#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:26:23 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541906.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_1541906 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 'C51 H55 Al F3 N3 O' _chemical_formula_sum 'C51 H55 Al F3 N3 O' _chemical_formula_weight 809.96 _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 101.4104(7) _cell_angle_beta 98.4568(6) _cell_angle_gamma 114.4940(7) _cell_formula_units_Z 2 _cell_length_a 11.2001(2) _cell_length_b 12.4244(2) _cell_length_c 18.0337(3) _cell_measurement_reflns_used 9924 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 68.62 _cell_measurement_theta_min 2.59 _cell_volume 2163.42(7) _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 0.959 _diffrn_measured_fraction_theta_max 0.956 _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_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_laue_measured_fraction_full 0.959 _diffrn_reflns_laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 14518 _diffrn_reflns_point_group_measured_fraction_full 0.959 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.635 _diffrn_reflns_theta_min 2.586 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_T_max 0.8993 _exptl_absorpt_correction_T_min 0.8071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/3 (Sheldrick, 2014)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.243 _exptl_crystal_description Plate _exptl_crystal_F_000 860 _exptl_crystal_size_max 0.219 _exptl_crystal_size_mid 0.195 _exptl_crystal_size_min 0.102 _refine_diff_density_max 0.444 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 593 _refine_ls_number_reflns 7646 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0404 _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^)+(0.0611P)^2^+0.9681P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.1136 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6661 _reflns_number_total 7646 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc03169a2.cif _cod_data_source_block TJS17FMI _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_original_cell_volume 2163.41(6) _cod_database_code 1541906 _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 0.836 _shelx_estimated_absorpt_t_max 0.919 _shelx_res_file ; TJS17FMI.res created by SHELXL-2014/7 TITL TJS17Fmi in P-1 JCF 5AUG2015 MERGE-I ALL DATA CELL 1.54178 11.2001 12.4244 18.0337 101.4104 98.4568 114.4940 ZERR 2.00 0.0002 0.0002 0.0003 0.0007 0.0006 0.0007 LATT 1 SFAC C H N O F Al UNIT 102 110 6 2 6 2 OMIT 2 -4 4 ! 0.00 652.75 17.20 0.121 2.69 OMIT -3 1 5 ! -2.94 140.70 11.25 0.056 2.76 L.S. 15 ACTA FMAP 2 PLAN 20 CONF BOND $H WPDB -2 HTAB CONF SIZE 0.102 0.195 0.219 SIMU 0.003 AL1 H1 TEMP -183.000 WGHT 0.061100 0.968100 FVAR 0.14319 AL1 6 0.789775 0.802169 0.187564 11.00000 0.01525 0.01363 = 0.01878 0.00531 0.00536 0.00644 H1 2 0.703512 0.812105 0.109666 11.00000 0.01176 C1 1 0.542242 0.621802 0.232361 11.00000 0.01488 0.01197 = 0.02210 0.00454 0.00633 0.00477 N1 3 0.661873 0.636267 0.206168 11.00000 0.01374 0.01479 = 0.01511 0.00389 0.00286 0.00478 O1 4 0.794109 0.899501 0.272579 11.00000 0.01997 0.01902 = 0.02570 0.00326 0.00832 0.00877 C2 1 0.542496 0.633084 0.311405 11.00000 0.02110 0.01480 = 0.02208 0.00467 0.00787 0.00536 N2 3 0.884374 0.707364 0.167604 11.00000 0.01430 0.01357 = 0.01684 0.00424 0.00496 0.00535 C3 1 0.427024 0.630407 0.333285 11.00000 0.02654 0.02153 = 0.02605 0.00664 0.01401 0.00820 AFIX 43 H3A 2 0.424185 0.637890 0.386376 11.00000 0.02375 AFIX 0 N3 3 0.974786 0.938433 0.169712 11.00000 0.01688 0.01522 = 0.01686 0.00615 0.00510 0.00771 H3 2 0.931615 0.950855 0.131252 11.00000 0.01797 C4 1 0.316300 0.617064 0.279231 11.00000 0.02101 0.02342 = 0.04006 0.00672 0.01504 0.00935 AFIX 43 H4A 2 0.239278 0.616569 0.295595 11.00000 0.03379 AFIX 0 C5 1 0.318110 0.604482 0.201506 11.00000 0.01769 0.02241 = 0.03567 0.00813 0.00742 0.00906 AFIX 43 H5A 2 0.241491 0.594577 0.164818 11.00000 0.02694 AFIX 0 C6 1 0.430052 0.606069 0.176094 11.00000 0.01749 0.01288 = 0.02582 0.00600 0.00505 0.00558 C7 1 0.662502 0.650924 0.373684 11.00000 0.02449 0.02222 = 0.01791 0.00593 0.00753 0.00864 AFIX 13 H7A 2 0.731747 0.643171 0.346793 11.00000 0.01510 AFIX 0 C8 1 0.728578 0.779755 0.432176 11.00000 0.02991 0.02518 = 0.01939 0.00457 0.00473 0.00841 AFIX 33 H8A 2 0.805184 0.788785 0.471452 11.00000 0.03081 H8B 2 0.761184 0.842328 0.404429 11.00000 0.03210 H8C 2 0.661676 0.790642 0.458100 11.00000 0.03292 AFIX 0 C9 1 0.619793 0.551196 0.416350 11.00000 0.03530 0.02733 = 0.02393 0.00984 0.00818 0.01212 AFIX 33 H9A 2 0.698733 0.564973 0.455899 11.00000 0.04136 H9B 2 0.549689 0.555212 0.441867 11.00000 0.04874 H9C 2 0.583653 0.469649 0.378560 11.00000 0.03593 AFIX 0 C10 1 0.426282 0.587133 0.089486 11.00000 0.01655 0.02272 = 0.02375 0.00755 0.00257 0.00865 AFIX 13 H10A 2 0.518226 0.599594 0.083807 11.00000 0.01857 AFIX 0 C11 1 0.395833 0.680522 0.057535 11.00000 0.02910 0.02851 = 0.03453 0.01432 0.00519 0.01378 AFIX 33 H11A 2 0.394363 0.665069 0.001890 11.00000 0.03948 H11B 2 0.307264 0.672177 0.063854 11.00000 0.04827 H11C 2 0.466322 0.764283 0.086347 11.00000 0.04526 AFIX 0 C12 1 0.323610 0.455816 0.040246 11.00000 0.02899 0.02602 = 0.02364 0.00686 0.00126 0.00946 AFIX 33 H12A 2 0.323924 0.447007 -0.014932 11.00000 0.03264 H12B 2 0.348455 0.396464 0.057957 11.00000 0.03708 H12C 2 0.232725 0.439910 0.046192 11.00000 0.03181 AFIX 0 C13 1 0.706353 0.554430 0.201191 11.00000 0.01480 0.01509 = 0.01273 0.00263 0.00098 0.00494 C14 1 0.649572 0.439636 0.224429 11.00000 0.01876 0.01477 = 0.01678 0.00556 0.00655 0.00703 C15 1 0.737739 0.411782 0.271138 11.00000 0.01853 0.02015 = 0.02169 0.00775 0.00661 0.00844 AFIX 43 H15A 2 0.832781 0.464150 0.284653 11.00000 0.02763 AFIX 0 C16 1 0.687729 0.308612 0.297832 11.00000 0.02717 0.02473 = 0.02655 0.01354 0.00907 0.01409 AFIX 43 H16A 2 0.748298 0.291062 0.330066 11.00000 0.02894 AFIX 0 C17 1 0.549261 0.230875 0.277538 11.00000 0.03122 0.01921 = 0.03022 0.01413 0.01319 0.01068 AFIX 43 H17A 2 0.515085 0.159914 0.295705 11.00000 0.03513 AFIX 0 C18 1 0.460610 0.256612 0.230747 11.00000 0.02119 0.01769 = 0.02660 0.00705 0.00840 0.00403 AFIX 43 H18A 2 0.365842 0.202976 0.216729 11.00000 0.02429 AFIX 0 C19 1 0.509946 0.360590 0.204302 11.00000 0.01845 0.01712 = 0.01948 0.00565 0.00442 0.00650 AFIX 43 H19A 2 0.448795 0.378080 0.172494 11.00000 0.01969 AFIX 0 C20 1 0.828011 0.587759 0.170141 11.00000 0.01401 0.01428 = 0.01432 0.00476 0.00203 0.00479 C21 1 0.870084 0.504173 0.138889 11.00000 0.01750 0.01448 = 0.01890 0.00572 0.00343 0.00689 AFIX 43 H21A 2 0.831429 0.422557 0.143497 11.00000 0.02594 AFIX 0 C22 1 0.974803 0.544732 0.098931 11.00000 0.01807 0.01751 = 0.01819 0.00364 0.00459 0.00967 AFIX 43 H22A 2 1.003079 0.487969 0.073918 11.00000 0.02448 AFIX 0 C23 1 1.033900 0.663197 0.096458 11.00000 0.01609 0.01958 = 0.01777 0.00519 0.00561 0.00761 AFIX 43 H23A 2 1.103045 0.688287 0.069555 11.00000 0.01526 AFIX 0 C24 1 0.993636 0.752394 0.134080 11.00000 0.01388 0.01727 = 0.01396 0.00501 0.00383 0.00562 C25 1 1.048709 0.874146 0.137105 11.00000 0.01683 0.01670 = 0.01569 0.00310 0.00482 0.00775 C26 1 1.165683 0.941357 0.107569 11.00000 0.02113 0.01313 = 0.01674 0.00243 0.00682 0.00373 C27 1 1.280833 0.921861 0.117178 11.00000 0.02386 0.01616 = 0.03056 0.00485 0.01241 0.00670 AFIX 43 H27A 2 1.285260 0.865314 0.144721 11.00000 0.02561 AFIX 0 C28 1 1.388882 0.983829 0.087105 11.00000 0.02870 0.02051 = 0.04518 0.00522 0.02256 0.00802 AFIX 43 H28A 2 1.465365 0.968210 0.093596 11.00000 0.03506 AFIX 0 C29 1 1.385668 1.068167 0.047755 11.00000 0.03998 0.02210 = 0.03921 0.00706 0.02985 0.00633 AFIX 43 H29A 2 1.458930 1.109419 0.026588 11.00000 0.03943 AFIX 0 C30 1 1.274508 1.091798 0.039558 11.00000 0.03923 0.01938 = 0.02335 0.00647 0.01507 0.00484 AFIX 43 H30A 2 1.272144 1.150478 0.013430 11.00000 0.01727 AFIX 0 C31 1 1.166339 1.029594 0.069591 11.00000 0.02728 0.01946 = 0.01738 0.00364 0.00575 0.00723 AFIX 43 H31A 2 1.091345 1.047402 0.064199 11.00000 0.02655 AFIX 0 C32 1 1.058704 1.058410 0.227646 11.00000 0.01639 0.01392 = 0.01834 0.00484 0.00850 0.00473 C33 1 1.140129 1.065330 0.297571 11.00000 0.01690 0.01702 = 0.01937 0.00687 0.00831 0.00635 C34 1 1.223004 1.181835 0.350523 11.00000 0.01943 0.02098 = 0.01905 0.00588 0.00566 0.00534 AFIX 43 H34A 2 1.280940 1.188729 0.397231 11.00000 0.02466 AFIX 0 C35 1 1.223099 1.287426 0.336877 11.00000 0.02371 0.01504 = 0.02500 0.00149 0.00820 0.00259 AFIX 43 H35A 2 1.281257 1.365872 0.373480 11.00000 0.02272 AFIX 0 C36 1 1.137739 1.277952 0.269421 11.00000 0.02759 0.01365 = 0.02992 0.00910 0.01220 0.00832 AFIX 43 H36A 2 1.135994 1.350408 0.260928 11.00000 0.02654 AFIX 0 C37 1 1.054040 1.164117 0.213516 11.00000 0.02077 0.01770 = 0.02185 0.00774 0.00945 0.00812 C38 1 0.956561 1.160247 0.143276 11.00000 0.03056 0.01825 = 0.02540 0.00924 0.00698 0.01239 AFIX 13 H38A 2 0.923462 1.078938 0.103322 11.00000 0.03330 AFIX 0 C39 1 0.833062 1.165741 0.166513 11.00000 0.03952 0.06131 = 0.04431 0.02333 0.01197 0.03405 AFIX 33 H39A 2 0.791535 1.100262 0.190935 11.00000 0.05535 H39B 2 0.861501 1.246284 0.203731 11.00000 0.06201 H39C 2 0.766879 1.154204 0.119789 11.00000 0.05317 AFIX 0 C40 1 1.023678 1.260864 0.105090 11.00000 0.05424 0.02887 = 0.03332 0.01779 0.00536 0.01360 AFIX 33 H40A 2 0.956541 1.253916 0.060497 11.00000 0.05563 H40B 2 1.059724 1.342011 0.143322 11.00000 0.04547 H40C 2 1.097992 1.251464 0.086859 11.00000 0.06791 AFIX 0 C41 1 1.135510 0.952343 0.320362 11.00000 0.02017 0.01883 = 0.01815 0.00557 0.00386 0.00787 AFIX 13 H41A 2 1.069115 0.877516 0.276821 11.00000 0.02051 AFIX 0 C42 1 1.084760 0.943389 0.394596 11.00000 0.02815 0.02336 = 0.02332 0.01099 0.00836 0.01109 AFIX 33 H42A 2 1.082534 0.870179 0.408262 11.00000 0.03670 H42B 2 1.146127 1.017448 0.437793 11.00000 0.04452 H42C 2 0.993231 0.936825 0.385110 11.00000 0.03947 AFIX 0 C43 1 1.273240 0.951597 0.331299 11.00000 0.02628 0.02981 = 0.03547 0.01405 0.01030 0.01595 AFIX 33 H43A 2 1.265874 0.877600 0.345885 11.00000 0.03580 H43B 2 1.301072 0.951330 0.282250 11.00000 0.03736 H43C 2 1.340979 1.025383 0.372767 11.00000 0.04041 AFIX 0 C44 1 0.692828 0.933245 0.288460 11.00000 0.02102 0.02113 = 0.02731 0.00616 0.00883 0.00991 AFIX 23 H44A 2 0.619619 0.863840 0.299210 11.00000 0.02675 H44B 2 0.652909 0.949527 0.241816 11.00000 0.01677 AFIX 0 C45 1 0.749176 1.047082 0.357942 11.00000 0.02364 0.01940 = 0.02392 0.00930 0.00817 0.01161 C46 1 0.884278 1.135523 0.377906 11.00000 0.02335 0.02278 = 0.02582 0.00821 0.00951 0.01203 AFIX 43 H46A 2 0.943557 1.123907 0.348181 11.00000 0.02984 AFIX 0 C47 1 0.933691 1.240683 0.440785 11.00000 0.02392 0.02310 = 0.02615 0.00816 0.00653 0.01077 AFIX 43 H47A 2 1.026189 1.300587 0.453714 11.00000 0.03316 AFIX 0 C48 1 0.848278 1.258267 0.484618 11.00000 0.03198 0.02313 = 0.02259 0.00984 0.00917 0.01565 C49 1 0.713010 1.170305 0.465482 11.00000 0.03133 0.02943 = 0.02852 0.01110 0.01526 0.01811 AFIX 43 H49A 2 0.654086 1.182092 0.495437 11.00000 0.03268 AFIX 0 C50 1 0.664199 1.065689 0.402885 11.00000 0.02288 0.02380 = 0.03275 0.01155 0.01149 0.01120 AFIX 43 H50A 2 0.571772 1.005745 0.390287 11.00000 0.02063 AFIX 0 C51 1 0.899889 1.369158 0.554074 11.00000 0.03884 0.02736 = 0.02788 0.00973 0.01340 0.01670 F51 5 1.027065 1.452923 0.561441 11.00000 0.03794 0.02992 = 0.03181 0.00013 0.00766 0.00781 F52 5 0.903495 1.339529 0.622170 11.00000 0.06523 0.03641 = 0.02560 0.00835 0.01707 0.02263 F53 5 0.822914 1.427633 0.552496 11.00000 0.04826 0.03182 = 0.04633 0.00275 0.01321 0.02502 HKLF 4 REM TJS17Fmi in P-1 JCF 5AUG2015 MERGE-I ALL DATA REM R1 = 0.0404 for 6661 Fo > 4sig(Fo) and 0.0470 for all 7646 data REM 593 parameters refined using 6 restraints END WGHT 0.0611 0.9681 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.444, deepest hole -0.366, 1-sigma level 0.049 Q1 1 0.7990 1.3087 0.6050 11.00000 0.05 0.44 Q2 1 1.0550 0.8279 0.1636 11.00000 0.05 0.31 Q3 1 1.3000 1.0444 0.0152 11.00000 0.05 0.30 Q4 1 0.4235 0.5974 0.1330 11.00000 0.05 0.29 Q5 1 1.1208 0.9527 0.3595 11.00000 0.05 0.28 Q6 1 1.2956 1.2180 -0.0263 11.00000 0.05 0.27 Q7 1 1.0229 0.7168 0.1182 11.00000 0.05 0.26 Q8 1 1.1381 1.0885 0.0442 11.00000 0.05 0.25 Q9 1 1.2112 0.9245 0.0911 11.00000 0.05 0.25 Q10 1 0.9999 0.8124 0.1144 11.00000 0.05 0.24 Q11 1 1.0866 1.2204 0.2466 11.00000 0.05 0.24 Q12 1 0.8630 0.5478 0.1664 11.00000 0.05 0.24 Q13 1 0.7576 0.5636 0.1836 11.00000 0.05 0.24 Q14 1 1.1432 1.2865 0.3148 11.00000 0.05 0.23 Q15 1 0.3416 0.6521 0.2420 11.00000 0.05 0.23 Q16 1 0.8238 0.8991 0.2244 11.00000 0.05 0.23 Q17 1 0.8445 0.7399 0.1784 11.00000 0.05 0.23 Q18 1 0.8632 1.2980 0.5143 11.00000 0.05 0.23 Q19 1 1.1619 0.9818 0.0899 11.00000 0.05 0.23 Q20 1 1.2331 0.9608 0.1225 11.00000 0.05 0.22 ; _shelx_res_checksum 60560 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 Al1 Al 0.78978(4) 0.80217(4) 0.18756(3) 0.01573(12) Uani 1 1 d . U H1 H 0.7035(17) 0.8121(16) 0.1097(10) 0.0118(16) Uiso 1 1 d . U C1 C 0.54224(15) 0.62180(14) 0.23236(9) 0.0167(3) Uani 1 1 d . . N1 N 0.66187(13) 0.63627(12) 0.20617(7) 0.0153(3) Uani 1 1 d . . O1 O 0.79411(11) 0.89950(11) 0.27258(7) 0.0218(3) Uani 1 1 d . . C2 C 0.54250(16) 0.63308(15) 0.31141(9) 0.0202(3) Uani 1 1 d . . N2 N 0.88437(13) 0.70736(12) 0.16760(7) 0.0152(3) Uani 1 1 d . . C3 C 0.42702(18) 0.63041(17) 0.33328(10) 0.0249(4) Uani 1 1 d . . H3A H 0.4242 0.6379 0.3864 0.024(5) Uiso 1 1 calc R . N3 N 0.97479(13) 0.93843(12) 0.16971(7) 0.0158(3) Uani 1 1 d . . H3 H 0.932(2) 0.9509(18) 0.1313(12) 0.018(5) Uiso 1 1 d . . C4 C 0.31630(18) 0.61706(17) 0.27923(11) 0.0280(4) Uani 1 1 d . . H4A H 0.2393 0.6166 0.2956 0.034(6) Uiso 1 1 calc R . C5 C 0.31811(17) 0.60448(17) 0.20151(11) 0.0253(4) Uani 1 1 d . . H5A H 0.2415 0.5946 0.1648 0.027(5) Uiso 1 1 calc R . C6 C 0.43005(16) 0.60607(15) 0.17609(9) 0.0192(3) Uani 1 1 d . . C7 C 0.66250(17) 0.65092(16) 0.37368(9) 0.0220(3) Uani 1 1 d . . H7A H 0.7317 0.6432 0.3468 0.015(4) Uiso 1 1 calc R . C8 C 0.72858(19) 0.77975(17) 0.43218(10) 0.0268(4) Uani 1 1 d . . H8A H 0.8052 0.7888 0.4715 0.031(5) Uiso 1 1 calc R . H8B H 0.7612 0.8423 0.4044 0.032(6) Uiso 1 1 calc R . H8C H 0.6617 0.7906 0.4581 0.033(6) Uiso 1 1 calc R . C9 C 0.6198(2) 0.55120(18) 0.41635(10) 0.0292(4) Uani 1 1 d . . H9A H 0.6987 0.5650 0.4559 0.041(6) Uiso 1 1 calc R . H9B H 0.5497 0.5552 0.4419 0.049(7) Uiso 1 1 calc R . H9C H 0.5837 0.4696 0.3786 0.036(6) Uiso 1 1 calc R . C10 C 0.42628(16) 0.58713(16) 0.08949(9) 0.0213(3) Uani 1 1 d . . H10A H 0.5182 0.5996 0.0838 0.019(4) Uiso 1 1 calc R . C11 C 0.39583(19) 0.68052(18) 0.05754(11) 0.0300(4) Uani 1 1 d . . H11A H 0.3944 0.6651 0.0019 0.039(6) Uiso 1 1 calc R . H11B H 0.3073 0.6722 0.0639 0.048(7) Uiso 1 1 calc R . H11C H 0.4663 0.7643 0.0863 0.045(7) Uiso 1 1 calc R . C12 C 0.32361(19) 0.45582(17) 0.04025(10) 0.0280(4) Uani 1 1 d . . H12A H 0.3239 0.4470 -0.0149 0.033(6) Uiso 1 1 calc R . H12B H 0.3485 0.3965 0.0580 0.037(6) Uiso 1 1 calc R . H12C H 0.2327 0.4399 0.0462 0.032(6) Uiso 1 1 calc R . C13 C 0.70635(15) 0.55443(15) 0.20119(8) 0.0154(3) Uani 1 1 d . . C14 C 0.64957(16) 0.43964(15) 0.22443(9) 0.0166(3) Uani 1 1 d . . C15 C 0.73774(16) 0.41178(16) 0.27114(9) 0.0198(3) Uani 1 1 d . . H15A H 0.8328 0.4642 0.2847 0.028(5) Uiso 1 1 calc R . C16 C 0.68773(18) 0.30861(17) 0.29783(10) 0.0241(4) Uani 1 1 d . . H16A H 0.7483 0.2911 0.3301 0.029(5) Uiso 1 1 calc R . C17 C 0.54926(19) 0.23088(17) 0.27754(10) 0.0254(4) Uani 1 1 d . . H17A H 0.5151 0.1599 0.2957 0.035(6) Uiso 1 1 calc R . C18 C 0.46061(17) 0.25661(16) 0.23075(10) 0.0232(4) Uani 1 1 d . . H18A H 0.3658 0.2030 0.2167 0.024(5) Uiso 1 1 calc R . C19 C 0.50995(16) 0.36059(15) 0.20430(9) 0.0189(3) Uani 1 1 d . . H19A H 0.4488 0.3781 0.1725 0.020(5) Uiso 1 1 calc R . C20 C 0.82801(15) 0.58776(15) 0.17014(8) 0.0149(3) Uani 1 1 d . . C21 C 0.87008(16) 0.50417(15) 0.13889(9) 0.0171(3) Uani 1 1 d . . H21A H 0.8314 0.4226 0.1435 0.026(5) Uiso 1 1 calc R . C22 C 0.97480(16) 0.54473(15) 0.09893(9) 0.0176(3) Uani 1 1 d . . H22A H 1.0031 0.4880 0.0739 0.024(5) Uiso 1 1 calc R . C23 C 1.03390(15) 0.66320(15) 0.09646(9) 0.0179(3) Uani 1 1 d . . H23A H 1.1030 0.6883 0.0696 0.015(4) Uiso 1 1 calc R . C24 C 0.99364(15) 0.75239(15) 0.13408(8) 0.0155(3) Uani 1 1 d . . C25 C 1.04871(15) 0.87415(15) 0.13711(8) 0.0166(3) Uani 1 1 d . . C26 C 1.16568(16) 0.94136(15) 0.10757(9) 0.0185(3) Uani 1 1 d . . C27 C 1.28083(17) 0.92186(16) 0.11718(10) 0.0241(4) Uani 1 1 d . . H27A H 1.2853 0.8653 0.1447 0.026(5) Uiso 1 1 calc R . C28 C 1.38888(19) 0.98383(18) 0.08711(12) 0.0318(4) Uani 1 1 d . . H28A H 1.4654 0.9682 0.0936 0.035(6) Uiso 1 1 calc R . C29 C 1.3857(2) 1.06817(18) 0.04776(11) 0.0346(5) Uani 1 1 d . . H29A H 1.4589 1.1094 0.0266 0.039(6) Uiso 1 1 calc R . C30 C 1.2745(2) 1.09180(17) 0.03956(10) 0.0295(4) Uani 1 1 d . . H30A H 1.2721 1.1505 0.0134 0.017(4) Uiso 1 1 calc R . C31 C 1.16634(18) 1.02959(16) 0.06959(9) 0.0229(4) Uani 1 1 d . . H31A H 1.0913 1.0474 0.0642 0.027(5) Uiso 1 1 calc R . C32 C 1.05870(15) 1.05841(15) 0.22765(9) 0.0165(3) Uani 1 1 d . . C33 C 1.14013(16) 1.06533(15) 0.29757(9) 0.0176(3) Uani 1 1 d . . C34 C 1.22300(16) 1.18184(16) 0.35052(9) 0.0211(3) Uani 1 1 d . . H34A H 1.2809 1.1887 0.3972 0.025(5) Uiso 1 1 calc R . C35 C 1.22310(17) 1.28743(16) 0.33688(10) 0.0240(4) Uani 1 1 d . . H35A H 1.2813 1.3659 0.3735 0.023(5) Uiso 1 1 calc R . C36 C 1.13774(17) 1.27795(16) 0.26942(10) 0.0231(4) Uani 1 1 d . . H36A H 1.1360 1.3504 0.2609 0.027(5) Uiso 1 1 calc R . C37 C 1.05404(16) 1.16412(16) 0.21352(9) 0.0196(3) Uani 1 1 d . . C38 C 0.95656(18) 1.16025(16) 0.14328(10) 0.0239(4) Uani 1 1 d . . H38A H 0.9235 1.0789 0.1033 0.033(6) Uiso 1 1 calc R . C39 C 0.8331(2) 1.1657(2) 0.16651(13) 0.0430(5) Uani 1 1 d . . H39A H 0.7915 1.1003 0.1909 0.055(8) Uiso 1 1 calc R . H39B H 0.8615 1.2463 0.2037 0.062(8) Uiso 1 1 calc R . H39C H 0.7669 1.1542 0.1198 0.053(7) Uiso 1 1 calc R . C40 C 1.0237(2) 1.2609(2) 0.10509(12) 0.0400(5) Uani 1 1 d . . H40A H 0.9565 1.2539 0.0605 0.056(8) Uiso 1 1 calc R . H40B H 1.0597 1.3420 0.1433 0.045(7) Uiso 1 1 calc R . H40C H 1.0980 1.2515 0.0869 0.068(9) Uiso 1 1 calc R . C41 C 1.13551(16) 0.95234(16) 0.32036(9) 0.0195(3) Uani 1 1 d . . H41A H 1.0691 0.8775 0.2768 0.021(5) Uiso 1 1 calc R . C42 C 1.08476(18) 0.94339(17) 0.39460(10) 0.0243(4) Uani 1 1 d . . H42A H 1.0825 0.8702 0.4083 0.037(6) Uiso 1 1 calc R . H42B H 1.1461 1.0174 0.4378 0.045(7) Uiso 1 1 calc R . H42C H 0.9932 0.9368 0.3851 0.039(6) Uiso 1 1 calc R . C43 C 1.27324(18) 0.95160(18) 0.33130(11) 0.0284(4) Uani 1 1 d . . H43A H 1.2659 0.8776 0.3459 0.036(6) Uiso 1 1 calc R . H43B H 1.3011 0.9513 0.2822 0.037(6) Uiso 1 1 calc R . H43C H 1.3410 1.0254 0.3728 0.040(6) Uiso 1 1 calc R . C44 C 0.69283(17) 0.93325(16) 0.28846(10) 0.0229(4) Uani 1 1 d . . H44A H 0.6196 0.8638 0.2992 0.027(5) Uiso 1 1 calc R . H44B H 0.6529 0.9495 0.2418 0.017(4) Uiso 1 1 calc R . C45 C 0.74918(17) 1.04708(16) 0.35794(9) 0.0209(3) Uani 1 1 d . . C46 C 0.88428(17) 1.13552(16) 0.37791(10) 0.0229(4) Uani 1 1 d . . H46A H 0.9436 1.1239 0.3482 0.030(5) Uiso 1 1 calc R . C47 C 0.93369(18) 1.24068(17) 0.44078(10) 0.0242(4) Uani 1 1 d . . H47A H 1.0262 1.3006 0.4537 0.033(6) Uiso 1 1 calc R . C48 C 0.84828(18) 1.25827(17) 0.48462(10) 0.0240(4) Uani 1 1 d . . C49 C 0.71301(19) 1.17031(18) 0.46548(10) 0.0269(4) Uani 1 1 d . . H49A H 0.6541 1.1821 0.4954 0.033(6) Uiso 1 1 calc R . C50 C 0.66420(18) 1.06569(17) 0.40289(10) 0.0252(4) Uani 1 1 d . . H50A H 0.5718 1.0057 0.3903 0.021(5) Uiso 1 1 calc R . C51 C 0.8999(2) 1.36916(18) 0.55407(11) 0.0299(4) Uani 1 1 d . . F51 F 1.02706(12) 1.45292(11) 0.56144(6) 0.0376(3) Uani 1 1 d . . F52 F 0.90350(14) 1.33953(11) 0.62217(6) 0.0421(3) Uani 1 1 d . . F53 F 0.82291(13) 1.42763(11) 0.55250(7) 0.0410(3) 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 0.0153(2) 0.0136(2) 0.0188(2) 0.00531(17) 0.00536(17) 0.00644(19) C1 0.0149(7) 0.0120(8) 0.0221(7) 0.0045(6) 0.0063(6) 0.0048(6) N1 0.0137(6) 0.0148(7) 0.0151(6) 0.0039(5) 0.0029(5) 0.0048(5) O1 0.0200(6) 0.0190(6) 0.0257(6) 0.0033(5) 0.0083(4) 0.0088(5) C2 0.0211(8) 0.0148(8) 0.0221(8) 0.0047(6) 0.0079(6) 0.0054(7) N2 0.0143(6) 0.0136(7) 0.0168(6) 0.0042(5) 0.0050(5) 0.0054(5) C3 0.0265(9) 0.0215(9) 0.0261(8) 0.0066(7) 0.0140(7) 0.0082(7) N3 0.0169(6) 0.0152(7) 0.0169(6) 0.0062(5) 0.0051(5) 0.0077(6) C4 0.0210(8) 0.0234(9) 0.0401(10) 0.0067(8) 0.0150(7) 0.0094(7) C5 0.0177(8) 0.0224(9) 0.0357(9) 0.0081(7) 0.0074(7) 0.0091(7) C6 0.0175(7) 0.0129(8) 0.0258(8) 0.0060(6) 0.0050(6) 0.0056(6) C7 0.0245(8) 0.0222(9) 0.0179(7) 0.0059(6) 0.0075(6) 0.0086(7) C8 0.0299(9) 0.0252(10) 0.0194(8) 0.0046(7) 0.0047(7) 0.0084(8) C9 0.0353(10) 0.0273(10) 0.0239(8) 0.0098(7) 0.0082(7) 0.0121(8) C10 0.0166(7) 0.0227(9) 0.0238(8) 0.0076(7) 0.0026(6) 0.0086(7) C11 0.0291(9) 0.0285(10) 0.0345(9) 0.0143(8) 0.0052(7) 0.0138(8) C12 0.0290(9) 0.0260(10) 0.0236(8) 0.0069(7) 0.0013(7) 0.0095(8) C13 0.0148(7) 0.0151(8) 0.0127(7) 0.0026(6) 0.0010(5) 0.0049(6) C14 0.0188(7) 0.0148(8) 0.0168(7) 0.0056(6) 0.0065(6) 0.0070(7) C15 0.0185(8) 0.0202(9) 0.0217(8) 0.0077(6) 0.0066(6) 0.0084(7) C16 0.0272(9) 0.0247(9) 0.0266(8) 0.0135(7) 0.0091(7) 0.0141(8) C17 0.0312(9) 0.0192(9) 0.0302(9) 0.0141(7) 0.0132(7) 0.0107(8) C18 0.0212(8) 0.0177(9) 0.0266(8) 0.0070(7) 0.0084(7) 0.0040(7) C19 0.0184(8) 0.0171(8) 0.0195(7) 0.0057(6) 0.0044(6) 0.0065(7) C20 0.0140(7) 0.0143(8) 0.0143(7) 0.0048(6) 0.0020(5) 0.0048(6) C21 0.0175(7) 0.0145(8) 0.0189(7) 0.0057(6) 0.0034(6) 0.0069(6) C22 0.0181(7) 0.0175(8) 0.0182(7) 0.0036(6) 0.0046(6) 0.0097(7) C23 0.0161(7) 0.0196(9) 0.0178(7) 0.0052(6) 0.0056(6) 0.0076(7) C24 0.0139(7) 0.0173(8) 0.0140(7) 0.0050(6) 0.0038(5) 0.0056(6) C25 0.0168(7) 0.0167(8) 0.0157(7) 0.0031(6) 0.0048(6) 0.0077(7) C26 0.0211(8) 0.0131(8) 0.0167(7) 0.0024(6) 0.0068(6) 0.0037(7) C27 0.0239(8) 0.0162(9) 0.0306(9) 0.0049(7) 0.0124(7) 0.0067(7) C28 0.0287(9) 0.0205(9) 0.0452(11) 0.0052(8) 0.0226(8) 0.0080(8) C29 0.0400(11) 0.0221(10) 0.0392(10) 0.0071(8) 0.0298(9) 0.0063(9) C30 0.0392(10) 0.0194(9) 0.0234(8) 0.0065(7) 0.0151(7) 0.0048(8) C31 0.0273(9) 0.0195(9) 0.0174(7) 0.0036(6) 0.0058(6) 0.0072(7) C32 0.0164(7) 0.0139(8) 0.0183(7) 0.0048(6) 0.0085(6) 0.0047(6) C33 0.0169(7) 0.0170(8) 0.0194(7) 0.0069(6) 0.0083(6) 0.0063(7) C34 0.0194(8) 0.0210(9) 0.0191(7) 0.0059(6) 0.0057(6) 0.0053(7) C35 0.0237(8) 0.0150(8) 0.0250(8) 0.0015(7) 0.0082(7) 0.0026(7) C36 0.0276(9) 0.0137(8) 0.0299(9) 0.0091(7) 0.0122(7) 0.0083(7) C37 0.0208(8) 0.0177(8) 0.0219(8) 0.0077(6) 0.0094(6) 0.0081(7) C38 0.0306(9) 0.0183(9) 0.0254(8) 0.0092(7) 0.0070(7) 0.0124(8) C39 0.0395(11) 0.0613(16) 0.0443(12) 0.0233(11) 0.0120(9) 0.0341(12) C40 0.0542(13) 0.0289(11) 0.0333(10) 0.0178(9) 0.0054(9) 0.0136(10) C41 0.0202(8) 0.0188(9) 0.0182(7) 0.0056(6) 0.0039(6) 0.0079(7) C42 0.0281(9) 0.0234(9) 0.0233(8) 0.0110(7) 0.0084(7) 0.0111(8) C43 0.0263(9) 0.0298(10) 0.0355(10) 0.0140(8) 0.0103(7) 0.0160(8) C44 0.0210(8) 0.0211(9) 0.0273(8) 0.0062(7) 0.0088(7) 0.0099(7) C45 0.0236(8) 0.0194(9) 0.0239(8) 0.0093(7) 0.0082(6) 0.0116(7) C46 0.0233(8) 0.0228(9) 0.0258(8) 0.0082(7) 0.0095(7) 0.0120(7) C47 0.0239(8) 0.0231(9) 0.0261(8) 0.0082(7) 0.0065(7) 0.0108(8) C48 0.0320(9) 0.0231(9) 0.0226(8) 0.0098(7) 0.0092(7) 0.0156(8) C49 0.0313(9) 0.0294(10) 0.0285(9) 0.0111(7) 0.0153(7) 0.0181(8) C50 0.0229(8) 0.0238(9) 0.0328(9) 0.0115(7) 0.0115(7) 0.0112(8) C51 0.0388(10) 0.0274(10) 0.0279(9) 0.0097(8) 0.0134(8) 0.0167(9) F51 0.0379(6) 0.0299(6) 0.0318(6) 0.0001(5) 0.0077(5) 0.0078(5) F52 0.0652(8) 0.0364(7) 0.0256(5) 0.0084(5) 0.0171(5) 0.0226(6) F53 0.0483(7) 0.0318(6) 0.0463(7) 0.0028(5) 0.0132(5) 0.0250(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 N2 132.39(6) O1 Al1 N1 96.68(6) N2 Al1 N1 78.43(5) O1 Al1 N3 94.85(6) N2 Al1 N3 79.02(5) N1 Al1 N3 156.92(5) O1 Al1 H1 111.5(6) N2 Al1 H1 115.4(6) N1 Al1 H1 105.6(6) N3 Al1 H1 88.5(6) C2 C1 C6 122.26(14) C2 C1 N1 121.00(13) C6 C1 N1 116.53(14) C13 N1 C1 122.90(14) C13 N1 Al1 115.29(11) C1 N1 Al1 121.35(10) C44 O1 Al1 128.10(10) C3 C2 C1 117.29(15) C3 C2 C7 119.21(15) C1 C2 C7 123.48(14) C20 N2 C24 120.77(13) C20 N2 Al1 119.35(10) C24 N2 Al1 118.36(11) C4 C3 C2 121.49(16) C4 C3 H3A 119.3 C2 C3 H3A 119.3 C32 N3 C25 115.74(12) C32 N3 Al1 121.52(9) C25 N3 Al1 108.51(10) C32 N3 H3 107.0(13) C25 N3 H3 107.3(13) Al1 N3 H3 93.7(13) C5 C4 C3 119.98(15) C5 C4 H4A 120.0 C3 C4 H4A 120.0 C4 C5 C6 121.21(16) C4 C5 H5A 119.4 C6 C5 H5A 119.4 C5 C6 C1 117.76(15) C5 C6 C10 119.71(14) C1 C6 C10 122.50(14) C2 C7 C8 111.13(14) C2 C7 C9 111.30(14) C8 C7 C9 110.53(14) C2 C7 H7A 107.9 C8 C7 H7A 107.9 C9 C7 H7A 107.9 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 C11 112.18(14) C6 C10 C12 111.72(14) C11 C10 C12 109.79(14) C6 C10 H10A 107.6 C11 C10 H10A 107.6 C12 C10 H10A 107.6 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 C14 126.58(14) N1 C13 C20 112.99(14) C14 C13 C20 120.42(13) C15 C14 C19 118.91(15) C15 C14 C13 118.83(14) C19 C14 C13 122.20(14) C16 C15 C14 120.61(15) C16 C15 H15A 119.7 C14 C15 H15A 119.7 C15 C16 C17 120.03(16) C15 C16 H16A 120.0 C17 C16 H16A 120.0 C16 C17 C18 120.07(17) C16 C17 H17A 120.0 C18 C17 H17A 120.0 C17 C18 C19 120.22(16) C17 C18 H18A 119.9 C19 C18 H18A 119.9 C18 C19 C14 120.15(15) C18 C19 H19A 119.9 C14 C19 H19A 119.9 N2 C20 C21 123.33(14) N2 C20 C13 112.78(13) C21 C20 C13 123.47(15) C20 C21 C22 117.27(15) C20 C21 H21A 121.4 C22 C21 H21A 121.4 C23 C22 C21 120.64(14) C23 C22 H22A 119.7 C21 C22 H22A 119.7 C22 C23 C24 121.22(14) C22 C23 H23A 119.4 C24 C23 H23A 119.4 C25 C24 N2 117.40(14) C25 C24 C23 126.07(14) N2 C24 C23 116.48(14) C24 C25 C26 126.54(14) C24 C25 N3 113.88(13) C26 C25 N3 119.47(14) C27 C26 C31 117.33(15) C27 C26 C25 122.00(15) C31 C26 C25 120.67(15) C28 C27 C26 121.20(17) C28 C27 H27A 119.4 C26 C27 H27A 119.4 C29 C28 C27 120.46(18) C29 C28 H28A 119.8 C27 C28 H28A 119.8 C28 C29 C30 119.40(16) C28 C29 H29A 120.3 C30 C29 H29A 120.3 C29 C30 C31 120.08(18) C29 C30 H30A 120.0 C31 C30 H30A 120.0 C30 C31 C26 121.47(17) C30 C31 H31A 119.3 C26 C31 H31A 119.3 C37 C32 C33 121.34(14) C37 C32 N3 119.47(14) C33 C32 N3 119.16(14) C34 C33 C32 117.82(15) C34 C33 C41 118.63(14) C32 C33 C41 123.43(14) C35 C34 C33 121.79(15) C35 C34 H34A 119.1 C33 C34 H34A 119.1 C34 C35 C36 119.43(15) C34 C35 H35A 120.3 C36 C35 H35A 120.3 C35 C36 C37 121.45(16) C35 C36 H36A 119.3 C37 C36 H36A 119.3 C36 C37 C32 118.04(15) C36 C37 C38 118.26(15) C32 C37 C38 123.59(15) C40 C38 C37 113.05(15) C40 C38 C39 110.88(17) C37 C38 C39 110.37(14) C40 C38 H38A 107.4 C37 C38 H38A 107.4 C39 C38 H38A 107.4 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 C33 C41 C43 112.08(14) C33 C41 C42 110.75(13) C43 C41 C42 110.51(14) C33 C41 H41A 107.8 C43 C41 H41A 107.8 C42 C41 H41A 107.8 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 111.71(13) O1 C44 H44A 109.3 C45 C44 H44A 109.3 O1 C44 H44B 109.3 C45 C44 H44B 109.3 H44A C44 H44B 107.9 C46 C45 C50 118.57(16) C46 C45 C44 121.50(15) C50 C45 C44 119.92(16) C47 C46 C45 120.80(16) C47 C46 H46A 119.6 C45 C46 H46A 119.6 C48 C47 C46 120.05(17) C48 C47 H47A 120.0 C46 C47 H47A 120.0 C47 C48 C49 119.76(16) C47 C48 C51 121.12(17) C49 C48 C51 119.10(16) C50 C49 C48 120.04(16) C50 C49 H49A 120.0 C48 C49 H49A 120.0 C49 C50 C45 120.78(17) C49 C50 H50A 119.6 C45 C50 H50A 119.6 F51 C51 F53 106.98(16) F51 C51 F52 104.88(15) F53 C51 F52 106.18(14) F51 C51 C48 113.30(15) F53 C51 C48 112.71(15) F52 C51 C48 112.20(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 O1 1.7353(12) Al1 N2 1.9023(13) Al1 N1 2.0928(14) Al1 N3 2.1832(14) Al1 H1 1.640(17) C1 C2 1.404(2) C1 C6 1.411(2) C1 N1 1.4390(19) N1 C13 1.299(2) O1 C44 1.4096(19) C2 C3 1.396(2) C2 C7 1.526(2) N2 C20 1.366(2) N2 C24 1.3999(19) C3 C4 1.388(3) C3 H3A 0.9500 N3 C32 1.460(2) N3 C25 1.4748(19) N3 H3 0.86(2) C4 C5 1.383(3) C4 H4A 0.9500 C5 C6 1.391(2) C5 H5A 0.9500 C6 C10 1.524(2) C7 C8 1.531(2) C7 C9 1.533(3) C7 H7A 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 C11 1.526(2) C10 C12 1.531(2) C10 H10A 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 C14 1.475(2) C13 C20 1.480(2) C14 C15 1.399(2) C14 C19 1.400(2) C15 C16 1.384(3) C15 H15A 0.9500 C16 C17 1.387(3) C16 H16A 0.9500 C17 C18 1.387(3) C17 H17A 0.9500 C18 C19 1.390(3) C18 H18A 0.9500 C19 H19A 0.9500 C20 C21 1.368(2) C21 C22 1.432(2) C21 H21A 0.9500 C22 C23 1.354(2) C22 H22A 0.9500 C23 C24 1.449(2) C23 H23A 0.9500 C24 C25 1.362(2) C25 C26 1.474(2) C26 C27 1.401(2) C26 C31 1.401(2) C27 C28 1.392(3) C27 H27A 0.9500 C28 C29 1.386(3) C28 H28A 0.9500 C29 C30 1.387(3) C29 H29A 0.9500 C30 C31 1.393(3) C30 H30A 0.9500 C31 H31A 0.9500 C32 C37 1.406(2) C32 C33 1.408(2) C33 C34 1.395(2) C33 C41 1.522(2) C34 C35 1.381(3) C34 H34A 0.9500 C35 C36 1.384(3) C35 H35A 0.9500 C36 C37 1.398(2) C36 H36A 0.9500 C37 C38 1.525(2) C38 C40 1.522(3) C38 C39 1.527(3) C38 H38A 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 1.530(2) C41 C42 1.536(2) C41 H41A 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 1.515(2) C44 H44A 0.9900 C44 H44B 0.9900 C45 C46 1.390(2) C45 C50 1.397(2) C46 C47 1.389(2) C46 H46A 0.9500 C47 C48 1.384(2) C47 H47A 0.9500 C48 C49 1.390(3) C48 C51 1.498(2) C49 C50 1.383(3) C49 H49A 0.9500 C50 H50A 0.9500 C51 F51 1.338(2) C51 F53 1.339(2) C51 F52 1.350(2) 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 72.3(2) C6 C1 N1 C13 -112.68(17) C2 C1 N1 Al1 -99.52(16) C6 C1 N1 Al1 75.47(16) N2 Al1 O1 C44 -156.52(13) N1 Al1 O1 C44 -76.11(14) N3 Al1 O1 C44 123.92(14) C6 C1 C2 C3 -1.1(2) N1 C1 C2 C3 173.56(15) C6 C1 C2 C7 -179.63(15) N1 C1 C2 C7 -4.9(2) C1 C2 C3 C4 0.0(3) C7 C2 C3 C4 178.61(16) C2 C3 C4 C5 0.8(3) C3 C4 C5 C6 -0.6(3) C4 C5 C6 C1 -0.4(3) C4 C5 C6 C10 177.72(16) C2 C1 C6 C5 1.3(2) N1 C1 C6 C5 -173.59(15) C2 C1 C6 C10 -176.77(16) N1 C1 C6 C10 8.3(2) C3 C2 C7 C8 -66.6(2) C1 C2 C7 C8 111.83(18) C3 C2 C7 C9 57.0(2) C1 C2 C7 C9 -124.52(17) C5 C6 C10 C11 56.3(2) C1 C6 C10 C11 -125.65(17) C5 C6 C10 C12 -67.5(2) C1 C6 C10 C12 110.59(17) C1 N1 C13 C14 -3.4(2) Al1 N1 C13 C14 168.89(11) C1 N1 C13 C20 177.94(12) Al1 N1 C13 C20 -9.75(15) N1 C13 C14 C15 -131.55(16) C20 C13 C14 C15 47.0(2) N1 C13 C14 C19 45.5(2) C20 C13 C14 C19 -135.97(15) C19 C14 C15 C16 -0.8(2) C13 C14 C15 C16 176.37(14) C14 C15 C16 C17 0.8(2) C15 C16 C17 C18 -0.3(3) C16 C17 C18 C19 -0.3(3) C17 C18 C19 C14 0.3(2) C15 C14 C19 C18 0.2(2) C13 C14 C19 C18 -176.84(14) C24 N2 C20 C21 -2.0(2) Al1 N2 C20 C21 163.69(11) C24 N2 C20 C13 -174.84(12) Al1 N2 C20 C13 -9.14(16) N1 C13 C20 N2 12.12(18) C14 C13 C20 N2 -166.61(13) N1 C13 C20 C21 -160.70(14) C14 C13 C20 C21 20.6(2) N2 C20 C21 C22 -2.7(2) C13 C20 C21 C22 169.40(13) C20 C21 C22 C23 3.5(2) C21 C22 C23 C24 0.1(2) C20 N2 C24 C25 -176.87(13) Al1 N2 C24 C25 17.29(17) C20 N2 C24 C23 5.56(19) Al1 N2 C24 C23 -160.27(10) C22 C23 C24 C25 178.03(15) C22 C23 C24 N2 -4.7(2) N2 C24 C25 C26 178.30(13) C23 C24 C25 C26 -4.4(2) N2 C24 C25 N3 -5.37(19) C23 C24 C25 N3 171.92(13) C32 N3 C25 C24 134.14(14) Al1 N3 C25 C24 -6.52(15) C32 N3 C25 C26 -49.25(18) Al1 N3 C25 C26 170.09(11) C24 C25 C26 C27 -40.7(2) N3 C25 C26 C27 143.17(15) C24 C25 C26 C31 140.40(16) N3 C25 C26 C31 -35.7(2) C31 C26 C27 C28 -2.8(2) C25 C26 C27 C28 178.31(15) C26 C27 C28 C29 1.0(3) C27 C28 C29 C30 1.0(3) C28 C29 C30 C31 -1.0(3) C29 C30 C31 C26 -0.8(3) C27 C26 C31 C30 2.7(2) C25 C26 C31 C30 -178.37(15) C25 N3 C32 C37 120.62(15) Al1 N3 C32 C37 -104.23(14) C25 N3 C32 C33 -61.02(18) Al1 N3 C32 C33 74.13(16) C37 C32 C33 C34 -4.0(2) N3 C32 C33 C34 177.68(13) C37 C32 C33 C41 171.99(14) N3 C32 C33 C41 -6.3(2) C32 C33 C34 C35 2.1(2) C41 C33 C34 C35 -174.10(14) C33 C34 C35 C36 0.8(2) C34 C35 C36 C37 -1.9(3) C35 C36 C37 C32 0.0(2) C35 C36 C37 C38 176.27(15) C33 C32 C37 C36 3.0(2) N3 C32 C37 C36 -178.70(14) C33 C32 C37 C38 -173.06(15) N3 C32 C37 C38 5.3(2) C36 C37 C38 C40 47.1(2) C32 C37 C38 C40 -136.86(17) C36 C37 C38 C39 -77.7(2) C32 C37 C38 C39 98.3(2) C34 C33 C41 C43 -63.64(19) C32 C33 C41 C43 120.40(16) C34 C33 C41 C42 60.27(19) C32 C33 C41 C42 -115.68(16) Al1 O1 C44 C45 -162.93(11) O1 C44 C45 C46 27.7(2) O1 C44 C45 C50 -153.14(15) C50 C45 C46 C47 -0.5(3) C44 C45 C46 C47 178.62(16) C45 C46 C47 C48 0.2(3) C46 C47 C48 C49 0.0(3) C46 C47 C48 C51 178.30(16) C47 C48 C49 C50 0.0(3) C51 C48 C49 C50 -178.28(17) C48 C49 C50 C45 -0.3(3) C46 C45 C50 C49 0.6(3) C44 C45 C50 C49 -178.59(16) C47 C48 C51 F51 8.4(2) C49 C48 C51 F51 -173.33(16) C47 C48 C51 F53 130.05(18) C49 C48 C51 F53 -51.7(2) C47 C48 C51 F52 -110.14(19) C49 C48 C51 F52 68.1(2)