#------------------------------------------------------------------------------ #$Date: 2021-07-05 21:13:41 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267243 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158107.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_7158107 loop_ _publ_author_name 'Li, Jun' 'Daniliuc, Constantin G.' 'Kehr, Gerald' 'Erker, Gerhard' _publ_section_title ; Formation of amidino-borate derivatives by a multi-component reaction. ; _journal_issue 25 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 5551 _journal_page_last 5554 _journal_paper_doi 10.1039/d1ob00775k _journal_volume 19 _journal_year 2021 _chemical_formula_sum 'C56 H56 B F9 N3 P' _chemical_formula_weight 983.81 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method 'APEX3 v2016.1-0' _audit_update_record ; 2021-02-23 deposited with the CCDC. 2021-06-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.316(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3489(4) _cell_length_b 16.9297(6) _cell_length_c 23.6112(8) _cell_measurement_reflns_used 9997 _cell_measurement_temperature 111.(2) _cell_measurement_theta_max 68.6284 _cell_measurement_theta_min 3.2339 _cell_volume 5232.2(3) _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_collection ; APEX3 v2016.1-0 (Bruker AXS Inc., 2016) ; _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 111.(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON 100 CMOS' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'MX mirror' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.2304 _diffrn_reflns_av_unetI/netI 0.1176 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 73908 _diffrn_reflns_theta_full 66.59 _diffrn_reflns_theta_max 66.59 _diffrn_reflns_theta_min 3.23 _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2056 _exptl_crystal_size_max 0.106 _exptl_crystal_size_mid 0.039 _exptl_crystal_size_min 0.027 _refine_diff_density_max 0.364 _refine_diff_density_min -0.303 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 651 _refine_ls_number_reflns 9189 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.1655 _refine_ls_R_factor_gt 0.1005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+15.9501P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1703 _refine_ls_wR_factor_ref 0.1945 _reflns_number_gt 5397 _reflns_number_total 9189 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob00775k2.cif _cod_data_source_block erk9313 _cod_depositor_comments 'Adding full bibliography for 7158104--7158107.cif.' _cod_database_code 7158107 _shelx_res_file ; erk9313.res created by SHELXL-2014/7 TITL erk9313.res in P2(1)/c CELL 1.54178 13.3489 16.9297 23.6112 90.000 101.316 90.000 ZERR 4.000 0.0004 0.0006 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H B N F P UNIT 224 224 4 12 36 4 SIZE 0.027 0.039 0.106 TEMP -162.110 ACTA CONF OMIT -1 0 2 OMIT -2 18 1 OMIT 1 16 4 OMIT -3 16 2 OMIT -4 12 1 OMIT 3 14 1 OMIT -13 4 12 OMIT 8 3 19 L.S. 25 BOND $H FMAP 2 PLAN 10 ABIN WGHT 0.038300 15.950100 FVAR 0.30185 P1 6 0.323954 0.820379 0.761938 11.00000 0.02493 0.03198 = 0.03631 -0.00424 0.00978 -0.00006 C1 1 0.450126 0.770059 0.785008 11.00000 0.02454 0.03682 = 0.03291 -0.00568 0.01408 -0.00240 AFIX 23 H1A 2 0.484476 0.788961 0.823629 11.00000 -1.20000 H1B 2 0.440717 0.712176 0.786848 11.00000 -1.20000 AFIX 0 C2 1 0.512211 0.790132 0.740923 11.00000 0.02850 0.03147 = 0.02770 -0.00195 0.00653 -0.00358 AFIX 43 H2 2 0.504877 0.843494 0.728347 11.00000 -1.20000 AFIX 0 C3 1 0.576421 0.748189 0.715337 11.00000 0.01801 0.03094 = 0.03153 -0.00356 0.00827 -0.00377 C4 1 0.630592 0.782863 0.670613 11.00000 0.01999 0.02818 = 0.02359 -0.00133 0.00074 -0.00351 C5 1 0.673166 0.643503 0.692762 11.00000 0.02124 0.02781 = 0.02396 -0.00614 0.00377 -0.00505 C11 1 0.234746 0.790507 0.808881 11.00000 0.02016 0.03246 = 0.03633 -0.00565 0.00540 0.00390 C12 1 0.257352 0.753181 0.862951 11.00000 0.02850 0.03087 = 0.03799 -0.01278 0.00897 -0.00391 C13 1 0.177540 0.736694 0.892168 11.00000 0.03853 0.03839 = 0.03849 -0.00839 0.01523 -0.00493 AFIX 43 H13 2 0.193230 0.710630 0.928463 11.00000 -1.20000 AFIX 0 C14 1 0.076701 0.757027 0.870034 11.00000 0.02936 0.04771 = 0.05374 -0.02110 0.02101 -0.00528 C15 1 0.055860 0.795953 0.818473 11.00000 0.02300 0.04445 = 0.05497 -0.01848 0.01517 -0.00671 AFIX 43 H15 2 -0.012674 0.810946 0.803138 11.00000 -1.20000 AFIX 0 C16 1 0.132174 0.814711 0.787166 11.00000 0.02786 0.03324 = 0.03591 -0.00675 0.01127 0.00160 C17 1 0.362657 0.726366 0.892829 11.00000 0.03543 0.04868 = 0.03031 -0.00613 0.01217 0.00366 AFIX 137 H17A 2 0.383876 0.681246 0.871995 11.00000 -1.50000 H17B 2 0.360930 0.710705 0.932584 11.00000 -1.50000 H17C 2 0.411353 0.769785 0.893254 11.00000 -1.50000 AFIX 0 C18 1 -0.005998 0.738728 0.903959 11.00000 0.02775 0.08222 = 0.05777 -0.00887 0.01952 -0.01144 AFIX 137 H18A 2 -0.048999 0.785493 0.904673 11.00000 -1.50000 H18B 2 0.025675 0.724018 0.943572 11.00000 -1.50000 H18C 2 -0.048070 0.694855 0.885538 11.00000 -1.50000 AFIX 0 C19 1 0.099841 0.859651 0.731684 11.00000 0.02280 0.04347 = 0.04840 -0.00443 0.00628 0.00823 AFIX 137 H19A 2 0.091588 0.822913 0.699021 11.00000 -1.50000 H19B 2 0.152074 0.898962 0.728006 11.00000 -1.50000 H19C 2 0.034778 0.886377 0.731852 11.00000 -1.50000 AFIX 0 C21 1 0.277391 0.764605 0.694864 11.00000 0.02519 0.03018 = 0.04326 -0.00321 0.01764 -0.00032 C22 1 0.241193 0.686317 0.692456 11.00000 0.01668 0.04215 = 0.03240 -0.00658 0.01029 0.00283 C23 1 0.205560 0.650808 0.639823 11.00000 0.02671 0.03138 = 0.03458 -0.01084 0.00153 0.00041 AFIX 43 H23 2 0.181944 0.597826 0.639281 11.00000 -1.20000 AFIX 0 C24 1 0.202725 0.689111 0.587679 11.00000 0.03223 0.05163 = 0.02483 -0.00393 -0.00476 0.01110 C25 1 0.239639 0.766095 0.590327 11.00000 0.03792 0.05101 = 0.03547 0.00233 0.01158 0.00620 AFIX 43 H25 2 0.239740 0.793486 0.555222 11.00000 -1.20000 AFIX 0 C26 1 0.276084 0.804290 0.641783 11.00000 0.02800 0.04281 = 0.03759 -0.00228 0.01219 0.00449 C27 1 0.239910 0.636861 0.745868 11.00000 0.02751 0.03220 = 0.04437 -0.00673 0.01460 -0.00584 AFIX 137 H27A 2 0.181114 0.651928 0.762660 11.00000 -1.50000 H27B 2 0.303071 0.645861 0.774207 11.00000 -1.50000 H27C 2 0.234717 0.580838 0.735250 11.00000 -1.50000 AFIX 0 C28 1 0.163391 0.648929 0.531941 11.00000 0.06278 0.05708 = 0.04088 -0.01220 0.00537 0.00475 AFIX 137 H28A 2 0.191275 0.674649 0.501216 11.00000 -1.50000 H28B 2 0.088654 0.652244 0.522988 11.00000 -1.50000 H28C 2 0.184252 0.593340 0.534785 11.00000 -1.50000 AFIX 0 C29 1 0.318023 0.886834 0.639084 11.00000 0.04320 0.04098 = 0.05090 0.00351 0.01655 -0.00383 AFIX 137 H29A 2 0.392834 0.884837 0.646548 11.00000 -1.50000 H29B 2 0.295678 0.919980 0.668297 11.00000 -1.50000 H29C 2 0.292753 0.909207 0.600655 11.00000 -1.50000 AFIX 0 B1 3 0.703896 0.714486 0.652772 11.00000 0.02172 0.02313 = 0.03140 0.00046 0.00935 0.00340 H1 2 0.781865 0.727770 0.673684 11.00000 0.00255 C31 1 0.698255 0.691512 0.584555 11.00000 0.02948 0.02159 = 0.02982 0.00045 0.00893 -0.00035 C32 1 0.613101 0.658609 0.547706 11.00000 0.01980 0.02622 = 0.02554 0.00154 0.00663 -0.00186 C33 1 0.616673 0.627558 0.493886 11.00000 0.03135 0.02971 = 0.02974 -0.00371 0.00610 -0.00384 AFIX 43 H33 2 0.556964 0.605065 0.471042 11.00000 -1.20000 AFIX 0 C34 1 0.707056 0.629105 0.473101 11.00000 0.03105 0.03038 = 0.03087 -0.00437 0.00863 -0.00408 C35 1 0.790560 0.666077 0.505272 11.00000 0.03308 0.02504 = 0.03860 0.00042 0.01592 -0.00013 AFIX 43 H35 2 0.851798 0.669773 0.490633 11.00000 -1.20000 AFIX 0 C36 1 0.786958 0.698139 0.558831 11.00000 0.02461 0.02167 = 0.02862 0.00214 0.00666 0.00142 C37 1 0.506366 0.653517 0.560392 11.00000 0.02763 0.03100 = 0.02661 -0.00300 0.00555 -0.00325 F1 5 0.491970 0.688764 0.607813 11.00000 0.02522 0.08026 = 0.04161 -0.02221 0.01104 -0.00770 F2 5 0.437063 0.684239 0.517602 11.00000 0.03053 0.08446 = 0.03511 0.01090 0.00259 0.01095 F3 5 0.475636 0.578711 0.563858 11.00000 0.04257 0.03432 = 0.09284 -0.00027 0.03232 -0.00689 C38 1 0.709786 0.590138 0.416864 11.00000 0.03634 0.04142 = 0.03405 -0.00359 0.01157 -0.00596 F4 5 0.631183 0.611413 0.375029 11.00000 0.05471 0.06534 = 0.03409 -0.01140 0.00450 0.00573 F5 5 0.704580 0.512300 0.419381 11.00000 0.08965 0.02888 = 0.05043 -0.00967 0.02440 -0.00287 F6 5 0.793993 0.608213 0.396544 11.00000 0.05273 0.07440 = 0.04848 -0.01805 0.03203 -0.01259 C39 1 0.881376 0.740606 0.588907 11.00000 0.02996 0.03509 = 0.03738 0.00277 0.02013 -0.00409 F7 5 0.946003 0.753444 0.551747 11.00000 0.03170 0.04967 = 0.05297 -0.00597 0.02545 -0.01120 F8 5 0.937043 0.701780 0.633582 11.00000 0.02493 0.04098 = 0.05030 0.00708 0.00563 -0.00028 F9 5 0.862357 0.812354 0.607808 11.00000 0.02967 0.02861 = 0.05279 -0.01054 0.01259 -0.00599 N1 4 0.613370 0.854542 0.657699 11.00000 0.02574 0.02891 = 0.03112 -0.00152 0.01007 0.00260 C41 1 0.665850 0.900520 0.622638 11.00000 0.02998 0.02267 = 0.03513 0.00164 0.01733 0.00565 C42 1 0.752983 0.941150 0.652037 11.00000 0.02512 0.03224 = 0.04768 -0.01258 0.01389 -0.00232 C43 1 0.796907 0.997171 0.621220 11.00000 0.04379 0.02852 = 0.07733 -0.01787 0.03516 -0.00777 AFIX 43 H43 2 0.855364 1.025464 0.640239 11.00000 -1.20000 AFIX 0 C44 1 0.757408 1.012720 0.563386 11.00000 0.06572 0.04072 = 0.06484 -0.00441 0.04475 -0.00519 AFIX 43 H44 2 0.788479 1.051113 0.543077 11.00000 -1.20000 AFIX 0 C45 1 0.672505 0.971683 0.535859 11.00000 0.06256 0.02499 = 0.04776 0.00732 0.03095 0.00646 AFIX 43 H45 2 0.645558 0.982046 0.496257 11.00000 -1.20000 AFIX 0 C46 1 0.625176 0.915205 0.564858 11.00000 0.04315 0.03083 = 0.03439 0.00254 0.01861 0.00400 C47 1 0.797294 0.923223 0.713731 11.00000 0.02986 0.02996 = 0.05755 -0.01480 0.00946 0.00075 AFIX 137 H47A 2 0.824111 0.869178 0.716898 11.00000 -1.50000 H47B 2 0.744102 0.928313 0.736811 11.00000 -1.50000 H47C 2 0.852775 0.960403 0.728011 11.00000 -1.50000 AFIX 0 C48 1 0.532176 0.871870 0.533960 11.00000 0.04123 0.04003 = 0.03639 0.00284 0.00729 0.00156 AFIX 137 H48A 2 0.552905 0.821746 0.518968 11.00000 -1.50000 H48B 2 0.496445 0.904211 0.501842 11.00000 -1.50000 H48C 2 0.486504 0.861379 0.560909 11.00000 -1.50000 AFIX 0 N2 4 0.709390 0.570879 0.700387 11.00000 0.02461 0.02471 = 0.03187 -0.00116 0.01128 0.00042 H2A 2 0.687018 0.536451 0.729854 11.00000 0.07699 C51 1 0.793587 0.541424 0.675375 11.00000 0.02503 0.02865 = 0.02760 0.00323 0.00954 0.00136 C52 1 0.772559 0.490642 0.628582 11.00000 0.04124 0.03031 = 0.02209 0.00166 0.00955 0.00185 C53 1 0.855461 0.464041 0.605192 11.00000 0.06867 0.02859 = 0.03666 -0.00686 0.02599 0.00642 AFIX 43 H53 2 0.843850 0.429785 0.572693 11.00000 -1.20000 AFIX 0 C54 1 0.953026 0.487219 0.628983 11.00000 0.04196 0.04034 = 0.06232 0.00207 0.02621 0.01204 AFIX 43 H54 2 1.008120 0.470414 0.611840 11.00000 -1.20000 AFIX 0 C55 1 0.972251 0.534145 0.677001 11.00000 0.03030 0.02595 = 0.05733 0.00139 0.01462 0.00338 AFIX 43 H55 2 1.040652 0.548078 0.693599 11.00000 -1.20000 AFIX 0 C56 1 0.892633 0.561679 0.701782 11.00000 0.02520 0.02820 = 0.02745 0.00426 0.00251 0.00319 C57 1 0.666278 0.460881 0.604258 11.00000 0.04643 0.03590 = 0.04066 0.00030 0.00071 -0.00410 AFIX 137 H57A 2 0.668598 0.424627 0.572184 11.00000 -1.50000 H57B 2 0.621703 0.505652 0.590281 11.00000 -1.50000 H57C 2 0.639505 0.433035 0.634511 11.00000 -1.50000 AFIX 0 C58 1 0.916205 0.612332 0.754851 11.00000 0.02935 0.04626 = 0.04830 -0.00509 -0.00098 -0.00376 AFIX 137 H58A 2 0.889869 0.665782 0.745542 11.00000 -1.50000 H58B 2 0.990329 0.614574 0.768693 11.00000 -1.50000 H58C 2 0.883820 0.589736 0.784990 11.00000 -1.50000 AFIX 0 N3 4 0.607941 0.669133 0.725986 11.00000 0.02483 0.02110 = 0.02870 0.00351 0.00878 0.00237 C61 1 0.585615 0.624709 0.774392 11.00000 0.02644 0.03013 = 0.02444 -0.00149 0.01022 0.00031 C62 1 0.637536 0.645110 0.829423 11.00000 0.02600 0.03185 = 0.02637 -0.00129 0.00695 0.00296 C63 1 0.610286 0.607133 0.875765 11.00000 0.03357 0.03215 = 0.03100 -0.00220 0.00851 0.00263 AFIX 43 H63 2 0.644539 0.620007 0.913815 11.00000 -1.20000 AFIX 0 C64 1 0.533427 0.550203 0.867841 11.00000 0.03512 0.02912 = 0.04134 0.00562 0.01779 0.00154 AFIX 43 H64 2 0.514720 0.525387 0.900330 11.00000 -1.20000 AFIX 0 C65 1 0.484105 0.529750 0.812258 11.00000 0.03055 0.03112 = 0.03818 -0.00039 0.01489 -0.00577 AFIX 43 H65 2 0.432462 0.490323 0.806696 11.00000 -1.20000 AFIX 0 C66 1 0.510776 0.567404 0.764604 11.00000 0.02719 0.02212 = 0.03107 0.00146 0.01099 -0.00018 C67 1 0.718770 0.708017 0.839147 11.00000 0.02865 0.04111 = 0.02899 -0.00454 0.00333 -0.00707 AFIX 137 H67A 2 0.772684 0.694263 0.818069 11.00000 -1.50000 H67B 2 0.747999 0.711883 0.880501 11.00000 -1.50000 H67C 2 0.688521 0.758867 0.825202 11.00000 -1.50000 AFIX 0 C68 1 0.454473 0.546553 0.704747 11.00000 0.03368 0.03674 = 0.03163 -0.01103 0.00818 -0.01046 AFIX 137 H68A 2 0.423139 0.594229 0.685384 11.00000 -1.50000 H68B 2 0.401149 0.507694 0.707345 11.00000 -1.50000 H68C 2 0.502510 0.524175 0.682579 11.00000 -1.50000 AFIX 0 HKLF 4 REM erk9313.res in P2(1)/c REM R1 = 0.1005 for 5397 Fo > 4sig(Fo) and 0.1655 for all 9189 data REM 651 parameters refined using 0 restraints END WGHT 0.0379 16.0501 REM Highest difference peak 0.364, deepest hole -0.303, 1-sigma level 0.070 Q1 1 0.5005 0.6183 0.6100 11.00000 0.05 0.36 Q2 1 0.8230 0.5557 0.4248 11.00000 0.05 0.34 Q3 1 0.9818 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-0.87 0.00 -7 16 14 -0.82 0.00 4 16 14 -2.26 0.00 -5 17 14 1.54 0.00 2 17 14 -0.03 0.00 11 5 15 -0.72 0.00 -14 6 15 -0.73 0.00 -13 7 15 -0.85 0.00 10 8 15 0.36 0.00 -13 9 15 0.58 0.00 7 13 15 1.11 0.00 6 14 15 -0.63 0.00 -8 15 15 0.86 0.00 3 16 15 -1.00 0.00 -3 17 15 1.13 0.00 0 17 15 -0.28 0.00 11 1 16 0.06 0.00 11 2 16 -0.19 0.00 -14 5 16 0.36 0.00 10 7 16 0.46 0.00 -13 8 16 0.27 0.00 9 9 16 -0.47 0.00 -12 10 16 -1.06 0.00 8 11 16 -1.18 0.00 4 15 16 1.68 0.00 2 16 16 -1.25 0.00 -14 4 17 -0.64 0.00 10 5 17 0.61 0.00 9 8 17 -0.21 0.00 8 10 17 1.09 0.00 -11 11 17 -0.56 0.00 -8 14 17 0.05 0.00 -4 16 17 -0.86 0.00 -3 16 17 0.07 0.00 0 16 17 -0.36 0.00 -14 0 18 0.00 0.00 10 0 18 -0.77 0.00 -14 1 18 -0.65 0.00 10 1 18 -0.33 0.00 -14 2 18 0.28 0.00 10 2 18 -0.36 0.00 6 11 18 -0.73 0.00 -5 15 18 0.54 0.00 1 15 18 -0.54 0.00 9 4 19 0.05 0.00 -13 5 19 0.96 0.00 -10 11 19 -0.09 0.00 -9 12 19 2.10 0.00 -8 13 19 1.30 0.00 -6 14 19 -0.19 0.00 2 14 19 -0.20 0.00 -3 15 19 -0.52 0.00 -2 15 19 0.17 0.00 -1 15 19 0.74 0.00 -13 3 20 0.10 0.00 7 8 20 0.45 0.00 -10 10 20 -0.58 0.00 -7 13 20 -0.12 0.00 -4 14 20 0.10 0.00 0 14 20 0.41 0.00 8 1 21 1.39 0.00 8 2 21 0.69 0.00 -12 5 21 0.06 0.00 7 6 21 0.48 0.00 6 8 21 0.19 0.00 -7 12 21 -0.01 0.00 -5 13 21 -0.78 0.00 -2 13 21 -0.44 0.00 6 2 22 0.01 0.00 -12 3 22 2.08 0.00 7 3 22 -1.18 0.00 6 5 22 -0.79 0.00 -11 6 22 0.95 0.00 -10 8 22 -0.77 0.00 1 12 22 -0.39 0.00 -11 4 23 -0.54 0.00 6 4 23 0.63 0.00 4 8 23 0.17 0.00 -7 9 23 -0.38 0.00 2 10 23 0.58 0.00 -6 11 23 -0.70 0.00 -11 0 24 -1.76 0.00 4 1 24 0.39 0.00 5 4 24 0.40 0.00 -10 5 24 -1.13 0.00 4 6 24 -0.40 0.00 -9 7 24 -0.72 0.00 -4 7 24 1.05 0.00 -8 8 24 -0.31 0.00 -7 9 24 1.04 0.00 0 10 24 -1.15 0.00 -10 1 25 0.23 0.00 -10 2 25 1.64 0.00 4 3 25 -0.45 0.00 -9 5 25 -0.52 0.00 2 7 25 0.84 0.00 1 8 25 0.05 0.00 -5 9 25 -0.35 0.00 -1 9 25 0.82 0.00 -9 0 26 0.98 0.00 2 0 26 1.46 0.00 -9 1 26 -0.15 0.00 1 1 26 -0.31 0.00 3 1 26 -0.31 0.00 3 2 26 0.47 0.00 -8 4 26 -0.27 0.00 2 5 26 0.31 0.00 -7 6 26 -0.12 0.00 1 6 26 1.06 0.00 -6 7 26 0.77 0.00 0 7 26 0.53 0.00 -3 8 26 -0.60 0.00 -2 8 26 -0.27 0.00 1 1 27 -0.80 0.00 -7 3 27 2.32 0.00 -2 3 27 1.23 0.00 1 3 27 -1.22 0.00 -3 4 27 0.37 0.00 -5 5 27 1.53 0.00 -1 5 27 -0.90 0.00 -4 6 27 0.93 0.00 -3 6 27 1.77 0.00 -2 6 27 1.87 0.00 -5 0 28 -1.53 0.00 -1 0 28 -1.42 0.00 -5 1 28 0.96 0.00 -1 1 28 -1.32 0.00 -4 2 28 -0.44 0.00 -3 2 28 -0.39 0.00 -2 2 28 -0.63 0.00 -3 3 28 -0.32 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 160617) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 27 1 ' ' 2 0.000 0.000 0.500 203 48 ' ' 3 0.000 0.500 0.000 203 48 ' ' 4 0.000 0.500 0.500 27 1 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta -2 1 1 7.156 -1 1 1 4.398 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) A badly disordered half pentane molecule was found in the asymmetrical unit and could not be satisfactorily refined. The program SQUEEZE (Spek, A.L. (2015). Acta Cryst. C71, 9-18) was therefore used to remove mathematically the effect of the solvent. The quoted formula and derived parameters are not included the squeezed solvent molecule. ) ) TITL erk9313 P 21/c R = 0.13 CELL 13.3489 16.9297 23.6112 90.00 101.32 90.00 SPGR P21/c # Solvent Accessible Volume = 462 # Electrons Found in S.A.V. = 98 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 1.003 0.028 0.488 ! 3.30 eA-3 C102 0.957 0.029 0.449 ! 2.84 eA-3 C103 0.923 1.001 0.397 ! 2.62 eA-3 C104 0.139 0.451 0.072 ! 1.61 eA-3 C105 0.049 0.078 0.499 ! 1.21 eA-3 C106 0.997 0.075 0.485 ! 1.13 eA-3 C107 0.094 0.423 0.024 ! 1.10 eA-3 C108 0.874 0.013 0.459 ! 0.94 eA-3 C109 1.000 0.926 0.466 ! 0.94 eA-3 Q110 0.082 0.528 0.151 ! 0.87 eA-3 Q111 0.064 0.360 0.007 ! 0.85 eA-3 Q112 0.090 0.091 0.464 ! 0.81 eA-3 Q113 0.137 0.560 0.132 ! 0.78 eA-3 Q114 0.230 0.393 0.094 ! 0.73 eA-3 Q115 0.981 0.138 0.336 ! 0.73 eA-3 Q116 0.512 0.766 0.472 ! 0.73 eA-3 Q117 0.077 0.417 0.075 ! 0.72 eA-3 Q118 0.032 0.933 0.678 ! 0.71 eA-3 Q119 0.951 0.029 0.595 ! 0.71 eA-3 Q120 0.763 0.030 0.752 ! 0.70 eA-3 Q121 0.938 0.419 0.049 ! 0.70 eA-3 Q122 0.249 0.456 0.133 ! 0.69 eA-3 Q123 0.606 0.264 0.200 ! 0.69 eA-3 Q124 0.885 0.529 0.848 ! 0.69 eA-3 Q125 0.141 0.895 0.043 ! 0.68 eA-3 Q126 0.344 0.988 0.146 ! 0.67 eA-3 Q127 0.644 0.267 0.403 ! 0.66 eA-3 Q128 0.406 0.814 0.971 ! 0.66 eA-3 Q129 0.251 0.861 0.471 ! 0.66 eA-3 Q130 1.000 0.974 0.377 ! 0.66 eA-3 Q131 0.312 0.657 0.608 ! 0.65 eA-3 Q132 0.907 0.889 0.797 ! 0.65 eA-3 Q133 0.015 0.834 0.040 ! 0.64 eA-3 Q134 0.947 0.083 0.357 ! 0.64 eA-3 Q135 0.877 0.093 0.432 ! 0.64 eA-3 Q136 0.026 0.191 0.366 ! 0.64 eA-3 Q137 0.263 0.531 0.697 ! 0.64 eA-3 Q138 0.877 0.406 0.927 ! 0.64 eA-3 Q139 0.926 0.637 0.945 ! 0.64 eA-3 Q140 0.684 0.551 0.649 ! 0.64 eA-3 Q141 0.829 0.974 0.474 ! 0.64 eA-3 Q142 0.357 0.965 0.207 ! 0.63 eA-3 Q143 0.233 0.940 0.822 ! 0.63 eA-3 C144 0.938 0.092 0.448 ! 0.63 eA-3 Q145 0.517 0.986 0.112 ! 0.63 eA-3 Q146 0.036 0.600 0.432 ! 0.63 eA-3 Q147 0.299 0.787 0.729 ! 0.63 eA-3 Q148 0.251 0.957 0.678 ! 0.63 eA-3 Q149 0.733 0.097 0.728 ! 0.62 eA-3 Q150 0.184 0.062 0.082 ! 0.62 eA-3 Q151 0.826 0.484 0.682 ! 0.62 eA-3 Q152 0.200 0.731 0.035 ! 0.62 eA-3 Q153 0.371 0.592 0.249 ! 0.61 eA-3 Q154 0.843 0.590 0.490 ! 0.61 eA-3 Q155 0.918 0.655 0.042 ! 0.61 eA-3 Q156 0.014 0.173 0.826 ! 0.61 eA-3 Q157 0.980 0.379 0.514 ! 0.61 eA-3 Q158 0.782 0.955 0.273 ! 0.61 eA-3 Q159 0.112 0.877 0.381 ! 0.61 eA-3 Q160 0.344 0.439 0.065 ! 0.60 eA-3 Q161 0.219 0.591 0.711 ! 0.60 eA-3 Q162 0.297 0.453 0.387 ! 0.60 eA-3 Q163 0.233 0.707 0.933 ! 0.60 eA-3 Q164 0.530 0.356 0.678 ! 0.60 eA-3 Q165 0.121 0.656 0.360 ! 0.60 eA-3 Q166 0.379 0.940 0.984 ! 0.60 eA-3 Q167 0.465 0.205 0.997 ! 0.60 eA-3 Q168 0.858 0.654 0.464 ! 0.59 eA-3 Q169 0.360 0.754 0.543 ! 0.59 eA-3 Q170 0.297 0.687 0.416 ! 0.59 eA-3 Q171 1.004 0.922 0.046 ! 0.59 eA-3 Q172 0.028 0.814 0.447 ! 0.59 eA-3 Q173 0.253 0.388 0.170 ! 0.59 eA-3 Q174 0.453 0.424 0.412 ! 0.59 eA-3 Q175 0.826 0.821 0.760 ! 0.59 eA-3 Q176 0.578 0.047 0.371 ! 0.59 eA-3 Q177 0.766 0.719 0.317 ! 0.58 eA-3 Q178 0.553 0.254 0.430 ! 0.58 eA-3 Q179 0.295 0.326 0.689 ! 0.58 eA-3 Q180 0.659 0.470 0.143 ! 0.58 eA-3 Q181 0.050 0.393 0.608 ! 0.58 eA-3 Q182 0.500 0.890 0.590 ! 0.58 eA-3 Q183 0.191 0.382 0.132 ! 0.58 eA-3 Q184 0.828 0.831 0.298 ! 0.58 eA-3 Q185 0.939 0.657 0.075 ! 0.58 eA-3 Q186 0.618 0.833 0.521 ! 0.58 eA-3 Q187 0.858 0.670 0.337 ! 0.57 eA-3 Q188 0.128 0.911 0.479 ! 0.57 eA-3 Q189 0.105 0.781 0.195 ! 0.57 eA-3 Q190 0.250 0.453 0.100 ! 0.57 eA-3 Q191 0.203 0.816 0.979 ! 0.57 eA-3 Q192 0.728 0.229 0.928 ! 0.57 eA-3 Q193 0.905 0.765 0.661 ! 0.57 eA-3 Q194 0.439 0.155 0.945 ! 0.57 eA-3 Q195 0.792 0.953 0.319 ! 0.57 eA-3 Q196 0.048 0.705 0.418 ! 0.57 eA-3 Q197 0.221 0.296 0.025 ! 0.57 eA-3 Q198 0.844 0.510 0.463 ! 0.57 eA-3 Q199 0.314 1.001 0.560 ! 0.57 eA-3 ) ; _shelx_fab_checksum 2896 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P P1 0.32395(10) 0.82038(9) 0.76194(6) 0.0306(3) Uani d . . . 1 . . C C1 0.4501(4) 0.7701(3) 0.7850(2) 0.0303(13) Uani d . . . 1 . . H H1A 0.4845 0.789 0.8236 0.036 Uiso calc U . R 1 . . H H1B 0.4407 0.7122 0.7868 0.036 Uiso calc U . R 1 . . C C2 0.5122(4) 0.7901(3) 0.7409(2) 0.0291(13) Uani d . . . 1 . . H H2 0.5049 0.8435 0.7283 0.035 Uiso calc U . R 1 . . C C3 0.5764(4) 0.7482(3) 0.7153(2) 0.0264(12) Uani d . . . 1 . . C C4 0.6306(4) 0.7829(3) 0.6706(2) 0.0244(12) Uani d . . . 1 . . C C5 0.6732(4) 0.6435(3) 0.6928(2) 0.0244(12) Uani d . . . 1 . . C C11 0.2347(4) 0.7905(3) 0.8089(2) 0.0297(13) Uani d . . . 1 . . C C12 0.2574(4) 0.7532(3) 0.8630(2) 0.0321(14) Uani d . . . 1 . . C C13 0.1775(4) 0.7367(4) 0.8922(3) 0.0374(15) Uani d . . . 1 . . H H13 0.1932 0.7106 0.9285 0.045 Uiso calc U . R 1 . . C C14 0.0767(4) 0.7570(4) 0.8700(3) 0.0419(16) Uani d . . . 1 . . C C15 0.0559(4) 0.7960(4) 0.8185(3) 0.0398(16) Uani d . . . 1 . . H H15 -0.0127 0.8109 0.8031 0.048 Uiso calc U . R 1 . . C C16 0.1322(4) 0.8147(4) 0.7872(2) 0.0317(13) Uani d . . . 1 . . C C17 0.3627(4) 0.7264(4) 0.8928(2) 0.0374(15) Uani d . . . 1 . . H H17A 0.3839 0.6812 0.872 0.056 Uiso calc U . R 1 . . H H17B 0.3609 0.7107 0.9326 0.056 Uiso calc U . R 1 . . H H17C 0.4114 0.7698 0.8933 0.056 Uiso calc U . R 1 . . C C18 -0.0060(4) 0.7387(5) 0.9040(3) 0.054(2) Uani d . . . 1 . . H H18A -0.049 0.7855 0.9047 0.082 Uiso calc U . R 1 . . H H18B 0.0257 0.724 0.9436 0.082 Uiso calc U . R 1 . . H H18C -0.0481 0.6949 0.8855 0.082 Uiso calc U . R 1 . . C C19 0.0998(4) 0.8597(4) 0.7317(2) 0.0383(15) Uani d . . . 1 . . H H19A 0.0916 0.8229 0.699 0.057 Uiso calc U . R 1 . . H H19B 0.1521 0.899 0.728 0.057 Uiso calc U . R 1 . . H H19C 0.0348 0.8864 0.7319 0.057 Uiso calc U . R 1 . . C C21 0.2774(4) 0.7646(3) 0.6949(2) 0.0314(13) Uani d . . . 1 . . C C22 0.2412(4) 0.6863(4) 0.6925(2) 0.0297(13) Uani d . . . 1 . . C C23 0.2056(4) 0.6508(4) 0.6398(2) 0.0315(13) Uani d . . . 1 . . H H23 0.1819 0.5978 0.6393 0.038 Uiso calc U . R 1 . . C C24 0.2027(4) 0.6891(4) 0.5877(2) 0.0376(15) Uani d . . . 1 . . C C25 0.2396(4) 0.7661(4) 0.5903(3) 0.0409(16) Uani d . . . 1 . . H H25 0.2397 0.7935 0.5552 0.049 Uiso calc U . R 1 . . C C26 0.2761(4) 0.8043(4) 0.6418(2) 0.0354(14) Uani d . . . 1 . . C C27 0.2399(4) 0.6369(3) 0.7459(2) 0.0337(14) Uani d . . . 1 . . H H27A 0.1811 0.6519 0.7627 0.051 Uiso calc U . R 1 . . H H27B 0.3031 0.6459 0.7742 0.051 Uiso calc U . R 1 . . H H27C 0.2347 0.5808 0.7353 0.051 Uiso calc U . R 1 . . C C28 0.1634(5) 0.6489(4) 0.5319(3) 0.0542(19) Uani d . . . 1 . . H H28A 0.1913 0.6746 0.5012 0.081 Uiso calc U . R 1 . . H H28B 0.0887 0.6522 0.523 0.081 Uiso calc U . R 1 . . H H28C 0.1843 0.5933 0.5348 0.081 Uiso calc U . R 1 . . C C29 0.3180(5) 0.8868(4) 0.6391(3) 0.0440(16) Uani d . . . 1 . . H H29A 0.3928 0.8848 0.6465 0.066 Uiso calc U . R 1 . . H H29B 0.2957 0.92 0.6683 0.066 Uiso calc U . R 1 . . H H29C 0.2928 0.9092 0.6007 0.066 Uiso calc U . R 1 . . B B1 0.7039(4) 0.7145(4) 0.6528(3) 0.0249(14) Uani d . . . 1 . . H H1 0.782(3) 0.728(2) 0.6737(16) 0.003(10) Uiso d . . . 1 . . C C31 0.6983(4) 0.6915(3) 0.5846(2) 0.0265(12) Uani d . . . 1 . . C C32 0.6131(4) 0.6586(3) 0.5477(2) 0.0236(12) Uani d . . . 1 . . C C33 0.6167(4) 0.6276(3) 0.4939(2) 0.0303(13) Uani d . . . 1 . . H H33 0.557 0.6051 0.471 0.036 Uiso calc U . R 1 . . C C34 0.7071(4) 0.6291(3) 0.4731(2) 0.0304(13) Uani d . . . 1 . . C C35 0.7906(4) 0.6661(3) 0.5053(2) 0.0310(13) Uani d . . . 1 . . H H35 0.8518 0.6698 0.4906 0.037 Uiso calc U . R 1 . . C C36 0.7870(4) 0.6981(3) 0.5588(2) 0.0248(12) Uani d . . . 1 . . C C37 0.5064(4) 0.6535(3) 0.5604(2) 0.0284(13) Uani d . . . 1 . . F F1 0.4920(2) 0.6888(2) 0.60781(14) 0.0484(10) Uani d . . . 1 . . F F2 0.4371(2) 0.6842(2) 0.51760(13) 0.0506(10) Uani d . . . 1 . . F F3 0.4756(3) 0.5787(2) 0.56386(17) 0.0540(10) Uani d . . . 1 . . C C38 0.7098(4) 0.5901(4) 0.4169(2) 0.0366(15) Uani d . . . 1 . . F F4 0.6312(3) 0.6114(2) 0.37503(14) 0.0520(10) Uani d . . . 1 . . F F5 0.7046(3) 0.5123(2) 0.41938(15) 0.0549(10) Uani d . . . 1 . . F F6 0.7940(3) 0.6082(2) 0.39654(15) 0.0555(11) Uani d . . . 1 . . C C39 0.8814(4) 0.7406(4) 0.5889(2) 0.0323(14) Uani d . . . 1 . . F F7 0.9460(2) 0.7534(2) 0.55175(14) 0.0424(9) Uani d . . . 1 . . F F8 0.9370(2) 0.7018(2) 0.63358(14) 0.0390(8) Uani d . . . 1 . . F F9 0.8624(2) 0.81235(19) 0.60781(13) 0.0364(8) Uani d . . . 1 . . N N1 0.6134(3) 0.8545(3) 0.65770(18) 0.0280(10) Uani d . . . 1 . . C C41 0.6658(4) 0.9005(3) 0.6226(2) 0.0278(13) Uani d . . . 1 . . C C42 0.7530(4) 0.9411(4) 0.6520(3) 0.0341(14) Uani d . . . 1 . . C C43 0.7969(5) 0.9972(4) 0.6212(3) 0.0467(18) Uani d . . . 1 . . H H43 0.8554 1.0255 0.6402 0.056 Uiso calc U . R 1 . . C C44 0.7574(5) 1.0127(4) 0.5634(3) 0.0527(19) Uani d . . . 1 . . H H44 0.7885 1.0511 0.5431 0.063 Uiso calc U . R 1 . . C C45 0.6725(5) 0.9717(4) 0.5359(3) 0.0424(16) Uani d . . . 1 . . H H45 0.6456 0.982 0.4963 0.051 Uiso calc U . R 1 . . C C46 0.6252(4) 0.9152(4) 0.5649(2) 0.0346(14) Uani d . . . 1 . . C C47 0.7973(4) 0.9232(4) 0.7137(3) 0.0390(15) Uani d . . . 1 . . H H47A 0.8241 0.8692 0.7169 0.059 Uiso calc U . R 1 . . H H47B 0.7441 0.9283 0.7368 0.059 Uiso calc U . R 1 . . H H47C 0.8528 0.9604 0.728 0.059 Uiso calc U . R 1 . . C C48 0.5322(4) 0.8719(4) 0.5340(2) 0.0393(15) Uani d . . . 1 . . H H48A 0.5529 0.8217 0.519 0.059 Uiso calc U . R 1 . . H H48B 0.4964 0.9042 0.5018 0.059 Uiso calc U . R 1 . . H H48C 0.4865 0.8614 0.5609 0.059 Uiso calc U . R 1 . . N N2 0.7094(3) 0.5709(3) 0.70039(19) 0.0263(10) Uani d . . . 1 . . H H2A 0.687(5) 0.536(4) 0.730(3) 0.08(2) Uiso d . . . 1 . . C C51 0.7936(4) 0.5414(3) 0.6754(2) 0.0265(12) Uani d . . . 1 . . C C52 0.7726(4) 0.4906(3) 0.6286(2) 0.0308(13) Uani d . . . 1 . . C C53 0.8555(5) 0.4640(4) 0.6052(3) 0.0425(16) Uani d . . . 1 . . H H53 0.8438 0.4298 0.5727 0.051 Uiso calc U . R 1 . . C C54 0.9530(5) 0.4872(4) 0.6290(3) 0.0460(17) Uani d . . . 1 . . H H54 1.0081 0.4704 0.6118 0.055 Uiso calc U . R 1 . . C C55 0.9723(4) 0.5341(3) 0.6770(3) 0.0370(15) Uani d . . . 1 . . H H55 1.0407 0.5481 0.6936 0.044 Uiso calc U . R 1 . . C C56 0.8926(4) 0.5617(3) 0.7018(2) 0.0273(12) Uani d . . . 1 . . C C57 0.6663(4) 0.4609(4) 0.6043(3) 0.0421(16) Uani d . . . 1 . . H H57A 0.6686 0.4246 0.5722 0.063 Uiso calc U . R 1 . . H H57B 0.6217 0.5057 0.5903 0.063 Uiso calc U . R 1 . . H H57C 0.6395 0.433 0.6345 0.063 Uiso calc U . R 1 . . C C58 0.9162(4) 0.6123(4) 0.7549(3) 0.0425(16) Uani d . . . 1 . . H H58A 0.8899 0.6658 0.7455 0.064 Uiso calc U . R 1 . . H H58B 0.9903 0.6146 0.7687 0.064 Uiso calc U . R 1 . . H H58C 0.8838 0.5897 0.785 0.064 Uiso calc U . R 1 . . N N3 0.6079(3) 0.6691(3) 0.72599(17) 0.0244(10) Uani d . . . 1 . . C C61 0.5856(4) 0.6247(3) 0.7744(2) 0.0263(12) Uani d . . . 1 . . C C62 0.6375(4) 0.6451(3) 0.8294(2) 0.0278(13) Uani d . . . 1 . . C C63 0.6103(4) 0.6071(3) 0.8758(2) 0.0319(13) Uani d . . . 1 . . H H63 0.6445 0.62 0.9138 0.038 Uiso calc U . R 1 . . C C64 0.5334(4) 0.5502(3) 0.8678(3) 0.0338(14) Uani d . . . 1 . . H H64 0.5147 0.5254 0.9003 0.041 Uiso calc U . R 1 . . C C65 0.4841(4) 0.5298(3) 0.8123(2) 0.0322(14) Uani d . . . 1 . . H H65 0.4325 0.4903 0.8067 0.039 Uiso calc U . R 1 . . C C66 0.5108(4) 0.5674(3) 0.7646(2) 0.0261(12) Uani d . . . 1 . . C C67 0.7188(4) 0.7080(4) 0.8391(2) 0.0332(14) Uani d . . . 1 . . H H67A 0.7727 0.6943 0.8181 0.05 Uiso calc U . R 1 . . H H67B 0.748 0.7119 0.8805 0.05 Uiso calc U . R 1 . . H H67C 0.6885 0.7589 0.8252 0.05 Uiso calc U . R 1 . . C C68 0.4545(4) 0.5466(4) 0.7047(2) 0.0338(14) Uani d . . . 1 . . H H68A 0.4231 0.5942 0.6854 0.051 Uiso calc U . R 1 . . H H68B 0.4011 0.5077 0.7073 0.051 Uiso calc U . R 1 . . H H68C 0.5025 0.5242 0.6826 0.051 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P1 0.0249(7) 0.0320(9) 0.0363(8) -0.0001(6) 0.0098(6) -0.0042(7) C1 0.025(3) 0.037(4) 0.033(3) -0.002(2) 0.014(2) -0.006(3) C2 0.029(3) 0.031(4) 0.028(3) -0.004(2) 0.007(2) -0.002(2) C3 0.018(3) 0.031(3) 0.032(3) -0.004(2) 0.008(2) -0.004(3) C4 0.020(3) 0.028(3) 0.024(3) -0.004(2) 0.001(2) -0.001(2) C5 0.021(3) 0.028(3) 0.024(3) -0.005(2) 0.004(2) -0.006(2) C11 0.020(3) 0.032(4) 0.036(3) 0.004(2) 0.005(2) -0.006(3) C12 0.029(3) 0.031(4) 0.038(3) -0.004(2) 0.009(3) -0.013(3) C13 0.039(3) 0.038(4) 0.038(4) -0.005(3) 0.015(3) -0.008(3) C14 0.029(3) 0.048(4) 0.054(4) -0.005(3) 0.021(3) -0.021(3) C15 0.023(3) 0.044(4) 0.055(4) -0.007(3) 0.015(3) -0.018(3) C16 0.028(3) 0.033(4) 0.036(3) 0.002(3) 0.011(2) -0.007(3) C17 0.035(3) 0.049(4) 0.030(3) 0.004(3) 0.012(3) -0.006(3) C18 0.028(3) 0.082(6) 0.058(4) -0.011(3) 0.020(3) -0.009(4) C19 0.023(3) 0.043(4) 0.048(4) 0.008(3) 0.006(3) -0.004(3) C21 0.025(3) 0.030(4) 0.043(4) 0.000(2) 0.018(3) -0.003(3) C22 0.017(3) 0.042(4) 0.032(3) 0.003(2) 0.010(2) -0.007(3) C23 0.027(3) 0.031(4) 0.035(3) 0.000(2) 0.002(2) -0.011(3) C24 0.032(3) 0.052(5) 0.025(3) 0.011(3) -0.005(2) -0.004(3) C25 0.038(3) 0.051(5) 0.035(4) 0.006(3) 0.012(3) 0.002(3) C26 0.028(3) 0.043(4) 0.038(4) 0.004(3) 0.012(3) -0.002(3) C27 0.028(3) 0.032(4) 0.044(4) -0.006(2) 0.015(3) -0.007(3) C28 0.063(5) 0.057(5) 0.041(4) 0.005(4) 0.005(3) -0.012(3) C29 0.043(4) 0.041(4) 0.051(4) -0.004(3) 0.017(3) 0.004(3) B1 0.022(3) 0.023(4) 0.031(4) 0.003(3) 0.009(3) 0.000(3) C31 0.029(3) 0.022(3) 0.030(3) 0.000(2) 0.009(2) 0.000(2) C32 0.020(3) 0.026(3) 0.026(3) -0.002(2) 0.007(2) 0.002(2) C33 0.031(3) 0.030(4) 0.030(3) -0.004(2) 0.006(2) -0.004(3) C34 0.031(3) 0.030(4) 0.031(3) -0.004(2) 0.009(2) -0.004(3) C35 0.033(3) 0.025(3) 0.039(3) 0.000(2) 0.016(3) 0.000(3) C36 0.025(3) 0.022(3) 0.029(3) 0.001(2) 0.007(2) 0.002(2) C37 0.028(3) 0.031(4) 0.027(3) -0.003(2) 0.006(2) -0.003(3) F1 0.0252(17) 0.080(3) 0.042(2) -0.0077(17) 0.0110(15) -0.0222(19) F2 0.0305(18) 0.084(3) 0.0351(19) 0.0109(19) 0.0026(15) 0.0109(19) F3 0.043(2) 0.034(2) 0.093(3) -0.0069(17) 0.032(2) 0.000(2) C38 0.036(3) 0.041(4) 0.034(3) -0.006(3) 0.012(3) -0.004(3) F4 0.055(2) 0.065(3) 0.034(2) 0.0057(19) 0.0045(17) -0.0114(18) F5 0.090(3) 0.029(2) 0.050(2) -0.0029(19) 0.024(2) -0.0097(17) F6 0.053(2) 0.074(3) 0.048(2) -0.013(2) 0.0320(19) -0.018(2) C39 0.030(3) 0.035(4) 0.037(3) -0.004(3) 0.020(3) 0.003(3) F7 0.0317(17) 0.050(2) 0.053(2) -0.0112(16) 0.0254(16) -0.0060(17) F8 0.0249(16) 0.041(2) 0.050(2) -0.0003(15) 0.0056(15) 0.0071(17) F9 0.0297(17) 0.029(2) 0.053(2) -0.0060(14) 0.0126(15) -0.0105(16) N1 0.026(2) 0.029(3) 0.031(3) 0.003(2) 0.010(2) -0.002(2) C41 0.030(3) 0.023(3) 0.035(3) 0.006(2) 0.017(3) 0.002(2) C42 0.025(3) 0.032(4) 0.048(4) -0.002(3) 0.014(3) -0.013(3) C43 0.044(4) 0.029(4) 0.077(5) -0.008(3) 0.035(4) -0.018(3) C44 0.066(5) 0.041(5) 0.065(5) -0.005(4) 0.045(4) -0.004(4) C45 0.063(4) 0.025(4) 0.048(4) 0.006(3) 0.031(3) 0.007(3) C46 0.043(3) 0.031(4) 0.034(3) 0.004(3) 0.019(3) 0.003(3) C47 0.030(3) 0.030(4) 0.058(4) 0.001(3) 0.009(3) -0.015(3) C48 0.041(3) 0.040(4) 0.036(4) 0.002(3) 0.007(3) 0.003(3) N2 0.025(2) 0.025(3) 0.032(3) 0.000(2) 0.011(2) -0.001(2) C51 0.025(3) 0.029(3) 0.028(3) 0.001(2) 0.010(2) 0.003(2) C52 0.041(3) 0.030(4) 0.022(3) 0.002(3) 0.010(3) 0.002(2) C53 0.069(5) 0.029(4) 0.037(4) 0.006(3) 0.026(3) -0.007(3) C54 0.042(4) 0.040(4) 0.062(5) 0.012(3) 0.026(3) 0.002(3) C55 0.030(3) 0.026(4) 0.057(4) 0.003(3) 0.015(3) 0.001(3) C56 0.025(3) 0.028(3) 0.027(3) 0.003(2) 0.003(2) 0.004(2) C57 0.046(4) 0.036(4) 0.041(4) -0.004(3) 0.001(3) 0.000(3) C58 0.029(3) 0.046(4) 0.048(4) -0.004(3) -0.001(3) -0.005(3) N3 0.025(2) 0.021(3) 0.029(2) 0.0024(18) 0.0088(19) 0.0035(19) C61 0.026(3) 0.030(4) 0.024(3) 0.000(2) 0.010(2) -0.001(2) C62 0.026(3) 0.032(4) 0.026(3) 0.003(2) 0.007(2) -0.001(2) C63 0.034(3) 0.032(4) 0.031(3) 0.003(3) 0.009(3) -0.002(3) C64 0.035(3) 0.029(4) 0.041(4) 0.002(3) 0.018(3) 0.006(3) C65 0.031(3) 0.031(4) 0.038(3) -0.006(3) 0.015(3) 0.000(3) C66 0.027(3) 0.022(3) 0.031(3) 0.000(2) 0.011(2) 0.001(2) C67 0.029(3) 0.041(4) 0.029(3) -0.007(3) 0.003(2) -0.005(3) C68 0.034(3) 0.037(4) 0.032(3) -0.010(3) 0.008(3) -0.011(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C21 P1 C11 . . 103.1(2) ? C21 P1 C1 . . 98.6(2) ? C11 P1 C1 . . 110.5(2) ? C2 C1 P1 . . 106.6(4) ? C2 C1 H1A . . 110.4 ? P1 C1 H1A . . 110.4 ? C2 C1 H1B . . 110.4 ? P1 C1 H1B . . 110.4 ? H1A C1 H1B . . 108.6 ? C3 C2 C1 . . 133.2(5) ? C3 C2 H2 . . 113.4 ? C1 C2 H2 . . 113.4 ? C2 C3 N3 . . 128.0(5) ? C2 C3 C4 . . 122.9(5) ? N3 C3 C4 . . 109.0(4) ? N1 C4 C3 . . 117.0(5) ? N1 C4 B1 . . 135.5(5) ? C3 C4 B1 . . 107.4(4) ? N2 C5 N3 . . 118.7(5) ? N2 C5 B1 . . 129.7(5) ? N3 C5 B1 . . 111.3(5) ? C12 C11 C16 . . 118.5(5) ? C12 C11 P1 . . 128.3(4) ? C16 C11 P1 . . 113.1(4) ? C11 C12 C13 . . 119.2(5) ? C11 C12 C17 . . 125.0(5) ? C13 C12 C17 . . 115.8(5) ? C14 C13 C12 . . 122.6(6) ? C14 C13 H13 . . 118.7 ? C12 C13 H13 . . 118.7 ? C15 C14 C13 . . 117.9(5) ? C15 C14 C18 . . 121.8(6) ? C13 C14 C18 . . 120.2(6) ? C14 C15 C16 . . 122.4(5) ? C14 C15 H15 . . 118.8 ? C16 C15 H15 . . 118.8 ? C15 C16 C11 . . 119.3(5) ? C15 C16 C19 . . 117.3(5) ? C11 C16 C19 . . 123.4(5) ? C12 C17 H17A . . 109.5 ? C12 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C12 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C14 C18 H18A . . 109.5 ? C14 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C14 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? C16 C19 H19A . . 109.5 ? C16 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C16 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? C22 C21 C26 . . 117.7(5) ? C22 C21 P1 . . 124.9(4) ? C26 C21 P1 . . 117.4(4) ? C23 C22 C21 . . 120.1(5) ? C23 C22 C27 . . 116.8(5) ? C21 C22 C27 . . 123.1(5) ? C22 C23 C24 . . 122.8(6) ? C22 C23 H23 . . 118.6 ? C24 C23 H23 . . 118.6 ? C23 C24 C25 . . 116.8(5) ? C23 C24 C28 . . 121.1(6) ? C25 C24 C28 . . 122.0(6) ? C26 C25 C24 . . 122.7(6) ? C26 C25 H25 . . 118.7 ? C24 C25 H25 . . 118.7 ? C25 C26 C21 . . 119.8(6) ? C25 C26 C29 . . 117.8(6) ? C21 C26 C29 . . 122.3(5) ? C22 C27 H27A . . 109.5 ? C22 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C22 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C24 C28 H28A . . 109.5 ? C24 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C24 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C26 C29 H29A . . 109.5 ? C26 C29 H29B . . 109.5 ? H29A C29 H29B . . 109.5 ? C26 C29 H29C . . 109.5 ? H29A C29 H29C . . 109.5 ? H29B C29 H29C . . 109.5 ? C4 B1 C5 . . 98.2(4) ? C4 B1 C31 . . 120.6(5) ? C5 B1 C31 . . 115.1(5) ? C4 B1 H1 . . 108.(2) ? C5 B1 H1 . . 103.(2) ? C31 B1 H1 . . 111.(2) ? C32 C31 C36 . . 113.8(4) ? C32 C31 B1 . . 125.2(4) ? C36 C31 B1 . . 120.8(4) ? C33 C32 C31 . . 123.4(4) ? C33 C32 C37 . . 111.3(4) ? C31 C32 C37 . . 125.4(4) ? C32 C33 C34 . . 120.4(5) ? C32 C33 H33 . . 119.8 ? C34 C33 H33 . . 119.8 ? C35 C34 C33 . . 118.8(5) ? C35 C34 C38 . . 122.5(5) ? C33 C34 C38 . . 118.8(5) ? C34 C35 C36 . . 121.0(5) ? C34 C35 H35 . . 119.5 ? C36 C35 H35 . . 119.5 ? C35 C36 C31 . . 122.3(5) ? C35 C36 C39 . . 116.3(4) ? C31 C36 C39 . . 121.4(5) ? F1 C37 F2 . . 105.8(4) ? F1 C37 F3 . . 106.2(4) ? F2 C37 F3 . . 103.9(4) ? F1 C37 C32 . . 116.3(4) ? F2 C37 C32 . . 111.6(4) ? F3 C37 C32 . . 112.2(4) ? F5 C38 F6 . . 107.4(5) ? F5 C38 F4 . . 105.1(5) ? F6 C38 F4 . . 105.3(5) ? F5 C38 C34 . . 113.0(5) ? F6 C38 C34 . . 112.7(5) ? F4 C38 C34 . . 112.6(5) ? F9 C39 F8 . . 107.2(5) ? F9 C39 F7 . . 104.8(4) ? F8 C39 F7 . . 105.2(4) ? F9 C39 C36 . . 113.3(4) ? F8 C39 C36 . . 115.0(5) ? F7 C39 C36 . . 110.5(4) ? C4 N1 C41 . . 125.6(4) ? C46 C41 C42 . . 121.5(5) ? C46 C41 N1 . . 122.0(5) ? C42 C41 N1 . . 115.8(5) ? C43 C42 C41 . . 117.8(6) ? C43 C42 C47 . . 121.4(5) ? C41 C42 C47 . . 120.8(5) ? C44 C43 C42 . . 121.7(6) ? C44 C43 H43 . . 119.2 ? C42 C43 H43 . . 119.2 ? C45 C44 C43 . . 119.1(6) ? C45 C44 H44 . . 120.4 ? C43 C44 H44 . . 120.4 ? C44 C45 C46 . . 121.5(6) ? C44 C45 H45 . . 119.2 ? C46 C45 H45 . . 119.2 ? C41 C46 C45 . . 118.5(6) ? C41 C46 C48 . . 121.1(5) ? C45 C46 C48 . . 120.4(5) ? C42 C47 H47A . . 109.5 ? C42 C47 H47B . . 109.5 ? H47A C47 H47B . . 109.5 ? C42 C47 H47C . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? C46 C48 H48A . . 109.5 ? C46 C48 H48B . . 109.5 ? H48A C48 H48B . . 109.5 ? C46 C48 H48C . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? C5 N2 C51 . . 123.7(5) ? C5 N2 H2A . . 119.(4) ? C51 N2 H2A . . 116.(4) ? C52 C51 C56 . . 122.5(5) ? C52 C51 N2 . . 119.0(5) ? C56 C51 N2 . . 118.4(5) ? C51 C52 C53 . . 117.4(5) ? C51 C52 C57 . . 122.6(5) ? C53 C52 C57 . . 119.9(5) ? C54 C53 C52 . . 120.4(6) ? C54 C53 H53 . . 119.8 ? C52 C53 H53 . . 119.8 ? C55 C54 C53 . . 121.0(5) ? C55 C54 H54 . . 119.5 ? C53 C54 H54 . . 119.5 ? C54 C55 C56 . . 120.6(6) ? C54 C55 H55 . . 119.7 ? C56 C55 H55 . . 119.7 ? C51 C56 C55 . . 117.8(5) ? C51 C56 C58 . . 122.8(5) ? C55 C56 C58 . . 119.4(5) ? C52 C57 H57A . . 109.5 ? C52 C57 H57B . . 109.5 ? H57A C57 H57B . . 109.5 ? C52 C57 H57C . . 109.5 ? H57A C57 H57C . . 109.5 ? H57B C57 H57C . . 109.5 ? C56 C58 H58A . . 109.5 ? C56 C58 H58B . . 109.5 ? H58A C58 H58B . . 109.5 ? C56 C58 H58C . . 109.5 ? H58A C58 H58C . . 109.5 ? H58B C58 H58C . . 109.5 ? C5 N3 C3 . . 113.9(4) ? C5 N3 C61 . . 123.2(5) ? C3 N3 C61 . . 122.2(4) ? C66 C61 C62 . . 122.9(5) ? C66 C61 N3 . . 119.2(5) ? C62 C61 N3 . . 117.8(5) ? C63 C62 C61 . . 117.7(5) ? C63 C62 C67 . . 120.2(5) ? C61 C62 C67 . . 122.0(5) ? C62 C63 C64 . . 121.2(5) ? C62 C63 H63 . . 119.4 ? C64 C63 H63 . . 119.4 ? C65 C64 C63 . . 119.9(5) ? C65 C64 H64 . . 120.1 ? C63 C64 H64 . . 120.1 ? C64 C65 C66 . . 119.8(5) ? C64 C65 H65 . . 120.1 ? C66 C65 H65 . . 120.1 ? C61 C66 C65 . . 118.4(5) ? C61 C66 C68 . . 122.2(5) ? C65 C66 C68 . . 119.3(5) ? C62 C67 H67A . . 109.5 ? C62 C67 H67B . . 109.5 ? H67A C67 H67B . . 109.5 ? C62 C67 H67C . . 109.5 ? H67A C67 H67C . . 109.5 ? H67B C67 H67C . . 109.5 ? C66 C68 H68A . . 109.5 ? C66 C68 H68B . . 109.5 ? H68A C68 H68B . . 109.5 ? C66 C68 H68C . . 109.5 ? H68A C68 H68C . . 109.5 ? H68B C68 H68C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1 C21 . 1.844(6) ? P1 C11 . 1.849(5) ? P1 C1 . 1.871(5) ? C1 C2 . 1.491(7) ? C1 H1A . 0.99 ? C1 H1B . 0.99 ? C2 C3 . 1.344(7) ? C2 H2 . 0.95 ? C3 N3 . 1.411(7) ? C3 C4 . 1.511(7) ? C4 N1 . 1.261(7) ? C4 B1 . 1.624(8) ? C5 N2 . 1.321(7) ? C5 N3 . 1.353(6) ? C5 B1 . 1.630(8) ? C11 C12 . 1.403(8) ? C11 C16 . 1.425(7) ? C12 C13 . 1.406(7) ? C12 C17 . 1.513(7) ? C13 C14 . 1.388(8) ? C13 H13 . 0.95 ? C14 C15 . 1.364(9) ? C14 C18 . 1.518(8) ? C15 C16 . 1.407(7) ? C15 H15 . 0.95 ? C16 C19 . 1.503(8) ? C17 H17A . 0.98 ? C17 H17B . 0.98 ? C17 H17C . 0.98 ? C18 H18A . 0.98 ? C18 H18B . 0.98 ? C18 H18C . 0.98 ? C19 H19A . 0.98 ? C19 H19B . 0.98 ? C19 H19C . 0.98 ? C21 C22 . 1.408(8) ? C21 C26 . 1.419(8) ? C22 C23 . 1.378(7) ? C22 C27 . 1.517(8) ? C23 C24 . 1.385(8) ? C23 H23 . 0.95 ? C24 C25 . 1.390(9) ? C24 C28 . 1.483(8) ? C25 C26 . 1.378(8) ? C25 H25 . 0.95 ? C26 C29 . 1.511(8) ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 H29A . 0.98 ? C29 H29B . 0.98 ? C29 H29C . 0.98 ? B1 C31 . 1.644(8) ? B1 H1 . 1.08(4) ? C31 C32 . 1.404(7) ? C31 C36 . 1.437(7) ? C32 C33 . 1.385(7) ? C32 C37 . 1.515(7) ? C33 C34 . 1.389(7) ? C33 H33 . 0.95 ? C34 C35 . 1.371(7) ? C34 C38 . 1.489(8) ? C35 C36 . 1.386(7) ? C35 H35 . 0.95 ? C36 C39 . 1.503(7) ? C37 F1 . 1.316(6) ? C37 F2 . 1.334(6) ? C37 F3 . 1.339(6) ? C38 F5 . 1.322(7) ? C38 F6 . 1.341(6) ? C38 F4 . 1.342(6) ? C39 F9 . 1.335(6) ? C39 F8 . 1.338(6) ? C39 F7 . 1.363(5) ? N1 C41 . 1.418(6) ? C41 C46 . 1.388(7) ? C41 C42 . 1.411(7) ? C42 C43 . 1.393(8) ? C42 C47 . 1.492(8) ? C43 C44 . 1.389(9) ? C43 H43 . 0.95 ? C44 C45 . 1.379(9) ? C44 H44 . 0.95 ? C45 C46 . 1.397(8) ? C45 H45 . 0.95 ? C46 C48 . 1.502(8) ? C47 H47A . 0.98 ? C47 H47B . 0.98 ? C47 H47C . 0.98 ? C48 H48A . 0.98 ? C48 H48B . 0.98 ? C48 H48C . 0.98 ? N2 C51 . 1.456(6) ? N2 H2A . 1.00(7) ? C51 C52 . 1.385(7) ? C51 C56 . 1.390(7) ? C52 C53 . 1.404(8) ? C52 C57 . 1.509(8) ? C53 C54 . 1.371(9) ? C53 H53 . 0.95 ? C54 C55 . 1.367(8) ? C54 H54 . 0.95 ? C55 C56 . 1.390(7) ? C55 H55 . 0.95 ? C56 C58 . 1.500(8) ? C57 H57A . 0.98 ? C57 H57B . 0.98 ? C57 H57C . 0.98 ? C58 H58A . 0.98 ? C58 H58B . 0.98 ? C58 H58C . 0.98 ? N3 C61 . 1.447(6) ? C61 C66 . 1.379(7) ? C61 C62 . 1.391(7) ? C62 C63 . 1.378(7) ? C62 C67 . 1.505(7) ? C63 C64 . 1.393(8) ? C63 H63 . 0.95 ? C64 C65 . 1.392(8) ? C64 H64 . 0.95 ? C65 C66 . 1.399(7) ? C65 H65 . 0.95 ? C66 C68 . 1.507(7) ? C67 H67A . 0.98 ? C67 H67B . 0.98 ? C67 H67C . 0.98 ? C68 H68A . 0.98 ? C68 H68B . 0.98 ? C68 H68C . 0.98 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C21 P1 C1 C2 . . . . 66.0(4) ? C11 P1 C1 C2 . . . . 173.5(4) ? P1 C1 C2 C3 . . . . -139.5(6) ? C1 C2 C3 N3 . . . . -3.3(10) ? C1 C2 C3 C4 . . . . 179.5(5) ? C2 C3 C4 N1 . . . . 0.1(8) ? N3 C3 C4 N1 . . . . -177.6(4) ? C2 C3 C4 B1 . . . . 177.6(5) ? N3 C3 C4 B1 . . . . 0.0(6) ? C21 P1 C11 C12 . . . . 120.4(5) ? C1 P1 C11 C12 . . . . 15.9(6) ? C21 P1 C11 C16 . . . . -64.3(5) ? C1 P1 C11 C16 . . . . -168.8(4) ? C16 C11 C12 C13 . . . . 3.8(8) ? P1 C11 C12 C13 . . . . 178.9(4) ? C16 C11 C12 C17 . . . . -177.9(5) ? P1 C11 C12 C17 . . . . -2.8(9) ? C11 C12 C13 C14 . . . . -1.0(9) ? C17 C12 C13 C14 . . . . -179.5(5) ? C12 C13 C14 C15 . . . . -1.4(9) ? C12 C13 C14 C18 . . . . -179.1(6) ? C13 C14 C15 C16 . . . . 1.0(9) ? C18 C14 C15 C16 . . . . 178.7(6) ? C14 C15 C16 C11 . . . . 1.8(9) ? C14 C15 C16 C19 . . . . -178.4(6) ? C12 C11 C16 C15 . . . . -4.2(8) ? P1 C11 C16 C15 . . . . 180.0(4) ? C12 C11 C16 C19 . . . . 176.1(5) ? P1 C11 C16 C19 . . . . 0.2(7) ? C11 P1 C21 C22 . . . . -39.2(5) ? C1 P1 C21 C22 . . . . 74.3(5) ? C11 P1 C21 C26 . . . . 139.4(4) ? C1 P1 C21 C26 . . . . -107.1(4) ? C26 C21 C22 C23 . . . . -0.3(7) ? P1 C21 C22 C23 . . . . 178.3(4) ? C26 C21 C22 C27 . . . . 179.0(5) ? P1 C21 C22 C27 . . . . -2.3(7) ? C21 C22 C23 C24 . . . . -0.4(8) ? C27 C22 C23 C24 . . . . -179.8(5) ? C22 C23 C24 C25 . . . . 1.1(8) ? C22 C23 C24 C28 . . . . -179.7(5) ? C23 C24 C25 C26 . . . . -1.1(8) ? C28 C24 C25 C26 . . . . 179.8(6) ? C24 C25 C26 C21 . . . . 0.4(8) ? C24 C25 C26 C29 . . . . 177.7(5) ? C22 C21 C26 C25 . . . . 0.4(8) ? P1 C21 C26 C25 . . . . -178.4(4) ? C22 C21 C26 C29 . . . . -176.8(5) ? P1 C21 C26 C29 . . . . 4.5(7) ? N1 C4 B1 C5 . . . . 179.0(6) ? C3 C4 B1 C5 . . . . 2.2(5) ? N1 C4 B1 C31 . . . . -55.3(9) ? C3 C4 B1 C31 . . . . 127.9(5) ? N2 C5 B1 C4 . . . . -176.9(5) ? N3 C5 B1 C4 . . . . -3.9(5) ? N2 C5 B1 C31 . . . . 53.7(7) ? N3 C5 B1 C31 . . . . -133.3(4) ? C4 B1 C31 C32 . . . . -64.2(8) ? C5 B1 C31 C32 . . . . 53.1(7) ? C4 B1 C31 C36 . . . . 121.1(6) ? C5 B1 C31 C36 . . . . -121.5(5) ? C36 C31 C32 C33 . . . . 6.6(8) ? B1 C31 C32 C33 . . . . -168.4(5) ? C36 C31 C32 C37 . . . . -172.3(5) ? B1 C31 C32 C37 . . . . 12.7(9) ? C31 C32 C33 C34 . . . . -1.2(9) ? C37 C32 C33 C34 . . . . 177.7(5) ? C32 C33 C34 C35 . . . . -3.9(9) ? C32 C33 C34 C38 . . . . 175.8(5) ? C33 C34 C35 C36 . . . . 3.1(9) ? C38 C34 C35 C36 . . . . -176.6(5) ? C34 C35 C36 C31 . . . . 2.8(9) ? C34 C35 C36 C39 . . . . -177.2(5) ? C32 C31 C36 C35 . . . . -7.3(8) ? B1 C31 C36 C35 . . . . 167.9(5) ? C32 C31 C36 C39 . . . . 172.6(5) ? B1 C31 C36 C39 . . . . -12.1(8) ? C33 C32 C37 F1 . . . . -173.2(5) ? C31 C32 C37 F1 . . . . 5.8(8) ? C33 C32 C37 F2 . . . . -51.7(6) ? C31 C32 C37 F2 . . . . 127.2(6) ? C33 C32 C37 F3 . . . . 64.3(6) ? C31 C32 C37 F3 . . . . -116.7(6) ? C35 C34 C38 F5 . . . . 109.9(6) ? C33 C34 C38 F5 . . . . -69.7(7) ? C35 C34 C38 F6 . . . . -12.1(9) ? C33 C34 C38 F6 . . . . 168.3(5) ? C35 C34 C38 F4 . . . . -131.1(6) ? C33 C34 C38 F4 . . . . 49.2(8) ? C35 C36 C39 F9 . . . . 130.0(5) ? C31 C36 C39 F9 . . . . -50.0(7) ? C35 C36 C39 F8 . . . . -106.2(5) ? C31 C36 C39 F8 . . . . 73.8(7) ? C35 C36 C39 F7 . . . . 12.7(7) ? C31 C36 C39 F7 . . . . -167.3(5) ? C3 C4 N1 C41 . . . . 171.5(5) ? B1 C4 N1 C41 . . . . -5.1(10) ? C4 N1 C41 C46 . . . . 100.0(7) ? C4 N1 C41 C42 . . . . -90.3(7) ? C46 C41 C42 C43 . . . . 0.4(8) ? N1 C41 C42 C43 . . . . -169.4(5) ? C46 C41 C42 C47 . . . . -178.4(5) ? N1 C41 C42 C47 . . . . 11.7(7) ? C41 C42 C43 C44 . . . . -0.4(9) ? C47 C42 C43 C44 . . . . 178.4(5) ? C42 C43 C44 C45 . . . . 0.1(9) ? C43 C44 C45 C46 . . . . 0.3(10) ? C42 C41 C46 C45 . . . . 0.0(8) ? N1 C41 C46 C45 . . . . 169.1(5) ? C42 C41 C46 C48 . . . . -179.8(5) ? N1 C41 C46 C48 . . . . -10.6(8) ? C44 C45 C46 C41 . . . . -0.3(9) ? C44 C45 C46 C48 . . . . 179.4(6) ? N3 C5 N2 C51 . . . . -168.2(5) ? B1 C5 N2 C51 . . . . 4.4(8) ? C5 N2 C51 C52 . . . . -105.1(6) ? C5 N2 C51 C56 . . . . 78.8(7) ? C56 C51 C52 C53 . . . . -4.7(8) ? N2 C51 C52 C53 . . . . 179.4(5) ? C56 C51 C52 C57 . . . . 172.5(5) ? N2 C51 C52 C57 . . . . -3.4(8) ? C51 C52 C53 C54 . . . . 1.0(9) ? C57 C52 C53 C54 . . . . -176.4(6) ? C52 C53 C54 C55 . . . . 2.4(10) ? C53 C54 C55 C56 . . . . -2.1(10) ? C52 C51 C56 C55 . . . . 5.0(8) ? N2 C51 C56 C55 . . . . -179.1(5) ? C52 C51 C56 C58 . . . . -175.8(5) ? N2 C51 C56 C58 . . . . 0.1(8) ? C54 C55 C56 C51 . . . . -1.5(9) ? C54 C55 C56 C58 . . . . 179.3(6) ? N2 C5 N3 C3 . . . . 178.3(4) ? B1 C5 N3 C3 . . . . 4.4(6) ? N2 C5 N3 C61 . . . . 8.0(7) ? B1 C5 N3 C61 . . . . -165.9(5) ? C2 C3 N3 C5 . . . . 179.7(5) ? C4 C3 N3 C5 . . . . -2.8(6) ? C2 C3 N3 C61 . . . . -9.9(8) ? C4 C3 N3 C61 . . . . 167.6(4) ? C5 N3 C61 C66 . . . . -85.1(6) ? C3 N3 C61 C66 . . . . 105.4(6) ? C5 N3 C61 C62 . . . . 98.3(6) ? C3 N3 C61 C62 . . . . -71.2(6) ? C66 C61 C62 C63 . . . . -1.6(8) ? N3 C61 C62 C63 . . . . 174.9(5) ? C66 C61 C62 C67 . . . . -179.8(5) ? N3 C61 C62 C67 . . . . -3.4(8) ? C61 C62 C63 C64 . . . . 0.0(8) ? C67 C62 C63 C64 . . . . 178.3(5) ? C62 C63 C64 C65 . . . . 1.3(8) ? C63 C64 C65 C66 . . . . -1.1(8) ? C62 C61 C66 C65 . . . . 1.8(8) ? N3 C61 C66 C65 . . . . -174.6(5) ? C62 C61 C66 C68 . . . . 179.4(5) ? N3 C61 C66 C68 . . . . 3.0(8) ? C64 C65 C66 C61 . . . . -0.4(8) ? C64 C65 C66 C68 . . . . -178.1(5) ?