#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:31:52 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253841 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557865.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_1557865 loop_ _publ_author_name 'Goonesinghe, Chatura' 'Roshandel, Hootan' 'Diaz, Carlos' 'Jung, Hyuk-Joon' 'Nyamayaro, Kudzanai' 'Ezhova, Maria' 'Mehrkhodavandi, Parisa' _publ_section_title ; Cationic indium catalysts for ring opening polymerization: tuning reactivity with hemilabile ligands ; _journal_issue 25 _journal_name_full 'Chemical Science' _journal_page_first 6485 _journal_paper_doi 10.1039/D0SC01291B _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C44 H59 In N2 O2' _chemical_formula_sum 'C44 H59 In N2 O2' _chemical_formula_weight 762.75 _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 geom _audit_creation_date 2019-11-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-03-02 deposited with the CCDC. 2020-04-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 117.891(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.5732(15) _cell_length_b 13.8493(11) _cell_length_c 18.4226(15) _cell_measurement_reflns_used 9858 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 30.63 _cell_measurement_theta_min 2.22 _cell_volume 3962.8(6) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS, 2016)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_unetI/netI 0.0337 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 63957 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.627 _diffrn_reflns_theta_min 1.930 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0531 before and 0.0467 after correction. The Ratio of minimum to maximum transmission is 0.9389. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.278 _exptl_crystal_description tablet _exptl_crystal_F_000 1608 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.201 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 481 _refine_ls_number_reflns 12154 _refine_ls_number_restraints 860 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0369 _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^)+(0.0292P)^2^+5.6646P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.0887 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9833 _reflns_number_total 12154 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL pm208_0m_a.res in P2(1)/c pm208_0m(1).res created by SHELXL-2017/1 at 23:55:09 on 16-Nov-2019 REM Old TITL pm208_0m in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.082, Rweak 0.002, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C45 In N2 O CELL 0.71073 17.5732 13.8493 18.4226 90 117.891 90 ZERR 4 0.0015 0.0011 0.0015 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H In N O UNIT 176 236 4 8 8 SADI 0.01 O2B C41 O2A C41 SADI 0.01 C41 C42B C42A C41 SADI 0.01 O2B C44B O2A C44A SADI 0.01 C43B C42B C42A C43A SADI 0.01 C44A C43A C43B C44B SIMU RIGU EADP C42B O2A L.S. 10 0 0 PLAN 20 SIZE 0.11 0.21 0.29 TEMP 23 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.029200 5.664600 FVAR 0.26485 0.62477 IN1 3 0.360375 0.644997 0.657015 11.00000 0.01579 0.01654 = 0.01276 -0.00078 0.00457 -0.00207 O1 5 0.266938 0.612898 0.528626 11.00000 0.01524 0.01508 = 0.01596 -0.00148 0.00238 -0.00017 PART 1 O2A 5 0.513995 0.684069 0.945868 -21.00000 0.02123 0.03587 = 0.01783 0.00259 0.01060 0.01304 PART 0 PART 2 O2B 5 0.421373 0.776122 0.863627 21.00000 0.03459 0.02526 = 0.04200 -0.00832 0.01337 -0.00414 PART 0 N1 4 0.514969 0.637901 0.771886 11.00000 0.01906 0.02055 = 0.01192 -0.00225 0.00528 -0.00605 AFIX 13 H1 2 0.522670 0.579393 0.804529 11.00000 -1.20000 AFIX 0 N2 4 0.438207 0.542645 0.621464 11.00000 0.01317 0.02001 = 0.01150 -0.00059 0.00239 -0.00288 C1 1 0.136120 0.826994 0.301516 11.00000 0.02906 0.02375 = 0.03957 0.01306 0.01397 -0.00150 AFIX 43 H1A 2 0.145285 0.880259 0.275851 11.00000 -1.20000 AFIX 0 C2 1 0.101896 0.838575 0.354730 11.00000 0.03218 0.01676 = 0.03078 0.00393 0.00837 0.00077 AFIX 43 H2 2 0.087573 0.899958 0.364868 11.00000 -1.20000 AFIX 0 C3 1 0.088729 0.758889 0.393257 11.00000 0.02855 0.02152 = 0.02260 0.00336 0.01027 0.00198 AFIX 43 H3 2 0.065651 0.767909 0.429043 11.00000 -1.20000 AFIX 0 C4 1 0.109239 0.665798 0.379616 11.00000 0.01450 0.01889 = 0.01662 0.00452 0.00245 0.00019 C5 1 0.142584 0.655240 0.325087 11.00000 0.03650 0.02072 = 0.03271 0.00726 0.02156 0.00370 AFIX 43 H5 2 0.155787 0.593819 0.313875 11.00000 -1.20000 AFIX 0 C6 1 0.156671 0.735119 0.286757 11.00000 0.04719 0.03073 = 0.04609 0.01381 0.03382 0.00570 AFIX 43 H6 2 0.179990 0.726570 0.251112 11.00000 -1.20000 AFIX 0 C7 1 0.090503 0.576809 0.418252 11.00000 0.01350 0.01866 = 0.01602 0.00502 0.00286 -0.00056 C8 1 0.002056 0.537610 0.354362 11.00000 0.01434 0.02406 = 0.02212 0.00736 0.00067 -0.00149 AFIX 137 H8A 2 0.004432 0.520848 0.304898 11.00000 -1.50000 H8B 2 -0.041101 0.586258 0.342456 11.00000 -1.50000 H8C 2 -0.012151 0.481351 0.376010 11.00000 -1.50000 AFIX 0 C9 1 0.082648 0.601258 0.496057 11.00000 0.01826 0.02547 = 0.02193 0.00468 0.00873 0.00161 AFIX 137 H9A 2 0.078040 0.542617 0.521514 11.00000 -1.50000 H9B 2 0.032262 0.640038 0.481388 11.00000 -1.50000 H9C 2 0.132746 0.636355 0.533752 11.00000 -1.50000 AFIX 0 C10 1 0.161678 0.501091 0.440042 11.00000 0.01424 0.01788 = 0.01252 0.00435 0.00225 -0.00086 C11 1 0.144759 0.408673 0.409671 11.00000 0.01608 0.01864 = 0.01337 0.00214 0.00103 -0.00410 AFIX 43 H11 2 0.087974 0.392666 0.373770 11.00000 -1.20000 AFIX 0 C12 1 0.208313 0.336032 0.429526 11.00000 0.01839 0.01564 = 0.01350 0.00038 0.00221 -0.00395 C13 1 0.291640 0.360909 0.481859 11.00000 0.01663 0.01487 = 0.01304 0.00082 0.00348 -0.00109 AFIX 43 H13 2 0.335016 0.315472 0.494557 11.00000 -1.20000 AFIX 0 C14 1 0.313449 0.454271 0.517190 11.00000 0.01389 0.01543 = 0.01012 0.00007 0.00199 -0.00254 C15 1 0.249021 0.526837 0.497671 11.00000 0.01484 0.01632 = 0.01000 0.00185 0.00306 -0.00138 C16 1 0.023041 0.121114 0.501800 11.00000 0.04377 0.02174 = 0.05097 -0.00086 0.02908 -0.00438 AFIX 43 H16 2 -0.009527 0.096013 0.525194 11.00000 -1.20000 AFIX 0 C17 1 -0.002382 0.107865 0.419872 11.00000 0.04201 0.04314 = 0.05490 -0.02100 0.02677 -0.02164 AFIX 43 H17 2 -0.052787 0.074037 0.387594 11.00000 -1.20000 AFIX 0 C18 1 0.046209 0.144340 0.384471 11.00000 0.03205 0.03379 = 0.03609 -0.01495 0.01374 -0.01473 AFIX 43 H18 2 0.027575 0.135003 0.328697 11.00000 -1.20000 AFIX 0 C19 1 0.122110 0.194485 0.431008 11.00000 0.02212 0.01430 = 0.02152 0.00050 0.00370 -0.00089 C20 1 0.146243 0.208413 0.514226 11.00000 0.02957 0.03085 = 0.02148 0.00548 0.00359 -0.00599 AFIX 43 H20 2 0.196170 0.242842 0.546832 11.00000 -1.20000 AFIX 0 C21 1 0.097412 0.172057 0.549070 11.00000 0.03679 0.03039 = 0.02979 0.00864 0.01331 0.00096 AFIX 43 H21 2 0.114860 0.182049 0.604559 11.00000 -1.20000 AFIX 0 C22 1 0.178918 0.234070 0.395194 11.00000 0.02265 0.01622 = 0.01601 -0.00230 0.00280 -0.00523 C23 1 0.129649 0.237451 0.300700 11.00000 0.03697 0.02663 = 0.01865 -0.00388 0.00503 -0.01274 AFIX 137 H23A 2 0.077358 0.273484 0.283544 11.00000 -1.50000 H23B 2 0.116114 0.172906 0.279469 11.00000 -1.50000 H23C 2 0.164765 0.268072 0.280189 11.00000 -1.50000 AFIX 0 C24 1 0.255589 0.164923 0.419974 11.00000 0.02796 0.02056 = 0.02877 -0.00510 0.00955 -0.00198 AFIX 137 H24A 2 0.293128 0.189142 0.399546 11.00000 -1.50000 H24B 2 0.234855 0.102189 0.397093 11.00000 -1.50000 H24C 2 0.286640 0.160277 0.478751 11.00000 -1.50000 AFIX 0 C25 1 0.402793 0.470256 0.572697 11.00000 0.01501 0.01653 = 0.01129 0.00123 0.00321 -0.00054 AFIX 43 H25 2 0.440290 0.422206 0.573802 11.00000 -1.20000 AFIX 0 C26 1 0.533159 0.538783 0.671339 11.00000 0.01302 0.01926 = 0.01223 0.00090 0.00236 -0.00216 AFIX 13 H26 2 0.547959 0.481771 0.706878 11.00000 -1.20000 AFIX 0 C27 1 0.579480 0.531194 0.618850 11.00000 0.01506 0.02769 = 0.01416 0.00147 0.00437 -0.00128 AFIX 23 H27A 2 0.559135 0.474531 0.584011 11.00000 -1.20000 H27B 2 0.566178 0.587521 0.583700 11.00000 -1.20000 AFIX 0 C28 1 0.676946 0.524125 0.672932 11.00000 0.01528 0.03536 = 0.01842 0.00224 0.00598 0.00004 AFIX 23 H28A 2 0.690682 0.465759 0.705763 11.00000 -1.20000 H28B 2 0.705102 0.520640 0.638571 11.00000 -1.20000 AFIX 0 C29 1 0.709770 0.611501 0.728956 11.00000 0.01656 0.03725 = 0.02363 0.00058 0.00662 -0.00607 AFIX 23 H29A 2 0.701725 0.668961 0.696033 11.00000 -1.20000 H29B 2 0.770939 0.604102 0.765293 11.00000 -1.20000 AFIX 0 C30 1 0.662814 0.623939 0.780080 11.00000 0.01591 0.03292 = 0.01616 -0.00212 0.00323 -0.00743 AFIX 23 H30A 2 0.682371 0.682815 0.812078 11.00000 -1.20000 H30B 2 0.676836 0.570256 0.818022 11.00000 -1.20000 AFIX 0 C31 1 0.565070 0.628611 0.726085 11.00000 0.01482 0.02245 = 0.01363 -0.00115 0.00418 -0.00617 AFIX 13 H31 2 0.552289 0.685061 0.690170 11.00000 -1.20000 AFIX 0 C32 1 0.376984 0.794994 0.631686 11.00000 0.02408 0.01785 = 0.02335 0.00147 0.00845 -0.00344 AFIX 23 H32A 2 0.397535 0.831909 0.682112 11.00000 -1.20000 H32B 2 0.420621 0.798243 0.613571 11.00000 -1.20000 AFIX 0 C33 1 0.293816 0.841303 0.566090 11.00000 0.03446 0.01926 = 0.02032 0.00041 0.00761 0.00214 AFIX 13 H33 2 0.268532 0.797541 0.518848 11.00000 -1.20000 AFIX 0 C34 1 0.229201 0.854168 0.598573 11.00000 0.03280 0.03047 = 0.04342 -0.00302 0.01601 0.00397 AFIX 137 H34A 2 0.213016 0.792034 0.609991 11.00000 -1.50000 H34B 2 0.179045 0.886800 0.558150 11.00000 -1.50000 H34C 2 0.254773 0.891787 0.648074 11.00000 -1.50000 AFIX 0 C35 1 0.310322 0.937901 0.536644 11.00000 0.06414 0.02206 = 0.03566 0.00540 0.02599 0.00654 AFIX 137 H35A 2 0.339751 0.980136 0.582817 11.00000 -1.50000 H35B 2 0.256438 0.966406 0.498726 11.00000 -1.50000 H35C 2 0.345189 0.928103 0.509811 11.00000 -1.50000 AFIX 0 C36 1 0.296138 0.585297 0.723963 11.00000 0.02357 0.02238 = 0.02325 0.00234 0.01084 -0.00341 AFIX 23 H36A 2 0.315640 0.623459 0.773641 11.00000 -1.20000 H36B 2 0.235352 0.599338 0.690962 11.00000 -1.20000 AFIX 0 C37 1 0.301666 0.479545 0.750464 11.00000 0.02923 0.02678 = 0.02893 0.00470 0.01198 -0.00450 AFIX 13 H37 2 0.274111 0.475283 0.785916 11.00000 -1.20000 AFIX 0 C38 1 0.394270 0.445696 0.801139 11.00000 0.03004 0.03558 = 0.04317 0.01856 0.00707 -0.00106 AFIX 137 H38A 2 0.423533 0.448934 0.768361 11.00000 -1.50000 H38B 2 0.394620 0.380309 0.818590 11.00000 -1.50000 H38C 2 0.423046 0.486502 0.848415 11.00000 -1.50000 AFIX 0 C39 1 0.253027 0.412335 0.678661 11.00000 0.03960 0.02991 = 0.03548 -0.00015 0.01800 -0.00852 AFIX 137 H39A 2 0.194985 0.434975 0.647178 11.00000 -1.50000 H39B 2 0.252422 0.348514 0.698722 11.00000 -1.50000 H39C 2 0.280810 0.410870 0.644523 11.00000 -1.50000 AFIX 0 C40 1 0.539274 0.723155 0.826556 11.00000 0.02564 0.02589 = 0.01895 -0.00702 0.00914 -0.00914 AFIX 23 H40A 2 0.528256 0.781327 0.793825 11.00000 -1.20000 H40B 2 0.600439 0.720627 0.864312 11.00000 -1.20000 AFIX 0 C41 1 0.490625 0.727619 0.874058 11.00000 0.02306 0.02817 = 0.01605 -0.00607 0.00545 -0.00798 PART 1 C42A 1 0.412089 0.784038 0.834625 -21.00000 0.05153 0.06963 = 0.03885 0.00065 0.02061 0.00293 AFIX 43 H42A 2 0.386431 0.815144 0.784014 -21.00000 -1.20000 AFIX 0 PART 0 PART 2 C42B 1 0.525124 0.660428 0.939200 21.00000 0.02123 0.03587 = 0.01783 0.00259 0.01060 0.01304 AFIX 43 H42B 2 0.569561 0.616026 0.953496 21.00000 -1.20000 AFIX 0 PART 0 PART 1 C43A 1 0.385567 0.777016 0.898932 -21.00000 0.04694 0.04019 = 0.07243 -0.02039 0.04408 -0.00944 AFIX 43 H43A 2 0.336902 0.806679 0.896392 -21.00000 -1.20000 AFIX 0 PART 0 PART 2 C43B 1 0.471779 0.680612 0.976739 21.00000 0.02957 0.05659 = 0.02132 0.00657 0.01167 0.01869 AFIX 43 H43B 2 0.479857 0.650546 1.024966 21.00000 -1.20000 AFIX 0 PART 0 PART 1 C44A 1 0.440041 0.722686 0.961626 -21.00000 0.04585 0.06455 = 0.05499 -0.00914 0.04234 -0.00711 AFIX 43 H44A 2 0.434459 0.709707 1.008441 -21.00000 -1.20000 AFIX 0 PART 0 PART 2 C44B 1 0.409325 0.745760 0.937823 21.00000 0.02282 0.02950 = 0.03181 -0.00096 0.01429 0.00450 AFIX 43 H44B 2 0.368234 0.767533 0.952356 21.00000 -1.20000 AFIX 0 HKLF 4 REM pm208_0m_a.res in P2(1)/c REM R1 = 0.0369 for 9833 Fo > 4sig(Fo) and 0.0523 for all 12154 data REM 481 parameters refined using 860 restraints END WGHT 0.0292 5.6645 REM Highest difference peak 1.201, deepest hole -1.115, 1-sigma level 0.088 Q1 1 0.4999 0.7137 0.9564 11.00000 0.05 1.20 Q2 1 0.0838 0.1409 0.4726 11.00000 0.05 0.94 Q3 1 0.6395 0.5743 0.8403 11.00000 0.05 0.87 Q4 1 0.3787 0.6765 0.6479 11.00000 0.05 0.83 Q5 1 0.3197 0.6598 0.6608 11.00000 0.05 0.67 Q6 1 0.3174 0.4655 0.7167 11.00000 0.05 0.54 Q7 1 0.4215 0.5800 0.5980 11.00000 0.05 0.52 Q8 1 0.1054 0.2013 0.4618 11.00000 0.05 0.51 Q9 1 0.1143 0.6678 0.3476 11.00000 0.05 0.49 Q10 1 0.2400 0.4396 0.7317 11.00000 0.05 0.49 Q11 1 0.2208 0.1967 0.4169 11.00000 0.05 0.49 Q12 1 0.2820 0.4827 0.5138 11.00000 0.05 0.48 Q13 1 0.1574 0.2208 0.4200 11.00000 0.05 0.48 Q14 1 0.3365 0.6001 0.7055 11.00000 0.05 0.46 Q15 1 0.0911 0.5968 0.4635 11.00000 0.05 0.46 Q16 1 0.1037 0.8223 0.3178 11.00000 0.05 0.45 Q17 1 0.6791 0.5739 0.6993 11.00000 0.05 0.44 Q18 1 0.2008 0.5207 0.4615 11.00000 0.05 0.44 Q19 1 0.0992 0.6185 0.3864 11.00000 0.05 0.44 Q20 1 0.5575 0.5546 0.6433 11.00000 0.05 0.44 REM The information below was added by Olex2. REM REM R1 = 0.0369 for 9833 Fo > 4sig(Fo) and 0.0523 for all 65152 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.20, deepest hole -1.12 REM Mean Shift 0, Max Shift -0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0523 REM R1_gt = 0.0369 REM wR_ref = 0.0887 REM GOOF = 1.054 REM Shift_max = -0.002 REM Shift_mean = 0 REM Reflections_all = 65152 REM Reflections_gt = 9833 REM Parameters = n/a REM Hole = -1.12 REM Peak = 1.20 REM Flack = n/a ; _cod_data_source_file d0sc01291b2.cif _cod_data_source_block Complex1b _cod_depositor_comments 'Adding full bibliography for 1557864--1557868.cif.' _cod_database_code 1557865 _shelx_shelxl_version_number 2017/1 _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 0.934 _shelx_estimated_absorpt_t_min 0.838 _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 O2B-C41 \\sim O2A-C41 with sigma of 0.01 C41-C42B \\sim C42A-C41 with sigma of 0.01 O2B-C44B \\sim O2A-C44A with sigma of 0.01 C43B-C42B \\sim C42A-C43A with sigma of 0.01 C44A-C43A \\sim C43B-C44B with sigma of 0.01 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C42B) = Uanis(O2A) 4. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O2A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=1-FVAR(1) Sof(O2B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=Sof(H43B)=Sof(C44B)=Sof(H44B)=FVAR(1) 6.a Ternary CH refined with riding coordinates: N1(H1), C26(H26), C31(H31), C33(H33), C37(H37) 6.b Secondary CH2 refined with riding coordinates: C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A, H32B), C36(H36A,H36B), C40(H40A,H40B) 6.c Aromatic/amide H refined with riding coordinates: C1(H1A), C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C13(H13), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C25(H25), C42A(H42A), C42B(H42B), C43A(H43A), C43B(H43B), C44A(H44A), C44B(H44B) 6.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B, H39C) ; _olex2_submission_special_instructions 'No special instructions were received' 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 In1 In 0.36037(2) 0.64500(2) 0.65701(2) 0.01587(4) Uani 1 1 d . U . . . O1 O 0.26694(9) 0.61290(10) 0.52863(8) 0.0174(3) Uani 1 1 d . U . . . O2A O 0.5140(6) 0.6841(7) 0.9459(5) 0.0244(10) Uani 0.375(7) 1 d D U P A 1 O2B O 0.4214(3) 0.7761(4) 0.8636(3) 0.0358(11) Uani 0.625(7) 1 d D U P A 2 N1 N 0.51497(11) 0.63790(13) 0.77189(10) 0.0180(3) Uani 1 1 d . U . . . H1 H 0.522670 0.579393 0.804529 0.022 Uiso 1 1 calc R . . . . N2 N 0.43821(11) 0.54264(12) 0.62146(10) 0.0162(3) Uani 1 1 d . U . . . C1 C 0.13612(17) 0.82699(18) 0.30152(16) 0.0316(5) Uani 1 1 d . U . . . H1A H 0.145285 0.880259 0.275851 0.038 Uiso 1 1 calc R . . . . C2 C 0.10190(16) 0.83858(16) 0.35473(15) 0.0291(5) Uani 1 1 d . U . . . H2 H 0.087573 0.899958 0.364868 0.035 Uiso 1 1 calc R . . . . C3 C 0.08873(15) 0.75889(16) 0.39326(14) 0.0249(4) Uani 1 1 d . U . . . H3 H 0.065651 0.767909 0.429043 0.030 Uiso 1 1 calc R . . . . C4 C 0.10924(13) 0.66580(15) 0.37962(12) 0.0186(4) Uani 1 1 d . U . . . C5 C 0.14258(17) 0.65524(17) 0.32509(15) 0.0278(5) Uani 1 1 d . U . . . H5 H 0.155787 0.593819 0.313875 0.033 Uiso 1 1 calc R . . . . C6 C 0.15667(19) 0.73512(19) 0.28676(18) 0.0365(6) Uani 1 1 d . U . . . H6 H 0.179990 0.726570 0.251112 0.044 Uiso 1 1 calc R . . . . C7 C 0.09050(13) 0.57681(15) 0.41825(12) 0.0177(4) Uani 1 1 d . U . . . C8 C 0.00206(13) 0.53761(16) 0.35436(13) 0.0233(4) Uani 1 1 d . U . . . H8A H 0.004432 0.520848 0.304898 0.035 Uiso 1 1 calc GR . . . . H8B H -0.041101 0.586258 0.342456 0.035 Uiso 1 1 calc GR . . . . H8C H -0.012151 0.481351 0.376010 0.035 Uiso 1 1 calc GR . . . . C9 C 0.08265(14) 0.60126(17) 0.49606(13) 0.0222(4) Uani 1 1 d . U . . . H9A H 0.078040 0.542617 0.521514 0.033 Uiso 1 1 calc GR . . . . H9B H 0.032262 0.640038 0.481388 0.033 Uiso 1 1 calc GR . . . . H9C H 0.132746 0.636355 0.533752 0.033 Uiso 1 1 calc GR . . . . C10 C 0.16168(12) 0.50109(15) 0.44004(11) 0.0165(4) Uani 1 1 d . U . . . C11 C 0.14476(13) 0.40867(15) 0.40967(12) 0.0184(4) Uani 1 1 d . U . . . H11 H 0.087974 0.392666 0.373770 0.022 Uiso 1 1 calc R . . . . C12 C 0.20831(13) 0.33603(14) 0.42953(12) 0.0179(4) Uani 1 1 d . U . . . C13 C 0.29164(13) 0.36091(14) 0.48186(11) 0.0162(4) Uani 1 1 d . U . . . H13 H 0.335016 0.315472 0.494557 0.019 Uiso 1 1 calc R . . . . C14 C 0.31345(12) 0.45427(14) 0.51719(11) 0.0146(3) Uani 1 1 d . U . . . C15 C 0.24902(12) 0.52684(14) 0.49767(11) 0.0148(3) Uani 1 1 d . U . . . C16 C 0.02304(19) 0.12111(18) 0.50180(18) 0.0361(6) Uani 1 1 d . U . . . H16 H -0.009527 0.096013 0.525194 0.043 Uiso 1 1 calc R . . . . C17 C -0.0024(2) 0.1079(2) 0.4199(2) 0.0450(7) Uani 1 1 d . U . . . H17 H -0.052787 0.074037 0.387594 0.054 Uiso 1 1 calc R . . . . C18 C 0.04621(17) 0.14434(19) 0.38447(17) 0.0349(6) Uani 1 1 d . U . . . H18 H 0.027575 0.135003 0.328697 0.042 Uiso 1 1 calc R . . . . C19 C 0.12211(14) 0.19449(15) 0.43101(13) 0.0219(4) Uani 1 1 d . U . . . C20 C 0.14624(16) 0.20841(18) 0.51423(14) 0.0306(5) Uani 1 1 d . U . . . H20 H 0.196170 0.242842 0.546832 0.037 Uiso 1 1 calc R . . . . C21 C 0.09741(18) 0.17206(19) 0.54907(16) 0.0332(5) Uani 1 1 d . U . . . H21 H 0.114860 0.182049 0.604559 0.040 Uiso 1 1 calc R . . . . C22 C 0.17892(14) 0.23407(15) 0.39519(12) 0.0208(4) Uani 1 1 d . U . . . C23 C 0.12965(17) 0.23745(18) 0.30070(13) 0.0306(5) Uani 1 1 d . U . . . H23A H 0.077358 0.273484 0.283544 0.046 Uiso 1 1 calc GR . . . . H23B H 0.116114 0.172906 0.279469 0.046 Uiso 1 1 calc GR . . . . H23C H 0.164765 0.268072 0.280189 0.046 Uiso 1 1 calc GR . . . . C24 C 0.25559(16) 0.16492(16) 0.41997(15) 0.0273(5) Uani 1 1 d . U . . . H24A H 0.293128 0.189142 0.399546 0.041 Uiso 1 1 calc GR . . . . H24B H 0.234855 0.102189 0.397093 0.041 Uiso 1 1 calc GR . . . . H24C H 0.286640 0.160277 0.478751 0.041 Uiso 1 1 calc GR . . . . C25 C 0.40279(12) 0.47026(14) 0.57270(11) 0.0155(4) Uani 1 1 d . U . . . H25 H 0.440290 0.422206 0.573802 0.019 Uiso 1 1 calc R . . . . C26 C 0.53316(12) 0.53878(15) 0.67134(11) 0.0163(4) Uani 1 1 d . U . . . H26 H 0.547959 0.481771 0.706878 0.020 Uiso 1 1 calc R . . . . C27 C 0.57948(13) 0.53119(16) 0.61885(12) 0.0200(4) Uani 1 1 d . U . . . H27A H 0.559135 0.474531 0.584011 0.024 Uiso 1 1 calc R . . . . H27B H 0.566178 0.587521 0.583700 0.024 Uiso 1 1 calc R . . . . C28 C 0.67695(14) 0.52413(18) 0.67293(13) 0.0238(4) Uani 1 1 d . U . . . H28A H 0.690682 0.465759 0.705763 0.029 Uiso 1 1 calc R . . . . H28B H 0.705102 0.520640 0.638571 0.029 Uiso 1 1 calc R . . . . C29 C 0.70977(14) 0.61150(19) 0.72896(14) 0.0269(5) Uani 1 1 d . U . . . H29A H 0.701725 0.668961 0.696033 0.032 Uiso 1 1 calc R . . . . H29B H 0.770939 0.604102 0.765293 0.032 Uiso 1 1 calc R . . . . C30 C 0.66281(13) 0.62394(17) 0.78008(13) 0.0234(4) Uani 1 1 d . U . . . H30A H 0.682371 0.682815 0.812078 0.028 Uiso 1 1 calc R . . . . H30B H 0.676836 0.570256 0.818022 0.028 Uiso 1 1 calc R . . . . C31 C 0.56507(13) 0.62861(15) 0.72609(12) 0.0180(4) Uani 1 1 d . U . . . H31 H 0.552289 0.685061 0.690170 0.022 Uiso 1 1 calc R . . . . C32 C 0.37698(15) 0.79499(15) 0.63169(13) 0.0228(4) Uani 1 1 d . U . . . H32A H 0.397535 0.831909 0.682112 0.027 Uiso 1 1 calc R . . . . H32B H 0.420621 0.798243 0.613571 0.027 Uiso 1 1 calc R . . . . C33 C 0.29382(16) 0.84130(16) 0.56609(14) 0.0268(5) Uani 1 1 d . U . . . H33 H 0.268532 0.797541 0.518848 0.032 Uiso 1 1 calc R . . . . C34 C 0.22920(18) 0.8542(2) 0.59857(18) 0.0363(6) Uani 1 1 d . U . . . H34A H 0.213016 0.792034 0.609991 0.054 Uiso 1 1 calc GR . . . . H34B H 0.179045 0.886800 0.558150 0.054 Uiso 1 1 calc GR . . . . H34C H 0.254773 0.891787 0.648074 0.054 Uiso 1 1 calc GR . . . . C35 C 0.3103(2) 0.93790(19) 0.53664(17) 0.0396(7) Uani 1 1 d . U . . . H35A H 0.339751 0.980136 0.582817 0.059 Uiso 1 1 calc GR . . . . H35B H 0.256438 0.966406 0.498726 0.059 Uiso 1 1 calc GR . . . . H35C H 0.345189 0.928103 0.509811 0.059 Uiso 1 1 calc GR . . . . C36 C 0.29614(15) 0.58530(16) 0.72396(14) 0.0231(4) Uani 1 1 d . U . . . H36A H 0.315640 0.623459 0.773641 0.028 Uiso 1 1 calc R . . . . H36B H 0.235352 0.599338 0.690962 0.028 Uiso 1 1 calc R . . . . C37 C 0.30167(16) 0.47954(18) 0.75046(15) 0.0290(5) Uani 1 1 d . U . . . H37 H 0.274111 0.475283 0.785916 0.035 Uiso 1 1 calc R . . . . C38 C 0.39427(17) 0.4457(2) 0.80114(18) 0.0403(7) Uani 1 1 d . U . . . H38A H 0.423533 0.448934 0.768361 0.060 Uiso 1 1 calc GR . . . . H38B H 0.394620 0.380309 0.818590 0.060 Uiso 1 1 calc GR . . . . H38C H 0.423046 0.486502 0.848415 0.060 Uiso 1 1 calc GR . . . . C39 C 0.25303(18) 0.41233(19) 0.67866(16) 0.0348(6) Uani 1 1 d . U . . . H39A H 0.194985 0.434975 0.647178 0.052 Uiso 1 1 calc GR . . . . H39B H 0.252422 0.348514 0.698722 0.052 Uiso 1 1 calc GR . . . . H39C H 0.280810 0.410870 0.644523 0.052 Uiso 1 1 calc GR . . . . C40 C 0.53927(15) 0.72316(17) 0.82656(13) 0.0240(4) Uani 1 1 d . U . . . H40A H 0.528256 0.781327 0.793825 0.029 Uiso 1 1 calc R . . . . H40B H 0.600439 0.720627 0.864312 0.029 Uiso 1 1 calc R . . . . C41 C 0.49063(14) 0.72762(16) 0.87406(12) 0.0239(4) Uani 1 1 d D U . . . C42A C 0.4121(9) 0.7840(13) 0.8346(7) 0.054(3) Uani 0.375(7) 1 d D U P A 1 H42A H 0.386431 0.815144 0.784014 0.064 Uiso 0.375(7) 1 calc R . P A 1 C42B C 0.5251(5) 0.6604(5) 0.9392(4) 0.0244(10) Uani 0.625(7) 1 d D U P A 2 H42B H 0.569561 0.616026 0.953496 0.029 Uiso 0.625(7) 1 calc R . P A 2 C43A C 0.3856(7) 0.7770(7) 0.8989(7) 0.047(2) Uani 0.375(7) 1 d D U P A 1 H43A H 0.336902 0.806679 0.896392 0.056 Uiso 0.375(7) 1 calc R . P A 1 C43B C 0.4718(3) 0.6806(4) 0.9767(3) 0.0359(12) Uani 0.625(7) 1 d D U P A 2 H43B H 0.479857 0.650546 1.024966 0.043 Uiso 0.625(7) 1 calc R . P A 2 C44A C 0.4400(7) 0.7227(10) 0.9616(7) 0.048(3) Uani 0.375(7) 1 d D U P A 1 H44A H 0.434459 0.709707 1.008441 0.057 Uiso 0.375(7) 1 calc R . P A 1 C44B C 0.4093(3) 0.7458(4) 0.9378(3) 0.0274(11) Uani 0.625(7) 1 d D U P A 2 H44B H 0.368234 0.767533 0.952356 0.033 Uiso 0.625(7) 1 calc R . 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 In1 0.01579(7) 0.01654(7) 0.01276(6) -0.00078(5) 0.00457(5) -0.00207(5) O1 0.0152(6) 0.0151(6) 0.0160(6) -0.0015(5) 0.0024(5) -0.0002(5) O2A 0.021(2) 0.036(3) 0.0178(13) 0.0026(19) 0.0106(10) 0.0130(17) O2B 0.0346(19) 0.0253(17) 0.042(3) -0.0083(18) 0.013(2) -0.0041(13) N1 0.0191(8) 0.0205(8) 0.0119(7) -0.0023(6) 0.0053(6) -0.0061(7) N2 0.0132(7) 0.0200(8) 0.0115(7) -0.0006(6) 0.0024(6) -0.0029(6) C1 0.0291(12) 0.0238(11) 0.0396(13) 0.0131(10) 0.0140(10) -0.0015(9) C2 0.0322(12) 0.0168(10) 0.0308(12) 0.0039(8) 0.0084(10) 0.0008(9) C3 0.0285(11) 0.0215(10) 0.0226(10) 0.0034(8) 0.0103(9) 0.0020(9) C4 0.0145(9) 0.0189(9) 0.0166(9) 0.0045(7) 0.0024(7) 0.0002(7) C5 0.0365(13) 0.0207(10) 0.0327(12) 0.0073(9) 0.0216(10) 0.0037(9) C6 0.0472(16) 0.0307(13) 0.0461(15) 0.0138(11) 0.0338(13) 0.0057(11) C7 0.0135(8) 0.0187(9) 0.0160(8) 0.0050(7) 0.0029(7) -0.0006(7) C8 0.0143(9) 0.0241(10) 0.0221(10) 0.0074(8) 0.0007(7) -0.0015(8) C9 0.0183(9) 0.0255(11) 0.0219(10) 0.0047(8) 0.0087(8) 0.0016(8) C10 0.0142(8) 0.0179(9) 0.0125(8) 0.0043(7) 0.0023(7) -0.0009(7) C11 0.0161(9) 0.0186(9) 0.0134(8) 0.0021(7) 0.0010(7) -0.0041(7) C12 0.0184(9) 0.0156(9) 0.0135(8) 0.0004(6) 0.0022(7) -0.0039(7) C13 0.0166(8) 0.0149(8) 0.0130(8) 0.0008(7) 0.0035(7) -0.0011(7) C14 0.0139(8) 0.0154(8) 0.0101(7) 0.0001(6) 0.0020(6) -0.0025(7) C15 0.0148(8) 0.0163(8) 0.0100(7) 0.0019(6) 0.0031(6) -0.0014(7) C16 0.0438(15) 0.0217(11) 0.0510(16) -0.0009(11) 0.0291(13) -0.0044(10) C17 0.0420(16) 0.0431(16) 0.0549(17) -0.0210(14) 0.0268(14) -0.0216(13) C18 0.0320(13) 0.0338(13) 0.0361(13) -0.0150(11) 0.0137(10) -0.0147(11) C19 0.0221(10) 0.0143(9) 0.0215(9) 0.0005(7) 0.0037(8) -0.0009(7) C20 0.0296(12) 0.0309(12) 0.0215(10) 0.0055(9) 0.0036(9) -0.0060(10) C21 0.0368(14) 0.0304(12) 0.0298(12) 0.0086(10) 0.0133(10) 0.0010(10) C22 0.0226(10) 0.0162(9) 0.0160(9) -0.0023(7) 0.0028(7) -0.0052(7) C23 0.0370(13) 0.0266(12) 0.0187(10) -0.0039(8) 0.0050(9) -0.0127(10) C24 0.0280(11) 0.0206(11) 0.0288(11) -0.0051(8) 0.0095(9) -0.0020(8) C25 0.0150(8) 0.0165(9) 0.0113(8) 0.0012(6) 0.0032(6) -0.0005(7) C26 0.0130(8) 0.0193(9) 0.0122(8) 0.0009(7) 0.0024(6) -0.0022(7) C27 0.0151(9) 0.0277(11) 0.0142(8) 0.0015(7) 0.0044(7) -0.0013(8) C28 0.0153(9) 0.0354(12) 0.0184(9) 0.0022(8) 0.0060(7) 0.0000(8) C29 0.0166(10) 0.0372(13) 0.0236(10) 0.0006(9) 0.0066(8) -0.0061(9) C30 0.0159(9) 0.0329(12) 0.0162(9) -0.0021(8) 0.0032(7) -0.0074(8) C31 0.0148(8) 0.0224(10) 0.0136(8) -0.0011(7) 0.0042(7) -0.0062(7) C32 0.0241(10) 0.0178(9) 0.0233(10) 0.0015(8) 0.0084(8) -0.0034(8) C33 0.0345(12) 0.0193(10) 0.0203(10) 0.0004(8) 0.0076(9) 0.0021(9) C34 0.0328(13) 0.0305(13) 0.0434(15) -0.0030(11) 0.0160(11) 0.0040(11) C35 0.064(2) 0.0221(12) 0.0357(13) 0.0054(10) 0.0260(13) 0.0065(12) C36 0.0236(10) 0.0224(10) 0.0232(10) 0.0023(8) 0.0108(8) -0.0034(8) C37 0.0292(12) 0.0268(11) 0.0289(11) 0.0047(9) 0.0120(9) -0.0045(9) C38 0.0300(13) 0.0356(14) 0.0432(15) 0.0186(12) 0.0071(11) -0.0011(11) C39 0.0396(14) 0.0299(13) 0.0355(13) -0.0001(10) 0.0180(11) -0.0085(11) C40 0.0256(11) 0.0259(11) 0.0189(9) -0.0070(8) 0.0091(8) -0.0091(9) C41 0.0231(10) 0.0282(11) 0.0161(9) -0.0061(8) 0.0054(8) -0.0080(8) C42A 0.052(6) 0.070(7) 0.039(6) 0.001(5) 0.021(5) 0.003(4) C42B 0.021(2) 0.036(3) 0.0178(13) 0.0026(19) 0.0106(10) 0.0130(17) C43A 0.047(5) 0.040(5) 0.072(6) -0.020(4) 0.044(5) -0.009(4) C43B 0.030(2) 0.057(3) 0.0213(18) 0.0066(18) 0.0117(16) 0.019(2) C44A 0.046(7) 0.065(8) 0.055(6) -0.009(5) 0.042(5) -0.007(5) C44B 0.023(3) 0.029(3) 0.032(3) -0.0010(19) 0.014(2) 0.0045(18) 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' In In -0.7276 1.3100 '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' 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 In1 N1 148.60(6) . . ? O1 In1 N2 79.12(5) . . ? N2 In1 N1 70.31(6) . . ? C32 In1 O1 94.00(7) . . ? C32 In1 N1 90.98(7) . . ? C32 In1 N2 112.01(8) . . ? C32 In1 C36 129.61(9) . . ? C36 In1 O1 101.95(7) . . ? C36 In1 N1 98.52(7) . . ? C36 In1 N2 117.81(8) . . ? C15 O1 In1 124.33(12) . . ? C41 O2A C44A 97.7(6) . . ? C41 O2B C44B 103.4(3) . . ? In1 N1 H1 109.2 . . ? C31 N1 In1 102.53(11) . . ? C31 N1 H1 109.2 . . ? C40 N1 In1 113.01(13) . . ? C40 N1 H1 109.2 . . ? C40 N1 C31 113.42(16) . . ? C25 N2 In1 121.68(14) . . ? C25 N2 C26 116.01(17) . . ? C26 N2 In1 119.97(12) . . ? C2 C1 H1A 120.4 . . ? C2 C1 C6 119.2(2) . . ? C6 C1 H1A 120.4 . . ? C1 C2 H2 119.9 . . ? C1 C2 C3 120.2(2) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 119.2 . . ? C2 C3 C4 121.6(2) . . ? C4 C3 H3 119.2 . . ? C3 C4 C7 122.0(2) . . ? C5 C4 C3 117.4(2) . . ? C5 C4 C7 120.42(19) . . ? C4 C5 H5 119.4 . . ? C4 C5 C6 121.2(2) . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 120.3(2) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C4 C7 C8 106.66(15) . . ? C4 C7 C9 112.78(17) . . ? C4 C7 C10 110.17(17) . . ? C9 C7 C8 106.87(17) . . ? C10 C7 C8 111.45(17) . . ? C10 C7 C9 108.88(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C7 122.40(17) . . ? C11 C10 C15 118.88(18) . . ? C15 C10 C7 118.65(17) . . ? C10 C11 H11 117.9 . . ? C10 C11 C12 124.20(18) . . ? C12 C11 H11 117.9 . . ? C11 C12 C22 118.28(18) . . ? C13 C12 C11 117.21(18) . . ? C13 C12 C22 124.41(19) . . ? C12 C13 H13 119.2 . . ? C12 C13 C14 121.58(19) . . ? C14 C13 H13 119.2 . . ? C13 C14 C15 120.93(17) . . ? C13 C14 C25 116.03(18) . . ? C15 C14 C25 123.04(17) . . ? O1 C15 C10 120.45(18) . . ? O1 C15 C14 122.41(17) . . ? C14 C15 C10 117.13(17) . . ? C17 C16 H16 120.4 . . ? C17 C16 C21 119.2(3) . . ? C21 C16 H16 120.4 . . ? C16 C17 H17 119.6 . . ? C16 C17 C18 120.8(3) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.5 . . ? C19 C18 C17 121.1(3) . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 117.2(2) . . ? C18 C19 C22 123.0(2) . . ? C20 C19 C22 119.84(19) . . ? C19 C20 H20 119.3 . . ? C21 C20 C19 121.4(2) . . ? C21 C20 H20 119.3 . . ? C16 C21 C20 120.2(3) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C12 C22 C23 109.92(17) . . ? C12 C22 C24 111.80(17) . . ? C19 C22 C12 108.25(18) . . ? C19 C22 C23 111.25(18) . . ? C19 C22 C24 107.82(18) . . ? C24 C22 C23 107.8(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 C14 128.66(19) . . ? N2 C25 H25 115.7 . . ? C14 C25 H25 115.7 . . ? N2 C26 H26 108.3 . . ? N2 C26 C27 112.82(15) . . ? N2 C26 C31 109.74(16) . . ? C27 C26 H26 108.3 . . ? C27 C26 C31 109.40(17) . . ? C31 C26 H26 108.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.0 . . ? C28 C27 C26 110.92(16) . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C27 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C29 C28 C27 110.20(19) . . ? C29 C28 H28A 109.6 . . ? C29 C28 H28B 109.6 . . ? C28 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C28 C29 C30 111.51(19) . . ? H29A C29 H29B 108.0 . . ? C30 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C29 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C29 C30 C31 111.73(17) . . ? H30A C30 H30B 107.9 . . ? C31 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? N1 C31 C26 108.24(16) . . ? N1 C31 C30 114.72(16) . . ? N1 C31 H31 107.8 . . ? C26 C31 H31 107.8 . . ? C30 C31 C26 110.30(18) . . ? C30 C31 H31 107.8 . . ? In1 C32 H32A 108.9 . . ? In1 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? C33 C32 In1 113.17(15) . . ? C33 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? C32 C33 H33 108.1 . . ? C34 C33 C32 110.5(2) . . ? C34 C33 H33 108.1 . . ? C34 C33 C35 109.8(2) . . ? C35 C33 C32 112.2(2) . . ? C35 C33 H33 108.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? In1 C36 H36A 106.2 . . ? In1 C36 H36B 106.2 . . ? H36A C36 H36B 106.4 . . ? C37 C36 In1 124.65(17) . . ? C37 C36 H36A 106.2 . . ? C37 C36 H36B 106.2 . . ? C36 C37 H37 107.0 . . ? C38 C37 C36 112.3(2) . . ? C38 C37 H37 107.0 . . ? C39 C37 C36 112.6(2) . . ? C39 C37 H37 107.0 . . ? C39 C37 C38 110.6(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N1 C40 H40A 109.2 . . ? N1 C40 H40B 109.2 . . ? N1 C40 C41 111.86(18) . . ? H40A C40 H40B 107.9 . . ? C41 C40 H40A 109.2 . . ? C41 C40 H40B 109.2 . . ? O2A C41 C40 124.9(4) . . ? O2A C41 C42A 121.3(5) . . ? O2B C41 C40 132.9(3) . . ? O2B C41 C42B 117.3(3) . . ? C42A C41 C40 113.8(5) . . ? C42B C41 C40 109.7(3) . . ? C41 C42A H42A 130.8 . . ? C41 C42A C43A 98.5(7) . . ? C43A C42A H42A 130.8 . . ? C41 C42B H42B 130.3 . . ? C41 C42B C43B 99.5(4) . . ? C43B C42B H42B 130.3 . . ? C42A C43A H43A 124.3 . . ? C44A C43A C42A 111.5(9) . . ? C44A C43A H43A 124.3 . . ? C42B C43B H43B 122.2 . . ? C44B C43B C42B 115.5(5) . . ? C44B C43B H43B 122.2 . . ? O2A C44A H44A 124.6 . . ? C43A C44A O2A 110.9(8) . . ? C43A C44A H44A 124.6 . . ? O2B C44B H44B 128.0 . . ? C43B C44B O2B 103.9(4) . . ? C43B C44B H44B 128.0 . . ? 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 In1 O1 2.2033(14) . ? In1 N1 2.5475(17) . ? In1 N2 2.2687(18) . ? In1 C32 2.178(2) . ? In1 C36 2.187(2) . ? O1 C15 1.295(2) . ? O2A C41 1.332(8) . ? O2A C44A 1.553(8) . ? O2B C41 1.323(5) . ? O2B C44B 1.536(6) . ? N1 H1 0.9800 . ? N1 C31 1.483(3) . ? N1 C40 1.479(3) . ? N2 C25 1.295(2) . ? N2 C26 1.482(2) . ? C1 H1A 0.9300 . ? C1 C2 1.378(4) . ? C1 C6 1.384(4) . ? C2 H2 0.9300 . ? C2 C3 1.389(3) . ? C3 H3 0.9300 . ? C3 C4 1.393(3) . ? C4 C5 1.387(3) . ? C4 C7 1.534(3) . ? C5 H5 0.9300 . ? C5 C6 1.395(3) . ? C6 H6 0.9300 . ? C7 C8 1.544(3) . ? C7 C9 1.541(3) . ? C7 C10 1.535(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.373(3) . ? C10 C15 1.444(3) . ? C11 H11 0.9300 . ? C11 C12 1.418(3) . ? C12 C13 1.368(3) . ? C12 C22 1.535(3) . ? C13 H13 0.9300 . ? C13 C14 1.417(3) . ? C14 C15 1.428(3) . ? C14 C25 1.434(3) . ? C16 H16 0.9300 . ? C16 C17 1.371(4) . ? C16 C21 1.378(4) . ? C17 H17 0.9300 . ? C17 C18 1.389(4) . ? C18 H18 0.9300 . ? C18 C19 1.388(3) . ? C19 C20 1.400(3) . ? C19 C22 1.533(3) . ? C20 H20 0.9300 . ? C20 C21 1.385(4) . ? C21 H21 0.9300 . ? C22 C23 1.540(3) . ? C22 C24 1.538(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9300 . ? C26 H26 0.9800 . ? C26 C27 1.531(3) . ? C26 C31 1.533(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.529(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.518(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.525(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.532(3) . ? C31 H31 0.9800 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C33 1.535(3) . ? C33 H33 0.9800 . ? C33 C34 1.521(4) . ? C33 C35 1.522(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 C37 1.532(3) . ? C37 H37 0.9800 . ? C37 C38 1.523(4) . ? C37 C39 1.513(4) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 C41 1.483(3) . ? C41 C42A 1.451(10) . ? C41 C42B 1.412(7) . ? C42A H42A 0.9300 . ? C42A C43A 1.465(10) . ? C42B H42B 0.9300 . ? C42B C43B 1.429(7) . ? C43A H43A 0.9300 . ? C43A C44A 1.335(10) . ? C43B H43B 0.9300 . ? C43B C44B 1.340(6) . ? C44A H44A 0.9300 . ? C44B H44B 0.9300 . ?