#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:50:52 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705222.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_7705222 loop_ _publ_author_name 'Boreen, Michael A.' 'Gro\&s, Oliver A.' 'Hohloch, Stephan' 'Arnold, John' _publ_section_title ; Isocyanide adducts of tri- and tetravalent uranium metallocenes supported by tetra(isopropyl)cyclopentadienyl ligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02005B _journal_year 2020 _chemical_formula_moiety 'C39 H67 I N U' _chemical_formula_sum 'C39 H67 I N U' _chemical_formula_weight 914.86 _chemical_name_systematic Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-(tert-butyl-isocyano)-iodo-uranium(iii) _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2020-04-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-05-28 deposited with the CCDC. 2020-08-11 downloaded from the CCDC. ; _cell_angle_alpha 100.465(5) _cell_angle_beta 96.791(5) _cell_angle_gamma 110.915(4) _cell_formula_units_Z 2 _cell_length_a 10.3988(9) _cell_length_b 11.2181(11) _cell_length_c 18.702(2) _cell_measurement_reflns_used 8074 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.42 _cell_measurement_theta_min 2.30 _cell_volume 1963.8(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution SHELXT-2014 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.366 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 20926 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 2.003 _diffrn_source 'microfocus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.943 _exptl_absorpt_correction_T_max 0.4901 _exptl_absorpt_correction_T_min 0.3401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.547 _exptl_crystal_description Plate _exptl_crystal_F_000 906 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.628 _refine_diff_density_min -2.862 _refine_diff_density_rms 0.220 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 7025 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0452 _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^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1108 _refine_ls_wR_factor_ref 0.1209 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5777 _reflns_number_total 7025 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02005b2.cif _cod_data_source_block mab_iii_194_0ma _cod_original_cell_volume 1963.8(4) _cod_database_code 7705222 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.790 _shelx_estimated_absorpt_t_min 0.360 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C20) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C21) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006 3.a Ternary CH refined with riding coordinates: C26(H26), C15(H15), C29(H29), C12(H12), C9(H9), C23(H23), C6(H6), C32(H32) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C18(H18) 3.c Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C28(H28A,H28B, H28C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C30(H30A, H30B,H30C), C38(H38A,H38B,H38C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C37(H37A,H37B, H37C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C34(H34A, H34B,H34C) ; _shelx_res_file ; mab_iii_194_0ma.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 0.71073 10.3988 11.2181 18.7019 100.465 96.791 110.915 ZERR 2 0.0009 0.0011 0.0023 0.005 0.005 0.004 LATT 1 SFAC C H I N U UNIT 78 134 2 2 2 ISOR 0.005 0.01 C20 C22 ISOR 0.003 0.006 C21 L.S. 10 PLAN 20 SIZE 0.05 0.18 0.26 TEMP -173(2) BOND $H LIST 4 more -1 fmap 2 acta MERG 2 SHEL 1000 0.83 REM REM REM WGHT 0.073100 FVAR 0.09924 U1 5 0.730808 0.302678 0.743452 11.00000 0.01679 0.01637 = 0.00855 0.00441 0.00808 0.00597 I1 3 0.941165 0.227501 0.835587 11.00000 0.01867 0.02651 = 0.01560 0.01017 0.00784 0.00989 N1 4 0.884769 0.651527 0.857258 11.00000 0.01891 0.02261 = 0.00544 0.00274 0.00438 0.01085 C26 1 0.884971 0.603503 0.645034 11.00000 0.01752 0.01499 = 0.01138 0.00498 0.00621 0.00657 AFIX 13 H26 2 0.972793 0.650088 0.683913 11.00000 -1.20000 AFIX 0 C31 1 1.131543 0.562293 0.774403 11.00000 0.01334 0.02443 = 0.01418 0.00604 0.00570 0.00604 AFIX 137 H31A 2 1.098704 0.632771 0.769697 11.00000 -1.50000 H31B 2 1.233517 0.600187 0.792434 11.00000 -1.50000 H31C 2 1.085442 0.515422 0.809614 11.00000 -1.50000 AFIX 0 C1 1 0.453433 0.235524 0.744128 11.00000 0.01524 0.01868 = 0.01395 0.00641 0.00562 0.00447 AFIX 43 H1 2 0.407877 0.258233 0.704786 11.00000 -1.20000 AFIX 0 C18 1 0.733726 0.234842 0.595488 11.00000 0.01950 0.01416 = 0.01259 0.00231 0.00781 0.00503 AFIX 43 H18 2 0.663572 0.150101 0.572572 11.00000 -1.20000 AFIX 0 C10 1 0.529291 0.289742 0.987508 11.00000 0.02631 0.02361 = 0.01388 0.00649 0.01289 0.00959 AFIX 137 H10A 2 0.509652 0.369009 0.987845 11.00000 -1.50000 H10B 2 0.566295 0.290242 1.038297 11.00000 -1.50000 H10C 2 0.442418 0.211663 0.967246 11.00000 -1.50000 AFIX 0 C19 1 0.714681 0.354517 0.597982 11.00000 0.01913 0.01548 = 0.00895 0.00176 0.00546 0.00035 C7 1 0.334815 0.391476 0.861032 11.00000 0.02650 0.03174 = 0.01679 0.00982 0.01675 0.01746 AFIX 137 H7A 2 0.268112 0.342919 0.814116 11.00000 -1.50000 H7B 2 0.314909 0.467714 0.882851 11.00000 -1.50000 H7C 2 0.325503 0.333877 0.895382 11.00000 -1.50000 AFIX 0 C4 1 0.543468 0.120488 0.808627 11.00000 0.01204 0.02265 = 0.02046 0.00784 0.00777 0.00355 C28 1 0.779002 0.662686 0.667324 11.00000 0.02501 0.02073 = 0.02278 0.00811 0.00851 0.01233 AFIX 137 H28A 2 0.695636 0.627872 0.627419 11.00000 -1.50000 H28B 2 0.822149 0.758603 0.675905 11.00000 -1.50000 H28C 2 0.751610 0.639345 0.712870 11.00000 -1.50000 AFIX 0 C14 1 0.590930 -0.095123 0.779270 11.00000 0.03147 0.02237 = 0.02559 0.00752 0.00958 0.01081 AFIX 137 H14A 2 0.629719 -0.147979 0.804304 11.00000 -1.50000 H14B 2 0.653622 -0.054846 0.747522 11.00000 -1.50000 H14C 2 0.498066 -0.151633 0.748823 11.00000 -1.50000 AFIX 0 C5 1 0.469670 0.114907 0.739009 11.00000 0.01873 0.01892 = 0.01303 0.00243 0.00714 0.00903 C20 1 0.843221 0.456791 0.639232 11.00000 0.01952 0.02119 = 0.00809 0.00373 0.00798 0.00682 C15 1 0.387350 -0.007752 0.674579 11.00000 0.01965 0.01337 = 0.02025 -0.00185 -0.00237 0.00423 AFIX 13 H15 2 0.444946 -0.062282 0.667913 11.00000 -1.20000 AFIX 0 C29 1 1.095334 0.465613 0.698108 11.00000 0.02154 0.01768 = 0.00966 0.00289 0.00921 0.00873 AFIX 13 H29 2 1.126016 0.393481 0.706518 11.00000 -1.20000 AFIX 0 C36 1 0.951012 0.785670 0.903732 11.00000 0.02366 0.02025 = 0.01546 0.00135 0.00648 0.00766 C24 1 0.553302 0.272995 0.472330 11.00000 0.02603 0.03046 = 0.01224 0.00050 0.00175 0.01036 AFIX 137 H24A 2 0.635235 0.283125 0.449269 11.00000 -1.50000 H24B 2 0.483226 0.289951 0.440435 11.00000 -1.50000 H24C 2 0.512453 0.183210 0.478790 11.00000 -1.50000 AFIX 0 C21 1 0.939330 0.399162 0.661969 11.00000 0.01306 0.01684 = 0.00887 0.00433 0.00736 0.00429 C12 1 0.577515 0.012431 0.837123 11.00000 0.02316 0.01365 = 0.02296 0.00766 0.00777 0.00794 AFIX 13 H12 2 0.670581 0.057513 0.872045 11.00000 -1.20000 AFIX 0 C3 1 0.573641 0.247419 0.856550 11.00000 0.01456 0.01554 = 0.01689 0.00410 0.00776 0.00469 C9 1 0.638701 0.287082 0.938927 11.00000 0.02858 0.02716 = 0.00818 0.00813 0.01227 0.00922 AFIX 13 H9 2 0.671835 0.217291 0.949182 11.00000 -1.20000 AFIX 0 C16 1 0.250414 -0.088614 0.695820 11.00000 0.04169 0.02486 = 0.03587 0.01312 0.00857 -0.00659 AFIX 137 H16A 2 0.194593 -0.035032 0.704463 11.00000 -1.50000 H16B 2 0.272335 -0.115756 0.741132 11.00000 -1.50000 H16C 2 0.196788 -0.166740 0.655441 11.00000 -1.50000 AFIX 0 C23 1 0.598986 0.371786 0.548742 11.00000 0.02207 0.02370 = 0.01096 0.00860 0.00780 0.01043 AFIX 13 H23 2 0.642664 0.460713 0.538795 11.00000 -1.20000 AFIX 0 C22 1 0.870438 0.258254 0.631490 11.00000 0.01907 0.01591 = 0.00762 0.00318 0.00915 0.00528 C2 1 0.513676 0.316546 0.815048 11.00000 0.01189 0.01554 = 0.01941 0.00700 0.00604 0.00296 C30 1 1.184184 0.532369 0.646331 11.00000 0.01826 0.03040 = 0.01732 0.00898 0.01037 0.01018 AFIX 137 H30A 2 1.159759 0.470951 0.597658 11.00000 -1.50000 H30B 2 1.283938 0.558589 0.667299 11.00000 -1.50000 H30C 2 1.165858 0.610399 0.640818 11.00000 -1.50000 AFIX 0 C38 1 0.849662 0.807376 0.952436 11.00000 0.04038 0.02274 = 0.02514 0.00143 0.01772 0.01086 AFIX 137 H38A 2 0.761585 0.795458 0.920921 11.00000 -1.50000 H38B 2 0.891788 0.896828 0.984243 11.00000 -1.50000 H38C 2 0.830535 0.743778 0.983418 11.00000 -1.50000 AFIX 0 C6 1 0.483876 0.437967 0.846655 11.00000 0.01801 0.02224 = 0.01743 0.00469 0.00264 0.00926 AFIX 13 H6 2 0.551284 0.487958 0.894680 11.00000 -1.20000 AFIX 0 C35 1 0.832449 0.545260 0.820822 11.00000 0.01384 0.03558 = 0.01730 0.01067 0.01031 0.01342 C8 1 0.495692 0.529438 0.794409 11.00000 0.02377 0.02188 = 0.01865 0.00749 0.01227 0.01043 AFIX 137 H8A 2 0.422092 0.484414 0.749653 11.00000 -1.50000 H8B 2 0.588068 0.553849 0.780637 11.00000 -1.50000 H8C 2 0.484510 0.608836 0.819361 11.00000 -1.50000 AFIX 0 C27 1 0.921480 0.637742 0.572575 11.00000 0.02443 0.02580 = 0.01424 0.00642 0.00365 0.00670 AFIX 137 H27A 2 0.985936 0.597607 0.556135 11.00000 -1.50000 H27B 2 0.966488 0.733449 0.580598 11.00000 -1.50000 H27C 2 0.835431 0.604129 0.534519 11.00000 -1.50000 AFIX 0 C32 1 0.936816 0.158105 0.630397 11.00000 0.02924 0.02348 = 0.01509 0.00530 0.01147 0.01714 AFIX 13 H32 2 1.000893 0.180188 0.679384 11.00000 -1.20000 AFIX 0 C39 1 1.087492 0.794647 0.950419 11.00000 0.03145 0.02830 = 0.02390 0.00352 0.00616 0.00918 AFIX 137 H39A 2 1.064757 0.736402 0.984318 11.00000 -1.50000 H39B 2 1.140627 0.885418 0.979167 11.00000 -1.50000 H39C 2 1.144162 0.767849 0.917556 11.00000 -1.50000 AFIX 0 C11 1 0.766990 0.419115 0.965340 11.00000 0.02754 0.02494 = 0.01057 0.00633 0.00524 0.01136 AFIX 137 H11A 2 0.839671 0.416759 0.936842 11.00000 -1.50000 H11B 2 0.804407 0.433480 1.018180 11.00000 -1.50000 H11C 2 0.738297 0.490888 0.957757 11.00000 -1.50000 AFIX 0 C25 1 0.472709 0.371778 0.580532 11.00000 0.02756 0.02712 = 0.01916 0.01465 0.01725 0.01244 AFIX 137 H25A 2 0.404522 0.281159 0.571767 11.00000 -1.50000 H25B 2 0.429506 0.422807 0.556524 11.00000 -1.50000 H25C 2 0.501824 0.411363 0.634016 11.00000 -1.50000 AFIX 0 C37 1 0.980121 0.880328 0.852458 11.00000 0.04019 0.02282 = 0.02290 0.00195 0.00719 0.00515 AFIX 137 H37A 2 1.029609 0.853153 0.815297 11.00000 -1.50000 H37B 2 1.038377 0.969639 0.881816 11.00000 -1.50000 H37C 2 0.890995 0.878734 0.827469 11.00000 -1.50000 AFIX 0 C17 1 0.351521 0.024115 0.601726 11.00000 0.03152 0.02276 = 0.01782 -0.00121 0.00760 0.00980 AFIX 137 H17A 2 0.297058 0.079491 0.607824 11.00000 -1.50000 H17B 2 0.295915 -0.057588 0.564116 11.00000 -1.50000 H17C 2 0.438313 0.071148 0.585903 11.00000 -1.50000 AFIX 0 C33 1 1.024211 0.163476 0.568897 11.00000 0.03326 0.03099 = 0.01818 0.00601 0.01659 0.01763 AFIX 137 H33A 2 0.962321 0.140666 0.520467 11.00000 -1.50000 H33B 2 1.069774 0.100733 0.569704 11.00000 -1.50000 H33C 2 1.095988 0.252437 0.577498 11.00000 -1.50000 AFIX 0 C13 1 0.470517 -0.050512 0.882887 11.00000 0.03692 0.02569 = 0.02294 0.01428 0.00764 0.00743 AFIX 137 H13A 2 0.375915 -0.089011 0.851944 11.00000 -1.50000 H13B 2 0.474528 0.016756 0.925618 11.00000 -1.50000 H13C 2 0.492749 -0.119494 0.900336 11.00000 -1.50000 AFIX 0 C34 1 0.827731 0.017483 0.616607 11.00000 0.03302 0.02121 = 0.02762 0.00713 0.01419 0.01063 AFIX 137 H34A 2 0.774293 0.011268 0.656528 11.00000 -1.50000 H34B 2 0.875574 -0.043714 0.615512 11.00000 -1.50000 H34C 2 0.763547 -0.005055 0.568962 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0452 for 5777 Fo > 4sig(Fo) and 0.0613 for all 7025 data REM 398 parameters refined using 18 restraints END WGHT 0.0731 0.0000 REM Highest difference peak 2.628, deepest hole -2.862, 1-sigma level 0.220 Q1 1 0.8220 0.3138 0.7807 11.00000 0.05 2.63 Q2 1 0.7019 0.2012 0.7339 11.00000 0.05 2.60 Q3 1 0.7674 0.3973 0.7558 11.00000 0.05 2.55 Q4 1 0.6596 0.3446 0.7278 11.00000 0.05 2.48 Q5 1 0.5206 0.3775 0.6553 11.00000 0.05 2.41 Q6 1 0.6465 0.2808 0.7084 11.00000 0.05 2.27 Q7 1 0.5925 0.1687 0.6811 11.00000 0.05 2.02 Q8 1 0.8518 0.2078 0.7955 11.00000 0.05 1.90 Q9 1 0.9186 0.1328 0.8279 11.00000 0.05 1.64 Q10 1 1.0154 0.2043 0.8506 11.00000 0.05 1.59 Q11 1 0.8102 0.0977 0.7712 11.00000 0.05 1.53 Q12 1 0.9210 0.3200 0.8220 11.00000 0.05 1.51 Q13 1 1.0406 0.2830 0.8727 11.00000 0.05 1.51 Q14 1 0.7520 0.4840 0.7765 11.00000 0.05 0.82 Q15 1 0.4550 0.3018 0.5997 11.00000 0.05 0.80 Q16 1 0.6227 0.1190 0.7413 11.00000 0.05 0.77 Q17 1 0.9590 0.5044 0.8426 11.00000 0.05 0.77 Q18 1 0.6148 0.4021 0.7040 11.00000 0.05 0.76 Q19 1 0.8798 0.3498 0.6444 11.00000 0.05 0.72 Q20 1 0.5541 0.3216 0.6971 11.00000 0.05 0.71 ; _shelx_res_checksum 36828 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 U1 U 0.73081(3) 0.30268(2) 0.74345(2) 0.01334(11) Uani 1 1 d . . . . . I1 I 0.94117(5) 0.22750(5) 0.83559(2) 0.01884(14) Uani 1 1 d . . . . . N1 N 0.8848(6) 0.6515(6) 0.8573(3) 0.0148(13) Uani 1 1 d . . . . . C26 C 0.8850(7) 0.6035(6) 0.6450(4) 0.0140(15) Uani 1 1 d . . . . . H26 H 0.9728 0.6501 0.6839 0.017 Uiso 1 1 calc R . . . . C31 C 1.1315(7) 0.5623(7) 0.7744(4) 0.0172(16) Uani 1 1 d . . . . . H31A H 1.0987 0.6328 0.7697 0.026 Uiso 1 1 calc GR . . . . H31B H 1.2335 0.6002 0.7924 0.026 Uiso 1 1 calc GR . . . . H31C H 1.0854 0.5154 0.8096 0.026 Uiso 1 1 calc GR . . . . C1 C 0.4534(7) 0.2355(7) 0.7441(4) 0.0160(16) Uani 1 1 d . . . . . H1 H 0.4079 0.2582 0.7048 0.019 Uiso 1 1 calc R . . . . C18 C 0.7337(7) 0.2348(7) 0.5955(4) 0.0156(15) Uani 1 1 d . . . . . H18 H 0.6636 0.1501 0.5726 0.019 Uiso 1 1 calc R . . . . C10 C 0.5293(8) 0.2897(7) 0.9875(4) 0.0202(17) Uani 1 1 d . . . . . H10A H 0.5097 0.3690 0.9878 0.030 Uiso 1 1 calc GR . . . . H10B H 0.5663 0.2902 1.0383 0.030 Uiso 1 1 calc GR . . . . H10C H 0.4424 0.2117 0.9672 0.030 Uiso 1 1 calc GR . . . . C19 C 0.7147(7) 0.3545(7) 0.5980(4) 0.0163(16) Uani 1 1 d . . . . . C7 C 0.3348(8) 0.3915(8) 0.8610(4) 0.0216(17) Uani 1 1 d . . . . . H7A H 0.2681 0.3429 0.8141 0.032 Uiso 1 1 calc GR . . . . H7B H 0.3149 0.4677 0.8829 0.032 Uiso 1 1 calc GR . . . . H7C H 0.3255 0.3339 0.8954 0.032 Uiso 1 1 calc GR . . . . C4 C 0.5435(7) 0.1205(7) 0.8086(4) 0.0185(16) Uani 1 1 d . . . . . C28 C 0.7790(8) 0.6627(7) 0.6673(4) 0.0211(17) Uani 1 1 d . . . . . H28A H 0.6956 0.6279 0.6274 0.032 Uiso 1 1 calc GR . . . . H28B H 0.8221 0.7586 0.6759 0.032 Uiso 1 1 calc GR . . . . H28C H 0.7516 0.6393 0.7129 0.032 Uiso 1 1 calc GR . . . . C14 C 0.5909(9) -0.0951(7) 0.7793(4) 0.0258(18) Uani 1 1 d . . . . . H14A H 0.6297 -0.1480 0.8043 0.039 Uiso 1 1 calc GR . . . . H14B H 0.6536 -0.0548 0.7475 0.039 Uiso 1 1 calc GR . . . . H14C H 0.4981 -0.1516 0.7488 0.039 Uiso 1 1 calc GR . . . . C5 C 0.4697(7) 0.1149(7) 0.7390(4) 0.0162(16) Uani 1 1 d . . . . . C20 C 0.8432(7) 0.4568(7) 0.6392(4) 0.0161(15) Uani 1 1 d . U . . . C15 C 0.3873(8) -0.0078(7) 0.6746(4) 0.0198(17) Uani 1 1 d . . . . . H15 H 0.4449 -0.0623 0.6679 0.024 Uiso 1 1 calc R . . . . C29 C 1.0953(7) 0.4656(7) 0.6981(4) 0.0155(15) Uani 1 1 d . . . . . H29 H 1.1260 0.3935 0.7065 0.019 Uiso 1 1 calc R . . . . C36 C 0.9510(8) 0.7857(7) 0.9037(4) 0.0202(17) Uani 1 1 d . . . . . C24 C 0.5533(8) 0.2730(8) 0.4723(4) 0.0239(18) Uani 1 1 d . . . . . H24A H 0.6352 0.2831 0.4493 0.036 Uiso 1 1 calc GR . . . . H24B H 0.4832 0.2900 0.4404 0.036 Uiso 1 1 calc GR . . . . H24C H 0.5125 0.1832 0.4788 0.036 Uiso 1 1 calc GR . . . . C21 C 0.9393(7) 0.3992(7) 0.6620(4) 0.0127(15) Uani 1 1 d . U . . . C12 C 0.5775(8) 0.0124(7) 0.8371(4) 0.0190(16) Uani 1 1 d . . . . . H12 H 0.6706 0.0575 0.8720 0.023 Uiso 1 1 calc R . . . . C3 C 0.5736(7) 0.2474(7) 0.8566(4) 0.0156(15) Uani 1 1 d . . . . . C9 C 0.6387(8) 0.2871(7) 0.9389(4) 0.0205(17) Uani 1 1 d . . . . . H9 H 0.6718 0.2173 0.9492 0.025 Uiso 1 1 calc R . . . . C16 C 0.2504(9) -0.0886(8) 0.6958(5) 0.039(2) Uani 1 1 d . . . . . H16A H 0.1946 -0.0350 0.7045 0.058 Uiso 1 1 calc GR . . . . H16B H 0.2723 -0.1158 0.7411 0.058 Uiso 1 1 calc GR . . . . H16C H 0.1968 -0.1667 0.6554 0.058 Uiso 1 1 calc GR . . . . C23 C 0.5990(8) 0.3718(7) 0.5487(4) 0.0174(16) Uani 1 1 d . . . . . H23 H 0.6427 0.4607 0.5388 0.021 Uiso 1 1 calc R . . . . C22 C 0.8704(7) 0.2583(7) 0.6315(4) 0.0140(15) Uani 1 1 d . U . . . C2 C 0.5137(7) 0.3165(7) 0.8150(4) 0.0156(16) Uani 1 1 d . . . . . C30 C 1.1842(8) 0.5324(8) 0.6463(4) 0.0207(17) Uani 1 1 d . . . . . H30A H 1.1598 0.4710 0.5977 0.031 Uiso 1 1 calc GR . . . . H30B H 1.2839 0.5586 0.6673 0.031 Uiso 1 1 calc GR . . . . H30C H 1.1659 0.6104 0.6408 0.031 Uiso 1 1 calc GR . . . . C38 C 0.8497(9) 0.8074(8) 0.9524(4) 0.0294(19) Uani 1 1 d . . . . . H38A H 0.7616 0.7955 0.9209 0.044 Uiso 1 1 calc GR . . . . H38B H 0.8918 0.8968 0.9842 0.044 Uiso 1 1 calc GR . . . . H38C H 0.8305 0.7438 0.9834 0.044 Uiso 1 1 calc GR . . . . C6 C 0.4839(8) 0.4380(7) 0.8467(4) 0.0189(16) Uani 1 1 d . . . . . H6 H 0.5513 0.4880 0.8947 0.023 Uiso 1 1 calc R . . . . C35 C 0.8324(7) 0.5453(8) 0.8208(4) 0.0199(17) Uani 1 1 d . . . . . C8 C 0.4957(8) 0.5294(7) 0.7944(4) 0.0199(16) Uani 1 1 d . . . . . H8A H 0.4221 0.4844 0.7497 0.030 Uiso 1 1 calc GR . . . . H8B H 0.5881 0.5538 0.7806 0.030 Uiso 1 1 calc GR . . . . H8C H 0.4845 0.6088 0.8194 0.030 Uiso 1 1 calc GR . . . . C27 C 0.9215(8) 0.6377(7) 0.5726(4) 0.0222(17) Uani 1 1 d . . . . . H27A H 0.9859 0.5976 0.5561 0.033 Uiso 1 1 calc GR . . . . H27B H 0.9665 0.7334 0.5806 0.033 Uiso 1 1 calc GR . . . . H27C H 0.8354 0.6041 0.5345 0.033 Uiso 1 1 calc GR . . . . C32 C 0.9368(8) 0.1581(7) 0.6304(4) 0.0199(17) Uani 1 1 d . . . . . H32 H 1.0009 0.1802 0.6794 0.024 Uiso 1 1 calc R . . . . C39 C 1.0875(8) 0.7946(8) 0.9504(4) 0.0289(19) Uani 1 1 d . . . . . H39A H 1.0648 0.7364 0.9843 0.043 Uiso 1 1 calc GR . . . . H39B H 1.1406 0.8854 0.9792 0.043 Uiso 1 1 calc GR . . . . H39C H 1.1442 0.7678 0.9176 0.043 Uiso 1 1 calc GR . . . . C11 C 0.7670(8) 0.4191(7) 0.9653(4) 0.0203(17) Uani 1 1 d . . . . . H11A H 0.8397 0.4168 0.9368 0.030 Uiso 1 1 calc GR . . . . H11B H 0.8044 0.4335 1.0182 0.030 Uiso 1 1 calc GR . . . . H11C H 0.7383 0.4909 0.9578 0.030 Uiso 1 1 calc GR . . . . C25 C 0.4727(8) 0.3718(7) 0.5805(4) 0.0217(17) Uani 1 1 d . . . . . H25A H 0.4045 0.2812 0.5718 0.033 Uiso 1 1 calc GR . . . . H25B H 0.4295 0.4228 0.5565 0.033 Uiso 1 1 calc GR . . . . H25C H 0.5018 0.4114 0.6340 0.033 Uiso 1 1 calc GR . . . . C37 C 0.9801(9) 0.8803(7) 0.8525(4) 0.031(2) Uani 1 1 d . . . . . H37A H 1.0296 0.8532 0.8153 0.047 Uiso 1 1 calc GR . . . . H37B H 1.0384 0.9696 0.8818 0.047 Uiso 1 1 calc GR . . . . H37C H 0.8910 0.8787 0.8275 0.047 Uiso 1 1 calc GR . . . . C17 C 0.3515(8) 0.0241(7) 0.6017(4) 0.0248(18) Uani 1 1 d . . . . . H17A H 0.2971 0.0795 0.6078 0.037 Uiso 1 1 calc GR . . . . H17B H 0.2959 -0.0576 0.5641 0.037 Uiso 1 1 calc GR . . . . H17C H 0.4383 0.0711 0.5859 0.037 Uiso 1 1 calc GR . . . . C33 C 1.0242(9) 0.1635(8) 0.5689(4) 0.0250(18) Uani 1 1 d . . . . . H33A H 0.9623 0.1407 0.5205 0.037 Uiso 1 1 calc GR . . . . H33B H 1.0698 0.1007 0.5697 0.037 Uiso 1 1 calc GR . . . . H33C H 1.0960 0.2524 0.5775 0.037 Uiso 1 1 calc GR . . . . C13 C 0.4705(9) -0.0505(8) 0.8829(4) 0.0286(19) Uani 1 1 d . . . . . H13A H 0.3759 -0.0890 0.8519 0.043 Uiso 1 1 calc GR . . . . H13B H 0.4745 0.0168 0.9256 0.043 Uiso 1 1 calc GR . . . . H13C H 0.4927 -0.1195 0.9003 0.043 Uiso 1 1 calc GR . . . . C34 C 0.8277(8) 0.0175(7) 0.6166(4) 0.0263(18) Uani 1 1 d . . . . . H34A H 0.7743 0.0113 0.6565 0.040 Uiso 1 1 calc GR . . . . H34B H 0.8756 -0.0437 0.6155 0.040 Uiso 1 1 calc GR . . . . H34C H 0.7635 -0.0051 0.5690 0.040 Uiso 1 1 calc GR . . . . 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 U1 0.01679(17) 0.01637(16) 0.00855(15) 0.00441(10) 0.00808(11) 0.00597(12) I1 0.0187(3) 0.0265(3) 0.0156(3) 0.0102(2) 0.0078(2) 0.0099(2) N1 0.019(3) 0.023(3) 0.005(3) 0.003(3) 0.004(3) 0.011(3) C26 0.018(4) 0.015(4) 0.011(4) 0.005(3) 0.006(3) 0.007(3) C31 0.013(4) 0.024(4) 0.014(4) 0.006(3) 0.006(3) 0.006(3) C1 0.015(4) 0.019(4) 0.014(4) 0.006(3) 0.006(3) 0.004(3) C18 0.020(4) 0.014(4) 0.013(4) 0.002(3) 0.008(3) 0.005(3) C10 0.026(4) 0.024(4) 0.014(4) 0.006(3) 0.013(3) 0.010(4) C19 0.019(4) 0.015(4) 0.009(3) 0.002(3) 0.005(3) 0.000(3) C7 0.026(4) 0.032(4) 0.017(4) 0.010(3) 0.017(3) 0.017(4) C4 0.012(4) 0.023(4) 0.020(4) 0.008(3) 0.008(3) 0.004(3) C28 0.025(4) 0.021(4) 0.023(4) 0.008(3) 0.009(3) 0.012(3) C14 0.031(5) 0.022(4) 0.026(4) 0.008(3) 0.010(4) 0.011(4) C5 0.019(4) 0.019(4) 0.013(4) 0.002(3) 0.007(3) 0.009(3) C20 0.020(3) 0.021(3) 0.008(3) 0.004(2) 0.008(3) 0.007(3) C15 0.020(4) 0.013(4) 0.020(4) -0.002(3) -0.002(3) 0.004(3) C29 0.022(4) 0.018(4) 0.010(4) 0.003(3) 0.009(3) 0.009(3) C36 0.024(4) 0.020(4) 0.015(4) 0.001(3) 0.006(3) 0.008(3) C24 0.026(4) 0.030(4) 0.012(4) 0.000(3) 0.002(3) 0.010(4) C21 0.013(3) 0.017(2) 0.009(2) 0.004(2) 0.007(2) 0.004(2) C12 0.023(4) 0.014(4) 0.023(4) 0.008(3) 0.008(3) 0.008(3) C3 0.015(4) 0.016(4) 0.017(4) 0.004(3) 0.008(3) 0.005(3) C9 0.029(4) 0.027(4) 0.008(4) 0.008(3) 0.012(3) 0.009(4) C16 0.042(6) 0.025(5) 0.036(5) 0.013(4) 0.009(4) -0.007(4) C23 0.022(4) 0.024(4) 0.011(4) 0.009(3) 0.008(3) 0.010(3) C22 0.019(3) 0.016(3) 0.008(3) 0.003(2) 0.009(3) 0.005(3) C2 0.012(4) 0.016(4) 0.019(4) 0.007(3) 0.006(3) 0.003(3) C30 0.018(4) 0.030(4) 0.017(4) 0.009(3) 0.010(3) 0.010(3) C38 0.040(5) 0.023(4) 0.025(4) 0.001(3) 0.018(4) 0.011(4) C6 0.018(4) 0.022(4) 0.017(4) 0.005(3) 0.003(3) 0.009(3) C35 0.014(4) 0.036(5) 0.017(4) 0.011(4) 0.010(3) 0.013(4) C8 0.024(4) 0.022(4) 0.019(4) 0.007(3) 0.012(3) 0.010(3) C27 0.024(4) 0.026(4) 0.014(4) 0.006(3) 0.004(3) 0.007(4) C32 0.029(4) 0.023(4) 0.015(4) 0.005(3) 0.011(3) 0.017(4) C39 0.031(5) 0.028(4) 0.024(4) 0.004(3) 0.006(4) 0.009(4) C11 0.028(4) 0.025(4) 0.011(4) 0.006(3) 0.005(3) 0.011(4) C25 0.028(4) 0.027(4) 0.019(4) 0.015(3) 0.017(3) 0.012(4) C37 0.040(5) 0.023(4) 0.023(4) 0.002(3) 0.007(4) 0.005(4) C17 0.032(5) 0.023(4) 0.018(4) -0.001(3) 0.008(4) 0.010(4) C33 0.033(5) 0.031(4) 0.018(4) 0.006(3) 0.017(4) 0.018(4) C13 0.037(5) 0.026(4) 0.023(4) 0.014(3) 0.008(4) 0.007(4) C34 0.033(5) 0.021(4) 0.028(5) 0.007(3) 0.014(4) 0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' U U -9.6767 9.6646 '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 C1 U1 I1 127.90(14) . . ? C1 U1 C18 102.8(2) . . ? C1 U1 C19 95.4(2) . . ? C1 U1 C4 48.2(2) . . ? C1 U1 C5 29.9(2) . . ? C1 U1 C20 116.7(2) . . ? C1 U1 C21 143.5(2) . . ? C1 U1 C3 48.2(2) . . ? C1 U1 C22 131.6(2) . . ? C1 U1 C2 29.2(2) . . ? C18 U1 I1 110.41(15) . . ? C18 U1 C19 29.1(2) . . ? C18 U1 C4 119.9(2) . . ? C18 U1 C5 97.0(2) . . ? C18 U1 C20 47.4(2) . . ? C18 U1 C21 48.7(2) . . ? C18 U1 C3 145.5(2) . . ? C18 U1 C22 29.7(2) . . ? C18 U1 C2 130.7(2) . . ? C19 U1 I1 131.94(15) . . ? C19 U1 C20 28.53(19) . . ? C4 U1 I1 80.23(14) . . ? C4 U1 C19 133.5(2) . . ? C4 U1 C20 161.7(2) . . ? C4 U1 C3 29.4(2) . . ? C5 U1 I1 105.46(14) . . ? C5 U1 C19 104.7(2) . . ? C5 U1 C4 29.1(2) . . ? C5 U1 C20 132.6(2) . . ? C5 U1 C21 145.5(2) . . ? C5 U1 C3 48.5(2) . . ? C5 U1 C2 48.9(2) . . ? C20 U1 I1 115.39(14) . . ? C21 U1 I1 87.39(14) . . ? C21 U1 C19 48.29(19) . . ? C21 U1 C4 158.4(2) . . ? C21 U1 C20 28.97(19) . . ? C21 U1 C3 165.7(2) . . ? C3 U1 I1 84.16(14) . . ? C3 U1 C19 143.0(2) . . ? C3 U1 C20 153.1(2) . . ? C22 U1 I1 83.92(14) . . ? C22 U1 C19 48.8(2) . . ? C22 U1 C4 129.7(2) . . ? C22 U1 C5 118.0(2) . . ? C22 U1 C20 48.3(2) . . ? C22 U1 C21 30.2(2) . . ? C22 U1 C3 158.0(2) . . ? C22 U1 C2 160.3(2) . . ? C2 U1 I1 112.59(14) . . ? C2 U1 C19 115.5(2) . . ? C2 U1 C4 48.4(2) . . ? C2 U1 C20 125.5(2) . . ? C2 U1 C21 152.8(2) . . ? C2 U1 C3 29.34(19) . . ? C35 U1 I1 93.71(15) . . ? C35 U1 C1 100.7(2) . . ? C35 U1 C18 122.9(2) . . ? C35 U1 C19 97.9(2) . . ? C35 U1 C4 114.6(2) . . ? C35 U1 C5 126.0(2) . . ? C35 U1 C20 75.6(2) . . ? C35 U1 C21 83.7(2) . . ? C35 U1 C3 85.3(2) . . ? C35 U1 C22 113.8(2) . . ? C35 U1 C2 77.1(2) . . ? C35 N1 C36 179.7(7) . . ? C28 C26 H26 106.8 . . ? C20 C26 H26 106.8 . . ? C20 C26 C28 116.9(6) . . ? C20 C26 C27 110.9(6) . . ? C27 C26 H26 106.8 . . ? C27 C26 C28 108.1(6) . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? U1 C1 H1 111.6 . . ? C5 C1 U1 77.0(4) . . ? C5 C1 H1 124.8 . . ? C2 C1 U1 78.7(4) . . ? C2 C1 H1 124.8 . . ? C2 C1 C5 110.3(6) . . ? U1 C18 H18 110.8 . . ? C19 C18 U1 81.0(4) . . ? C19 C18 H18 124.5 . . ? C22 C18 U1 75.8(4) . . ? C22 C18 H18 124.5 . . ? C22 C18 C19 111.1(6) . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? C18 C19 U1 69.9(4) . . ? C18 C19 C20 106.2(6) . . ? C18 C19 C23 125.6(6) . . ? C20 C19 U1 76.9(4) . . ? C20 C19 C23 126.1(6) . . ? C23 C19 U1 131.0(5) . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? C5 C4 U1 72.2(4) . . ? C5 C4 C12 129.8(7) . . ? C5 C4 C3 107.8(6) . . ? C12 C4 U1 123.1(5) . . ? C3 C4 U1 75.4(4) . . ? C3 C4 C12 122.0(6) . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C1 C5 U1 73.1(4) . . ? C1 C5 C15 123.3(6) . . ? C4 C5 U1 78.7(4) . . ? C4 C5 C1 107.3(6) . . ? C4 C5 C15 127.8(6) . . ? C15 C5 U1 125.3(5) . . ? C26 C20 U1 129.5(5) . . ? C19 C20 U1 74.6(4) . . ? C19 C20 C26 126.0(6) . . ? C19 C20 C21 108.9(6) . . ? C21 C20 U1 71.6(4) . . ? C21 C20 C26 123.9(6) . . ? C5 C15 H15 108.6 . . ? C16 C15 C5 108.4(7) . . ? C16 C15 H15 108.6 . . ? C17 C15 C5 113.8(6) . . ? C17 C15 H15 108.6 . . ? C17 C15 C16 108.6(6) . . ? C31 C29 H29 106.2 . . ? C21 C29 C31 115.8(6) . . ? C21 C29 H29 106.2 . . ? C30 C29 C31 109.8(6) . . ? C30 C29 H29 106.2 . . ? C30 C29 C21 112.0(6) . . ? N1 C36 C38 107.9(6) . . ? N1 C36 C39 106.3(6) . . ? N1 C36 C37 108.0(6) . . ? C38 C36 C39 111.5(6) . . ? C38 C36 C37 111.2(6) . . ? C37 C36 C39 111.7(7) . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? C20 C21 U1 79.4(4) . . ? C20 C21 C29 129.5(6) . . ? C20 C21 C22 107.4(6) . . ? C29 C21 U1 122.1(4) . . ? C22 C21 U1 72.8(4) . . ? C22 C21 C29 122.2(6) . . ? C4 C12 H12 106.6 . . ? C14 C12 C4 116.9(6) . . ? C14 C12 H12 106.6 . . ? C14 C12 C13 109.5(6) . . ? C13 C12 C4 110.2(6) . . ? C13 C12 H12 106.6 . . ? C4 C3 U1 75.2(4) . . ? C4 C3 C9 124.2(6) . . ? C9 C3 U1 123.9(5) . . ? C2 C3 U1 73.3(4) . . ? C2 C3 C4 107.3(6) . . ? C2 C3 C9 128.0(6) . . ? C10 C9 H9 106.8 . . ? C10 C9 C11 108.6(6) . . ? C3 C9 C10 111.7(6) . . ? C3 C9 H9 106.8 . . ? C3 C9 C11 115.6(6) . . ? C11 C9 H9 106.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C23 C24 111.0(6) . . ? C19 C23 H23 105.7 . . ? C24 C23 H23 105.7 . . ? C25 C23 C19 117.2(6) . . ? C25 C23 C24 110.5(6) . . ? C25 C23 H23 105.7 . . ? C18 C22 U1 74.5(4) . . ? C18 C22 C21 106.3(6) . . ? C18 C22 C32 126.4(6) . . ? C21 C22 U1 77.0(4) . . ? C21 C22 C32 126.9(6) . . ? C32 C22 U1 119.5(4) . . ? C1 C2 U1 72.1(4) . . ? C1 C2 C3 107.3(6) . . ? C1 C2 C6 124.3(6) . . ? C3 C2 U1 77.4(4) . . ? C3 C2 C6 126.5(6) . . ? C6 C2 U1 128.7(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C7 C6 C2 108.3(6) . . ? C7 C6 H6 109.0 . . ? C7 C6 C8 108.1(6) . . ? C2 C6 H6 109.0 . . ? C8 C6 C2 113.2(6) . . ? C8 C6 H6 109.0 . . ? N1 C35 U1 175.6(6) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C32 H32 108.7 . . ? C22 C32 C33 109.9(6) . . ? C22 C32 C34 112.5(6) . . ? C33 C32 H32 108.7 . . ? C34 C32 H32 108.7 . . ? C34 C32 C33 108.4(6) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 U1 I1 3.0690(5) . ? U1 C1 2.711(7) . ? U1 C18 2.740(7) . ? U1 C19 2.882(7) . ? U1 C4 2.843(7) . ? U1 C5 2.760(7) . ? U1 C20 2.911(7) . ? U1 C21 2.811(7) . ? U1 C3 2.846(7) . ? U1 C22 2.756(7) . ? U1 C2 2.794(7) . ? U1 C35 2.602(8) . ? N1 C36 1.462(9) . ? N1 C35 1.156(9) . ? C26 H26 1.0000 . ? C26 C28 1.536(10) . ? C26 C20 1.524(9) . ? C26 C27 1.528(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C31 C29 1.541(9) . ? C1 H1 0.9500 . ? C1 C5 1.410(10) . ? C1 C2 1.392(10) . ? C18 H18 0.9500 . ? C18 C19 1.419(10) . ? C18 C22 1.409(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 C9 1.543(10) . ? C19 C20 1.428(10) . ? C19 C23 1.517(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 C6 1.523(10) . ? C4 C5 1.410(10) . ? C4 C12 1.541(10) . ? C4 C3 1.442(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 C12 1.526(10) . ? C5 C15 1.546(9) . ? C20 C21 1.435(10) . ? C15 H15 1.0000 . ? C15 C16 1.533(11) . ? C15 C17 1.508(10) . ? C29 H29 1.0000 . ? C29 C21 1.529(10) . ? C29 C30 1.527(10) . ? C36 C38 1.526(11) . ? C36 C39 1.536(11) . ? C36 C37 1.532(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 C23 1.544(10) . ? C21 C22 1.451(9) . ? C12 H12 1.0000 . ? C12 C13 1.534(11) . ? C3 C9 1.523(10) . ? C3 C2 1.429(9) . ? C9 H9 1.0000 . ? C9 C11 1.544(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C23 H23 1.0000 . ? C23 C25 1.504(10) . ? C22 C32 1.513(10) . ? C2 C6 1.534(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C6 H6 1.0000 . ? C6 C8 1.525(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C32 H32 1.0000 . ? C32 C33 1.545(10) . ? C32 C34 1.532(10) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ?