#------------------------------------------------------------------------------ #$Date: 2019-12-06 11:25:25 +0200 (Fri, 06 Dec 2019) $ #$Revision: 244929 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556432.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_1556432 loop_ _publ_author_name 'Tsukao, M.' 'Hashikawa, Y.' 'Toyama, N.' 'Muraoka, M.' 'Murata, M.' 'Sasamori, T.' 'Wakamiya, A.' 'Murata, Y.' _publ_section_title ; Propeller-Shaped Aluminum Complexes with an Azaperylene Core in the Ligands ; _journal_name_full Inorganics _journal_page_first 109 _journal_paper_doi 10.3390/inorganics7090109 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C33 H26 N2 O3' _chemical_formula_sum 'C33 H26 N2 O3' _chemical_formula_weight 498.56 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.195(3) _cell_length_b 8.5030(13) _cell_length_c 30.611(5) _cell_measurement_reflns_used 8097 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.99 _cell_measurement_theta_min 1.33 _cell_volume 4996.2(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)' _computing_publication_material 'Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0458 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 22947 _diffrn_reflns_point_group_measured_fraction_full 0.921 _diffrn_reflns_point_group_measured_fraction_max 0.921 _diffrn_reflns_theta_full 24.987 _diffrn_reflns_theta_max 24.987 _diffrn_reflns_theta_min 2.122 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) or APEX2 Software ; _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.326 _exptl_crystal_description needle _exptl_crystal_F_000 2096 _exptl_crystal_size_max 1.000 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.140 _exptl_transmission_factor_max 0.7452 _exptl_transmission_factor_min 0.6331 _refine_diff_density_max 0.277 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Flack x determined using 2269 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.3(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 720 _refine_ls_number_reflns 8093 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0455 _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^)+(0.0526P)^2^+1.6848P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.1185 _reflns_Friedel_coverage 0.812 _reflns_Friedel_fraction_full 0.843 _reflns_Friedel_fraction_max 0.843 _reflns_number_gt 6207 _reflns_number_total 8093 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file compoundL3.cif _cod_data_source_block compoundL3 _cod_original_cell_volume 4996.2(13) _cod_database_code 1556432 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.920 _shelx_estimated_absorpt_t_max 0.988 _shelx_res_file ; 1pimoh_a.res created by SHELXL-2014/7 TITL 1PimOH_a.res in Pca2(1) REM Yadorkari-X generated CELL 0.71073 19.1954 8.5030 30.6105 90.0000 90.0000 90.0000 ZERR 4.0 0.0028 0.0013 0.0046 0.0000 0.0000 0.0000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2-X, +Y, 1/2+Z SYMM 1/2+X, -Y, +Z REM SPGR Pca21 orthorhombic SFAC C H N O UNIT 264 208 16 24 SIZE 0.14 0.15 1.00 TEMP -173.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H OMIT -10.000000 51.000000 OMIT 0 0 -2 OMIT 2 4 0 OMIT 9 3 -6 OMIT 9 3 6 DFIX 2.87 0.01 C13 N2B DFIX 2.86 0.01 C20 C16B DFIX 1.45 0.01 C49B O6B WGHT 0.052600 1.684800 FVAR 0.28925 0.61596 0.61332 C1 1 0.267808 0.635046 0.633816 11.00000 0.02739 0.02614 = 0.02559 -0.00351 -0.00278 0.00626 C2 1 0.330335 0.685549 0.650700 11.00000 0.03628 0.03792 = 0.03001 -0.00271 -0.01053 0.00233 AFIX 43 H2 2 0.344177 0.652378 0.679036 11.00000 -1.20000 AFIX 0 C3 1 0.373358 0.784264 0.626840 11.00000 0.02691 0.03925 = 0.03419 -0.00288 -0.01014 -0.00194 AFIX 43 H3 2 0.416706 0.815536 0.639039 11.00000 -1.20000 AFIX 0 C4 1 0.355090 0.838899 0.585661 11.00000 0.02550 0.03118 = 0.03166 -0.00413 -0.00262 0.00528 C5 1 0.290794 0.785905 0.566485 11.00000 0.02470 0.02480 = 0.02779 -0.00409 -0.00463 0.00723 C6 1 0.268535 0.834105 0.523856 11.00000 0.02323 0.03188 = 0.02595 -0.00302 0.00009 0.01375 C7 1 0.206267 0.778074 0.507883 11.00000 0.03256 0.03706 = 0.02242 -0.00490 -0.00356 0.00942 AFIX 43 H7 2 0.191599 0.809091 0.479522 11.00000 -1.20000 AFIX 0 C8 1 0.164042 0.676915 0.532191 11.00000 0.02463 0.03352 = 0.02940 -0.00944 -0.00293 0.00540 AFIX 43 H8 2 0.121372 0.640697 0.520109 11.00000 -1.20000 AFIX 0 C9 1 0.183362 0.628858 0.573445 11.00000 0.02859 0.02741 = 0.02373 -0.00750 -0.00492 0.00724 C10 1 0.246886 0.683630 0.591518 11.00000 0.02815 0.02373 = 0.02710 -0.00607 -0.00216 0.00616 C11 1 0.221425 0.532961 0.660151 11.00000 0.03508 0.02513 = 0.03431 -0.00685 -0.00520 0.00059 C12 1 0.137625 0.526439 0.598651 11.00000 0.02778 0.03155 = 0.03017 -0.01043 -0.00362 0.00615 C13 1 0.399232 0.946253 0.559893 11.00000 0.02717 0.03123 = 0.03388 -0.00374 0.00008 0.00536 C14 1 0.461626 1.006349 0.575500 11.00000 0.03289 0.03981 = 0.03925 0.00158 -0.00494 -0.00324 AFIX 43 H14 2 0.476873 0.978662 0.604006 11.00000 -1.20000 AFIX 0 C15 1 0.502586 1.107211 0.549959 11.00000 0.03366 0.04186 = 0.04214 -0.00169 -0.00627 -0.00487 PART 1 AFIX 43 H15 2 0.545836 1.145834 0.560567 21.00000 -1.20000 PART 2 AFIX 43 H15A 2 0.544533 1.146941 0.562186 -21.00000 -1.20000 PART 1 AFIX 0 C16A 1 0.480083 1.146730 0.511438 21.00000 0.04949 0.05444 = 0.07471 0.00568 0.01707 0.01041 PART 0 C17 1 0.420404 1.092235 0.492430 11.00000 0.02807 0.02611 = 0.04567 -0.00592 0.00523 0.00670 C18 1 0.343152 1.089897 0.434057 11.00000 0.03587 0.03794 = 0.03040 0.00210 -0.00138 0.01320 PART 1 AFIX 43 H18 2 0.330439 1.125854 0.405776 21.00000 -1.20000 PART 2 AFIX 43 H18A 2 0.331448 1.115636 0.404762 -21.00000 -1.20000 PART 0 AFIX 0 C19 1 0.297699 0.990573 0.457056 11.00000 0.03729 0.03542 = 0.03265 -0.00318 0.00127 0.01135 AFIX 43 H19 2 0.255236 0.958476 0.443842 11.00000 -1.20000 AFIX 0 C20 1 0.313771 0.938907 0.498540 11.00000 0.02575 0.03116 = 0.03170 -0.00077 0.00180 0.01039 C21 1 0.377235 0.991739 0.517491 11.00000 0.03017 0.02763 = 0.03390 -0.00629 0.00080 0.01145 C22 1 0.110334 0.394101 0.667190 11.00000 0.03767 0.02882 = 0.02713 -0.00055 -0.00496 -0.00264 C23 1 0.117654 0.230990 0.666778 11.00000 0.04897 0.02705 = 0.03942 -0.00555 -0.01911 -0.00329 C24 1 0.069067 0.145735 0.691110 11.00000 0.06771 0.02474 = 0.05031 0.00177 -0.01326 -0.00908 AFIX 43 H24 2 0.072494 0.034299 0.691712 11.00000 -1.20000 AFIX 0 C25 1 0.017405 0.215936 0.713808 11.00000 0.07004 0.04354 = 0.03796 0.00740 -0.00484 -0.02247 AFIX 43 H25 2 -0.014467 0.153605 0.730054 11.00000 -1.20000 AFIX 0 C26 1 0.010338 0.381387 0.713605 11.00000 0.05371 0.04229 = 0.03438 -0.00363 0.00197 -0.01105 AFIX 43 H26 2 -0.026642 0.430308 0.729121 11.00000 -1.20000 AFIX 0 C27 1 0.058293 0.472169 0.690354 11.00000 0.04172 0.03272 = 0.02338 -0.00142 -0.00071 -0.00847 C28 1 0.174694 0.148306 0.642088 11.00000 0.04766 0.03129 = 0.07089 -0.01351 -0.01489 0.00948 AFIX 13 H28 2 0.205276 0.230480 0.628731 11.00000 -1.20000 AFIX 0 C29 1 0.144763 0.049029 0.605226 11.00000 0.04472 0.03982 = 0.05894 -0.01001 -0.00463 0.00185 AFIX 137 H29 2 0.115719 -0.034781 0.617524 11.00000 -1.50000 H29A 2 0.182908 0.002391 0.588346 11.00000 -1.50000 H29B 2 0.116388 0.115547 0.586071 11.00000 -1.50000 AFIX 0 C30 1 0.219827 0.047073 0.671984 11.00000 0.11348 0.08590 = 0.12289 -0.03824 -0.06921 0.05786 AFIX 137 H30 2 0.234703 0.109428 0.697241 11.00000 -1.50000 H30A 2 0.260899 0.010654 0.655882 11.00000 -1.50000 H30B 2 0.192862 -0.043870 0.682027 11.00000 -1.50000 AFIX 0 C31 1 0.053231 0.649122 0.692200 11.00000 0.04302 0.03298 = 0.03189 -0.00300 0.00611 -0.00065 AFIX 13 H31 2 0.091404 0.691724 0.673381 11.00000 -1.20000 AFIX 0 C32 1 0.066919 0.707122 0.738530 11.00000 0.10843 0.03311 = 0.03588 -0.00832 -0.00675 -0.00056 AFIX 137 H32 2 0.030351 0.667912 0.758036 11.00000 -1.50000 H32A 2 0.066892 0.822369 0.738870 11.00000 -1.50000 H32B 2 0.112313 0.668375 0.748469 11.00000 -1.50000 AFIX 0 C33 1 -0.015156 0.707924 0.673151 11.00000 0.06405 0.03964 = 0.07757 0.00565 -0.01232 -0.00145 AFIX 137 H33 2 -0.017340 0.681214 0.642037 11.00000 -1.50000 H33A 2 -0.018043 0.822307 0.676635 11.00000 -1.50000 H33B 2 -0.054150 0.658138 0.688506 11.00000 -1.50000 AFIX 0 C34 1 0.454081 0.860357 0.366806 11.00000 0.03044 0.02450 = 0.02516 -0.00451 -0.00095 0.00097 C35 1 0.389982 0.814352 0.350173 11.00000 0.03060 0.03298 = 0.02862 -0.00182 -0.00509 0.00468 AFIX 43 H35 2 0.375429 0.851188 0.322331 11.00000 -1.20000 AFIX 0 C36 1 0.346835 0.714466 0.374058 11.00000 0.02534 0.03616 = 0.03574 -0.00350 -0.00410 0.00038 AFIX 43 H36 2 0.303356 0.683646 0.361954 11.00000 -1.20000 AFIX 0 C37 1 0.365550 0.658751 0.414996 11.00000 0.02350 0.02727 = 0.02868 -0.00553 -0.00030 0.00356 C38 1 0.430402 0.709177 0.433630 11.00000 0.02220 0.02527 = 0.02892 -0.00609 0.00142 0.00697 C39 1 0.451535 0.661881 0.476113 11.00000 0.02512 0.02549 = 0.02620 -0.00254 0.00050 0.00662 C40 1 0.515116 0.715576 0.492487 11.00000 0.02591 0.03436 = 0.02649 0.00276 0.00101 0.00702 AFIX 43 H40 2 0.529791 0.682842 0.520697 11.00000 -1.20000 AFIX 0 C41 1 0.557438 0.816067 0.468332 11.00000 0.02370 0.03703 = 0.02497 -0.00376 -0.00194 0.00453 AFIX 43 H41 2 0.599804 0.853640 0.480515 11.00000 -1.20000 AFIX 0 C42 1 0.538206 0.861270 0.426880 11.00000 0.02454 0.02738 = 0.02822 -0.00471 0.00071 0.00189 C43 1 0.474222 0.809830 0.408782 11.00000 0.02525 0.02428 = 0.02239 -0.00435 -0.00010 0.00391 C44 1 0.585687 0.963517 0.401231 11.00000 0.02918 0.03095 = 0.02401 -0.00097 -0.00115 -0.00108 C45 1 0.499677 0.960994 0.340215 11.00000 0.03535 0.02622 = 0.02577 -0.00162 -0.00217 0.00265 C46 1 0.321587 0.550312 0.440041 11.00000 0.02459 0.03035 = 0.03285 -0.00263 0.00459 0.00517 C47 1 0.259654 0.487882 0.424431 11.00000 0.02626 0.04113 = 0.04139 -0.00320 -0.00155 -0.00233 AFIX 43 H47 2 0.244583 0.514624 0.395819 11.00000 -1.20000 AFIX 0 C48 1 0.218906 0.386809 0.449665 11.00000 0.02919 0.04508 = 0.04549 0.00364 -0.00221 -0.00414 PART 1 AFIX 43 H48 2 0.176430 0.351580 0.437098 31.00000 -1.20000 PART 2 AFIX 43 H48A 2 0.177423 0.341377 0.438385 -31.00000 -1.20000 PART 1 AFIX 0 C49A 1 0.232586 0.338959 0.486522 31.00000 0.02357 0.03035 = 0.05750 -0.01387 -0.00146 -0.01098 PART 0 C50 1 0.299329 0.403469 0.507489 11.00000 0.02797 0.03116 = 0.03973 0.00032 0.00753 0.00936 C51 1 0.375857 0.405742 0.566319 11.00000 0.03564 0.04018 = 0.02911 0.00599 0.00476 0.01278 PART 1 AFIX 43 H51 2 0.388329 0.372315 0.594881 31.00000 -1.20000 PART 2 AFIX 43 H51A 2 0.387502 0.375356 0.595278 -31.00000 -1.20000 PART 0 AFIX 0 C52 1 0.421745 0.505057 0.543560 11.00000 0.02380 0.03704 = 0.03505 0.00410 -0.00076 0.01077 AFIX 43 H52 2 0.463992 0.537304 0.557016 11.00000 -1.20000 AFIX 0 C53 1 0.406156 0.556581 0.501724 11.00000 0.02633 0.02587 = 0.02887 -0.00081 0.00520 0.00871 C54 1 0.342588 0.504903 0.482528 11.00000 0.02395 0.02570 = 0.03428 -0.00273 0.00576 0.00658 C55 1 0.610601 1.100882 0.332908 11.00000 0.03806 0.03018 = 0.02439 -0.00217 -0.00236 -0.00872 C56 1 0.599900 1.263384 0.334569 11.00000 0.04630 0.03005 = 0.03563 -0.00353 -0.00137 -0.00480 C57 1 0.644288 1.356710 0.309310 11.00000 0.07742 0.02437 = 0.04098 0.00106 -0.00134 -0.01143 AFIX 43 H57 2 0.638705 1.467720 0.309502 11.00000 -1.20000 AFIX 0 C58 1 0.695897 1.290450 0.284194 11.00000 0.07917 0.04766 = 0.03759 0.00082 0.01141 -0.02550 AFIX 43 H58 2 0.725198 1.355890 0.267015 11.00000 -1.20000 AFIX 0 C59 1 0.705320 1.132102 0.283753 11.00000 0.05824 0.04946 = 0.03716 -0.00388 0.01609 -0.00792 AFIX 43 H59 2 0.741588 1.089191 0.266322 11.00000 -1.20000 AFIX 0 C60 1 0.663597 1.030799 0.307990 11.00000 0.05297 0.03630 = 0.02783 -0.00224 0.00606 -0.00252 C61 1 0.543943 1.337329 0.362397 11.00000 0.05123 0.02927 = 0.04500 -0.00499 -0.00775 0.00256 AFIX 13 H61 2 0.518682 1.250467 0.377698 11.00000 -1.20000 AFIX 0 C62 1 0.576109 1.442174 0.397193 11.00000 0.06412 0.03947 = 0.04300 -0.00792 0.00297 -0.00018 AFIX 137 H62 2 0.609619 1.381209 0.414415 11.00000 -1.50000 H62A 2 0.539385 1.482357 0.416430 11.00000 -1.50000 H62B 2 0.600061 1.530551 0.383168 11.00000 -1.50000 AFIX 0 C63 1 0.490766 1.427862 0.335509 11.00000 0.10590 0.09494 = 0.04962 -0.02167 -0.02599 0.05473 AFIX 137 H63 2 0.454663 1.470150 0.354859 11.00000 -1.50000 H63A 2 0.469370 1.357188 0.314072 11.00000 -1.50000 H63B 2 0.513992 1.514598 0.320266 11.00000 -1.50000 AFIX 0 C64 1 0.672832 0.853484 0.305678 11.00000 0.05223 0.03338 = 0.04173 -0.00208 0.01480 0.00270 AFIX 13 H64 2 0.645945 0.805319 0.330254 11.00000 -1.20000 AFIX 0 C65 1 0.642963 0.793985 0.263593 11.00000 0.06865 0.04511 = 0.07343 -0.00702 -0.00777 -0.00609 AFIX 137 H65 2 0.593164 0.818991 0.262353 11.00000 -1.50000 H65A 2 0.649265 0.679779 0.261883 11.00000 -1.50000 H65B 2 0.666920 0.844263 0.239012 11.00000 -1.50000 AFIX 0 C66 1 0.748905 0.801970 0.309945 11.00000 0.09857 0.07441 = 0.14857 -0.02207 -0.06584 0.02482 AFIX 137 H66 2 0.751093 0.687276 0.312783 11.00000 -1.50000 H66A 2 0.769540 0.850899 0.335884 11.00000 -1.50000 H66B 2 0.774807 0.834742 0.283901 11.00000 -1.50000 PART 2 AFIX 0 C16B 1 0.401220 1.150245 0.450345 -21.00000 0.02393 C49B 1 0.323725 0.358690 0.551075 -31.00000 0.03640 PART 0 N1 3 0.158370 0.487218 0.641192 11.00000 0.03036 0.02482 = 0.02728 -0.00607 -0.00280 0.00055 PART 1 N2A 3 0.403647 1.134534 0.451136 21.00000 0.03986 0.03040 = 0.03897 0.00825 0.00691 0.01323 PART 0 N3 3 0.564731 1.000499 0.358694 11.00000 0.03381 0.02691 = 0.02936 -0.00097 0.00245 -0.00510 PART 1 N4A 3 0.313183 0.354405 0.548919 31.00000 0.01914 0.03104 = 0.04066 0.00564 0.01398 0.00665 PART 2 N2B 3 0.485418 1.151427 0.508435 -21.00000 0.01169 N4B 3 0.242178 0.353943 0.493533 -31.00000 0.02161 PART 0 O1 4 0.236338 0.489163 0.697182 11.00000 0.04939 0.04082 = 0.03425 0.00555 -0.01296 -0.00938 O2 4 0.082261 0.476152 0.584805 11.00000 0.03032 0.05871 = 0.03322 -0.00180 -0.00577 -0.00895 PART 1 O3A 4 0.522247 1.245233 0.482466 21.00000 0.03985 0.05216 = 0.03057 0.00278 -0.00222 -0.01001 AFIX 83 H3A 2 0.500129 1.262697 0.459290 21.00000 -1.50000 PART 0 AFIX 0 O4 4 0.484950 1.007724 0.304025 11.00000 0.04936 0.04618 = 0.02650 0.00743 -0.00768 -0.00964 O5 4 0.640685 1.013605 0.415301 11.00000 0.03404 0.05681 = 0.03471 0.00130 -0.00493 -0.01389 PART 1 O6A 4 0.199535 0.248719 0.518121 31.00000 0.03458 0.05183 = 0.05038 0.01636 0.00014 -0.00552 AFIX 83 H6A 2 0.225626 0.239792 0.540012 31.00000 -1.50000 PART 2 AFIX 0 O3B 4 0.446849 1.239658 0.432195 -21.00000 0.05685 AFIX 147 H3B 2 0.479269 1.257703 0.449932 -21.00000 -1.50000 AFIX 0 O6B 4 0.268656 0.256624 0.567437 -31.00000 0.03683 AFIX 83 H6B 2 0.236793 0.250075 0.548715 -31.00000 -1.50000 PART 0 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 1PimOH_a.res in Pca2(1) REM R1 = 0.0455 for 6207 Fo > 4sig(Fo) and 0.0659 for all 8093 data REM 720 parameters refined using 4 restraints END WGHT 0.0526 1.6848 REM Highest difference peak 0.277, deepest hole -0.207, 1-sigma level 0.039 Q1 1 0.7076 0.8017 0.3387 11.00000 0.05 0.28 Q2 1 0.6965 0.7942 0.2574 11.00000 0.05 0.23 Q3 1 0.2925 0.5065 0.7015 11.00000 0.05 0.23 Q4 1 0.4322 0.9964 0.3011 11.00000 0.05 0.19 Q5 1 0.3556 0.2091 0.3085 11.00000 0.05 0.18 Q6 1 0.3116 0.2176 0.6193 11.00000 0.05 0.17 Q7 1 0.4239 1.2015 0.4135 11.00000 0.05 0.17 Q8 1 0.3500 0.3085 0.2871 11.00000 0.05 0.17 Q9 1 0.3285 0.3906 0.2908 11.00000 0.05 0.16 Q10 1 0.6423 0.8430 0.2299 11.00000 0.05 0.15 Q11 1 0.0862 0.7034 0.4892 11.00000 0.05 0.15 Q12 1 0.2046 1.0119 0.4164 11.00000 0.05 0.15 Q13 1 0.2726 0.4619 0.6685 11.00000 0.05 0.15 Q14 1 0.6019 1.1506 0.4270 11.00000 0.05 0.15 Q15 1 0.5388 0.9794 0.2910 11.00000 0.05 0.14 Q16 1 0.6661 0.6683 0.2493 11.00000 0.05 0.14 Q17 1 0.1999 0.4797 0.6402 11.00000 0.05 0.14 Q18 1 0.5217 1.0176 0.3617 11.00000 0.05 0.14 Q19 1 0.1217 0.3585 0.5693 11.00000 0.05 0.14 Q20 1 0.4309 0.6958 0.6738 11.00000 0.05 0.14 ; _shelx_res_checksum 18470 _shelx_hkl_file ; 0 1 0 0.10 0.30 0 2 0 229.88 9.50 0 3 0 4.10 1.00 0 4 0 400.26 16.70 0 5 0 1.70 1.50 0 6 0 1463.05 59.09 0 7 0 9.60 2.30 0 8 0 93.69 5.70 0 -8 0 85.89 5.40 0 -10 0 1.10 2.20 -1 0 0 0.00 0.10 1 0 0 0.00 0.10 1 1 0 657.03 26.30 -1 1 0 660.03 26.30 -1 2 0 475.05 19.60 1 2 0 491.55 19.50 -1 3 0 128.69 5.60 1 3 0 119.29 5.50 1 4 0 333.17 14.00 -1 4 0 331.67 14.10 1 5 0 -0.40 1.20 -1 5 0 -0.90 1.40 1 6 0 18.80 2.40 -1 6 0 20.20 2.60 1 7 0 190.68 8.90 -1 7 0 173.28 8.90 -1 8 0 8.00 2.40 1 8 0 8.40 2.40 1 -10 0 4.40 2.70 -2 0 0 60.69 2.50 2 0 0 62.19 2.60 -2 0 0 60.99 2.50 -2 -1 0 1030.30 40.30 -2 1 0 1039.50 40.40 2 1 0 972.40 40.40 -2 2 0 4.70 1.00 -2 -2 0 6.50 0.80 2 2 0 3.50 0.70 2 3 0 9.20 1.10 -2 3 0 7.80 1.30 2 4 0 31.10 2.50 2 5 0 9.50 1.60 -2 5 0 9.10 2.00 -2 6 0 -2.80 1.40 2 6 0 0.80 1.40 2 -7 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286.97 11.90 0 -1 -6 288.67 11.90 0 -2 -6 109.89 4.60 0 2 -6 99.09 4.70 0 -2 6 102.09 4.60 0 4 -6 3.20 1.50 0 -4 6 1.40 1.10 0 -4 -6 1.30 1.30 0 -5 -6 2.40 1.20 0 -5 6 3.30 1.20 0 5 -6 1.40 1.60 0 6 -6 3.00 1.90 0 -6 6 5.20 1.50 0 -6 -6 6.20 1.60 0 7 -6 1.60 2.20 0 -7 6 0.50 1.50 0 -7 -6 1.10 1.60 0 -8 -6 12.30 2.50 0 -8 6 8.80 2.20 0 8 -6 12.10 2.80 0 9 -6 1.90 2.50 0 -9 -6 6.00 2.30 1 0 -6 0.90 0.60 -1 0 -6 0.80 0.50 -1 0 -6 0.30 0.70 -1 -1 6 197.38 8.00 1 -1 -6 198.28 8.00 -1 1 -6 186.58 7.70 -1 1 -6 191.48 8.10 1 1 -6 192.78 8.00 1 1 -6 182.68 7.60 1 -1 6 200.98 7.90 -1 -1 -6 192.28 7.90 1 -2 -6 562.24 22.30 -1 -2 6 576.64 22.40 -1 2 -6 549.54 22.30 -1 -2 6 541.65 21.90 -1 -2 -6 510.55 22.10 1 -2 6 589.64 22.20 1 2 -6 525.75 22.20 1 -3 -6 11.70 1.50 -1 3 -6 11.50 1.60 -1 -3 6 11.40 1.50 1 3 -6 11.10 1.50 1 -3 6 10.70 1.20 -1 -3 -6 7.30 1.10 -1 -4 6 38.90 2.90 1 -4 -6 45.70 3.00 -1 4 -6 43.50 3.20 -1 -4 -6 42.60 2.90 1 4 -6 44.70 3.00 1 -4 6 43.00 2.70 1 -5 -6 104.69 5.40 -1 5 -6 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4 -7 -6 37.90 3.70 -4 -7 -6 38.30 3.00 -4 -7 -6 41.40 3.80 4 7 -6 36.90 3.40 4 -8 -6 23.00 3.20 -4 8 -6 19.10 3.60 -4 -8 6 25.60 3.40 -4 -8 -6 20.10 3.10 -4 -9 6 5.60 2.60 4 -9 -6 5.20 2.60 -4 9 -6 9.40 3.40 -4 -9 -6 5.20 2.70 -5 0 6 0.40 0.60 5 0 -6 -0.20 0.50 -5 0 6 0.30 0.60 -5 0 -6 -0.10 0.70 -5 0 -6 0.00 0.50 -5 -1 6 279.87 11.20 -5 1 -6 261.87 10.80 -5 1 -6 254.47 11.10 -5 -1 6 269.67 10.80 5 -1 -6 271.07 11.00 -5 -1 -6 249.97 11.00 -5 1 6 266.47 10.80 -5 1 6 268.87 11.10 5 1 -6 268.47 10.80 -5 -1 -6 269.47 10.80 5 -2 -6 9.80 1.40 -5 2 -6 10.40 1.60 -5 -2 6 10.30 1.60 -5 -2 6 10.40 0.90 -5 2 -6 9.70 1.10 -5 -2 -6 10.30 1.40 5 2 -6 9.20 1.00 -5 -2 -6 10.00 0.90 5 -3 -6 8.10 1.70 -5 -3 6 8.30 1.00 -5 3 -6 9.10 1.30 -5 3 -6 4.60 2.10 -5 -3 6 8.70 1.70 -5 -3 -6 4.60 1.40 -5 -3 -6 13.00 1.10 5 3 -6 8.40 1.40 5 -4 -6 292.57 12.80 -5 4 -6 292.87 12.90 -5 -4 6 306.17 13.00 -5 -4 6 270.87 12.10 5 4 -6 275.97 12.30 -5 -4 -6 321.27 12.20 -5 -4 -6 302.47 12.70 5 -4 6 284.17 12.00 5 -5 -6 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0 -33 0.20 2.60 -9 0 -33 2.30 2.80 9 -1 -33 -2.90 2.40 -9 1 -33 2.00 3.00 9 1 -33 -0.50 2.90 -9 -1 -33 -1.10 2.80 0 0 -34 135.19 8.20 0 -1 -34 3.00 3.10 0 1 -34 3.10 2.70 0 2 -34 38.70 4.40 0 -2 -34 31.90 4.00 0 -3 -34 8.90 3.00 0 3 -34 5.70 2.90 -1 0 -34 3.00 2.70 1 0 -34 -1.10 2.50 -1 1 -34 17.20 3.30 1 -1 -34 17.80 3.60 -1 -1 -34 10.40 3.10 1 1 -34 15.40 3.60 1 -2 -34 7.40 3.10 -1 2 -34 5.50 2.70 -1 -2 -34 4.20 2.70 1 2 -34 3.00 2.80 1 -3 -34 0.60 2.60 -1 3 -34 4.60 2.90 1 3 -34 4.60 3.10 -1 -3 -34 1.60 2.70 2 0 -34 10.00 3.00 -2 0 -34 5.20 2.80 -2 1 -34 12.20 3.10 2 -1 -34 9.50 3.00 2 1 -34 11.20 3.00 -2 -1 -34 8.40 3.20 2 -2 -34 12.60 3.10 -2 2 -34 5.70 3.10 2 2 -34 7.30 3.30 -2 -2 -34 9.70 3.30 2 -3 -34 -0.30 2.80 -2 3 -34 4.80 3.30 2 3 -34 1.00 3.00 -2 -3 -34 4.40 2.70 3 0 -34 -1.70 2.50 -3 0 -34 2.50 3.00 3 -1 -34 5.20 2.70 -3 1 -34 3.30 2.80 3 1 -34 2.30 2.60 -3 -1 -34 7.80 2.90 -3 2 -34 -1.40 2.90 3 -2 -34 -1.80 2.80 -3 -2 -34 0.40 2.90 3 2 -34 0.10 2.90 -3 3 -34 15.70 3.70 3 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-35 40.50 4.60 -1 1 -35 39.40 4.40 1 1 -35 36.40 4.30 -1 -1 -35 31.80 4.20 -1 2 -35 8.60 3.40 1 -2 -35 7.70 3.30 -1 -2 -35 7.50 2.90 1 2 -35 6.10 3.00 2 0 -35 12.40 3.20 -2 0 -35 8.50 3.30 -2 1 -35 19.50 3.60 2 -1 -35 15.40 3.40 2 1 -35 21.80 3.90 -2 -1 -35 18.30 3.50 2 -2 -35 2.10 2.80 -2 2 -35 5.20 2.90 2 2 -35 -0.90 3.10 -2 -2 -35 0.60 2.70 -3 0 -35 -2.30 2.50 3 0 -35 -2.10 2.40 -3 1 -35 12.60 3.20 3 -1 -35 7.30 3.00 3 1 -35 7.10 3.20 -3 -1 -35 9.80 3.10 -3 2 -35 0.10 2.70 3 -2 -35 0.60 2.60 -3 -2 -35 1.70 3.00 3 2 -35 -0.20 3.10 4 0 -35 8.90 3.10 -4 0 -35 14.70 3.30 -4 1 -35 0.80 2.60 4 -1 -35 -0.50 2.60 -4 -1 -35 2.00 2.60 4 1 -35 5.30 3.10 -4 2 -35 -1.70 2.60 4 2 -35 -0.80 2.70 -4 -2 -35 2.20 2.70 -5 0 -35 0.40 3.10 5 0 -35 -0.80 2.70 -5 1 -35 3.80 2.80 5 -1 -35 2.70 2.80 5 1 -35 -0.90 2.60 -5 -1 -35 -1.80 2.80 6 0 -35 13.10 3.70 -6 0 -35 17.40 3.70 0 0 -36 41.20 4.70 0 -1 -36 1.00 2.70 0 1 -36 6.00 3.40 1 0 -36 -0.10 2.60 -1 0 -36 0.40 2.70 1 -1 -36 5.90 3.00 -1 1 -36 5.20 3.10 1 1 -36 6.60 3.00 -1 -1 -36 7.60 3.40 2 0 -36 19.00 4.00 -2 0 -36 20.90 3.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 47295 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2678(2) 0.6350(5) 0.63382(13) 0.0264(9) Uani 1 1 d . . . . . C2 C 0.3303(2) 0.6855(5) 0.65070(15) 0.0347(11) Uani 1 1 d . . . . . H2 H 0.3442 0.6524 0.6790 0.042 Uiso 1 1 calc R U . . . C3 C 0.3734(2) 0.7843(5) 0.62684(14) 0.0334(11) Uani 1 1 d . . . . . H3 H 0.4167 0.8155 0.6390 0.040 Uiso 1 1 calc R U . . . C4 C 0.3551(2) 0.8389(5) 0.58566(14) 0.0294(10) Uani 1 1 d . . . . . C5 C 0.2908(2) 0.7859(5) 0.56648(14) 0.0258(9) Uani 1 1 d . . . . . C6 C 0.2685(2) 0.8341(5) 0.52386(14) 0.0270(10) Uani 1 1 d . . . . . C7 C 0.2063(2) 0.7781(5) 0.50788(14) 0.0307(10) Uani 1 1 d . . . . . H7 H 0.1916 0.8091 0.4795 0.037 Uiso 1 1 calc R U . . . C8 C 0.1640(2) 0.6769(5) 0.53219(14) 0.0292(10) Uani 1 1 d . . . . . H8 H 0.1214 0.6407 0.5201 0.035 Uiso 1 1 calc R U . . . C9 C 0.1834(2) 0.6289(5) 0.57344(14) 0.0266(9) Uani 1 1 d . . . . . C10 C 0.2469(2) 0.6836(4) 0.59152(14) 0.0263(9) Uani 1 1 d . . . . . C11 C 0.2214(2) 0.5330(5) 0.66015(15) 0.0315(11) Uani 1 1 d . . . . . C12 C 0.1376(2) 0.5264(5) 0.59865(15) 0.0298(11) Uani 1 1 d . . . . . C13 C 0.3992(2) 0.9463(5) 0.55989(15) 0.0308(10) Uani 1 1 d D . . . . C14 C 0.4616(2) 1.0063(5) 0.57550(17) 0.0373(12) Uani 1 1 d . . . . . H14 H 0.4769 0.9787 0.6040 0.045 Uiso 1 1 calc R U . . . C15 C 0.5026(2) 1.1072(6) 0.54996(18) 0.0392(11) Uani 1 1 d . . . . . H15 H 0.5458 1.1458 0.5606 0.047 Uiso 0.616(8) 1 calc R U P A 1 H15A H 0.5445 1.1469 0.5622 0.047 Uiso 0.384(8) 1 calc R U P A 2 C16A C 0.4801(16) 1.147(4) 0.5114(10) 0.060(7) Uani 0.616(8) 1 d . . P A 1 C17 C 0.4204(2) 1.0922(5) 0.49243(16) 0.0333(11) Uani 1 1 d . . . . . C18 C 0.3432(2) 1.0899(6) 0.43406(15) 0.0347(11) Uani 1 1 d . . . . . H18 H 0.3304 1.1259 0.4058 0.042 Uiso 0.616(8) 1 calc R U P A 1 H18A H 0.3314 1.1156 0.4048 0.042 Uiso 0.384(8) 1 calc R U P A 2 C19 C 0.2977(2) 0.9906(5) 0.45706(15) 0.0351(11) Uani 1 1 d . . . . . H19 H 0.2552 0.9585 0.4438 0.042 Uiso 1 1 calc R U . . . C20 C 0.3138(2) 0.9389(5) 0.49854(14) 0.0295(10) Uani 1 1 d D . . . . C21 C 0.3772(2) 0.9917(5) 0.51749(16) 0.0306(10) Uani 1 1 d . . . . . C22 C 0.1103(2) 0.3941(5) 0.66719(15) 0.0312(10) Uani 1 1 d . . . . . C23 C 0.1177(2) 0.2310(5) 0.66678(16) 0.0385(11) Uani 1 1 d . . . . . C24 C 0.0691(3) 0.1457(6) 0.69111(18) 0.0476(13) Uani 1 1 d . . . . . H24 H 0.0725 0.0343 0.6917 0.057 Uiso 1 1 calc R U . . . C25 C 0.0174(3) 0.2159(6) 0.71381(18) 0.0505(13) Uani 1 1 d . . . . . H25 H -0.0145 0.1536 0.7301 0.061 Uiso 1 1 calc R U . . . C26 C 0.0103(3) 0.3814(6) 0.71361(16) 0.0435(12) Uani 1 1 d . . . . . H26 H -0.0266 0.4303 0.7291 0.052 Uiso 1 1 calc R U . . . C27 C 0.0583(2) 0.4722(5) 0.69035(14) 0.0326(10) Uani 1 1 d . . . . . C28 C 0.1747(3) 0.1483(6) 0.6421(2) 0.0499(13) Uani 1 1 d . . . . . H28 H 0.2053 0.2305 0.6287 0.060 Uiso 1 1 calc R U . . . C29 C 0.1448(3) 0.0490(6) 0.60523(18) 0.0478(13) Uani 1 1 d . . . . . H29 H 0.1157 -0.0348 0.6175 0.072 Uiso 1 1 calc R U . . . H29A H 0.1829 0.0024 0.5883 0.072 Uiso 1 1 calc R U . . . H29B H 0.1164 0.1155 0.5861 0.072 Uiso 1 1 calc R U . . . C30 C 0.2198(4) 0.0471(9) 0.6720(3) 0.107(3) Uani 1 1 d . . . . . H30 H 0.2347 0.1094 0.6972 0.161 Uiso 1 1 calc R U . . . H30A H 0.2609 0.0107 0.6559 0.161 Uiso 1 1 calc R U . . . H30B H 0.1929 -0.0439 0.6820 0.161 Uiso 1 1 calc R U . . . C31 C 0.0532(2) 0.6491(5) 0.69220(16) 0.0360(11) Uani 1 1 d . . . . . H31 H 0.0914 0.6917 0.6734 0.043 Uiso 1 1 calc R U . . . C32 C 0.0669(3) 0.7071(6) 0.73853(18) 0.0591(16) Uani 1 1 d . . . . . H32 H 0.0304 0.6679 0.7580 0.089 Uiso 1 1 calc R U . . . H32A H 0.0669 0.8224 0.7389 0.089 Uiso 1 1 calc R U . . . H32B H 0.1123 0.6684 0.7485 0.089 Uiso 1 1 calc R U . . . C33 C -0.0152(3) 0.7079(6) 0.6732(2) 0.0604(15) Uani 1 1 d . . . . . H33 H -0.0173 0.6812 0.6420 0.091 Uiso 1 1 calc R U . . . H33A H -0.0180 0.8223 0.6766 0.091 Uiso 1 1 calc R U . . . H33B H -0.0542 0.6581 0.6885 0.091 Uiso 1 1 calc R U . . . C34 C 0.4541(2) 0.8604(5) 0.36681(13) 0.0267(9) Uani 1 1 d . . . . . C35 C 0.3900(2) 0.8144(5) 0.35017(14) 0.0307(10) Uani 1 1 d . . . . . H35 H 0.3754 0.8512 0.3223 0.037 Uiso 1 1 calc R U . . . C36 C 0.3468(2) 0.7145(5) 0.37406(14) 0.0324(11) Uani 1 1 d . . . . . H36 H 0.3034 0.6836 0.3620 0.039 Uiso 1 1 calc R U . . . C37 C 0.36555(19) 0.6588(5) 0.41500(14) 0.0265(9) Uani 1 1 d . . . . . C38 C 0.43040(19) 0.7092(5) 0.43363(14) 0.0255(9) Uani 1 1 d . . . . . C39 C 0.45154(19) 0.6619(5) 0.47611(13) 0.0256(9) Uani 1 1 d . . . . . C40 C 0.5151(2) 0.7156(5) 0.49249(14) 0.0289(10) Uani 1 1 d . . . . . H40 H 0.5298 0.6828 0.5207 0.035 Uiso 1 1 calc R U . . . C41 C 0.5574(2) 0.8161(5) 0.46833(14) 0.0286(10) Uani 1 1 d . . . . . H41 H 0.5998 0.8536 0.4805 0.034 Uiso 1 1 calc R U . . . C42 C 0.5382(2) 0.8613(5) 0.42688(13) 0.0267(9) Uani 1 1 d . . . . . C43 C 0.4742(2) 0.8098(4) 0.40878(13) 0.0240(9) Uani 1 1 d . . . . . C44 C 0.5857(2) 0.9635(5) 0.40123(14) 0.0280(10) Uani 1 1 d . . . . . C45 C 0.4997(2) 0.9610(5) 0.34021(14) 0.0291(10) Uani 1 1 d . . . . . C46 C 0.3216(2) 0.5503(5) 0.44004(15) 0.0293(11) Uani 1 1 d . . . . . C47 C 0.2597(2) 0.4879(5) 0.42443(16) 0.0363(11) Uani 1 1 d . . . . . H47 H 0.2446 0.5146 0.3958 0.044 Uiso 1 1 calc R U . . . C48 C 0.2189(2) 0.3868(6) 0.44966(17) 0.0399(12) Uani 1 1 d . . . . . H48 H 0.1764 0.3516 0.4371 0.048 Uiso 0.613(8) 1 calc R U P B 1 H48A H 0.1774 0.3414 0.4384 0.048 Uiso 0.387(8) 1 calc R U P B 2 C49A C 0.2326(9) 0.339(2) 0.4865(7) 0.037(4) Uani 0.613(8) 1 d . . P B 1 C50 C 0.2993(2) 0.4035(5) 0.50749(15) 0.0330(11) Uani 1 1 d . . . . . C51 C 0.3759(2) 0.4057(5) 0.56632(15) 0.0350(11) Uani 1 1 d . . . . . H51 H 0.3883 0.3723 0.5949 0.042 Uiso 0.613(8) 1 calc R U P B 1 H51A H 0.3875 0.3754 0.5953 0.042 Uiso 0.387(8) 1 calc R U P B 2 C52 C 0.4217(2) 0.5051(5) 0.54356(15) 0.0320(10) Uani 1 1 d . . . . . H52 H 0.4640 0.5373 0.5570 0.038 Uiso 1 1 calc R U . . . C53 C 0.4062(2) 0.5566(5) 0.50172(14) 0.0270(10) Uani 1 1 d . . . . . C54 C 0.3426(2) 0.5049(5) 0.48253(15) 0.0280(10) Uani 1 1 d . . . . . C55 C 0.6106(2) 1.1009(5) 0.33291(14) 0.0309(10) Uani 1 1 d . . . . . C56 C 0.5999(2) 1.2634(5) 0.33457(15) 0.0373(11) Uani 1 1 d . . . . . C57 C 0.6443(3) 1.3567(6) 0.30931(17) 0.0476(13) Uani 1 1 d . . . . . H57 H 0.6387 1.4677 0.3095 0.057 Uiso 1 1 calc R U . . . C58 C 0.6959(3) 1.2904(6) 0.28419(18) 0.0548(15) Uani 1 1 d . . . . . H58 H 0.7252 1.3559 0.2670 0.066 Uiso 1 1 calc R U . . . C59 C 0.7053(3) 1.1321(6) 0.28375(17) 0.0483(13) Uani 1 1 d . . . . . H59 H 0.7416 1.0892 0.2663 0.058 Uiso 1 1 calc R U . . . C60 C 0.6636(2) 1.0308(5) 0.30799(15) 0.0390(11) Uani 1 1 d . . . . . C61 C 0.5439(3) 1.3373(5) 0.36240(17) 0.0418(11) Uani 1 1 d . . . . . H61 H 0.5187 1.2505 0.3777 0.050 Uiso 1 1 calc R U . . . C62 C 0.5761(3) 1.4422(6) 0.39719(18) 0.0489(13) Uani 1 1 d . . . . . H62 H 0.6096 1.3812 0.4144 0.073 Uiso 1 1 calc R U . . . H62A H 0.5394 1.4824 0.4164 0.073 Uiso 1 1 calc R U . . . H62B H 0.6001 1.5306 0.3832 0.073 Uiso 1 1 calc R U . . . C63 C 0.4908(4) 1.4279(8) 0.3355(2) 0.083(2) Uani 1 1 d . . . . . H63 H 0.4547 1.4702 0.3549 0.125 Uiso 1 1 calc R U . . . H63A H 0.4694 1.3572 0.3141 0.125 Uiso 1 1 calc R U . . . H63B H 0.5140 1.5146 0.3203 0.125 Uiso 1 1 calc R U . . . C64 C 0.6728(2) 0.8535(5) 0.30568(17) 0.0424(12) Uani 1 1 d . . . . . H64 H 0.6459 0.8053 0.3303 0.051 Uiso 1 1 calc R U . . . C65 C 0.6430(3) 0.7940(7) 0.2636(2) 0.0624(16) Uani 1 1 d . . . . . H65 H 0.5932 0.8190 0.2624 0.094 Uiso 1 1 calc R U . . . H65A H 0.6493 0.6798 0.2619 0.094 Uiso 1 1 calc R U . . . H65B H 0.6669 0.8443 0.2390 0.094 Uiso 1 1 calc R U . . . C66 C 0.7489(4) 0.8020(8) 0.3099(3) 0.107(3) Uani 1 1 d . . . . . H66 H 0.7511 0.6873 0.3128 0.161 Uiso 1 1 calc R U . . . H66A H 0.7695 0.8509 0.3359 0.161 Uiso 1 1 calc R U . . . H66B H 0.7748 0.8347 0.2839 0.161 Uiso 1 1 calc R U . . . C16B C 0.401(3) 1.150(5) 0.4503(15) 0.024(9) Uiso 0.384(8) 1 d D . P A 2 C49B C 0.324(2) 0.359(6) 0.551(2) 0.036(10) Uiso 0.387(8) 1 d D . P B 2 N1 N 0.15837(17) 0.4872(4) 0.64119(12) 0.0275(8) Uani 1 1 d . . . . . N2A N 0.4036(14) 1.135(3) 0.4511(9) 0.036(6) Uani 0.616(8) 1 d . . P A 1 N3 N 0.56473(18) 1.0005(4) 0.35869(12) 0.0300(9) Uani 1 1 d . . . . . N4A N 0.3132(10) 0.354(2) 0.5489(9) 0.030(5) Uani 0.613(8) 1 d . . P B 1 N2B N 0.4854(13) 1.151(3) 0.5084(7) 0.012(5) Uiso 0.384(8) 1 d D . P A 2 N4B N 0.2422(12) 0.354(3) 0.4935(7) 0.022(5) Uiso 0.387(8) 1 d . . P B 2 O1 O 0.23634(16) 0.4892(4) 0.69718(10) 0.0415(8) Uani 1 1 d . . . . . O2 O 0.08226(15) 0.4762(4) 0.58481(10) 0.0407(8) Uani 1 1 d . . . . . O3A O 0.5222(2) 1.2452(7) 0.48247(17) 0.0409(18) Uani 0.616(8) 1 d . . P A 1 H3A H 0.5001 1.2627 0.4593 0.061 Uiso 0.616(8) 1 calc R U P A 1 O4 O 0.48495(15) 1.0077(4) 0.30402(10) 0.0407(8) Uani 1 1 d . . . . . O5 O 0.64069(16) 1.0136(4) 0.41530(11) 0.0419(9) Uani 1 1 d . . . . . O6A O 0.1995(2) 0.2487(7) 0.51812(19) 0.0456(19) Uani 0.613(8) 1 d . . P B 1 H6A H 0.2256 0.2398 0.5400 0.068 Uiso 0.613(8) 1 calc R U P B 1 O3B O 0.4468(5) 1.2397(12) 0.4322(3) 0.057(3) Uiso 0.384(8) 1 d . . P A 2 H3B H 0.4793 1.2577 0.4499 0.085 Uiso 0.384(8) 1 calc R U P A 2 O6B O 0.2687(4) 0.2566(9) 0.5674(3) 0.037(3) Uiso 0.387(8) 1 d D . P B 2 H6B H 0.2368 0.2501 0.5487 0.055 Uiso 0.387(8) 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(2) 0.026(2) 0.026(2) -0.0035(18) -0.0028(18) 0.0063(18) C2 0.036(2) 0.038(3) 0.030(3) -0.003(2) -0.011(2) 0.002(2) C3 0.027(2) 0.039(3) 0.034(3) -0.003(2) -0.0101(19) -0.002(2) C4 0.026(2) 0.031(2) 0.032(3) -0.0041(19) -0.0026(19) 0.0053(18) C5 0.025(2) 0.025(2) 0.028(2) -0.0041(18) -0.0046(18) 0.0072(18) C6 0.023(2) 0.032(2) 0.026(2) -0.0030(19) 0.0001(17) 0.0138(19) C7 0.033(2) 0.037(3) 0.022(2) -0.0049(19) -0.0036(19) 0.009(2) C8 0.025(2) 0.034(2) 0.029(3) -0.009(2) -0.0029(18) 0.0054(18) C9 0.029(2) 0.027(2) 0.024(2) -0.0075(18) -0.0049(18) 0.0072(18) C10 0.028(2) 0.024(2) 0.027(2) -0.0061(18) -0.0022(17) 0.0062(18) C11 0.035(2) 0.025(2) 0.034(3) -0.007(2) -0.005(2) 0.0006(19) C12 0.028(2) 0.032(2) 0.030(3) -0.010(2) -0.0036(19) 0.0061(19) C13 0.027(2) 0.031(2) 0.034(3) -0.004(2) 0.0001(19) 0.0054(19) C14 0.033(3) 0.040(3) 0.039(3) 0.002(2) -0.005(2) -0.003(2) C15 0.034(2) 0.042(3) 0.042(3) -0.002(2) -0.006(2) -0.005(2) C16A 0.049(10) 0.054(9) 0.075(12) 0.006(6) 0.017(6) 0.010(5) C17 0.028(2) 0.026(2) 0.046(3) -0.006(2) 0.005(2) 0.007(2) C18 0.036(3) 0.038(3) 0.030(3) 0.002(2) -0.001(2) 0.013(2) C19 0.037(3) 0.035(3) 0.033(3) -0.003(2) 0.001(2) 0.011(2) C20 0.026(2) 0.031(2) 0.032(3) -0.0008(19) 0.0018(18) 0.0104(19) C21 0.030(2) 0.028(2) 0.034(3) -0.006(2) 0.001(2) 0.011(2) C22 0.038(2) 0.029(2) 0.027(3) -0.0005(19) -0.005(2) -0.003(2) C23 0.049(3) 0.027(2) 0.039(3) -0.006(2) -0.019(2) -0.003(2) C24 0.068(3) 0.025(2) 0.050(3) 0.002(2) -0.013(3) -0.009(2) C25 0.070(3) 0.044(3) 0.038(3) 0.007(2) -0.005(3) -0.022(3) C26 0.054(3) 0.042(3) 0.034(3) -0.004(2) 0.002(2) -0.011(2) C27 0.042(2) 0.033(2) 0.023(2) -0.001(2) -0.0007(18) -0.008(2) C28 0.048(3) 0.031(3) 0.071(4) -0.014(3) -0.015(3) 0.009(2) C29 0.045(3) 0.040(3) 0.059(4) -0.010(3) -0.005(2) 0.002(2) C30 0.113(6) 0.086(5) 0.123(7) -0.038(5) -0.069(5) 0.058(4) C31 0.043(2) 0.033(2) 0.032(3) -0.003(2) 0.006(2) -0.001(2) C32 0.108(5) 0.033(3) 0.036(3) -0.008(2) -0.007(3) -0.001(3) C33 0.064(3) 0.040(3) 0.078(4) 0.006(3) -0.012(3) -0.001(3) C34 0.030(2) 0.024(2) 0.025(2) -0.0045(18) -0.0009(18) 0.0010(18) C35 0.031(2) 0.033(2) 0.029(3) -0.0018(19) -0.0051(18) 0.0047(19) C36 0.025(2) 0.036(3) 0.036(3) -0.004(2) -0.0041(19) 0.0004(19) C37 0.024(2) 0.027(2) 0.029(2) -0.0055(19) -0.0003(18) 0.0036(17) C38 0.022(2) 0.025(2) 0.029(2) -0.0061(18) 0.0014(17) 0.0070(18) C39 0.025(2) 0.025(2) 0.026(2) -0.0025(18) 0.0005(18) 0.0066(17) C40 0.026(2) 0.034(3) 0.026(2) 0.0028(19) 0.0010(18) 0.0070(19) C41 0.024(2) 0.037(3) 0.025(2) -0.004(2) -0.0019(18) 0.0045(19) C42 0.025(2) 0.027(2) 0.028(3) -0.0047(18) 0.0007(18) 0.0019(18) C43 0.025(2) 0.024(2) 0.022(2) -0.0044(17) -0.0001(17) 0.0039(17) C44 0.029(2) 0.031(2) 0.024(2) -0.0010(19) -0.0011(18) -0.0011(19) C45 0.035(2) 0.026(2) 0.026(3) -0.0016(19) -0.002(2) 0.0027(18) C46 0.025(2) 0.030(3) 0.033(3) -0.003(2) 0.0046(19) 0.005(2) C47 0.026(2) 0.041(3) 0.041(3) -0.003(2) -0.002(2) -0.002(2) C48 0.029(2) 0.045(3) 0.045(4) 0.004(2) -0.002(2) -0.004(2) C49A 0.024(6) 0.030(6) 0.057(10) -0.014(6) -0.001(6) -0.011(4) C50 0.028(2) 0.031(3) 0.040(3) 0.000(2) 0.008(2) 0.009(2) C51 0.036(3) 0.040(3) 0.029(3) 0.006(2) 0.005(2) 0.013(2) C52 0.024(2) 0.037(3) 0.035(3) 0.004(2) -0.0008(19) 0.011(2) C53 0.026(2) 0.026(2) 0.029(3) -0.0008(18) 0.0052(18) 0.0087(19) C54 0.024(2) 0.026(2) 0.034(3) -0.003(2) 0.0058(19) 0.0066(18) C55 0.038(2) 0.030(2) 0.024(3) -0.0022(19) -0.002(2) -0.009(2) C56 0.046(3) 0.030(2) 0.036(3) -0.004(2) -0.001(2) -0.005(2) C57 0.077(3) 0.024(3) 0.041(3) 0.001(2) -0.001(3) -0.011(2) C58 0.079(4) 0.048(3) 0.038(3) 0.001(3) 0.011(3) -0.026(3) C59 0.058(3) 0.049(3) 0.037(3) -0.004(2) 0.016(3) -0.008(3) C60 0.053(3) 0.036(3) 0.028(3) -0.002(2) 0.006(2) -0.003(2) C61 0.051(3) 0.029(2) 0.045(3) -0.005(2) -0.008(2) 0.003(2) C62 0.064(3) 0.039(3) 0.043(3) -0.008(2) 0.003(3) 0.000(3) C63 0.106(5) 0.095(5) 0.050(4) -0.022(3) -0.026(3) 0.055(4) C64 0.052(3) 0.033(3) 0.042(3) -0.002(2) 0.015(2) 0.003(2) C65 0.069(4) 0.045(3) 0.073(4) -0.007(3) -0.008(3) -0.006(3) C66 0.099(5) 0.074(5) 0.149(8) -0.022(5) -0.066(5) 0.025(4) N1 0.030(2) 0.0248(18) 0.027(2) -0.0061(15) -0.0028(15) 0.0005(15) N2A 0.040(7) 0.030(8) 0.039(7) 0.008(5) 0.007(3) 0.013(5) N3 0.034(2) 0.027(2) 0.029(2) -0.0010(17) 0.0024(16) -0.0051(16) N4A 0.019(6) 0.031(6) 0.041(8) 0.006(4) 0.014(7) 0.007(4) O1 0.049(2) 0.0408(19) 0.034(2) 0.0056(15) -0.0130(15) -0.0094(16) O2 0.0303(17) 0.059(2) 0.033(2) -0.0018(16) -0.0058(14) -0.0090(15) O3A 0.040(3) 0.052(4) 0.031(3) 0.003(3) -0.002(2) -0.010(3) O4 0.0494(19) 0.046(2) 0.0265(19) 0.0074(15) -0.0077(14) -0.0096(16) O5 0.0340(19) 0.057(2) 0.035(2) 0.0013(17) -0.0049(15) -0.0139(16) O6A 0.035(3) 0.052(4) 0.050(4) 0.016(3) 0.000(3) -0.006(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C2 C1 C10 120.0(4) . . C2 C1 C11 120.2(4) . . C10 C1 C11 119.8(4) . . C1 C2 C3 120.7(4) . . C1 C2 H2 119.6 . . C3 C2 H2 119.6 . . C2 C3 C4 122.1(4) . . C2 C3 H3 119.0 . . C4 C3 H3 119.0 . . C3 C4 C5 118.8(4) . . C3 C4 C13 123.2(4) . . C5 C4 C13 117.9(4) . . C6 C5 C10 119.0(4) . . C6 C5 C4 122.5(4) . . C10 C5 C4 118.4(4) . . C7 C6 C5 118.9(4) . . C7 C6 C20 122.5(4) . . C5 C6 C20 118.6(4) . . C6 C7 C8 121.9(4) . . C6 C7 H7 119.1 . . C8 C7 H7 119.1 . . C9 C8 C7 121.0(4) . . C9 C8 H8 119.5 . . C7 C8 H8 119.5 . . C8 C9 C10 119.4(4) . . C8 C9 C12 120.0(4) . . C10 C9 C12 120.5(4) . . C1 C10 C9 120.3(4) . . C1 C10 C5 119.9(4) . . C9 C10 C5 119.8(4) . . O1 C11 N1 120.1(4) . . O1 C11 C1 122.7(4) . . N1 C11 C1 117.2(4) . . O2 C12 N1 119.1(4) . . O2 C12 C9 123.3(4) . . N1 C12 C9 117.6(4) . . C14 C13 C21 118.1(4) . . C14 C13 C4 122.7(4) . . C21 C13 C4 119.2(4) . . C13 C14 C15 121.2(5) . . C13 C14 H14 119.4 . . C15 C14 H14 119.4 . . C16A C15 C14 118.5(11) . . N2B C15 C14 123.5(9) . . C16A C15 H15 120.7 . . C14 C15 H15 120.7 . . N2B C15 H15A 118.2 . . C14 C15 H15A 118.2 . . C15 C16A C17 125.3(15) . . C15 C16A O3A 121(2) . . C17 C16A O3A 114(2) . . N2A C17 C16A 120.5(14) . . N2A C17 C21 121.8(9) . . C16A C17 C21 117.7(11) . . C21 C17 C16B 123.1(13) . . C21 C17 N2B 122.5(8) . . C16B C17 N2B 114.3(14) . . C16B C18 C19 124.6(15) . . N2A C18 C19 121.2(8) . . N2A C18 H18 119.4 . . C19 C18 H18 119.4 . . C16B C18 H18A 117.7 . . C19 C18 H18A 117.7 . . C20 C19 C18 121.0(4) . . C20 C19 H19 119.5 . . C18 C19 H19 119.5 . . C19 C20 C21 117.8(4) . . C19 C20 C6 123.2(4) . . C21 C20 C6 118.9(4) . . C17 C21 C13 119.1(4) . . C17 C21 C20 118.1(4) . . C13 C21 C20 122.8(4) . . C27 C22 C23 123.4(4) . . C27 C22 N1 118.3(4) . . C23 C22 N1 118.2(4) . . C22 C23 C24 116.4(4) . . C22 C23 C28 122.9(4) . . C24 C23 C28 120.7(4) . . C25 C24 C23 122.4(5) . . C25 C24 H24 118.8 . . C23 C24 H24 118.8 . . C24 C25 C26 120.6(5) . . C24 C25 H25 119.7 . . C26 C25 H25 119.7 . . C27 C26 C25 119.3(5) . . C27 C26 H26 120.4 . . C25 C26 H26 120.4 . . C22 C27 C26 117.9(4) . . C22 C27 C31 122.7(4) . . C26 C27 C31 119.3(4) . . C23 C28 C29 110.9(4) . . C23 C28 C30 112.1(6) . . C29 C28 C30 110.2(5) . . C23 C28 H28 107.8 . . C29 C28 H28 107.8 . . C30 C28 H28 107.8 . . C28 C29 H29 109.5 . . C28 C29 H29A 109.5 . . H29 C29 H29A 109.5 . . C28 C29 H29B 109.5 . . H29 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . C28 C30 H30 109.5 . . C28 C30 H30A 109.5 . . H30 C30 H30A 109.5 . . C28 C30 H30B 109.5 . . H30 C30 H30B 109.5 . . H30A C30 H30B 109.5 . . C27 C31 C33 111.7(4) . . C27 C31 C32 110.3(4) . . C33 C31 C32 113.5(5) . . C27 C31 H31 107.0 . . C33 C31 H31 107.0 . . C32 C31 H31 107.0 . . C31 C32 H32 109.5 . . C31 C32 H32A 109.5 . . H32 C32 H32A 109.5 . . C31 C32 H32B 109.5 . . H32 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C31 C33 H33 109.5 . . C31 C33 H33A 109.5 . . H33 C33 H33A 109.5 . . C31 C33 H33B 109.5 . . H33 C33 H33B 109.5 . . H33A C33 H33B 109.5 . . C35 C34 C43 119.5(4) . . C35 C34 C45 119.3(4) . . C43 C34 C45 121.3(4) . . C34 C35 C36 120.4(4) . . C34 C35 H35 119.8 . . C36 C35 H35 119.8 . . C37 C36 C35 121.9(4) . . C37 C36 H36 119.1 . . C35 C36 H36 119.1 . . C36 C37 C38 118.8(4) . . C36 C37 C46 122.6(4) . . C38 C37 C46 118.6(4) . . C39 C38 C43 119.4(4) . . C39 C38 C37 121.8(4) . . C43 C38 C37 118.7(4) . . C40 C39 C38 119.1(4) . . C40 C39 C53 121.6(4) . . C38 C39 C53 119.3(4) . . C41 C40 C39 121.4(4) . . C41 C40 H40 119.3 . . C39 C40 H40 119.3 . . C42 C41 C40 120.3(4) . . C42 C41 H41 119.8 . . C40 C41 H41 119.8 . . C41 C42 C43 120.5(4) . . C41 C42 C44 119.1(4) . . C43 C42 C44 120.4(4) . . C34 C43 C42 120.0(4) . . C34 C43 C38 120.6(4) . . C42 C43 C38 119.3(4) . . O5 C44 N3 120.0(4) . . O5 C44 C42 123.4(4) . . N3 C44 C42 116.6(4) . . O4 C45 N3 119.7(4) . . O4 C45 C34 124.0(4) . . N3 C45 C34 116.3(4) . . C47 C46 C54 117.2(4) . . C47 C46 C37 123.6(4) . . C54 C46 C37 119.2(4) . . C46 C47 C48 121.7(5) . . C46 C47 H47 119.1 . . C48 C47 H47 119.1 . . C49A C48 C47 126.4(8) . . C47 C48 N4B 117.5(9) . . C49A C48 H48 116.8 . . C47 C48 H48 116.8 . . C47 C48 H48A 121.3 . . N4B C48 H48A 121.3 . . C48 C49A O6A 136.5(14) . . C48 C49A C50 116.4(13) . . O6A C49A C50 106.7(13) . . N4B C50 C54 122.3(11) . . N4A C50 C54 125.0(7) . . N4B C50 C49B 120.3(14) . . C54 C50 C49B 117.5(9) . . N4A C50 C49A 116.3(11) . . C54 C50 C49A 118.7(8) . . C49B C51 C52 123(2) . . N4A C51 C52 122.9(10) . . N4A C51 H51 118.6 . . C52 C51 H51 118.6 . . C49B C51 H51A 118.6 . . C52 C51 H51A 118.6 . . C53 C52 C51 120.8(4) . . C53 C52 H52 119.6 . . C51 C52 H52 119.6 . . C52 C53 C54 118.0(4) . . C52 C53 C39 123.7(4) . . C54 C53 C39 118.3(4) . . C46 C54 C50 119.6(4) . . C46 C54 C53 122.6(4) . . C50 C54 C53 117.8(4) . . C56 C55 C60 123.1(4) . . C56 C55 N3 118.0(4) . . C60 C55 N3 118.9(4) . . C57 C56 C55 116.8(4) . . C57 C56 C61 120.7(4) . . C55 C56 C61 122.5(4) . . C58 C57 C56 121.1(4) . . C58 C57 H57 119.5 . . C56 C57 H57 119.5 . . C59 C58 C57 120.5(5) . . C59 C58 H58 119.7 . . C57 C58 H58 119.7 . . C58 C59 C60 122.1(5) . . C58 C59 H59 118.9 . . C60 C59 H59 118.9 . . C59 C60 C55 116.4(4) . . C59 C60 C64 121.5(4) . . C55 C60 C64 122.1(4) . . C56 C61 C62 110.5(4) . . C56 C61 C63 112.5(4) . . C62 C61 C63 110.8(4) . . C56 C61 H61 107.6 . . C62 C61 H61 107.6 . . C63 C61 H61 107.6 . . C61 C62 H62 109.5 . . C61 C62 H62A 109.5 . . H62 C62 H62A 109.5 . . C61 C62 H62B 109.5 . . H62 C62 H62B 109.5 . . H62A C62 H62B 109.5 . . C61 C63 H63 109.5 . . C61 C63 H63A 109.5 . . H63 C63 H63A 109.5 . . C61 C63 H63B 109.5 . . H63 C63 H63B 109.5 . . H63A C63 H63B 109.5 . . C65 C64 C60 109.3(4) . . C65 C64 C66 110.0(5) . . C60 C64 C66 113.0(5) . . C65 C64 H64 108.1 . . C60 C64 H64 108.1 . . C66 C64 H64 108.1 . . C64 C65 H65 109.5 . . C64 C65 H65A 109.5 . . H65 C65 H65A 109.5 . . C64 C65 H65B 109.5 . . H65 C65 H65B 109.5 . . H65A C65 H65B 109.5 . . C64 C66 H66 109.5 . . C64 C66 H66A 109.5 . . H66 C66 H66A 109.5 . . C64 C66 H66B 109.5 . . H66 C66 H66B 109.5 . . H66A C66 H66B 109.5 . . O3B C16B C18 130(4) . . O3B C16B C17 115(4) . . C18 C16B C17 115.0(11) . . C51 C49B O6B 133(5) . . C51 C49B C50 123(2) . . O6B C49B C50 104(3) . . C11 N1 C12 124.4(4) . . C11 N1 C22 118.3(4) . . C12 N1 C22 117.3(3) . . C18 N2A C17 120.0(9) . . C44 N3 C45 125.0(4) . . C44 N3 C55 117.5(3) . . C45 N3 C55 117.2(4) . . C50 N4A C51 115.5(8) . . C15 N2B C17 115.6(10) . . C50 N4B C48 121.6(17) . . C16A O3A H3A 109.5 . . C49A O6A H6A 109.5 . . C16B O3B H3B 109.5 . . C49B O6B H6B 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.376(6) . C1 C10 1.417(6) . C1 C11 1.482(6) . C2 C3 1.386(6) . C2 H2 0.9500 . C3 C4 1.388(6) . C3 H3 0.9500 . C4 C5 1.439(6) . C4 C13 1.474(6) . C5 C6 1.433(6) . C5 C10 1.433(6) . C6 C7 1.376(6) . C6 C20 1.466(6) . C7 C8 1.397(6) . C7 H7 0.9500 . C8 C9 1.378(6) . C8 H8 0.9500 . C9 C10 1.418(6) . C9 C12 1.458(6) . C11 O1 1.227(5) . C11 N1 1.398(5) . C12 O2 1.221(5) . C12 N1 1.402(6) . C13 C14 1.387(6) . C13 C21 1.419(6) . C14 C15 1.402(7) . C14 H14 0.9500 . C15 C16A 1.30(3) . C15 N2B 1.37(2) . C15 H15 0.9500 . C15 H15A 0.9500 . C16A C17 1.37(3) . C16A O3A 1.46(2) . C17 N2A 1.35(3) . C17 C21 1.416(6) . C17 C16B 1.43(5) . C17 N2B 1.43(2) . C18 C16B 1.32(5) . C18 N2A 1.33(3) . C18 C19 1.404(6) . C18 H18 0.9500 . C18 H18A 0.9500 . C19 C20 1.379(6) . C19 H19 0.9500 . C20 C21 1.422(6) . C22 C27 1.393(6) . C22 C23 1.394(6) . C22 N1 1.453(6) . C23 C24 1.396(7) . C23 C28 1.505(7) . C24 C25 1.350(8) . C24 H24 0.9500 . C25 C26 1.413(7) . C25 H25 0.9500 . C26 C27 1.396(6) . C26 H26 0.9500 . C27 C31 1.509(6) . C28 C29 1.522(7) . C28 C30 1.526(8) . C28 H28 1.0000 . C29 H29 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C30 H30 0.9800 . C30 H30A 0.9800 . C30 H30B 0.9800 . C31 C33 1.521(7) . C31 C32 1.524(7) . C31 H31 1.0000 . C32 H32 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C33 H33 0.9800 . C33 H33A 0.9800 . C33 H33B 0.9800 . C34 C35 1.388(6) . C34 C43 1.409(6) . C34 C45 1.470(6) . C35 C36 1.393(6) . C35 H35 0.9500 . C36 C37 1.387(6) . C36 H36 0.9500 . C37 C38 1.435(6) . C37 C46 1.466(6) . C38 C39 1.420(6) . C38 C43 1.421(6) . C39 C40 1.396(6) . C39 C53 1.475(6) . C40 C41 1.392(6) . C40 H40 0.9500 . C41 C42 1.376(6) . C41 H41 0.9500 . C42 C43 1.417(6) . C42 C44 1.484(6) . C44 O5 1.217(5) . C44 N3 1.399(6) . C45 O4 1.210(5) . C45 N3 1.411(5) . C46 C47 1.387(6) . C46 C54 1.415(6) . C47 C48 1.395(6) . C47 H47 0.9500 . C48 C49A 1.23(2) . C48 N4B 1.44(2) . C48 H48 0.9500 . C48 H48A 0.9500 . C49A O6A 1.39(2) . C49A C50 1.534(17) . C50 N4B 1.25(2) . C50 N4A 1.36(3) . C50 C54 1.420(6) . C50 C49B 1.46(6) . C51 C49B 1.17(5) . C51 N4A 1.39(2) . C51 C52 1.405(6) . C51 H51 0.9500 . C51 H51A 0.9500 . C52 C53 1.386(6) . C52 H52 0.9500 . C53 C54 1.424(6) . C55 C56 1.398(6) . C55 C60 1.404(6) . C55 N3 1.458(5) . C56 C57 1.398(7) . C56 C61 1.508(6) . C57 C58 1.375(7) . C57 H57 0.9500 . C58 C59 1.359(8) . C58 H58 0.9500 . C59 C60 1.391(7) . C59 H59 0.9500 . C60 C64 1.520(6) . C61 C62 1.520(7) . C61 C63 1.521(7) . C61 H61 1.0000 . C62 H62 0.9800 . C62 H62A 0.9800 . C62 H62B 0.9800 . C63 H63 0.9800 . C63 H63A 0.9800 . C63 H63B 0.9800 . C64 C65 1.498(8) . C64 C66 1.530(8) . C64 H64 1.0000 . C65 H65 0.9800 . C65 H65A 0.9800 . C65 H65B 0.9800 . C66 H66 0.9800 . C66 H66A 0.9800 . C66 H66B 0.9800 . C16B O3B 1.29(2) . C49B O6B 1.457(14) . O3A H3A 0.8400 . O6A H6A 0.8400 . O3B H3B 0.8400 . O6B H6B 0.8400 . 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 C10 C1 C2 C3 0.2(6) . . . . C11 C1 C2 C3 -178.4(4) . . . . C1 C2 C3 C4 1.3(7) . . . . C2 C3 C4 C5 -2.7(6) . . . . C2 C3 C4 C13 178.9(4) . . . . C3 C4 C5 C6 -178.9(4) . . . . C13 C4 C5 C6 -0.3(6) . . . . C3 C4 C5 C10 2.5(6) . . . . C13 C4 C5 C10 -179.0(4) . . . . C10 C5 C6 C7 -1.3(6) . . . . C4 C5 C6 C7 -180.0(4) . . . . C10 C5 C6 C20 179.9(4) . . . . C4 C5 C6 C20 1.3(6) . . . . C5 C6 C7 C8 0.6(6) . . . . C20 C6 C7 C8 179.3(4) . . . . C6 C7 C8 C9 -0.1(6) . . . . C7 C8 C9 C10 0.3(6) . . . . C7 C8 C9 C12 178.4(4) . . . . C2 C1 C10 C9 178.4(4) . . . . C11 C1 C10 C9 -3.1(6) . . . . C2 C1 C10 C5 -0.3(6) . . . . C11 C1 C10 C5 178.3(4) . . . . C8 C9 C10 C1 -179.7(4) . . . . C12 C9 C10 C1 2.1(6) . . . . C8 C9 C10 C5 -1.1(6) . . . . C12 C9 C10 C5 -179.2(4) . . . . C6 C5 C10 C1 -179.8(4) . . . . C4 C5 C10 C1 -1.0(5) . . . . C6 C5 C10 C9 1.6(6) . . . . C4 C5 C10 C9 -179.7(3) . . . . C2 C1 C11 O1 -0.4(6) . . . . C10 C1 C11 O1 -178.9(4) . . . . C2 C1 C11 N1 179.4(4) . . . . C10 C1 C11 N1 0.8(6) . . . . C8 C9 C12 O2 1.7(7) . . . . C10 C9 C12 O2 179.8(4) . . . . C8 C9 C12 N1 -177.1(4) . . . . C10 C9 C12 N1 1.0(6) . . . . C3 C4 C13 C14 -2.5(7) . . . . C5 C4 C13 C14 179.0(4) . . . . C3 C4 C13 C21 178.0(4) . . . . C5 C4 C13 C21 -0.5(6) . . . . C21 C13 C14 C15 -1.0(7) . . . . C4 C13 C14 C15 179.5(4) . . . . C13 C14 C15 C16A 1.6(19) . . . . C13 C14 C15 N2B -1.1(16) . . . . C14 C15 C16A C17 -3(4) . . . . C14 C15 C16A O3A -176.9(17) . . . . C15 C16A C17 N2A -176(2) . . . . O3A C16A C17 N2A -2(3) . . . . C15 C16A C17 C21 4(4) . . . . O3A C16A C17 C21 178.1(14) . . . . C16B C18 C19 C20 -5(3) . . . . N2A C18 C19 C20 1.4(16) . . . . C18 C19 C20 C21 1.1(6) . . . . C18 C19 C20 C6 -179.5(4) . . . . C7 C6 C20 C19 0.4(6) . . . . C5 C6 C20 C19 179.2(4) . . . . C7 C6 C20 C21 179.9(4) . . . . C5 C6 C20 C21 -1.4(6) . . . . N2A C17 C21 C13 177.3(15) . . . . C16A C17 C21 C13 -3.1(17) . . . . C16B C17 C21 C13 -177(3) . . . . N2B C17 C21 C13 -0.7(15) . . . . N2A C17 C21 C20 -1.9(16) . . . . C16A C17 C21 C20 177.8(17) . . . . C16B C17 C21 C20 4(3) . . . . N2B C17 C21 C20 -179.8(14) . . . . C14 C13 C21 C17 1.8(6) . . . . C4 C13 C21 C17 -178.7(4) . . . . C14 C13 C21 C20 -179.1(4) . . . . C4 C13 C21 C20 0.4(6) . . . . C19 C20 C21 C17 -0.8(6) . . . . C6 C20 C21 C17 179.7(4) . . . . C19 C20 C21 C13 -179.9(4) . . . . C6 C20 C21 C13 0.6(6) . . . . C27 C22 C23 C24 0.3(7) . . . . N1 C22 C23 C24 -178.1(4) . . . . C27 C22 C23 C28 -179.2(4) . . . . N1 C22 C23 C28 2.5(7) . . . . C22 C23 C24 C25 0.2(7) . . . . C28 C23 C24 C25 179.7(5) . . . . C23 C24 C25 C26 0.3(8) . . . . C24 C25 C26 C27 -1.3(8) . . . . C23 C22 C27 C26 -1.3(7) . . . . N1 C22 C27 C26 177.0(4) . . . . C23 C22 C27 C31 177.0(4) . . . . N1 C22 C27 C31 -4.7(6) . . . . C25 C26 C27 C22 1.8(7) . . . . C25 C26 C27 C31 -176.6(4) . . . . C22 C23 C28 C29 -114.6(5) . . . . C24 C23 C28 C29 66.0(6) . . . . C22 C23 C28 C30 121.7(6) . . . . C24 C23 C28 C30 -57.7(7) . . . . C22 C27 C31 C33 119.1(5) . . . . C26 C27 C31 C33 -62.6(6) . . . . C22 C27 C31 C32 -113.7(5) . . . . C26 C27 C31 C32 64.6(6) . . . . C43 C34 C35 C36 -2.3(6) . . . . C45 C34 C35 C36 177.7(4) . . . . C34 C35 C36 C37 0.6(6) . . . . C35 C36 C37 C38 1.7(6) . . . . C35 C36 C37 C46 -178.3(4) . . . . C36 C37 C38 C39 177.4(4) . . . . C46 C37 C38 C39 -2.5(6) . . . . C36 C37 C38 C43 -2.2(6) . . . . C46 C37 C38 C43 177.8(4) . . . . C43 C38 C39 C40 0.0(5) . . . . C37 C38 C39 C40 -179.7(4) . . . . C43 C38 C39 C53 -179.6(4) . . . . C37 C38 C39 C53 0.7(6) . . . . C38 C39 C40 C41 1.0(6) . . . . C53 C39 C40 C41 -179.4(4) . . . . C39 C40 C41 C42 -1.9(6) . . . . C40 C41 C42 C43 1.8(6) . . . . C40 C41 C42 C44 -177.6(4) . . . . C35 C34 C43 C42 -177.4(4) . . . . C45 C34 C43 C42 2.6(6) . . . . C35 C34 C43 C38 1.7(6) . . . . C45 C34 C43 C38 -178.3(4) . . . . C41 C42 C43 C34 178.2(4) . . . . C44 C42 C43 C34 -2.3(6) . . . . C41 C42 C43 C38 -0.9(6) . . . . C44 C42 C43 C38 178.6(3) . . . . C39 C38 C43 C34 -179.1(4) . . . . C37 C38 C43 C34 0.6(5) . . . . C39 C38 C43 C42 0.0(5) . . . . C37 C38 C43 C42 179.6(4) . . . . C41 C42 C44 O5 -1.9(6) . . . . C43 C42 C44 O5 178.7(4) . . . . C41 C42 C44 N3 177.5(4) . . . . C43 C42 C44 N3 -2.0(6) . . . . C35 C34 C45 O4 0.0(6) . . . . C43 C34 C45 O4 -180.0(4) . . . . C35 C34 C45 N3 -178.6(4) . . . . C43 C34 C45 N3 1.4(6) . . . . C36 C37 C46 C47 3.3(7) . . . . C38 C37 C46 C47 -176.7(4) . . . . C36 C37 C46 C54 -176.8(4) . . . . C38 C37 C46 C54 3.1(6) . . . . C54 C46 C47 C48 1.1(6) . . . . C37 C46 C47 C48 -179.0(4) . . . . C46 C47 C48 C49A -2.0(13) . . . . C46 C47 C48 N4B 2.4(12) . . . . C47 C48 C49A O6A 175.2(14) . . . . C47 C48 C49A C50 3.2(19) . . . . C48 C49A C50 N4A 177.9(15) . . . . O6A C49A C50 N4A 3.5(18) . . . . C48 C49A C50 C54 -3.8(17) . . . . O6A C49A C50 C54 -178.1(7) . . . . C49B C51 C52 C53 2(3) . . . . N4A C51 C52 C53 -0.3(13) . . . . C51 C52 C53 C54 -0.4(6) . . . . C51 C52 C53 C39 179.4(4) . . . . C40 C39 C53 C52 1.1(6) . . . . C38 C39 C53 C52 -179.3(4) . . . . C40 C39 C53 C54 -179.1(4) . . . . C38 C39 C53 C54 0.5(5) . . . . C47 C46 C54 C50 -1.9(6) . . . . C37 C46 C54 C50 178.2(4) . . . . C47 C46 C54 C53 177.9(4) . . . . C37 C46 C54 C53 -2.0(6) . . . . N4B C50 C54 C46 -1.1(14) . . . . N4A C50 C54 C46 -178.6(13) . . . . C49B C50 C54 C46 179(3) . . . . C49A C50 C54 C46 3.2(9) . . . . N4B C50 C54 C53 179.0(13) . . . . N4A C50 C54 C53 1.6(14) . . . . C49B C50 C54 C53 0(3) . . . . C49A C50 C54 C53 -176.6(8) . . . . C52 C53 C54 C46 180.0(4) . . . . C39 C53 C54 C46 0.1(6) . . . . C52 C53 C54 C50 -0.2(6) . . . . C39 C53 C54 C50 180.0(4) . . . . C60 C55 C56 C57 1.0(7) . . . . N3 C55 C56 C57 -179.6(4) . . . . C60 C55 C56 C61 -178.4(4) . . . . N3 C55 C56 C61 1.0(6) . . . . C55 C56 C57 C58 -0.1(7) . . . . C61 C56 C57 C58 179.3(5) . . . . C56 C57 C58 C59 -0.7(8) . . . . C57 C58 C59 C60 0.5(9) . . . . C58 C59 C60 C55 0.4(8) . . . . C58 C59 C60 C64 177.4(5) . . . . C56 C55 C60 C59 -1.2(7) . . . . N3 C55 C60 C59 179.4(4) . . . . C56 C55 C60 C64 -178.2(4) . . . . N3 C55 C60 C64 2.4(7) . . . . C57 C56 C61 C62 -62.5(6) . . . . C55 C56 C61 C62 116.9(5) . . . . C57 C56 C61 C63 62.0(6) . . . . C55 C56 C61 C63 -118.6(6) . . . . C59 C60 C64 C65 -75.5(6) . . . . C55 C60 C64 C65 101.4(5) . . . . C59 C60 C64 C66 47.4(8) . . . . C55 C60 C64 C66 -135.8(6) . . . . C19 C18 C16B O3B 179(4) . . . . C19 C18 C16B C17 7(6) . . . . C21 C17 C16B O3B -180(2) . . . . N2B C17 C16B O3B 4(5) . . . . C21 C17 C16B C18 -7(5) . . . . N2B C17 C16B C18 176(3) . . . . C52 C51 C49B O6B 180(4) . . . . C52 C51 C49B C50 -3(6) . . . . N4B C50 C49B C51 -178(4) . . . . C54 C50 C49B C51 2(6) . . . . N4B C50 C49B O6B 1(4) . . . . C54 C50 C49B O6B -179.9(18) . . . . O1 C11 N1 C12 -177.7(4) . . . . C1 C11 N1 C12 2.5(6) . . . . O1 C11 N1 C22 3.0(6) . . . . C1 C11 N1 C22 -176.8(4) . . . . O2 C12 N1 C11 177.7(4) . . . . C9 C12 N1 C11 -3.5(6) . . . . O2 C12 N1 C22 -2.9(6) . . . . C9 C12 N1 C22 175.9(4) . . . . C27 C22 N1 C11 93.9(5) . . . . C23 C22 N1 C11 -87.7(5) . . . . C27 C22 N1 C12 -85.5(5) . . . . C23 C22 N1 C12 92.9(5) . . . . C19 C18 N2A C17 -4(3) . . . . C16A C17 N2A C18 -175(2) . . . . C21 C17 N2A C18 4(3) . . . . O5 C44 N3 C45 -174.2(4) . . . . C42 C44 N3 C45 6.4(6) . . . . O5 C44 N3 C55 -0.6(6) . . . . C42 C44 N3 C55 180.0(3) . . . . O4 C45 N3 C44 175.1(4) . . . . C34 C45 N3 C44 -6.2(6) . . . . O4 C45 N3 C55 1.6(6) . . . . C34 C45 N3 C55 -179.7(3) . . . . C56 C55 N3 C44 -91.0(5) . . . . C60 C55 N3 C44 88.4(5) . . . . C56 C55 N3 C45 83.1(5) . . . . C60 C55 N3 C45 -97.5(5) . . . . C54 C50 N4A C51 -2(2) . . . . C49A C50 N4A C51 176.0(13) . . . . C52 C51 N4A C50 2(2) . . . . C14 C15 N2B C17 2(3) . . . . C21 C17 N2B C15 -1(3) . . . . C16B C17 N2B C15 175(3) . . . . C54 C50 N4B C48 5(2) . . . . C49B C50 N4B C48 -176(3) . . . . C47 C48 N4B C50 -6(2) . . . .