O5 5 0.148752 0.250829 0.622865 11.00000 0.06007 0.08087 = 0.09111 -0.01696 -0.00911 -0.02269 N1 4 0.629819 0.293936 0.829839 11.00000 0.04373 0.02284 = 0.03246 -0.00102 -0.00043 0.00395 AFIX 43 H1 2 0.636140 0.287190 0.740514 11.00000 -1.20000 AFIX 0 N2 4 0.222639 0.256342 0.551607 11.00000 0.06211 0.03864 = 0.06240 -0.00150 -0.02031 -0.00846 C1 1 0.500000 0.500000 0.816747 10.50000 0.03353 0.02665 = 0.02846 0.00000 0.00000 0.00233 C2 1 0.509420 0.456213 0.744777 11.00000 0.03589 0.02081 = 0.03363 0.00024 -0.00191 0.00130 C3 1 0.508520 0.456145 0.599538 11.00000 0.05087 0.02513 = 0.03493 -0.00409 -0.00043 0.00019 AFIX 43 H3 2 0.513678 0.426429 0.549371 11.00000 -1.20000 AFIX 0 C4 1 0.500000 0.500000 0.529092 10.50000 0.06201 0.03432 = 0.02913 0.00000 0.00000 0.00184 AFIX 43 H4 2 0.500001 0.499999 0.429969 10.50000 -1.20000 AFIX 0 C5 1 0.548477 0.370140 0.759394 11.00000 0.04214 0.01899 = 0.03268 -0.00203 0.00357 0.00321 AFIX 13 H5 2 0.592774 0.378006 0.678486 11.00000 -1.20000 AFIX 0 C6 1 0.460666 0.340842 0.707738 11.00000 0.04268 0.02042 = 0.03530 0.00036 -0.00260 0.00614 C7 1 0.466808 0.319200 0.576114 11.00000 0.05426 0.03039 = 0.03697 -0.00340 0.00052 -0.00035 AFIX 43 H7 2 0.524885 0.323783 0.520747 11.00000 -1.20000 AFIX 0 C8 1 0.388913 0.291129 0.525754 11.00000 0.06880 0.03107 = 0.03749 -0.00507 -0.00867 -0.00023 AFIX 43 H8 2 0.393220 0.276009 0.436814 11.00000 -1.20000 AFIX 0 C9 1 0.305535 0.285625 0.606865 11.00000 0.04905 0.02806 = 0.04816 -0.00080 -0.01431 -0.00145 C10 1 0.296895 0.305906 0.738641 11.00000 0.04027 0.03770 = 0.04881 -0.00127 -0.00326 0.00103 AFIX 43 H10 2 0.238788 0.300821 0.793587 11.00000 -1.20000 AFIX 0 C11 1 0.375541 0.333844 0.787993 11.00000 0.04364 0.03163 = 0.03847 -0.00338 -0.00102 0.00226 AFIX 43 H11 2 0.371142 0.348366 0.877741 11.00000 -1.20000 AFIX 0 C12 1 0.610370 0.344003 0.871491 11.00000 0.04003 0.02389 = 0.03029 -0.00235 0.00176 0.00121 AFIX 13 H12 2 0.571831 0.343832 0.960855 11.00000 -1.20000 AFIX 0 C13 1 0.638490 0.257493 0.923608 11.00000 0.03934 0.02807 = 0.03968 0.00262 -0.00325 -0.00097 C14 1 0.680592 0.211226 0.861867 11.00000 0.05002 0.02480 = 0.03736 0.00599 0.00034 0.00389 C15 1 0.616591 0.176123 0.805694 11.00000 0.05734 0.02936 = 0.04318 0.00094 -0.00079 0.00085 C16 1 0.658794 0.135180 0.744437 11.00000 0.07940 0.03225 = 0.05240 -0.00353 0.00134 0.00197 AFIX 43 H16 2 0.616221 0.111115 0.705364 11.00000 -1.20000 AFIX 0 C17 1 0.760973 0.128469 0.738735 11.00000 0.08996 0.03420 = 0.05501 0.00227 0.01312 0.01715 C18 1 0.822706 0.163140 0.797270 11.00000 0.05816 0.04036 = 0.06279 0.01645 0.01109 0.01725 AFIX 43 H18 2 0.892917 0.158250 0.796085 11.00000 -1.20000 AFIX 0 C19 1 0.784014 0.205158 0.858039 11.00000 0.04823 0.03474 = 0.04711 0.01081 0.00151 0.00665 C20 1 0.505865 0.183128 0.808172 11.00000 0.05649 0.04867 = 0.07098 -0.00821 -0.01038 -0.00805 AFIX 137 H20A 2 0.485483 0.194999 0.900294 11.00000 -1.50000 H20B 2 0.472769 0.152028 0.788970 11.00000 -1.50000 H20C 2 0.486791 0.206946 0.736875 11.00000 -1.50000 AFIX 0 C21 1 0.805883 0.084168 0.666568 11.00000 0.12642 0.04670 = 0.11198 -0.01388 0.03157 0.02854 AFIX 137 H21A 2 0.866510 0.074092 0.715995 11.00000 -1.50000 H21B 2 0.822606 0.092474 0.569909 11.00000 -1.50000 H21C 2 0.757419 0.057446 0.667382 11.00000 -1.50000 AFIX 0 C22 1 0.852726 0.244350 0.912582 11.00000 0.04701 0.04997 = 0.07819 0.00994 -0.00916 0.00027 AFIX 137 H22A 2 0.846478 0.273498 0.854291 11.00000 -1.50000 H22B 2 0.921838 0.232674 0.909929 11.00000 -1.50000 H22C 2 0.834461 0.252316 1.008929 11.00000 -1.50000 AFIX 0 C23 1 0.708940 0.370464 0.894997 11.00000 0.04439 0.03040 = 0.03225 -0.00342 0.00018 -0.00136 AFIX 23 H23A 2 0.696283 0.405208 0.915909 11.00000 -1.20000 H23B 2 0.744717 0.355921 0.975201 11.00000 -1.20000 AFIX 0 C24 1 0.965023 0.383900 0.677139 11.00000 0.04567 0.04507 = 0.08991 -0.00949 0.01602 -0.00296 C25 1 1.004951 0.367416 0.818023 11.00000 0.05193 0.06221 = 0.12951 -0.00285 -0.01842 -0.00074 AFIX 137 H25A 2 1.012395 0.395690 0.879490 11.00000 -1.50000 H25B 2 1.070011 0.351708 0.805311 11.00000 -1.50000 H25C 2 0.958170 0.344231 0.860026 11.00000 -1.50000 AFIX 0 C26 1 1.033786 0.422436 0.612569 11.00000 0.06503 0.07689 = 0.13157 -0.02051 0.04627 -0.02226 AFIX 137 H26A 2 1.008996 0.431244 0.519735 11.00000 -1.50000 H26B 2 1.101552 0.409280 0.604513 11.00000 -1.50000 H26C 2 1.034750 0.451410 0.672198 11.00000 -1.50000 AFIX 0 C27 1 0.961544 0.339463 0.579714 11.00000 0.05437 0.05789 = 0.13363 -0.03526 0.01472 0.00806 AFIX 137 H27A 2 0.915326 0.315200 0.617746 11.00000 -1.50000 H27B 2 1.028429 0.325238 0.572237 11.00000 -1.50000 H27C 2 0.938659 0.349631 0.487067 11.00000 -1.50000 AFIX 0 C28 1 0.820322 0.467698 0.787423 11.00000 0.04989 0.03846 = 0.05613 -0.01005 0.01694 -0.01197 C29 1 0.870297 0.477467 0.910680 11.00000 0.06950 0.05444 = 0.06148 -0.01060 0.00921 -0.01244 AFIX 43 H29 2 0.915737 0.454119 0.946918 11.00000 -1.20000 AFIX 0 C30 1 0.855206 0.520832 0.982427 11.00000 0.08079 0.08360 = 0.06825 -0.03166 0.02174 -0.03286 AFIX 43 H30 2 0.890792 0.526820 1.066437 11.00000 -1.20000 AFIX 0 C31 1 0.789840 0.554877 0.933479 11.00000 0.06150 0.06111 = 0.11653 -0.04795 0.04157 -0.02211 AFIX 43 H31 2 0.779447 0.584309 0.983442 11.00000 -1.20000 AFIX 0 C32 1 0.739561 0.546302 0.812254 11.00000 0.04829 0.04819 = 0.12633 -0.03410 0.02188 -0.00771 AFIX 43 H32 2 0.694579 0.570010 0.776830 11.00000 -1.20000 AFIX 0 C33 1 0.754028 0.502911 0.740407 11.00000 0.04684 0.03818 = 0.08852 -0.01541 0.01113 -0.00372 AFIX 43 H33 2 0.717592 0.497207 0.656948 11.00000 -1.20000 AFIX 0 PART 1 C34 1 0.769330 0.411864 0.511657 21.00000 0.04789 0.03041 = 0.04086 0.00315 0.01479 0.00602 C35 1 0.778398 0.451201 0.419164 21.00000 0.07403 0.03242 = 0.04702 0.00511 0.01265 0.00009 AFIX 43 H35 2 0.817041 0.478538 0.446878 21.00000 -1.20000 AFIX 0 C36 1 0.733413 0.451812 0.289371 21.00000 0.10716 0.04079 = 0.03979 0.01181 0.01201 0.01244 AFIX 43 H36 2 0.739859 0.479604 0.231085 21.00000 -1.20000 AFIX 0 C37 1 0.679382 0.412276 0.244536 21.00000 0.09119 0.04935 = 0.03144 0.00069 0.00026 0.02358 AFIX 43 H37 2 0.647977 0.412914 0.155677 21.00000 -1.20000 AFIX 0 C38 1 0.670624 0.371562 0.328487 21.00000 0.06566 0.03902 = 0.03615 -0.00347 0.00096 0.00939 AFIX 43 H38 2 0.634116 0.343962 0.297467 21.00000 -1.20000 AFIX 0 C39 1 0.716263 0.371608 0.459640 21.00000 0.05637 0.03304 = 0.03123 0.00412 0.00757 0.00469 AFIX 43 H39 2 0.711219 0.343263 0.515973 21.00000 -1.20000 AFIX 66 PART 2 C34A 1 0.800521 0.416964 0.513352 -21.00000 0.06893 0.03753 = 0.05558 -0.00304 0.01004 0.00413 C39A 1 0.740004 0.382628 0.448596 -21.00000 0.07321 0.05206 = 0.04636 -0.00016 -0.00281 0.01281 AFIX 43 H39A 2 0.717427 0.355002 0.499177 -21.00000 -1.20000 AFIX 65 C38A 1 0.712520 0.388711 0.309833 -21.00000 0.10658 0.06730 = 0.05418 -0.01250 -0.01919 -0.00133 AFIX 43 H38A 2 0.671159 0.365244 0.265576 -21.00000 -1.20000 AFIX 65 C37A 1 0.745553 0.429132 0.235825 -21.00000 0.19875 0.09893 = 0.04996 0.00138 -0.04242 -0.02061 AFIX 43 H37A 2 0.726769 0.433290 0.140987 -21.00000 -1.20000 AFIX 65 C36A 1 0.806070 0.463469 0.300579 -21.00000 0.24477 0.07460 = 0.06668 0.00496 -0.03101 -0.01978 AFIX 43 H36A 2 0.828647 0.491094 0.249997 -21.00000 -1.20000 AFIX 65 C35A 1 0.833555 0.457386 0.439342 -21.00000 0.17970 0.04849 = 0.04847 0.00600 -0.02046 -0.02419 AFIX 43 H35A 2 0.874916 0.480853 0.483598 -21.00000 -1.20000 AFIX 0 HKLF 4 REM mo_230104_zhj_mes_a.res in P2(1)2(1)2 REM wR2 = 0.0584, GooF = S = 1.046, Restrained GooF = 1.047 for all data REM R1 = 0.0245 for 7539 Fo > 4sig(Fo) and 0.0285 for all 8123 data REM 470 parameters refined using 111 restraints END WGHT 0.0255 0.5842 REM Instructions for potential hydrogen bonds EQIV $2 x+1/2, -y+1/2, -z+1 HTAB N1 O4_$2 REM Highest difference peak 0.434, deepest hole -0.268, 1-sigma level 0.036 Q1 1 0.5000 0.5000 0.9101 10.50000 0.05 0.43 Q2 1 0.5017 0.4571 0.6771 11.00000 0.05 0.21 Q3 1 0.6739 0.2930 0.7571 11.00000 0.05 0.21 Q4 1 0.3365 0.2983 0.5391 11.00000 0.05 0.18 Q5 1 0.5000 0.5000 1.1436 10.50000 0.05 0.18 Q6 1 0.5274 0.4210 0.3896 11.00000 0.05 0.18 ; _shelx_res_checksum 46767 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' '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 I1 I 0.500000 0.500000 1.03429(2) 0.04045(7) Uani 1 2 d S T P . . Si1 Si 0.83400(6) 0.40827(3) 0.69208(8) 0.04070(17) Uani 1 1 d D U . . . O1 O 0.51782(13) 0.41505(5) 0.82541(16) 0.0328(4) Uani 1 1 d . . . . . O2 O 0.61635(18) 0.26165(7) 1.0461(2) 0.0545(5) Uani 1 1 d . . . . . O3 O 0.76781(13) 0.36623(6) 0.77213(19) 0.0386(4) Uani 1 1 d . . . . . O4 O 0.2328(2) 0.23889(9) 0.4338(3) 0.0708(7) Uani 1 1 d . . . . . O5 O 0.1488(2) 0.25083(10) 0.6229(3) 0.0773(8) Uani 1 1 d . . . . . N1 N 0.62982(15) 0.29394(7) 0.8298(2) 0.0330(4) Uani 1 1 d . . . . . H1 H 0.636140 0.287190 0.740514 0.040 Uiso 1 1 calc R U . . . N2 N 0.2226(2) 0.25634(9) 0.5516(3) 0.0544(6) Uani 1 1 d . . . . . C1 C 0.500000 0.500000 0.8167(3) 0.0295(5) Uani 1 2 d S T P . . C2 C 0.5094(2) 0.45621(7) 0.7448(2) 0.0301(4) Uani 1 1 d . . . . . C3 C 0.5085(2) 0.45615(7) 0.5995(2) 0.0370(5) Uani 1 1 d . . . . . H3 H 0.513678 0.426429 0.549371 0.044 Uiso 1 1 calc R U . . . C4 C 0.500000 0.500000 0.5291(3) 0.0418(7) Uani 1 2 d S T P . . H4 H 0.500001 0.499999 0.429969 0.050 Uiso 1 2 calc R U P . . C5 C 0.54848(18) 0.37014(8) 0.7594(3) 0.0313(5) Uani 1 1 d . . . . . H5 H 0.592774 0.378006 0.678486 0.038 Uiso 1 1 calc R U . . . C6 C 0.46067(18) 0.34084(8) 0.7077(3) 0.0328(5) Uani 1 1 d . . . . . C7 C 0.4668(2) 0.31920(9) 0.5761(3) 0.0405(6) Uani 1 1 d . . . . . H7 H 0.524885 0.323783 0.520747 0.049 Uiso 1 1 calc R U . . . C8 C 0.3889(2) 0.29113(9) 0.5258(3) 0.0458(6) Uani 1 1 d . . . . . H8 H 0.393220 0.276009 0.436814 0.055 Uiso 1 1 calc R U . . . C9 C 0.3055(2) 0.28562(9) 0.6069(3) 0.0418(6) Uani 1 1 d . . . . . C10 C 0.2969(2) 0.30591(9) 0.7386(3) 0.0423(6) Uani 1 1 d . . . . . H10 H 0.238788 0.300821 0.793587 0.051 Uiso 1 1 calc R U . . . C11 C 0.37554(19) 0.33384(9) 0.7880(3) 0.0379(5) Uani 1 1 d . . . . . H11 H 0.371142 0.348366 0.877741 0.045 Uiso 1 1 calc R U . . . C12 C 0.61037(18) 0.34400(8) 0.8715(3) 0.0314(5) Uani 1 1 d . . . . . H12 H 0.571831 0.343832 0.960855 0.038 Uiso 1 1 calc R U . . . C13 C 0.63849(19) 0.25749(9) 0.9236(3) 0.0357(5) Uani 1 1 d . . . . . C14 C 0.6806(2) 0.21123(8) 0.8619(3) 0.0374(5) Uani 1 1 d . . . . . C15 C 0.6166(2) 0.17612(9) 0.8057(3) 0.0433(6) Uani 1 1 d . . . . . C16 C 0.6588(3) 0.13518(10) 0.7444(3) 0.0547(8) Uani 1 1 d . . . . . H16 H 0.616221 0.111115 0.705364 0.066 Uiso 1 1 calc R U . . . C17 C 0.7610(3) 0.12847(11) 0.7387(4) 0.0597(9) Uani 1 1 d . . . . . C18 C 0.8227(2) 0.16314(10) 0.7973(4) 0.0538(8) Uani 1 1 d . . . . . H18 H 0.892917 0.158250 0.796085 0.065 Uiso 1 1 calc R U . . . C19 C 0.7840(2) 0.20516(10) 0.8580(3) 0.0434(6) Uani 1 1 d . . . . . C20 C 0.5059(3) 0.18313(10) 0.8082(3) 0.0587(7) Uani 1 1 d . . . . . H20A H 0.485483 0.194999 0.900294 0.088 Uiso 1 1 calc R U . . . H20B H 0.472769 0.152028 0.788970 0.088 Uiso 1 1 calc R U . . . H20C H 0.486791 0.206946 0.736875 0.088 Uiso 1 1 calc R U . . . C21 C 0.8059(4) 0.08417(14) 0.6666(6) 0.0950(16) Uani 1 1 d . . . . . H21A H 0.866510 0.074092 0.715995 0.143 Uiso 1 1 calc R U . . . H21B H 0.822606 0.092474 0.569909 0.143 Uiso 1 1 calc R U . . . H21C H 0.757419 0.057446 0.667382 0.143 Uiso 1 1 calc R U . . . C22 C 0.8527(2) 0.24435(12) 0.9126(4) 0.0584(9) Uani 1 1 d . . . . . H22A H 0.846478 0.273498 0.854291 0.088 Uiso 1 1 calc R U . . . H22B H 0.921838 0.232674 0.909929 0.088 Uiso 1 1 calc R U . . . H22C H 0.834461 0.252316 1.008929 0.088 Uiso 1 1 calc R U . . . C23 C 0.70894(19) 0.37046(9) 0.8950(3) 0.0357(5) Uani 1 1 d . . . . . H23A H 0.696283 0.405208 0.915909 0.043 Uiso 1 1 calc R U . . . H23B H 0.744717 0.355921 0.975201 0.043 Uiso 1 1 calc R U . . . C24 C 0.9650(2) 0.38390(11) 0.6771(4) 0.0602(9) Uani 1 1 d . . . . . C25 C 1.0050(3) 0.36742(13) 0.8180(5) 0.0812(11) Uani 1 1 d . . . . . H25A H 1.012395 0.395690 0.879490 0.122 Uiso 1 1 calc R U . . . H25B H 1.070011 0.351708 0.805311 0.122 Uiso 1 1 calc R U . . . H25C H 0.958170 0.344231 0.860026 0.122 Uiso 1 1 calc R U . . . C26 C 1.0338(3) 0.42244(15) 0.6126(6) 0.0912(15) Uani 1 1 d . . . . . H26A H 1.008996 0.431244 0.519735 0.137 Uiso 1 1 calc R U . . . H26B H 1.101552 0.409280 0.604513 0.137 Uiso 1 1 calc R U . . . H26C H 1.034750 0.451410 0.672198 0.137 Uiso 1 1 calc R U . . . C27 C 0.9615(3) 0.33946(13) 0.5797(5) 0.0820(14) Uani 1 1 d . . . . . H27A H 0.915326 0.315200 0.617746 0.123 Uiso 1 1 calc R U . . . H27B H 1.028429 0.325238 0.572237 0.123 Uiso 1 1 calc R U . . . H27C H 0.938659 0.349631 0.487067 0.123 Uiso 1 1 calc R U . . . C28 C 0.8203(2) 0.46770(10) 0.7874(3) 0.0482(7) Uani 1 1 d . . . . . C29 C 0.8703(3) 0.47747(13) 0.9107(4) 0.0618(9) Uani 1 1 d . . . . . H29 H 0.915737 0.454119 0.946918 0.074 Uiso 1 1 calc R U . . . C30 C 0.8552(3) 0.52083(15) 0.9824(4) 0.0775(12) Uani 1 1 d . . . . . H30 H 0.890792 0.526820 1.066437 0.093 Uiso 1 1 calc R U . . . C31 C 0.7898(3) 0.55488(14) 0.9335(5) 0.0797(14) Uani 1 1 d . . . . . H31 H 0.779447 0.584309 0.983442 0.096 Uiso 1 1 calc R U . . . C32 C 0.7396(3) 0.54630(12) 0.8123(5) 0.0743(12) Uani 1 1 d . . . . . H32 H 0.694579 0.570010 0.776830 0.089 Uiso 1 1 calc R U . . . C33 C 0.7540(2) 0.50291(13) 0.7404(4) 0.0578(7) Uani 1 1 d . . . . . H33 H 0.717592 0.497207 0.656948 0.069 Uiso 1 1 calc R U . . . C34 C 0.7693(7) 0.4119(3) 0.5117(7) 0.0397(16) Uani 0.592(16) 1 d D U P A 1 C35 C 0.7784(6) 0.4512(2) 0.4192(7) 0.0512(19) Uani 0.592(16) 1 d D U P A 1 H35 H 0.817041 0.478538 0.446878 0.061 Uiso 0.592(16) 1 calc R U P A 1 C36 C 0.7334(7) 0.4518(3) 0.2894(7) 0.063(3) Uani 0.592(16) 1 d D U P A 1 H36 H 0.739859 0.479604 0.231085 0.075 Uiso 0.592(16) 1 calc R U P A 1 C37 C 0.6794(7) 0.4123(3) 0.2445(6) 0.057(2) Uani 0.592(16) 1 d D U P A 1 H37 H 0.647977 0.412914 0.155677 0.069 Uiso 0.592(16) 1 calc R U P A 1 C38 C 0.6706(6) 0.3716(3) 0.3285(6) 0.0469(17) Uani 0.592(16) 1 d D U P A 1 H38 H 0.634116 0.343962 0.297467 0.056 Uiso 0.592(16) 1 calc R U P A 1 C39 C 0.7163(7) 0.3716(3) 0.4596(8) 0.0402(14) Uani 0.592(16) 1 d D U P A 1 H39 H 0.711219 0.343263 0.515973 0.048 Uiso 0.592(16) 1 calc R U P A 1 C34A C 0.8005(11) 0.4170(4) 0.5134(7) 0.054(4) Uani 0.408(16) 1 d DG U P A 2 C39A C 0.7400(10) 0.3826(4) 0.4486(11) 0.057(4) Uani 0.408(16) 1 d DG U P A 2 H39A H 0.717427 0.355002 0.499177 0.069 Uiso 0.408(16) 1 calc R U P A 2 C38A C 0.7125(12) 0.3887(5) 0.3098(11) 0.076(4) Uani 0.408(16) 1 d DG . P A 2 H38A H 0.671159 0.365244 0.265576 0.091 Uiso 0.408(16) 1 calc R U P A 2 C37A C 0.7456(18) 0.4291(4) 0.2358(8) 0.116(7) Uani 0.408(16) 1 d DG . P A 2 H37A H 0.726769 0.433290 0.140987 0.139 Uiso 0.408(16) 1 calc R U P A 2 C36A C 0.806(2) 0.4635(3) 0.3006(8) 0.129(8) Uani 0.408(16) 1 d DG . P A 2 H36A H 0.828647 0.491094 0.249997 0.154 Uiso 0.408(16) 1 calc R U P A 2 C35A C 0.8336(15) 0.4574(3) 0.4393(8) 0.092(6) Uani 0.408(16) 1 d DG . P A 2 H35A H 0.874916 0.480853 0.483598 0.111 Uiso 0.408(16) 1 calc R U P A 2 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 I1 0.06143(14) 0.02970(10) 0.03023(10) 0.000 0.000 0.00499(12) Si1 0.0463(4) 0.0293(3) 0.0465(4) -0.0033(3) 0.0095(3) -0.0019(3) O1 0.0478(11) 0.0180(6) 0.0327(8) -0.0012(6) 0.0021(7) 0.0035(7) O2 0.0858(15) 0.0384(10) 0.0394(12) 0.0076(10) 0.0120(12) 0.0107(10) O3 0.0415(9) 0.0337(9) 0.0405(10) -0.0075(8) 0.0047(8) -0.0044(7) O4 0.0956(18) 0.0589(13) 0.0578(16) -0.0081(12) -0.0237(14) -0.0249(14) O5 0.0601(15) 0.0809(18) 0.091(2) -0.0170(16) -0.0091(15) -0.0227(13) N1 0.0437(11) 0.0228(9) 0.0325(11) -0.0010(8) -0.0004(9) 0.0040(8) N2 0.0621(15) 0.0386(13) 0.0624(18) -0.0015(13) -0.0203(15) -0.0085(11) C1 0.0335(14) 0.0266(13) 0.0285(13) 0.000 0.000 0.0023(17) C2 0.0359(12) 0.0208(8) 0.0336(10) 0.0002(7) -0.0019(12) 0.0013(10) C3 0.0509(14) 0.0251(9) 0.0349(10) -0.0041(8) -0.0004(15) 0.0002(13) C4 0.0620(19) 0.0343(15) 0.0291(14) 0.000 0.000 0.002(2) C5 0.0421(12) 0.0190(10) 0.0327(12) -0.0020(9) 0.0036(10) 0.0032(9) C6 0.0427(12) 0.0204(10) 0.0353(13) 0.0004(9) -0.0026(10) 0.0061(9) C7 0.0543(15) 0.0304(11) 0.0370(13) -0.0034(10) 0.0005(10) -0.0004(10) C8 0.0688(18) 0.0311(12) 0.0375(14) -0.0051(12) -0.0087(14) -0.0002(12) C9 0.0491(15) 0.0281(12) 0.0482(16) -0.0008(11) -0.0143(13) -0.0014(11) C10 0.0403(13) 0.0377(13) 0.0488(16) -0.0013(12) -0.0033(12) 0.0010(11) C11 0.0436(13) 0.0316(12) 0.0385(14) -0.0034(11) -0.0010(11) 0.0023(10) C12 0.0400(13) 0.0239(11) 0.0303(12) -0.0023(9) 0.0018(10) 0.0012(9) C13 0.0393(13) 0.0281(11) 0.0397(14) 0.0026(10) -0.0032(10) -0.0010(10) C14 0.0500(15) 0.0248(11) 0.0374(13) 0.0060(10) 0.0003(11) 0.0039(10) C15 0.0573(16) 0.0294(12) 0.0432(15) 0.0009(11) -0.0008(13) 0.0008(11) C16 0.079(2) 0.0322(14) 0.0524(18) -0.0035(13) 0.0013(17) 0.0020(14) C17 0.090(2) 0.0342(15) 0.055(2) 0.0023(14) 0.0131(18) 0.0171(16) C18 0.0582(17) 0.0404(15) 0.063(2) 0.0164(14) 0.0111(16) 0.0172(13) C19 0.0482(15) 0.0347(13) 0.0471(16) 0.0108(11) 0.0015(12) 0.0067(11) C20 0.0565(16) 0.0487(14) 0.0710(18) -0.0082(13) -0.010(2) -0.0080(17) C21 0.126(4) 0.047(2) 0.112(4) -0.014(2) 0.032(3) 0.029(2) C22 0.0470(16) 0.0500(18) 0.078(3) 0.0099(17) -0.0092(16) 0.0003(14) C23 0.0444(13) 0.0304(12) 0.0322(12) -0.0034(10) 0.0002(11) -0.0014(10) C24 0.0457(16) 0.0451(16) 0.090(3) -0.0095(17) 0.0160(16) -0.0030(12) C25 0.0519(17) 0.0622(19) 0.130(3) -0.003(2) -0.018(3) -0.001(2) C26 0.065(2) 0.077(3) 0.132(4) -0.021(3) 0.046(2) -0.0223(19) C27 0.0544(18) 0.058(2) 0.134(4) -0.035(2) 0.015(2) 0.0081(16) C28 0.0499(16) 0.0385(14) 0.0561(18) -0.0101(13) 0.0169(14) -0.0120(12) C29 0.069(2) 0.0544(18) 0.061(2) -0.0106(16) 0.0092(17) -0.0124(16) C30 0.081(3) 0.084(2) 0.068(2) -0.032(2) 0.022(2) -0.033(2) C31 0.061(2) 0.061(2) 0.117(4) -0.048(2) 0.042(2) -0.0221(18) C32 0.0483(17) 0.0482(18) 0.126(4) -0.034(2) 0.022(2) -0.0077(15) C33 0.0468(14) 0.0382(14) 0.089(2) -0.015(2) 0.0111(14) -0.0037(15) C34 0.048(4) 0.030(3) 0.041(3) 0.003(2) 0.015(2) 0.006(3) C35 0.074(4) 0.032(3) 0.047(4) 0.005(2) 0.013(3) 0.000(3) C36 0.107(6) 0.041(4) 0.040(3) 0.012(3) 0.012(4) 0.012(4) C37 0.091(5) 0.049(4) 0.031(3) 0.001(2) 0.000(3) 0.024(3) C38 0.066(4) 0.039(3) 0.036(3) -0.003(2) 0.001(3) 0.009(3) C39 0.056(4) 0.033(3) 0.031(3) 0.004(2) 0.008(3) 0.005(3) C34A 0.069(8) 0.038(5) 0.056(6) -0.003(4) 0.010(5) 0.004(5) C39A 0.073(8) 0.052(7) 0.046(6) 0.000(5) -0.003(5) 0.013(5) C38A 0.107(11) 0.067(8) 0.054(7) -0.012(6) -0.019(7) -0.001(7) C37A 0.20(2) 0.099(11) 0.050(7) 0.001(7) -0.042(11) -0.021(13) C36A 0.24(3) 0.075(8) 0.067(8) 0.005(6) -0.031(12) -0.020(12) C35A 0.180(17) 0.048(5) 0.048(6) 0.006(4) -0.020(8) -0.024(8) 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' I I -0.4742 1.8119 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Si1 C24 106.72(13) . . ? O3 Si1 C28 109.30(11) . . ? O3 Si1 C34 102.2(3) . . ? O3 Si1 C34A 113.9(4) . . ? C24 Si1 C34 111.5(3) . . ? C28 Si1 C24 115.88(15) . . ? C28 Si1 C34 110.3(3) . . ? C34A Si1 C24 102.0(5) . . ? C34A Si1 C28 109.0(4) . . ? C2 O1 C5 118.64(17) . . ? C23 O3 Si1 128.84(15) . . ? C12 N1 H1 118.9 . . ? C13 N1 H1 118.9 . . ? C13 N1 C12 122.2(2) . . ? O4 N2 C9 117.3(3) . . ? O5 N2 O4 123.9(3) . . ? O5 N2 C9 118.8(3) . . ? C2 C1 I1 119.69(13) 2_665 . ? C2 C1 I1 119.69(13) . . ? C2 C1 C2 120.6(3) . 2_665 ? O1 C2 C1 116.09(18) . . ? O1 C2 C3 124.19(18) . . ? C3 C2 C1 119.72(19) . . ? C2 C3 H3 120.4 . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3 120.4 . . ? C3 C4 C3 121.7(3) . 2_665 ? C3 C4 H4 119.2 2_665 . ? C3 C4 H4 119.2 . . ? O1 C5 H5 108.9 . . ? O1 C5 C6 112.17(19) . . ? O1 C5 C12 104.25(18) . . ? C6 C5 H5 108.9 . . ? C6 C5 C12 113.64(19) . . ? C12 C5 H5 108.9 . . ? C7 C6 C5 118.5(2) . . ? C11 C6 C5 122.1(2) . . ? C11 C6 C7 119.3(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.7 . . ? C7 C8 H8 120.7 . . ? C9 C8 C7 118.6(3) . . ? C9 C8 H8 120.7 . . ? C8 C9 N2 118.2(3) . . ? C8 C9 C10 122.8(3) . . ? C10 C9 N2 119.0(3) . . ? C9 C10 H10 121.0 . . ? C9 C10 C11 118.0(3) . . ? C11 C10 H10 121.0 . . ? C6 C11 H11 119.6 . . ? C10 C11 C6 120.8(3) . . ? C10 C11 H11 119.6 . . ? N1 C12 C5 110.28(19) . . ? N1 C12 H12 108.8 . . ? N1 C12 C23 109.65(19) . . ? C5 C12 H12 108.8 . . ? C23 C12 C5 110.37(19) . . ? C23 C12 H12 108.8 . . ? O2 C13 N1 123.5(2) . . ? O2 C13 C14 123.2(2) . . ? N1 C13 C14 113.3(2) . . ? C15 C14 C13 120.1(2) . . ? C19 C14 C13 118.8(2) . . ? C19 C14 C15 121.1(2) . . ? C14 C15 C20 120.9(2) . . ? C16 C15 C14 118.2(3) . . ? C16 C15 C20 121.0(3) . . ? C15 C16 H16 119.1 . . ? C17 C16 C15 121.9(3) . . ? C17 C16 H16 119.1 . . ? C16 C17 C21 121.0(4) . . ? C18 C17 C16 119.0(3) . . ? C18 C17 C21 119.9(4) . . ? C17 C18 H18 119.4 . . ? C17 C18 C19 121.3(3) . . ? C19 C18 H18 119.4 . . ? C14 C19 C22 120.7(3) . . ? C18 C19 C14 118.6(3) . . ? C18 C19 C22 120.6(3) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C12 108.6(2) . . ? O3 C23 H23A 110.0 . . ? O3 C23 H23B 110.0 . . ? C12 C23 H23A 110.0 . . ? C12 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C25 C24 Si1 111.5(3) . . ? C25 C24 C26 110.6(3) . . ? C25 C24 C27 108.3(3) . . ? C26 C24 Si1 110.2(2) . . ? C26 C24 C27 108.7(3) . . ? C27 C24 Si1 107.5(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 Si1 122.4(3) . . ? C29 C28 C33 116.8(3) . . ? C33 C28 Si1 120.6(2) . . ? C28 C29 H29 119.4 . . ? C28 C29 C30 121.2(4) . . ? C30 C29 H29 119.4 . . ? C29 C30 H30 119.6 . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 120.3 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C31 C32 H32 120.0 . . ? C31 C32 C33 120.1(4) . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 121.7(3) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C35 C34 Si1 124.4(6) . . ? C35 C34 C39 115.2(6) . . ? C39 C34 Si1 120.2(5) . . ? C34 C35 H35 118.7 . . ? C36 C35 C34 122.7(6) . . ? C36 C35 H35 118.7 . . ? C35 C36 H36 120.0 . . ? C37 C36 C35 120.1(6) . . ? C37 C36 H36 120.0 . . ? C36 C37 H37 119.9 . . ? C36 C37 C38 120.1(6) . . ? C38 C37 H37 119.9 . . ? C37 C38 H38 120.5 . . ? C37 C38 C39 119.0(6) . . ? C39 C38 H38 120.5 . . ? C34 C39 H39 118.6 . . ? C38 C39 C34 122.7(6) . . ? C38 C39 H39 118.6 . . ? C39A C34A Si1 118.9(5) . . ? C39A C34A C35A 120.0 . . ? C35A C34A Si1 121.1(5) . . ? C34A C39A H39A 120.0 . . ? C38A C39A C34A 120.0 . . ? C38A C39A H39A 120.0 . . ? C39A C38A H38A 120.0 . . ? C39A C38A C37A 120.0 . . ? C37A C38A H38A 120.0 . . ? C38A C37A H37A 120.0 . . ? C36A C37A C38A 120.0 . . ? C36A C37A H37A 120.0 . . ? C37A C36A H36A 120.0 . . ? C37A C36A C35A 120.0 . . ? C35A C36A H36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? 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 I1 C1 2.085(3) . ? Si1 O3 1.6460(19) . ? Si1 C24 1.884(3) . ? Si1 C28 1.880(3) . ? Si1 C34 1.937(8) . ? Si1 C34A 1.787(6) . ? O1 C2 1.374(2) . ? O1 C5 1.446(3) . ? O2 C13 1.216(4) . ? O3 C23 1.422(3) . ? O4 N2 1.234(4) . ? O5 N2 1.212(4) . ? N1 H1 0.8800 . ? N1 C12 1.456(3) . ? N1 C13 1.350(3) . ? N2 C9 1.470(4) . ? C1 C2 1.393(2) 2_665 ? C1 C2 1.392(2) . ? C2 C3 1.392(3) . ? C3 H3 0.9500 . ? C3 C4 1.386(3) . ? C4 H4 0.9500 . ? C5 H5 1.0000 . ? C5 C6 1.509(3) . ? C5 C12 1.535(3) . ? C6 C7 1.397(4) . ? C6 C11 1.389(4) . ? C7 H7 0.9500 . ? C7 C8 1.384(4) . ? C8 H8 0.9500 . ? C8 C9 1.369(4) . ? C9 C10 1.385(4) . ? C10 H10 0.9500 . ? C10 C11 1.387(4) . ? C11 H11 0.9500 . ? C12 H12 1.0000 . ? C12 C23 1.524(3) . ? C13 C14 1.511(3) . ? C14 C15 1.398(4) . ? C14 C19 1.396(4) . ? C15 C16 1.389(4) . ? C15 C20 1.496(5) . ? C16 H16 0.9500 . ? C16 C17 1.382(5) . ? C17 C18 1.380(5) . ? C17 C21 1.524(5) . ? C18 H18 0.9500 . ? C18 C19 1.393(4) . ? C19 C22 1.510(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.521(6) . ? C24 C26 1.534(5) . ? C24 C27 1.538(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.384(5) . ? C28 C33 1.388(5) . ? C29 H29 0.9500 . ? C29 C30 1.390(5) . ? C30 H30 0.9500 . ? C30 C31 1.364(6) . ? C31 H31 0.9500 . ? C31 C32 1.363(6) . ? C32 H32 0.9500 . ? C32 C33 1.390(4) . ? C33 H33 0.9500 . ? C34 C35 1.403(8) . ? C34 C39 1.406(9) . ? C35 H35 0.9500 . ? C35 C36 1.382(9) . ? C36 H36 0.9500 . ? C36 C37 1.374(9) . ? C37 H37 0.9500 . ? C37 C38 1.383(8) . ? C38 H38 0.9500 . ? C38 C39 1.398(8) . ? C39 H39 0.9500 . ? C34A C39A 1.3900 . ? C34A C35A 1.3900 . ? C39A H39A 0.9500 . ? C39A C38A 1.3900 . ? C38A H38A 0.9500 . ? C38A C37A 1.3900 . ? C37A H37A 0.9500 . ? C37A C36A 1.3900 . ? C36A H36A 0.9500 . ? C36A C35A 1.3900 . ? C35A H35A 0.9500 . ? 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 I1 C1 C2 O1 0.3(3) . . . . ? I1 C1 C2 C3 179.4(2) . . . . ? Si1 O3 C23 C12 136.17(18) . . . . ? Si1 C28 C29 C30 -177.0(2) . . . . ? Si1 C28 C33 C32 177.3(2) . . . . ? Si1 C34 C35 C36 178.0(6) . . . . ? Si1 C34 C39 C38 -178.0(7) . . . . ? Si1 C34A C39A C38A 179.7(10) . . . . ? Si1 C34A C35A C36A -179.7(10) . . . . ? O1 C2 C3 C4 -179.8(2) . . . . ? O1 C5 C6 C7 137.0(2) . . . . ? O1 C5 C6 C11 -44.6(3) . . . . ? O1 C5 C12 N1 168.73(18) . . . . ? O1 C5 C12 C23 -70.0(2) . . . . ? O2 C13 C14 C15 90.9(3) . . . . ? O2 C13 C14 C19 -91.2(3) . . . . ? O3 Si1 C24 C25 -52.8(3) . . . . ? O3 Si1 C24 C26 -176.0(3) . . . . ? O3 Si1 C24 C27 65.6(3) . . . . ? O3 Si1 C28 C29 77.1(3) . . . . ? O3 Si1 C28 C33 -99.0(2) . . . . ? O3 Si1 C34A C39A -13.3(8) . . . . ? O3 Si1 C34A C35A 166.3(6) . . . . ? O4 N2 C9 C8 -0.9(4) . . . . ? O4 N2 C9 C10 179.9(3) . . . . ? O5 N2 C9 C8 179.4(3) . . . . ? O5 N2 C9 C10 0.2(4) . . . . ? N1 C12 C23 O3 55.1(3) . . . . ? N1 C13 C14 C15 -90.3(3) . . . . ? N1 C13 C14 C19 87.6(3) . . . . ? N2 C9 C10 C11 -179.3(2) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C2 O1 C5 C6 -90.7(3) . . . . ? C2 O1 C5 C12 145.9(2) . . . . ? C2 C1 C2 O1 -179.7(3) 2_665 . . . ? C2 C1 C2 C3 -0.6(2) 2_665 . . . ? C2 C3 C4 C3 -0.6(2) . . . 2_665 ? C5 O1 C2 C1 -167.25(18) . . . . ? C5 O1 C2 C3 13.7(4) . . . . ? C5 C6 C7 C8 178.6(2) . . . . ? C5 C6 C11 C10 -178.7(2) . . . . ? C5 C12 C23 O3 -66.6(2) . . . . ? C6 C5 C12 N1 46.3(3) . . . . ? C6 C5 C12 C23 167.6(2) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C7 C6 C11 C10 -0.3(4) . . . . ? C7 C8 C9 N2 179.1(2) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C8 C9 C10 C11 1.6(4) . . . . ? C9 C10 C11 C6 -0.5(4) . . . . ? C11 C6 C7 C8 0.1(4) . . . . ? C12 N1 C13 O2 11.4(4) . . . . ? C12 N1 C13 C14 -167.3(2) . . . . ? C12 C5 C6 C7 -105.1(3) . . . . ? C12 C5 C6 C11 73.3(3) . . . . ? C13 N1 C12 C5 -148.2(2) . . . . ? C13 N1 C12 C23 90.1(3) . . . . ? C13 C14 C15 C16 177.2(2) . . . . ? C13 C14 C15 C20 -1.3(4) . . . . ? C13 C14 C19 C18 -178.1(2) . . . . ? C13 C14 C19 C22 -0.9(4) . . . . ? C14 C15 C16 C17 0.4(5) . . . . ? C15 C14 C19 C18 -0.2(4) . . . . ? C15 C14 C19 C22 177.0(3) . . . . ? C15 C16 C17 C18 0.9(5) . . . . ? C15 C16 C17 C21 -177.8(3) . . . . ? C16 C17 C18 C19 -1.8(5) . . . . ? C17 C18 C19 C14 1.5(4) . . . . ? C17 C18 C19 C22 -175.7(3) . . . . ? C19 C14 C15 C16 -0.7(4) . . . . ? C19 C14 C15 C20 -179.1(3) . . . . ? C20 C15 C16 C17 178.8(3) . . . . ? C21 C17 C18 C19 176.9(3) . . . . ? C24 Si1 O3 C23 125.0(2) . . . . ? C24 Si1 C28 C29 -43.5(3) . . . . ? C24 Si1 C28 C33 140.4(3) . . . . ? C24 Si1 C34A C39A 101.3(7) . . . . ? C24 Si1 C34A C35A -79.1(8) . . . . ? C28 Si1 O3 C23 -1.0(3) . . . . ? C28 Si1 C24 C25 69.1(3) . . . . ? C28 Si1 C24 C26 -54.1(3) . . . . ? C28 Si1 C24 C27 -172.4(3) . . . . ? C28 Si1 C34A C39A -135.7(5) . . . . ? C28 Si1 C34A C35A 44.0(8) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C28 C33 C32 1.0(4) . . . . ? C29 C30 C31 C32 -0.5(5) . . . . ? C30 C31 C32 C33 0.8(5) . . . . ? C31 C32 C33 C28 -1.1(5) . . . . ? C33 C28 C29 C30 -0.7(4) . . . . ? C34 Si1 O3 C23 -117.8(3) . . . . ? C34 Si1 C24 C25 -163.6(3) . . . . ? C34 Si1 C24 C26 73.1(4) . . . . ? C34 Si1 C24 C27 -45.2(4) . . . . ? C34 Si1 C28 C29 -171.4(4) . . . . ? C34 Si1 C28 C33 12.5(4) . . . . ? C34 C35 C36 C37 -1.9(10) . . . . ? C35 C34 C39 C38 -3.6(10) . . . . ? C35 C36 C37 C38 -0.6(9) . . . . ? C36 C37 C38 C39 0.9(9) . . . . ? C37 C38 C39 C34 1.4(10) . . . . ? C39 C34 C35 C36 3.8(10) . . . . ? C34A Si1 O3 C23 -123.2(5) . . . . ? C34A Si1 C24 C25 -172.6(4) . . . . ? C34A Si1 C24 C26 64.2(5) . . . . ? C34A Si1 C24 C27 -54.2(5) . . . . ? C34A Si1 C28 C29 -157.8(6) . . . . ? C34A Si1 C28 C33 26.1(6) . . . . ? C34A C39A C38A C37A 0.0 . . . . ? C39A C34A C35A C36A 0.0 . . . . ? C39A C38A C37A C36A 0.0 . . . . ? C38A C37A C36A C35A 0.0 . . . . ? C37A C36A C35A C34A 0.0 . . . . ? C35A C34A C39A C38A 0.0 . . . . ?