#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:26:23 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541905.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_1541905 loop_ _publ_author_name 'Loewen, Natalia D.' 'Thompson, Emily J.' 'Kagan, Michael' 'Banales, Carolina L.' 'Myers, Thomas W.' 'Fettinger, James C.' 'Berben, Louise' _publ_section_title ; A Pendant Proton Shuttle on [Fe4N(CO)12]- Alters Product Selectivity in Formate vs. H2 Production via the Hydride [H-Fe4N(CO)12]- ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C5SC03169A _journal_year 2016 _chemical_formula_moiety 'C59 H60 Al F6 N3 O2' _chemical_formula_sum 'C59 H60 Al F6 N3 O2' _chemical_formula_weight 984.08 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2015-08-06 deposited with the CCDC. 2016-01-05 downloaded from the CCDC. ; _cell_angle_alpha 73.0848(12) _cell_angle_beta 88.2081(14) _cell_angle_gamma 86.3652(14) _cell_formula_units_Z 2 _cell_length_a 10.2264(3) _cell_length_b 15.4589(4) _cell_length_c 17.0819(4) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 69.12 _cell_measurement_theta_min 4.58 _cell_volume 2578.20(12) _computing_cell_refinement 'SAINT (8.34a) (Bruker, 2013)' _computing_data_collection 'Apex2 (2014.9-1) (Bruker, 2014)' _computing_data_reduction 'SAINT (8.34a) (Bruker, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 90(2) _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_unetI/netI 0.0598 _diffrn_reflns_laue_measured_fraction_full 0.962 _diffrn_reflns_laue_measured_fraction_max 0.955 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 15576 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.955 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 69.127 _diffrn_reflns_theta_min 4.581 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_correction_T_min 0.5678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS V2012/1 (Sheldrick, 2012)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.268 _exptl_crystal_description Plate _exptl_crystal_F_000 1036 _exptl_crystal_size_max 0.446 _exptl_crystal_size_mid 0.237 _exptl_crystal_size_min 0.036 _refine_diff_density_max 0.437 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 712 _refine_ls_number_reflns 15576 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0470 _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^)+(0.0736P)^2^+0.7093P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1258 _refine_ls_wR_factor_ref 0.1293 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14420 _reflns_number_total 15576 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc03169a2.cif _cod_data_source_block TS14TW51 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_database_code 1541905 _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 0.688 _shelx_estimated_absorpt_t_max 0.968 _shelx_res_file ; TS14TW51.res created by SHELXL-2014/7 TITL TS14F in P-1 FINAL 2COMP 4MAR2015 CELL 1.54178 10.2264 15.4589 17.0819 73.0848 88.2081 86.3652 ZERR 2.00 0.0003 0.0004 0.0004 0.0012 0.0014 0.0014 LATT 1 SFAC C H N O F Al UNIT 118 120 6 4 12 2 MERG 0 L.S. 9 ACTA BOND $H FMAP 2 PLAN 12 HTAB HTAB N3 O2 SIZE 0.036 0.237 0.446 ! BLUE PLATE WPDB -2 CONF TEMP -183.000 WGHT 0.073600 0.709300 BASF 0.29002 FVAR 0.49443 AL1 6 0.944633 0.821112 0.223449 11.00000 0.02132 0.02299 = 0.01955 -0.00426 0.00048 -0.00004 C1 1 0.912134 0.641567 0.177571 11.00000 0.02424 0.02395 = 0.02516 -0.00809 0.00335 -0.00068 N1 3 0.997395 0.713627 0.175092 11.00000 0.02416 0.02193 = 0.02020 -0.00412 -0.00158 0.00043 O1 4 0.859562 0.758803 0.307611 11.00000 0.02590 0.02978 = 0.02413 -0.00564 0.00294 -0.00520 C2 1 0.813443 0.658225 0.118811 11.00000 0.02481 0.02910 = 0.02682 -0.01188 0.00346 -0.00116 N2 3 1.120889 0.843229 0.193788 11.00000 0.02294 0.02475 = 0.02224 -0.00517 0.00027 -0.00051 O2 4 0.839230 0.888039 0.149574 11.00000 0.02506 0.02568 = 0.02324 -0.00498 -0.00127 0.00042 C3 1 0.727681 0.590409 0.124519 11.00000 0.02722 0.03979 = 0.03363 -0.01543 0.00172 -0.00527 AFIX 43 H3 2 0.660343 0.599851 0.085347 11.00000 0.02442 AFIX 0 N3 3 0.973791 0.932392 0.274368 11.00000 0.02129 0.02545 = 0.02024 -0.00522 -0.00089 -0.00113 H3A 2 0.906003 0.963630 0.244267 11.00000 0.02700 C4 1 0.738529 0.509501 0.186110 11.00000 0.03156 0.03458 = 0.04341 -0.01549 0.00736 -0.01171 AFIX 43 H4 2 0.678672 0.464061 0.189088 11.00000 0.04991 AFIX 0 C5 1 0.836212 0.494475 0.243408 11.00000 0.03612 0.02649 = 0.03458 -0.00600 0.00868 -0.00452 AFIX 43 H5 2 0.842498 0.438573 0.285519 11.00000 0.03594 AFIX 0 C6 1 0.925419 0.559463 0.240682 11.00000 0.02846 0.02744 = 0.02762 -0.00812 0.00551 -0.00037 C7 1 0.797443 0.746582 0.049762 11.00000 0.02598 0.02973 = 0.02842 -0.00854 -0.00307 0.00045 AFIX 13 H7 2 0.866804 0.786991 0.055585 11.00000 0.01842 AFIX 0 C8 1 0.663930 0.794805 0.055905 11.00000 0.03053 0.04016 = 0.03634 -0.01436 -0.00663 0.00448 AFIX 137 H8A 2 0.594404 0.757665 0.047633 11.00000 0.03126 H8B 2 0.658441 0.853559 0.013859 11.00000 0.04545 H8C 2 0.653383 0.804097 0.110159 11.00000 0.03575 AFIX 0 C9 1 0.813921 0.731450 -0.035217 11.00000 0.03389 0.03918 = 0.02796 -0.01049 -0.00354 0.00065 AFIX 137 H9A 2 0.899846 0.701045 -0.039239 11.00000 0.04212 H9B 2 0.807497 0.789999 -0.077511 11.00000 0.04838 H9C 2 0.744916 0.693667 -0.043025 11.00000 0.02942 AFIX 0 C10 1 1.028885 0.538548 0.306085 11.00000 0.03376 0.02608 = 0.02968 -0.00070 -0.00079 -0.00035 AFIX 13 H10 2 1.087513 0.590366 0.293518 11.00000 0.02560 AFIX 0 C11 1 1.113116 0.452503 0.306619 11.00000 0.04353 0.03114 = 0.04276 0.00051 -0.00182 0.00557 AFIX 137 H11A 2 1.060206 0.399577 0.326481 11.00000 0.05401 H11B 2 1.187912 0.446214 0.342740 11.00000 0.05569 H11C 2 1.144968 0.456822 0.250978 11.00000 0.05058 AFIX 0 C12 1 0.967315 0.528054 0.391091 11.00000 0.05100 0.03571 = 0.02809 -0.00219 -0.00201 -0.00393 AFIX 137 H12A 2 0.919617 0.584839 0.391824 11.00000 0.04639 H12B 2 1.036434 0.513448 0.432118 11.00000 0.04334 H12C 2 0.906533 0.479166 0.403675 11.00000 0.03700 AFIX 0 C13 1 1.119593 0.709421 0.153056 11.00000 0.02416 0.02456 = 0.01784 -0.00276 -0.00124 0.00176 C14 1 1.187750 0.633151 0.128581 11.00000 0.02359 0.02386 = 0.02627 -0.00434 0.00359 -0.00004 C15 1 1.131365 0.594443 0.074171 11.00000 0.02513 0.02992 = 0.03422 -0.00928 0.00142 -0.00021 AFIX 43 H15 2 1.049080 0.618429 0.050594 11.00000 0.03167 AFIX 0 C16 1 1.194090 0.521707 0.054371 11.00000 0.03706 0.03556 = 0.04730 -0.01990 0.00352 -0.00311 AFIX 43 H16 2 1.155840 0.496787 0.016399 11.00000 0.04824 AFIX 0 C17 1 1.312654 0.485052 0.089788 11.00000 0.03711 0.02909 = 0.05711 -0.01599 0.00752 0.00398 AFIX 43 H17 2 1.355185 0.434448 0.076779 11.00000 0.04591 AFIX 0 C18 1 1.368831 0.522146 0.143959 11.00000 0.02764 0.03443 = 0.04570 -0.00450 0.00178 0.00617 AFIX 43 H18 2 1.449985 0.496717 0.168410 11.00000 0.04205 AFIX 0 C19 1 1.307732 0.596483 0.163131 11.00000 0.02844 0.03228 = 0.03231 -0.00698 -0.00075 0.00043 AFIX 43 H19 2 1.347891 0.622257 0.199827 11.00000 0.02673 AFIX 0 C20 1 1.191580 0.788627 0.155076 11.00000 0.02328 0.02560 = 0.02118 -0.00546 -0.00205 0.00207 C21 1 1.307636 0.810360 0.116538 11.00000 0.02398 0.03160 = 0.02912 -0.01147 0.00125 0.00091 AFIX 43 H21 2 1.355971 0.769866 0.092497 11.00000 0.02597 AFIX 0 C22 1 1.355081 0.896362 0.113219 11.00000 0.02500 0.03718 = 0.03138 -0.01060 0.00555 -0.00653 AFIX 43 H22 2 1.434309 0.914667 0.084356 11.00000 0.03602 AFIX 0 C23 1 1.288765 0.951949 0.150576 11.00000 0.02839 0.02836 = 0.02982 -0.00852 0.00133 -0.00554 AFIX 43 H23 2 1.320769 1.009480 0.146515 11.00000 0.02821 AFIX 0 C24 1 1.169341 0.924930 0.196800 11.00000 0.02493 0.02475 = 0.02274 -0.00476 -0.00170 -0.00227 C25 1 1.097612 0.972609 0.240817 11.00000 0.02195 0.02684 = 0.02203 -0.00448 -0.00143 -0.00203 C26 1 1.130634 1.059615 0.252269 11.00000 0.02653 0.02601 = 0.01853 -0.00512 0.00152 -0.00219 C27 1 1.259473 1.075988 0.267405 11.00000 0.02534 0.03048 = 0.02680 -0.00849 -0.00015 0.00114 AFIX 43 H27 2 1.325882 1.028742 0.273588 11.00000 0.02649 AFIX 0 C28 1 1.292206 1.159185 0.273546 11.00000 0.02806 0.03594 = 0.02953 -0.00994 0.00092 -0.00585 AFIX 43 H28 2 1.380500 1.168722 0.282943 11.00000 0.03276 AFIX 0 C29 1 1.196273 1.228960 0.266011 11.00000 0.03799 0.02692 = 0.03049 -0.01016 0.00142 -0.00502 AFIX 43 H29 2 1.218828 1.286629 0.268872 11.00000 0.03147 AFIX 0 C30 1 1.068496 1.213445 0.254380 11.00000 0.03743 0.02753 = 0.02818 -0.00725 -0.00159 0.00364 AFIX 43 H30 2 1.002138 1.260279 0.250700 11.00000 0.03037 AFIX 0 C31 1 1.035221 1.130014 0.247938 11.00000 0.02375 0.03145 = 0.02486 -0.00828 -0.00197 0.00039 AFIX 43 H31 2 0.946158 1.120525 0.240460 11.00000 0.02488 AFIX 0 C32 1 0.946197 0.924782 0.360732 11.00000 0.02587 0.02630 = 0.02126 -0.00651 0.00021 -0.00400 C33 1 0.833951 0.970816 0.382525 11.00000 0.02479 0.02949 = 0.02691 -0.00861 0.00058 -0.00253 C34 1 0.810266 0.961771 0.465240 11.00000 0.02852 0.03648 = 0.03021 -0.01324 0.00428 -0.00317 AFIX 43 H34 2 0.734567 0.991909 0.480959 11.00000 0.02990 AFIX 0 C35 1 0.894313 0.909970 0.525024 11.00000 0.03974 0.03998 = 0.02198 -0.00940 0.00264 -0.00835 AFIX 43 H35 2 0.877793 0.905970 0.580970 11.00000 0.03026 AFIX 0 C36 1 1.001832 0.864427 0.502576 11.00000 0.03408 0.03357 = 0.02405 -0.00367 -0.00482 -0.00416 AFIX 43 H36 2 1.058525 0.828233 0.543921 11.00000 0.03693 AFIX 0 C37 1 1.030655 0.869576 0.420769 11.00000 0.02722 0.02699 = 0.02498 -0.00594 -0.00186 -0.00469 C38 1 0.732534 1.025075 0.321081 11.00000 0.02457 0.03838 = 0.02688 -0.01023 0.00105 0.00381 AFIX 13 H38 2 0.774493 1.039362 0.265461 11.00000 0.02711 AFIX 0 C39 1 0.686620 1.115386 0.336752 11.00000 0.04582 0.04556 = 0.03905 -0.01502 -0.00494 0.01648 AFIX 137 H39A 2 0.636377 1.103363 0.388225 11.00000 0.04528 H39B 2 0.631180 1.151179 0.291661 11.00000 0.04467 H39C 2 0.763061 1.149134 0.340350 11.00000 0.08491 AFIX 0 C40 1 0.616494 0.967367 0.321024 11.00000 0.02797 0.05286 = 0.04440 -0.00772 -0.00458 -0.00149 AFIX 137 H40A 2 0.647497 0.912409 0.306929 11.00000 0.04437 H40B 2 0.552514 1.002079 0.280630 11.00000 0.04792 H40C 2 0.575113 0.950633 0.375475 11.00000 0.06507 AFIX 0 C41 1 1.146881 0.812664 0.401936 11.00000 0.03164 0.03065 = 0.02663 -0.00445 -0.00555 0.00359 AFIX 13 H41 2 1.148960 0.820983 0.341632 11.00000 0.03497 AFIX 0 C42 1 1.276497 0.843514 0.424734 11.00000 0.03299 0.03736 = 0.04113 -0.00739 -0.00565 0.00189 AFIX 137 H42A 2 1.283828 0.908058 0.396592 11.00000 0.05864 H42B 2 1.349925 0.808573 0.408136 11.00000 0.05543 H42C 2 1.278481 0.833606 0.484030 11.00000 0.04871 AFIX 0 C43 1 1.132606 0.711865 0.445320 11.00000 0.04254 0.03153 = 0.04661 -0.00760 -0.00938 0.00261 AFIX 137 H43A 2 1.138438 0.700994 0.504592 11.00000 0.04193 H43B 2 1.202802 0.676007 0.426779 11.00000 0.04059 H43C 2 1.047451 0.694137 0.432332 11.00000 0.04534 AFIX 0 C44 1 0.735333 0.724336 0.309608 11.00000 0.02985 0.03164 = 0.02769 -0.00865 0.00192 -0.00592 AFIX 23 H44A 2 0.743572 0.669056 0.291291 11.00000 0.03450 H44B 2 0.677382 0.769601 0.270939 11.00000 0.03125 AFIX 0 C45 1 0.673408 0.701689 0.394225 11.00000 0.02418 0.02562 = 0.02799 -0.00438 0.00229 0.00083 C46 1 0.716868 0.736821 0.454140 11.00000 0.02879 0.03148 = 0.02895 -0.00497 0.00403 -0.00740 AFIX 43 H46 2 0.788889 0.774693 0.442671 11.00000 0.02877 AFIX 0 C47 1 0.656173 0.717241 0.530945 11.00000 0.03655 0.03378 = 0.02544 -0.00708 0.00128 -0.00365 AFIX 43 H47 2 0.685778 0.742297 0.571384 11.00000 0.03490 AFIX 0 C48 1 0.552745 0.661199 0.547899 11.00000 0.02883 0.03037 = 0.02628 -0.00158 0.00363 -0.00051 C49 1 0.508880 0.624652 0.488616 11.00000 0.02830 0.03414 = 0.03336 -0.00532 0.00429 -0.00728 AFIX 43 H49 2 0.437731 0.586024 0.500417 11.00000 0.03777 AFIX 0 C50 1 0.569589 0.644960 0.412412 11.00000 0.03205 0.03349 = 0.03119 -0.00975 0.00223 -0.00531 AFIX 43 H50 2 0.539945 0.619822 0.372039 11.00000 0.03135 AFIX 0 C51 1 0.485839 0.637972 0.629719 11.00000 0.03463 0.04084 = 0.03250 -0.00400 0.00474 -0.00464 F51 5 0.358739 0.665117 0.625734 11.00000 0.04018 0.10219 = 0.03971 -0.00701 0.01300 0.00387 C52 1 0.871400 0.958749 0.080185 11.00000 0.03070 0.02954 = 0.02083 -0.00475 -0.00063 0.00253 AFIX 23 H52A 2 0.844975 0.944675 0.030177 11.00000 0.02609 H52B 2 0.967370 0.964745 0.077363 11.00000 0.04047 AFIX 0 F52 5 0.537849 0.672809 0.683135 11.00000 0.06525 0.07451 = 0.03332 -0.02127 0.01700 -0.02950 C53 1 0.802486 1.046806 0.084198 11.00000 0.02859 0.02963 = 0.01863 -0.00381 -0.00494 0.00190 F53 5 0.489258 0.548288 0.665601 11.00000 0.09046 0.04407 = 0.03614 0.00058 0.01893 -0.01507 C54 1 0.669245 1.049676 0.101228 11.00000 0.02668 0.03055 = 0.03264 -0.00615 -0.00373 -0.00146 AFIX 43 H54 2 0.622415 0.996604 0.109006 11.00000 0.03915 AFIX 0 C55 1 0.603249 1.128412 0.107102 11.00000 0.02865 0.03542 = 0.03269 -0.00717 -0.00203 0.00340 AFIX 43 H55 2 0.511565 1.129720 0.117904 11.00000 0.03771 AFIX 0 C56 1 0.671972 1.205513 0.097096 11.00000 0.03551 0.03109 = 0.02455 -0.00553 -0.00512 0.00553 C57 1 0.805767 1.203440 0.081362 11.00000 0.03990 0.02820 = 0.02863 -0.00534 -0.00321 -0.00305 AFIX 43 H57 2 0.853005 1.256017 0.075324 11.00000 0.03713 AFIX 0 C58 1 0.870385 1.124310 0.074472 11.00000 0.03000 0.03235 = 0.02563 -0.00282 -0.00217 -0.00056 AFIX 43 H58 2 0.961872 1.123126 0.063001 11.00000 0.03899 AFIX 0 C59 1 0.600969 1.291381 0.101193 11.00000 0.04462 0.03568 = 0.03590 -0.01087 -0.00191 0.00512 F59 5 0.547594 1.337730 0.028938 11.00000 0.05781 0.03605 = 0.04279 -0.00207 -0.00136 0.01482 F60 5 0.677495 1.348492 0.119299 11.00000 0.07478 0.05810 = 0.11398 -0.05679 -0.02981 0.01391 F61 5 0.501158 1.277950 0.154253 11.00000 0.08553 0.04653 = 0.05163 0.00010 0.02879 0.02412 HKLF 5 REM TS14F in P-1 FINAL 2COMP 4MAR2015 REM R1 = 0.0470 for 14420 Fo > 4sig(Fo) and 0.0505 for all 15576 data REM 712 parameters refined using 0 restraints END WGHT 0.0736 0.7093 REM Instructions for potential hydrogen bonds HTAB N3 O2 REM Highest difference peak 0.437, deepest hole -0.309, 1-sigma level 0.051 Q1 1 0.6107 1.3610 0.0582 11.00000 0.05 0.44 Q2 1 0.9550 0.7714 0.1913 11.00000 0.05 0.40 Q3 1 1.1108 1.0154 0.2449 11.00000 0.05 0.32 Q4 1 0.6328 1.3093 0.1810 11.00000 0.05 0.31 Q5 1 0.9682 0.8766 0.2506 11.00000 0.05 0.29 Q6 1 1.1623 0.6750 0.1380 11.00000 0.05 0.26 Q7 1 1.1627 0.7572 0.1403 11.00000 0.05 0.25 Q8 1 0.9007 0.5209 0.2277 11.00000 0.05 0.25 Q9 1 0.8766 0.8408 0.1687 11.00000 0.05 0.24 Q10 1 1.0574 1.1813 0.2380 11.00000 0.05 0.23 Q11 1 1.1823 1.0620 0.2651 11.00000 0.05 0.23 Q12 1 1.1874 1.0753 0.2367 11.00000 0.05 0.23 ; _shelx_res_checksum 6500 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 Al1 Al 0.94463(6) 0.82111(4) 0.22345(3) 0.02176(14) Uani 1 1 d . C1 C 0.9121(2) 0.64157(13) 0.17757(11) 0.0244(4) Uani 1 1 d . N1 N 0.99739(17) 0.71363(10) 0.17509(9) 0.0226(4) Uani 1 1 d . O1 O 0.85956(15) 0.75880(9) 0.30761(8) 0.0270(3) Uani 1 1 d . C2 C 0.8134(2) 0.65822(13) 0.11881(12) 0.0262(4) Uani 1 1 d . N2 N 1.12089(17) 0.84323(11) 0.19379(9) 0.0237(3) Uani 1 1 d . O2 O 0.83923(14) 0.88804(9) 0.14957(8) 0.0252(3) Uani 1 1 d . C3 C 0.7277(2) 0.59041(15) 0.12452(13) 0.0324(5) Uani 1 1 d . H3 H 0.6603 0.5999 0.0853 0.024(5) Uiso 1 1 calc R N3 N 0.97379(18) 0.93239(11) 0.27437(9) 0.0226(3) Uani 1 1 d . H3A H 0.906(2) 0.9636(16) 0.2443(15) 0.027(6) Uiso 1 1 d . C4 C 0.7385(2) 0.50950(15) 0.18611(14) 0.0354(5) Uani 1 1 d . H4 H 0.6787 0.4641 0.1891 0.050(8) Uiso 1 1 calc R C5 C 0.8362(2) 0.49448(14) 0.24341(13) 0.0331(5) Uani 1 1 d . H5 H 0.8425 0.4386 0.2855 0.036(6) Uiso 1 1 calc R C6 C 0.9254(2) 0.55946(13) 0.24068(12) 0.0280(4) Uani 1 1 d . C7 C 0.7974(2) 0.74658(14) 0.04976(12) 0.0280(4) Uani 1 1 d . H7 H 0.8668 0.7870 0.0556 0.018(5) Uiso 1 1 calc R C8 C 0.6639(2) 0.79481(16) 0.05590(14) 0.0351(5) Uani 1 1 d . H8A H 0.5944 0.7577 0.0476 0.031(6) Uiso 1 1 calc R H8B H 0.6584 0.8536 0.0139 0.045(7) Uiso 1 1 calc R H8C H 0.6534 0.8041 0.1102 0.036(6) Uiso 1 1 calc R C9 C 0.8139(2) 0.73145(15) -0.03522(13) 0.0336(5) Uani 1 1 d . H9A H 0.8998 0.7010 -0.0392 0.042(7) Uiso 1 1 calc R H9B H 0.8075 0.7900 -0.0775 0.048(8) Uiso 1 1 calc R H9C H 0.7449 0.6937 -0.0430 0.029(6) Uiso 1 1 calc R C10 C 1.0289(2) 0.53855(14) 0.30608(13) 0.0315(5) Uani 1 1 d . H10 H 1.0875 0.5904 0.2935 0.026(6) Uiso 1 1 calc R C11 C 1.1131(3) 0.45250(15) 0.30662(15) 0.0418(6) Uani 1 1 d . H11A H 1.0602 0.3996 0.3265 0.054(8) Uiso 1 1 calc R H11B H 1.1879 0.4462 0.3427 0.056(8) Uiso 1 1 calc R H11C H 1.1450 0.4568 0.2510 0.051(8) Uiso 1 1 calc R C12 C 0.9673(3) 0.52805(16) 0.39109(13) 0.0397(6) Uani 1 1 d . H12A H 0.9196 0.5848 0.3918 0.046(7) Uiso 1 1 calc R H12B H 1.0364 0.5134 0.4321 0.043(7) Uiso 1 1 calc R H12C H 0.9065 0.4792 0.4037 0.037(7) Uiso 1 1 calc R C13 C 1.1196(2) 0.70942(12) 0.15306(11) 0.0230(4) Uani 1 1 d . C14 C 1.1878(2) 0.63315(13) 0.12858(12) 0.0253(4) Uani 1 1 d . C15 C 1.1314(2) 0.59444(14) 0.07417(13) 0.0299(5) Uani 1 1 d . H15 H 1.0491 0.6184 0.0506 0.032(6) Uiso 1 1 calc R C16 C 1.1941(3) 0.52171(15) 0.05437(15) 0.0383(5) Uani 1 1 d . H16 H 1.1558 0.4968 0.0164 0.048(8) Uiso 1 1 calc R C17 C 1.3127(3) 0.48505(15) 0.08979(16) 0.0408(6) Uani 1 1 d . H17 H 1.3552 0.4344 0.0768 0.046(7) Uiso 1 1 calc R C18 C 1.3688(2) 0.52215(15) 0.14396(15) 0.0378(5) Uani 1 1 d . H18 H 1.4500 0.4967 0.1684 0.042(7) Uiso 1 1 calc R C19 C 1.3077(2) 0.59648(14) 0.16313(13) 0.0316(5) Uani 1 1 d . H19 H 1.3479 0.6223 0.1998 0.027(6) Uiso 1 1 calc R C20 C 1.1916(2) 0.78863(13) 0.15508(11) 0.0237(4) Uani 1 1 d . C21 C 1.3076(2) 0.81036(14) 0.11654(12) 0.0278(4) Uani 1 1 d . H21 H 1.3560 0.7699 0.0925 0.026(6) Uiso 1 1 calc R C22 C 1.3551(2) 0.89636(15) 0.11322(13) 0.0310(5) Uani 1 1 d . H22 H 1.4343 0.9147 0.0844 0.036(6) Uiso 1 1 calc R C23 C 1.2888(2) 0.95195(14) 0.15058(12) 0.0287(4) Uani 1 1 d . H23 H 1.3208 1.0095 0.1465 0.028(6) Uiso 1 1 calc R C24 C 1.1693(2) 0.92493(13) 0.19680(11) 0.0245(4) Uani 1 1 d . C25 C 1.0976(2) 0.97261(13) 0.24082(11) 0.0241(4) Uani 1 1 d . C26 C 1.1306(2) 1.05962(13) 0.25227(11) 0.0240(4) Uani 1 1 d . C27 C 1.2595(2) 1.07599(14) 0.26740(12) 0.0276(4) Uani 1 1 d . H27 H 1.3259 1.0287 0.2736 0.026(6) Uiso 1 1 calc R C28 C 1.2922(2) 1.15918(14) 0.27355(12) 0.0309(5) Uani 1 1 d . H28 H 1.3805 1.1687 0.2829 0.033(6) Uiso 1 1 calc R C29 C 1.1963(2) 1.22896(14) 0.26601(12) 0.0313(5) Uani 1 1 d . H29 H 1.2188 1.2866 0.2689 0.031(6) Uiso 1 1 calc R C30 C 1.0685(2) 1.21345(14) 0.25438(12) 0.0314(5) Uani 1 1 d . H30 H 1.0021 1.2603 0.2507 0.030(6) Uiso 1 1 calc R C31 C 1.0352(2) 1.13001(13) 0.24794(11) 0.0267(4) Uani 1 1 d . H31 H 0.9462 1.1205 0.2405 0.025(6) Uiso 1 1 calc R C32 C 0.9462(2) 0.92478(13) 0.36073(11) 0.0245(4) Uani 1 1 d . C33 C 0.8340(2) 0.97082(13) 0.38253(12) 0.0269(4) Uani 1 1 d . C34 C 0.8103(2) 0.96177(14) 0.46524(13) 0.0310(5) Uani 1 1 d . H34 H 0.7346 0.9919 0.4810 0.030(6) Uiso 1 1 calc R C35 C 0.8943(2) 0.90997(15) 0.52502(12) 0.0336(5) Uani 1 1 d . H35 H 0.8778 0.9060 0.5810 0.030(6) Uiso 1 1 calc R C36 C 1.0018(2) 0.86443(14) 0.50258(12) 0.0314(5) Uani 1 1 d . H36 H 1.0585 0.8282 0.5439 0.037(7) Uiso 1 1 calc R C37 C 1.0307(2) 0.86958(13) 0.42077(12) 0.0266(4) Uani 1 1 d . C38 C 0.7325(2) 1.02507(14) 0.32108(12) 0.0301(5) Uani 1 1 d . H38 H 0.7745 1.0394 0.2655 0.027(6) Uiso 1 1 calc R C39 C 0.6866(3) 1.11539(17) 0.33675(15) 0.0436(6) Uani 1 1 d . H39A H 0.6364 1.1034 0.3882 0.045(7) Uiso 1 1 calc R H39B H 0.6312 1.1512 0.2917 0.045(7) Uiso 1 1 calc R H39C H 0.7631 1.1491 0.3403 0.085(12) Uiso 1 1 calc R C40 C 0.6165(3) 0.96737(18) 0.32102(16) 0.0430(6) Uani 1 1 d . H40A H 0.6475 0.9124 0.3069 0.044(7) Uiso 1 1 calc R H40B H 0.5525 1.0021 0.2806 0.048(7) Uiso 1 1 calc R H40C H 0.5751 0.9506 0.3755 0.065(9) Uiso 1 1 calc R C41 C 1.1469(2) 0.81266(14) 0.40194(12) 0.0306(5) Uani 1 1 d . H41 H 1.1490 0.8210 0.3416 0.035(6) Uiso 1 1 calc R C42 C 1.2765(2) 0.84351(16) 0.42473(15) 0.0381(5) Uani 1 1 d . H42A H 1.2838 0.9081 0.3966 0.059(9) Uiso 1 1 calc R H42B H 1.3499 0.8086 0.4081 0.055(8) Uiso 1 1 calc R H42C H 1.2785 0.8336 0.4840 0.049(8) Uiso 1 1 calc R C43 C 1.1326(3) 0.71186(15) 0.44532(15) 0.0410(6) Uani 1 1 d . H43A H 1.1384 0.7010 0.5046 0.042(7) Uiso 1 1 calc R H43B H 1.2028 0.6760 0.4268 0.041(7) Uiso 1 1 calc R H43C H 1.0475 0.6941 0.4323 0.045(7) Uiso 1 1 calc R C44 C 0.7353(2) 0.72434(14) 0.30961(12) 0.0296(5) Uani 1 1 d . H44A H 0.7436 0.6691 0.2913 0.035(6) Uiso 1 1 calc R H44B H 0.6774 0.7696 0.2709 0.031(6) Uiso 1 1 calc R C45 C 0.6734(2) 0.70169(13) 0.39423(12) 0.0268(4) Uani 1 1 d . C46 C 0.7169(2) 0.73682(14) 0.45414(12) 0.0304(5) Uani 1 1 d . H46 H 0.7889 0.7747 0.4427 0.029(6) Uiso 1 1 calc R C47 C 0.6562(2) 0.71724(14) 0.53095(12) 0.0322(5) Uani 1 1 d . H47 H 0.6858 0.7423 0.5714 0.035(6) Uiso 1 1 calc R C48 C 0.5527(2) 0.66120(14) 0.54790(12) 0.0300(5) Uani 1 1 d . C49 C 0.5089(2) 0.62465(15) 0.48862(13) 0.0327(5) Uani 1 1 d . H49 H 0.4377 0.5860 0.5004 0.038(7) Uiso 1 1 calc R C50 C 0.5696(2) 0.64496(14) 0.41241(13) 0.0321(5) Uani 1 1 d . H50 H 0.5399 0.6198 0.3720 0.031(6) Uiso 1 1 calc R C51 C 0.4858(3) 0.63797(16) 0.62972(13) 0.0374(5) Uani 1 1 d . F51 F 0.35874(17) 0.66512(13) 0.62573(9) 0.0642(5) Uani 1 1 d . C52 C 0.8714(2) 0.95875(13) 0.08018(11) 0.0277(4) Uani 1 1 d . H52A H 0.8450 0.9447 0.0302 0.026(6) Uiso 1 1 calc R H52B H 0.9674 0.9647 0.0774 0.040(7) Uiso 1 1 calc R F52 F 0.53785(17) 0.67281(11) 0.68314(8) 0.0558(4) Uani 1 1 d . C53 C 0.8025(2) 1.04681(13) 0.08420(11) 0.0263(4) Uani 1 1 d . F53 F 0.48926(19) 0.54829(10) 0.66560(9) 0.0594(5) Uani 1 1 d . C54 C 0.6692(2) 1.04968(14) 0.10123(13) 0.0305(5) Uani 1 1 d . H54 H 0.6224 0.9966 0.1090 0.039(7) Uiso 1 1 calc R C55 C 0.6032(2) 1.12841(15) 0.10710(13) 0.0330(5) Uani 1 1 d . H55 H 0.5116 1.1297 0.1179 0.038(7) Uiso 1 1 calc R C56 C 0.6720(2) 1.20551(14) 0.09710(12) 0.0311(5) Uani 1 1 d . C57 C 0.8058(2) 1.20344(14) 0.08136(12) 0.0327(5) Uani 1 1 d . H57 H 0.8530 1.2560 0.0753 0.037(7) Uiso 1 1 calc R C58 C 0.8704(2) 1.12431(14) 0.07447(12) 0.0305(5) Uani 1 1 d . H58 H 0.9619 1.1231 0.0630 0.039(7) Uiso 1 1 calc R C59 C 0.6010(3) 1.29138(15) 0.10119(14) 0.0389(5) Uani 1 1 d . F59 F 0.54759(16) 1.33773(9) 0.02894(9) 0.0483(4) Uani 1 1 d . F60 F 0.6775(2) 1.34849(12) 0.11930(13) 0.0757(6) Uani 1 1 d . F61 F 0.50116(19) 1.27795(10) 0.15425(10) 0.0662(5) 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 0.0213(4) 0.0230(3) 0.0196(3) -0.0043(2) 0.0005(2) 0.0000(2) C1 0.0242(13) 0.0239(9) 0.0252(9) -0.0081(7) 0.0033(8) -0.0007(8) N1 0.0242(11) 0.0219(8) 0.0202(7) -0.0041(6) -0.0016(6) 0.0004(6) O1 0.0259(9) 0.0298(7) 0.0241(7) -0.0056(6) 0.0029(5) -0.0052(6) C2 0.0248(13) 0.0291(10) 0.0268(9) -0.0119(8) 0.0035(8) -0.0012(8) N2 0.0229(10) 0.0247(8) 0.0222(7) -0.0052(6) 0.0003(6) -0.0005(6) O2 0.0251(9) 0.0257(7) 0.0232(6) -0.0050(5) -0.0013(5) 0.0004(5) C3 0.0272(14) 0.0398(11) 0.0336(11) -0.0154(9) 0.0017(9) -0.0053(9) N3 0.0213(11) 0.0254(8) 0.0202(8) -0.0052(6) -0.0009(6) -0.0011(7) C4 0.0316(15) 0.0346(11) 0.0434(12) -0.0155(9) 0.0074(10) -0.0117(9) C5 0.0361(15) 0.0265(10) 0.0346(11) -0.0060(8) 0.0087(9) -0.0045(9) C6 0.0285(14) 0.0274(10) 0.0276(10) -0.0081(8) 0.0055(8) -0.0004(8) C7 0.0260(13) 0.0297(10) 0.0284(10) -0.0085(8) -0.0031(8) 0.0005(8) C8 0.0305(14) 0.0402(12) 0.0363(11) -0.0144(9) -0.0066(9) 0.0045(9) C9 0.0339(15) 0.0392(12) 0.0280(10) -0.0105(9) -0.0035(9) 0.0007(9) C10 0.0338(14) 0.0261(10) 0.0297(10) -0.0007(8) -0.0008(9) -0.0003(9) C11 0.0435(17) 0.0311(11) 0.0428(13) 0.0005(10) -0.0018(11) 0.0056(10) C12 0.0510(17) 0.0357(12) 0.0281(11) -0.0022(9) -0.0020(10) -0.0039(11) C13 0.0242(13) 0.0246(9) 0.0178(8) -0.0028(7) -0.0012(7) 0.0018(8) C14 0.0236(12) 0.0239(9) 0.0263(9) -0.0043(7) 0.0036(8) 0.0000(8) C15 0.0251(13) 0.0299(10) 0.0342(11) -0.0093(8) 0.0014(8) -0.0002(8) C16 0.0371(15) 0.0356(11) 0.0473(13) -0.0199(10) 0.0035(10) -0.0031(10) C17 0.0371(16) 0.0291(11) 0.0571(15) -0.0160(10) 0.0075(11) 0.0040(10) C18 0.0276(15) 0.0344(11) 0.0457(13) -0.0045(10) 0.0018(10) 0.0062(9) C19 0.0284(14) 0.0323(10) 0.0323(11) -0.0070(9) -0.0008(9) 0.0004(9) C20 0.0233(12) 0.0256(9) 0.0212(9) -0.0055(7) -0.0021(7) 0.0021(8) C21 0.0240(13) 0.0316(10) 0.0291(10) -0.0115(8) 0.0013(8) 0.0009(8) C22 0.0250(13) 0.0372(11) 0.0314(10) -0.0106(9) 0.0055(8) -0.0065(9) C23 0.0284(13) 0.0284(10) 0.0298(10) -0.0085(8) 0.0013(8) -0.0055(8) C24 0.0249(13) 0.0248(9) 0.0227(9) -0.0048(7) -0.0017(7) -0.0023(8) C25 0.0220(12) 0.0268(9) 0.0220(9) -0.0045(7) -0.0014(7) -0.0020(8) C26 0.0265(12) 0.0260(9) 0.0185(8) -0.0051(7) 0.0015(7) -0.0022(8) C27 0.0253(13) 0.0305(10) 0.0268(10) -0.0085(8) -0.0002(8) 0.0011(8) C28 0.0281(14) 0.0359(11) 0.0295(10) -0.0099(9) 0.0009(8) -0.0059(9) C29 0.0380(15) 0.0269(10) 0.0305(10) -0.0102(8) 0.0014(9) -0.0050(9) C30 0.0374(15) 0.0275(10) 0.0282(10) -0.0073(8) -0.0016(9) 0.0036(9) C31 0.0237(13) 0.0315(10) 0.0249(9) -0.0083(8) -0.0020(8) 0.0004(8) C32 0.0259(12) 0.0263(9) 0.0213(9) -0.0065(7) 0.0002(8) -0.0040(8) C33 0.0248(13) 0.0295(10) 0.0269(10) -0.0086(8) 0.0006(8) -0.0025(8) C34 0.0285(14) 0.0365(11) 0.0302(10) -0.0132(9) 0.0043(8) -0.0032(9) C35 0.0397(15) 0.0400(12) 0.0220(9) -0.0094(8) 0.0026(8) -0.0083(10) C36 0.0341(14) 0.0336(11) 0.0240(10) -0.0037(8) -0.0048(8) -0.0042(9) C37 0.0272(13) 0.0270(9) 0.0250(9) -0.0059(8) -0.0019(8) -0.0047(8) C38 0.0246(13) 0.0384(11) 0.0269(10) -0.0102(8) 0.0010(8) 0.0038(9) C39 0.0458(18) 0.0456(13) 0.0391(13) -0.0150(10) -0.0049(11) 0.0165(11) C40 0.0280(15) 0.0529(14) 0.0444(13) -0.0077(11) -0.0046(10) -0.0015(11) C41 0.0316(14) 0.0307(10) 0.0266(10) -0.0045(8) -0.0055(8) 0.0036(9) C42 0.0330(15) 0.0374(12) 0.0411(12) -0.0074(10) -0.0056(10) 0.0019(10) C43 0.0425(17) 0.0315(11) 0.0466(13) -0.0076(10) -0.0094(11) 0.0026(10) C44 0.0298(14) 0.0316(10) 0.0277(10) -0.0087(8) 0.0019(8) -0.0059(9) C45 0.0242(13) 0.0256(9) 0.0280(10) -0.0044(8) 0.0023(8) 0.0008(8) C46 0.0288(14) 0.0315(10) 0.0290(10) -0.0050(8) 0.0040(8) -0.0074(9) C47 0.0365(15) 0.0338(11) 0.0254(10) -0.0071(8) 0.0013(9) -0.0036(9) C48 0.0288(14) 0.0304(10) 0.0263(10) -0.0016(8) 0.0036(8) -0.0005(8) C49 0.0283(14) 0.0341(11) 0.0334(11) -0.0053(9) 0.0043(9) -0.0073(9) C50 0.0321(14) 0.0335(11) 0.0312(10) -0.0097(9) 0.0022(9) -0.0053(9) C51 0.0346(16) 0.0408(12) 0.0325(11) -0.0040(9) 0.0047(9) -0.0046(10) F51 0.0402(11) 0.1022(14) 0.0397(8) -0.0070(8) 0.0130(7) 0.0039(9) C52 0.0307(14) 0.0295(10) 0.0208(9) -0.0047(8) -0.0006(8) 0.0025(8) F52 0.0653(12) 0.0745(10) 0.0333(7) -0.0213(7) 0.0170(7) -0.0295(9) C53 0.0286(13) 0.0296(10) 0.0186(9) -0.0038(7) -0.0049(7) 0.0019(8) F53 0.0905(14) 0.0441(8) 0.0361(8) 0.0006(6) 0.0189(8) -0.0151(8) C54 0.0267(14) 0.0306(10) 0.0326(10) -0.0062(8) -0.0037(8) -0.0015(9) C55 0.0286(15) 0.0354(11) 0.0327(11) -0.0072(9) -0.0020(9) 0.0034(9) C56 0.0355(15) 0.0311(10) 0.0246(10) -0.0055(8) -0.0051(8) 0.0055(9) C57 0.0399(16) 0.0282(10) 0.0286(10) -0.0053(8) -0.0032(9) -0.0030(9) C58 0.0300(15) 0.0323(10) 0.0256(10) -0.0028(8) -0.0022(8) -0.0006(9) C59 0.0446(17) 0.0357(12) 0.0359(12) -0.0109(10) -0.0019(10) 0.0051(10) F59 0.0578(11) 0.0360(7) 0.0428(8) -0.0021(6) -0.0014(7) 0.0148(6) F60 0.0748(14) 0.0581(10) 0.1140(15) -0.0568(11) -0.0298(11) 0.0139(9) F61 0.0855(14) 0.0465(8) 0.0516(9) 0.0001(7) 0.0288(8) 0.0241(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 '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 O1 Al1 O2 111.41(7) O1 Al1 N2 137.03(8) O2 Al1 N2 111.32(7) O1 Al1 N1 96.59(7) O2 Al1 N1 101.77(7) N2 Al1 N1 79.00(7) O1 Al1 N3 94.78(6) O2 Al1 N3 92.24(7) N2 Al1 N3 79.26(7) N1 Al1 N3 157.27(8) C2 C1 C6 122.05(19) C2 C1 N1 118.24(17) C6 C1 N1 119.61(18) C13 N1 C1 121.62(16) C13 N1 Al1 114.30(12) C1 N1 Al1 123.39(13) C44 O1 Al1 127.80(12) C3 C2 C1 117.74(19) C3 C2 C7 119.32(19) C1 C2 C7 122.94(18) C20 N2 C24 120.43(17) C20 N2 Al1 119.61(13) C24 N2 Al1 118.74(13) C52 O2 Al1 127.61(14) C4 C3 C2 121.2(2) C4 C3 H3 119.4 C2 C3 H3 119.4 C32 N3 C25 116.04(15) C32 N3 Al1 121.68(12) C25 N3 Al1 108.12(11) C32 N3 H3A 108.8(15) C25 N3 H3A 110.0(16) Al1 N3 H3A 88.6(14) C3 C4 C5 120.2(2) C3 C4 H4 119.9 C5 C4 H4 119.9 C4 C5 C6 121.3(2) C4 C5 H5 119.3 C6 C5 H5 119.3 C5 C6 C1 117.5(2) C5 C6 C10 118.34(18) C1 C6 C10 124.16(19) C2 C7 C8 110.77(18) C2 C7 C9 112.18(16) C8 C7 C9 109.57(17) C2 C7 H7 108.1 C8 C7 H7 108.1 C9 C7 H7 108.1 C7 C8 H8A 109.5 C7 C8 H8B 109.5 H8A C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C7 C9 H9A 109.5 C7 C9 H9B 109.5 H9A C9 H9B 109.5 C7 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C6 C10 C12 111.41(19) C6 C10 C11 111.22(18) C12 C10 C11 109.67(18) C6 C10 H10 108.1 C12 C10 H10 108.1 C11 C10 H10 108.1 C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C10 C12 H12A 109.5 C10 C12 H12B 109.5 H12A C12 H12B 109.5 C10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 N1 C13 C20 114.00(17) N1 C13 C14 125.51(18) C20 C13 C14 120.49(18) C19 C14 C15 118.83(19) C19 C14 C13 119.60(18) C15 C14 C13 121.51(19) C16 C15 C14 120.7(2) C16 C15 H15 119.7 C14 C15 H15 119.7 C15 C16 C17 120.1(2) C15 C16 H16 120.0 C17 C16 H16 120.0 C18 C17 C16 119.8(2) C18 C17 H17 120.1 C16 C17 H17 120.1 C17 C18 C19 120.6(2) C17 C18 H18 119.7 C19 C18 H18 119.7 C18 C19 C14 120.0(2) C18 C19 H19 120.0 C14 C19 H19 120.0 C21 C20 N2 123.26(18) C21 C20 C13 124.28(17) N2 C20 C13 112.15(17) C20 C21 C22 117.69(18) C20 C21 H21 121.2 C22 C21 H21 121.2 C23 C22 C21 120.9(2) C23 C22 H22 119.6 C21 C22 H22 119.6 C22 C23 C24 120.83(19) C22 C23 H23 119.6 C24 C23 H23 119.6 C25 C24 N2 116.99(18) C25 C24 C23 126.40(18) N2 C24 C23 116.58(17) C24 C25 N3 113.92(17) C24 C25 C26 125.97(19) N3 C25 C26 120.01(17) C31 C26 C27 116.86(18) C31 C26 C25 121.68(19) C27 C26 C25 121.46(18) C28 C27 C26 121.6(2) C28 C27 H27 119.2 C26 C27 H27 119.2 C27 C28 C29 120.2(2) C27 C28 H28 119.9 C29 C28 H28 119.9 C30 C29 C28 119.19(19) C30 C29 H29 120.4 C28 C29 H29 120.4 C29 C30 C31 120.8(2) C29 C30 H30 119.6 C31 C30 H30 119.6 C30 C31 C26 121.2(2) C30 C31 H31 119.4 C26 C31 H31 119.4 C37 C32 C33 121.05(17) C37 C32 N3 119.27(18) C33 C32 N3 119.65(17) C34 C33 C32 118.18(19) C34 C33 C38 118.16(19) C32 C33 C38 123.55(17) C35 C34 C33 121.6(2) C35 C34 H34 119.2 C33 C34 H34 119.2 C36 C35 C34 119.25(19) C36 C35 H35 120.4 C34 C35 H35 120.4 C35 C36 C37 122.1(2) C35 C36 H36 118.9 C37 C36 H36 118.9 C36 C37 C32 117.72(19) C36 C37 C41 118.57(18) C32 C37 C41 123.65(17) C33 C38 C40 109.80(18) C33 C38 C39 112.71(17) C40 C38 C39 111.1(2) C33 C38 H38 107.7 C40 C38 H38 107.7 C39 C38 H38 107.7 C38 C39 H39A 109.5 C38 C39 H39B 109.5 H39A C39 H39B 109.5 C38 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C38 C40 H40A 109.5 C38 C40 H40B 109.5 H40A C40 H40B 109.5 C38 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C37 C41 C43 111.06(19) C37 C41 C42 111.41(17) C43 C41 C42 110.61(18) C37 C41 H41 107.9 C43 C41 H41 107.9 C42 C41 H41 107.9 C41 C42 H42A 109.5 C41 C42 H42B 109.5 H42A C42 H42B 109.5 C41 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C41 C43 H43A 109.5 C41 C43 H43B 109.5 H43A C43 H43B 109.5 C41 C43 H43C 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 O1 C44 C45 112.25(16) O1 C44 H44A 109.2 C45 C44 H44A 109.2 O1 C44 H44B 109.2 C45 C44 H44B 109.2 H44A C44 H44B 107.9 C46 C45 C50 118.96(19) C46 C45 C44 121.63(19) C50 C45 C44 119.41(18) C45 C46 C47 120.8(2) C45 C46 H46 119.6 C47 C46 H46 119.6 C48 C47 C46 119.55(19) C48 C47 H47 120.2 C46 C47 H47 120.2 C47 C48 C49 120.33(19) C47 C48 C51 121.2(2) C49 C48 C51 118.5(2) C50 C49 C48 119.6(2) C50 C49 H49 120.2 C48 C49 H49 120.2 C49 C50 C45 120.80(19) C49 C50 H50 119.6 C45 C50 H50 119.6 F52 C51 F51 106.2(2) F52 C51 F53 105.49(19) F51 C51 F53 105.4(2) F52 C51 C48 114.1(2) F51 C51 C48 112.90(19) F53 C51 C48 112.00(19) O2 C52 C53 110.21(16) O2 C52 H52A 109.6 C53 C52 H52A 109.6 O2 C52 H52B 109.6 C53 C52 H52B 109.6 H52A C52 H52B 108.1 C54 C53 C58 118.9(2) C54 C53 C52 119.41(19) C58 C53 C52 121.6(2) C55 C54 C53 121.1(2) C55 C54 H54 119.4 C53 C54 H54 119.4 C54 C55 C56 119.5(2) C54 C55 H55 120.3 C56 C55 H55 120.3 C57 C56 C55 120.2(2) C57 C56 C59 120.0(2) C55 C56 C59 119.8(2) C56 C57 C58 119.7(2) C56 C57 H57 120.1 C58 C57 H57 120.1 C57 C58 C53 120.6(2) C57 C58 H58 119.7 C53 C58 H58 119.7 F60 C59 F61 108.0(2) F60 C59 F59 105.0(2) F61 C59 F59 105.0(2) F60 C59 C56 113.4(2) F61 C59 C56 113.0(2) F59 C59 C56 111.84(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 O1 1.7244(14) Al1 O2 1.7346(14) Al1 N2 1.8822(18) Al1 N1 2.0956(16) Al1 N3 2.1810(16) C1 C2 1.404(3) C1 C6 1.408(3) C1 N1 1.448(2) N1 C13 1.297(3) O1 C44 1.404(3) C2 C3 1.389(3) C2 C7 1.526(3) N2 C20 1.375(2) N2 C24 1.401(2) O2 C52 1.405(2) C3 C4 1.381(3) C3 H3 0.9500 N3 C32 1.465(2) N3 C25 1.472(3) N3 H3A 0.90(3) C4 C5 1.382(3) C4 H4 0.9500 C5 C6 1.389(3) C5 H5 0.9500 C6 C10 1.514(3) C7 C8 1.529(3) C7 C9 1.539(3) C7 H7 1.0000 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 C12 1.533(3) C10 C11 1.536(3) C10 H10 1.0000 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 C20 1.477(3) C13 C14 1.488(3) C14 C19 1.392(3) C14 C15 1.398(3) C15 C16 1.381(3) C15 H15 0.9500 C16 C17 1.384(4) C16 H16 0.9500 C17 C18 1.378(3) C17 H17 0.9500 C18 C19 1.390(3) C18 H18 0.9500 C19 H19 0.9500 C20 C21 1.352(3) C21 C22 1.429(3) C21 H21 0.9500 C22 C23 1.350(3) C22 H22 0.9500 C23 C24 1.450(3) C23 H23 0.9500 C24 C25 1.366(3) C25 C26 1.475(3) C26 C31 1.402(3) C26 C27 1.403(3) C27 C28 1.383(3) C27 H27 0.9500 C28 C29 1.391(3) C28 H28 0.9500 C29 C30 1.374(3) C29 H29 0.9500 C30 C31 1.390(3) C30 H30 0.9500 C31 H31 0.9500 C32 C37 1.407(3) C32 C33 1.409(3) C33 C34 1.394(3) C33 C38 1.525(3) C34 C35 1.384(3) C34 H34 0.9500 C35 C36 1.373(3) C35 H35 0.9500 C36 C37 1.399(3) C36 H36 0.9500 C37 C41 1.516(3) C38 C40 1.529(3) C38 C39 1.539(3) C38 H38 1.0000 C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 H40A 0.9800 C40 H40B 0.9800 C40 H40C 0.9800 C41 C43 1.533(3) C41 C42 1.535(3) C41 H41 1.0000 C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C44 C45 1.513(3) C44 H44A 0.9900 C44 H44B 0.9900 C45 C46 1.387(3) C45 C50 1.390(3) C46 C47 1.393(3) C46 H46 0.9500 C47 C48 1.380(3) C47 H47 0.9500 C48 C49 1.393(3) C48 C51 1.493(3) C49 C50 1.384(3) C49 H49 0.9500 C50 H50 0.9500 C51 F52 1.326(3) C51 F51 1.338(3) C51 F53 1.342(3) C52 C53 1.511(3) C52 H52A 0.9900 C52 H52B 0.9900 C53 C54 1.385(3) C53 C58 1.388(3) C54 C55 1.382(3) C54 H54 0.9500 C55 C56 1.387(3) C55 H55 0.9500 C56 C57 1.386(3) C56 C59 1.491(3) C57 C58 1.387(3) C57 H57 0.9500 C58 H58 0.9500 C59 F60 1.323(3) C59 F61 1.329(3) C59 F59 1.346(3) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N3 H3A O2 0.90(3) 2.39(2) 2.839(2) 110.8(17) 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 C2 C1 N1 C13 -109.7(2) C6 C1 N1 C13 73.8(2) C2 C1 N1 Al1 80.37(19) C6 C1 N1 Al1 -96.2(2) O2 Al1 O1 C44 31.48(17) N2 Al1 O1 C44 -154.86(15) N1 Al1 O1 C44 -73.94(16) N3 Al1 O1 C44 125.78(16) C6 C1 C2 C3 -0.1(3) N1 C1 C2 C3 -176.51(17) C6 C1 C2 C7 -179.83(18) N1 C1 C2 C7 3.7(3) O1 Al1 N2 C20 90.99(16) O2 Al1 N2 C20 -95.35(14) N1 Al1 N2 C20 3.12(13) N3 Al1 N2 C20 176.45(15) O1 Al1 N2 C24 -101.54(15) O2 Al1 N2 C24 72.12(15) N1 Al1 N2 C24 170.59(14) N3 Al1 N2 C24 -16.08(13) O1 Al1 O2 C52 167.81(14) N2 Al1 O2 C52 -7.56(16) N1 Al1 O2 C52 -90.21(15) N3 Al1 O2 C52 71.78(15) C1 C2 C3 C4 0.3(3) C7 C2 C3 C4 -179.9(2) C2 C3 C4 C5 -0.3(3) C3 C4 C5 C6 -0.1(3) C4 C5 C6 C1 0.4(3) C4 C5 C6 C10 179.4(2) C2 C1 C6 C5 -0.3(3) N1 C1 C6 C5 176.11(18) C2 C1 C6 C10 -179.22(18) N1 C1 C6 C10 -2.8(3) C3 C2 C7 C8 61.5(2) C1 C2 C7 C8 -118.7(2) C3 C2 C7 C9 -61.3(3) C1 C2 C7 C9 118.5(2) C5 C6 C10 C12 -64.4(2) C1 C6 C10 C12 114.5(2) C5 C6 C10 C11 58.3(3) C1 C6 C10 C11 -122.8(2) C1 N1 C13 C20 -179.40(15) Al1 N1 C13 C20 -8.60(19) C1 N1 C13 C14 -0.4(3) Al1 N1 C13 C14 170.43(14) N1 C13 C14 C19 -131.1(2) C20 C13 C14 C19 47.9(3) N1 C13 C14 C15 46.0(3) C20 C13 C14 C15 -135.0(2) C19 C14 C15 C16 -0.6(3) C13 C14 C15 C16 -177.8(2) C14 C15 C16 C17 1.4(3) C15 C16 C17 C18 -0.9(4) C16 C17 C18 C19 -0.3(4) C17 C18 C19 C14 1.1(3) C15 C14 C19 C18 -0.6(3) C13 C14 C19 C18 176.59(19) C24 N2 C20 C21 -1.7(3) Al1 N2 C20 C21 165.53(15) C24 N2 C20 C13 -175.61(16) Al1 N2 C20 C13 -8.4(2) N1 C13 C20 C21 -162.91(18) C14 C13 C20 C21 18.0(3) N1 C13 C20 N2 10.9(2) C14 C13 C20 N2 -168.18(16) N2 C20 C21 C22 -2.9(3) C13 C20 C21 C22 170.25(18) C20 C21 C22 C23 2.9(3) C21 C22 C23 C24 1.6(3) C20 N2 C24 C25 -175.90(17) Al1 N2 C24 C25 16.7(2) C20 N2 C24 C23 6.0(3) Al1 N2 C24 C23 -161.34(14) C22 C23 C24 C25 176.2(2) C22 C23 C24 N2 -6.0(3) N2 C24 C25 N3 -3.8(2) C23 C24 C25 N3 174.06(18) N2 C24 C25 C26 179.77(17) C23 C24 C25 C26 -2.4(3) C32 N3 C25 C24 132.74(18) Al1 N3 C25 C24 -8.06(19) C32 N3 C25 C26 -50.6(2) Al1 N3 C25 C26 168.61(14) C24 C25 C26 C31 137.8(2) N3 C25 C26 C31 -38.5(3) C24 C25 C26 C27 -41.7(3) N3 C25 C26 C27 142.02(18) C31 C26 C27 C28 -3.3(3) C25 C26 C27 C28 176.26(18) C26 C27 C28 C29 1.0(3) C27 C28 C29 C30 1.5(3) C28 C29 C30 C31 -1.7(3) C29 C30 C31 C26 -0.6(3) C27 C26 C31 C30 3.1(3) C25 C26 C31 C30 -176.46(18) C25 N3 C32 C37 -62.9(2) Al1 N3 C32 C37 72.2(2) C25 N3 C32 C33 118.7(2) Al1 N3 C32 C33 -106.19(18) C37 C32 C33 C34 1.4(3) N3 C32 C33 C34 179.69(18) C37 C32 C33 C38 -174.61(19) N3 C32 C33 C38 3.7(3) C32 C33 C34 C35 0.6(3) C38 C33 C34 C35 176.8(2) C33 C34 C35 C36 -1.7(3) C34 C35 C36 C37 0.9(3) C35 C36 C37 C32 1.0(3) C35 C36 C37 C41 -176.4(2) C33 C32 C37 C36 -2.1(3) N3 C32 C37 C36 179.54(18) C33 C32 C37 C41 175.12(19) N3 C32 C37 C41 -3.2(3) C34 C33 C38 C40 -78.4(2) C32 C33 C38 C40 97.6(2) C34 C33 C38 C39 46.1(3) C32 C33 C38 C39 -138.0(2) C36 C37 C41 C43 57.8(3) C32 C37 C41 C43 -119.5(2) C36 C37 C41 C42 -66.0(2) C32 C37 C41 C42 116.8(2) Al1 O1 C44 C45 -160.56(13) O1 C44 C45 C46 18.2(3) O1 C44 C45 C50 -162.42(18) C50 C45 C46 C47 -1.2(3) C44 C45 C46 C47 178.2(2) C45 C46 C47 C48 0.9(3) C46 C47 C48 C49 -0.2(3) C46 C47 C48 C51 179.5(2) C47 C48 C49 C50 -0.1(3) C51 C48 C49 C50 -179.8(2) C48 C49 C50 C45 -0.3(3) C46 C45 C50 C49 0.9(3) C44 C45 C50 C49 -178.5(2) C47 C48 C51 F52 -2.4(3) C49 C48 C51 F52 177.3(2) C47 C48 C51 F51 119.0(2) C49 C48 C51 F51 -61.3(3) C47 C48 C51 F53 -122.2(2) C49 C48 C51 F53 57.5(3) Al1 O2 C52 C53 -118.71(16) O2 C52 C53 C54 -49.3(2) O2 C52 C53 C58 128.06(19) C58 C53 C54 C55 1.2(3) C52 C53 C54 C55 178.64(18) C53 C54 C55 C56 -1.1(3) C54 C55 C56 C57 0.0(3) C54 C55 C56 C59 178.42(19) C55 C56 C57 C58 0.9(3) C59 C56 C57 C58 -177.50(19) C56 C57 C58 C53 -0.8(3) C54 C53 C58 C57 -0.3(3) C52 C53 C58 C57 -177.64(18) C57 C56 C59 F60 -23.8(3) C55 C56 C59 F60 157.7(2) C57 C56 C59 F61 -147.2(2) C55 C56 C59 F61 34.4(3) C57 C56 C59 F59 94.6(3) C55 C56 C59 F59 -83.8(3)