#------------------------------------------------------------------------------ #$Date: 2020-04-30 01:10:05 +0300 (Thu, 30 Apr 2020) $ #$Revision: 251295 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126460.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_7126460 loop_ _publ_author_name 'Xiao, Lin' 'Chen, Weixing' 'Shen, Lingyi' 'Liu, Li' 'Xue, Yujie' 'Zhao, Yanxia' 'Yang, Xiao-Juan' _publ_section_title ; Reduction of carbodiimides by a dialumane through insertion and cycloaddition ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC02048F _journal_year 2020 _chemical_formula_sum 'C70 H108 Al2 N8' _chemical_formula_weight 1115.60 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-03-16 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 71.614(6) _cell_angle_beta 88.934(6) _cell_angle_gamma 76.753(6) _cell_formula_units_Z 2 _cell_length_a 11.946(2) _cell_length_b 14.183(3) _cell_length_c 21.699(4) _cell_measurement_reflns_used 9920 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.92 _cell_measurement_theta_min 2.56 _cell_volume 3390.2(11) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 'fine-focus sealed tube' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0544 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 39706 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.973 _diffrn_reflns_theta_min 2.446 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 1220 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max 0.7453 _exptl_transmission_factor_min 0.7000 _refine_diff_density_max 0.417 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 749 _refine_ls_number_reflns 13216 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0498 _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^)+(0.1000P)^2^+0.6679P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1443 _refine_ls_wR_factor_ref 0.1623 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10616 _reflns_number_total 13216 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02048f2.cif _cod_data_source_block 3 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 3390.1(11) _cod_database_code 7126460 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.978 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in P-1 CELL 0.71073 11.9458 14.1831 21.6987 71.614 88.934 76.753 ZERR 2.000 0.0022 0.0026 0.0042 0.006 0.006 0.006 LATT 1 SFAC C H Al N UNIT 140 216 4 16 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.25 0.25 0.20 TEMP -123.120 WGHT 0.100000 0.667930 FVAR 0.59833 AL1 3 0.668072 0.906150 0.776231 11.00000 0.02009 0.01909 = 0.02155 -0.00797 0.00219 -0.00653 AL2 3 0.828614 0.653880 0.702613 11.00000 0.02106 0.01969 = 0.02246 -0.00831 -0.00187 -0.00437 C1 1 0.608082 1.081027 0.801304 11.00000 0.02459 0.02213 = 0.03420 -0.01301 0.00359 -0.00653 C2 1 0.520958 1.035348 0.821357 11.00000 0.02394 0.02166 = 0.02552 -0.01007 0.00243 -0.00579 C3 1 0.602147 1.192375 0.790777 11.00000 0.03443 0.02667 = 0.06322 -0.01996 0.01248 -0.01345 AFIX 137 H3A 2 0.575596 1.232396 0.745640 11.00000 -1.50000 H3B 2 0.678783 1.200820 0.799605 11.00000 -1.50000 H3C 2 0.548204 1.216288 0.820244 11.00000 -1.50000 AFIX 0 C4 1 0.411073 1.085044 0.845366 11.00000 0.02971 0.03185 = 0.04021 -0.01972 0.00790 -0.00931 AFIX 137 H4A 2 0.416175 1.152427 0.846580 11.00000 -1.50000 H4B 2 0.399721 1.042161 0.889181 11.00000 -1.50000 H4C 2 0.345902 1.092843 0.815943 11.00000 -1.50000 AFIX 0 C5 1 0.814505 1.046164 0.783535 11.00000 0.02253 0.01824 = 0.04117 -0.01315 0.00498 -0.00654 C6 1 0.863425 1.041512 0.843850 11.00000 0.02858 0.02843 = 0.04449 -0.01674 0.00188 -0.00799 C7 1 0.968166 1.068347 0.845002 11.00000 0.02933 0.03398 = 0.05980 -0.02440 -0.00258 -0.00701 AFIX 43 H7 2 1.000274 1.067194 0.885035 11.00000 -1.20000 AFIX 0 C8 1 1.026071 1.096514 0.789254 11.00000 0.02475 0.04367 = 0.07755 -0.03111 0.00487 -0.01396 AFIX 43 H8 2 1.097304 1.114907 0.790956 11.00000 -1.20000 AFIX 0 C9 1 0.980762 1.098027 0.731039 11.00000 0.02847 0.03927 = 0.06045 -0.02374 0.01810 -0.01528 AFIX 43 H9 2 1.022225 1.115945 0.692964 11.00000 -1.20000 AFIX 0 C10 1 0.874566 1.073619 0.726896 11.00000 0.02585 0.02475 = 0.04620 -0.01756 0.01036 -0.01008 C11 1 0.808252 1.006229 0.908321 11.00000 0.04085 0.06391 = 0.03786 -0.01732 0.00027 -0.02178 AFIX 13 H11 2 0.738671 0.982985 0.900070 11.00000 -1.20000 AFIX 0 C12 1 0.888671 0.917174 0.958502 11.00000 0.08002 0.05624 = 0.04077 -0.02015 -0.00930 -0.01758 AFIX 137 H12A 2 0.911574 0.859697 0.941458 11.00000 -1.50000 H12B 2 0.848856 0.896099 0.998663 11.00000 -1.50000 H12C 2 0.957336 0.938418 0.967676 11.00000 -1.50000 AFIX 0 C13 1 0.769518 1.091907 0.938153 11.00000 0.07650 0.08611 = 0.05621 -0.03016 0.01124 0.01262 AFIX 137 H13A 2 0.835237 1.119944 0.943219 11.00000 -1.50000 H13B 2 0.739538 1.064610 0.980820 11.00000 -1.50000 H13C 2 0.708949 1.146090 0.909543 11.00000 -1.50000 AFIX 0 C14 1 0.823958 1.081218 0.661501 11.00000 0.03640 0.03666 = 0.04097 -0.01728 0.01501 -0.01758 AFIX 13 H14 2 0.775311 1.030214 0.669811 11.00000 -1.20000 AFIX 0 C15 1 0.746592 1.183974 0.630533 11.00000 0.07151 0.06477 = 0.08034 -0.03627 -0.03189 0.02196 AFIX 137 H15A 2 0.686864 1.197892 0.660180 11.00000 -1.50000 H15B 2 0.710353 1.185575 0.589951 11.00000 -1.50000 H15C 2 0.791649 1.236076 0.621087 11.00000 -1.50000 AFIX 0 C16 1 0.913972 1.055391 0.615265 11.00000 0.06583 0.06074 = 0.04142 -0.01600 0.01173 0.00219 AFIX 137 H16A 2 0.876851 1.043226 0.579517 11.00000 -1.50000 H16B 2 0.972134 0.993781 0.638787 11.00000 -1.50000 H16C 2 0.950994 1.112507 0.597667 11.00000 -1.50000 AFIX 0 C17 1 0.446730 0.883563 0.844888 11.00000 0.02246 0.01974 = 0.02506 -0.00835 0.00466 -0.00644 C18 1 0.347793 0.895778 0.806538 11.00000 0.02296 0.02290 = 0.02954 -0.00848 0.00382 -0.00726 C19 1 0.253942 0.862187 0.837076 11.00000 0.02416 0.03199 = 0.04359 -0.01014 0.00221 -0.01117 AFIX 43 H19 2 0.185416 0.872560 0.811829 11.00000 -1.20000 AFIX 0 C20 1 0.258844 0.814155 0.903306 11.00000 0.02733 0.03645 = 0.04480 -0.00582 0.01175 -0.01454 AFIX 43 H20 2 0.192748 0.795042 0.923723 11.00000 -1.20000 AFIX 0 C21 1 0.360022 0.793874 0.939919 11.00000 0.03564 0.03282 = 0.02835 -0.00194 0.00878 -0.01008 AFIX 43 H21 2 0.364381 0.756943 0.985067 11.00000 -1.20000 AFIX 0 C22 1 0.455927 0.826797 0.911608 11.00000 0.02741 0.02568 = 0.02646 -0.00752 0.00511 -0.00539 C23 1 0.344591 0.941519 0.732757 11.00000 0.02267 0.04029 = 0.02777 -0.01175 0.00045 -0.00847 AFIX 13 H23 2 0.423910 0.917511 0.719518 11.00000 -1.20000 AFIX 0 C24 1 0.316401 1.058139 0.706801 11.00000 0.04301 0.04421 = 0.02976 0.00194 -0.00194 -0.01261 AFIX 137 H24A 2 0.309262 1.080915 0.659156 11.00000 -1.50000 H24B 2 0.378243 1.082832 0.721103 11.00000 -1.50000 H24C 2 0.243600 1.085532 0.723480 11.00000 -1.50000 AFIX 0 C25 1 0.263713 0.901916 0.698424 11.00000 0.03152 0.05808 = 0.04353 -0.02393 -0.00491 -0.00935 AFIX 137 H25A 2 0.183647 0.930694 0.705524 11.00000 -1.50000 H25B 2 0.280242 0.827167 0.716088 11.00000 -1.50000 H25C 2 0.275473 0.922533 0.651681 11.00000 -1.50000 AFIX 0 C26 1 0.566444 0.802083 0.952650 11.00000 0.02972 0.04944 = 0.02337 -0.00713 0.00137 -0.00689 AFIX 13 H26 2 0.630274 0.808172 0.922232 11.00000 -1.20000 AFIX 0 C27 1 0.594644 0.692549 0.999470 11.00000 0.05297 0.05988 = 0.03659 0.00398 -0.00674 -0.00145 AFIX 137 H27A 2 0.537529 0.685448 1.032614 11.00000 -1.50000 H27B 2 0.671527 0.676932 1.020556 11.00000 -1.50000 H27C 2 0.592954 0.645039 0.975259 11.00000 -1.50000 AFIX 0 C28 1 0.564865 0.878115 0.989404 11.00000 0.05492 0.07874 = 0.04648 -0.02606 -0.00541 -0.02321 AFIX 137 H28A 2 0.554531 0.947124 0.958258 11.00000 -1.50000 H28B 2 0.637905 0.859762 1.015006 11.00000 -1.50000 H28C 2 0.501145 0.876254 1.018533 11.00000 -1.50000 AFIX 0 C29 1 0.856566 0.510623 0.659802 11.00000 0.02039 0.02236 = 0.02592 -0.00987 -0.00055 -0.00457 C30 1 0.840384 0.457368 0.731770 11.00000 0.02264 0.02282 = 0.02896 -0.00793 -0.00142 -0.00591 C31 1 0.849941 0.446442 0.616274 11.00000 0.02463 0.02915 = 0.03479 -0.01713 0.00101 -0.00740 AFIX 137 H31A 2 0.773316 0.432155 0.617470 11.00000 -1.50000 H31B 2 0.908431 0.381907 0.631716 11.00000 -1.50000 H31C 2 0.863798 0.483837 0.571540 11.00000 -1.50000 AFIX 0 C32 1 0.841121 0.349048 0.756519 11.00000 0.05691 0.02508 = 0.03725 -0.00867 0.00091 -0.01364 AFIX 137 H32A 2 0.829248 0.329662 0.803246 11.00000 -1.50000 H32B 2 0.915442 0.308747 0.749144 11.00000 -1.50000 H32C 2 0.779169 0.335867 0.733816 11.00000 -1.50000 AFIX 0 C33 1 0.704962 0.647867 0.580945 11.00000 0.02103 0.02334 = 0.02231 -0.01119 -0.00027 -0.00161 C34 1 0.737286 0.720358 0.526571 11.00000 0.02822 0.02833 = 0.02497 -0.00919 0.00100 -0.00498 C35 1 0.667010 0.759646 0.469575 11.00000 0.04268 0.03973 = 0.02521 -0.00261 -0.00278 -0.00740 AFIX 43 H35 2 0.688534 0.809098 0.433381 11.00000 -1.20000 AFIX 0 C36 1 0.567191 0.729204 0.463876 11.00000 0.03638 0.04811 = 0.02929 -0.01300 -0.00983 0.00228 AFIX 43 H36 2 0.520599 0.757152 0.424418 11.00000 -1.20000 AFIX 0 C37 1 0.536517 0.658221 0.515920 11.00000 0.02341 0.04144 = 0.03615 -0.02156 -0.00506 -0.00200 AFIX 43 H37 2 0.468154 0.636570 0.511996 11.00000 -1.20000 AFIX 0 C38 1 0.602504 0.616335 0.574845 11.00000 0.02190 0.03250 = 0.02801 -0.01677 0.00087 -0.00443 C39 1 0.848153 0.755093 0.527155 11.00000 0.03981 0.03971 = 0.02649 -0.00330 0.00193 -0.01868 AFIX 13 H39 2 0.874360 0.738717 0.573640 11.00000 -1.20000 AFIX 0 C40 1 0.942258 0.696143 0.495676 11.00000 0.03170 0.04955 = 0.06204 -0.00858 0.00745 -0.01286 AFIX 137 H40A 2 0.954336 0.622700 0.518626 11.00000 -1.50000 H40B 2 1.014065 0.717390 0.498221 11.00000 -1.50000 H40C 2 0.918786 0.710494 0.449972 11.00000 -1.50000 AFIX 0 C41 1 0.833681 0.870758 0.494072 11.00000 0.06003 0.04243 = 0.03730 -0.00691 0.01311 -0.02448 AFIX 137 H41A 2 0.818067 0.887730 0.447170 11.00000 -1.50000 H41B 2 0.904532 0.890070 0.501835 11.00000 -1.50000 H41C 2 0.769228 0.908134 0.512142 11.00000 -1.50000 AFIX 0 C42 1 0.558121 0.539707 0.629692 11.00000 0.02561 0.04379 = 0.03853 -0.01346 -0.00122 -0.01452 AFIX 13 H42 2 0.614314 0.515361 0.668180 11.00000 -1.20000 AFIX 0 C43 1 0.440417 0.588072 0.649692 11.00000 0.03815 0.06714 = 0.05119 -0.03137 0.01347 -0.02749 AFIX 137 H43A 2 0.448556 0.641847 0.667451 11.00000 -1.50000 H43B 2 0.411673 0.535525 0.682829 11.00000 -1.50000 H43C 2 0.385920 0.617706 0.611559 11.00000 -1.50000 AFIX 0 C44 1 0.546721 0.446602 0.610500 11.00000 0.03498 0.04258 = 0.07043 -0.01990 -0.00544 -0.01649 AFIX 137 H44A 2 0.486362 0.468098 0.575595 11.00000 -1.50000 H44B 2 0.526380 0.395246 0.648349 11.00000 -1.50000 H44C 2 0.620159 0.417158 0.595332 11.00000 -1.50000 AFIX 0 C45 1 0.813435 0.481852 0.836069 11.00000 0.03993 0.01927 = 0.02280 -0.00344 -0.00104 -0.00965 C46 1 0.911641 0.435082 0.879043 11.00000 0.04430 0.02446 = 0.02972 -0.00329 -0.00562 -0.00796 C47 1 0.894030 0.401221 0.945562 11.00000 0.06030 0.03552 = 0.02748 0.00217 -0.01030 -0.01297 AFIX 43 H47 2 0.958832 0.368479 0.975586 11.00000 -1.20000 AFIX 0 C48 1 0.785625 0.413993 0.968692 11.00000 0.07018 0.04249 = 0.02284 -0.00070 0.00523 -0.02380 AFIX 43 H48 2 0.776097 0.391520 1.014174 11.00000 -1.20000 AFIX 0 C49 1 0.691110 0.459412 0.925730 11.00000 0.05281 0.03852 = 0.02998 -0.00965 0.01037 -0.02072 AFIX 43 H49 2 0.616410 0.467287 0.942100 11.00000 -1.20000 AFIX 0 C50 1 0.701926 0.494407 0.858465 11.00000 0.04164 0.02401 = 0.02742 -0.00606 0.00291 -0.01258 C51 1 1.033550 0.419430 0.856450 11.00000 0.03988 0.03585 = 0.03265 -0.00364 -0.01095 -0.00166 AFIX 13 H51 2 1.030245 0.457967 0.808919 11.00000 -1.20000 AFIX 0 C52 1 1.111753 0.460075 0.891845 11.00000 0.04069 0.05115 = 0.04725 -0.00909 -0.01455 -0.00483 AFIX 137 H52A 2 1.078908 0.532770 0.885158 11.00000 -1.50000 H52B 2 1.188462 0.451433 0.874544 11.00000 -1.50000 H52C 2 1.117908 0.422017 0.938470 11.00000 -1.50000 AFIX 0 C53 1 1.087391 0.306031 0.866036 11.00000 0.06038 0.05093 = 0.07681 -0.02346 -0.00977 0.00522 AFIX 137 H53A 2 1.089818 0.266498 0.912269 11.00000 -1.50000 H53B 2 1.165830 0.298573 0.851014 11.00000 -1.50000 H53C 2 1.040846 0.280737 0.840937 11.00000 -1.50000 AFIX 0 C54 1 0.594234 0.541496 0.813263 11.00000 0.03351 0.03353 = 0.02893 -0.00978 0.00766 -0.01230 AFIX 13 H54 2 0.619080 0.559124 0.767578 11.00000 -1.20000 AFIX 0 C55 1 0.519462 0.464590 0.821351 11.00000 0.06151 0.05438 = 0.06228 -0.01097 -0.00275 -0.03398 AFIX 137 H55A 2 0.562879 0.405093 0.810329 11.00000 -1.50000 H55B 2 0.449811 0.496734 0.792369 11.00000 -1.50000 H55C 2 0.497778 0.442655 0.866540 11.00000 -1.50000 AFIX 0 C56 1 0.525515 0.639935 0.823208 11.00000 0.04609 0.04889 = 0.05170 -0.02020 0.00472 -0.00309 AFIX 137 H56A 2 0.495050 0.624146 0.866592 11.00000 -1.50000 H56B 2 0.461524 0.671871 0.790166 11.00000 -1.50000 H56C 2 0.575831 0.687015 0.819254 11.00000 -1.50000 AFIX 0 C57 1 0.760440 0.775177 0.733743 11.00000 0.01918 0.02046 = 0.02350 -0.00607 0.00122 -0.00815 C58 1 0.982819 0.529743 0.661568 11.00000 0.02233 0.02489 = 0.02670 -0.00963 0.00026 -0.00554 C59 1 0.632960 0.871489 0.636254 11.00000 0.02912 0.02989 = 0.02280 -0.01087 -0.00521 0.00088 AFIX 13 H59 2 0.698856 0.844990 0.612429 11.00000 -1.20000 AFIX 0 C60 1 0.587901 0.984956 0.600624 11.00000 0.06330 0.03635 = 0.03366 -0.00732 -0.01734 0.00248 AFIX 137 H60A 2 0.530877 1.014797 0.626448 11.00000 -1.50000 H60B 2 0.551807 0.994267 0.558261 11.00000 -1.50000 H60C 2 0.651969 1.018950 0.594196 11.00000 -1.50000 AFIX 0 C61 1 0.540944 0.812701 0.636886 11.00000 0.02800 0.05635 = 0.05046 -0.03726 -0.00253 -0.00448 AFIX 137 H61A 2 0.570444 0.740793 0.662705 11.00000 -1.50000 H61B 2 0.520883 0.817483 0.592236 11.00000 -1.50000 H61C 2 0.472249 0.841969 0.656122 11.00000 -1.50000 AFIX 0 C62 1 0.883596 0.715743 0.835161 11.00000 0.02519 0.02424 = 0.02565 -0.00927 -0.00409 -0.00313 AFIX 13 H62 2 0.915576 0.656532 0.819302 11.00000 -1.20000 AFIX 0 C63 1 0.975937 0.775006 0.832232 11.00000 0.02769 0.03265 = 0.04208 -0.01696 -0.00440 -0.00650 AFIX 137 H63A 2 0.998805 0.798632 0.787380 11.00000 -1.50000 H63B 2 1.043094 0.730491 0.860504 11.00000 -1.50000 H63C 2 0.945377 0.834059 0.846925 11.00000 -1.50000 AFIX 0 C64 1 0.849185 0.674811 0.904624 11.00000 0.03984 0.03280 = 0.02556 -0.00811 -0.00513 -0.00526 AFIX 137 H64A 2 0.820047 0.731891 0.921373 11.00000 -1.50000 H64B 2 0.916453 0.628253 0.931922 11.00000 -1.50000 H64C 2 0.788877 0.637909 0.905346 11.00000 -1.50000 AFIX 0 C65 1 1.081770 0.659445 0.673913 11.00000 0.02166 0.03250 = 0.03800 -0.01560 0.00390 -0.01142 AFIX 13 H65 2 1.129274 0.640941 0.639167 11.00000 -1.20000 AFIX 0 C66 1 1.041209 0.775507 0.652995 11.00000 0.03613 0.03614 = 0.04867 -0.01299 -0.00026 -0.01899 AFIX 137 H66A 2 0.999851 0.800470 0.610223 11.00000 -1.50000 H66B 2 1.107986 0.805554 0.650475 11.00000 -1.50000 H66C 2 0.989704 0.795142 0.684833 11.00000 -1.50000 AFIX 0 C67 1 1.157254 0.619363 0.736893 11.00000 0.02523 0.03890 = 0.04512 -0.01998 -0.00280 -0.00760 AFIX 137 H67A 2 1.114088 0.641062 0.770870 11.00000 -1.50000 H67B 2 1.226362 0.646734 0.729749 11.00000 -1.50000 H67C 2 1.179832 0.544532 0.750542 11.00000 -1.50000 AFIX 0 C68 1 1.186519 0.450305 0.646164 11.00000 0.02051 0.04043 = 0.05082 -0.02425 0.00067 -0.00359 AFIX 13 H68 2 1.211226 0.493344 0.669524 11.00000 -1.20000 AFIX 0 C69 1 1.217090 0.483605 0.575492 11.00000 0.02755 0.05562 = 0.05599 -0.02659 0.00649 -0.00829 AFIX 137 H69A 2 1.183157 0.447714 0.551623 11.00000 -1.50000 H69B 2 1.301027 0.467074 0.573242 11.00000 -1.50000 H69C 2 1.186802 0.557503 0.556037 11.00000 -1.50000 AFIX 0 C70 1 1.242612 0.338132 0.679669 11.00000 0.03155 0.04935 = 0.06715 -0.01966 -0.00151 0.00338 AFIX 137 H70A 2 1.220672 0.317889 0.724871 11.00000 -1.50000 H70B 2 1.326552 0.327595 0.678873 11.00000 -1.50000 H70C 2 1.216793 0.296561 0.656874 11.00000 -1.50000 AFIX 0 N1 4 0.705630 1.022226 0.779593 11.00000 0.02018 0.02258 = 0.03470 -0.01258 0.00559 -0.00880 N2 4 0.535383 0.934369 0.816935 11.00000 0.02195 0.02155 = 0.02380 -0.00936 0.00464 -0.00940 N3 4 0.769657 0.610941 0.642036 11.00000 0.01894 0.01977 = 0.02215 -0.00774 -0.00105 -0.00311 N4 4 0.826366 0.519584 0.766712 11.00000 0.02585 0.02045 = 0.02295 -0.00510 -0.00088 -0.00541 N5 4 0.676671 0.856641 0.702315 11.00000 0.02309 0.02066 = 0.02244 -0.00762 -0.00123 -0.00337 N6 4 0.782701 0.780959 0.792893 11.00000 0.02327 0.02182 = 0.02120 -0.00850 -0.00066 -0.00550 N7 4 0.981242 0.614285 0.679594 11.00000 0.01998 0.02566 = 0.03344 -0.01232 0.00108 -0.00799 N8 4 1.061570 0.461542 0.647840 11.00000 0.02184 0.03244 = 0.04346 -0.01840 0.00128 -0.00337 HKLF 4 REM 1_a.res in P-1 REM R1 = 0.0498 for 10616 Fo > 4sig(Fo) and 0.0648 for all 13216 data REM 749 parameters refined using 0 restraints END WGHT 0.0536 1.4717 REM Highest difference peak 0.417, deepest hole -0.376, 1-sigma level 0.053 Q1 1 0.8005 1.2117 0.6037 11.00000 0.05 0.42 Q2 1 0.8592 1.0150 0.6236 11.00000 0.05 0.36 Q3 1 0.9143 0.5169 0.6594 11.00000 0.05 0.28 Q4 1 1.0361 0.4017 0.6455 11.00000 0.05 0.27 Q5 1 0.7996 0.7261 0.7181 11.00000 0.05 0.26 Q6 1 0.9215 0.6319 0.6874 11.00000 0.05 0.23 Q7 1 0.5729 0.9174 0.7926 11.00000 0.05 0.22 Q8 1 0.3419 0.9259 0.7679 11.00000 0.05 0.21 Q9 1 0.6567 0.9906 0.5853 11.00000 0.05 0.21 Q10 1 0.3605 1.1606 0.8065 11.00000 0.05 0.21 Q11 1 0.9425 0.6056 0.7057 11.00000 0.05 0.21 Q12 1 0.7526 0.4600 0.8485 11.00000 0.05 0.21 Q13 1 0.6048 0.8779 0.8211 11.00000 0.05 0.21 Q14 1 0.5044 0.5702 0.6373 11.00000 0.05 0.20 Q15 1 0.8230 0.6571 0.6406 11.00000 0.05 0.20 Q16 1 0.8191 0.9690 0.6694 11.00000 0.05 0.19 Q17 1 0.5428 0.4713 0.6423 11.00000 0.05 0.19 Q18 1 0.8383 0.3114 0.7280 11.00000 0.05 0.19 Q19 1 0.5389 1.0735 0.7875 11.00000 0.05 0.19 Q20 1 0.5948 0.9850 0.5506 11.00000 0.05 0.19 ; _shelx_res_checksum 14185 _shelx_hkl_file ; -2 0 0 15.30 2.20 -2 0 0 15.90 2.10 -2 0 0 17.00 1.60 -2 0 0 16.30 2.10 2 0 0 16.60 2.30 2 0 0 17.40 2.20 2 0 0 17.40 1.60 2 0 0 17.90 2.10 -3 0 0 2582.14 139.69 -3 0 0 2470.45 141.09 -3 0 0 2493.95 141.19 3 0 0 2436.96 141.09 3 0 0 2660.53 141.09 -4 0 0 16.40 3.00 -4 0 0 10.70 2.60 -4 0 0 13.90 2.90 -4 0 0 20.70 3.60 4 0 0 16.30 3.00 4 0 0 12.30 2.50 4 0 0 15.80 1.90 4 0 0 10.80 2.60 -5 0 0 645.84 38.40 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1 0 40.80 7.90 9 -1 0 89.49 9.20 -9 1 0 103.69 8.50 -9 1 0 89.79 10.60 -9 1 0 103.89 10.70 8 -1 0 50.89 6.80 8 -1 0 49.20 5.40 -8 1 0 54.79 5.30 -8 1 0 45.80 7.60 -8 1 0 46.40 6.70 -8 1 0 44.40 7.80 7 -1 0 153.18 11.10 7 -1 0 139.79 14.00 7 -1 0 155.78 13.20 -7 1 0 158.18 13.10 -7 1 0 160.68 13.50 -7 1 0 130.69 12.30 -7 1 0 158.08 10.80 6 -1 0 31.30 5.50 6 -1 0 25.10 5.00 6 -1 0 24.00 3.30 -6 1 0 33.40 3.40 -6 1 0 26.00 4.90 -6 1 0 38.40 5.00 -6 1 0 20.00 4.30 5 -1 0 48.70 5.60 5 -1 0 48.00 5.50 5 -1 0 56.09 4.80 -5 1 0 51.59 6.00 -5 1 0 53.39 5.80 -5 1 0 55.09 4.60 -5 1 0 47.80 5.60 4 -1 0 31.50 4.10 4 -1 0 33.30 4.10 4 -1 0 35.20 3.30 -4 1 0 30.30 3.80 -4 1 0 30.00 4.00 -4 1 0 33.60 3.00 -4 1 0 29.10 4.00 3 -1 0 6090.19 361.16 -3 1 0 6415.06 361.76 2 -1 0 404.56 23.10 2 -1 0 381.66 22.40 2 -1 0 401.16 23.20 -2 1 0 399.46 22.30 -2 1 0 369.86 23.00 -2 1 0 369.86 23.10 1 -1 0 80.69 5.90 1 -1 0 99.89 5.90 -1 1 0 94.09 6.20 -1 1 0 90.59 5.80 -1 1 0 95.79 6.10 -2 -1 0 24.30 2.70 -2 -1 0 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796.82 46.70 -10 -6 0 24.90 6.10 -10 -6 0 18.10 3.50 10 6 0 23.60 2.90 10 6 0 25.30 4.70 -11 -6 0 77.69 10.30 -11 -6 0 61.59 6.80 11 6 0 72.79 5.90 11 6 0 91.39 9.30 -12 -6 0 21.00 4.00 -12 -6 0 24.40 6.90 12 6 0 27.80 3.30 -13 -6 0 36.70 5.80 -13 -6 0 35.60 9.20 13 6 0 46.70 4.60 -14 -6 0 58.19 12.10 -11 7 0 -5.90 2.80 -11 7 0 -2.10 3.90 -11 7 0 -3.50 3.60 -10 7 0 12.20 5.10 -10 7 0 4.80 3.60 -10 7 0 7.40 4.50 -9 7 0 6.10 3.20 -9 7 0 5.50 3.40 -9 7 0 0.40 3.10 -8 7 0 6.40 3.30 -8 7 0 7.80 3.00 -8 7 0 15.00 5.60 -7 7 0 0.30 2.80 -7 7 0 1.70 2.20 -7 7 0 -1.40 2.40 -6 7 0 217.78 19.30 -6 7 0 225.38 18.60 -5 7 0 0.70 2.20 -5 7 0 0.70 2.90 4 -7 0 143.89 11.80 -4 7 0 131.49 13.10 -4 7 0 140.59 12.40 3 -7 0 161.28 13.20 -3 7 0 200.98 15.90 -3 7 0 188.28 16.80 2 -7 0 310.97 22.90 -2 7 0 363.96 22.50 -2 7 0 299.47 21.90 -2 7 0 364.36 24.30 1 -7 0 310.57 22.70 1 -7 0 371.86 21.50 -1 7 0 330.97 21.90 0 -7 0 2190.88 131.09 0 -7 0 2371.86 133.09 0 7 0 2460.75 131.99 0 7 0 2406.76 132.39 0 7 0 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2.80 3.10 -11 -4 8 113.09 13.80 -10 -4 8 4.00 3.70 -9 -4 8 -2.80 2.40 8 4 -8 305.87 22.00 -8 -4 8 310.07 24.20 7 4 -8 160.38 12.70 -7 -4 8 141.29 14.20 6 4 -8 31.40 5.30 -6 -4 8 28.20 6.40 5 4 -8 138.39 10.50 -5 -4 8 110.69 11.70 4 4 -8 194.68 13.90 4 4 -8 191.68 12.10 4 4 -8 196.88 15.70 3 4 -8 80.79 5.70 3 4 -8 77.09 6.90 -3 -4 8 57.29 6.30 2 4 -8 302.87 20.50 2 4 -8 302.87 18.80 2 4 -8 360.56 20.70 2 4 -8 292.37 21.50 -2 -4 8 302.37 19.30 -2 -4 8 272.27 19.50 1 4 -8 118.69 8.30 1 4 -8 83.99 9.50 1 4 -8 91.99 9.30 -1 -4 8 124.69 8.90 -1 -4 8 107.39 8.40 0 4 -8 318.97 19.30 0 4 -8 279.67 20.40 0 4 -8 297.37 20.20 0 -4 8 277.07 19.40 0 -4 8 323.87 19.80 -1 4 -8 40.60 5.40 -1 4 -8 36.80 4.50 -1 4 -8 41.30 5.30 1 -4 8 46.80 4.90 1 -4 8 45.20 8.70 -2 4 -8 0.40 1.00 -2 4 -8 1.80 1.90 -2 4 -8 -0.50 1.00 2 -4 8 1.20 1.40 2 -4 8 4.70 1.80 2 -4 8 0.50 0.90 -3 4 -8 352.36 23.90 -3 4 -8 303.17 23.00 3 -4 8 335.37 22.60 3 -4 8 351.76 22.70 -4 4 -8 21.90 5.10 -4 4 -8 28.20 6.00 4 -4 8 16.20 3.80 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6 21 108.89 11.70 0 -6 -21 62.99 7.10 0 6 21 69.39 9.20 -1 -6 -21 43.30 5.90 1 6 21 31.40 8.00 -2 -6 -21 4.50 2.40 2 6 21 3.20 2.20 -3 -6 -21 73.49 7.90 -3 -6 -21 50.39 7.80 3 6 21 68.69 9.00 -4 -6 -21 41.40 6.60 -4 -6 -21 49.90 6.70 -4 -6 -21 41.90 6.90 4 6 21 44.80 8.00 -5 -6 -21 106.39 9.80 -5 -6 -21 110.69 9.20 -5 -6 -21 112.79 10.70 5 6 21 80.69 10.80 -6 -6 -21 9.00 4.10 -6 -6 -21 3.30 2.80 -6 -6 -21 5.30 2.60 6 6 21 2.40 3.30 -7 -6 -21 21.80 5.50 7 6 21 10.60 4.70 -8 -6 -21 5.40 6.10 -8 -6 -21 0.30 2.50 8 6 21 4.40 3.30 -9 -6 -21 43.50 8.40 -9 -6 -21 42.40 8.40 9 6 21 29.80 7.30 7 -7 -21 3.20 2.70 -7 7 21 12.90 4.90 -6 7 21 109.09 12.30 5 -7 -21 7.70 3.30 5 -7 -21 2.50 2.20 -5 7 21 0.40 3.00 4 -7 -21 144.49 12.30 4 -7 -21 153.38 13.00 -4 7 21 161.38 15.10 3 -7 -21 4.60 2.10 3 -7 -21 4.50 3.10 -3 7 21 3.80 3.20 2 -7 -21 58.49 6.60 2 -7 -21 53.59 7.80 -2 7 21 66.39 10.50 1 -7 -21 -3.30 1.80 1 -7 -21 5.70 3.30 -1 7 21 -0.70 2.10 0 -7 -21 113.69 9.70 0 7 21 97.19 20.10 -1 -7 -21 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2 22 18.60 3.70 5 -2 -22 47.30 7.80 -5 2 22 46.20 5.80 4 -2 -22 15.60 4.70 -4 2 22 20.30 4.10 3 -2 -22 189.28 15.60 -3 2 22 173.08 14.00 2 -2 -22 61.99 7.90 -2 2 22 60.89 7.20 1 -2 -22 14.70 4.90 -1 2 22 9.70 3.50 0 2 22 24.90 8.60 -1 -2 -22 59.49 12.50 -1 -2 -22 55.99 7.60 1 2 22 62.59 8.00 -2 -2 -22 32.00 7.30 -2 -2 -22 31.30 6.20 2 2 22 37.40 6.90 -3 -2 -22 -0.50 2.40 -3 -2 -22 -1.60 1.60 3 2 22 2.80 2.50 -4 -2 -22 15.40 4.20 -4 -2 -22 8.00 3.90 4 2 22 18.10 4.60 -5 -2 -22 2.70 3.10 -5 -2 -22 3.50 3.70 5 2 22 13.10 4.20 -6 -2 -22 11.50 4.40 -6 -2 -22 10.10 4.10 6 2 22 10.20 4.20 -7 -2 -22 33.60 8.20 -7 -2 -22 37.80 7.10 7 2 22 22.00 6.10 8 -3 -22 -1.50 2.20 -8 3 22 0.90 3.40 7 -3 -22 6.20 3.40 -7 3 22 2.00 2.10 6 -3 -22 -2.20 2.10 -6 3 22 -3.60 1.70 5 -3 -22 65.99 8.30 -5 3 22 73.09 7.60 4 -3 -22 17.60 4.40 -4 3 22 15.60 3.90 -3 3 22 -4.30 1.90 2 -3 -22 16.20 4.60 -2 3 22 11.10 3.80 1 -3 -22 154.98 13.50 -1 3 22 155.58 13.50 0 -3 -22 3.30 2.40 0 3 22 1.60 3.20 -1 -3 -22 45.00 6.70 1 3 22 55.09 7.30 -2 -3 -22 1.60 2.20 -2 -3 -22 1.30 3.30 2 3 22 6.90 3.20 -3 -3 -22 98.79 10.00 -3 -3 -22 108.19 11.00 3 3 22 89.39 10.60 -4 -3 -22 18.50 4.80 -4 -3 -22 24.30 5.90 4 3 22 19.30 5.10 -5 -3 -22 -4.30 1.90 5 3 22 -1.40 2.20 -6 -3 -22 2.60 3.10 -6 -3 -22 12.20 4.70 6 3 22 9.50 3.80 -7 -3 -22 6.70 3.50 -7 -3 -22 5.80 4.20 7 3 22 4.30 5.20 8 -4 -22 160.58 14.80 7 -4 -22 19.20 4.60 -7 4 22 8.30 3.40 6 -4 -22 1.60 2.30 -6 4 22 5.20 2.80 5 -4 -22 6.90 3.10 -5 4 22 18.50 4.40 4 -4 -22 7.50 5.20 -4 4 22 4.20 3.00 3 -4 -22 42.20 7.00 -3 4 22 35.00 6.30 2 -4 -22 -0.80 1.70 -2 4 22 -1.10 2.10 1 -4 -22 133.39 12.30 -1 4 22 148.19 13.10 0 -4 -22 19.90 4.70 0 4 22 24.20 8.00 -1 -4 -22 49.80 7.00 1 4 22 57.49 7.70 -2 -4 -22 11.90 3.90 2 4 22 3.30 3.10 -3 -4 -22 21.90 4.90 -3 -4 -22 32.50 6.30 3 4 22 17.50 5.00 -4 -4 -22 151.78 12.10 -4 -4 -22 129.09 13.00 4 4 22 113.59 12.60 -5 -4 -22 48.90 6.70 5 4 22 50.29 8.50 -6 -4 -22 8.00 3.50 -6 -4 -22 7.40 3.20 6 4 22 8.00 3.80 -7 -4 -22 2.10 2.90 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31.10 6.30 -3 -2 -24 77.79 9.40 -3 -2 -24 79.09 10.40 3 2 24 75.19 9.60 -4 -2 -24 17.00 6.50 -4 -2 -24 13.20 5.70 4 2 24 20.90 6.10 -5 -2 -24 -0.50 2.90 5 2 24 4.00 3.20 6 -3 -24 1.70 2.70 -6 3 24 4.20 2.50 5 -3 -24 -1.00 1.90 -5 3 24 -4.40 1.70 4 -3 -24 9.70 3.50 -4 3 24 3.70 2.80 3 -3 -24 71.19 8.80 -3 3 24 58.69 7.50 2 -3 -24 3.00 2.50 -2 3 24 0.10 2.20 1 -3 -24 109.29 11.60 -1 3 24 116.59 11.20 0 -3 -24 -1.30 2.20 0 3 24 1.60 2.50 -1 -3 -24 12.40 3.90 -1 -3 -24 22.00 5.90 1 3 24 20.30 5.10 -2 -3 -24 18.80 5.50 2 3 24 14.50 4.60 -3 -3 -24 1.10 2.60 -3 -3 -24 -0.40 2.60 3 3 24 2.50 2.70 -4 -3 -24 -1.50 2.70 -4 -3 -24 6.50 3.60 4 3 24 4.70 3.30 -5 -3 -24 0.60 2.80 -5 -3 -24 5.20 3.00 5 3 24 4.10 4.30 6 -4 -24 8.40 3.80 -6 4 24 4.40 3.40 5 -4 -24 9.40 3.70 -5 4 24 3.30 3.30 4 -4 -24 57.99 7.50 -4 4 24 44.30 7.40 3 -4 -24 1.20 2.20 -3 4 24 2.10 2.60 2 -4 -24 190.28 16.20 -2 4 24 201.08 16.50 1 -4 -24 0.70 2.70 -1 4 24 -0.60 2.50 0 -4 -24 9.90 4.80 0 4 24 3.60 3.00 -1 -4 -24 0.70 3.20 1 4 24 1.10 2.40 -2 -4 -24 8.10 4.20 -2 -4 -24 3.90 2.40 2 4 24 11.40 3.80 -3 -4 -24 47.40 8.20 -3 -4 -24 30.90 6.20 3 4 24 38.70 7.90 -4 -4 -24 7.90 3.60 -4 -4 -24 6.80 4.10 4 4 24 8.60 4.20 -5 -4 -24 -2.40 2.70 -5 -4 -24 7.90 3.40 5 4 24 4.20 3.10 -6 -4 -24 43.10 8.30 -6 -4 -24 28.10 6.30 6 4 24 23.20 5.90 6 -5 -24 54.59 7.60 5 -5 -24 6.00 2.90 -5 5 24 5.40 3.40 4 -5 -24 2.20 3.10 -4 5 24 -1.10 2.40 3 -5 -24 19.80 5.10 -3 5 24 16.60 5.60 2 -5 -24 37.30 7.00 -2 5 24 42.20 7.50 1 -5 -24 189.48 16.00 -1 5 24 203.08 17.00 0 -5 -24 31.00 6.00 0 5 24 28.70 6.10 -1 -5 -24 20.30 5.10 1 5 24 16.30 4.90 -2 -5 -24 27.80 5.60 2 5 24 12.40 4.80 -3 -5 -24 31.10 6.60 -3 -5 -24 28.80 5.70 3 5 24 26.70 6.40 -4 -5 -24 4.50 2.90 4 5 24 -0.50 3.00 -5 -5 -24 24.30 5.10 -5 -5 -24 21.90 5.90 5 5 24 12.10 4.90 -6 -5 -24 103.59 9.90 -6 -5 -24 71.69 10.30 6 5 24 79.19 11.00 5 -6 -24 52.49 6.80 -5 6 24 38.20 7.40 4 -6 -24 59.89 7.80 -4 6 24 70.39 9.30 3 -6 -24 1.40 2.30 -3 6 24 7.40 3.80 2 -6 -24 0.90 1.80 -2 6 24 0.00 3.00 1 -6 -24 54.49 7.30 -1 6 24 70.69 9.50 0 -6 -24 76.99 8.70 0 6 24 92.29 10.70 -1 -6 -24 19.80 4.70 1 6 24 16.90 5.60 -2 -6 -24 112.39 10.90 2 6 24 94.79 11.40 -3 -6 -24 78.19 9.50 -3 -6 -24 83.89 8.60 3 6 24 94.09 11.20 -4 -6 -24 -1.60 2.30 -4 -6 -24 5.90 3.20 4 6 24 2.20 3.00 -5 -6 -24 -2.50 2.40 -5 -6 -24 4.50 3.40 5 6 24 -3.20 2.40 -6 -6 -24 0.50 3.30 -6 -6 -24 4.10 3.00 6 6 24 -1.90 2.50 5 -7 -24 89.69 9.50 -5 7 24 85.69 10.70 4 -7 -24 11.60 3.60 -4 7 24 13.30 4.40 3 -7 -24 51.79 6.70 -3 7 24 34.30 7.40 2 -7 -24 1.60 2.50 -2 7 24 -2.00 2.60 1 -7 -24 54.19 7.10 -1 7 24 63.29 8.80 0 -7 -24 4.60 2.30 0 7 24 2.70 3.30 -1 -7 -24 70.09 8.10 1 7 24 53.29 9.60 -2 -7 -24 13.40 4.00 2 7 24 19.70 5.40 -3 -7 -24 117.19 11.00 3 7 24 99.39 12.20 -4 -7 -24 28.40 5.10 -4 -7 -24 35.40 6.30 4 7 24 29.30 6.50 -5 -7 -24 36.60 5.60 -5 -7 -24 22.60 5.70 5 7 24 11.20 5.30 -6 -7 -24 0.50 3.70 -6 -7 -24 -0.30 2.80 6 7 24 -2.60 3.10 4 -8 -24 9.20 3.30 -4 8 24 3.00 4.10 3 -8 -24 15.50 3.90 -3 8 24 17.50 6.20 2 -8 -24 65.09 7.30 -2 8 24 59.89 10.40 1 -8 -24 11.50 3.60 -1 8 24 1.30 3.60 0 -8 -24 109.99 10.10 0 8 24 103.49 12.50 -1 -8 -24 0.50 2.30 1 8 24 2.90 2.90 -2 -8 -24 19.10 4.50 2 8 24 18.80 6.40 -3 -8 -24 9.30 3.60 3 8 24 13.80 4.70 -4 -8 -24 22.60 5.30 -4 -8 -24 10.80 3.20 4 8 24 12.40 5.10 -5 -8 -24 21.00 4.80 -5 -8 -24 8.90 3.10 5 8 24 6.70 4.00 -6 -8 -24 236.18 18.30 6 8 24 200.48 19.80 4 -9 -24 2.70 2.60 -4 9 24 8.80 4.40 3 -9 -24 1.60 2.30 -3 9 24 7.30 4.40 2 -9 -24 -0.60 2.10 -2 9 24 1.10 3.10 1 -9 -24 13.10 3.30 -1 9 24 8.60 4.80 0 -9 -24 23.40 4.40 0 9 24 23.40 6.80 -1 -9 -24 117.09 9.80 1 9 24 97.39 13.20 -2 -9 -24 4.60 2.50 2 9 24 2.30 3.40 -3 -9 -24 28.00 5.20 3 9 24 21.90 6.80 -4 -9 -24 95.19 9.60 -4 -9 -24 92.29 8.40 4 9 24 104.09 12.50 -5 -9 -24 22.90 6.20 -5 -9 -24 22.30 5.50 -5 -9 -24 21.20 3.90 5 9 24 16.80 9.40 -6 -9 -24 1.00 3.40 -6 -9 -24 3.20 3.10 6 9 24 2.40 4.00 3 -10 -24 8.20 2.70 -3 10 24 4.00 4.40 2 -10 -24 5.50 2.80 -2 10 24 9.30 4.90 1 -10 -24 36.00 5.50 -1 10 24 23.60 7.30 0 -10 -24 -0.10 2.00 0 10 24 4.90 3.50 -1 -10 -24 20.40 4.00 1 10 24 26.70 7.40 2 10 24 277.27 24.60 -3 -10 -24 -0.30 2.70 -3 -10 -24 4.50 2.60 3 10 24 16.80 6.20 -4 -10 -24 29.20 7.10 -4 -10 -24 28.20 5.10 4 10 24 36.50 8.80 -5 -10 -24 3.80 3.90 -5 -10 -24 7.00 3.20 5 10 24 11.90 6.00 -1 11 24 6.40 4.40 0 11 24 26.10 7.60 -1 -11 -24 -0.60 2.70 1 11 24 5.10 3.90 -2 -11 -24 3.90 3.40 2 11 24 13.50 5.80 -3 -11 -24 93.39 10.00 3 11 24 76.39 15.00 -4 -11 -24 6.50 3.30 4 11 24 -4.30 3.60 -5 -11 -24 4.10 3.80 -2 -12 -24 9.90 3.70 2 12 24 -4.20 3.20 -3 -12 -24 -0.70 3.00 3 12 24 -6.70 3.50 3 0 -25 8.40 4.50 2 0 -25 4.70 4.10 -2 0 25 21.20 4.70 1 0 -25 -0.60 2.70 1 0 -25 0.80 2.50 -1 0 25 1.00 2.50 0 0 -25 57.19 10.20 0 0 -25 53.89 9.30 0 0 25 61.29 8.20 -1 0 -25 5.80 4.00 -1 0 -25 -3.30 3.10 1 0 25 -0.20 2.70 4 -1 -25 75.19 9.70 -4 1 25 68.49 7.50 3 -1 -25 -2.00 3.10 -3 1 25 1.80 2.80 2 -1 -25 9.20 3.30 -2 1 25 -1.60 2.20 1 -1 -25 2.00 3.00 1 -1 -25 0.50 2.50 -1 1 25 -0.60 2.50 0 -1 -25 11.50 4.50 0 -1 -25 12.90 5.10 0 1 25 13.90 4.60 -1 -1 -25 10.90 3.80 -1 -1 -25 15.00 5.40 1 1 25 16.40 4.70 -2 -1 -25 11.30 6.00 -2 -1 -25 10.40 4.40 2 1 25 16.20 4.60 4 -2 -25 33.30 6.70 -4 2 25 44.70 6.10 3 -2 -25 0.80 2.70 -3 2 25 -0.50 2.60 2 -2 -25 3.40 3.30 -2 2 25 4.30 3.00 1 -2 -25 6.70 2.90 -1 2 25 3.40 3.00 0 -2 -25 4.60 3.80 0 -2 -25 1.00 2.20 0 2 25 1.10 2.90 -1 -2 -25 16.40 4.70 -1 -2 -25 7.60 3.90 1 2 25 10.70 4.00 -2 -2 -25 97.99 11.10 -2 -2 -25 104.59 12.20 2 2 25 90.99 10.70 -3 -2 -25 -2.60 2.40 -3 -2 -25 -4.00 2.70 3 2 25 3.90 3.20 4 -3 -25 103.79 10.70 -4 3 25 71.59 8.70 3 -3 -25 -0.40 2.90 -3 3 25 4.70 3.20 2 -3 -25 75.09 9.10 -2 3 25 74.39 8.50 1 -3 -25 24.40 5.90 -1 3 25 29.70 6.10 0 -3 -25 2.10 2.60 0 3 25 2.20 2.40 -1 -3 -25 15.50 5.10 -1 -3 -25 15.00 4.40 1 3 25 12.60 4.60 -2 -3 -25 39.90 7.70 -2 -3 -25 52.39 8.60 2 3 25 60.89 8.30 -3 -3 -25 185.98 17.60 -3 -3 -25 194.28 16.70 3 3 25 194.38 17.30 -4 -3 -25 27.30 6.80 4 3 25 25.10 8.10 4 -4 -25 7.00 4.20 -4 4 25 5.90 4.30 3 -4 -25 0.70 2.30 -3 4 25 -3.10 2.50 2 -4 -25 46.20 7.80 -2 4 25 37.40 7.10 1 -4 -25 38.10 7.00 -1 4 25 31.70 6.30 0 -4 -25 39.70 7.50 0 4 25 38.10 7.20 -1 -4 -25 -2.30 2.50 1 4 25 1.50 3.20 -2 -4 -25 38.40 8.10 -2 -4 -25 45.00 8.00 2 4 25 43.10 7.90 -3 -4 -25 5.40 3.70 -3 -4 -25 6.80 3.70 3 4 25 1.30 3.40 -4 -4 -25 36.10 8.10 -4 -4 -25 34.40 6.40 4 4 25 29.10 6.60 4 -5 -25 26.40 6.20 -4 5 25 30.30 6.20 3 -5 -25 2.50 2.80 -3 5 25 5.90 3.10 2 -5 -25 9.20 3.80 -2 5 25 5.60 3.20 1 -5 -25 39.90 7.00 -1 5 25 30.00 6.30 0 -5 -25 12.10 5.20 0 5 25 14.20 5.10 -1 -5 -25 135.19 17.10 1 5 25 145.49 14.20 -2 -5 -25 96.59 10.20 -2 -5 -25 107.89 11.20 2 5 25 81.69 10.90 -3 -5 -25 9.70 4.00 -3 -5 -25 9.40 3.70 3 5 25 9.40 4.70 -4 -5 -25 5.50 3.40 -4 -5 -25 23.30 6.00 4 5 25 12.70 4.50 -5 -5 -25 12.00 4.40 -5 -5 -25 15.50 5.10 5 5 25 19.90 5.40 4 -6 -25 3.70 2.60 -4 6 25 -1.50 3.00 3 -6 -25 -4.40 1.90 -3 6 25 -0.70 2.70 2 -6 -25 -5.80 2.80 -2 6 25 7.30 3.70 1 -6 -25 6.70 3.30 -1 6 25 2.90 3.50 0 -6 -25 -3.00 1.90 0 6 25 5.30 3.30 -1 -6 -25 181.78 15.20 1 6 25 153.68 15.50 -2 -6 -25 12.60 4.60 2 6 25 12.90 4.70 -3 -6 -25 10.40 4.30 -3 -6 -25 10.90 3.60 3 6 25 14.10 4.90 -4 -6 -25 -0.70 2.20 -4 -6 -25 -5.50 3.10 4 6 25 -2.30 2.90 -5 -6 -25 1.60 3.20 -5 -6 -25 -1.00 3.30 4 -7 -25 32.60 6.00 -4 7 25 31.50 7.20 3 -7 -25 46.70 7.70 -3 7 25 46.30 8.60 2 -7 -25 225.18 17.60 -2 7 25 237.48 20.20 1 -7 -25 13.30 3.90 -1 7 25 9.80 4.70 0 -7 -25 2.60 2.80 0 7 25 -1.40 3.00 -1 -7 -25 -2.70 2.50 1 7 25 -0.80 2.60 -2 -7 -25 23.70 5.70 2 7 25 22.40 6.00 -3 -7 -25 9.00 3.70 -3 -7 -25 4.50 2.50 3 7 25 2.40 3.40 -4 -7 -25 11.40 4.30 -4 -7 -25 14.90 3.60 4 7 25 5.10 3.70 -5 -7 -25 -3.20 2.80 -5 -7 -25 -2.50 2.50 5 7 25 5.60 4.20 3 -8 -25 2.70 2.90 -3 8 25 10.00 4.90 2 -8 -25 4.80 2.80 -2 8 25 3.90 4.10 1 -8 -25 150.08 12.30 -1 8 25 123.39 14.50 0 -8 -25 11.00 3.90 0 8 25 11.80 5.80 -1 -8 -25 26.70 5.60 1 8 25 29.80 7.30 -2 -8 -25 1.20 2.60 2 8 25 0.50 2.60 -3 -8 -25 28.70 5.80 3 8 25 29.30 6.70 -4 -8 -25 7.80 2.70 -4 -8 -25 3.10 3.50 4 8 25 2.10 4.20 -5 -8 -25 93.69 10.50 5 8 25 78.19 11.20 2 -9 -25 1.40 2.40 -2 9 25 3.40 3.60 1 -9 -25 14.90 4.40 -1 9 25 13.50 5.50 0 -9 -25 12.70 4.00 0 9 25 6.20 4.10 -1 -9 -25 1.50 2.60 1 9 25 9.80 4.70 -2 -9 -25 83.49 9.00 2 9 25 86.99 12.10 -3 -9 -25 68.09 7.90 3 9 25 64.79 11.30 -4 -9 -25 3.60 3.60 -4 -9 -25 0.90 2.20 4 9 25 -0.60 3.80 1 -10 -25 -0.50 2.50 -1 10 25 -2.00 3.40 0 -10 -25 3.30 3.80 0 10 25 2.70 3.80 -1 -10 -25 0.60 2.10 1 10 25 0.30 3.40 2 10 25 174.98 18.40 -3 -10 -25 132.09 13.40 -3 -10 -25 145.79 11.80 3 10 25 122.09 22.50 -4 -10 -25 23.40 4.20 -4 -10 -25 20.20 5.70 1 -2 -26 -2.70 2.40 -1 2 26 1.10 2.60 0 -2 -26 28.10 6.30 0 -2 -26 18.00 6.10 0 2 26 36.40 6.80 -1 -2 -26 38.00 8.00 2 -3 -26 6.90 3.30 -2 3 26 5.70 3.10 1 -3 -26 29.30 6.60 -1 3 26 40.50 7.20 0 -3 -26 -1.70 2.50 0 3 26 2.20 2.80 -1 -3 -26 9.40 3.80 -1 -3 -26 3.60 3.90 1 3 26 3.40 3.50 -2 -3 -26 0.00 2.40 -2 -3 -26 1.70 3.00 2 3 26 2.70 3.10 3 -4 -26 43.10 8.10 2 -4 -26 -3.80 2.50 -2 4 26 -0.70 2.20 1 -4 -26 11.60 3.70 -1 4 26 5.30 3.40 0 -4 -26 28.80 6.70 0 4 26 26.80 5.60 -1 -4 -26 -2.50 1.80 -1 -4 -26 -0.70 2.90 1 4 26 1.30 3.10 -2 -4 -26 -5.90 2.40 2 4 26 -2.10 2.70 -3 -4 -26 3.30 3.40 3 -5 -26 9.30 3.90 2 -5 -26 -0.30 2.30 -2 5 26 5.40 3.50 1 -5 -26 -3.60 2.10 -1 5 26 2.60 3.20 0 -5 -26 149.29 14.00 0 5 26 147.19 14.60 -1 -5 -26 21.70 5.70 1 5 26 10.40 4.80 -2 -5 -26 106.49 11.40 -2 -5 -26 79.59 9.60 2 5 26 96.89 11.70 -3 -5 -26 -1.60 2.90 -3 -5 -26 5.30 3.30 3 5 26 0.30 3.00 2 -6 -26 151.78 13.40 -2 6 26 130.09 13.50 1 -6 -26 21.10 5.30 -1 6 26 2.90 3.60 0 -6 -26 198.98 19.70 0 6 26 192.58 17.40 -1 -6 -26 54.79 13.40 1 6 26 30.80 6.60 -2 -6 -26 13.90 5.50 2 6 26 7.60 4.40 -3 -6 -26 15.40 4.30 -3 -6 -26 18.10 5.50 3 6 26 10.60 5.00 -2 7 26 31.50 7.00 1 -7 -26 53.39 7.70 -1 7 26 49.00 9.30 0 -7 -26 5.10 2.70 0 7 26 0.40 3.00 -1 -7 -26 6.20 3.10 1 7 26 9.10 3.80 -2 -7 -26 -0.10 2.30 2 7 26 6.20 3.80 -3 -7 -26 60.99 7.00 -3 -7 -26 44.20 8.50 3 7 26 36.00 10.10 1 -8 -26 14.20 3.90 -1 8 26 5.40 4.50 0 -8 -26 275.47 20.10 0 8 26 266.27 23.20 -1 -8 -26 0.60 2.50 1 8 26 -4.30 2.80 -2 -8 -26 3.90 3.30 2 8 26 9.80 4.60 -3 -8 -26 3.40 2.60 -3 -8 -26 -0.50 3.10 3 8 26 2.80 3.90 -1 -9 -26 67.69 8.20 1 9 26 77.89 12.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 51593 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.66807(4) 0.90615(4) 0.77623(2) 0.01957(13) Uani 1 1 d . . . . . Al2 Al 0.82861(4) 0.65388(4) 0.70261(2) 0.02072(13) Uani 1 1 d . . . . . C1 C 0.60808(15) 1.08103(13) 0.80130(9) 0.0259(4) Uani 1 1 d . . . . . C2 C 0.52096(14) 1.03535(12) 0.82136(8) 0.0230(3) Uani 1 1 d . . . . . C3 C 0.60215(17) 1.19238(14) 0.79078(11) 0.0392(5) Uani 1 1 d . . . . . H3A H 0.5756 1.2324 0.7456 0.059 Uiso 1 1 calc R U . . . H3B H 0.6788 1.2008 0.7996 0.059 Uiso 1 1 calc R U . . . H3C H 0.5482 1.2163 0.8202 0.059 Uiso 1 1 calc R U . . . C4 C 0.41107(16) 1.08504(14) 0.84537(9) 0.0317(4) Uani 1 1 d . . . . . H4A H 0.4162 1.1524 0.8466 0.048 Uiso 1 1 calc R U . . . H4B H 0.3997 1.0422 0.8892 0.048 Uiso 1 1 calc R U . . . H4C H 0.3459 1.0928 0.8159 0.048 Uiso 1 1 calc R U . . . C5 C 0.81450(15) 1.04616(12) 0.78354(9) 0.0262(4) Uani 1 1 d . . . . . C6 C 0.86343(16) 1.04151(14) 0.84385(10) 0.0324(4) Uani 1 1 d . . . . . C7 C 0.96817(17) 1.06835(15) 0.84500(11) 0.0388(5) Uani 1 1 d . . . . . H7 H 1.0003 1.0672 0.8850 0.047 Uiso 1 1 calc R U . . . C8 C 1.02607(17) 1.09651(17) 0.78925(12) 0.0448(5) Uani 1 1 d . . . . . H8 H 1.0973 1.1149 0.7910 0.054 Uiso 1 1 calc R U . . . C9 C 0.98076(17) 1.09803(16) 0.73104(11) 0.0398(5) Uani 1 1 d . . . . . H9 H 1.0222 1.1159 0.6930 0.048 Uiso 1 1 calc R U . . . C10 C 0.87457(16) 1.07362(13) 0.72690(10) 0.0302(4) Uani 1 1 d . . . . . C11 C 0.80825(19) 1.00623(19) 0.90832(10) 0.0456(5) Uani 1 1 d . . . . . H11 H 0.7387 0.9830 0.9001 0.055 Uiso 1 1 calc R U . . . C12 C 0.8887(2) 0.91717(19) 0.95850(11) 0.0575(7) Uani 1 1 d . . . . . H12A H 0.9116 0.8597 0.9415 0.086 Uiso 1 1 calc R U . . . H12B H 0.8489 0.8961 0.9987 0.086 Uiso 1 1 calc R U . . . H12C H 0.9573 0.9384 0.9677 0.086 Uiso 1 1 calc R U . . . C13 C 0.7695(3) 1.0919(2) 0.93815(14) 0.0767(9) Uani 1 1 d . . . . . H13A H 0.8352 1.1199 0.9432 0.115 Uiso 1 1 calc R U . . . H13B H 0.7395 1.0646 0.9808 0.115 Uiso 1 1 calc R U . . . H13C H 0.7089 1.1461 0.9095 0.115 Uiso 1 1 calc R U . . . C14 C 0.82396(17) 1.08122(15) 0.66150(10) 0.0355(4) Uani 1 1 d . . . . . H14 H 0.7753 1.0302 0.6698 0.043 Uiso 1 1 calc R U . . . C15 C 0.7466(3) 1.1840(2) 0.63053(15) 0.0750(9) Uani 1 1 d . . . . . H15A H 0.6869 1.1979 0.6602 0.113 Uiso 1 1 calc R U . . . H15B H 0.7104 1.1856 0.5900 0.113 Uiso 1 1 calc R U . . . H15C H 0.7916 1.2361 0.6211 0.113 Uiso 1 1 calc R U . . . C16 C 0.9140(2) 1.0554(2) 0.61526(12) 0.0591(7) Uani 1 1 d . . . . . H16A H 0.8769 1.0432 0.5795 0.089 Uiso 1 1 calc R U . . . H16B H 0.9721 0.9938 0.6388 0.089 Uiso 1 1 calc R U . . . H16C H 0.9510 1.1125 0.5977 0.089 Uiso 1 1 calc R U . . . C17 C 0.44673(14) 0.88356(12) 0.84489(8) 0.0219(3) Uani 1 1 d . . . . . C18 C 0.34779(15) 0.89578(13) 0.80654(8) 0.0248(4) Uani 1 1 d . . . . . C19 C 0.25394(16) 0.86219(14) 0.83708(10) 0.0329(4) Uani 1 1 d . . . . . H19 H 0.1854 0.8726 0.8118 0.040 Uiso 1 1 calc R U . . . C20 C 0.25884(17) 0.81415(15) 0.90331(10) 0.0369(5) Uani 1 1 d . . . . . H20 H 0.1927 0.7950 0.9237 0.044 Uiso 1 1 calc R U . . . C21 C 0.36002(17) 0.79387(15) 0.93992(9) 0.0339(4) Uani 1 1 d . . . . . H21 H 0.3644 0.7569 0.9851 0.041 Uiso 1 1 calc R U . . . C22 C 0.45593(15) 0.82680(13) 0.91161(8) 0.0269(4) Uani 1 1 d . . . . . C23 C 0.34459(15) 0.94152(15) 0.73276(8) 0.0298(4) Uani 1 1 d . . . . . H23 H 0.4239 0.9175 0.7195 0.036 Uiso 1 1 calc R U . . . C24 C 0.31640(19) 1.05814(16) 0.70680(10) 0.0419(5) Uani 1 1 d . . . . . H24A H 0.3093 1.0809 0.6592 0.063 Uiso 1 1 calc R U . . . H24B H 0.3782 1.0828 0.7211 0.063 Uiso 1 1 calc R U . . . H24C H 0.2436 1.0855 0.7235 0.063 Uiso 1 1 calc R U . . . C25 C 0.26371(18) 0.90192(18) 0.69842(11) 0.0426(5) Uani 1 1 d . . . . . H25A H 0.1836 0.9307 0.7055 0.064 Uiso 1 1 calc R U . . . H25B H 0.2802 0.8272 0.7161 0.064 Uiso 1 1 calc R U . . . H25C H 0.2755 0.9225 0.6517 0.064 Uiso 1 1 calc R U . . . C26 C 0.56644(17) 0.80208(16) 0.95265(9) 0.0357(4) Uani 1 1 d . . . . . H26 H 0.6303 0.8082 0.9222 0.043 Uiso 1 1 calc R U . . . C27 C 0.5946(2) 0.6925(2) 0.99947(11) 0.0564(6) Uani 1 1 d . . . . . H27A H 0.5375 0.6854 1.0326 0.085 Uiso 1 1 calc R U . . . H27B H 0.6715 0.6769 1.0206 0.085 Uiso 1 1 calc R U . . . H27C H 0.5930 0.6450 0.9753 0.085 Uiso 1 1 calc R U . . . C28 C 0.5649(2) 0.8781(2) 0.98940(12) 0.0572(6) Uani 1 1 d . . . . . H28A H 0.5545 0.9471 0.9583 0.086 Uiso 1 1 calc R U . . . H28B H 0.6379 0.8598 1.0150 0.086 Uiso 1 1 calc R U . . . H28C H 0.5011 0.8763 1.0185 0.086 Uiso 1 1 calc R U . . . C29 C 0.85657(14) 0.51062(13) 0.65980(8) 0.0224(3) Uani 1 1 d . . . . . C30 C 0.84038(14) 0.45737(13) 0.73177(8) 0.0248(4) Uani 1 1 d . . . . . C31 C 0.84994(15) 0.44644(14) 0.61627(9) 0.0277(4) Uani 1 1 d . . . . . H31A H 0.7733 0.4322 0.6175 0.042 Uiso 1 1 calc R U . . . H31B H 0.9084 0.3819 0.6317 0.042 Uiso 1 1 calc R U . . . H31C H 0.8638 0.4838 0.5715 0.042 Uiso 1 1 calc R U . . . C32 C 0.8411(2) 0.34905(14) 0.75652(10) 0.0394(5) Uani 1 1 d . . . . . H32A H 0.8292 0.3297 0.8032 0.059 Uiso 1 1 calc R U . . . H32B H 0.9154 0.3087 0.7491 0.059 Uiso 1 1 calc R U . . . H32C H 0.7792 0.3359 0.7338 0.059 Uiso 1 1 calc R U . . . C33 C 0.70496(14) 0.64787(12) 0.58095(8) 0.0219(3) Uani 1 1 d . . . . . C34 C 0.73729(15) 0.72036(14) 0.52657(8) 0.0273(4) Uani 1 1 d . . . . . C35 C 0.66701(18) 0.75965(16) 0.46957(9) 0.0381(5) Uani 1 1 d . . . . . H35 H 0.6885 0.8091 0.4334 0.046 Uiso 1 1 calc R U . . . C36 C 0.56719(18) 0.72920(17) 0.46388(10) 0.0397(5) Uani 1 1 d . . . . . H36 H 0.5206 0.7572 0.4244 0.048 Uiso 1 1 calc R U . . . C37 C 0.53652(16) 0.65822(15) 0.51592(9) 0.0323(4) Uani 1 1 d . . . . . H37 H 0.4682 0.6366 0.5120 0.039 Uiso 1 1 calc R U . . . C38 C 0.60250(15) 0.61633(14) 0.57485(8) 0.0261(4) Uani 1 1 d . . . . . C39 C 0.84815(17) 0.75509(15) 0.52715(9) 0.0355(4) Uani 1 1 d . . . . . H39 H 0.8744 0.7387 0.5736 0.043 Uiso 1 1 calc R U . . . C40 C 0.94226(19) 0.69614(18) 0.49568(12) 0.0495(6) Uani 1 1 d . . . . . H40A H 0.9543 0.6227 0.5186 0.074 Uiso 1 1 calc R U . . . H40B H 1.0141 0.7174 0.4982 0.074 Uiso 1 1 calc R U . . . H40C H 0.9188 0.7105 0.4500 0.074 Uiso 1 1 calc R U . . . C41 C 0.8337(2) 0.87076(16) 0.49407(10) 0.0460(5) Uani 1 1 d . . . . . H41A H 0.8181 0.8877 0.4472 0.069 Uiso 1 1 calc R U . . . H41B H 0.9045 0.8901 0.5018 0.069 Uiso 1 1 calc R U . . . H41C H 0.7692 0.9081 0.5121 0.069 Uiso 1 1 calc R U . . . C42 C 0.55812(16) 0.53971(15) 0.62969(10) 0.0348(4) Uani 1 1 d . . . . . H42 H 0.6143 0.5154 0.6682 0.042 Uiso 1 1 calc R U . . . C43 C 0.44042(18) 0.58807(19) 0.64969(11) 0.0467(5) Uani 1 1 d . . . . . H43A H 0.4486 0.6418 0.6675 0.070 Uiso 1 1 calc R U . . . H43B H 0.4117 0.5355 0.6828 0.070 Uiso 1 1 calc R U . . . H43C H 0.3859 0.6177 0.6116 0.070 Uiso 1 1 calc R U . . . C44 C 0.54672(19) 0.44660(17) 0.61050(12) 0.0475(6) Uani 1 1 d . . . . . H44A H 0.4864 0.4681 0.5756 0.071 Uiso 1 1 calc R U . . . H44B H 0.5264 0.3952 0.6483 0.071 Uiso 1 1 calc R U . . . H44C H 0.6202 0.4172 0.5953 0.071 Uiso 1 1 calc R U . . . C45 C 0.81344(16) 0.48185(13) 0.83607(8) 0.0276(4) Uani 1 1 d . . . . . C46 C 0.91164(18) 0.43508(14) 0.87904(9) 0.0340(4) Uani 1 1 d . . . . . C47 C 0.8940(2) 0.40122(16) 0.94556(10) 0.0436(5) Uani 1 1 d . . . . . H47 H 0.9588 0.3685 0.9756 0.052 Uiso 1 1 calc R U . . . C48 C 0.7856(2) 0.41399(17) 0.96869(10) 0.0457(5) Uani 1 1 d . . . . . H48 H 0.7761 0.3915 1.0142 0.055 Uiso 1 1 calc R U . . . C49 C 0.6911(2) 0.45941(16) 0.92573(9) 0.0392(5) Uani 1 1 d . . . . . H49 H 0.6164 0.4673 0.9421 0.047 Uiso 1 1 calc R U . . . C50 C 0.70193(17) 0.49441(14) 0.85846(9) 0.0307(4) Uani 1 1 d . . . . . C51 C 1.03355(18) 0.41943(16) 0.85645(10) 0.0389(5) Uani 1 1 d . . . . . H51 H 1.0302 0.4580 0.8089 0.047 Uiso 1 1 calc R U . . . C52 C 1.11175(19) 0.46007(19) 0.89184(11) 0.0487(6) Uani 1 1 d . . . . . H52A H 1.0789 0.5328 0.8852 0.073 Uiso 1 1 calc R U . . . H52B H 1.1885 0.4514 0.8745 0.073 Uiso 1 1 calc R U . . . H52C H 1.1179 0.4220 0.9385 0.073 Uiso 1 1 calc R U . . . C53 C 1.0874(2) 0.3060(2) 0.86604(15) 0.0649(7) Uani 1 1 d . . . . . H53A H 1.0898 0.2665 0.9123 0.097 Uiso 1 1 calc R U . . . H53B H 1.1658 0.2986 0.8510 0.097 Uiso 1 1 calc R U . . . H53C H 1.0408 0.2807 0.8409 0.097 Uiso 1 1 calc R U . . . C54 C 0.59423(16) 0.54150(14) 0.81326(9) 0.0314(4) Uani 1 1 d . . . . . H54 H 0.6191 0.5591 0.7676 0.038 Uiso 1 1 calc R U . . . C55 C 0.5195(2) 0.4646(2) 0.82135(13) 0.0577(7) Uani 1 1 d . . . . . H55A H 0.5629 0.4051 0.8103 0.087 Uiso 1 1 calc R U . . . H55B H 0.4498 0.4967 0.7924 0.087 Uiso 1 1 calc R U . . . H55C H 0.4978 0.4427 0.8665 0.087 Uiso 1 1 calc R U . . . C56 C 0.5255(2) 0.63993(18) 0.82321(12) 0.0493(6) Uani 1 1 d . . . . . H56A H 0.4951 0.6241 0.8666 0.074 Uiso 1 1 calc R U . . . H56B H 0.4615 0.6719 0.7902 0.074 Uiso 1 1 calc R U . . . H56C H 0.5758 0.6870 0.8193 0.074 Uiso 1 1 calc R U . . . C57 C 0.76044(13) 0.77518(12) 0.73374(8) 0.0207(3) Uani 1 1 d . . . . . C58 C 0.98282(14) 0.52974(13) 0.66157(8) 0.0243(4) Uani 1 1 d . . . . . C59 C 0.63296(16) 0.87149(14) 0.63625(8) 0.0279(4) Uani 1 1 d . . . . . H59 H 0.6989 0.8450 0.6124 0.034 Uiso 1 1 calc R U . . . C60 C 0.5879(2) 0.98496(16) 0.60062(10) 0.0475(6) Uani 1 1 d . . . . . H60A H 0.5309 1.0148 0.6264 0.071 Uiso 1 1 calc R U . . . H60B H 0.5518 0.9943 0.5583 0.071 Uiso 1 1 calc R U . . . H60C H 0.6520 1.0190 0.5942 0.071 Uiso 1 1 calc R U . . . C61 C 0.54094(17) 0.81270(17) 0.63689(11) 0.0409(5) Uani 1 1 d . . . . . H61A H 0.5704 0.7408 0.6627 0.061 Uiso 1 1 calc R U . . . H61B H 0.5209 0.8175 0.5922 0.061 Uiso 1 1 calc R U . . . H61C H 0.4722 0.8420 0.6561 0.061 Uiso 1 1 calc R U . . . C62 C 0.88360(15) 0.71574(13) 0.83516(8) 0.0251(4) Uani 1 1 d . . . . . H62 H 0.9156 0.6565 0.8193 0.030 Uiso 1 1 calc R U . . . C63 C 0.97594(16) 0.77501(15) 0.83223(10) 0.0330(4) Uani 1 1 d . . . . . H63A H 0.9988 0.7986 0.7874 0.049 Uiso 1 1 calc R U . . . H63B H 1.0431 0.7305 0.8605 0.049 Uiso 1 1 calc R U . . . H63C H 0.9454 0.8341 0.8469 0.049 Uiso 1 1 calc R U . . . C64 C 0.84918(17) 0.67481(15) 0.90462(9) 0.0335(4) Uani 1 1 d . . . . . H64A H 0.8200 0.7319 0.9214 0.050 Uiso 1 1 calc R U . . . H64B H 0.9165 0.6283 0.9319 0.050 Uiso 1 1 calc R U . . . H64C H 0.7889 0.6379 0.9053 0.050 Uiso 1 1 calc R U . . . C65 C 1.08177(15) 0.65944(14) 0.67391(9) 0.0288(4) Uani 1 1 d . . . . . H65 H 1.1293 0.6409 0.6392 0.035 Uiso 1 1 calc R U . . . C66 C 1.04121(18) 0.77551(15) 0.65299(11) 0.0386(5) Uani 1 1 d . . . . . H66A H 0.9999 0.8005 0.6102 0.058 Uiso 1 1 calc R U . . . H66B H 1.1080 0.8056 0.6505 0.058 Uiso 1 1 calc R U . . . H66C H 0.9897 0.7951 0.6848 0.058 Uiso 1 1 calc R U . . . C67 C 1.15725(16) 0.61936(16) 0.73689(10) 0.0348(4) Uani 1 1 d . . . . . H67A H 1.1141 0.6411 0.7709 0.052 Uiso 1 1 calc R U . . . H67B H 1.2264 0.6467 0.7297 0.052 Uiso 1 1 calc R U . . . H67C H 1.1798 0.5445 0.7505 0.052 Uiso 1 1 calc R U . . . C68 C 1.18652(15) 0.45030(15) 0.64616(10) 0.0355(4) Uani 1 1 d . . . . . H68 H 1.2112 0.4933 0.6695 0.043 Uiso 1 1 calc R U . . . C69 C 1.21709(18) 0.48361(18) 0.57549(11) 0.0446(5) Uani 1 1 d . . . . . H69A H 1.1832 0.4477 0.5516 0.067 Uiso 1 1 calc R U . . . H69B H 1.3010 0.4671 0.5732 0.067 Uiso 1 1 calc R U . . . H69C H 1.1868 0.5575 0.5560 0.067 Uiso 1 1 calc R U . . . C70 C 1.24261(19) 0.33813(18) 0.67967(13) 0.0512(6) Uani 1 1 d . . . . . H70A H 1.2207 0.3179 0.7249 0.077 Uiso 1 1 calc R U . . . H70B H 1.3266 0.3276 0.6789 0.077 Uiso 1 1 calc R U . . . H70C H 1.2168 0.2966 0.6569 0.077 Uiso 1 1 calc R U . . . N1 N 0.70563(12) 1.02223(11) 0.77959(7) 0.0244(3) Uani 1 1 d . . . . . N2 N 0.53538(12) 0.93437(10) 0.81693(6) 0.0212(3) Uani 1 1 d . . . . . N3 N 0.76966(11) 0.61094(10) 0.64204(6) 0.0203(3) Uani 1 1 d . . . . . N4 N 0.82637(12) 0.51958(10) 0.76671(7) 0.0235(3) Uani 1 1 d . . . . . N5 N 0.67667(12) 0.85664(10) 0.70231(6) 0.0222(3) Uani 1 1 d . . . . . N6 N 0.78270(12) 0.78096(10) 0.79289(6) 0.0216(3) Uani 1 1 d . . . . . N7 N 0.98124(12) 0.61429(11) 0.67959(7) 0.0252(3) Uani 1 1 d . . . . . N8 N 1.06157(13) 0.46154(12) 0.64784(8) 0.0316(4) Uani 1 1 d . . . . . 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 Al1 0.0201(3) 0.0191(3) 0.0216(2) -0.0080(2) 0.00219(19) -0.00653(19) Al2 0.0211(3) 0.0197(3) 0.0225(2) -0.0083(2) -0.00187(19) -0.0044(2) C1 0.0246(9) 0.0221(9) 0.0342(9) -0.0130(7) 0.0036(7) -0.0065(7) C2 0.0239(9) 0.0217(8) 0.0255(8) -0.0101(7) 0.0024(7) -0.0058(7) C3 0.0344(11) 0.0267(10) 0.0632(14) -0.0200(10) 0.0125(10) -0.0134(8) C4 0.0297(10) 0.0318(10) 0.0402(10) -0.0197(9) 0.0079(8) -0.0093(8) C5 0.0225(9) 0.0182(8) 0.0412(10) -0.0132(8) 0.0050(7) -0.0065(7) C6 0.0286(10) 0.0284(10) 0.0445(11) -0.0167(9) 0.0019(8) -0.0080(8) C7 0.0293(10) 0.0340(11) 0.0598(13) -0.0244(10) -0.0026(9) -0.0070(8) C8 0.0247(10) 0.0437(12) 0.0775(16) -0.0311(12) 0.0049(10) -0.0140(9) C9 0.0285(10) 0.0393(11) 0.0605(13) -0.0237(10) 0.0181(9) -0.0153(9) C10 0.0258(9) 0.0247(9) 0.0462(11) -0.0176(8) 0.0104(8) -0.0101(7) C11 0.0409(12) 0.0639(15) 0.0379(11) -0.0173(11) 0.0003(9) -0.0218(11) C12 0.0800(18) 0.0562(15) 0.0408(12) -0.0202(11) -0.0093(12) -0.0176(13) C13 0.077(2) 0.086(2) 0.0562(16) -0.0302(16) 0.0112(14) 0.0126(17) C14 0.0364(11) 0.0367(11) 0.0410(11) -0.0173(9) 0.0150(9) -0.0176(9) C15 0.0715(19) 0.0648(18) 0.080(2) -0.0363(16) -0.0319(15) 0.0220(15) C16 0.0658(17) 0.0607(16) 0.0414(13) -0.0160(12) 0.0117(12) 0.0022(13) C17 0.0225(8) 0.0197(8) 0.0251(8) -0.0083(7) 0.0047(7) -0.0064(7) C18 0.0230(9) 0.0229(9) 0.0295(9) -0.0085(7) 0.0038(7) -0.0073(7) C19 0.0242(9) 0.0320(10) 0.0436(11) -0.0101(9) 0.0022(8) -0.0112(8) C20 0.0273(10) 0.0365(11) 0.0448(11) -0.0058(9) 0.0117(8) -0.0145(8) C21 0.0356(11) 0.0328(10) 0.0284(9) -0.0019(8) 0.0088(8) -0.0101(8) C22 0.0274(9) 0.0257(9) 0.0265(9) -0.0075(7) 0.0051(7) -0.0054(7) C23 0.0227(9) 0.0403(11) 0.0278(9) -0.0118(8) 0.0005(7) -0.0085(8) C24 0.0430(12) 0.0442(12) 0.0298(10) 0.0019(9) -0.0019(9) -0.0126(10) C25 0.0315(11) 0.0581(14) 0.0435(11) -0.0239(10) -0.0049(9) -0.0093(10) C26 0.0297(10) 0.0494(12) 0.0234(9) -0.0071(9) 0.0014(7) -0.0069(9) C27 0.0530(15) 0.0599(16) 0.0366(12) 0.0040(11) -0.0067(10) -0.0014(12) C28 0.0549(15) 0.0787(18) 0.0465(13) -0.0261(13) -0.0054(11) -0.0232(13) C29 0.0204(8) 0.0224(8) 0.0259(8) -0.0099(7) -0.0006(7) -0.0046(7) C30 0.0226(9) 0.0228(9) 0.0290(9) -0.0079(7) -0.0014(7) -0.0059(7) C31 0.0246(9) 0.0292(9) 0.0348(9) -0.0171(8) 0.0010(7) -0.0074(7) C32 0.0569(13) 0.0251(10) 0.0373(10) -0.0087(8) 0.0009(9) -0.0136(9) C33 0.0210(8) 0.0233(8) 0.0223(8) -0.0112(7) -0.0003(6) -0.0016(7) C34 0.0282(9) 0.0283(9) 0.0250(8) -0.0092(7) 0.0010(7) -0.0050(7) C35 0.0427(12) 0.0397(11) 0.0252(9) -0.0026(8) -0.0028(8) -0.0074(9) C36 0.0364(11) 0.0481(12) 0.0293(10) -0.0130(9) -0.0098(8) 0.0023(9) C37 0.0234(9) 0.0414(11) 0.0361(10) -0.0216(9) -0.0051(8) -0.0020(8) C38 0.0219(9) 0.0325(10) 0.0280(9) -0.0168(8) 0.0009(7) -0.0044(7) C39 0.0398(11) 0.0397(11) 0.0265(9) -0.0033(8) 0.0019(8) -0.0187(9) C40 0.0317(11) 0.0495(13) 0.0620(14) -0.0086(11) 0.0075(10) -0.0129(10) C41 0.0600(14) 0.0424(12) 0.0373(11) -0.0069(10) 0.0131(10) -0.0245(11) C42 0.0256(9) 0.0438(11) 0.0385(10) -0.0135(9) -0.0012(8) -0.0145(8) C43 0.0382(12) 0.0671(15) 0.0512(13) -0.0314(12) 0.0135(10) -0.0275(11) C44 0.0350(11) 0.0426(12) 0.0704(15) -0.0199(11) -0.0054(10) -0.0165(10) C45 0.0399(10) 0.0193(8) 0.0228(8) -0.0034(7) -0.0010(7) -0.0096(7) C46 0.0443(12) 0.0245(9) 0.0297(9) -0.0033(8) -0.0056(8) -0.0080(8) C47 0.0603(14) 0.0355(11) 0.0275(10) 0.0022(9) -0.0103(10) -0.0130(10) C48 0.0702(16) 0.0425(12) 0.0228(9) -0.0007(9) 0.0052(10) -0.0238(11) C49 0.0528(13) 0.0385(11) 0.0300(10) -0.0097(9) 0.0104(9) -0.0207(10) C50 0.0416(11) 0.0240(9) 0.0274(9) -0.0061(7) 0.0029(8) -0.0126(8) C51 0.0399(11) 0.0358(11) 0.0326(10) -0.0036(9) -0.0109(9) -0.0017(9) C52 0.0407(12) 0.0512(14) 0.0472(12) -0.0091(11) -0.0145(10) -0.0048(10) C53 0.0604(16) 0.0509(15) 0.0768(18) -0.0235(14) -0.0098(14) 0.0052(13) C54 0.0335(10) 0.0335(10) 0.0289(9) -0.0098(8) 0.0077(8) -0.0123(8) C55 0.0615(16) 0.0544(15) 0.0623(15) -0.0110(12) -0.0028(12) -0.0340(13) C56 0.0461(13) 0.0489(13) 0.0517(13) -0.0202(11) 0.0047(10) -0.0031(11) C57 0.0192(8) 0.0205(8) 0.0235(8) -0.0061(7) 0.0012(6) -0.0081(6) C58 0.0223(9) 0.0249(9) 0.0267(8) -0.0096(7) 0.0003(7) -0.0055(7) C59 0.0291(9) 0.0299(9) 0.0228(8) -0.0109(7) -0.0052(7) 0.0009(7) C60 0.0633(15) 0.0363(12) 0.0337(11) -0.0073(9) -0.0173(10) 0.0025(10) C61 0.0280(10) 0.0564(13) 0.0505(12) -0.0373(11) -0.0025(9) -0.0045(9) C62 0.0252(9) 0.0242(9) 0.0256(8) -0.0093(7) -0.0041(7) -0.0031(7) C63 0.0277(10) 0.0327(10) 0.0421(11) -0.0170(9) -0.0044(8) -0.0065(8) C64 0.0398(11) 0.0328(10) 0.0256(9) -0.0081(8) -0.0051(8) -0.0053(8) C65 0.0217(9) 0.0325(10) 0.0380(10) -0.0156(8) 0.0039(7) -0.0114(7) C66 0.0361(11) 0.0361(11) 0.0487(12) -0.0130(9) -0.0003(9) -0.0190(9) C67 0.0252(10) 0.0389(11) 0.0451(11) -0.0200(9) -0.0028(8) -0.0076(8) C68 0.0205(9) 0.0404(11) 0.0508(12) -0.0242(10) 0.0007(8) -0.0036(8) C69 0.0275(10) 0.0556(14) 0.0560(13) -0.0266(11) 0.0065(9) -0.0083(10) C70 0.0315(11) 0.0493(14) 0.0671(15) -0.0197(12) -0.0015(10) 0.0034(10) N1 0.0202(7) 0.0226(7) 0.0347(8) -0.0126(6) 0.0056(6) -0.0088(6) N2 0.0219(7) 0.0215(7) 0.0238(7) -0.0094(6) 0.0046(6) -0.0094(6) N3 0.0189(7) 0.0198(7) 0.0222(7) -0.0077(6) -0.0010(5) -0.0031(5) N4 0.0259(7) 0.0204(7) 0.0230(7) -0.0051(6) -0.0009(6) -0.0054(6) N5 0.0231(7) 0.0207(7) 0.0224(7) -0.0076(6) -0.0012(6) -0.0034(6) N6 0.0233(7) 0.0218(7) 0.0212(7) -0.0085(6) -0.0007(6) -0.0055(6) N7 0.0200(7) 0.0257(8) 0.0334(8) -0.0123(6) 0.0011(6) -0.0080(6) N8 0.0218(8) 0.0324(8) 0.0435(9) -0.0184(7) 0.0013(7) -0.0034(6) 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' Al Al 0.0645 0.0514 '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' 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 N1 Al1 N2 91.23(6) . . ? N1 Al1 N6 120.97(7) . . ? N2 Al1 N6 129.66(6) . . ? N1 Al1 N5 126.92(7) . . ? N2 Al1 N5 123.39(6) . . ? N6 Al1 N5 69.06(6) . . ? N1 Al1 C57 132.66(6) . . ? N2 Al1 C57 136.11(6) . . ? N6 Al1 C57 34.60(5) . . ? N5 Al1 C57 34.46(5) . . ? N3 Al2 N7 92.64(6) . . ? N3 Al2 N4 87.35(6) . . ? N7 Al2 N4 95.61(6) . . ? N3 Al2 C57 129.37(7) . . ? N7 Al2 C57 127.20(6) . . ? N4 Al2 C57 114.06(7) . . ? N3 Al2 C29 37.68(6) . . ? N7 Al2 C29 67.41(6) . . ? N4 Al2 C29 64.10(6) . . ? C57 Al2 C29 164.77(6) . . ? C2 C1 N1 116.20(14) . . ? C2 C1 C3 124.49(16) . . ? N1 C1 C3 118.62(15) . . ? C1 C2 N2 116.09(15) . . ? C1 C2 C4 123.98(15) . . ? N2 C2 C4 119.90(14) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 119.57(16) . . ? C10 C5 N1 119.35(16) . . ? C6 C5 N1 121.08(16) . . ? C7 C6 C5 119.02(18) . . ? C7 C6 C11 117.71(18) . . ? C5 C6 C11 123.26(16) . . ? C8 C7 C6 121.22(19) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 119.95(18) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 121.18(19) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C5 119.01(18) . . ? C9 C10 C14 119.96(17) . . ? C5 C10 C14 120.98(16) . . ? C6 C11 C12 112.45(19) . . ? C6 C11 C13 112.4(2) . . ? C12 C11 C13 107.79(19) . . ? C6 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? C13 C11 H11 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 110.80(18) . . ? C15 C14 C16 110.6(2) . . ? C10 C14 C16 113.67(18) . . ? C15 C14 H14 107.1 . . ? C10 C14 H14 107.1 . . ? C16 C14 H14 107.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.18(15) . . ? C18 C17 N2 119.78(14) . . ? C22 C17 N2 119.92(15) . . ? C19 C18 C17 118.71(16) . . ? C19 C18 C23 120.60(16) . . ? C17 C18 C23 120.66(15) . . ? C20 C19 C18 121.11(17) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.87(18) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 121.00(17) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 118.57(16) . . ? C21 C22 C26 119.93(16) . . ? C17 C22 C26 121.50(16) . . ? C18 C23 C24 115.00(15) . . ? C18 C23 C25 112.35(16) . . ? C24 C23 C25 109.52(16) . . ? C18 C23 H23 106.5 . . ? C24 C23 H23 106.5 . . ? C25 C23 H23 106.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C28 112.07(18) . . ? C22 C26 C27 112.31(18) . . ? C28 C26 C27 110.62(18) . . ? C22 C26 H26 107.2 . . ? C28 C26 H26 107.2 . . ? C27 C26 H26 107.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C31 114.77(13) . . ? N3 C29 C30 105.01(13) . . ? C31 C29 C30 113.79(14) . . ? N3 C29 C58 109.43(13) . . ? C31 C29 C58 110.30(13) . . ? C30 C29 C58 102.77(12) . . ? N3 C29 Al2 48.15(7) . . ? C31 C29 Al2 162.34(12) . . ? C30 C29 Al2 79.02(9) . . ? C58 C29 Al2 76.74(9) . . ? N4 C30 C32 125.34(16) . . ? N4 C30 C29 112.90(14) . . ? C32 C30 C29 121.76(15) . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 118.45(15) . . ? C34 C33 N3 121.34(14) . . ? C38 C33 N3 120.11(15) . . ? C35 C34 C33 119.25(17) . . ? C35 C34 C39 118.28(16) . . ? C33 C34 C39 122.45(15) . . ? C36 C35 C34 122.17(18) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C37 C36 C35 118.78(17) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 122.06(17) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C37 C38 C33 119.29(16) . . ? C37 C38 C42 117.18(16) . . ? C33 C38 C42 123.53(15) . . ? C34 C39 C40 110.62(16) . . ? C34 C39 C41 113.37(17) . . ? C40 C39 C41 109.83(17) . . ? C34 C39 H39 107.6 . . ? C40 C39 H39 107.6 . . ? C41 C39 H39 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 C43 111.56(17) . . ? C38 C42 C44 111.46(17) . . ? C43 C42 C44 108.56(16) . . ? C38 C42 H42 108.4 . . ? C43 C42 H42 108.4 . . ? C44 C42 H42 108.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 121.80(16) . . ? C50 C45 N4 118.32(15) . . ? C46 C45 N4 119.87(17) . . ? C47 C46 C45 117.39(19) . . ? C47 C46 C51 119.42(18) . . ? C45 C46 C51 123.20(17) . . ? C48 C47 C46 121.8(2) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C49 C48 C47 119.66(19) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 121.7(2) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C49 C50 C45 117.57(18) . . ? C49 C50 C54 119.38(18) . . ? C45 C50 C54 123.04(16) . . ? C46 C51 C52 111.97(18) . . ? C46 C51 C53 111.52(19) . . ? C52 C51 C53 108.95(18) . . ? C46 C51 H51 108.1 . . ? C52 C51 H51 108.1 . . ? C53 C51 H51 108.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 C56 111.88(16) . . ? C50 C54 C55 110.69(17) . . ? C56 C54 C55 110.99(19) . . ? C50 C54 H54 107.7 . . ? C56 C54 H54 107.7 . . ? C55 C54 H54 107.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N5 C57 N6 108.46(14) . . ? N5 C57 Al2 125.99(11) . . ? N6 C57 Al2 125.13(12) . . ? N5 C57 Al1 54.73(8) . . ? N6 C57 Al1 53.74(8) . . ? Al2 C57 Al1 174.04(8) . . ? N8 C58 N7 135.33(16) . . ? N8 C58 C29 113.61(14) . . ? N7 C58 C29 111.02(14) . . ? N5 C59 C60 109.69(14) . . ? N5 C59 C61 111.86(15) . . ? C60 C59 C61 111.22(16) . . ? N5 C59 H59 108.0 . . ? C60 C59 H59 108.0 . . ? C61 C59 H59 108.0 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N6 C62 C64 110.23(14) . . ? N6 C62 C63 110.25(14) . . ? C64 C62 C63 110.77(14) . . ? N6 C62 H62 108.5 . . ? C64 C62 H62 108.5 . . ? C63 C62 H62 108.5 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N7 C65 C66 109.42(14) . . ? N7 C65 C67 112.34(15) . . ? C66 C65 C67 110.63(15) . . ? N7 C65 H65 108.1 . . ? C66 C65 H65 108.1 . . ? C67 C65 H65 108.1 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N8 C68 C70 107.25(17) . . ? N8 C68 C69 108.39(16) . . ? C70 C68 C69 110.76(18) . . ? N8 C68 H68 110.1 . . ? C70 C68 H68 110.1 . . ? C69 C68 H68 110.1 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C5 N1 C1 117.69(13) . . ? C5 N1 Al1 131.55(11) . . ? C1 N1 Al1 107.72(10) . . ? C17 N2 C2 114.73(13) . . ? C17 N2 Al1 137.49(11) . . ? C2 N2 Al1 107.78(10) . . ? C33 N3 C29 119.51(12) . . ? C33 N3 Al2 142.32(11) . . ? C29 N3 Al2 94.17(9) . . ? C30 N4 C45 120.54(14) . . ? C30 N4 Al2 103.94(11) . . ? C45 N4 Al2 135.52(11) . . ? C57 N5 C59 121.25(14) . . ? C57 N5 Al1 90.82(10) . . ? C59 N5 Al1 147.93(11) . . ? C57 N6 C62 122.88(14) . . ? C57 N6 Al1 91.67(10) . . ? C62 N6 Al1 143.66(11) . . ? C58 N7 C65 121.92(14) . . ? C58 N7 Al2 104.43(11) . . ? C65 N7 Al2 133.45(11) . . ? C58 N8 C68 130.25(16) . . ? 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 Al1 N1 1.8255(14) . ? Al1 N2 1.8256(15) . ? Al1 N6 1.9125(15) . ? Al1 N5 1.9358(14) . ? Al1 C57 2.3709(17) . ? Al2 N3 1.8250(14) . ? Al2 N7 1.8876(15) . ? Al2 N4 1.9784(15) . ? Al2 C57 2.0371(17) . ? Al2 C29 2.4436(17) . ? C1 C2 1.344(2) . ? C1 N1 1.434(2) . ? C1 C3 1.508(2) . ? C2 N2 1.436(2) . ? C2 C4 1.508(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.404(3) . ? C5 C6 1.420(3) . ? C5 N1 1.428(2) . ? C6 C7 1.392(3) . ? C6 C11 1.522(3) . ? C7 C8 1.376(3) . ? C7 H7 0.9500 . ? C8 C9 1.376(3) . ? C8 H8 0.9500 . ? C9 C10 1.401(3) . ? C9 H9 0.9500 . ? C10 C14 1.515(3) . ? C11 C12 1.523(3) . ? C11 C13 1.529(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.489(3) . ? C14 C16 1.519(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.404(2) . ? C17 C22 1.409(2) . ? C17 N2 1.435(2) . ? C18 C19 1.393(2) . ? C18 C23 1.524(2) . ? C19 C20 1.378(3) . ? C19 H19 0.9500 . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.395(3) . ? C21 H21 0.9500 . ? C22 C26 1.514(2) . ? C23 C24 1.527(3) . ? C23 C25 1.531(3) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.527(3) . ? C26 C27 1.529(3) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N3 1.498(2) . ? C29 C31 1.518(2) . ? C29 C30 1.536(2) . ? C29 C58 1.596(2) . ? C30 N4 1.316(2) . ? C30 C32 1.457(2) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.414(2) . ? C33 C38 1.418(2) . ? C33 N3 1.429(2) . ? C34 C35 1.391(2) . ? C34 C39 1.517(3) . ? C35 C36 1.378(3) . ? C35 H35 0.9500 . ? C36 C37 1.364(3) . ? C36 H36 0.9500 . ? C37 C38 1.397(2) . ? C37 H37 0.9500 . ? C38 C42 1.518(3) . ? C39 C40 1.527(3) . ? C39 C41 1.539(3) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.536(3) . ? C42 C44 1.539(3) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.401(3) . ? C45 C46 1.407(3) . ? C45 N4 1.448(2) . ? C46 C47 1.399(3) . ? C46 C51 1.518(3) . ? C47 C48 1.374(3) . ? C47 H47 0.9500 . ? C48 C49 1.373(3) . ? C48 H48 0.9500 . ? C49 C50 1.400(3) . ? C49 H49 0.9500 . ? C50 C54 1.518(3) . ? C51 C52 1.532(3) . ? C51 C53 1.537(3) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C56 1.526(3) . ? C54 C55 1.529(3) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N5 1.342(2) . ? C57 N6 1.347(2) . ? C58 N8 1.290(2) . ? C58 N7 1.370(2) . ? C59 N5 1.469(2) . ? C59 C60 1.520(3) . ? C59 C61 1.522(3) . ? C59 H59 1.0000 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 N6 1.464(2) . ? C62 C64 1.521(2) . ? C62 C63 1.522(2) . ? C62 H62 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 N7 1.471(2) . ? C65 C66 1.524(3) . ? C65 C67 1.525(3) . ? C65 H65 1.0000 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 N8 1.465(2) . ? C68 C70 1.519(3) . ? C68 C69 1.520(3) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ?