#------------------------------------------------------------------------------ #$Date: 2015-10-09 16:07:17 +0300 (Fri, 09 Oct 2015) $ #$Revision: 162082 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/48/7054809.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_7054809 loop_ _publ_author_name 'Kahan, Rachel J.' 'Cloke, F. Geoffrey N.' 'Roe, S. Mark' 'Nief, Fran\,cois' _publ_section_title ; Activation of carbon dioxide by new mixed sandwich uranium(iii) complexes incorporating cyclooctatetraenyl and pyrrolide, phospholide, or arsolide ligands ; _journal_issue 10 _journal_name_full 'New J. Chem.' _journal_page_first 7602 _journal_paper_doi 10.1039/C5NJ00590F _journal_volume 39 _journal_year 2015 _chemical_formula_moiety '0.5(C68 H120 N2 Si4 U2)' _chemical_formula_sum 'C34 H60 N Si2 U' _chemical_formula_weight 777.04 _chemical_name_systematic ; 1 ; _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2b' _space_group_name_H-M_alt 'P b c 21' _symmetry_space_group_name_Hall 'P 2c -2b' _symmetry_space_group_name_H-M 'P b c 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-03-02 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2015-04-16 deposited with the CCDC. 2015-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.54240(10) _cell_length_b 22.7691(3) _cell_length_c 24.9695(2) _cell_measurement_reflns_used 11478 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 61.0560 _cell_measurement_theta_min 3.9570 _cell_volume 7130.77(12) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies Version 1.171.37.31 ; _computing_data_collection ; CrysAlisPro, Agilent Technologies Version 1.171.37.31 ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies Version 1.171.37.31 ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXL (Sheldrick, 2008)' _diffrn_ambient_temperature 173.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.0403 _diffrn_reflns_laue_measured_fraction_full 1.000 _diffrn_reflns_laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 96143 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 1.624 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time 0 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.641 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.52799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_crystal_colour 'dark purple' _exptl_crystal_density_diffrn 1.448 _exptl_crystal_description needle _exptl_crystal_F_000 3128 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: pentane' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.869 _refine_diff_density_min -1.895 _refine_diff_density_rms 0.414 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.267(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 686 _refine_ls_number_reflns 15976 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.223 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0334 _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^)+(0.0524P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.0982 _reflns_Friedel_coverage 0.954 _reflns_friedel_fraction_full 1.000 _reflns_friedel_fraction_max 0.999 _reflns_number_gt 14154 _reflns_number_total 15976 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL import in P222 CELL 0.71073 12.5424 22.7691 24.9695 90 90 90 ZERR 8 0.0001 0.0003 0.0002 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM -X,0.5+Y,+Z SYMM +X,0.5-Y,0.5+Z SFAC C H N O Si U UNIT 272 480 8 0 16 8 L.S. 20 PLAN 5 SIZE 0.1 0.12 0.18 TEMP -100 BOND $H fmap 2 acta MORE -1 CONF MERG 2 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.052400 BASF 0.26741 FVAR 0.12081 U1 6 0.140535 0.725853 0.279490 11.00000 0.02165 0.02676 = 0.02282 0.00158 -0.00142 -0.00129 U51 6 -0.183390 0.732619 0.220340 11.00000 0.02074 0.02710 = 0.02146 -0.00066 -0.00044 0.00060 SI1 5 0.198949 0.849706 0.417329 11.00000 0.04091 0.02724 = 0.03580 -0.00471 -0.00906 0.00155 SI6 5 -0.229571 0.848528 0.071470 11.00000 0.04236 0.03049 = 0.02889 0.00617 -0.00692 -0.00072 C51 1 -0.122817 0.782012 0.317400 11.00000 0.03255 0.02583 = 0.02098 -0.00707 -0.00101 -0.00358 C3 1 0.189706 0.765770 0.170936 11.00000 0.03530 0.03818 = 0.02750 0.00682 0.00056 -0.00539 SI2 5 0.253827 0.558594 0.355631 11.00000 0.03125 0.02819 = 0.03022 0.00272 -0.00314 0.00256 SI3 5 -0.324523 0.568857 0.152871 11.00000 0.03022 0.02898 = 0.03276 -0.00470 -0.00169 0.00005 C10 1 0.173748 0.733509 0.386923 11.00000 0.03949 0.02956 = 0.02609 0.00238 -0.00583 -0.00040 AFIX 43 H10 2 0.131068 0.738983 0.417955 11.00000 -1.20000 AFIX 0 C23 1 0.309015 0.834928 0.468098 11.00000 0.04763 0.03903 = 0.04260 -0.01320 -0.01441 0.00351 AFIX 13 H23 2 0.306563 0.867484 0.494952 11.00000 -1.20000 AFIX 0 N1 3 0.017488 0.738693 0.192537 11.00000 0.02089 0.03281 = 0.02135 0.00379 -0.00049 -0.00399 N51 3 -0.058335 0.732488 0.307975 11.00000 0.02747 0.03496 = 0.02164 -0.00192 -0.00473 -0.00293 C14 1 0.351166 0.708676 0.274191 11.00000 0.00917 0.04591 = 0.03752 -0.00135 -0.00014 0.00095 AFIX 43 H14 2 0.400137 0.702411 0.245734 11.00000 -1.20000 AFIX 0 C82 1 -0.356704 0.838239 0.029399 11.00000 0.05114 0.05097 = 0.04494 0.01384 -0.02174 -0.00859 AFIX 13 H82 2 -0.354111 0.868511 0.000412 11.00000 -1.20000 AFIX 0 C26 1 0.221894 0.503157 0.300906 11.00000 0.05675 0.03152 = 0.04372 -0.00369 -0.00497 0.00163 AFIX 13 H26 2 0.227103 0.463787 0.318461 11.00000 -1.20000 AFIX 0 C62 1 -0.243917 0.794148 0.128140 11.00000 0.02522 0.03185 = 0.03304 0.00670 -0.00101 0.00245 C27 1 0.105680 0.507956 0.281024 11.00000 0.06013 0.03945 = 0.04982 0.00078 -0.01661 0.00671 AFIX 33 H27A 2 0.057405 0.509514 0.311852 11.00000 -1.50000 H27B 2 0.097479 0.543752 0.259623 11.00000 -1.50000 H27C 2 0.088379 0.473649 0.258974 11.00000 -1.50000 AFIX 0 C25 1 0.295814 0.778059 0.498653 11.00000 0.06140 0.06709 = 0.05119 -0.00494 -0.02527 0.00714 AFIX 33 H25A 2 0.225119 0.777070 0.515343 11.00000 -1.50000 H25B 2 0.303026 0.744842 0.473959 11.00000 -1.50000 H25C 2 0.350742 0.775406 0.526462 11.00000 -1.50000 AFIX 0 C60 1 -0.236280 0.677601 0.129822 11.00000 0.02750 0.03215 = 0.02753 -0.00555 -0.00239 0.00380 AFIX 43 H60 2 -0.195352 0.649576 0.110540 11.00000 -1.20000 AFIX 0 C2 1 0.179259 0.701886 0.166136 11.00000 0.03146 0.05029 = 0.02360 0.00616 0.00013 -0.00367 C72 1 -0.135770 0.509089 0.193059 11.00000 0.04310 0.03755 = 0.03636 0.00164 -0.00124 0.00345 AFIX 33 H72A 2 -0.127140 0.543342 0.216426 11.00000 -1.50000 H72B 2 -0.176914 0.478823 0.211810 11.00000 -1.50000 H72C 2 -0.065456 0.493443 0.183604 11.00000 -1.50000 AFIX 0 C54 1 -0.124139 0.684246 0.318421 11.00000 0.03129 0.03161 = 0.02016 -0.00076 -0.00320 -0.00148 C5 1 0.025015 0.630166 0.172744 11.00000 0.04409 0.03646 = 0.03865 -0.00019 -0.00010 -0.00054 AFIX 33 H5A 2 -0.049241 0.632665 0.184743 11.00000 -1.50000 H5B 2 0.026959 0.618198 0.135057 11.00000 -1.50000 H5C 2 0.063151 0.601169 0.194522 11.00000 -1.50000 AFIX 0 C1 1 0.076794 0.688445 0.178670 11.00000 0.03427 0.03114 = 0.01894 0.00346 -0.00008 0.00005 C53 1 -0.226749 0.702479 0.333635 11.00000 0.02919 0.04530 = 0.02448 -0.00070 0.00337 -0.01121 C83 1 -0.364185 0.779550 0.001942 11.00000 0.08752 0.06278 = 0.08188 0.00402 -0.05270 -0.01017 AFIX 33 H83A 2 -0.298470 0.772184 -0.018199 11.00000 -1.50000 H83B 2 -0.373921 0.748648 0.028820 11.00000 -1.50000 H83C 2 -0.425038 0.779599 -0.022677 11.00000 -1.50000 AFIX 0 C15 1 0.340133 0.767601 0.286100 11.00000 0.01892 0.04220 = 0.03885 0.01407 -0.00308 -0.01508 AFIX 43 H15 2 0.383947 0.791515 0.264018 11.00000 -1.20000 AFIX 0 C13 1 0.308561 0.655631 0.293358 11.00000 0.02485 0.04127 = 0.02680 0.00257 -0.00367 0.00493 AFIX 43 H13 2 0.332107 0.622923 0.272910 11.00000 -1.20000 AFIX 0 C61 1 -0.214426 0.735301 0.111745 11.00000 0.02378 0.03713 = 0.02312 -0.00459 -0.00401 0.00123 AFIX 43 H61 2 -0.169118 0.735477 0.081257 11.00000 -1.20000 AFIX 0 C71 1 -0.206249 0.472228 0.106902 11.00000 0.06619 0.05190 = 0.04893 -0.01715 -0.01033 0.02548 AFIX 33 H71A 2 -0.243838 0.482181 0.073712 11.00000 -1.50000 H71B 2 -0.135260 0.456937 0.098273 11.00000 -1.50000 H71C 2 -0.246717 0.442318 0.126479 11.00000 -1.50000 AFIX 0 C22 1 0.239628 0.972977 0.423020 11.00000 0.07126 0.04230 = 0.07253 -0.00199 -0.00372 -0.00422 AFIX 33 H22A 2 0.289799 0.961834 0.451340 11.00000 -1.50000 H22B 2 0.266278 1.007911 0.404407 11.00000 -1.50000 H22C 2 0.169896 0.981607 0.438882 11.00000 -1.50000 AFIX 0 C11 1 0.181768 0.673684 0.373716 11.00000 0.02575 0.03179 = 0.02453 0.00459 -0.00143 -0.00451 AFIX 43 H11 2 0.137253 0.650378 0.395984 11.00000 -1.20000 AFIX 0 C70 1 -0.195182 0.527413 0.141720 11.00000 0.03348 0.03206 = 0.02822 -0.00032 0.00151 0.00357 AFIX 13 H70 2 -0.146628 0.554691 0.121963 11.00000 -1.20000 AFIX 0 C58 1 -0.080256 0.622945 0.318799 11.00000 0.04249 0.03319 = 0.03375 -0.00242 -0.01094 0.00035 AFIX 33 H58A 2 -0.137683 0.595108 0.326795 11.00000 -1.50000 H58B 2 -0.049761 0.613886 0.283621 11.00000 -1.50000 H58C 2 -0.024662 0.619802 0.346228 11.00000 -1.50000 AFIX 0 C31 1 0.199223 0.568805 0.468344 11.00000 0.05588 0.06505 = 0.03464 0.01078 0.00150 -0.00008 AFIX 33 H31A 2 0.210517 0.611009 0.463136 11.00000 -1.50000 H31B 2 0.144419 0.562692 0.495758 11.00000 -1.50000 H31C 2 0.266047 0.550465 0.479920 11.00000 -1.50000 AFIX 0 C67 1 -0.404270 0.566235 0.087802 11.00000 0.04588 0.03332 = 0.05606 -0.01653 -0.01865 0.01069 AFIX 13 H67 2 -0.420057 0.523979 0.080301 11.00000 -1.20000 AFIX 0 C80 1 -0.138416 0.948901 0.126967 11.00000 0.06056 0.04216 = 0.08538 -0.02178 -0.01390 0.00336 AFIX 33 H80A 2 -0.118601 0.919379 0.153737 11.00000 -1.50000 H80B 2 -0.079175 0.954547 0.101899 11.00000 -1.50000 H80C 2 -0.154352 0.986153 0.144923 11.00000 -1.50000 AFIX 0 C59 1 -0.302828 0.649248 0.169091 11.00000 0.02297 0.03703 = 0.02674 -0.00241 0.00185 -0.00018 C55 1 -0.074752 0.842849 0.315765 11.00000 0.05634 0.02722 = 0.04406 -0.00622 -0.00080 -0.00468 AFIX 33 H55A 2 -0.000518 0.840316 0.303738 11.00000 -1.50000 H55B 2 -0.115398 0.867441 0.290852 11.00000 -1.50000 H55C 2 -0.077170 0.860240 0.351646 11.00000 -1.50000 AFIX 0 C21 1 0.151926 0.938973 0.339582 11.00000 0.04944 0.04312 = 0.06589 0.01775 -0.00642 -0.00690 AFIX 33 H21A 2 0.146324 0.905885 0.314639 11.00000 -1.50000 H21B 2 0.081611 0.947372 0.354887 11.00000 -1.50000 H21C 2 0.177992 0.973676 0.320412 11.00000 -1.50000 AFIX 0 C24 1 0.416177 0.836826 0.442606 11.00000 0.04880 0.07038 = 0.06495 -0.00997 -0.02520 -0.00538 AFIX 33 H24A 2 0.424247 0.873766 0.422875 11.00000 -1.50000 H24B 2 0.471292 0.834264 0.470328 11.00000 -1.50000 H24C 2 0.423577 0.803700 0.417825 11.00000 -1.50000 AFIX 0 C63 1 -0.303073 0.814671 0.172553 11.00000 0.03699 0.02374 = 0.03804 -0.00507 -0.00718 0.00146 AFIX 43 H63 2 -0.297695 0.856094 0.176214 11.00000 -1.20000 AFIX 0 C19 1 0.077389 0.884830 0.510277 11.00000 0.06567 0.07986 = 0.04738 -0.01445 -0.00450 0.01347 AFIX 33 H19A 2 0.129554 0.916874 0.510279 11.00000 -1.50000 H19B 2 0.008092 0.899790 0.522223 11.00000 -1.50000 H19C 2 0.101287 0.853754 0.534634 11.00000 -1.50000 AFIX 0 C12 1 0.238408 0.638234 0.336033 11.00000 0.03039 0.02805 = 0.02415 0.00311 -0.00235 0.00032 C77 1 -0.000437 0.825917 0.054254 11.00000 0.04705 0.05195 = 0.03721 0.00687 0.00329 0.00067 AFIX 33 H77A 2 -0.005211 0.800022 0.085512 11.00000 -1.50000 H77B 2 0.051068 0.809759 0.028681 11.00000 -1.50000 H77C 2 0.022954 0.865029 0.065671 11.00000 -1.50000 AFIX 0 C32 1 0.401946 0.550847 0.372210 11.00000 0.03362 0.04870 = 0.05093 0.00862 0.00020 0.00141 AFIX 13 H32 2 0.439494 0.557496 0.337405 11.00000 -1.20000 AFIX 0 C75 1 -0.363150 0.526755 0.261312 11.00000 0.06767 0.06547 = 0.05335 0.01356 0.02005 0.00639 AFIX 33 H75A 2 -0.339913 0.565704 0.273261 11.00000 -1.50000 H75B 2 -0.417334 0.511607 0.285986 11.00000 -1.50000 H75C 2 -0.301930 0.500018 0.260772 11.00000 -1.50000 AFIX 0 C69 1 -0.343946 0.590950 0.037937 11.00000 0.08023 0.05390 = 0.02534 -0.01039 -0.01627 0.01151 AFIX 33 H69A 2 -0.275040 0.571042 0.034353 11.00000 -1.50000 H69B 2 -0.386651 0.584102 0.005668 11.00000 -1.50000 H69C 2 -0.332297 0.633215 0.042501 11.00000 -1.50000 AFIX 0 C78 1 -0.101469 0.872172 -0.022589 11.00000 0.05344 0.08402 = 0.04051 0.02523 0.00766 -0.00305 AFIX 33 H78A 2 -0.171137 0.875510 -0.040096 11.00000 -1.50000 H78B 2 -0.077735 0.911129 -0.010914 11.00000 -1.50000 H78C 2 -0.049621 0.855860 -0.047904 11.00000 -1.50000 AFIX 0 C34 1 0.435834 0.489477 0.389629 11.00000 0.04743 0.05468 = 0.08969 0.02221 -0.00646 0.01253 AFIX 33 H34A 2 0.405746 0.460375 0.364977 11.00000 -1.50000 H34B 2 0.513803 0.486730 0.389144 11.00000 -1.50000 H34C 2 0.409745 0.481863 0.425967 11.00000 -1.50000 AFIX 0 C79 1 -0.235611 0.928306 0.096697 11.00000 0.07562 0.02918 = 0.03983 -0.00095 -0.00016 0.00438 AFIX 13 H79 2 -0.294586 0.928694 0.123645 11.00000 -1.20000 AFIX 0 C29 1 0.162445 0.540803 0.415056 11.00000 0.03793 0.03806 = 0.03290 0.01017 -0.00185 -0.00178 AFIX 13 H29 2 0.090988 0.557914 0.406565 11.00000 -1.20000 AFIX 0 C9 1 0.211710 0.788487 0.366828 11.00000 0.03340 0.02850 = 0.03185 0.00297 -0.01559 -0.00102 C30 1 0.145456 0.474852 0.424473 11.00000 0.05853 0.04727 = 0.06017 0.01995 0.00258 -0.00933 AFIX 33 H30A 2 0.122066 0.456281 0.391072 11.00000 -1.50000 H30B 2 0.212540 0.456968 0.436261 11.00000 -1.50000 H30C 2 0.090912 0.469195 0.452098 11.00000 -1.50000 AFIX 0 C6 1 0.263084 0.661954 0.145167 11.00000 0.03454 0.06361 = 0.03583 -0.00533 0.00765 0.00880 AFIX 33 H6A 2 0.329316 0.684041 0.139884 11.00000 -1.50000 H6B 2 0.275438 0.630151 0.170875 11.00000 -1.50000 H6C 2 0.239805 0.645322 0.110908 11.00000 -1.50000 AFIX 0 C33 1 0.447831 0.597041 0.410004 11.00000 0.04066 0.07270 = 0.05085 0.00078 -0.00987 -0.00921 AFIX 33 H33A 2 0.425324 0.636193 0.398259 11.00000 -1.50000 H33B 2 0.421790 0.589866 0.446426 11.00000 -1.50000 H33C 2 0.525849 0.594733 0.409603 11.00000 -1.50000 AFIX 0 C7 1 0.280538 0.803338 0.155484 11.00000 0.04452 0.07183 = 0.04988 0.02353 0.00889 -0.01863 AFIX 33 H7A 2 0.341684 0.778594 0.146105 11.00000 -1.50000 H7B 2 0.260580 0.827432 0.124546 11.00000 -1.50000 H7C 2 0.299662 0.828931 0.185542 11.00000 -1.50000 AFIX 0 C28 1 0.298888 0.500657 0.253141 11.00000 0.06476 0.07146 = 0.07308 -0.04068 0.01618 -0.00367 AFIX 33 H28A 2 0.372303 0.497619 0.266287 11.00000 -1.50000 H28B 2 0.282198 0.466327 0.231002 11.00000 -1.50000 H28C 2 0.291298 0.536430 0.231652 11.00000 -1.50000 AFIX 0 C73 1 -0.410490 0.531350 0.204886 11.00000 0.04617 0.03300 = 0.05380 -0.00766 0.00738 -0.00331 AFIX 13 H73 2 -0.476858 0.555415 0.208198 11.00000 -1.20000 AFIX 0 C18 1 -0.016232 0.808998 0.453766 11.00000 0.05575 0.05644 = 0.05872 -0.00655 0.01412 0.00193 AFIX 33 H18A 2 -0.025585 0.791700 0.418135 11.00000 -1.50000 H18B 2 0.008715 0.778763 0.478730 11.00000 -1.50000 H18C 2 -0.084480 0.824799 0.466318 11.00000 -1.50000 AFIX 0 C8 1 0.054241 0.848214 0.192919 11.00000 0.05845 0.03843 = 0.04389 0.00939 -0.01213 -0.00140 AFIX 33 H8A 2 0.115779 0.874056 0.187478 11.00000 -1.50000 H8B 2 -0.000689 0.857258 0.166253 11.00000 -1.50000 H8C 2 0.025306 0.854348 0.228944 11.00000 -1.50000 AFIX 0 C20 1 0.228813 0.923524 0.384016 11.00000 0.04582 0.03077 = 0.05736 0.00538 -0.00547 -0.00529 AFIX 13 H20 2 0.300217 0.919143 0.366652 11.00000 -1.20000 AFIX 0 C76 1 -0.110943 0.830553 0.027303 11.00000 0.04494 0.04263 = 0.03506 0.00054 -0.00331 -0.00246 AFIX 13 H76 2 -0.125762 0.790625 0.012375 11.00000 -1.20000 AFIX 0 C68 1 -0.511755 0.597905 0.092708 11.00000 0.04405 0.06467 = 0.08827 -0.02058 -0.01815 0.00010 AFIX 33 H68A 2 -0.550440 0.582773 0.123892 11.00000 -1.50000 H68B 2 -0.499575 0.640146 0.097100 11.00000 -1.50000 H68C 2 -0.553929 0.591033 0.060268 11.00000 -1.50000 AFIX 0 C17 1 0.066307 0.858741 0.450808 11.00000 0.05382 0.04588 = 0.04542 -0.01234 -0.00735 0.01171 AFIX 13 H17 2 0.030035 0.890519 0.430018 11.00000 -1.20000 AFIX 0 C74 1 -0.446164 0.469178 0.187450 11.00000 0.08052 0.03208 = 0.12595 -0.01493 0.04405 -0.01942 AFIX 33 H74A 2 -0.476795 0.470996 0.151382 11.00000 -1.50000 H74B 2 -0.384445 0.442784 0.187355 11.00000 -1.50000 H74C 2 -0.499849 0.454373 0.212569 11.00000 -1.50000 AFIX 0 C4 1 0.088622 0.785052 0.186884 11.00000 0.02990 0.03958 = 0.02312 0.00820 -0.00443 -0.00450 C81 1 -0.268136 0.973162 0.054957 11.00000 0.10655 0.04720 = 0.07673 0.00807 -0.01486 0.01026 AFIX 33 H81A 2 -0.331269 0.959053 0.035742 11.00000 -1.50000 H81B 2 -0.284677 1.010526 0.072578 11.00000 -1.50000 H81C 2 -0.209499 0.978920 0.029554 11.00000 -1.50000 AFIX 0 C65 1 -0.397535 0.731223 0.226103 11.00000 0.03000 0.02805 = 0.03348 -0.00427 -0.00310 0.00165 AFIX 43 H65 2 -0.449299 0.730298 0.253865 11.00000 -1.20000 AFIX 0 C64 1 -0.368468 0.789882 0.213207 11.00000 0.02591 0.03867 = 0.03496 -0.01011 0.00217 0.00770 AFIX 43 H64 2 -0.398927 0.818304 0.236483 11.00000 -1.20000 AFIX 0 C66 1 -0.371042 0.674479 0.209245 11.00000 0.02211 0.03328 = 0.03595 -0.00557 -0.00072 -0.00009 AFIX 43 H66 2 -0.407243 0.645250 0.229407 11.00000 -1.20000 AFIX 0 C57 1 -0.318500 0.664624 0.352897 11.00000 0.03836 0.06173 = 0.03210 0.00532 0.00181 -0.00971 AFIX 33 H57A 2 -0.380308 0.689562 0.360604 11.00000 -1.50000 H57B 2 -0.337241 0.636122 0.325036 11.00000 -1.50000 H57C 2 -0.297258 0.643720 0.385504 11.00000 -1.50000 AFIX 0 C56 1 -0.313344 0.805693 0.350483 11.00000 0.04469 0.05258 = 0.03716 -0.01220 0.00736 0.01623 AFIX 33 H56A 2 -0.376742 0.781949 0.358064 11.00000 -1.50000 H56B 2 -0.291387 0.826421 0.383063 11.00000 -1.50000 H56C 2 -0.329904 0.834330 0.322389 11.00000 -1.50000 AFIX 0 C52 1 -0.224580 0.766482 0.332016 11.00000 0.03386 0.03976 = 0.02426 -0.00455 0.00225 0.01107 C16 1 0.280334 0.801168 0.322710 11.00000 0.03612 0.03145 = 0.03335 0.00248 -0.00678 -0.01033 AFIX 43 H16 2 0.287351 0.842162 0.316567 11.00000 -1.20000 AFIX 0 C84 1 -0.459140 0.849157 0.060511 11.00000 0.03812 0.12480 = 0.06194 0.02076 -0.01798 -0.01010 AFIX 33 H84A 2 -0.454900 0.887325 0.078525 11.00000 -1.50000 H84B 2 -0.519801 0.849063 0.035774 11.00000 -1.50000 H84C 2 -0.468683 0.818113 0.087270 11.00000 -1.50000 AFIX 0 HKLF 4 REM import in P222 REM R1 = 0.0334 for 14154 Fo > 4sig(Fo) and 0.0468 for all 15976 data REM 686 parameters refined using 1 restraints END WGHT 0.0525 0.0000 REM Highest difference peak 0.869, deepest hole -1.895, 1-sigma level 0.414 Q1 1 -0.4380 0.5198 0.2497 11.00000 0.05 0.87 Q2 1 -0.3334 0.4695 0.2178 11.00000 0.05 0.86 Q3 1 0.4574 0.4854 0.2975 11.00000 0.05 0.84 Q4 1 -0.4787 0.4810 0.3221 11.00000 0.05 0.82 Q5 1 0.4759 0.4995 0.2503 11.00000 0.05 0.80 REM The information below was added by Olex2. REM REM R1 = 0.0334 for 14154 Fo > 4sig(Fo) and 0.0468 for all 100028 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.87, deepest hole -1.89 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0468 REM R1_gt = 0.0334 REM wR_ref = 0.0982 REM GOOF = 1.223 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 100028 REM Reflections_gt = 14154 REM Parameters = n/a REM Hole = -1.89 REM Peak = 0.87 REM Flack = n/a ; _cod_data_source_file c5nj00590f2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7054809--7054814.cif.' _cod_database_code 7054809 _shelxl_version_number 2014-3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.654 _shelx_estimated_absorpt_t_min 0.489 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.733(7) 0.267(7) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3.a Ternary CH refined with riding coordinates: C23(H23), C82(H82), C26(H26), C70(H70), C67(H67), C32(H32), C79(H79), C29(H29), C73(H73), C20(H20), C76(H76), C17(H17) 3.b Me refined with riding coordinates: C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C72(H72A,H72B,H72C), C5(H5A,H5B, H5C), C83(H83A,H83B,H83C), C71(H71A,H71B,H71C), C22(H22A,H22B,H22C), C58(H58A, H58B,H58C), C31(H31A,H31B,H31C), C80(H80A,H80B,H80C), C55(H55A,H55B,H55C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C77(H77A,H77B, H77C), C75(H75A,H75B,H75C), C69(H69A,H69B,H69C), C78(H78A,H78B,H78C), C34(H34A, H34B,H34C), C30(H30A,H30B,H30C), C6(H6A,H6B,H6C), C33(H33A,H33B,H33C), C7(H7A, H7B,H7C), C28(H28A,H28B,H28C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C68(H68A, H68B,H68C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C), C84(H84A,H84B,H84C) 3.c Aromatic/amide H refined with riding coordinates: C10(H10), C14(H14), C60(H60), C15(H15), C13(H13), C61(H61), C11(H11), C63(H63), C65(H65), C64(H64), C66(H66), C16(H16) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, 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 U1 U 0.14054(3) 0.72585(2) 0.27949(2) 0.02374(9) Uani 1 1 d . U51 U -0.18339(3) 0.73262(2) 0.22034(2) 0.02310(9) Uani 1 1 d . Si1 Si 0.1989(2) 0.84971(12) 0.41733(11) 0.0346(6) Uani 1 1 d . Si6 Si -0.2296(2) 0.84853(12) 0.07147(11) 0.0339(6) Uani 1 1 d . C51 C -0.1228(8) 0.7820(4) 0.3174(4) 0.026(2) Uani 1 1 d . C3 C 0.1897(9) 0.7658(5) 0.1709(4) 0.034(3) Uani 1 1 d . Si2 Si 0.2538(2) 0.55859(11) 0.35563(10) 0.0299(6) Uani 1 1 d . Si3 Si -0.3245(2) 0.56886(12) 0.15287(11) 0.0307(6) Uani 1 1 d . C10 C 0.1737(10) 0.7335(4) 0.3869(4) 0.032(2) Uani 1 1 d . H10 H 0.1311 0.7390 0.4180 0.038 Uiso 1 1 calc R C23 C 0.3090(9) 0.8349(5) 0.4681(5) 0.043(3) Uani 1 1 d . H23 H 0.3066 0.8675 0.4950 0.052 Uiso 1 1 calc R N1 N 0.0175(6) 0.7387(3) 0.1925(3) 0.0250(17) Uani 1 1 d . N51 N -0.0583(7) 0.7325(3) 0.3080(3) 0.0280(18) Uani 1 1 d . C14 C 0.3512(6) 0.7087(4) 0.2742(5) 0.031(2) Uani 1 1 d . H14 H 0.4001 0.7024 0.2457 0.037 Uiso 1 1 calc R C82 C -0.3567(9) 0.8382(5) 0.0294(5) 0.049(3) Uani 1 1 d . H82 H -0.3541 0.8685 0.0004 0.059 Uiso 1 1 calc R C26 C 0.2219(10) 0.5032(5) 0.3009(4) 0.044(3) Uani 1 1 d . H26 H 0.2271 0.4638 0.3185 0.053 Uiso 1 1 calc R C62 C -0.2439(8) 0.7941(4) 0.1281(4) 0.030(2) Uani 1 1 d . C27 C 0.1057(9) 0.5080(4) 0.2810(5) 0.050(3) Uani 1 1 d . H27A H 0.0574 0.5095 0.3119 0.075 Uiso 1 1 calc R H27B H 0.0975 0.5438 0.2596 0.075 Uiso 1 1 calc R H27C H 0.0884 0.4736 0.2590 0.075 Uiso 1 1 calc R C25 C 0.2958(13) 0.7781(6) 0.4987(6) 0.060(4) Uani 1 1 d . H25A H 0.2251 0.7771 0.5153 0.090 Uiso 1 1 calc R H25B H 0.3030 0.7448 0.4740 0.090 Uiso 1 1 calc R H25C H 0.3507 0.7754 0.5265 0.090 Uiso 1 1 calc R C60 C -0.2363(8) 0.6776(4) 0.1298(4) 0.029(2) Uani 1 1 d . H60 H -0.1954 0.6496 0.1105 0.035 Uiso 1 1 calc R C2 C 0.1793(8) 0.7019(5) 0.1661(4) 0.035(2) Uani 1 1 d . C72 C -0.1358(9) 0.5091(4) 0.1931(4) 0.039(2) Uani 1 1 d . H72A H -0.1271 0.5433 0.2164 0.059 Uiso 1 1 calc R H72B H -0.1769 0.4788 0.2118 0.059 Uiso 1 1 calc R H72C H -0.0655 0.4934 0.1836 0.059 Uiso 1 1 calc R C54 C -0.1241(8) 0.6842(4) 0.3184(4) 0.028(2) Uani 1 1 d . C5 C 0.0250(9) 0.6302(4) 0.1727(4) 0.040(2) Uani 1 1 d . H5A H -0.0492 0.6327 0.1847 0.060 Uiso 1 1 calc R H5B H 0.0270 0.6182 0.1351 0.060 Uiso 1 1 calc R H5C H 0.0632 0.6012 0.1945 0.060 Uiso 1 1 calc R C1 C 0.0768(8) 0.6884(4) 0.1787(3) 0.028(2) Uani 1 1 d . C53 C -0.2267(8) 0.7025(5) 0.3336(4) 0.033(2) Uani 1 1 d . C83 C -0.3642(14) 0.7796(6) 0.0019(7) 0.077(5) Uani 1 1 d . H83A H -0.2985 0.7722 -0.0182 0.116 Uiso 1 1 calc R H83B H -0.3739 0.7486 0.0288 0.116 Uiso 1 1 calc R H83C H -0.4250 0.7796 -0.0227 0.116 Uiso 1 1 calc R C15 C 0.3401(8) 0.7676(4) 0.2861(5) 0.033(2) Uani 1 1 d . H15 H 0.3839 0.7915 0.2640 0.040 Uiso 1 1 calc R C13 C 0.3086(7) 0.6556(5) 0.2934(4) 0.031(2) Uani 1 1 d . H13 H 0.3321 0.6229 0.2729 0.037 Uiso 1 1 calc R C61 C -0.2144(9) 0.7353(4) 0.1117(4) 0.028(2) Uani 1 1 d . H61 H -0.1691 0.7355 0.0813 0.034 Uiso 1 1 calc R C71 C -0.2062(11) 0.4722(5) 0.1069(5) 0.056(3) Uani 1 1 d . H71A H -0.2438 0.4822 0.0737 0.084 Uiso 1 1 calc R H71B H -0.1353 0.4569 0.0983 0.084 Uiso 1 1 calc R H71C H -0.2467 0.4423 0.1265 0.084 Uiso 1 1 calc R C22 C 0.2396(12) 0.9730(5) 0.4230(5) 0.062(3) Uani 1 1 d . H22A H 0.2898 0.9618 0.4513 0.093 Uiso 1 1 calc R H22B H 0.2663 1.0079 0.4044 0.093 Uiso 1 1 calc R H22C H 0.1699 0.9816 0.4389 0.093 Uiso 1 1 calc R C11 C 0.1818(8) 0.6737(4) 0.3737(4) 0.027(2) Uani 1 1 d . H11 H 0.1373 0.6504 0.3960 0.033 Uiso 1 1 calc R C70 C -0.1952(8) 0.5274(4) 0.1417(4) 0.031(2) Uani 1 1 d . H70 H -0.1466 0.5547 0.1220 0.038 Uiso 1 1 calc R C58 C -0.0803(9) 0.6229(4) 0.3188(4) 0.036(2) Uani 1 1 d . H58A H -0.1377 0.5951 0.3268 0.055 Uiso 1 1 calc R H58B H -0.0498 0.6139 0.2836 0.055 Uiso 1 1 calc R H58C H -0.0247 0.6198 0.3462 0.055 Uiso 1 1 calc R C31 C 0.1992(10) 0.5688(6) 0.4683(5) 0.052(3) Uani 1 1 d . H31A H 0.2105 0.6110 0.4631 0.078 Uiso 1 1 calc R H31B H 0.1444 0.5627 0.4958 0.078 Uiso 1 1 calc R H31C H 0.2660 0.5505 0.4799 0.078 Uiso 1 1 calc R C67 C -0.4043(9) 0.5662(5) 0.0878(4) 0.045(3) Uani 1 1 d . H67 H -0.4201 0.5240 0.0803 0.054 Uiso 1 1 calc R C80 C -0.1384(11) 0.9489(6) 0.1270(6) 0.063(4) Uani 1 1 d . H80A H -0.1186 0.9194 0.1537 0.094 Uiso 1 1 calc R H80B H -0.0792 0.9545 0.1019 0.094 Uiso 1 1 calc R H80C H -0.1544 0.9862 0.1449 0.094 Uiso 1 1 calc R C59 C -0.3028(7) 0.6492(4) 0.1691(4) 0.029(2) Uani 1 1 d . C55 C -0.0748(10) 0.8428(4) 0.3158(4) 0.043(3) Uani 1 1 d . H55A H -0.0005 0.8403 0.3037 0.064 Uiso 1 1 calc R H55B H -0.1154 0.8674 0.2909 0.064 Uiso 1 1 calc R H55C H -0.0772 0.8602 0.3516 0.064 Uiso 1 1 calc R C21 C 0.1519(10) 0.9390(5) 0.3396(5) 0.053(3) Uani 1 1 d . H21A H 0.1463 0.9059 0.3146 0.079 Uiso 1 1 calc R H21B H 0.0816 0.9474 0.3549 0.079 Uiso 1 1 calc R H21C H 0.1780 0.9737 0.3204 0.079 Uiso 1 1 calc R C24 C 0.4162(10) 0.8368(6) 0.4426(5) 0.061(4) Uani 1 1 d . H24A H 0.4242 0.8738 0.4229 0.092 Uiso 1 1 calc R H24B H 0.4713 0.8343 0.4703 0.092 Uiso 1 1 calc R H24C H 0.4236 0.8037 0.4178 0.092 Uiso 1 1 calc R C63 C -0.3031(8) 0.8147(4) 0.1726(4) 0.033(2) Uani 1 1 d . H63 H -0.2977 0.8561 0.1762 0.040 Uiso 1 1 calc R C19 C 0.0774(11) 0.8848(6) 0.5103(5) 0.064(4) Uani 1 1 d . H19A H 0.1296 0.9169 0.5103 0.096 Uiso 1 1 calc R H19B H 0.0081 0.8998 0.5222 0.096 Uiso 1 1 calc R H19C H 0.1013 0.8538 0.5346 0.096 Uiso 1 1 calc R C12 C 0.2384(7) 0.6382(4) 0.3360(4) 0.0275(19) Uani 1 1 d . C77 C -0.0004(9) 0.8259(5) 0.0543(4) 0.045(3) Uani 1 1 d . H77A H -0.0052 0.8000 0.0855 0.068 Uiso 1 1 calc R H77B H 0.0511 0.8098 0.0287 0.068 Uiso 1 1 calc R H77C H 0.0230 0.8650 0.0657 0.068 Uiso 1 1 calc R C32 C 0.4019(9) 0.5508(5) 0.3722(5) 0.044(3) Uani 1 1 d . H32 H 0.4395 0.5575 0.3374 0.053 Uiso 1 1 calc R C75 C -0.3631(11) 0.5268(6) 0.2613(5) 0.062(4) Uani 1 1 d . H75A H -0.3399 0.5657 0.2733 0.093 Uiso 1 1 calc R H75B H -0.4173 0.5116 0.2860 0.093 Uiso 1 1 calc R H75C H -0.3019 0.5000 0.2608 0.093 Uiso 1 1 calc R C69 C -0.3439(11) 0.5910(5) 0.0379(4) 0.053(3) Uani 1 1 d . H69A H -0.2750 0.5710 0.0344 0.080 Uiso 1 1 calc R H69B H -0.3867 0.5841 0.0057 0.080 Uiso 1 1 calc R H69C H -0.3323 0.6332 0.0425 0.080 Uiso 1 1 calc R C78 C -0.1015(10) 0.8722(6) -0.0226(5) 0.059(3) Uani 1 1 d . H78A H -0.1711 0.8755 -0.0401 0.089 Uiso 1 1 calc R H78B H -0.0777 0.9111 -0.0109 0.089 Uiso 1 1 calc R H78C H -0.0496 0.8559 -0.0479 0.089 Uiso 1 1 calc R C34 C 0.4358(11) 0.4895(5) 0.3896(6) 0.064(4) Uani 1 1 d . H34A H 0.4057 0.4604 0.3650 0.096 Uiso 1 1 calc R H34B H 0.5138 0.4867 0.3891 0.096 Uiso 1 1 calc R H34C H 0.4097 0.4819 0.4260 0.096 Uiso 1 1 calc R C79 C -0.2356(11) 0.9283(4) 0.0967(4) 0.048(3) Uani 1 1 d . H79 H -0.2946 0.9287 0.1236 0.058 Uiso 1 1 calc R C29 C 0.1624(8) 0.5408(5) 0.4151(4) 0.036(2) Uani 1 1 d . H29 H 0.0910 0.5579 0.4066 0.044 Uiso 1 1 calc R C9 C 0.2117(8) 0.7885(4) 0.3668(4) 0.031(2) Uani 1 1 d . C30 C 0.1455(10) 0.4749(5) 0.4245(5) 0.055(3) Uani 1 1 d . H30A H 0.1221 0.4563 0.3911 0.083 Uiso 1 1 calc R H30B H 0.2125 0.4570 0.4363 0.083 Uiso 1 1 calc R H30C H 0.0909 0.4692 0.4521 0.083 Uiso 1 1 calc R C6 C 0.2631(9) 0.6620(5) 0.1452(4) 0.045(3) Uani 1 1 d . H6A H 0.3293 0.6840 0.1399 0.067 Uiso 1 1 calc R H6B H 0.2754 0.6302 0.1709 0.067 Uiso 1 1 calc R H6C H 0.2398 0.6453 0.1109 0.067 Uiso 1 1 calc R C33 C 0.4478(10) 0.5970(6) 0.4100(5) 0.055(3) Uani 1 1 d . H33A H 0.4253 0.6362 0.3983 0.082 Uiso 1 1 calc R H33B H 0.4218 0.5899 0.4464 0.082 Uiso 1 1 calc R H33C H 0.5258 0.5947 0.4096 0.082 Uiso 1 1 calc R C7 C 0.2805(10) 0.8033(6) 0.1555(5) 0.055(3) Uani 1 1 d . H7A H 0.3417 0.7786 0.1461 0.083 Uiso 1 1 calc R H7B H 0.2606 0.8274 0.1245 0.083 Uiso 1 1 calc R H7C H 0.2997 0.8289 0.1855 0.083 Uiso 1 1 calc R C28 C 0.2989(11) 0.5007(6) 0.2531(6) 0.070(4) Uani 1 1 d . H28A H 0.3723 0.4976 0.2663 0.105 Uiso 1 1 calc R H28B H 0.2822 0.4663 0.2310 0.105 Uiso 1 1 calc R H28C H 0.2913 0.5364 0.2317 0.105 Uiso 1 1 calc R C73 C -0.4105(9) 0.5314(4) 0.2049(4) 0.044(3) Uani 1 1 d . H73 H -0.4769 0.5554 0.2082 0.053 Uiso 1 1 calc R C18 C -0.0162(10) 0.8090(5) 0.4538(5) 0.057(3) Uani 1 1 d . H18A H -0.0256 0.7917 0.4181 0.085 Uiso 1 1 calc R H18B H 0.0087 0.7788 0.4787 0.085 Uiso 1 1 calc R H18C H -0.0845 0.8248 0.4663 0.085 Uiso 1 1 calc R C8 C 0.0542(10) 0.8482(5) 0.1929(4) 0.047(3) Uani 1 1 d . H8A H 0.1158 0.8741 0.1875 0.070 Uiso 1 1 calc R H8B H -0.0007 0.8573 0.1663 0.070 Uiso 1 1 calc R H8C H 0.0253 0.8543 0.2289 0.070 Uiso 1 1 calc R C20 C 0.2288(10) 0.9235(4) 0.3840(5) 0.045(3) Uani 1 1 d . H20 H 0.3002 0.9191 0.3667 0.054 Uiso 1 1 calc R C76 C -0.1109(9) 0.8306(5) 0.0273(4) 0.041(2) Uani 1 1 d . H76 H -0.1258 0.7906 0.0124 0.049 Uiso 1 1 calc R C68 C -0.5118(10) 0.5979(6) 0.0927(6) 0.066(4) Uani 1 1 d . H68A H -0.5504 0.5828 0.1239 0.098 Uiso 1 1 calc R H68B H -0.4996 0.6401 0.0971 0.098 Uiso 1 1 calc R H68C H -0.5539 0.5910 0.0603 0.098 Uiso 1 1 calc R C17 C 0.0663(10) 0.8587(5) 0.4508(4) 0.048(3) Uani 1 1 d . H17 H 0.0300 0.8905 0.4300 0.058 Uiso 1 1 calc R C74 C -0.4462(13) 0.4692(5) 0.1875(7) 0.080(5) Uani 1 1 d . H74A H -0.4768 0.4710 0.1514 0.119 Uiso 1 1 calc R H74B H -0.3844 0.4428 0.1874 0.119 Uiso 1 1 calc R H74C H -0.4998 0.4544 0.2126 0.119 Uiso 1 1 calc R C4 C 0.0886(9) 0.7851(4) 0.1869(4) 0.031(2) Uani 1 1 d . C81 C -0.2681(14) 0.9732(6) 0.0550(6) 0.077(4) Uani 1 1 d . H81A H -0.3313 0.9591 0.0357 0.115 Uiso 1 1 calc R H81B H -0.2847 1.0105 0.0726 0.115 Uiso 1 1 calc R H81C H -0.2095 0.9789 0.0296 0.115 Uiso 1 1 calc R C65 C -0.3975(8) 0.7312(3) 0.2261(5) 0.031(2) Uani 1 1 d . H65 H -0.4493 0.7303 0.2539 0.037 Uiso 1 1 calc R C64 C -0.3685(7) 0.7899(5) 0.2132(5) 0.033(2) Uani 1 1 d . H64 H -0.3989 0.8183 0.2365 0.040 Uiso 1 1 calc R C66 C -0.3710(7) 0.6745(4) 0.2092(4) 0.030(2) Uani 1 1 d . H66 H -0.4072 0.6453 0.2294 0.037 Uiso 1 1 calc R C57 C -0.3185(9) 0.6646(6) 0.3529(4) 0.044(3) Uani 1 1 d . H57A H -0.3803 0.6896 0.3606 0.066 Uiso 1 1 calc R H57B H -0.3372 0.6361 0.3250 0.066 Uiso 1 1 calc R H57C H -0.2973 0.6437 0.3855 0.066 Uiso 1 1 calc R C56 C -0.3133(9) 0.8057(5) 0.3505(4) 0.045(3) Uani 1 1 d . H56A H -0.3767 0.7819 0.3581 0.067 Uiso 1 1 calc R H56B H -0.2914 0.8264 0.3831 0.067 Uiso 1 1 calc R H56C H -0.3299 0.8343 0.3224 0.067 Uiso 1 1 calc R C52 C -0.2246(9) 0.7665(4) 0.3320(4) 0.033(2) Uani 1 1 d . C16 C 0.2803(8) 0.8012(4) 0.3227(4) 0.034(2) Uani 1 1 d . H16 H 0.2874 0.8422 0.3166 0.040 Uiso 1 1 calc R C84 C -0.4591(10) 0.8492(8) 0.0605(6) 0.075(4) Uani 1 1 d . H84A H -0.4549 0.8873 0.0785 0.112 Uiso 1 1 calc R H84B H -0.5198 0.8491 0.0358 0.112 Uiso 1 1 calc R H84C H -0.4687 0.8181 0.0873 0.112 Uiso 1 1 calc R 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 0.02165(17) 0.02676(15) 0.02282(16) 0.00158(15) -0.00142(15) -0.00129(12) U51 0.02074(17) 0.02710(15) 0.02146(16) -0.00066(16) -0.00044(14) 0.00060(12) Si1 0.0409(17) 0.0272(14) 0.0358(15) -0.0047(11) -0.0091(12) 0.0015(11) Si6 0.0424(17) 0.0305(14) 0.0289(14) 0.0062(11) -0.0069(12) -0.0007(12) C51 0.033(6) 0.026(5) 0.021(4) -0.007(4) -0.001(4) -0.004(4) C3 0.035(6) 0.038(6) 0.028(6) 0.007(4) 0.001(4) -0.005(5) Si2 0.0312(15) 0.0282(13) 0.0302(13) 0.0027(10) -0.0031(11) 0.0026(11) Si3 0.0302(14) 0.0290(13) 0.0328(14) -0.0047(11) -0.0017(11) 0.0001(11) C10 0.039(6) 0.030(5) 0.026(5) 0.002(4) -0.006(5) 0.000(4) C23 0.048(7) 0.039(6) 0.043(6) -0.013(5) -0.014(5) 0.004(5) N1 0.021(4) 0.033(4) 0.021(4) 0.004(3) 0.000(3) -0.004(3) N51 0.027(4) 0.035(5) 0.022(4) -0.002(3) -0.005(3) -0.003(3) C14 0.009(4) 0.046(5) 0.038(6) -0.001(5) 0.000(4) 0.001(4) C82 0.051(8) 0.051(6) 0.045(7) 0.014(6) -0.022(6) -0.009(5) C26 0.057(7) 0.032(5) 0.044(6) -0.004(4) -0.005(5) 0.002(5) C62 0.025(5) 0.032(5) 0.033(5) 0.007(4) -0.001(4) 0.002(4) C27 0.060(7) 0.039(5) 0.050(6) 0.001(6) -0.017(7) 0.007(5) C25 0.061(9) 0.067(9) 0.051(8) -0.005(6) -0.025(7) 0.007(6) C60 0.028(5) 0.032(5) 0.028(5) -0.006(4) -0.002(4) 0.004(4) C2 0.031(6) 0.050(7) 0.024(5) 0.006(5) 0.000(4) -0.004(5) C72 0.043(6) 0.038(6) 0.036(6) 0.002(4) -0.001(5) 0.003(5) C54 0.031(6) 0.032(5) 0.020(4) -0.001(4) -0.003(4) -0.001(4) C5 0.044(7) 0.036(5) 0.039(6) 0.000(4) 0.000(5) -0.001(5) C1 0.034(6) 0.031(5) 0.019(4) 0.003(4) 0.000(4) 0.000(4) C53 0.029(6) 0.045(6) 0.024(5) -0.001(4) 0.003(4) -0.011(5) C83 0.088(12) 0.063(9) 0.082(12) 0.004(7) -0.053(9) -0.010(8) C15 0.019(4) 0.042(6) 0.039(6) 0.014(5) -0.003(4) -0.015(4) C13 0.025(5) 0.041(6) 0.027(5) 0.003(4) -0.004(4) 0.005(4) C61 0.024(5) 0.037(6) 0.023(5) -0.005(4) -0.004(4) 0.001(4) C71 0.066(9) 0.052(7) 0.049(7) -0.017(6) -0.010(6) 0.025(6) C22 0.071(10) 0.042(7) 0.073(9) -0.002(6) -0.004(7) -0.004(6) C11 0.026(5) 0.032(5) 0.025(5) 0.005(4) -0.001(4) -0.005(4) C70 0.033(6) 0.032(5) 0.028(5) 0.000(4) 0.002(4) 0.004(4) C58 0.042(6) 0.033(5) 0.034(5) -0.002(4) -0.011(4) 0.000(4) C31 0.056(8) 0.065(8) 0.035(6) 0.011(6) 0.002(5) 0.000(6) C67 0.046(7) 0.033(5) 0.056(7) -0.017(5) -0.019(5) 0.011(5) C80 0.061(9) 0.042(7) 0.085(10) -0.022(7) -0.014(7) 0.003(6) C59 0.023(5) 0.037(5) 0.027(5) -0.002(4) 0.002(4) 0.000(4) C55 0.056(7) 0.027(5) 0.044(6) -0.006(4) -0.001(5) -0.005(5) C21 0.049(7) 0.043(7) 0.066(8) 0.018(6) -0.006(6) -0.007(5) C24 0.049(8) 0.070(8) 0.065(9) -0.010(7) -0.025(7) -0.005(6) C63 0.037(6) 0.024(5) 0.038(6) -0.005(4) -0.007(4) 0.001(4) C19 0.066(9) 0.080(9) 0.047(7) -0.014(6) -0.004(7) 0.013(7) C12 0.030(5) 0.028(5) 0.024(4) 0.003(4) -0.002(4) 0.000(4) C77 0.047(7) 0.052(7) 0.037(6) 0.007(5) 0.003(5) 0.001(5) C32 0.034(6) 0.049(6) 0.051(7) 0.009(5) 0.000(5) 0.001(5) C75 0.068(9) 0.065(8) 0.053(8) 0.014(6) 0.020(7) 0.006(7) C69 0.080(9) 0.054(7) 0.025(5) -0.010(5) -0.016(6) 0.012(6) C78 0.053(8) 0.084(9) 0.041(7) 0.025(6) 0.008(6) -0.003(7) C34 0.047(8) 0.055(8) 0.090(10) 0.022(7) -0.006(7) 0.013(6) C79 0.076(9) 0.029(5) 0.040(6) -0.001(4) 0.000(6) 0.004(5) C29 0.038(6) 0.038(6) 0.033(5) 0.010(4) -0.002(4) -0.002(4) C9 0.033(6) 0.028(5) 0.032(5) 0.003(4) -0.016(4) -0.001(4) C30 0.059(8) 0.047(7) 0.060(8) 0.020(6) 0.003(6) -0.009(6) C6 0.035(6) 0.064(7) 0.036(6) -0.005(5) 0.008(5) 0.009(5) C33 0.041(7) 0.073(8) 0.051(7) 0.001(6) -0.010(6) -0.009(6) C7 0.045(7) 0.072(9) 0.050(7) 0.024(6) 0.009(6) -0.019(6) C28 0.065(9) 0.071(9) 0.073(9) -0.041(8) 0.016(8) -0.004(7) C73 0.046(7) 0.033(5) 0.054(7) -0.008(4) 0.007(5) -0.003(5) C18 0.056(8) 0.056(8) 0.059(8) -0.007(6) 0.014(6) 0.002(6) C8 0.058(8) 0.038(6) 0.044(6) 0.009(5) -0.012(6) -0.001(5) C20 0.046(7) 0.031(5) 0.057(7) 0.005(5) -0.005(6) -0.005(5) C76 0.045(6) 0.043(5) 0.035(6) 0.001(5) -0.003(5) -0.002(4) C68 0.044(8) 0.065(8) 0.088(10) -0.021(7) -0.018(7) 0.000(6) C17 0.054(7) 0.046(6) 0.045(6) -0.012(5) -0.007(5) 0.012(5) C74 0.081(10) 0.032(6) 0.126(13) -0.015(7) 0.044(10) -0.019(6) C4 0.030(6) 0.040(5) 0.023(5) 0.008(4) -0.004(4) -0.005(4) C81 0.107(13) 0.047(8) 0.077(10) 0.008(7) -0.015(9) 0.010(8) C65 0.030(5) 0.028(5) 0.033(6) -0.004(4) -0.003(5) 0.002(3) C64 0.026(5) 0.039(5) 0.035(6) -0.010(5) 0.002(4) 0.008(4) C66 0.022(5) 0.033(5) 0.036(6) -0.006(4) -0.001(4) 0.000(4) C57 0.038(6) 0.062(7) 0.032(6) 0.005(5) 0.002(5) -0.010(6) C56 0.045(7) 0.053(7) 0.037(6) -0.012(5) 0.007(5) 0.016(6) C52 0.034(6) 0.040(6) 0.024(5) -0.005(4) 0.002(5) 0.011(4) C16 0.036(6) 0.031(5) 0.033(5) 0.002(4) -0.007(4) -0.010(4) C84 0.038(8) 0.125(13) 0.062(9) 0.021(9) -0.018(7) -0.010(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' 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' 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 C10 U1 C1 163.4(3) C10 U1 C12 57.9(3) C10 U1 C9 30.3(3) C10 U1 C4 146.4(3) N1 U1 C10 151.7(3) N1 U1 C1 29.8(2) N1 U1 C15 123.3(3) N1 U1 C11 150.3(3) N1 U1 C12 139.1(2) N1 U1 C9 140.5(3) N1 U1 C4 29.6(3) N51 U1 C10 82.7(3) N51 U1 N1 70.3(2) N51 U1 C14 166.1(3) N51 U1 C1 89.4(3) N51 U1 C15 149.1(3) N51 U1 C13 139.3(3) N51 U1 C11 88.3(3) N51 U1 C12 109.4(3) N51 U1 C9 93.7(3) N51 U1 C4 88.5(3) N51 U1 C16 118.7(3) C14 U1 C10 84.7(4) C14 U1 N1 123.0(3) C14 U1 C1 101.2(3) C14 U1 C15 29.9(3) C14 U1 C11 77.8(3) C14 U1 C12 58.4(3) C14 U1 C9 78.2(3) C14 U1 C4 105.3(3) C14 U1 C16 57.8(3) C15 U1 C10 76.9(4) C15 U1 C1 115.7(3) C15 U1 C11 85.6(3) C15 U1 C12 78.9(3) C15 U1 C9 57.7(3) C15 U1 C4 95.7(3) C13 U1 C10 77.8(3) C13 U1 N1 128.7(3) C13 U1 C14 30.5(3) C13 U1 C1 99.3(3) C13 U1 C15 57.8(3) C13 U1 C11 57.9(3) C13 U1 C12 30.8(3) C13 U1 C9 87.2(3) C13 U1 C4 126.1(3) C13 U1 C16 79.3(3) C11 U1 C10 30.1(3) C11 U1 C1 135.6(3) C11 U1 C12 30.5(3) C11 U1 C9 58.2(3) C11 U1 C4 175.8(3) C12 U1 C1 111.9(3) C12 U1 C9 79.8(3) C12 U1 C4 153.7(3) C9 U1 C1 166.0(3) C4 U1 C1 47.2(3) C4 U1 C9 119.2(3) C16 U1 C10 57.4(3) C16 U1 N1 129.3(3) C16 U1 C1 138.6(3) C16 U1 C15 30.4(3) C16 U1 C11 78.7(3) C16 U1 C12 88.0(3) C16 U1 C9 30.4(3) C16 U1 C4 100.3(3) C51 U51 C62 126.1(3) C51 U51 C54 47.2(3) N1 U51 C51 86.9(3) N1 U51 N51 69.8(2) N1 U51 C62 90.9(3) N1 U51 C60 92.3(3) N1 U51 C54 89.8(3) N1 U51 C61 82.7(3) N1 U51 C59 116.1(2) N1 U51 C63 112.6(3) N1 U51 C65 167.4(3) N1 U51 C64 142.6(3) N1 U51 C66 146.5(3) N51 U51 C51 29.8(3) N51 U51 C62 145.8(3) N51 U51 C54 29.5(3) N51 U51 C61 152.5(3) N51 U51 C59 134.3(2) N51 U51 C66 126.0(3) C60 U51 C51 175.8(3) C60 U51 N51 146.4(3) C60 U51 C62 58.1(3) C60 U51 C54 128.7(3) C60 U51 C61 30.3(3) C60 U51 C59 30.9(3) C60 U51 C63 79.1(3) C60 U51 C65 78.0(3) C60 U51 C64 87.5(3) C60 U51 C66 57.9(3) C54 U51 C62 173.2(3) C61 U51 C51 153.3(3) C61 U51 C62 30.3(3) C61 U51 C54 156.4(3) C59 U51 C51 147.0(3) C59 U51 C62 79.3(3) C59 U51 C54 106.4(3) C59 U51 C61 58.3(3) C63 U51 C51 105.1(3) C63 U51 N51 133.6(2) C63 U51 C62 29.8(3) C63 U51 C54 144.8(3) C63 U51 C61 57.6(3) C63 U51 C59 88.2(3) C63 U51 C65 58.1(3) C63 U51 C66 79.0(3) C65 U51 C51 103.4(3) C65 U51 N51 122.6(3) C65 U51 C62 77.2(3) C65 U51 C54 102.4(3) C65 U51 C61 84.9(3) C65 U51 C59 58.0(3) C65 U51 C66 30.0(3) C64 U51 C51 95.6(3) C64 U51 N51 124.2(3) C64 U51 C62 57.6(3) C64 U51 C54 118.9(3) C64 U51 C61 78.4(3) C64 U51 C59 80.3(3) C64 U51 C63 30.9(3) C64 U51 C65 30.8(3) C64 U51 C66 58.5(3) C66 U51 C51 121.6(3) C66 U51 C62 85.7(3) C66 U51 C54 97.4(3) C66 U51 C61 77.7(3) C66 U51 C59 30.6(3) C23 Si1 C20 107.6(5) C9 Si1 C23 104.7(5) C9 Si1 C20 110.0(5) C17 Si1 C23 111.5(5) C17 Si1 C9 117.1(5) C17 Si1 C20 105.8(5) C62 Si6 C82 104.5(5) C62 Si6 C79 111.7(5) C62 Si6 C76 111.6(4) C79 Si6 C82 105.1(5) C76 Si6 C82 107.8(5) C76 Si6 C79 115.1(5) N51 C51 U51 71.8(5) N51 C51 C55 120.0(9) C55 C51 U51 117.2(6) C52 C51 U51 82.7(6) C52 C51 N51 111.8(9) C52 C51 C55 127.9(9) C2 C3 U1 75.4(5) C2 C3 C7 128.5(11) C7 C3 U1 125.8(8) C4 C3 U1 69.1(6) C4 C3 C2 104.7(9) C4 C3 C7 126.3(10) C26 Si2 C32 107.4(5) C26 Si2 C29 106.8(5) C12 Si2 C26 115.4(4) C12 Si2 C32 104.1(4) C12 Si2 C29 110.0(4) C32 Si2 C29 113.2(5) C70 Si3 C67 107.9(4) C59 Si3 C70 112.9(4) C59 Si3 C67 106.7(4) C73 Si3 C70 111.3(5) C73 Si3 C67 105.8(5) C73 Si3 C59 111.8(4) U1 C10 H10 136.6 C11 C10 U1 73.6(6) C11 C10 H10 111.0 C11 C10 C9 137.9(11) C9 C10 U1 76.2(6) C9 C10 H10 111.0 Si1 C23 H23 107.0 C25 C23 Si1 114.1(8) C25 C23 H23 107.0 C24 C23 Si1 111.4(9) C24 C23 H23 107.0 C24 C23 C25 109.9(11) U51 N1 U1 109.5(3) C1 N1 U1 78.8(5) C1 N1 U51 122.1(6) C4 N1 U1 78.2(5) C4 N1 U51 133.3(6) C4 N1 C1 104.7(8) U1 N51 U51 109.7(3) C51 N51 U1 130.1(6) C51 N51 U51 78.5(5) C54 N51 U1 124.9(6) C54 N51 U51 79.0(5) C54 N51 C51 105.0(9) U1 C14 H14 134.2 C15 C14 U1 75.4(5) C15 C14 H14 111.8 C15 C14 C13 136.4(10) C13 C14 U1 74.5(5) C13 C14 H14 111.8 Si6 C82 H82 106.5 C83 C82 Si6 114.1(9) C83 C82 H82 106.5 C83 C82 C84 109.0(12) C84 C82 Si6 113.6(8) C84 C82 H82 106.5 Si2 C26 H26 105.4 C27 C26 Si2 112.5(7) C27 C26 H26 105.4 C28 C26 Si2 116.7(8) C28 C26 H26 105.4 C28 C26 C27 110.3(10) Si6 C62 U51 156.7(5) C61 C62 U51 72.6(5) C61 C62 Si6 111.7(7) C63 C62 U51 70.3(5) C63 C62 Si6 114.9(7) C63 C62 C61 131.4(9) 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 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 U51 C60 H60 127.6 C61 C60 U51 77.7(5) C61 C60 H60 110.9 C61 C60 C59 138.2(9) C59 C60 U51 77.2(5) C59 C60 H60 110.9 C3 C2 U1 75.5(6) C3 C2 C6 125.0(9) C1 C2 U1 70.2(5) C1 C2 C3 106.8(10) C1 C2 C6 127.8(10) C6 C2 U1 125.0(7) H72A C72 H72B 109.5 H72A C72 H72C 109.5 H72B C72 H72C 109.5 C70 C72 H72A 109.5 C70 C72 H72B 109.5 C70 C72 H72C 109.5 N51 C54 U51 71.5(5) N51 C54 C53 111.0(9) N51 C54 C58 121.0(9) C53 C54 U51 82.9(6) C53 C54 C58 127.5(9) C58 C54 U51 118.1(6) H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C1 C5 H5A 109.5 C1 C5 H5B 109.5 C1 C5 H5C 109.5 N1 C1 U1 71.3(5) N1 C1 C5 121.3(9) C2 C1 U1 82.4(6) C2 C1 N1 111.9(9) C2 C1 C5 126.3(9) C5 C1 U1 119.4(6) C54 C53 U51 69.0(5) C54 C53 C57 127.8(10) C54 C53 C52 105.7(8) C57 C53 U51 125.0(7) C52 C53 U51 74.8(5) C52 C53 C57 126.2(10) C82 C83 H83A 109.5 C82 C83 H83B 109.5 C82 C83 H83C 109.5 H83A C83 H83B 109.5 H83A C83 H83C 109.5 H83B C83 H83C 109.5 U1 C15 H15 135.0 C14 C15 U1 74.7(5) C14 C15 H15 112.0 C14 C15 C16 136.1(9) C16 C15 U1 74.6(6) C16 C15 H15 112.0 U1 C13 H13 130.2 C14 C13 U1 75.0(5) C14 C13 H13 111.9 C14 C13 C12 136.2(10) C12 C13 U1 77.2(5) C12 C13 H13 111.9 U51 C61 H61 135.1 C62 C61 U51 77.1(5) C62 C61 H61 112.0 C60 C61 U51 72.0(5) C60 C61 C62 135.9(10) C60 C61 H61 112.0 H71A C71 H71B 109.5 H71A C71 H71C 109.5 H71B C71 H71C 109.5 C70 C71 H71A 109.5 C70 C71 H71B 109.5 C70 C71 H71C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 C20 C22 H22C 109.5 U1 C11 H11 130.3 C10 C11 U1 76.3(6) C10 C11 H11 111.2 C10 C11 C12 137.5(9) C12 C11 U1 76.6(5) C12 C11 H11 111.2 Si3 C70 H70 106.5 C72 C70 Si3 115.2(7) C72 C70 H70 106.5 C71 C70 Si3 114.4(7) C71 C70 C72 107.1(8) C71 C70 H70 106.5 C54 C58 H58A 109.5 C54 C58 H58B 109.5 C54 C58 H58C 109.5 H58A C58 H58B 109.5 H58A C58 H58C 109.5 H58B C58 H58C 109.5 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 Si3 C67 H67 107.1 C69 C67 Si3 114.4(8) C69 C67 H67 107.1 C68 C67 Si3 112.2(8) C68 C67 H67 107.1 C68 C67 C69 108.7(10) H80A C80 H80B 109.5 H80A C80 H80C 109.5 H80B C80 H80C 109.5 C79 C80 H80A 109.5 C79 C80 H80B 109.5 C79 C80 H80C 109.5 Si3 C59 U51 148.1(5) C60 C59 U51 71.9(5) C60 C59 Si3 111.8(7) C66 C59 U51 73.9(5) C66 C59 Si3 116.7(7) C66 C59 C60 129.8(9) C51 C55 H55A 109.5 C51 C55 H55B 109.5 C51 C55 H55C 109.5 H55A C55 H55B 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C21 H21A 109.5 C20 C21 H21B 109.5 C20 C21 H21C 109.5 C23 C24 H24A 109.5 C23 C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 U51 C63 H63 127.6 C62 C63 U51 79.9(6) C62 C63 H63 111.5 C62 C63 C64 137.0(9) C64 C63 U51 74.2(6) C64 C63 H63 111.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C17 C19 H19A 109.5 C17 C19 H19B 109.5 C17 C19 H19C 109.5 Si2 C12 U1 151.7(5) C13 C12 U1 72.0(5) C13 C12 Si2 113.2(7) C11 C12 U1 72.8(5) C11 C12 Si2 115.0(7) C11 C12 C13 129.6(9) H77A C77 H77B 109.5 H77A C77 H77C 109.5 H77B C77 H77C 109.5 C76 C77 H77A 109.5 C76 C77 H77B 109.5 C76 C77 H77C 109.5 Si2 C32 H32 104.8 C34 C32 Si2 114.7(8) C34 C32 H32 104.8 C33 C32 Si2 115.9(8) C33 C32 H32 104.8 C33 C32 C34 110.5(10) H75A C75 H75B 109.5 H75A C75 H75C 109.5 H75B C75 H75C 109.5 C73 C75 H75A 109.5 C73 C75 H75B 109.5 C73 C75 H75C 109.5 C67 C69 H69A 109.5 C67 C69 H69B 109.5 C67 C69 H69C 109.5 H69A C69 H69B 109.5 H69A C69 H69C 109.5 H69B C69 H69C 109.5 H78A C78 H78B 109.5 H78A C78 H78C 109.5 H78B C78 H78C 109.5 C76 C78 H78A 109.5 C76 C78 H78B 109.5 C76 C78 H78C 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 Si6 C79 H79 104.9 C80 C79 Si6 115.2(9) C80 C79 H79 104.9 C80 C79 C81 110.6(11) C81 C79 Si6 114.9(9) C81 C79 H79 104.9 Si2 C29 H29 106.8 C31 C29 Si2 113.6(7) C31 C29 H29 106.8 C30 C29 Si2 114.1(8) C30 C29 C31 108.2(9) C30 C29 H29 106.8 Si1 C9 U1 152.2(5) C10 C9 U1 73.5(6) C10 C9 Si1 112.6(8) C10 C9 C16 130.4(10) C16 C9 U1 71.9(5) C16 C9 Si1 114.7(7) 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 C2 C6 H6A 109.5 C2 C6 H6B 109.5 C2 C6 H6C 109.5 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 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 C3 C7 H7A 109.5 C3 C7 H7B 109.5 C3 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 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 Si3 C73 H73 106.5 C75 C73 Si3 116.2(8) C75 C73 H73 106.5 C75 C73 C74 108.0(10) C74 C73 Si3 112.6(8) C74 C73 H73 106.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C17 C18 H18A 109.5 C17 C18 H18B 109.5 C17 C18 H18C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C4 C8 H8A 109.5 C4 C8 H8B 109.5 C4 C8 H8C 109.5 Si1 C20 H20 106.0 C22 C20 Si1 113.4(8) C22 C20 C21 111.1(10) C22 C20 H20 106.0 C21 C20 Si1 113.5(8) C21 C20 H20 106.0 Si6 C76 H76 105.5 C77 C76 Si6 117.7(7) C77 C76 C78 108.6(9) C77 C76 H76 105.5 C78 C76 Si6 113.0(8) C78 C76 H76 105.5 C67 C68 H68A 109.5 C67 C68 H68B 109.5 C67 C68 H68C 109.5 H68A C68 H68B 109.5 H68A C68 H68C 109.5 H68B C68 H68C 109.5 Si1 C17 H17 104.6 C19 C17 Si1 112.1(8) C19 C17 H17 104.6 C18 C17 Si1 122.6(8) C18 C17 C19 106.7(10) C18 C17 H17 104.6 C73 C74 H74A 109.5 C73 C74 H74B 109.5 C73 C74 H74C 109.5 H74A C74 H74B 109.5 H74A C74 H74C 109.5 H74B C74 H74C 109.5 C3 C4 U1 82.6(6) C3 C4 C8 125.9(10) N1 C4 U1 72.2(5) N1 C4 C3 111.9(9) N1 C4 C8 122.0(10) C8 C4 U1 116.7(7) C79 C81 H81A 109.5 C79 C81 H81B 109.5 C79 C81 H81C 109.5 H81A C81 H81B 109.5 H81A C81 H81C 109.5 H81B C81 H81C 109.5 U51 C65 H65 136.2 C64 C65 U51 73.8(6) C64 C65 H65 111.2 C66 C65 U51 76.0(6) C66 C65 H65 111.2 C66 C65 C64 137.6(11) U51 C64 H64 129.9 C63 C64 U51 74.9(5) C63 C64 H64 113.5 C65 C64 U51 75.5(6) C65 C64 C63 133.1(10) C65 C64 H64 113.5 U51 C66 H66 134.6 C59 C66 U51 75.5(5) C59 C66 H66 112.0 C65 C66 U51 74.0(6) C65 C66 C59 136.1(10) C65 C66 H66 112.0 C53 C57 H57A 109.5 C53 C57 H57B 109.5 C53 C57 H57C 109.5 H57A C57 H57B 109.5 H57A C57 H57C 109.5 H57B C57 H57C 109.5 H56A C56 H56B 109.5 H56A C56 H56C 109.5 H56B C56 H56C 109.5 C52 C56 H56A 109.5 C52 C56 H56B 109.5 C52 C56 H56C 109.5 C51 C52 U51 69.6(6) C51 C52 C53 106.4(9) C51 C52 C56 128.2(10) C53 C52 U51 76.5(5) C53 C52 C56 124.9(10) C56 C52 U51 125.3(7) U1 C16 H16 128.6 C15 C16 U1 74.9(6) C15 C16 C9 135.4(9) C15 C16 H16 112.3 C9 C16 U1 77.7(6) C9 C16 H16 112.3 C82 C84 H84A 109.5 C82 C84 H84B 109.5 C82 C84 H84C 109.5 H84A C84 H84B 109.5 H84A C84 H84C 109.5 H84B C84 H84C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance U1 C10 2.720(10) U1 N1 2.680(8) U1 N51 2.598(9) U1 C14 2.674(8) U1 C1 2.775(9) U1 C15 2.683(9) U1 C13 2.668(9) U1 C11 2.686(9) U1 C12 2.735(9) U1 C9 2.754(10) U1 C4 2.755(9) U1 C16 2.680(10) U51 C51 2.778(9) U51 N1 2.617(8) U51 N51 2.692(8) U51 C62 2.800(9) U51 C60 2.668(9) U51 C54 2.786(9) U51 C61 2.740(10) U51 C59 2.736(9) U51 C63 2.677(9) U51 C65 2.690(10) U51 C64 2.668(10) U51 C66 2.715(10) Si1 C23 1.904(11) Si1 C9 1.886(11) Si1 C20 1.912(11) Si1 C17 1.873(12) Si6 C82 1.924(11) Si6 C62 1.889(10) Si6 C79 1.924(11) Si6 C76 1.897(11) C51 N51 1.407(12) C51 C55 1.511(14) C51 C52 1.374(16) C3 C2 1.465(16) C3 C7 1.476(15) C3 C4 1.400(16) Si2 C26 1.903(11) Si2 C12 1.888(9) Si2 C32 1.911(11) Si2 C29 1.918(10) Si3 C70 1.897(10) Si3 C67 1.909(11) Si3 C59 1.894(10) Si3 C73 1.892(11) C10 H10 0.9500 C10 C11 1.405(13) C10 C9 1.430(14) C23 H23 1.0000 C23 C25 1.512(17) C23 C24 1.488(17) N1 C1 1.408(12) N1 C4 1.389(12) N51 C54 1.398(12) C14 H14 0.9500 C14 C15 1.381(14) C14 C13 1.405(14) C82 H82 1.0000 C82 C83 1.505(18) C82 C84 1.522(18) C26 H26 1.0000 C26 C27 1.544(17) C26 C28 1.536(16) C62 C61 1.449(13) C62 C63 1.414(14) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C60 H60 0.9500 C60 C61 1.416(13) C60 C59 1.440(13) C2 C1 1.358(14) C2 C6 1.485(15) C72 H72A 0.9800 C72 H72B 0.9800 C72 H72C 0.9800 C72 C70 1.540(13) C54 C53 1.405(15) C54 C58 1.500(13) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C5 C1 1.485(13) C53 C57 1.516(15) C53 C52 1.458(16) C83 H83A 0.9800 C83 H83B 0.9800 C83 H83C 0.9800 C15 H15 0.9500 C15 C16 1.408(15) C13 H13 0.9500 C13 C12 1.438(13) C61 H61 0.9500 C71 H71A 0.9800 C71 H71B 0.9800 C71 H71C 0.9800 C71 C70 1.534(15) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C22 C20 1.495(16) C11 H11 0.9500 C11 C12 1.429(13) C70 H70 1.0000 C58 H58A 0.9800 C58 H58B 0.9800 C58 H58C 0.9800 C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C31 C29 1.546(15) C67 H67 1.0000 C67 C69 1.562(17) C67 C68 1.534(16) C80 H80A 0.9800 C80 H80B 0.9800 C80 H80C 0.9800 C80 C79 1.509(17) C59 C66 1.438(13) C55 H55A 0.9800 C55 H55B 0.9800 C55 H55C 0.9800 C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C21 C20 1.512(16) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C63 H63 0.9500 C63 C64 1.422(15) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C19 C17 1.605(15) C77 H77A 0.9800 C77 H77B 0.9800 C77 H77C 0.9800 C77 C76 1.544(15) C32 H32 1.0000 C32 C34 1.524(15) C32 C33 1.526(15) C75 H75A 0.9800 C75 H75B 0.9800 C75 H75C 0.9800 C75 C73 1.533(17) C69 H69A 0.9800 C69 H69B 0.9800 C69 H69C 0.9800 C78 H78A 0.9800 C78 H78B 0.9800 C78 H78C 0.9800 C78 C76 1.570(14) C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C79 H79 1.0000 C79 C81 1.515(16) C29 H29 1.0000 C29 C30 1.535(15) C9 C16 1.427(15) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C73 H73 1.0000 C73 C74 1.547(15) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C18 C17 1.536(17) C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C8 C4 1.509(15) C20 H20 1.0000 C76 H76 1.0000 C68 H68A 0.9800 C68 H68B 0.9800 C68 H68C 0.9800 C17 H17 1.0000 C74 H74A 0.9800 C74 H74B 0.9800 C74 H74C 0.9800 C81 H81A 0.9800 C81 H81B 0.9800 C81 H81C 0.9800 C65 H65 0.9500 C65 C64 1.421(13) C65 C66 1.399(12) C64 H64 0.9500 C66 H66 0.9500 C57 H57A 0.9800 C57 H57B 0.9800 C57 H57C 0.9800 C56 H56A 0.9800 C56 H56B 0.9800 C56 H56C 0.9800 C56 C52 1.500(14) C16 H16 0.9500 C84 H84A 0.9800 C84 H84B 0.9800 C84 H84C 0.9800 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 U1 C3 C2 C1 63.7(7) U1 C3 C2 C6 -122.8(10) U1 C3 C4 N1 -67.4(7) U1 C3 C4 C8 117.8(10) U1 C10 C11 C12 51.7(12) U1 C10 C9 Si1 151.1(6) U1 C10 C9 C16 -47.4(10) U1 N1 C1 C2 -73.3(7) U1 N1 C1 C5 113.6(8) U1 N1 C4 C3 74.1(8) U1 N1 C4 C8 -110.9(9) U1 N51 C54 U51 -106.4(5) U1 N51 C54 C53 179.1(6) U1 N51 C54 C58 5.8(12) U1 C14 C15 C16 47.1(13) U1 C14 C13 C12 -52.2(11) U1 C2 C1 N1 66.3(6) U1 C2 C1 C5 -121.1(9) U1 C15 C16 C9 54.0(12) U1 C13 C12 Si2 150.2(5) U1 C13 C12 C11 -47.9(9) U1 C11 C12 Si2 -150.8(6) U1 C11 C12 C13 47.6(9) U1 C9 C16 C15 -53.0(12) U51 C51 N51 U1 106.1(6) U51 C51 N51 C54 -75.1(6) U51 C51 C52 C53 68.4(7) U51 C51 C52 C56 -119.5(11) U51 N1 C1 U1 -106.1(5) U51 N1 C1 C2 -179.4(6) U51 N1 C1 C5 7.5(11) U51 N1 C4 U1 105.8(6) U51 N1 C4 C3 179.8(7) U51 N1 C4 C8 -5.2(13) U51 N51 C54 C53 -74.4(7) U51 N51 C54 C58 112.2(8) U51 C62 C61 C60 46.3(12) U51 C62 C63 C64 -53.4(12) U51 C60 C61 C62 -47.8(12) U51 C60 C59 Si3 -146.3(5) U51 C60 C59 C66 49.3(10) U51 C54 C53 C57 118.7(10) U51 C54 C53 C52 -66.5(7) U51 C53 C52 C51 -63.7(7) U51 C53 C52 C56 123.9(11) U51 C59 C66 C65 47.3(12) U51 C63 C64 C65 -52.6(11) U51 C65 C64 C63 52.4(11) U51 C65 C66 C59 -47.8(12) Si1 C9 C16 U1 -150.9(6) Si1 C9 C16 C15 156.1(11) Si6 C62 C61 U51 155.6(6) Si6 C62 C61 C60 -158.1(10) Si6 C62 C63 U51 -155.4(6) Si6 C62 C63 C64 151.2(11) C51 N51 C54 U51 74.8(6) C51 N51 C54 C53 0.3(11) C51 N51 C54 C58 -173.0(8) C3 C2 C1 U1 -67.3(7) C3 C2 C1 N1 -1.0(11) C3 C2 C1 C5 171.6(9) Si3 C59 C66 U51 147.6(6) Si3 C59 C66 C65 -165.1(10) C10 C11 C12 U1 -51.6(12) C10 C11 C12 Si2 157.6(11) C10 C11 C12 C13 -4.1(19) C10 C9 C16 U1 47.9(10) C10 C9 C16 C15 -5(2) C23 Si1 C9 U1 171.6(11) C23 Si1 C9 C10 74.2(9) C23 Si1 C9 C16 -90.4(8) C23 Si1 C17 C19 29.4(10) C23 Si1 C17 C18 -99.5(10) N51 C51 C52 U51 -67.0(7) N51 C51 C52 C53 1.5(11) N51 C51 C52 C56 173.5(10) N51 C54 C53 U51 67.0(6) N51 C54 C53 C57 -174.2(9) N51 C54 C53 C52 0.5(11) C14 C15 C16 U1 -47.2(13) C14 C15 C16 C9 7(2) C14 C13 C12 U1 51.5(11) C14 C13 C12 Si2 -158.3(10) C14 C13 C12 C11 3.7(18) C82 Si6 C62 U51 176.8(12) C82 Si6 C62 C61 80.5(8) C82 Si6 C62 C63 -85.3(8) C82 Si6 C76 C77 -170.5(8) C82 Si6 C76 C78 61.6(9) C26 Si2 C12 U1 33.0(12) C26 Si2 C12 C13 -62.0(9) C26 Si2 C12 C11 133.3(7) C62 Si6 C76 C77 -56.2(9) C62 Si6 C76 C78 175.8(8) C62 C63 C64 U51 55.2(12) C62 C63 C64 C65 3(2) C60 C59 C66 U51 -48.6(10) C60 C59 C66 C65 -1.3(19) C2 C3 C4 U1 67.7(7) C2 C3 C4 N1 0.3(11) C2 C3 C4 C8 -174.5(9) C54 C53 C52 U51 62.5(6) C54 C53 C52 C51 -1.2(11) C54 C53 C52 C56 -173.6(10) C1 N1 C4 U1 -75.0(5) C1 N1 C4 C3 -0.9(10) C1 N1 C4 C8 174.1(9) C15 C14 C13 U1 48.0(12) C15 C14 C13 C12 -4(2) C13 C14 C15 U1 -47.7(12) C13 C14 C15 C16 -1(2) C61 C62 C63 U51 42.3(11) C61 C62 C63 C64 -11(2) C61 C60 C59 U51 -54.3(12) C61 C60 C59 Si3 159.4(11) C61 C60 C59 C66 -5.0(19) C11 C10 C9 U1 45.0(13) C11 C10 C9 Si1 -163.8(12) C11 C10 C9 C16 -2(2) C70 Si3 C59 U51 -37.7(10) C70 Si3 C59 C60 52.8(8) C70 Si3 C59 C66 -140.5(7) C70 Si3 C73 C75 62.1(9) C70 Si3 C73 C74 -63.1(11) C58 C54 C53 U51 -120.2(10) C58 C54 C53 C57 -1.5(17) C58 C54 C53 C52 173.3(9) C67 Si3 C70 C72 -162.8(8) C67 Si3 C70 C71 -38.0(9) C67 Si3 C59 U51 -156.1(8) C67 Si3 C59 C60 -65.5(8) C67 Si3 C59 C66 101.1(8) C67 Si3 C73 C75 179.1(8) C67 Si3 C73 C74 53.8(11) C59 Si3 C70 C72 79.5(8) C59 Si3 C70 C71 -155.7(8) C59 Si3 C73 C75 -65.2(9) C59 Si3 C73 C74 169.6(9) C59 C60 C61 U51 54.2(12) C59 C60 C61 C62 6(2) C55 C51 N51 U1 -5.3(13) C55 C51 N51 U51 -111.4(8) C55 C51 N51 C54 173.5(8) C55 C51 C52 U51 118.9(11) C55 C51 C52 C53 -172.6(10) C55 C51 C52 C56 -0.6(19) C63 C62 C61 U51 -41.6(10) C63 C62 C61 C60 5(2) C32 Si2 C12 U1 150.5(9) C32 Si2 C12 C13 55.5(8) C32 Si2 C12 C11 -109.2(7) C79 Si6 C62 U51 -70.0(14) C79 Si6 C62 C61 -166.3(8) C79 Si6 C62 C63 27.8(9) C79 Si6 C76 C77 72.5(9) C79 Si6 C76 C78 -55.4(9) C29 Si2 C12 U1 -87.9(10) C29 Si2 C12 C13 177.1(7) C29 Si2 C12 C11 12.4(8) C9 Si1 C17 C19 149.8(8) C9 Si1 C17 C18 20.9(11) C9 C10 C11 U1 -45.7(13) C9 C10 C11 C12 6(2) C6 C2 C1 U1 119.5(11) C6 C2 C1 N1 -174.3(10) C6 C2 C1 C5 -1.6(17) C7 C3 C2 U1 124.5(12) C7 C3 C2 C1 -171.8(11) C7 C3 C2 C6 1.6(17) C7 C3 C4 U1 -119.8(11) C7 C3 C4 N1 172.8(10) C7 C3 C4 C8 -2.0(18) C73 Si3 C70 C72 -47.2(9) C73 Si3 C70 C71 77.6(8) C73 Si3 C59 U51 88.7(9) C73 Si3 C59 C60 179.3(7) C73 Si3 C59 C66 -14.1(9) C20 Si1 C9 U1 -73.0(12) C20 Si1 C9 C10 -170.5(8) C20 Si1 C9 C16 24.9(9) C20 Si1 C17 C19 -87.3(9) C20 Si1 C17 C18 143.8(9) C76 Si6 C62 U51 60.5(14) C76 Si6 C62 C61 -35.8(9) C76 Si6 C62 C63 158.4(7) C17 Si1 C9 U1 47.7(13) C17 Si1 C9 C10 -49.8(9) C17 Si1 C9 C16 145.6(8) C4 C3 C2 U1 -63.3(7) C4 C3 C2 C1 0.4(11) C4 C3 C2 C6 173.9(10) C4 N1 C1 U1 74.5(6) C4 N1 C1 C2 1.2(10) C4 N1 C1 C5 -171.9(8) C64 C65 C66 U51 45.5(13) C64 C65 C66 C59 -2(2) C66 C65 C64 U51 -46.1(14) C66 C65 C64 C63 6(2) C57 C53 C52 U51 -122.6(10) C57 C53 C52 C51 173.7(10) C57 C53 C52 C56 1.3(16) C52 C51 N51 U1 -179.9(7) C52 C51 N51 U51 74.0(8) C52 C51 N51 C54 -1.1(11) loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.733(7) 2 0.267(7)