#------------------------------------------------------------------------------ #$Date: 2024-10-03 01:11:26 +0300 (Thu, 03 Oct 2024) $ #$Revision: 294990 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572734.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_1572734 loop_ _publ_author_name 'Shibutani, Yuki' 'Kusumoto, Shuhei' 'Nozaki, Kyoko' _publ_section_title ; Fully Conjugated Tetraborylethylene: Selenium Mediated C--C Double Bond Formation from Diborylcarbenoid ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05928J _journal_year 2024 _chemical_formula_moiety 'C62 H64 B4 N4 S, C3 H7' _chemical_formula_sum 'C65 H71 B4 N4 S' _chemical_formula_weight 983.55 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-07-09 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-09-02 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.896(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.6639(6) _cell_length_b 16.1414(7) _cell_length_c 23.3110(10) _cell_measurement_reflns_used 11706 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 27.8170 _cell_measurement_theta_min 2.5220 _cell_volume 5880.3(4) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 93(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.882 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -49.00 -24.00 0.50 90.00 -- 5.00 55.00-180.00 50 2 \w 26.00 93.00 0.50 90.00 -- 5.00 55.00-180.00 134 3 \w -90.00 -64.00 0.50 90.00 -- -8.20 37.00-120.00 52 4 \w -35.00 81.00 0.50 90.00 -- -8.20 37.00 -60.00 232 5 \w -71.00 -17.00 0.50 90.00 -- -8.20 9.00 30.00 108 6 \w -42.00 -16.00 0.50 90.00 -- -8.20 9.00 60.00 52 7 \w -34.00 77.00 0.50 90.00 -- -8.20 37.00-120.00 222 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0444345000 _diffrn_orient_matrix_UB_12 0.0074665000 _diffrn_orient_matrix_UB_13 0.0014481000 _diffrn_orient_matrix_UB_21 -0.0054041000 _diffrn_orient_matrix_UB_22 -0.0008065000 _diffrn_orient_matrix_UB_23 -0.0304566000 _diffrn_orient_matrix_UB_31 -0.0075638000 _diffrn_orient_matrix_UB_32 -0.0432818000 _diffrn_orient_matrix_UB_33 0.0008087000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_unetI/netI 0.0692 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.882 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 64257 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.882 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.877 _diffrn_reflns_theta_min 2.459 _diffrn_source_type 'Rigaku (Mo) X-ray DW Source' _exptl_absorpt_coefficient_mu 0.097 _exptl_crystal_density_diffrn 1.111 _exptl_crystal_description block _exptl_crystal_F_000 2100 _refine_diff_density_max 0.673 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 680 _refine_ls_number_reflns 13621 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0561 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+3.1250P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.1424 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8799 _reflns_number_total 13621 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05928j3.cif _cod_data_source_block compound3S _cod_database_code 1572734 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula C60H60B4N4S _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C63(H63A,H63B), C64(H64A,H64B) 2.b Aromatic/amide H refined with riding coordinates: C22(H22), C44(H44), C16(H16), C32(H32), C26(H26), C14(H14), C62(H62), C46(H46), C23(H23), C5(H5), C35(H35), C58(H58), C28(H28), C56(H56), C29(H29), C30(H30), C60(H60), C25(H25), C7(H7), C61(H61), C31(H31), C24(H24), C52(H52), C55(H55), C59(H59), C37(H37), C53(H53), C54(H54) 2.c Idealised Me refined as rotating group: C50(H50A,H50B,H50C), C18(H18A,H18B,H18C), C48(H48A,H48B,H48C), C39(H39A,H39B, H39C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C41(H41A, H41B,H41C), C19(H19A,H19B,H19C), C49(H49A,H49B,H49C), C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C65(H65A,H65B,H65C) ; _shelx_res_file ; TITL s_allene_auto_a.res in P2(1)/n s_allene_auto.res created by SHELXL-2017/1 at 10:12:18 on 09-Jul-2024 REM Old TITL S_allene_auto in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.155, Rweak 0.008, Alpha 0.034 REM 0.429 for 451 systematic absences, Orientation as input REM Formula found by SHELXT: C48 C1 S CELL 0.71073 15.663935 16.141417 23.310956 90 93.8959 90 ZERR 4 0.000642 0.000716 0.001034 0 0.0039 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B N S UNIT 260 284 16 16 4 L.S. 4 PLAN 14 TEMP -180(2) CONF MORE -1 BOND $H fmap 2 acta OMIT 0 1 2 OMIT 1 1 1 REM REM REM WGHT 0.057900 3.125000 FVAR 0.15805 S1 5 0.707406 0.651054 0.745941 11.00000 0.01933 0.02537 = 0.01796 -0.00200 0.00333 0.00008 N1 4 0.716082 0.601739 0.585492 11.00000 0.01626 0.02857 = 0.01810 -0.00259 0.00119 -0.00600 N2 4 0.802286 0.634733 0.591969 11.00000 0.01708 0.02947 = 0.01835 -0.00387 0.00370 -0.00492 N3 4 0.760068 0.704953 0.904767 11.00000 0.02066 0.02493 = 0.01954 -0.00347 0.00500 0.00445 N4 4 0.845930 0.677043 0.895167 11.00000 0.01910 0.02622 = 0.01863 -0.00183 0.00361 0.00421 C13 1 0.994620 0.659752 0.665106 11.00000 0.02210 0.02426 = 0.01397 -0.00032 0.00417 -0.00127 C21 1 0.673310 0.608171 0.529567 11.00000 0.02066 0.02451 = 0.01640 -0.00434 0.00315 0.00056 C42 1 0.933766 0.603827 0.819495 11.00000 0.02182 0.02630 = 0.01340 -0.00112 0.00172 0.00212 C12 1 0.915652 0.701447 0.662455 11.00000 0.02123 0.02390 = 0.01396 -0.00269 0.00414 -0.00305 C3 1 0.583429 0.582104 0.651054 11.00000 0.02008 0.02939 = 0.01456 -0.00288 0.00089 -0.00313 C27 1 0.853967 0.621388 0.544233 11.00000 0.01929 0.03150 = 0.01560 -0.00103 0.00295 0.00032 C47 1 1.012906 0.641145 0.811054 11.00000 0.02292 0.02933 = 0.01339 -0.00032 0.00177 0.00026 C57 1 0.892882 0.643488 0.944735 11.00000 0.02705 0.02239 = 0.01575 -0.00403 0.00286 0.00454 C51 1 0.749547 0.751595 0.955787 11.00000 0.02961 0.02310 = 0.01447 0.00037 0.00202 0.00773 C4 1 0.563205 0.506845 0.677520 11.00000 0.02425 0.02871 = 0.01786 -0.00048 -0.00108 -0.00530 C33 1 0.608488 0.722355 0.846223 11.00000 0.02318 0.02577 = 0.01606 -0.00216 0.00368 0.00165 C2 1 0.764882 0.672813 0.805536 11.00000 0.02255 0.02047 = 0.01821 0.00065 0.00368 0.00033 C1 1 0.748899 0.634441 0.684157 11.00000 0.02146 0.02209 = 0.01990 -0.00124 0.00225 -0.00037 C22 1 0.620411 0.544251 0.509358 11.00000 0.02462 0.02540 = 0.02229 -0.00051 0.00113 -0.00066 AFIX 43 H22 2 0.613020 0.496667 0.532486 11.00000 -1.20000 AFIX 0 C44 1 1.000539 0.469532 0.810102 11.00000 0.03321 0.02493 = 0.02315 0.00203 0.00818 0.00499 AFIX 43 H44 2 0.995813 0.410875 0.808848 11.00000 -1.20000 AFIX 0 C43 1 0.927799 0.516757 0.818017 11.00000 0.02438 0.02762 = 0.01840 -0.00164 0.00435 0.00201 C8 1 0.519918 0.643484 0.644059 11.00000 0.02440 0.03220 = 0.02032 -0.00076 0.00135 -0.00283 C34 1 0.579032 0.802105 0.831562 11.00000 0.02457 0.02867 = 0.01882 -0.00420 0.00451 0.00369 C50 1 1.019898 0.734048 0.809127 11.00000 0.02732 0.02875 = 0.02188 -0.00209 0.00435 -0.00337 AFIX 137 H50A 2 0.993325 0.754442 0.772549 11.00000 -1.50000 H50B 2 1.080361 0.750121 0.812572 11.00000 -1.50000 H50C 2 0.990561 0.758096 0.841003 11.00000 -1.50000 AFIX 0 C16 1 0.992823 0.831879 0.667580 11.00000 0.03599 0.01999 = 0.02569 0.00203 -0.00078 -0.00729 AFIX 43 H16 2 0.992010 0.890717 0.668335 11.00000 -1.20000 AFIX 0 C32 1 0.901690 0.685823 0.523813 11.00000 0.02414 0.02722 = 0.02324 -0.00122 0.00231 -0.00330 AFIX 43 H32 2 0.901258 0.738672 0.541725 11.00000 -1.20000 AFIX 0 C26 1 0.684060 0.678050 0.495734 11.00000 0.02292 0.02570 = 0.02378 -0.00343 0.00300 -0.00123 AFIX 43 H26 2 0.719628 0.722257 0.509817 11.00000 -1.20000 AFIX 0 C38 1 0.548382 0.658121 0.849478 11.00000 0.02624 0.02761 = 0.02332 -0.00103 0.00638 -0.00125 C14 1 1.070410 0.704981 0.669097 11.00000 0.01833 0.03572 = 0.02043 0.00095 0.00458 0.00102 AFIX 43 H14 2 1.123411 0.676157 0.671391 11.00000 -1.20000 AFIX 0 C17 1 0.915580 0.788790 0.664243 11.00000 0.02795 0.02472 = 0.02104 -0.00224 -0.00087 0.00044 C62 1 0.979732 0.660118 0.953555 11.00000 0.02761 0.02842 = 0.02201 -0.00321 0.00167 0.00169 AFIX 43 H62 2 1.007512 0.693353 0.926817 11.00000 -1.20000 AFIX 0 C18 1 0.996891 0.566600 0.663052 11.00000 0.02860 0.02522 = 0.02426 -0.00288 0.00153 0.00162 AFIX 137 H18A 2 0.970467 0.544061 0.696631 11.00000 -1.50000 H18B 2 1.056414 0.547824 0.663322 11.00000 -1.50000 H18C 2 0.965271 0.547252 0.627866 11.00000 -1.50000 AFIX 0 C46 1 1.084385 0.591845 0.804160 11.00000 0.01872 0.03961 = 0.02163 0.00214 0.00444 0.00043 AFIX 43 H46 2 1.137955 0.617658 0.799424 11.00000 -1.20000 AFIX 0 C23 1 0.578211 0.550057 0.455101 11.00000 0.02853 0.03014 = 0.02867 -0.00332 -0.00532 -0.00246 AFIX 43 H23 2 0.541371 0.506633 0.441306 11.00000 -1.20000 AFIX 0 C5 1 0.482113 0.495481 0.697132 11.00000 0.03125 0.03576 = 0.02219 0.00369 0.00173 -0.01192 AFIX 43 H5 2 0.469578 0.445143 0.715931 11.00000 -1.20000 AFIX 0 C35 1 0.491625 0.816253 0.821391 11.00000 0.02841 0.03362 = 0.02760 0.00159 0.00385 0.00788 AFIX 43 H35 2 0.472410 0.870220 0.810591 11.00000 -1.20000 AFIX 0 C58 1 0.852268 0.595988 0.984678 11.00000 0.02974 0.02557 = 0.02709 -0.00135 0.00503 0.00463 AFIX 43 H58 2 0.792836 0.584377 0.979016 11.00000 -1.20000 AFIX 0 C28 1 0.854384 0.543872 0.518097 11.00000 0.02491 0.02601 = 0.02095 0.00002 0.00365 -0.00271 AFIX 43 H28 2 0.821397 0.499785 0.532078 11.00000 -1.20000 AFIX 0 C56 1 0.813604 0.803943 0.978515 11.00000 0.03389 0.02380 = 0.02235 -0.00072 0.00562 -0.00053 AFIX 43 H56 2 0.865181 0.810242 0.959746 11.00000 -1.20000 AFIX 0 C15 1 1.070873 0.791032 0.669828 11.00000 0.02899 0.03417 = 0.02205 0.00098 0.00264 -0.01316 C45 1 1.079503 0.505793 0.804016 11.00000 0.02636 0.03560 = 0.02420 0.00490 0.00729 0.01094 C29 1 0.903313 0.531578 0.471531 11.00000 0.03288 0.02892 = 0.02479 -0.00492 0.00648 0.00292 AFIX 43 H29 2 0.904115 0.478781 0.453567 11.00000 -1.20000 AFIX 0 C30 1 0.950963 0.595890 0.451128 11.00000 0.03201 0.03879 = 0.02560 -0.00041 0.01338 0.00242 AFIX 43 H30 2 0.984393 0.587159 0.419158 11.00000 -1.20000 AFIX 0 C60 1 0.985901 0.581499 1.040969 11.00000 0.04446 0.03075 = 0.02254 -0.00079 -0.00497 0.01144 AFIX 43 H60 2 1.017689 0.560098 1.073838 11.00000 -1.20000 AFIX 0 C25 1 0.642620 0.682669 0.441504 11.00000 0.03061 0.02689 = 0.02673 0.00399 0.00207 0.00287 AFIX 43 H25 2 0.650501 0.729864 0.418095 11.00000 -1.20000 AFIX 0 C7 1 0.438926 0.628940 0.663377 11.00000 0.02374 0.04333 = 0.02831 0.00069 0.00289 0.00485 AFIX 43 H7 2 0.396254 0.670579 0.658090 11.00000 -1.20000 AFIX 0 C6 1 0.419072 0.555630 0.689991 11.00000 0.02333 0.05151 = 0.02472 0.00178 0.00419 -0.00688 C61 1 1.025945 0.628214 1.001401 11.00000 0.03013 0.03245 = 0.02643 -0.00420 -0.00459 0.00450 AFIX 43 H61 2 1.085622 0.638694 1.006876 11.00000 -1.20000 AFIX 0 C31 1 0.950185 0.672689 0.476984 11.00000 0.02793 0.03505 = 0.02709 0.00247 0.00894 -0.00527 AFIX 43 H31 2 0.982932 0.716733 0.462706 11.00000 -1.20000 AFIX 0 C24 1 0.589717 0.618921 0.421128 11.00000 0.03370 0.03330 = 0.02218 -0.00149 -0.00715 0.00517 AFIX 43 H24 2 0.561359 0.622463 0.383869 11.00000 -1.20000 AFIX 0 C52 1 0.673945 0.743114 0.983143 11.00000 0.02676 0.04105 = 0.02016 -0.00359 0.00366 0.00581 AFIX 43 H52 2 0.630350 0.706832 0.967905 11.00000 -1.20000 AFIX 0 C48 1 0.844270 0.473946 0.827349 11.00000 0.03153 0.02590 = 0.03521 -0.00204 0.00963 -0.00125 AFIX 137 H48A 2 0.823469 0.491927 0.864054 11.00000 -1.50000 H48B 2 0.853088 0.413837 0.828058 11.00000 -1.50000 H48C 2 0.801986 0.488261 0.795998 11.00000 -1.50000 AFIX 0 C55 1 0.801628 0.846886 1.028785 11.00000 0.04781 0.02374 = 0.02501 -0.00253 0.00055 0.00051 AFIX 43 H55 2 0.845715 0.882037 1.044756 11.00000 -1.20000 AFIX 0 C36 1 0.431863 0.753868 0.826572 11.00000 0.02274 0.04836 = 0.03484 0.00153 0.00272 0.00386 C59 1 0.899107 0.565818 1.032682 11.00000 0.04559 0.02773 = 0.02577 0.00570 0.00909 0.00715 AFIX 43 H59 2 0.871365 0.534012 1.060223 11.00000 -1.20000 AFIX 0 C37 1 0.461432 0.675108 0.840307 11.00000 0.02504 0.03940 = 0.03405 -0.00127 0.00483 -0.00809 AFIX 43 H37 2 0.421342 0.631481 0.843565 11.00000 -1.20000 AFIX 0 C53 1 0.662459 0.787855 1.032776 11.00000 0.03441 0.05434 = 0.02297 -0.00549 0.00810 0.01293 AFIX 43 H53 2 0.610254 0.783208 1.051023 11.00000 -1.20000 AFIX 0 C39 1 0.642142 0.871953 0.827551 11.00000 0.03057 0.02519 = 0.04410 0.00018 0.00408 0.00296 AFIX 137 H39A 2 0.660969 0.890852 0.866316 11.00000 -1.50000 H39B 2 0.614808 0.917941 0.805869 11.00000 -1.50000 H39C 2 0.691703 0.852503 0.807858 11.00000 -1.50000 AFIX 0 C11 1 0.538915 0.725248 0.617177 11.00000 0.03616 0.03517 = 0.04770 0.00802 0.01050 0.00548 AFIX 137 H11A 2 0.586997 0.751768 0.639150 11.00000 -1.50000 H11B 2 0.488362 0.760996 0.617335 11.00000 -1.50000 H11C 2 0.553802 0.716419 0.577479 11.00000 -1.50000 AFIX 0 C9 1 0.628965 0.438873 0.684987 11.00000 0.03729 0.03045 = 0.03596 0.00520 0.00122 -0.00320 AFIX 137 H9A 2 0.639092 0.415046 0.647382 11.00000 -1.50000 H9B 2 0.608009 0.395628 0.709978 11.00000 -1.50000 H9C 2 0.682561 0.461739 0.702455 11.00000 -1.50000 AFIX 0 C54 1 0.726596 0.839254 1.055904 11.00000 0.05112 0.03758 = 0.02064 -0.00941 0.00362 0.01304 AFIX 43 H54 2 0.718921 0.869112 1.090295 11.00000 -1.20000 AFIX 0 C20 1 0.831935 0.835805 0.661603 11.00000 0.03595 0.02846 = 0.04288 -0.00660 -0.00292 0.00480 AFIX 137 H20A 2 0.798296 0.821808 0.625937 11.00000 -1.50000 H20B 2 0.843547 0.895466 0.662520 11.00000 -1.50000 H20C 2 0.799737 0.820619 0.694643 11.00000 -1.50000 AFIX 0 B3 3 0.706810 0.701298 0.853424 11.00000 0.02295 0.01873 = 0.02021 0.00001 0.00384 0.00067 C41 1 0.577608 0.570371 0.860277 11.00000 0.03652 0.02984 = 0.04374 0.00343 0.00947 -0.00277 AFIX 137 H41A 2 0.597287 0.546822 0.824741 11.00000 -1.50000 H41B 2 0.529888 0.537313 0.872928 11.00000 -1.50000 H41C 2 0.624686 0.569820 0.890196 11.00000 -1.50000 AFIX 0 B2 3 0.828176 0.655879 0.649706 11.00000 0.02073 0.02140 = 0.02027 -0.00181 0.00359 0.00143 C19 1 1.154196 0.838418 0.673793 11.00000 0.03735 0.04691 = 0.04838 0.00008 0.00297 -0.02008 AFIX 137 H19A 2 1.143095 0.896737 0.664270 11.00000 -1.50000 H19B 2 1.192810 0.814934 0.646697 11.00000 -1.50000 H19C 2 1.180753 0.834334 0.712985 11.00000 -1.50000 AFIX 0 B4 3 0.853768 0.654743 0.836462 11.00000 0.02301 0.01940 = 0.02086 -0.00206 0.00589 -0.00235 B1 3 0.678666 0.602296 0.638853 11.00000 0.02390 0.02050 = 0.01924 0.00010 0.00249 0.00003 C49 1 1.158127 0.453495 0.797544 11.00000 0.03448 0.04785 = 0.05366 0.00596 0.01294 0.01632 AFIX 137 H49A 2 1.148029 0.397305 0.811495 11.00000 -1.50000 H49B 2 1.206930 0.477969 0.820014 11.00000 -1.50000 H49C 2 1.170478 0.451250 0.756921 11.00000 -1.50000 AFIX 0 C10 1 0.330723 0.540886 0.710762 11.00000 0.02833 0.08112 = 0.05384 0.01096 0.01515 -0.00756 AFIX 137 H10A 2 0.299305 0.502169 0.684730 11.00000 -1.50000 H10B 2 0.299670 0.593551 0.711376 11.00000 -1.50000 H10C 2 0.336071 0.517405 0.749609 11.00000 -1.50000 AFIX 0 C40 1 0.336600 0.771294 0.817715 11.00000 0.02510 0.07176 = 0.07375 0.01510 0.00124 0.00474 AFIX 137 H40A 2 0.321826 0.818219 0.841809 11.00000 -1.50000 H40B 2 0.304422 0.722230 0.828402 11.00000 -1.50000 H40C 2 0.322082 0.784678 0.777218 11.00000 -1.50000 AFIX 0 C63 1 0.468619 0.535738 0.998480 11.00000 0.13188 0.07039 = 0.05822 -0.00691 0.04223 -0.04309 AFIX 23 H63A 2 0.460689 0.554879 1.038115 11.00000 -1.20000 H63B 2 0.494142 0.582105 0.977736 11.00000 -1.20000 AFIX 0 C64 1 0.381957 0.516692 0.969460 11.00000 0.13783 0.07836 = 0.08356 -0.01827 0.04757 -0.05400 AFIX 23 H64A 2 0.357293 0.468607 0.988867 11.00000 -1.20000 H64B 2 0.389179 0.500717 0.929073 11.00000 -1.20000 AFIX 0 C65 1 0.318358 0.589691 0.970025 11.00000 0.12545 0.07720 = 0.11320 -0.00920 0.04353 -0.02534 AFIX 137 H65A 2 0.266398 0.575902 0.946139 11.00000 -1.50000 H65B 2 0.344717 0.639364 0.954734 11.00000 -1.50000 H65C 2 0.303581 0.600151 1.009559 11.00000 -1.50000 AFIX 0 HKLF 4 REM s_allene_auto_a.res in P2(1)/n REM R1 = 0.0561 for 8799 Fo > 4sig(Fo) and 0.1030 for all 13621 data REM 680 parameters refined using 0 restraints END WGHT 0.0579 3.1366 REM Highest difference peak 0.673, deepest hole -0.485, 1-sigma level 0.054 Q1 1 0.6996 0.7533 0.7086 11.00000 0.05 0.67 Q2 1 0.7937 0.7646 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0 4 -8 20.97 1.50 0 -4 -8 19.49 1.58 0 -4 8 21.46 1.43 0 4 8 21.18 1.65 0 -4 -9 12.24 1.19 0 4 9 10.53 1.13 0 -4 9 10.98 1.08 0 -4 -9 9.34 1.32 0 4 -9 10.06 1.16 0 4 9 13.24 1.29 0 4 10 257.86 13.91 0 -4 -10 240.91 13.90 0 -4 10 244.87 13.89 0 4 -10 226.24 13.89 0 4 10 246.71 13.94 0 -4 -11 6.39 1.09 0 4 11 8.70 1.04 0 4 -11 5.19 1.08 0 -4 11 5.52 0.93 0 4 11 10.81 1.28 0 4 12 81.32 4.87 0 -4 -12 87.37 4.88 0 -4 12 85.59 4.85 0 4 -12 75.95 4.87 0 4 12 80.20 4.92 0 -4 -13 6.49 1.14 0 4 13 6.33 1.10 0 4 -13 6.77 1.14 0 -4 13 8.24 1.05 0 4 13 8.48 1.24 0 -4 -14 0.99 1.03 0 4 14 0.73 0.97 0 4 -14 2.15 1.06 0 4 14 2.36 1.20 0 -4 14 2.02 0.93 0 4 14 2.25 1.16 0 -4 -15 54.03 3.25 0 4 15 53.56 3.26 0 4 -15 44.92 3.23 0 4 15 51.82 3.27 0 -4 15 50.50 3.19 0 4 15 54.79 3.28 0 -4 -16 2.19 1.18 0 4 16 0.45 1.12 0 4 -16 0.52 1.20 0 -4 -16 0.08 1.37 0 -4 16 0.48 1.04 0 4 16 1.66 1.26 0 4 16 1.31 1.25 0 4 17 38.76 2.60 0 -4 -17 37.87 2.61 0 -4 -17 36.75 2.69 0 -4 17 37.21 2.53 0 4 17 38.99 2.70 0 4 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41.70 0 5 3 784.37 41.73 0 -5 -3 712.66 41.70 0 5 4 0.75 0.63 0 -5 -4 0.56 0.69 0 5 -4 0.01 0.60 0 5 4 -0.02 0.74 0 -5 -4 0.09 0.83 0 5 -4 0.61 0.57 0 -5 -5 401.73 22.40 0 5 5 394.02 22.40 0 -5 -5 414.09 22.44 0 5 5 401.03 22.43 0 5 -5 374.19 22.39 0 5 -5 390.45 22.37 0 -5 -6 1.20 0.75 0 5 6 0.80 0.69 0 5 6 2.40 0.97 0 -5 -6 -0.30 0.83 0 5 -6 2.36 0.70 0 5 -6 1.15 0.47 0 5 6 0.95 1.07 0 5 -6 0.83 0.41 0 -5 -7 24.18 1.77 0 5 7 26.01 1.76 0 -5 -7 27.25 1.89 0 5 -7 27.02 1.74 0 5 7 27.61 1.88 0 -5 7 26.22 1.68 0 5 7 26.32 1.97 0 5 8 56.87 3.13 0 -5 -8 51.40 3.15 0 -5 -8 56.25 3.22 0 5 -8 48.60 3.12 0 -5 8 48.78 3.10 0 5 8 50.10 3.19 0 5 8 52.31 3.28 0 -5 -9 24.00 1.75 0 5 9 26.63 1.74 0 -5 9 21.93 1.65 0 5 -9 23.10 1.70 0 5 9 24.69 1.87 0 -5 -9 27.64 1.87 0 5 9 25.37 1.87 0 5 10 0.81 0.89 0 -5 -10 0.57 0.94 0 -5 10 0.90 0.79 0 5 -10 2.65 0.99 0 -5 -10 2.59 1.16 0 5 10 2.12 1.14 0 5 -11 5.14 1.07 0 -5 -11 5.51 1.03 0 5 11 5.08 0.98 0 -5 11 4.40 0.89 0 5 -11 5.41 0.98 0 -5 -11 4.35 1.20 0 5 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34.65 2.39 0 5 -21 31.51 2.45 0 5 21 26.36 2.50 0 -5 21 23.43 2.30 0 5 21 31.45 2.38 0 5 22 0.15 1.55 0 5 22 -1.75 1.79 0 -5 22 0.18 1.42 0 5 22 1.78 1.57 0 5 23 1.91 1.54 0 5 23 0.94 1.58 0 5 23 -0.49 1.90 0 -5 23 0.96 1.49 0 5 24 1.06 1.58 0 -5 24 0.30 1.53 0 5 24 0.44 1.96 0 5 25 4.81 2.07 0 -5 25 5.19 1.67 0 -5 26 -2.54 1.71 0 5 26 -0.07 1.99 0 5 27 1.42 2.12 0 -5 27 1.61 1.71 0 -5 28 7.03 1.89 0 5 28 6.97 2.28 0 -5 29 2.75 1.82 0 -5 30 1.30 1.91 0 6 0 444.70 25.34 0 6 0 445.47 25.34 0 6 -1 155.37 8.88 0 -6 1 153.40 8.85 0 6 1 158.86 8.87 0 6 -1 157.52 8.86 0 6 1 148.58 8.85 0 -6 2 146.96 8.64 0 6 -2 148.05 8.66 0 6 2 155.29 8.67 0 6 2 151.33 8.67 0 -6 -2 145.24 8.64 0 6 2 158.10 8.64 0 6 3 4.60 0.66 0 6 -3 3.43 0.80 0 -6 3 1.79 0.68 0 6 3 5.02 1.06 0 6 3 3.32 0.86 0 -6 -3 2.93 0.76 0 -6 -3 3.81 0.39 0 -6 -4 0.01 0.73 0 6 4 -0.31 0.65 0 6 -4 -0.59 0.71 0 6 4 0.08 0.82 0 6 5 90.68 4.99 0 6 -5 84.70 4.97 0 6 5 89.57 5.07 0 -6 -5 82.71 5.06 0 6 -5 83.83 4.98 0 -6 -5 84.54 5.00 0 6 6 62.74 3.36 0 -6 -6 52.85 3.37 0 -6 -6 61.29 3.45 0 6 6 55.77 3.43 0 6 -6 57.92 3.34 0 6 -6 57.44 3.28 0 6 -6 50.76 3.27 0 -6 -7 166.57 9.32 0 6 7 173.54 9.33 0 6 -7 159.60 9.30 0 6 7 181.21 9.38 0 -6 -7 160.22 9.38 0 6 7 158.98 9.40 0 6 -7 153.52 9.24 0 6 -7 163.53 9.25 0 6 8 11.06 1.13 0 -6 -8 10.75 1.13 0 6 8 11.55 1.46 0 6 -8 11.93 0.79 0 6 -8 11.38 1.13 0 6 8 12.19 1.32 0 -6 -8 10.80 1.28 0 -6 -9 3.18 0.92 0 6 9 3.14 0.86 0 6 9 3.82 1.24 0 6 9 2.76 1.08 0 -6 -9 4.12 1.14 0 6 -9 1.65 0.93 0 -6 9 3.62 0.80 0 -6 -10 17.64 1.38 0 6 10 15.32 1.31 0 6 10 20.57 1.61 0 6 10 16.91 1.59 0 6 -10 16.90 1.36 0 -6 -10 15.38 1.54 0 -6 10 14.38 1.24 0 6 11 24.66 1.67 0 -6 -11 23.41 1.67 0 6 11 25.47 1.83 0 6 -11 19.04 1.65 0 -6 -11 23.09 1.84 0 -6 11 20.44 1.59 0 6 11 24.53 1.85 0 6 -12 132.94 8.23 0 -6 -12 146.29 8.20 0 6 12 161.34 8.20 0 -6 12 132.77 8.16 0 -6 -12 147.78 8.26 0 6 -12 126.19 8.18 0 6 12 140.20 8.25 0 6 12 150.98 8.27 0 -6 -13 7.58 1.19 0 6 -13 9.24 1.29 0 6 13 11.40 1.18 0 -6 -13 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-0.22 0.79 0 -7 -7 2.35 1.08 0 7 7 0.84 1.06 0 7 -7 1.15 0.60 0 7 -7 0.90 0.56 0 7 8 13.35 1.12 0 -7 -8 13.30 1.13 0 7 -8 11.37 1.08 0 7 8 10.97 1.33 0 -7 -8 12.61 1.37 0 7 8 12.69 1.43 0 7 -8 10.78 0.83 0 7 -8 11.93 0.87 0 7 9 11.56 1.10 0 -7 -9 11.85 1.12 0 7 9 12.10 1.25 0 -7 -9 11.71 1.38 0 7 -9 10.62 1.09 0 7 9 11.75 1.47 0 7 -9 10.39 0.75 0 7 10 32.82 2.16 0 -7 -10 36.46 2.19 0 7 -10 28.36 2.15 0 -7 -10 32.32 2.31 0 7 10 35.99 2.32 0 7 10 37.90 2.42 0 7 11 12.02 1.18 0 -7 -11 9.84 1.17 0 7 11 11.58 1.50 0 7 11 12.72 1.36 0 7 -11 9.47 1.10 0 -7 -11 13.83 1.43 0 -7 -12 5.11 1.07 0 7 12 7.05 1.05 0 7 12 6.20 1.45 0 7 -12 6.99 1.04 0 7 12 5.02 1.31 0 -7 -12 5.73 1.27 0 -7 12 7.24 0.95 0 -7 -13 4.84 1.10 0 7 13 5.30 1.08 0 7 -13 3.97 1.23 0 7 13 5.79 1.38 0 7 -13 4.12 1.09 0 7 13 6.95 1.37 0 -7 -13 6.45 1.35 0 -7 13 3.24 0.92 0 -7 -14 4.08 1.17 0 7 14 0.22 1.12 0 7 -14 3.29 1.24 0 7 14 3.38 1.39 0 7 -14 2.86 1.10 0 7 14 3.40 1.40 0 -7 -14 5.08 1.33 0 -7 14 1.95 1.00 0 7 -15 7.09 1.39 0 7 15 8.01 1.22 0 -7 -15 6.23 1.28 0 7 15 4.15 1.43 0 7 -15 6.70 1.26 0 7 15 6.39 1.52 0 -7 -15 8.51 1.47 0 -7 15 5.71 1.15 0 -7 -16 -0.94 1.25 0 7 16 -0.07 1.19 0 7 -16 -1.09 1.34 0 7 -16 -0.41 1.23 0 -7 16 -0.03 1.07 0 -7 -16 0.97 1.44 0 7 16 1.51 1.50 0 7 17 36.66 2.39 0 -7 -17 30.77 2.37 0 7 -17 33.59 2.53 0 7 -17 31.14 2.34 0 -7 17 29.28 2.25 0 7 17 35.94 2.56 0 7 18 47.51 2.94 0 -7 -18 46.39 2.95 0 7 -18 36.30 2.91 0 -7 18 40.15 2.88 0 7 18 47.24 3.12 0 -7 -19 15.24 1.67 0 7 19 13.99 1.65 0 -7 19 10.65 1.53 0 7 -19 11.63 1.66 0 7 19 13.59 1.79 0 -7 -20 12.62 1.73 0 7 20 14.58 1.74 0 7 -20 12.09 1.75 0 -7 20 13.26 1.59 0 7 20 18.40 2.00 0 7 21 12.44 1.62 0 -7 21 10.42 1.57 0 7 -21 6.82 1.65 0 7 21 8.72 1.82 0 7 22 1.87 1.56 0 -7 22 1.90 1.43 0 7 22 0.21 1.66 0 7 23 2.31 1.60 0 -7 23 1.42 1.49 0 7 23 3.49 2.02 0 7 23 2.27 1.74 0 7 24 1.08 1.67 0 7 24 1.14 1.92 0 -7 24 0.65 1.48 0 7 25 -0.17 1.70 0 7 25 2.73 2.01 0 -7 25 2.91 1.57 0 7 26 6.94 2.21 0 -7 26 7.77 1.74 0 7 27 -1.57 2.24 0 -7 27 1.53 1.74 0 -7 28 -0.12 1.80 0 8 0 17.02 1.53 0 8 0 17.52 1.40 0 8 0 21.42 1.39 0 8 1 30.20 1.97 0 8 -1 29.37 2.00 0 8 1 30.42 2.11 0 8 1 28.66 1.96 0 8 -1 28.64 1.93 0 8 1 30.54 1.92 0 -8 2 18.13 1.50 0 8 2 21.43 1.58 0 8 2 21.79 1.78 0 8 -2 22.33 1.63 0 8 2 18.35 1.55 0 8 -2 21.71 1.26 0 8 2 23.59 1.50 0 8 3 19.51 1.55 0 -8 3 18.54 1.45 0 8 3 21.18 1.45 0 8 3 25.06 1.78 0 8 -3 19.33 1.57 0 8 3 21.47 1.55 0 -8 -3 19.31 1.47 0 8 4 2.18 0.78 0 8 -4 3.22 0.92 0 -8 4 1.09 0.81 0 8 4 4.13 1.22 0 8 4 2.57 1.02 0 -8 -4 2.50 0.35 0 -8 -4 1.17 0.84 0 8 5 44.27 2.71 0 -8 5 42.64 2.69 0 8 5 51.07 2.88 0 8 -5 44.20 2.70 0 8 5 49.15 2.79 0 -8 -5 43.65 2.71 0 -8 -5 42.31 2.57 0 8 6 66.29 3.82 0 8 -6 63.96 3.78 0 8 -6 56.36 3.79 0 8 6 70.59 3.91 0 -8 -6 67.78 3.82 0 8 7 3.02 0.86 0 -8 -7 2.31 0.85 0 8 -7 0.84 0.66 0 8 -7 0.47 0.63 0 8 7 0.79 1.07 0 8 -7 1.06 0.73 0 8 8 25.01 1.62 0 8 -8 19.06 1.40 0 8 -8 22.44 1.41 0 8 -8 19.20 1.53 0 -8 -8 25.51 1.76 0 8 8 23.38 1.75 0 -8 -8 25.83 1.60 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1.44 -2 3 11 16.39 1.51 2 3 -11 16.02 1.35 -2 -3 11 15.14 1.30 2 3 -10 3.74 1.01 -2 3 10 2.13 1.02 2 -3 -10 0.85 1.09 2 -3 -10 0.08 1.14 -2 3 10 3.20 1.10 2 3 -10 2.55 0.93 -2 -3 10 1.85 0.84 -2 3 9 183.20 9.83 2 -3 -9 180.72 9.83 2 3 -9 164.41 9.82 -2 3 9 170.48 9.83 2 -3 -9 175.64 9.83 -2 -3 9 168.99 9.77 2 3 -9 158.94 9.77 2 3 -8 1.17 0.93 2 -3 -8 1.12 0.98 -2 3 8 3.11 0.85 2 -3 -8 0.54 1.01 -2 3 8 1.59 0.89 -2 -3 8 2.53 0.65 2 3 -8 2.37 0.74 2 3 -8 1.57 0.42 -2 3 7 2.32 0.73 2 3 -7 1.85 0.81 2 -3 -7 0.66 0.82 -2 3 7 2.60 0.81 -2 -3 7 0.87 0.56 2 3 -7 2.03 0.62 -2 -3 7 1.95 0.40 2 -3 -6 9.27 0.94 2 3 -6 10.23 0.95 -2 3 6 9.77 0.95 -2 -3 6 9.13 0.70 -2 3 6 7.31 0.94 2 3 -6 8.69 0.76 -2 -3 6 7.65 0.67 2 3 -5 9.54 0.90 2 -3 -5 7.80 0.92 -2 3 5 9.76 0.93 2 3 -5 8.24 0.68 -2 -3 5 9.16 0.67 2 -3 -4 10.97 1.08 2 3 -4 12.03 0.97 -2 3 4 14.17 1.04 -2 3 4 10.69 1.05 2 3 -4 11.93 0.85 2 3 -4 12.46 0.79 -2 -3 4 11.98 0.77 2 -3 -4 13.51 0.95 2 3 -3 463.06 25.67 -2 3 3 388.97 25.69 2 3 -3 463.44 25.68 2 -3 -3 435.77 25.70 2 -3 -3 468.03 25.68 -2 3 3 472.96 25.68 2 3 -2 8.70 0.84 -2 -3 2 10.84 0.83 2 -3 -2 11.66 0.95 2 3 -2 10.46 0.78 -2 3 2 11.66 0.80 2 3 -2 9.10 0.81 2 -3 -1 198.65 11.90 2 3 -1 223.84 11.89 -2 -3 1 200.87 11.89 2 -3 -1 188.63 11.89 2 3 -1 218.87 11.85 2 3 -1 199.31 11.86 -2 -3 1 197.30 11.86 -2 3 1 226.85 11.87 2 -3 -1 211.85 11.90 2 -3 0 171.32 10.06 -2 -3 0 187.43 10.07 -2 3 0 199.92 10.06 2 -3 0 169.12 10.06 2 3 0 184.73 10.07 2 3 0 173.16 10.02 -2 3 0 187.07 10.04 -2 -3 0 171.05 10.02 2 -3 0 163.06 10.07 2 3 0 167.43 10.03 2 -3 1 18.08 1.30 -2 3 -1 20.97 1.28 -2 -3 -1 18.62 1.34 2 3 1 20.64 1.23 -2 3 -1 19.88 1.25 -2 -3 -1 17.42 1.19 2 3 1 20.98 1.22 2 -3 2 713.16 38.37 -2 -3 -2 629.69 38.37 2 3 2 723.87 38.37 -2 -3 -2 643.61 38.36 -2 3 -2 678.41 38.37 2 3 3 17.58 1.06 -2 -3 -3 16.93 1.06 2 -3 3 17.11 1.15 2 3 3 19.06 1.21 -2 3 -3 18.74 1.25 -2 -3 -3 17.45 1.22 -2 3 -3 17.64 1.19 -2 -3 -3 16.59 1.14 2 3 4 627.11 34.67 -2 -3 -4 607.77 34.70 2 3 4 626.96 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1.22 -5 5 12 5.61 1.21 5 5 -12 5.98 0.70 -5 -5 12 4.61 0.70 5 5 -12 4.84 0.76 -5 5 12 5.39 1.23 5 -5 -12 4.53 1.08 5 5 -11 101.28 5.94 -5 5 11 110.35 5.99 5 -5 -11 109.87 5.99 -5 5 11 107.02 5.97 -5 5 11 109.68 5.99 -5 -5 11 94.99 5.81 5 5 -11 93.68 5.82 5 -5 -11 108.05 5.95 5 -5 -10 4.19 1.17 5 5 -10 2.83 1.05 -5 5 10 5.51 1.14 -5 5 10 4.71 1.09 -5 -5 10 4.54 0.60 5 5 -10 3.70 0.61 -5 5 10 5.80 1.07 5 -5 -10 1.98 1.00 5 5 -10 4.43 1.05 5 -5 -9 167.99 9.15 -5 5 9 176.03 9.15 5 5 -9 151.51 9.09 -5 5 9 170.00 9.15 -5 5 9 165.08 9.16 5 5 -9 150.11 8.99 -5 -5 9 155.03 8.99 5 -5 -9 170.40 9.12 5 5 -9 146.59 9.11 -5 5 8 124.53 6.96 5 -5 -8 128.77 6.97 5 5 -8 116.89 6.91 -5 5 8 127.72 6.99 -5 5 8 128.87 6.97 -5 -5 8 120.81 6.88 -5 5 8 122.36 6.99 -5 -5 8 112.08 6.79 5 -5 -8 125.34 6.93 5 5 -8 119.39 6.93 -5 5 7 102.64 6.18 5 -5 -7 112.13 6.17 5 5 -7 103.16 6.11 -5 5 7 112.25 6.19 -5 5 7 100.09 6.17 -5 -5 7 107.79 6.10 -5 5 7 103.00 6.18 5 5 -7 97.37 6.13 5 -5 -7 107.87 6.13 -5 5 6 51.99 2.95 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1.28 -6 7 12 3.90 1.27 -6 7 12 5.87 1.28 6 -7 -12 2.82 1.08 -6 -7 12 2.10 0.49 6 7 -12 2.25 1.19 6 -7 -11 131.88 7.40 -6 7 11 127.29 7.40 6 7 -11 117.42 7.32 -6 7 11 140.46 7.41 -6 7 11 127.48 7.39 -6 7 11 127.01 7.40 6 7 -11 115.62 7.33 6 -7 -11 124.03 7.33 6 -7 -10 14.23 1.51 6 7 -10 12.28 1.33 -6 7 10 10.51 1.46 -6 7 10 12.02 1.48 -6 7 10 12.72 1.46 -6 -7 10 14.43 1.07 -6 7 10 14.61 1.51 6 -7 -10 13.55 1.31 6 7 -10 11.65 1.31 6 7 -9 14.62 1.43 6 -7 -9 15.03 1.61 -6 7 9 17.10 1.65 -6 7 9 14.40 1.58 -6 7 9 16.82 1.55 -6 -7 9 16.13 1.35 -6 7 9 21.17 1.63 6 -7 -9 19.99 1.44 6 7 -9 16.32 1.45 6 -7 -8 0.86 1.07 6 7 -8 1.30 0.85 -6 7 8 -1.17 1.17 -6 7 8 -0.15 1.14 -6 7 8 0.84 1.09 -6 -7 8 -0.32 0.94 -6 7 8 0.97 1.07 6 7 -8 -1.03 0.92 6 -7 -8 -0.05 0.90 -6 7 7 -0.04 1.09 -6 -7 7 1.16 0.95 -6 7 7 3.15 1.14 6 7 -7 1.93 0.84 6 -7 -7 1.96 1.04 6 -7 -7 3.47 0.91 6 7 -7 1.83 0.90 -6 -7 6 11.21 1.21 6 -7 -6 9.19 1.34 -6 7 6 13.75 1.35 6 7 -6 9.31 1.03 -6 7 6 13.12 1.16 6 -7 -6 12.57 1.15 6 7 -6 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-4 4.34 1.99 -18 7 -4 8.58 2.13 -18 -7 -4 5.77 1.97 18 -7 5 12.79 2.19 -18 7 -5 12.94 2.16 -18 -7 -5 14.37 2.11 -18 7 -6 0.21 1.94 -18 -7 -6 3.17 1.97 -18 7 -7 -1.00 1.99 -18 -7 -7 -2.06 1.94 -18 7 -8 5.44 2.08 -18 -7 -8 4.09 1.94 -18 7 -9 3.58 2.08 -18 -7 -9 4.97 2.07 -18 8 8 1.93 2.10 -18 8 7 4.54 2.13 -18 8 7 6.64 2.08 -18 8 6 4.90 2.17 -18 8 6 4.04 2.06 -18 8 5 3.05 2.18 -18 -8 5 2.90 1.95 -18 8 5 3.11 1.99 18 -8 -4 -3.13 2.06 -18 8 4 -3.18 2.01 -18 -8 4 -0.56 1.94 -18 8 4 1.80 1.96 18 -8 -3 6.65 2.10 -18 8 3 4.17 2.03 -18 -8 3 5.58 1.98 -18 8 3 5.68 2.07 18 -8 -2 -0.38 2.00 -18 8 2 0.80 1.97 -18 8 2 1.55 1.88 -18 -8 2 -0.76 1.86 18 -8 -1 5.31 2.13 -18 8 1 2.16 2.05 -18 8 1 3.63 1.87 -18 -8 1 2.68 1.92 18 -8 0 -2.51 2.04 -18 8 0 -3.60 2.14 -18 8 0 0.89 1.91 -18 -8 0 -3.05 1.89 18 -8 1 -1.00 1.99 -18 8 -1 0.79 1.96 -18 8 -1 3.22 1.92 -18 -8 -1 1.42 1.86 18 -8 2 -0.23 2.09 -18 8 -2 -0.58 2.04 -18 8 -2 0.23 1.92 -18 -8 -2 1.21 1.86 -18 8 -3 7.35 2.14 -18 8 -3 7.87 2.11 -18 -8 -3 7.69 2.02 -18 8 -4 2.49 2.05 -18 -8 -4 5.27 1.93 -18 8 -5 0.66 2.02 -18 -8 -5 3.69 1.87 -18 8 -6 5.89 2.17 -18 -8 -6 8.96 2.01 -18 -8 -7 2.74 1.93 -18 -8 -8 2.27 1.88 -18 -8 -9 1.07 1.99 -18 9 6 -0.91 2.02 -18 -9 5 20.53 2.43 -18 9 5 21.82 2.56 -18 -9 4 2.70 1.96 -18 9 4 4.38 2.01 -18 -9 3 2.45 1.94 -18 9 3 3.52 2.03 -18 -9 2 7.51 1.93 -18 9 2 8.32 2.11 -18 9 1 2.23 2.00 -18 -9 1 3.45 1.91 -18 9 0 2.53 2.01 -18 -9 0 0.67 1.89 -18 9 -1 2.17 1.98 -18 -9 -1 -0.87 1.87 -18 -9 -2 6.60 1.87 -18 -9 -3 4.77 1.92 -18 -9 -4 7.42 2.01 -18 -9 -5 0.40 1.85 -18 -9 -6 -0.88 1.85 -18 -10 4 3.61 1.87 -18 -10 3 5.76 2.00 -19 0 15 -0.60 1.96 -19 0 14 0.07 1.99 -19 0 13 -3.91 1.99 -19 0 12 -0.55 1.86 -19 0 11 0.36 1.89 -19 0 10 3.02 1.83 -19 0 9 4.80 1.80 -19 0 8 1.71 1.75 -19 0 8 0.40 2.01 -19 0 7 3.19 1.81 -19 0 7 4.44 2.04 -19 0 6 2.82 1.78 -19 0 6 2.21 2.01 -19 0 5 12.96 2.18 -19 0 4 0.77 1.85 19 0 -3 3.60 1.70 -19 0 3 4.16 1.86 19 0 -2 1.20 1.65 -19 0 2 0.46 1.91 19 0 -1 55.67 3.70 -19 0 1 52.46 3.91 19 0 0 -0.28 1.68 -19 0 0 -3.49 1.98 19 0 1 2.05 1.79 -19 0 -1 1.53 1.80 19 0 2 -1.44 1.63 -19 0 -2 0.31 1.93 19 0 3 2.59 1.83 -19 0 -3 -1.32 1.96 19 0 4 -0.18 1.73 -19 0 -4 1.25 1.89 -19 1 14 0.67 2.00 -19 1 13 1.17 1.98 -19 1 12 3.24 1.92 -19 1 11 4.09 1.86 -19 1 10 1.15 1.92 -19 1 9 -1.66 1.84 -19 1 8 2.90 1.74 -19 -1 8 7.78 2.02 -19 1 7 0.69 1.87 -19 -1 7 1.18 1.99 -19 1 6 20.91 2.28 -19 -1 6 20.56 2.49 -19 1 6 22.35 2.53 19 -1 -5 1.32 1.68 -19 1 5 2.82 1.75 -19 1 5 2.13 1.96 -19 -1 5 3.99 2.07 19 -1 -4 9.37 1.79 -19 1 4 10.67 1.88 -19 1 4 9.73 2.09 -19 -1 4 10.35 2.09 19 -1 -3 1.25 1.73 -19 1 3 0.21 1.68 -19 1 3 2.47 1.89 -19 -1 3 2.45 1.88 19 -1 -2 7.88 1.89 -19 1 2 9.82 1.82 -19 1 2 12.59 2.12 -19 -1 2 12.97 2.10 19 -1 -1 22.13 2.31 -19 1 1 28.24 2.52 -19 -1 1 18.22 2.40 19 1 0 4.80 1.68 19 -1 0 3.66 1.70 -19 1 0 4.81 1.94 -19 -1 0 2.87 1.91 19 1 1 10.72 1.76 19 -1 1 5.24 1.82 -19 1 -1 8.53 2.03 -19 -1 -1 4.93 1.92 19 1 2 6.00 1.75 19 -1 2 3.32 1.83 -19 1 -2 4.43 2.01 -19 -1 -2 3.29 1.98 19 -1 3 12.28 1.98 19 1 3 14.81 1.91 -19 1 -3 10.02 2.12 -19 -1 -3 13.14 2.20 19 -1 4 2.45 1.80 -19 1 -4 3.47 2.04 -19 -1 -4 -2.33 2.01 -19 -1 -5 -1.17 2.02 -19 2 14 0.07 2.02 -19 2 13 7.82 2.15 -19 2 12 1.31 2.01 -19 2 11 2.05 1.96 -19 2 10 6.00 1.99 -19 2 9 -0.50 1.87 -19 2 8 -0.25 1.93 -19 -2 8 2.48 2.04 -19 2 7 7.68 1.97 -19 -2 7 5.82 2.04 -19 2 6 1.48 1.81 -19 -2 6 4.45 1.99 19 -2 -5 0.64 1.77 -19 2 5 0.87 1.81 -19 -2 5 2.49 2.00 19 -2 -4 18.15 2.16 -19 2 4 17.43 2.17 -19 -2 4 21.40 2.44 19 -2 -3 -0.24 1.86 -19 2 3 1.59 1.74 -19 -2 3 2.06 1.98 19 -2 -2 0.42 1.85 -19 2 2 2.60 1.87 -19 -2 2 0.15 1.94 19 -2 -1 17.44 2.24 -19 2 1 18.14 2.15 -19 -2 1 20.94 2.36 19 -2 0 2.85 1.83 -19 -2 0 0.23 2.00 19 -2 1 4.75 1.85 -19 2 -1 6.46 1.83 -19 -2 -1 7.07 2.09 19 -2 2 3.54 1.90 -19 2 -2 3.23 1.73 -19 -2 -2 1.14 1.95 19 -2 3 1.34 1.81 -19 -2 -3 0.38 1.89 19 -2 4 5.08 1.94 -19 -2 -4 6.34 2.08 19 -2 5 4.79 1.97 -19 -2 -5 -0.55 1.97 -19 3 12 4.42 2.11 -19 3 11 2.68 2.02 -19 3 10 4.29 2.01 -19 3 9 4.77 1.99 -19 3 8 1.73 1.95 -19 -3 8 2.72 2.03 -19 3 7 14.95 2.23 -19 -3 7 16.99 2.35 -19 3 6 7.20 1.98 -19 -3 6 4.50 2.02 -19 3 6 2.32 2.06 19 -3 -5 25.51 2.38 -19 3 5 21.23 2.48 -19 -3 5 27.22 2.63 -19 3 5 25.77 2.65 19 -3 -4 2.17 1.83 -19 3 4 5.28 1.90 -19 3 4 -0.24 2.02 -19 -3 4 1.08 1.99 19 -3 -3 7.12 1.96 -19 3 3 5.18 1.93 -19 3 3 2.57 2.06 -19 -3 3 3.35 1.93 19 -3 -2 29.80 2.74 -19 3 2 31.06 2.70 -19 3 2 31.04 2.83 -19 -3 2 32.19 2.79 19 -3 -1 0.45 1.81 -19 3 1 2.16 1.84 -19 3 1 3.48 1.97 -19 -3 1 4.04 1.94 19 -3 0 13.51 2.10 -19 3 0 13.22 2.03 -19 3 0 14.73 2.21 -19 -3 0 10.69 2.10 19 -3 1 0.46 1.89 -19 3 -1 2.31 1.79 -19 -3 -1 -0.45 1.91 19 -3 2 16.29 2.20 -19 3 -2 12.78 2.00 -19 -3 -2 14.26 2.26 19 -3 3 0.73 1.93 -19 3 -3 -1.40 1.76 -19 -3 -3 -0.68 1.98 19 -3 4 0.07 1.95 -19 3 -4 -0.18 1.80 -19 -3 -4 -2.99 1.94 19 -3 5 12.25 2.23 -19 -3 -5 18.16 2.34 19 -3 6 -0.63 2.00 -19 4 11 -2.30 2.07 -19 4 10 1.66 2.00 -19 4 9 0.07 1.98 -19 4 8 -0.13 1.96 -19 -4 8 -1.51 1.94 -19 4 7 2.37 1.99 -19 -4 7 3.06 2.05 -19 4 6 -0.91 1.96 -19 -4 6 -2.40 2.11 -19 4 5 5.47 2.02 -19 -4 5 5.15 2.06 -19 4 5 1.67 2.09 19 -4 -4 3.46 1.96 -19 4 4 6.69 2.00 -19 4 4 8.27 2.12 -19 -4 4 3.75 2.01 19 -4 -3 4.41 1.91 -19 4 3 6.67 1.96 -19 4 3 9.22 2.13 -19 -4 3 6.98 2.03 19 -4 -2 -2.20 1.88 -19 4 2 -0.70 1.90 -19 4 2 -0.31 2.04 -19 -4 2 1.58 1.92 19 -4 -1 2.82 1.90 -19 4 1 -2.66 1.96 -19 4 1 -0.47 2.00 -19 -4 1 -1.72 1.91 19 -4 0 8.57 1.97 -19 4 0 5.91 1.94 -19 4 0 9.15 2.10 -19 -4 0 4.08 1.89 19 -4 1 1.44 1.93 -19 4 -1 2.24 1.88 -19 4 -1 0.47 1.94 -19 -4 -1 3.12 1.93 19 -4 2 0.41 1.93 -19 4 -2 0.12 1.84 -19 -4 -2 1.04 1.92 19 -4 3 -2.85 1.95 -19 4 -3 -1.42 1.87 -19 -4 -3 -1.20 2.00 19 -4 4 3.93 1.98 -19 4 -4 1.37 1.89 -19 -4 -4 3.05 2.01 19 -4 5 1.71 1.94 -19 4 -5 -2.75 1.88 -19 -4 -5 -2.30 2.07 19 -4 6 4.42 2.04 -19 4 -6 3.40 1.90 -19 5 12 3.25 2.07 -19 5 11 3.57 2.05 -19 5 10 22.62 2.54 -19 5 9 12.14 2.24 -19 5 8 6.67 2.04 -19 5 7 43.98 3.50 -19 -5 7 47.25 3.55 -19 5 6 2.04 1.96 -19 -5 6 -1.00 1.99 -19 5 5 0.87 1.94 -19 -5 5 7.31 2.09 19 -5 -4 11.56 2.13 -19 5 4 13.00 2.20 -19 -5 4 18.16 2.31 19 -5 -3 1.85 1.99 -19 5 3 -0.20 1.97 -19 -5 3 1.06 1.97 19 -5 -2 6.08 1.99 -19 5 2 7.24 2.05 -19 -5 2 1.20 1.96 19 -5 -1 -1.89 1.95 -19 5 1 0.27 2.02 -19 -5 1 1.12 1.98 19 -5 0 1.70 2.01 -19 5 0 3.81 1.93 -19 -5 0 2.07 1.97 19 -5 1 -1.00 1.94 -19 5 -1 -0.52 1.90 -19 -5 -1 -1.70 1.98 19 -5 2 2.15 2.04 -19 5 -2 5.93 1.94 -19 -5 -2 1.63 2.00 19 -5 3 23.76 2.53 -19 5 -3 22.48 2.50 -19 -5 -3 24.77 2.53 19 -5 4 5.99 2.12 -19 5 -4 2.10 1.90 -19 -5 -4 2.71 1.98 19 -5 5 15.11 2.26 -19 5 -5 13.72 2.19 -19 -5 -5 14.74 2.26 -19 5 -6 0.20 1.90 -19 5 -7 1.00 1.93 -19 5 -8 1.22 1.99 -19 6 12 10.48 2.24 -19 6 11 9.53 2.19 -19 6 8 3.90 2.14 -19 6 7 -0.43 2.06 -19 -6 7 1.24 2.07 -19 6 6 2.97 2.06 -19 -6 6 2.08 2.06 -19 6 5 5.71 2.13 -19 -6 5 8.72 2.15 19 -6 -4 -1.07 2.04 -19 6 4 0.85 2.01 -19 -6 4 2.11 2.02 19 -6 -3 1.44 1.97 -19 6 3 -1.13 2.00 -19 -6 3 0.98 1.97 19 -6 -2 -1.09 2.07 -19 6 2 2.59 1.97 -19 -6 2 0.15 1.97 19 -6 -1 6.80 2.12 -19 6 1 1.94 1.98 -19 -6 1 0.37 1.92 19 -6 0 3.24 2.06 -19 6 0 -0.27 1.98 -19 -6 0 0.59 1.97 19 -6 1 0.45 1.96 -19 6 -1 1.71 1.93 -19 -6 -1 -2.55 1.89 19 -6 2 9.30 2.26 -19 6 -2 10.98 2.10 -19 -6 -2 11.81 2.11 -19 6 -3 3.57 2.04 -19 -6 -3 6.24 2.00 -19 6 -4 -0.55 1.97 -19 -6 -4 -1.78 1.99 -19 6 -5 -0.90 2.00 -19 -6 -5 -1.13 1.96 -19 6 -6 0.07 1.95 -19 6 -7 11.79 2.18 -19 6 -8 1.64 2.04 -19 -7 6 -0.99 2.07 -19 7 5 0.29 2.12 -19 -7 5 4.39 2.04 19 -7 -4 4.93 2.11 -19 7 4 6.64 2.16 -19 -7 4 6.63 2.02 19 -7 -3 -1.58 2.08 -19 7 3 -1.62 2.04 -19 -7 3 -0.15 1.97 19 -7 -2 -0.30 2.08 -19 7 2 1.02 2.07 -19 -7 2 2.52 2.06 19 -7 -1 7.87 2.20 -19 7 1 5.92 2.13 -19 -7 1 7.88 2.08 -19 7 0 13.66 2.21 -19 -7 0 13.96 2.26 -19 7 -1 0.14 1.99 -19 -7 -1 3.56 1.94 -19 7 -2 1.87 2.10 -19 -7 -2 6.88 1.99 -19 7 -3 4.18 2.10 -19 -7 -3 6.63 2.00 -19 7 -4 16.52 2.46 -19 -7 -4 22.76 2.41 -19 7 -5 -1.02 2.08 -19 -8 5 -1.66 2.03 -19 -8 4 4.16 2.01 -19 -8 3 3.67 1.99 -19 -8 2 0.37 1.96 -19 -8 1 -0.51 1.93 -19 -8 0 2.11 1.98 -19 -8 -1 5.78 2.02 -19 -8 -2 6.91 2.02 -19 -8 -3 -1.36 1.95 -19 -8 -4 -1.01 1.95 -19 -9 4 -0.52 2.03 -19 -9 3 1.46 1.98 -19 -9 2 1.51 1.99 -19 -9 1 0.07 1.94 -19 -9 0 3.46 2.03 -19 -9 -1 2.65 2.00 -19 -9 -2 1.78 1.98 20 0 3 0.50 1.84 20 0 4 -1.52 1.87 20 0 5 0.13 1.93 20 -1 0 1.69 1.81 20 -1 1 2.84 1.85 20 -1 2 6.32 1.96 20 -1 3 1.23 1.92 20 -1 4 1.32 1.91 20 -1 5 2.29 1.99 20 -1 6 -0.62 2.00 -20 2 11 -2.00 2.06 -20 2 10 3.26 1.99 -20 2 9 0.64 1.97 -20 2 8 0.95 1.99 -20 2 7 -0.57 1.94 -20 2 6 0.68 1.91 -20 2 5 4.44 1.92 20 -2 -3 11.09 2.06 20 -2 -2 1.91 1.90 20 -2 -1 -1.68 1.94 20 -2 0 4.39 1.98 20 -2 1 -0.99 1.96 20 -2 2 -0.20 1.94 20 -2 3 6.02 2.00 20 -2 4 -1.71 1.95 20 -2 5 2.02 1.99 -20 3 10 10.37 2.18 -20 3 9 0.81 1.99 -20 3 8 2.55 2.03 -20 3 7 6.44 2.03 -20 3 6 8.61 2.08 -20 3 5 4.15 1.94 20 -3 -4 7.88 2.12 -20 3 4 9.67 2.07 20 -3 -3 -1.12 1.98 -20 3 3 0.81 1.87 20 -3 -2 2.34 2.06 -20 3 2 2.18 1.87 20 -3 -1 22.99 2.45 20 -3 0 1.78 2.03 20 -3 1 18.98 2.34 20 -3 2 3.69 2.00 20 -3 3 10.27 2.09 20 -3 4 2.06 1.99 -20 4 8 34.80 3.05 -20 4 7 2.67 2.09 -20 4 6 0.27 2.02 -20 4 5 4.42 2.01 20 -4 -4 15.79 2.35 -20 4 4 16.05 2.25 20 -4 -3 7.64 2.10 -20 4 3 11.15 2.15 20 -4 -2 6.64 2.11 -20 4 2 9.19 2.06 20 -4 -1 28.55 2.77 -20 4 1 29.56 2.74 20 -4 0 13.11 2.17 -20 4 0 13.29 2.16 20 -4 1 0.29 2.01 -20 4 -1 -0.13 1.96 20 -4 2 2.83 2.03 -20 5 5 4.97 2.15 20 -5 -4 4.29 2.04 -20 5 4 0.35 1.99 20 -5 -3 2.88 2.01 -20 5 3 1.32 1.99 20 -5 -2 2.98 2.11 -20 5 2 -0.97 2.07 20 -5 -1 6.11 2.07 -20 5 1 7.78 2.11 -20 5 0 1.52 2.02 -20 5 -1 8.13 2.13 -20 5 -2 22.63 2.52 -20 5 -3 2.58 2.02 -20 5 -4 10.95 2.14 -20 6 0 11.75 2.27 0 0 0 0.00 0.00 TITL S_allene_auto in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 15.663935 16.141417 23.310956 90.0000 93.8959 90.0000 ZERR 5.00 0.000642 0.000716 0.001034 0.0000 0.0039 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H B N S UNIT 300.00 300.00 20.00 20.00 5.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 93198 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.150 _oxdiff_exptl_absorpt_empirical_full_min 0.921 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.70741(3) 0.65105(3) 0.74594(2) 0.02079(12) Uani 1 1 d . . . . . N1 N 0.71608(9) 0.60174(10) 0.58549(7) 0.0210(4) Uani 1 1 d . . . . . N2 N 0.80229(9) 0.63473(10) 0.59197(7) 0.0215(4) Uani 1 1 d . . . . . N3 N 0.76007(10) 0.70495(10) 0.90477(7) 0.0215(4) Uani 1 1 d . . . . . N4 N 0.84593(10) 0.67704(10) 0.89517(7) 0.0212(4) Uani 1 1 d . . . . . C13 C 0.99462(12) 0.65975(12) 0.66511(8) 0.0200(4) Uani 1 1 d . . . . . C21 C 0.67331(12) 0.60817(12) 0.52957(8) 0.0204(4) Uani 1 1 d . . . . . C42 C 0.93377(12) 0.60383(12) 0.81950(8) 0.0205(4) Uani 1 1 d . . . . . C12 C 0.91565(12) 0.70145(12) 0.66246(8) 0.0196(4) Uani 1 1 d . . . . . C3 C 0.58343(12) 0.58210(12) 0.65105(8) 0.0214(4) Uani 1 1 d . . . . . C27 C 0.85397(12) 0.62139(13) 0.54423(8) 0.0220(4) Uani 1 1 d . . . . . C47 C 1.01291(12) 0.64115(12) 0.81105(8) 0.0219(4) Uani 1 1 d . . . . . C57 C 0.89288(12) 0.64349(12) 0.94473(8) 0.0217(4) Uani 1 1 d . . . . . C51 C 0.74955(12) 0.75160(12) 0.95579(8) 0.0224(4) Uani 1 1 d . . . . . C4 C 0.56320(12) 0.50685(13) 0.67752(8) 0.0237(4) Uani 1 1 d . . . . . C33 C 0.60849(12) 0.72235(12) 0.84622(8) 0.0216(4) Uani 1 1 d . . . . . C2 C 0.76488(12) 0.67281(12) 0.80554(8) 0.0203(4) Uani 1 1 d . . . . . C1 C 0.74890(12) 0.63444(12) 0.68416(8) 0.0211(4) Uani 1 1 d . . . . . C22 C 0.62041(12) 0.54425(13) 0.50936(8) 0.0241(4) Uani 1 1 d . . . . . H22 H 0.613020 0.496667 0.532486 0.029 Uiso 1 1 calc R U . . . C44 C 1.00054(13) 0.46953(13) 0.81010(9) 0.0268(5) Uani 1 1 d . . . . . H44 H 0.995813 0.410875 0.808848 0.032 Uiso 1 1 calc R U . . . C43 C 0.92780(12) 0.51676(13) 0.81802(8) 0.0233(4) Uani 1 1 d . . . . . C8 C 0.51992(12) 0.64348(13) 0.64406(8) 0.0256(4) Uani 1 1 d . . . . . C34 C 0.57903(12) 0.80210(12) 0.83156(8) 0.0239(4) Uani 1 1 d . . . . . C50 C 1.01990(13) 0.73405(12) 0.80913(9) 0.0259(4) Uani 1 1 d . . . . . H50A H 0.993325 0.754442 0.772549 0.039 Uiso 1 1 calc R U . . . H50B H 1.080361 0.750121 0.812572 0.039 Uiso 1 1 calc R U . . . H50C H 0.990561 0.758096 0.841003 0.039 Uiso 1 1 calc R U . . . C16 C 0.99282(13) 0.83188(13) 0.66758(9) 0.0274(5) Uani 1 1 d . . . . . H16 H 0.992010 0.890717 0.668335 0.033 Uiso 1 1 calc R U . . . C32 C 0.90169(12) 0.68582(13) 0.52381(9) 0.0248(4) Uani 1 1 d . . . . . H32 H 0.901258 0.738672 0.541725 0.030 Uiso 1 1 calc R U . . . C26 C 0.68406(12) 0.67805(13) 0.49573(8) 0.0241(4) Uani 1 1 d . . . . . H26 H 0.719628 0.722257 0.509817 0.029 Uiso 1 1 calc R U . . . C38 C 0.54838(13) 0.65812(13) 0.84948(9) 0.0255(4) Uani 1 1 d . . . . . C14 C 1.07041(12) 0.70498(13) 0.66910(8) 0.0247(4) Uani 1 1 d . . . . . H14 H 1.123411 0.676157 0.671391 0.030 Uiso 1 1 calc R U . . . C17 C 0.91558(13) 0.78879(12) 0.66424(8) 0.0247(4) Uani 1 1 d . . . . . C62 C 0.97973(13) 0.66012(13) 0.95356(9) 0.0260(4) Uani 1 1 d . . . . . H62 H 1.007512 0.693353 0.926817 0.031 Uiso 1 1 calc R U . . . C18 C 0.99689(13) 0.56660(12) 0.66305(9) 0.0260(4) Uani 1 1 d . . . . . H18A H 0.970467 0.544061 0.696631 0.039 Uiso 1 1 calc R U . . . H18B H 1.056414 0.547824 0.663322 0.039 Uiso 1 1 calc R U . . . H18C H 0.965271 0.547252 0.627866 0.039 Uiso 1 1 calc R U . . . C46 C 1.08438(12) 0.59184(14) 0.80416(8) 0.0265(5) Uani 1 1 d . . . . . H46 H 1.137955 0.617658 0.799424 0.032 Uiso 1 1 calc R U . . . C23 C 0.57821(13) 0.55006(13) 0.45510(9) 0.0294(5) Uani 1 1 d . . . . . H23 H 0.541371 0.506633 0.441306 0.035 Uiso 1 1 calc R U . . . C5 C 0.48211(13) 0.49548(14) 0.69713(9) 0.0297(5) Uani 1 1 d . . . . . H5 H 0.469578 0.445143 0.715931 0.036 Uiso 1 1 calc R U . . . C35 C 0.49162(13) 0.81625(14) 0.82139(9) 0.0298(5) Uani 1 1 d . . . . . H35 H 0.472410 0.870220 0.810591 0.036 Uiso 1 1 calc R U . . . C58 C 0.85227(13) 0.59599(12) 0.98468(9) 0.0273(5) Uani 1 1 d . . . . . H58 H 0.792836 0.584377 0.979016 0.033 Uiso 1 1 calc R U . . . C28 C 0.85438(12) 0.54387(13) 0.51810(8) 0.0239(4) Uani 1 1 d . . . . . H28 H 0.821397 0.499785 0.532078 0.029 Uiso 1 1 calc R U . . . C56 C 0.81360(13) 0.80394(12) 0.97851(9) 0.0265(5) Uani 1 1 d . . . . . H56 H 0.865181 0.810242 0.959746 0.032 Uiso 1 1 calc R U . . . C15 C 1.07087(13) 0.79103(14) 0.66983(9) 0.0284(5) Uani 1 1 d . . . . . C45 C 1.07950(13) 0.50579(14) 0.80402(9) 0.0285(5) Uani 1 1 d . . . . . C29 C 0.90331(13) 0.53158(13) 0.47153(9) 0.0287(5) Uani 1 1 d . . . . . H29 H 0.904115 0.478781 0.453567 0.034 Uiso 1 1 calc R U . . . C30 C 0.95096(14) 0.59589(14) 0.45113(9) 0.0316(5) Uani 1 1 d . . . . . H30 H 0.984393 0.587159 0.419158 0.038 Uiso 1 1 calc R U . . . C60 C 0.98590(15) 0.58150(14) 1.04097(9) 0.0329(5) Uani 1 1 d . . . . . H60 H 1.017689 0.560098 1.073838 0.039 Uiso 1 1 calc R U . . . C25 C 0.64262(13) 0.68267(13) 0.44150(9) 0.0281(5) Uani 1 1 d . . . . . H25 H 0.650501 0.729864 0.418095 0.034 Uiso 1 1 calc R U . . . C7 C 0.43893(13) 0.62894(15) 0.66338(9) 0.0317(5) Uani 1 1 d . . . . . H7 H 0.396254 0.670579 0.658090 0.038 Uiso 1 1 calc R U . . . C6 C 0.41907(13) 0.55563(15) 0.68999(9) 0.0331(5) Uani 1 1 d . . . . . C61 C 1.02594(14) 0.62821(13) 1.00140(9) 0.0300(5) Uani 1 1 d . . . . . H61 H 1.085622 0.638694 1.006876 0.036 Uiso 1 1 calc R U . . . C31 C 0.95018(13) 0.67269(14) 0.47698(9) 0.0297(5) Uani 1 1 d . . . . . H31 H 0.982932 0.716733 0.462706 0.036 Uiso 1 1 calc R U . . . C24 C 0.58972(13) 0.61892(13) 0.42113(9) 0.0301(5) Uani 1 1 d . . . . . H24 H 0.561359 0.622463 0.383869 0.036 Uiso 1 1 calc R U . . . C52 C 0.67395(13) 0.74311(14) 0.98314(9) 0.0292(5) Uani 1 1 d . . . . . H52 H 0.630350 0.706832 0.967905 0.035 Uiso 1 1 calc R U . . . C48 C 0.84427(13) 0.47395(13) 0.82735(10) 0.0305(5) Uani 1 1 d . . . . . H48A H 0.823469 0.491927 0.864054 0.046 Uiso 1 1 calc R U . . . H48B H 0.853088 0.413837 0.828058 0.046 Uiso 1 1 calc R U . . . H48C H 0.801986 0.488261 0.795998 0.046 Uiso 1 1 calc R U . . . C55 C 0.80163(15) 0.84689(13) 1.02878(9) 0.0323(5) Uani 1 1 d . . . . . H55 H 0.845715 0.882037 1.044756 0.039 Uiso 1 1 calc R U . . . C36 C 0.43186(13) 0.75387(15) 0.82657(10) 0.0353(5) Uani 1 1 d . . . . . C59 C 0.89911(15) 0.56582(13) 1.03268(9) 0.0327(5) Uani 1 1 d . . . . . H59 H 0.871365 0.534012 1.060223 0.039 Uiso 1 1 calc R U . . . C37 C 0.46143(13) 0.67511(14) 0.84031(10) 0.0327(5) Uani 1 1 d . . . . . H37 H 0.421342 0.631481 0.843565 0.039 Uiso 1 1 calc R U . . . C53 C 0.66246(15) 0.78785(16) 1.03278(9) 0.0370(6) Uani 1 1 d . . . . . H53 H 0.610254 0.783208 1.051023 0.044 Uiso 1 1 calc R U . . . C39 C 0.64214(14) 0.87195(13) 0.82755(10) 0.0332(5) Uani 1 1 d . . . . . H39A H 0.660969 0.890852 0.866316 0.050 Uiso 1 1 calc R U . . . H39B H 0.614808 0.917941 0.805869 0.050 Uiso 1 1 calc R U . . . H39C H 0.691703 0.852503 0.807858 0.050 Uiso 1 1 calc R U . . . C11 C 0.53891(15) 0.72525(14) 0.61718(11) 0.0393(6) Uani 1 1 d . . . . . H11A H 0.586997 0.751768 0.639150 0.059 Uiso 1 1 calc R U . . . H11B H 0.488362 0.760996 0.617335 0.059 Uiso 1 1 calc R U . . . H11C H 0.553802 0.716419 0.577479 0.059 Uiso 1 1 calc R U . . . C9 C 0.62897(14) 0.43887(14) 0.68499(10) 0.0346(5) Uani 1 1 d . . . . . H9A H 0.639092 0.415046 0.647382 0.052 Uiso 1 1 calc R U . . . H9B H 0.608009 0.395628 0.709978 0.052 Uiso 1 1 calc R U . . . H9C H 0.682561 0.461739 0.702455 0.052 Uiso 1 1 calc R U . . . C54 C 0.72660(15) 0.83925(14) 1.05590(9) 0.0364(5) Uani 1 1 d . . . . . H54 H 0.718921 0.869112 1.090295 0.044 Uiso 1 1 calc R U . . . C20 C 0.83193(14) 0.83581(14) 0.66160(11) 0.0360(5) Uani 1 1 d . . . . . H20A H 0.798296 0.821808 0.625937 0.054 Uiso 1 1 calc R U . . . H20B H 0.843547 0.895466 0.662520 0.054 Uiso 1 1 calc R U . . . H20C H 0.799737 0.820619 0.694643 0.054 Uiso 1 1 calc R U . . . B3 B 0.70681(14) 0.70130(13) 0.85342(9) 0.0205(5) Uani 1 1 d . . . . . C41 C 0.57761(15) 0.57037(14) 0.86028(11) 0.0364(5) Uani 1 1 d . . . . . H41A H 0.597287 0.546822 0.824741 0.055 Uiso 1 1 calc R U . . . H41B H 0.529888 0.537313 0.872928 0.055 Uiso 1 1 calc R U . . . H41C H 0.624686 0.569820 0.890196 0.055 Uiso 1 1 calc R U . . . B2 B 0.82818(13) 0.65588(14) 0.64971(9) 0.0207(5) Uani 1 1 d . . . . . C19 C 1.15420(15) 0.83842(16) 0.67379(11) 0.0442(6) Uani 1 1 d . . . . . H19A H 1.143095 0.896737 0.664270 0.066 Uiso 1 1 calc R U . . . H19B H 1.192810 0.814934 0.646697 0.066 Uiso 1 1 calc R U . . . H19C H 1.180753 0.834334 0.712985 0.066 Uiso 1 1 calc R U . . . B4 B 0.85377(14) 0.65474(14) 0.83646(10) 0.0209(5) Uani 1 1 d . . . . . B1 B 0.67867(14) 0.60230(14) 0.63885(9) 0.0212(5) Uani 1 1 d . . . . . C49 C 1.15813(15) 0.45350(16) 0.79754(12) 0.0449(6) Uani 1 1 d . . . . . H49A H 1.148029 0.397305 0.811495 0.067 Uiso 1 1 calc R U . . . H49B H 1.206930 0.477969 0.820014 0.067 Uiso 1 1 calc R U . . . H49C H 1.170478 0.451250 0.756921 0.067 Uiso 1 1 calc R U . . . C10 C 0.33072(15) 0.5409(2) 0.71076(12) 0.0539(7) Uani 1 1 d . . . . . H10A H 0.299305 0.502169 0.684730 0.081 Uiso 1 1 calc R U . . . H10B H 0.299670 0.593551 0.711376 0.081 Uiso 1 1 calc R U . . . H10C H 0.336071 0.517405 0.749609 0.081 Uiso 1 1 calc R U . . . C40 C 0.33660(15) 0.77129(19) 0.81771(14) 0.0570(8) Uani 1 1 d . . . . . H40A H 0.321826 0.818219 0.841809 0.085 Uiso 1 1 calc R U . . . H40B H 0.304422 0.722230 0.828402 0.085 Uiso 1 1 calc R U . . . H40C H 0.322082 0.784678 0.777218 0.085 Uiso 1 1 calc R U . . . C63 C 0.4686(3) 0.5357(2) 0.99848(15) 0.0852(12) Uani 1 1 d . . . . . H63A H 0.460689 0.554879 1.038115 0.102 Uiso 1 1 calc R U . . . H63B H 0.494142 0.582105 0.977736 0.102 Uiso 1 1 calc R U . . . C64 C 0.3820(3) 0.5167(2) 0.96946(17) 0.0981(14) Uani 1 1 d . . . . . H64A H 0.357293 0.468607 0.988867 0.118 Uiso 1 1 calc R U . . . H64B H 0.389179 0.500717 0.929073 0.118 Uiso 1 1 calc R U . . . C65 C 0.3184(3) 0.5897(3) 0.9700(2) 0.1037(14) Uani 1 1 d . . . . . H65A H 0.266398 0.575902 0.946139 0.156 Uiso 1 1 calc R U . . . H65B H 0.344717 0.639364 0.954734 0.156 Uiso 1 1 calc R U . . . H65C H 0.303581 0.600151 1.009559 0.156 Uiso 1 1 calc R U . . . 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 S1 0.0193(2) 0.0254(3) 0.0180(2) -0.0020(2) 0.00333(18) 0.00008(19) N1 0.0163(8) 0.0286(9) 0.0181(8) -0.0026(7) 0.0012(6) -0.0060(7) N2 0.0171(8) 0.0295(9) 0.0184(8) -0.0039(7) 0.0037(6) -0.0049(7) N3 0.0207(8) 0.0249(9) 0.0195(8) -0.0035(7) 0.0050(6) 0.0044(7) N4 0.0191(8) 0.0262(9) 0.0186(8) -0.0018(7) 0.0036(6) 0.0042(7) C13 0.0221(9) 0.0243(10) 0.0140(9) -0.0003(8) 0.0042(7) -0.0013(8) C21 0.0207(9) 0.0245(10) 0.0164(9) -0.0043(8) 0.0032(7) 0.0006(8) C42 0.0218(9) 0.0263(11) 0.0134(9) -0.0011(8) 0.0017(7) 0.0021(8) C12 0.0212(9) 0.0239(10) 0.0140(9) -0.0027(8) 0.0041(7) -0.0030(8) C3 0.0201(9) 0.0294(11) 0.0146(9) -0.0029(8) 0.0009(7) -0.0031(8) C27 0.0193(9) 0.0315(11) 0.0156(10) -0.0010(8) 0.0030(7) 0.0003(8) C47 0.0229(10) 0.0293(11) 0.0134(9) -0.0003(8) 0.0018(7) 0.0003(8) C57 0.0271(10) 0.0224(10) 0.0157(9) -0.0040(8) 0.0029(8) 0.0045(8) C51 0.0296(10) 0.0231(10) 0.0145(9) 0.0004(8) 0.0020(8) 0.0077(8) C4 0.0243(10) 0.0287(11) 0.0179(10) -0.0005(8) -0.0011(8) -0.0053(8) C33 0.0232(10) 0.0258(11) 0.0161(10) -0.0022(8) 0.0037(8) 0.0017(8) C2 0.0226(9) 0.0205(10) 0.0182(10) 0.0007(8) 0.0037(8) 0.0003(8) C1 0.0215(9) 0.0221(10) 0.0199(10) -0.0012(8) 0.0022(8) -0.0004(8) C22 0.0246(10) 0.0254(11) 0.0223(10) -0.0005(9) 0.0011(8) -0.0007(8) C44 0.0332(11) 0.0249(11) 0.0232(11) 0.0020(9) 0.0082(9) 0.0050(9) C43 0.0244(10) 0.0276(11) 0.0184(10) -0.0016(8) 0.0043(8) 0.0020(8) C8 0.0244(10) 0.0322(11) 0.0203(10) -0.0008(9) 0.0014(8) -0.0028(9) C34 0.0246(10) 0.0287(11) 0.0188(10) -0.0042(8) 0.0045(8) 0.0037(8) C50 0.0273(11) 0.0288(11) 0.0219(11) -0.0021(9) 0.0043(8) -0.0034(9) C16 0.0360(12) 0.0200(10) 0.0257(11) 0.0020(9) -0.0008(9) -0.0073(9) C32 0.0241(10) 0.0272(11) 0.0232(11) -0.0012(9) 0.0023(8) -0.0033(9) C26 0.0229(10) 0.0257(11) 0.0238(11) -0.0034(9) 0.0030(8) -0.0012(8) C38 0.0262(10) 0.0276(11) 0.0233(10) -0.0010(9) 0.0064(8) -0.0012(9) C14 0.0183(9) 0.0357(12) 0.0204(10) 0.0009(9) 0.0046(8) 0.0010(8) C17 0.0280(11) 0.0247(11) 0.0210(10) -0.0022(9) -0.0009(8) 0.0004(8) C62 0.0276(10) 0.0284(11) 0.0220(10) -0.0032(9) 0.0017(8) 0.0017(9) C18 0.0286(11) 0.0252(11) 0.0243(11) -0.0029(9) 0.0015(8) 0.0016(9) C46 0.0187(10) 0.0396(13) 0.0216(11) 0.0021(9) 0.0044(8) 0.0004(9) C23 0.0285(11) 0.0301(12) 0.0287(12) -0.0033(9) -0.0053(9) -0.0025(9) C5 0.0312(11) 0.0358(12) 0.0222(11) 0.0037(9) 0.0017(9) -0.0119(10) C35 0.0284(11) 0.0336(12) 0.0276(11) 0.0016(9) 0.0039(9) 0.0079(9) C58 0.0297(11) 0.0256(11) 0.0271(11) -0.0013(9) 0.0050(9) 0.0046(9) C28 0.0249(10) 0.0260(11) 0.0210(10) 0.0000(8) 0.0037(8) -0.0027(8) C56 0.0339(11) 0.0238(11) 0.0224(11) -0.0007(9) 0.0056(9) -0.0005(9) C15 0.0290(11) 0.0342(12) 0.0220(11) 0.0010(9) 0.0026(9) -0.0132(9) C45 0.0264(11) 0.0356(12) 0.0242(11) 0.0049(9) 0.0073(8) 0.0109(9) C29 0.0329(11) 0.0289(12) 0.0248(11) -0.0049(9) 0.0065(9) 0.0029(9) C30 0.0320(11) 0.0388(13) 0.0256(11) -0.0004(10) 0.0134(9) 0.0024(10) C60 0.0445(13) 0.0307(12) 0.0225(11) -0.0008(9) -0.0050(10) 0.0114(10) C25 0.0306(11) 0.0269(11) 0.0267(11) 0.0040(9) 0.0021(9) 0.0029(9) C7 0.0237(10) 0.0433(13) 0.0283(12) 0.0007(10) 0.0029(9) 0.0049(9) C6 0.0233(10) 0.0515(15) 0.0247(11) 0.0018(10) 0.0042(9) -0.0069(10) C61 0.0301(11) 0.0325(12) 0.0264(11) -0.0042(10) -0.0046(9) 0.0045(9) C31 0.0279(11) 0.0351(12) 0.0271(11) 0.0025(10) 0.0089(9) -0.0053(9) C24 0.0337(11) 0.0333(12) 0.0222(11) -0.0015(9) -0.0072(9) 0.0052(9) C52 0.0268(11) 0.0411(13) 0.0202(11) -0.0036(9) 0.0037(8) 0.0058(9) C48 0.0315(11) 0.0259(11) 0.0352(12) -0.0020(9) 0.0096(9) -0.0013(9) C55 0.0478(13) 0.0237(11) 0.0250(11) -0.0025(9) 0.0005(10) 0.0005(10) C36 0.0227(11) 0.0484(15) 0.0348(13) 0.0015(11) 0.0027(9) 0.0039(10) C59 0.0456(13) 0.0277(12) 0.0258(12) 0.0057(9) 0.0091(10) 0.0072(10) C37 0.0250(11) 0.0394(13) 0.0341(12) -0.0013(10) 0.0048(9) -0.0081(10) C53 0.0344(12) 0.0543(15) 0.0230(11) -0.0055(11) 0.0081(9) 0.0129(11) C39 0.0306(11) 0.0252(11) 0.0441(14) 0.0002(10) 0.0041(10) 0.0030(9) C11 0.0362(13) 0.0352(13) 0.0477(15) 0.0080(11) 0.0105(11) 0.0055(10) C9 0.0373(12) 0.0304(12) 0.0360(13) 0.0052(10) 0.0012(10) -0.0032(10) C54 0.0511(14) 0.0376(13) 0.0206(11) -0.0094(10) 0.0036(10) 0.0130(11) C20 0.0360(12) 0.0285(12) 0.0429(14) -0.0066(10) -0.0029(10) 0.0048(10) B3 0.0230(11) 0.0187(11) 0.0202(11) 0.0000(9) 0.0038(9) 0.0007(9) C41 0.0365(12) 0.0298(12) 0.0437(14) 0.0034(11) 0.0095(10) -0.0028(10) B2 0.0207(10) 0.0214(11) 0.0203(11) -0.0018(9) 0.0036(9) 0.0014(9) C19 0.0373(13) 0.0469(15) 0.0484(15) 0.0001(12) 0.0030(11) -0.0201(11) B4 0.0230(11) 0.0194(11) 0.0209(11) -0.0021(9) 0.0059(9) -0.0024(9) B1 0.0239(11) 0.0205(11) 0.0192(11) 0.0001(9) 0.0025(9) 0.0000(9) C49 0.0345(13) 0.0478(15) 0.0537(16) 0.0060(13) 0.0129(11) 0.0163(11) C10 0.0283(13) 0.081(2) 0.0538(17) 0.0110(15) 0.0152(12) -0.0076(13) C40 0.0251(12) 0.072(2) 0.074(2) 0.0151(16) 0.0012(12) 0.0047(12) C63 0.132(4) 0.070(2) 0.058(2) -0.0069(19) 0.042(2) -0.043(2) C64 0.138(4) 0.078(3) 0.084(3) -0.018(2) 0.048(3) -0.054(3) C65 0.125(4) 0.077(3) 0.113(3) -0.009(2) 0.044(3) -0.025(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 S1 C1 123.39(10) . . ? C21 N1 N2 116.37(14) . . ? B1 N1 N2 110.22(15) . . ? B1 N1 C21 127.38(16) . . ? C27 N2 N1 115.74(14) . . ? B2 N2 N1 113.00(15) . . ? B2 N2 C27 129.08(16) . . ? C51 N3 N4 116.97(15) . . ? B3 N3 N4 110.90(15) . . ? B3 N3 C51 129.29(16) . . ? C57 N4 N3 115.06(14) . . ? B4 N4 N3 111.54(15) . . ? B4 N4 C57 127.19(16) . . ? C12 C13 C18 119.97(17) . . ? C14 C13 C12 119.73(18) . . ? C14 C13 C18 120.30(17) . . ? C22 C21 N1 119.26(17) . . ? C22 C21 C26 120.19(18) . . ? C26 C21 N1 120.55(17) . . ? C47 C42 C43 118.84(17) . . ? C47 C42 B4 122.52(18) . . ? C43 C42 B4 118.37(17) . . ? C13 C12 C17 118.66(17) . . ? C13 C12 B2 122.65(17) . . ? C17 C12 B2 118.21(17) . . ? C4 C3 B1 120.18(17) . . ? C8 C3 C4 118.71(17) . . ? C8 C3 B1 120.39(18) . . ? C32 C27 N2 119.99(18) . . ? C32 C27 C28 120.42(18) . . ? C28 C27 N2 119.58(17) . . ? C42 C47 C50 119.90(17) . . ? C46 C47 C42 119.72(19) . . ? C46 C47 C50 120.38(18) . . ? C62 C57 N4 119.37(17) . . ? C62 C57 C58 119.67(18) . . ? C58 C57 N4 120.95(17) . . ? C56 C51 N3 121.18(17) . . ? C56 C51 C52 120.07(18) . . ? C52 C51 N3 118.75(18) . . ? C3 C4 C9 120.42(18) . . ? C5 C4 C3 119.69(19) . . ? C5 C4 C9 119.89(19) . . ? C34 C33 C38 118.67(18) . . ? C34 C33 B3 121.83(17) . . ? C38 C33 B3 119.25(17) . . ? B3 C2 S1 110.89(14) . . ? B4 C2 S1 140.93(15) . . ? B4 C2 B3 105.78(16) . . ? B2 C1 S1 142.22(15) . . ? B1 C1 S1 110.18(14) . . ? B1 C1 B2 105.90(16) . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.71(19) . . ? C23 C22 H22 120.1 . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C45 C44 C43 121.8(2) . . ? C42 C43 C48 120.68(17) . . ? C44 C43 C42 119.70(18) . . ? C44 C43 C48 119.57(19) . . ? C3 C8 C11 120.66(18) . . ? C7 C8 C3 119.74(19) . . ? C7 C8 C11 119.59(19) . . ? C33 C34 C39 119.72(18) . . ? C35 C34 C33 119.71(19) . . ? C35 C34 C39 120.56(19) . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C15 C16 C17 121.65(19) . . ? C27 C32 H32 120.2 . . ? C27 C32 C31 119.54(19) . . ? C31 C32 H32 120.2 . . ? C21 C26 H26 120.2 . . ? C25 C26 C21 119.59(19) . . ? C25 C26 H26 120.2 . . ? C33 C38 C41 120.40(18) . . ? C37 C38 C33 119.89(19) . . ? C37 C38 C41 119.65(19) . . ? C13 C14 H14 119.0 . . ? C15 C14 C13 121.95(18) . . ? C15 C14 H14 119.0 . . ? C12 C17 C20 120.20(18) . . ? C16 C17 C12 119.88(18) . . ? C16 C17 C20 119.91(19) . . ? C57 C62 H62 120.0 . . ? C61 C62 C57 120.0(2) . . ? C61 C62 H62 120.0 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C47 C46 H46 119.1 . . ? C45 C46 C47 121.78(19) . . ? C45 C46 H46 119.1 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.17(19) . . ? C24 C23 H23 119.9 . . ? C4 C5 H5 119.1 . . ? C6 C5 C4 121.8(2) . . ? C6 C5 H5 119.1 . . ? C34 C35 H35 119.1 . . ? C36 C35 C34 121.9(2) . . ? C36 C35 H35 119.1 . . ? C57 C58 H58 120.2 . . ? C59 C58 C57 119.5(2) . . ? C59 C58 H58 120.2 . . ? C27 C28 H28 120.3 . . ? C29 C28 C27 119.42(19) . . ? C29 C28 H28 120.3 . . ? C51 C56 H56 120.3 . . ? C55 C56 C51 119.4(2) . . ? C55 C56 H56 120.3 . . ? C16 C15 C14 118.10(18) . . ? C16 C15 C19 121.2(2) . . ? C14 C15 C19 120.7(2) . . ? C44 C45 C46 118.12(18) . . ? C44 C45 C49 121.0(2) . . ? C46 C45 C49 120.9(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.2(2) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 119.9 . . ? C31 C30 C29 120.26(19) . . ? C31 C30 H30 119.9 . . ? C61 C60 H60 120.2 . . ? C61 C60 C59 119.7(2) . . ? C59 C60 H60 120.2 . . ? C26 C25 H25 119.8 . . ? C26 C25 C24 120.4(2) . . ? C24 C25 H25 119.8 . . ? C8 C7 H7 119.1 . . ? C6 C7 C8 121.8(2) . . ? C6 C7 H7 119.1 . . ? C5 C6 C10 120.7(2) . . ? C7 C6 C5 118.26(19) . . ? C7 C6 C10 121.1(2) . . ? C62 C61 H61 119.8 . . ? C60 C61 C62 120.4(2) . . ? C60 C61 H61 119.8 . . ? C32 C31 H31 119.9 . . ? C30 C31 C32 120.18(19) . . ? C30 C31 H31 119.9 . . ? C23 C24 C25 119.92(19) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C51 C52 H52 120.2 . . ? C53 C52 C51 119.7(2) . . ? C53 C52 H52 120.2 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C56 C55 H55 119.6 . . ? C54 C55 C56 120.8(2) . . ? C54 C55 H55 119.6 . . ? C35 C36 C40 121.1(2) . . ? C37 C36 C35 118.07(19) . . ? C37 C36 C40 120.8(2) . . ? C58 C59 H59 119.7 . . ? C60 C59 C58 120.7(2) . . ? C60 C59 H59 119.7 . . ? C38 C37 H37 119.1 . . ? C36 C37 C38 121.7(2) . . ? C36 C37 H37 119.1 . . ? C52 C53 H53 119.8 . . ? C54 C53 C52 120.4(2) . . ? C54 C53 H53 119.8 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C55 C54 C53 119.6(2) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 B3 C33 126.73(18) . . ? N3 B3 C2 106.24(16) . . ? C2 B3 C33 127.03(17) . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N2 B2 C12 118.85(17) . . ? N2 B2 C1 104.36(16) . . ? C1 B2 C12 136.24(18) . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 B4 C42 119.66(17) . . ? N4 B4 C2 105.37(16) . . ? C2 B4 C42 133.41(18) . . ? N1 B1 C3 127.92(17) . . ? N1 B1 C1 106.42(16) . . ? C1 B1 C3 125.48(17) . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C63 C63 H63A 108.4 3_667 . ? C63 C63 H63B 108.4 3_667 . ? H63A C63 H63B 107.5 . . ? C64 C63 C63 115.3(4) . 3_667 ? C64 C63 H63A 108.4 . . ? C64 C63 H63B 108.4 . . ? C63 C64 H64A 108.8 . . ? C63 C64 H64B 108.8 . . ? C63 C64 C65 113.7(3) . . ? H64A C64 H64B 107.7 . . ? C65 C64 H64A 108.8 . . ? C65 C64 H64B 108.8 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65B 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C2 1.6413(19) . ? S1 C1 1.6419(19) . ? N1 N2 1.450(2) . ? N1 C21 1.428(2) . ? N1 B1 1.411(3) . ? N2 C27 1.436(2) . ? N2 B2 1.421(3) . ? N3 N4 1.450(2) . ? N3 C51 1.427(2) . ? N3 B3 1.413(3) . ? N4 C57 1.433(2) . ? N4 B4 1.428(3) . ? C13 C12 1.406(3) . ? C13 C14 1.391(3) . ? C13 C18 1.505(3) . ? C21 C22 1.386(3) . ? C21 C26 1.393(3) . ? C42 C47 1.404(3) . ? C42 C43 1.409(3) . ? C42 B4 1.571(3) . ? C12 C17 1.410(3) . ? C12 B2 1.566(3) . ? C3 C4 1.408(3) . ? C3 C8 1.406(3) . ? C3 B1 1.572(3) . ? C27 C32 1.384(3) . ? C27 C28 1.392(3) . ? C47 C50 1.504(3) . ? C47 C46 1.392(3) . ? C57 C62 1.388(3) . ? C57 C58 1.393(3) . ? C51 C56 1.389(3) . ? C51 C52 1.389(3) . ? C4 C5 1.391(3) . ? C4 C9 1.507(3) . ? C33 C34 1.402(3) . ? C33 C38 1.406(3) . ? C33 B3 1.575(3) . ? C2 B3 1.557(3) . ? C2 B4 1.551(3) . ? C1 B2 1.563(3) . ? C1 B1 1.561(3) . ? C22 H22 0.9500 . ? C22 C23 1.390(3) . ? C44 H44 0.9500 . ? C44 C43 1.394(3) . ? C44 C45 1.384(3) . ? C43 C48 1.508(3) . ? C8 C7 1.395(3) . ? C8 C11 1.499(3) . ? C34 C35 1.392(3) . ? C34 C39 1.507(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C16 H16 0.9500 . ? C16 C17 1.393(3) . ? C16 C15 1.387(3) . ? C32 H32 0.9500 . ? C32 C31 1.388(3) . ? C26 H26 0.9500 . ? C26 C25 1.383(3) . ? C38 C37 1.392(3) . ? C38 C41 1.504(3) . ? C14 H14 0.9500 . ? C14 C15 1.389(3) . ? C17 C20 1.512(3) . ? C62 H62 0.9500 . ? C62 C61 1.387(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C46 H46 0.9500 . ? C46 C45 1.391(3) . ? C23 H23 0.9500 . ? C23 C24 1.384(3) . ? C5 H5 0.9500 . ? C5 C6 1.387(3) . ? C35 H35 0.9500 . ? C35 C36 1.386(3) . ? C58 H58 0.9500 . ? C58 C59 1.384(3) . ? C28 H28 0.9500 . ? C28 C29 1.385(3) . ? C56 H56 0.9500 . ? C56 C55 1.385(3) . ? C15 C19 1.510(3) . ? C45 C49 1.509(3) . ? C29 H29 0.9500 . ? C29 C30 1.382(3) . ? C30 H30 0.9500 . ? C30 C31 1.379(3) . ? C60 H60 0.9500 . ? C60 C61 1.375(3) . ? C60 C59 1.383(3) . ? C25 H25 0.9500 . ? C25 C24 1.385(3) . ? C7 H7 0.9500 . ? C7 C6 1.381(3) . ? C6 C10 1.516(3) . ? C61 H61 0.9500 . ? C31 H31 0.9500 . ? C24 H24 0.9500 . ? C52 H52 0.9500 . ? C52 C53 1.386(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C55 H55 0.9500 . ? C55 C54 1.377(3) . ? C36 C37 1.383(3) . ? C36 C40 1.519(3) . ? C59 H59 0.9500 . ? C37 H37 0.9500 . ? C53 H53 0.9500 . ? C53 C54 1.384(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C54 H54 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C63 C63 1.514(8) 3_667 ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 C64 1.507(6) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 C65 1.544(6) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C2 B3 N3 170.45(14) . . . . ? S1 C2 B3 C33 -9.8(3) . . . . ? S1 C2 B4 N4 -163.03(19) . . . . ? S1 C2 B4 C42 2.1(4) . . . . ? S1 C1 B2 N2 -163.7(2) . . . . ? S1 C1 B2 C12 7.1(4) . . . . ? S1 C1 B1 N1 171.29(14) . . . . ? S1 C1 B1 C3 -4.2(3) . . . . ? N1 N2 C27 C32 134.22(18) . . . . ? N1 N2 C27 C28 -44.6(2) . . . . ? N1 N2 B2 C12 -173.23(16) . . . . ? N1 N2 B2 C1 -0.4(2) . . . . ? N1 C21 C22 C23 179.73(17) . . . . ? N1 C21 C26 C25 179.44(17) . . . . ? N2 N1 C21 C22 142.85(17) . . . . ? N2 N1 C21 C26 -37.6(2) . . . . ? N2 N1 B1 C3 172.34(19) . . . . ? N2 N1 B1 C1 -3.0(2) . . . . ? N2 C27 C32 C31 -178.81(18) . . . . ? N2 C27 C28 C29 179.05(18) . . . . ? N3 N4 C57 C62 -141.66(18) . . . . ? N3 N4 C57 C58 37.0(2) . . . . ? N3 N4 B4 C42 -165.75(16) . . . . ? N3 N4 B4 C2 1.8(2) . . . . ? N3 C51 C56 C55 -178.69(18) . . . . ? N3 C51 C52 C53 179.98(19) . . . . ? N4 N3 C51 C56 32.9(2) . . . . ? N4 N3 C51 C52 -146.35(18) . . . . ? N4 N3 B3 C33 177.09(18) . . . . ? N4 N3 B3 C2 -3.2(2) . . . . ? N4 C57 C62 C61 179.86(18) . . . . ? N4 C57 C58 C59 -178.75(18) . . . . ? C13 C12 C17 C16 1.1(3) . . . . ? C13 C12 C17 C20 -179.89(18) . . . . ? C13 C12 B2 N2 -79.1(2) . . . . ? C13 C12 B2 C1 111.1(3) . . . . ? C13 C14 C15 C16 1.2(3) . . . . ? C13 C14 C15 C19 -179.58(19) . . . . ? C21 N1 N2 C27 -38.1(2) . . . . ? C21 N1 N2 B2 157.08(17) . . . . ? C21 N1 B1 C3 21.1(3) . . . . ? C21 N1 B1 C1 -154.31(18) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C21 C26 C25 C24 1.0(3) . . . . ? C42 C47 C46 C45 1.5(3) . . . . ? C12 C13 C14 C15 -0.8(3) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C3 C8 C7 C6 0.7(3) . . . . ? C27 N2 B2 C12 24.5(3) . . . . ? C27 N2 B2 C1 -162.73(18) . . . . ? C27 C32 C31 C30 -0.2(3) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? C47 C42 C43 C44 2.0(3) . . . . ? C47 C42 C43 C48 179.49(18) . . . . ? C47 C42 B4 N4 -81.7(2) . . . . ? C47 C42 B4 C2 114.9(2) . . . . ? C47 C46 C45 C44 1.0(3) . . . . ? C47 C46 C45 C49 -178.9(2) . . . . ? C57 N4 B4 C42 -15.2(3) . . . . ? C57 N4 B4 C2 152.39(18) . . . . ? C57 C62 C61 C60 -1.4(3) . . . . ? C57 C58 C59 C60 -0.8(3) . . . . ? C51 N3 N4 C57 43.8(2) . . . . ? C51 N3 N4 B4 -161.81(17) . . . . ? C51 N3 B3 C33 -22.9(3) . . . . ? C51 N3 B3 C2 156.79(18) . . . . ? C51 C56 C55 C54 -1.0(3) . . . . ? C51 C52 C53 C54 -1.6(3) . . . . ? C4 C3 C8 C7 0.1(3) . . . . ? C4 C3 C8 C11 178.80(19) . . . . ? C4 C3 B1 N1 106.3(2) . . . . ? C4 C3 B1 C1 -79.2(3) . . . . ? C4 C5 C6 C7 -1.0(3) . . . . ? C4 C5 C6 C10 178.8(2) . . . . ? C33 C34 C35 C36 1.5(3) . . . . ? C33 C38 C37 C36 1.6(3) . . . . ? C2 S1 C1 B2 -26.8(3) . . . . ? C2 S1 C1 B1 171.32(13) . . . . ? C1 S1 C2 B3 169.31(13) . . . . ? C1 S1 C2 B4 -31.9(3) . . . . ? C22 C21 C26 C25 -1.0(3) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C43 C42 C47 C50 176.59(17) . . . . ? C43 C42 C47 C46 -3.0(3) . . . . ? C43 C42 B4 N4 92.2(2) . . . . ? C43 C42 B4 C2 -71.2(3) . . . . ? C43 C44 C45 C46 -2.0(3) . . . . ? C43 C44 C45 C49 177.9(2) . . . . ? C8 C3 C4 C5 -1.3(3) . . . . ? C8 C3 C4 C9 179.00(18) . . . . ? C8 C3 B1 N1 -83.6(3) . . . . ? C8 C3 B1 C1 90.9(2) . . . . ? C8 C7 C6 C5 -0.2(3) . . . . ? C8 C7 C6 C10 180.0(2) . . . . ? C34 C33 C38 C37 -2.4(3) . . . . ? C34 C33 C38 C41 174.97(19) . . . . ? C34 C33 B3 N3 91.5(3) . . . . ? C34 C33 B3 C2 -88.1(3) . . . . ? C34 C35 C36 C37 -2.3(3) . . . . ? C34 C35 C36 C40 177.4(2) . . . . ? C50 C47 C46 C45 -178.06(19) . . . . ? C32 C27 C28 C29 0.3(3) . . . . ? C26 C21 C22 C23 0.1(3) . . . . ? C26 C25 C24 C23 -0.1(3) . . . . ? C38 C33 C34 C35 0.9(3) . . . . ? C38 C33 C34 C39 -179.76(18) . . . . ? C38 C33 B3 N3 -94.3(3) . . . . ? C38 C33 B3 C2 86.1(3) . . . . ? C14 C13 C12 C17 -0.3(3) . . . . ? C14 C13 C12 B2 171.61(17) . . . . ? C17 C12 B2 N2 92.9(2) . . . . ? C17 C12 B2 C1 -77.0(3) . . . . ? C17 C16 C15 C14 -0.5(3) . . . . ? C17 C16 C15 C19 -179.6(2) . . . . ? C62 C57 C58 C59 -0.1(3) . . . . ? C18 C13 C12 C17 -179.75(17) . . . . ? C18 C13 C12 B2 -7.8(3) . . . . ? C18 C13 C14 C15 178.57(18) . . . . ? C35 C36 C37 C38 0.8(3) . . . . ? C58 C57 C62 C61 1.2(3) . . . . ? C28 C27 C32 C31 0.0(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C56 C51 C52 C53 0.8(3) . . . . ? C56 C55 C54 C53 0.2(3) . . . . ? C15 C16 C17 C12 -0.7(3) . . . . ? C15 C16 C17 C20 -179.72(19) . . . . ? C45 C44 C43 C42 0.5(3) . . . . ? C45 C44 C43 C48 -176.99(19) . . . . ? C29 C30 C31 C32 0.2(3) . . . . ? C61 C60 C59 C58 0.6(3) . . . . ? C52 C51 C56 C55 0.5(3) . . . . ? C52 C53 C54 C55 1.1(3) . . . . ? C59 C60 C61 C62 0.5(3) . . . . ? C39 C34 C35 C36 -177.9(2) . . . . ? C11 C8 C7 C6 -178.0(2) . . . . ? C9 C4 C5 C6 -178.5(2) . . . . ? B3 N3 N4 C57 -153.48(17) . . . . ? B3 N3 N4 B4 0.9(2) . . . . ? B3 N3 C51 C56 -126.1(2) . . . . ? B3 N3 C51 C52 54.7(3) . . . . ? B3 C33 C34 C35 175.12(18) . . . . ? B3 C33 C34 C39 -5.5(3) . . . . ? B3 C33 C38 C37 -176.75(19) . . . . ? B3 C33 C38 C41 0.6(3) . . . . ? B3 C2 B4 N4 -3.6(2) . . . . ? B3 C2 B4 C42 161.5(2) . . . . ? C41 C38 C37 C36 -175.8(2) . . . . ? B2 N2 C27 C32 -63.9(3) . . . . ? B2 N2 C27 C28 117.3(2) . . . . ? B2 C12 C17 C16 -171.22(18) . . . . ? B2 C12 C17 C20 7.8(3) . . . . ? B2 C1 B1 N1 2.7(2) . . . . ? B2 C1 B1 C3 -172.81(19) . . . . ? B4 N4 C57 C62 68.6(3) . . . . ? B4 N4 C57 C58 -112.7(2) . . . . ? B4 C42 C47 C50 -9.5(3) . . . . ? B4 C42 C47 C46 170.89(18) . . . . ? B4 C42 C43 C44 -172.14(18) . . . . ? B4 C42 C43 C48 5.3(3) . . . . ? B4 C2 B3 N3 4.2(2) . . . . ? B4 C2 B3 C33 -176.13(19) . . . . ? B1 N1 N2 C27 167.11(17) . . . . ? B1 N1 N2 B2 2.3(2) . . . . ? B1 N1 C21 C22 -67.4(3) . . . . ? B1 N1 C21 C26 112.2(2) . . . . ? B1 C3 C4 C5 168.91(18) . . . . ? B1 C3 C4 C9 -10.7(3) . . . . ? B1 C3 C8 C7 -170.09(18) . . . . ? B1 C3 C8 C11 8.6(3) . . . . ? B1 C1 B2 N2 -1.4(2) . . . . ? B1 C1 B2 C12 169.5(2) . . . . ? C40 C36 C37 C38 -179.0(2) . . . . ? C63 C63 C64 C65 177.0(4) 3_667 . . . ?