#------------------------------------------------------------------------------ #$Date: 2020-04-23 00:57:24 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251058 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557862.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_1557862 loop_ _publ_author_name 'Navarro, Marta' 'S\'ANCHEZ-BARBA MERLO, LUIS FERNANDO' 'Garc\'es Osado, Andr\'es' 'Juan, Fernandez-Baeza' 'Fernandez, Israel' 'Lara, Agustin' 'Rodr\'iguez, Ana Mar\'ia' _publ_section_title ; Bimetallic Scorpionate-based Helical Organoaluminums for the Efficient Carbon Dioxide Fixation into a Variety of Cyclic Carbonates ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D0CY00593B _journal_year 2020 _chemical_formula_moiety 'C20 H35 Al N6' _chemical_formula_sum 'C20 H35 Al N6' _chemical_formula_weight 386.52 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2020-03-24 deposited with the CCDC. 2020-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.8949(6) _cell_length_b 10.1078(4) _cell_length_c 23.9918(7) _cell_measurement_reflns_used 4273 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 21.358 _cell_measurement_theta_min 2.438 _cell_volume 4582.1(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_unetI/netI 0.0729 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 55093 _diffrn_reflns_point_group_measured_fraction_full 0.947 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 2.744 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.121 _exptl_crystal_description prism _exptl_crystal_F_000 1680 _exptl_crystal_size_max 0.147 _exptl_crystal_size_mid 0.144 _exptl_crystal_size_min 0.089 _refine_diff_density_max 0.316 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Flack x determined using 2314 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.08(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 507 _refine_ls_number_reflns 7935 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0463 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.5682P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.1064 _reflns_Friedel_coverage 0.847 _reflns_Friedel_fraction_full 0.893 _reflns_Friedel_fraction_max 0.891 _reflns_number_gt 6122 _reflns_number_total 7935 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy00593b3.cif _cod_data_source_block 1 _cod_database_code 1557862 _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 0.985 _shelx_estimated_absorpt_t_max 0.991 _shelxl_version_number 2013-4 _shelx_res_file ; TITL 02582 in Pna2(1) CELL 0.71073 18.8949 10.1078 23.9918 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0004 0.0007 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N AL UNIT 160 280 48 8 MERG 2 OMIT 2 0 2 OMIT 0 0 2 OMIT 0 1 1 OMIT 2 0 0 OMIT 0 1 -1 OMIT 1 1 0 OMIT 2 0 1 HTAB C16 N6 OMIT 1 1 -2 FMAP 2 PLAN 3 SIZE 0.089 0.144 0.147 ACTA BOND $H CONF L.S. 30 TEMP -163.15 WGHT 0.052000 0.568200 FVAR 0.07534 AL1 4 0.666962 0.711433 0.628548 11.00000 0.02033 0.01886 = 0.03029 -0.00393 0.00158 -0.00236 AL2 4 0.571351 0.553374 0.321927 11.00000 0.02274 0.03552 = 0.02364 0.00172 0.00155 -0.00275 C1 1 0.551582 0.934234 0.616182 11.00000 0.01612 0.02010 = 0.02508 -0.00105 0.00123 0.00060 C2 1 0.620235 0.974921 0.621658 11.00000 0.02226 0.02307 = 0.01663 0.00114 0.00212 -0.00116 C3 1 0.532827 0.596961 0.582089 11.00000 0.02520 0.03433 = 0.03507 -0.01157 0.00618 -0.01367 C4 1 0.474015 0.645737 0.554812 11.00000 0.02795 0.04940 = 0.02747 -0.01006 0.00513 -0.01932 AFIX 43 H4 2 0.439577 0.595169 0.535358 11.00000 -1.20000 AFIX 0 C5 1 0.474463 0.781026 0.560989 11.00000 0.01852 0.05274 = 0.01913 0.00096 0.00025 -0.00690 C6 1 0.557222 0.456897 0.587350 11.00000 0.05003 0.02987 = 0.07100 -0.01610 0.00561 -0.01505 AFIX 137 H6A 2 0.579011 0.443806 0.624006 11.00000 -1.50000 H6B 2 0.592005 0.437775 0.558141 11.00000 -1.50000 H6C 2 0.516650 0.397248 0.583355 11.00000 -1.50000 AFIX 0 C7 1 0.424734 0.883540 0.540653 11.00000 0.02639 0.06820 = 0.02845 0.00773 -0.00832 -0.00511 AFIX 137 H7A 2 0.451572 0.958296 0.525493 11.00000 -1.50000 H7B 2 0.395120 0.914144 0.571610 11.00000 -1.50000 H7C 2 0.394613 0.845995 0.511403 11.00000 -1.50000 AFIX 0 C8 1 0.449310 0.962049 0.680474 11.00000 0.02318 0.03797 = 0.02012 0.00247 0.00216 -0.00017 C9 1 0.401132 1.062055 0.688035 11.00000 0.02022 0.04323 = 0.03564 -0.00022 0.00625 0.00521 AFIX 43 H9 2 0.362609 1.062628 0.713479 11.00000 -1.20000 AFIX 0 C10 1 0.419847 1.163095 0.650917 11.00000 0.02238 0.03575 = 0.03867 -0.00133 -0.00183 0.00603 C11 1 0.456680 0.830477 0.707075 11.00000 0.02862 0.03986 = 0.03382 0.00785 0.00344 0.00079 AFIX 137 H11A 2 0.506982 0.809857 0.711939 11.00000 -1.50000 H11B 2 0.434652 0.763139 0.683354 11.00000 -1.50000 H11C 2 0.433281 0.831412 0.743527 11.00000 -1.50000 AFIX 0 C12 1 0.386690 1.294656 0.642899 11.00000 0.03213 0.04402 = 0.05531 -0.00018 -0.00482 0.01550 AFIX 137 H12A 2 0.394474 1.324356 0.604502 11.00000 -1.50000 H12B 2 0.407927 1.358279 0.668789 11.00000 -1.50000 H12C 2 0.335752 1.288299 0.650106 11.00000 -1.50000 AFIX 0 C13 1 0.670808 1.131966 0.690024 11.00000 0.02661 0.02140 = 0.02794 -0.00361 0.00097 0.00130 AFIX 13 H13 2 0.717083 1.084107 0.688421 11.00000 -1.20000 AFIX 0 C14 1 0.629832 1.080371 0.739749 11.00000 0.05284 0.04911 = 0.02549 -0.00401 0.00145 -0.01292 AFIX 137 H14A 2 0.621206 0.985396 0.735137 11.00000 -1.50000 H14B 2 0.584493 1.127014 0.742454 11.00000 -1.50000 H14C 2 0.657290 1.095325 0.773825 11.00000 -1.50000 AFIX 0 C15 1 0.685899 1.277644 0.694404 11.00000 0.04691 0.02919 = 0.04536 -0.00661 -0.00986 -0.00314 AFIX 137 H15A 2 0.641382 1.325892 0.699516 11.00000 -1.50000 H15B 2 0.709133 1.308027 0.660202 11.00000 -1.50000 H15C 2 0.717018 1.293966 0.726351 11.00000 -1.50000 AFIX 0 C16 1 0.744319 0.950453 0.595222 11.00000 0.01895 0.02213 = 0.03110 -0.00355 0.00840 -0.00582 AFIX 13 H16 2 0.742283 1.048101 0.601724 11.00000 -1.20000 AFIX 0 C17 1 0.756372 0.926610 0.532949 11.00000 0.03235 0.03900 = 0.03762 -0.00817 0.01439 -0.01038 AFIX 137 H17A 2 0.717310 0.965548 0.511667 11.00000 -1.50000 H17B 2 0.758466 0.831260 0.525733 11.00000 -1.50000 H17C 2 0.801059 0.967753 0.521571 11.00000 -1.50000 AFIX 0 C18 1 0.804183 0.893988 0.630156 11.00000 0.01821 0.03025 = 0.04264 -0.00629 0.00103 -0.00409 AFIX 137 H18A 2 0.806430 0.797935 0.624888 11.00000 -1.50000 H18B 2 0.795642 0.913733 0.669577 11.00000 -1.50000 H18C 2 0.849097 0.933870 0.618537 11.00000 -1.50000 AFIX 0 C19 1 0.674399 0.668882 0.708003 11.00000 0.03776 0.02817 = 0.04023 0.00099 -0.00693 -0.00397 AFIX 137 H19A 2 0.659786 0.745646 0.730142 11.00000 -1.50000 H19B 2 0.723511 0.646139 0.716985 11.00000 -1.50000 H19C 2 0.643619 0.593578 0.716626 11.00000 -1.50000 AFIX 0 C20 1 0.720200 0.592664 0.579239 11.00000 0.02922 0.02446 = 0.05604 -0.01010 0.00915 -0.00174 AFIX 137 H20A 2 0.770919 0.611220 0.582680 11.00000 -1.50000 H20B 2 0.705264 0.606852 0.540581 11.00000 -1.50000 H20C 2 0.710997 0.500623 0.589835 11.00000 -1.50000 AFIX 0 C21 1 0.485549 0.411375 0.412878 11.00000 0.01888 0.02250 = 0.02558 -0.00167 0.00350 0.00008 C22 1 0.474188 0.543070 0.405771 11.00000 0.01997 0.02771 = 0.01712 -0.00278 -0.00356 -0.00184 C23 1 0.647596 0.299272 0.359107 11.00000 0.03376 0.05159 = 0.02948 -0.00344 0.00250 0.01368 C24 1 0.642740 0.214752 0.403922 11.00000 0.03731 0.04412 = 0.03478 0.00030 -0.00097 0.01891 AFIX 43 H24 2 0.675233 0.146665 0.413420 11.00000 -1.20000 AFIX 0 C25 1 0.581924 0.247435 0.432406 11.00000 0.03819 0.02839 = 0.02529 -0.00305 -0.00367 0.00889 C26 1 0.704250 0.306530 0.315075 11.00000 0.03722 0.08388 = 0.04076 0.00602 0.01104 0.02257 AFIX 137 H26A 2 0.735888 0.380962 0.323094 11.00000 -1.50000 H26B 2 0.682245 0.319327 0.278481 11.00000 -1.50000 H26C 2 0.731489 0.224023 0.314992 11.00000 -1.50000 AFIX 0 C27 1 0.550385 0.186080 0.482846 11.00000 0.05528 0.02970 = 0.03129 0.00433 -0.00162 0.00645 AFIX 137 H27A 2 0.515453 0.119536 0.471635 11.00000 -1.50000 H27B 2 0.527164 0.254447 0.505305 11.00000 -1.50000 H27C 2 0.587719 0.143756 0.504892 11.00000 -1.50000 AFIX 0 C28 1 0.406784 0.220978 0.391300 11.00000 0.04107 0.02314 = 0.02815 -0.00054 -0.00382 -0.00044 C29 1 0.352462 0.161476 0.419939 11.00000 0.04437 0.01996 = 0.04171 -0.00009 -0.00749 -0.00831 AFIX 43 H29 2 0.325636 0.086979 0.408256 11.00000 -1.20000 AFIX 0 C30 1 0.344427 0.231862 0.469509 11.00000 0.03455 0.02195 = 0.03580 0.00659 -0.00226 -0.00497 C31 1 0.439165 0.194013 0.336077 11.00000 0.05523 0.03216 = 0.03088 -0.00526 -0.00175 -0.00173 AFIX 137 H31A 2 0.487707 0.162139 0.341237 11.00000 -1.50000 H31B 2 0.439801 0.275554 0.313984 11.00000 -1.50000 H31C 2 0.411361 0.126545 0.316556 11.00000 -1.50000 AFIX 0 C32 1 0.292251 0.207637 0.514799 11.00000 0.04429 0.04006 = 0.04714 0.01158 0.00931 -0.00921 AFIX 137 H32A 2 0.280173 0.291703 0.532789 11.00000 -1.50000 H32B 2 0.312808 0.147397 0.542408 11.00000 -1.50000 H32C 2 0.249396 0.167849 0.499038 11.00000 -1.50000 AFIX 0 C33 1 0.365347 0.661051 0.378140 11.00000 0.02633 0.03043 = 0.02115 0.00460 -0.00458 -0.00183 AFIX 13 H33 2 0.397301 0.687429 0.346828 11.00000 -1.20000 AFIX 0 C34 1 0.311134 0.564002 0.355433 11.00000 0.03714 0.04155 = 0.04879 0.00283 -0.01801 -0.00721 AFIX 137 H34A 2 0.279303 0.536423 0.385517 11.00000 -1.50000 H34B 2 0.335506 0.486320 0.340300 11.00000 -1.50000 H34C 2 0.283624 0.606663 0.325834 11.00000 -1.50000 AFIX 0 C35 1 0.331052 0.784580 0.400835 11.00000 0.03710 0.03722 = 0.03702 0.00219 -0.00749 0.00991 AFIX 137 H35A 2 0.367756 0.846027 0.413592 11.00000 -1.50000 H35B 2 0.300224 0.761271 0.432182 11.00000 -1.50000 H35C 2 0.302896 0.826698 0.371477 11.00000 -1.50000 AFIX 0 C36 1 0.531568 0.758913 0.407159 11.00000 0.03007 0.02476 = 0.03172 0.00105 -0.00096 -0.00802 AFIX 13 H36 2 0.490185 0.774644 0.432282 11.00000 -1.20000 AFIX 0 C37 1 0.530282 0.864957 0.361562 11.00000 0.05807 0.02991 = 0.04757 0.00869 -0.00994 -0.00801 AFIX 137 H37A 2 0.485076 0.860895 0.341611 11.00000 -1.50000 H37B 2 0.569170 0.849294 0.335352 11.00000 -1.50000 H37C 2 0.535778 0.952529 0.378551 11.00000 -1.50000 AFIX 0 C38 1 0.598639 0.768797 0.442241 11.00000 0.03250 0.04328 = 0.04120 -0.00380 -0.00415 -0.01256 AFIX 137 H38A 2 0.640191 0.760446 0.418050 11.00000 -1.50000 H38B 2 0.599027 0.697678 0.470002 11.00000 -1.50000 H38C 2 0.599812 0.854621 0.461222 11.00000 -1.50000 AFIX 0 C39 1 0.506301 0.524668 0.260012 11.00000 0.03525 0.03109 = 0.03290 0.00312 -0.00366 -0.00251 AFIX 137 H39A 2 0.497442 0.608851 0.240986 11.00000 -1.50000 H39B 2 0.461557 0.489090 0.274225 11.00000 -1.50000 H39C 2 0.527210 0.461637 0.233703 11.00000 -1.50000 AFIX 0 C40 1 0.661827 0.635032 0.301375 11.00000 0.03153 0.06437 = 0.03912 0.00236 0.00439 -0.01000 AFIX 137 H40A 2 0.693844 0.633422 0.333504 11.00000 -1.50000 H40B 2 0.653742 0.726831 0.289878 11.00000 -1.50000 H40C 2 0.683102 0.585643 0.270475 11.00000 -1.50000 AFIX 0 N1 3 0.568322 0.697409 0.605347 11.00000 0.02429 0.02372 = 0.02521 -0.00340 0.00292 -0.00313 N2 3 0.532506 0.811282 0.592105 11.00000 0.01768 0.02861 = 0.02251 -0.00103 0.00083 -0.00167 N3 3 0.493926 1.004379 0.639841 11.00000 0.01629 0.02573 = 0.02577 0.00293 0.00103 0.00303 N4 3 0.475839 1.128617 0.620170 11.00000 0.02162 0.02975 = 0.03607 0.00510 -0.00015 0.00731 N5 3 0.675921 0.892540 0.612516 11.00000 0.01477 0.02017 = 0.02752 -0.00329 0.00386 -0.00377 N6 3 0.632568 1.106408 0.637498 11.00000 0.02457 0.01634 = 0.02561 0.00548 -0.00115 -0.00091 AFIX 43 H6 2 0.617810 1.172333 0.616549 11.00000 -1.20000 AFIX 0 N7 3 0.592533 0.383162 0.358748 11.00000 0.02261 0.04116 = 0.02434 0.00048 0.00343 0.00389 N8 3 0.552321 0.350184 0.404874 11.00000 0.02570 0.02768 = 0.02356 -0.00135 0.00210 0.00289 N9 3 0.429835 0.321328 0.424250 11.00000 0.02854 0.01960 = 0.02314 0.00061 0.00216 -0.00273 N10 3 0.391932 0.328646 0.473200 11.00000 0.02908 0.02393 = 0.02759 -0.00105 0.00434 -0.00389 N11 3 0.524577 0.624295 0.383591 11.00000 0.02677 0.02288 = 0.02236 0.00034 0.00159 -0.00557 N12 3 0.409086 0.595906 0.421608 11.00000 0.02428 0.02663 = 0.01545 -0.00270 0.00032 0.00334 AFIX 43 H12 2 0.394348 0.590803 0.456336 11.00000 -1.20000 AFIX 0 HKLF 4 REM 02582 in Pna2(1) REM R1 = 0.0463 for 6122 Fo > 4sig(Fo) and 0.0751 for all 7935 data REM 507 parameters refined using 1 restraints END WGHT 0.0433 0.9292 REM Highest difference peak 0.316, deepest hole -0.331, 1-sigma level 0.044 Q1 1 0.5869 1.1521 0.6395 11.00000 0.05 0.32 Q2 1 0.3829 0.5184 0.4380 11.00000 0.05 0.28 Q3 1 0.5232 0.5293 0.2043 11.00000 0.05 0.18 ; _shelx_res_checksum 60693 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.66696(6) 0.71143(12) 0.62855(5) 0.0232(3) Uani 1 1 d . . . . . Al2 Al 0.57135(6) 0.55337(13) 0.32193(5) 0.0273(3) Uani 1 1 d . . . . . C1 C 0.55158(18) 0.9342(4) 0.61618(17) 0.0204(9) Uani 1 1 d . . . . . C2 C 0.6202(2) 0.9749(4) 0.62166(16) 0.0207(8) Uani 1 1 d . . . . . C3 C 0.5328(2) 0.5970(5) 0.58209(19) 0.0315(11) Uani 1 1 d . . . . . C4 C 0.4740(2) 0.6457(5) 0.55481(18) 0.0349(11) Uani 1 1 d . . . . . H4 H 0.4396 0.5952 0.5354 0.042 Uiso 1 1 calc R U . . . C5 C 0.4745(2) 0.7810(5) 0.56099(17) 0.0301(11) Uani 1 1 d . . . . . C6 C 0.5572(3) 0.4569(5) 0.5874(3) 0.0503(14) Uani 1 1 d . . . . . H6A H 0.5790 0.4438 0.6240 0.075 Uiso 1 1 calc R U . . . H6B H 0.5920 0.4378 0.5581 0.075 Uiso 1 1 calc R U . . . H6C H 0.5166 0.3972 0.5834 0.075 Uiso 1 1 calc R U . . . C7 C 0.4247(2) 0.8835(5) 0.54065(19) 0.0410(13) Uani 1 1 d . . . . . H7A H 0.4516 0.9583 0.5255 0.062 Uiso 1 1 calc R U . . . H7B H 0.3951 0.9141 0.5716 0.062 Uiso 1 1 calc R U . . . H7C H 0.3946 0.8460 0.5114 0.062 Uiso 1 1 calc R U . . . C8 C 0.4493(2) 0.9620(4) 0.68047(17) 0.0271(10) Uani 1 1 d . . . . . C9 C 0.4011(2) 1.0621(5) 0.68804(19) 0.0330(10) Uani 1 1 d . . . . . H9 H 0.3626 1.0626 0.7135 0.040 Uiso 1 1 calc R U . . . C10 C 0.4198(2) 1.1631(5) 0.65092(19) 0.0323(11) Uani 1 1 d . . . . . C11 C 0.4567(2) 0.8305(5) 0.70708(19) 0.0341(11) Uani 1 1 d . . . . . H11A H 0.5070 0.8099 0.7119 0.051 Uiso 1 1 calc R U . . . H11B H 0.4347 0.7631 0.6834 0.051 Uiso 1 1 calc R U . . . H11C H 0.4333 0.8314 0.7435 0.051 Uiso 1 1 calc R U . . . C12 C 0.3867(2) 1.2947(5) 0.6429(2) 0.0438(13) Uani 1 1 d . . . . . H12A H 0.3945 1.3244 0.6045 0.066 Uiso 1 1 calc R U . . . H12B H 0.4079 1.3583 0.6688 0.066 Uiso 1 1 calc R U . . . H12C H 0.3358 1.2883 0.6501 0.066 Uiso 1 1 calc R U . . . C13 C 0.6708(2) 1.1320(4) 0.69002(17) 0.0253(9) Uani 1 1 d . . . . . H13 H 0.7171 1.0841 0.6884 0.030 Uiso 1 1 calc R U . . . C14 C 0.6298(3) 1.0804(5) 0.73975(19) 0.0425(12) Uani 1 1 d . . . . . H14A H 0.6212 0.9854 0.7351 0.064 Uiso 1 1 calc R U . . . H14B H 0.5845 1.1270 0.7425 0.064 Uiso 1 1 calc R U . . . H14C H 0.6573 1.0953 0.7738 0.064 Uiso 1 1 calc R U . . . C15 C 0.6859(3) 1.2776(5) 0.6944(2) 0.0405(12) Uani 1 1 d . . . . . H15A H 0.6414 1.3259 0.6995 0.061 Uiso 1 1 calc R U . . . H15B H 0.7091 1.3080 0.6602 0.061 Uiso 1 1 calc R U . . . H15C H 0.7170 1.2940 0.7264 0.061 Uiso 1 1 calc R U . . . C16 C 0.74432(19) 0.9505(4) 0.59522(17) 0.0241(9) Uani 1 1 d . . . . . H16 H 0.7423 1.0481 0.6017 0.029 Uiso 1 1 calc R U . . . C17 C 0.7564(2) 0.9266(5) 0.53295(18) 0.0363(12) Uani 1 1 d . . . . . H17A H 0.7173 0.9655 0.5117 0.054 Uiso 1 1 calc R U . . . H17B H 0.7585 0.8313 0.5257 0.054 Uiso 1 1 calc R U . . . H17C H 0.8011 0.9678 0.5216 0.054 Uiso 1 1 calc R U . . . C18 C 0.80418(19) 0.8940(4) 0.63016(19) 0.0304(10) Uani 1 1 d . . . . . H18A H 0.8064 0.7979 0.6249 0.046 Uiso 1 1 calc R U . . . H18B H 0.7956 0.9137 0.6696 0.046 Uiso 1 1 calc R U . . . H18C H 0.8491 0.9339 0.6185 0.046 Uiso 1 1 calc R U . . . C19 C 0.6744(2) 0.6689(5) 0.70800(19) 0.0354(11) Uani 1 1 d . . . . . H19A H 0.6598 0.7456 0.7301 0.053 Uiso 1 1 calc R U . . . H19B H 0.7235 0.6461 0.7170 0.053 Uiso 1 1 calc R U . . . H19C H 0.6436 0.5936 0.7166 0.053 Uiso 1 1 calc R U . . . C20 C 0.7202(2) 0.5927(5) 0.5792(2) 0.0366(12) Uani 1 1 d . . . . . H20A H 0.7709 0.6112 0.5827 0.055 Uiso 1 1 calc R U . . . H20B H 0.7053 0.6069 0.5406 0.055 Uiso 1 1 calc R U . . . H20C H 0.7110 0.5006 0.5898 0.055 Uiso 1 1 calc R U . . . C21 C 0.4855(2) 0.4114(4) 0.41288(17) 0.0223(9) Uani 1 1 d . . . . . C22 C 0.4742(2) 0.5431(4) 0.40577(16) 0.0216(9) Uani 1 1 d . . . . . C23 C 0.6476(2) 0.2993(5) 0.35911(19) 0.0383(12) Uani 1 1 d . . . . . C24 C 0.6427(3) 0.2148(5) 0.40392(19) 0.0387(12) Uani 1 1 d . . . . . H24 H 0.6752 0.1467 0.4134 0.046 Uiso 1 1 calc R U . . . C25 C 0.5819(2) 0.2474(4) 0.43241(18) 0.0306(10) Uani 1 1 d . . . . . C26 C 0.7042(3) 0.3065(6) 0.3151(2) 0.0540(15) Uani 1 1 d . . . . . H26A H 0.7359 0.3810 0.3231 0.081 Uiso 1 1 calc R U . . . H26B H 0.6822 0.3193 0.2785 0.081 Uiso 1 1 calc R U . . . H26C H 0.7315 0.2240 0.3150 0.081 Uiso 1 1 calc R U . . . C27 C 0.5504(3) 0.1861(5) 0.48285(19) 0.0388(12) Uani 1 1 d . . . . . H27A H 0.5155 0.1195 0.4716 0.058 Uiso 1 1 calc R U . . . H27B H 0.5272 0.2544 0.5053 0.058 Uiso 1 1 calc R U . . . H27C H 0.5877 0.1438 0.5049 0.058 Uiso 1 1 calc R U . . . C28 C 0.4068(2) 0.2210(4) 0.39130(18) 0.0308(11) Uani 1 1 d . . . . . C29 C 0.3525(2) 0.1615(4) 0.4199(2) 0.0353(11) Uani 1 1 d . . . . . H29 H 0.3256 0.0870 0.4083 0.042 Uiso 1 1 calc R U . . . C30 C 0.3444(2) 0.2319(4) 0.46951(19) 0.0308(10) Uani 1 1 d . . . . . C31 C 0.4392(3) 0.1940(5) 0.33608(18) 0.0394(12) Uani 1 1 d . . . . . H31A H 0.4877 0.1621 0.3412 0.059 Uiso 1 1 calc R U . . . H31B H 0.4398 0.2756 0.3140 0.059 Uiso 1 1 calc R U . . . H31C H 0.4114 0.1265 0.3166 0.059 Uiso 1 1 calc R U . . . C32 C 0.2923(3) 0.2076(5) 0.5148(2) 0.0438(13) Uani 1 1 d . . . . . H32A H 0.2802 0.2917 0.5328 0.066 Uiso 1 1 calc R U . . . H32B H 0.3128 0.1474 0.5424 0.066 Uiso 1 1 calc R U . . . H32C H 0.2494 0.1678 0.4990 0.066 Uiso 1 1 calc R U . . . C33 C 0.3653(2) 0.6611(4) 0.37814(17) 0.0260(10) Uani 1 1 d . . . . . H33 H 0.3973 0.6874 0.3468 0.031 Uiso 1 1 calc R U . . . C34 C 0.3111(2) 0.5640(5) 0.3554(2) 0.0425(13) Uani 1 1 d . . . . . H34A H 0.2793 0.5364 0.3855 0.064 Uiso 1 1 calc R U . . . H34B H 0.3355 0.4863 0.3403 0.064 Uiso 1 1 calc R U . . . H34C H 0.2836 0.6067 0.3258 0.064 Uiso 1 1 calc R U . . . C35 C 0.3311(2) 0.7846(5) 0.4008(2) 0.0371(11) Uani 1 1 d . . . . . H35A H 0.3678 0.8460 0.4136 0.056 Uiso 1 1 calc R U . . . H35B H 0.3002 0.7613 0.4322 0.056 Uiso 1 1 calc R U . . . H35C H 0.3029 0.8267 0.3715 0.056 Uiso 1 1 calc R U . . . C36 C 0.5316(2) 0.7589(4) 0.40716(18) 0.0288(10) Uani 1 1 d . . . . . H36 H 0.4902 0.7746 0.4323 0.035 Uiso 1 1 calc R U . . . C37 C 0.5303(3) 0.8650(5) 0.3616(2) 0.0452(13) Uani 1 1 d . . . . . H37A H 0.4851 0.8609 0.3416 0.068 Uiso 1 1 calc R U . . . H37B H 0.5692 0.8493 0.3354 0.068 Uiso 1 1 calc R U . . . H37C H 0.5358 0.9525 0.3786 0.068 Uiso 1 1 calc R U . . . C38 C 0.5986(2) 0.7688(5) 0.4422(2) 0.0390(12) Uani 1 1 d . . . . . H38A H 0.6402 0.7604 0.4180 0.058 Uiso 1 1 calc R U . . . H38B H 0.5990 0.6977 0.4700 0.058 Uiso 1 1 calc R U . . . H38C H 0.5998 0.8546 0.4612 0.058 Uiso 1 1 calc R U . . . C39 C 0.5063(2) 0.5247(5) 0.26001(18) 0.0331(11) Uani 1 1 d . . . . . H39A H 0.4974 0.6089 0.2410 0.050 Uiso 1 1 calc R U . . . H39B H 0.4616 0.4891 0.2742 0.050 Uiso 1 1 calc R U . . . H39C H 0.5272 0.4616 0.2337 0.050 Uiso 1 1 calc R U . . . C40 C 0.6618(2) 0.6350(6) 0.3014(2) 0.0450(14) Uani 1 1 d . . . . . H40A H 0.6938 0.6334 0.3335 0.068 Uiso 1 1 calc R U . . . H40B H 0.6537 0.7268 0.2899 0.068 Uiso 1 1 calc R U . . . H40C H 0.6831 0.5856 0.2705 0.068 Uiso 1 1 calc R U . . . N1 N 0.56832(16) 0.6974(3) 0.60535(14) 0.0244(8) Uani 1 1 d . . . . . N2 N 0.53251(16) 0.8113(3) 0.59211(13) 0.0229(8) Uani 1 1 d . . . . . N3 N 0.49393(16) 1.0044(3) 0.63984(13) 0.0226(8) Uani 1 1 d . . . . . N4 N 0.47584(17) 1.1286(3) 0.62017(15) 0.0291(8) Uani 1 1 d . . . . . N5 N 0.67592(15) 0.8925(3) 0.61252(13) 0.0208(8) Uani 1 1 d . . . . . N6 N 0.63257(16) 1.1064(3) 0.63750(14) 0.0222(7) Uani 1 1 d . . . . . H6 H 0.6178 1.1723 0.6165 0.027 Uiso 1 1 calc R U . . . N7 N 0.59253(17) 0.3832(4) 0.35875(15) 0.0294(9) Uani 1 1 d . . . . . N8 N 0.55232(17) 0.3502(3) 0.40487(14) 0.0256(8) Uani 1 1 d . . . . . N9 N 0.42984(17) 0.3213(3) 0.42425(14) 0.0238(8) Uani 1 1 d . . . . . N10 N 0.39193(17) 0.3286(3) 0.47320(14) 0.0269(8) Uani 1 1 d . . . . . N11 N 0.52458(17) 0.6243(3) 0.38359(13) 0.0240(8) Uani 1 1 d . . . . . N12 N 0.40909(16) 0.5959(3) 0.42161(13) 0.0221(8) Uani 1 1 d . . . . . H12 H 0.3943 0.5908 0.4563 0.027 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0203(6) 0.0189(6) 0.0303(7) -0.0039(6) 0.0016(5) -0.0024(5) Al2 0.0227(6) 0.0355(8) 0.0236(6) 0.0017(6) 0.0016(6) -0.0027(6) C1 0.0161(19) 0.020(2) 0.025(2) -0.0010(18) 0.0012(16) 0.0006(16) C2 0.022(2) 0.023(2) 0.017(2) 0.0011(18) 0.0021(16) -0.0012(16) C3 0.025(2) 0.034(3) 0.035(3) -0.012(2) 0.006(2) -0.014(2) C4 0.028(2) 0.049(3) 0.027(3) -0.010(2) 0.005(2) -0.019(2) C5 0.019(2) 0.053(3) 0.019(2) 0.001(2) 0.0002(18) -0.007(2) C6 0.050(3) 0.030(3) 0.071(4) -0.016(3) 0.006(3) -0.015(2) C7 0.026(2) 0.068(4) 0.028(3) 0.008(3) -0.008(2) -0.005(2) C8 0.023(2) 0.038(3) 0.020(2) 0.002(2) 0.0022(18) -0.0002(19) C9 0.020(2) 0.043(3) 0.036(3) 0.000(2) 0.006(2) 0.005(2) C10 0.022(2) 0.036(3) 0.039(3) -0.001(2) -0.002(2) 0.006(2) C11 0.029(2) 0.040(3) 0.034(3) 0.008(2) 0.003(2) 0.001(2) C12 0.032(2) 0.044(3) 0.055(3) 0.000(3) -0.005(2) 0.015(2) C13 0.027(2) 0.021(2) 0.028(2) -0.0036(18) 0.0010(19) 0.0013(18) C14 0.053(3) 0.049(3) 0.025(2) -0.004(2) 0.001(2) -0.013(3) C15 0.047(3) 0.029(3) 0.045(3) -0.007(2) -0.010(2) -0.003(2) C16 0.019(2) 0.022(2) 0.031(2) -0.0036(19) 0.0084(18) -0.0058(18) C17 0.032(2) 0.039(3) 0.038(3) -0.008(2) 0.014(2) -0.010(2) C18 0.0182(19) 0.030(2) 0.043(3) -0.006(2) 0.001(2) -0.0041(17) C19 0.038(3) 0.028(3) 0.040(3) 0.001(2) -0.007(2) -0.004(2) C20 0.029(2) 0.024(3) 0.056(3) -0.010(2) 0.009(2) -0.002(2) C21 0.019(2) 0.022(2) 0.026(2) -0.0017(18) 0.0035(17) 0.0001(17) C22 0.020(2) 0.028(2) 0.017(2) -0.0028(18) -0.0036(17) -0.0018(18) C23 0.034(3) 0.052(3) 0.029(3) -0.003(2) 0.003(2) 0.014(2) C24 0.037(3) 0.044(3) 0.035(3) 0.000(2) -0.001(2) 0.019(2) C25 0.038(2) 0.028(2) 0.025(2) -0.003(2) -0.004(2) 0.009(2) C26 0.037(3) 0.084(4) 0.041(3) 0.006(3) 0.011(2) 0.023(3) C27 0.055(3) 0.030(3) 0.031(3) 0.004(2) -0.002(2) 0.006(2) C28 0.041(3) 0.023(3) 0.028(3) -0.001(2) -0.004(2) 0.000(2) C29 0.044(3) 0.020(2) 0.042(3) 0.000(2) -0.007(2) -0.008(2) C30 0.035(2) 0.022(2) 0.036(3) 0.007(2) -0.002(2) -0.005(2) C31 0.055(3) 0.032(3) 0.031(3) -0.005(2) -0.002(2) -0.002(2) C32 0.044(3) 0.040(3) 0.047(3) 0.012(3) 0.009(2) -0.009(2) C33 0.026(2) 0.030(2) 0.021(2) 0.0046(19) -0.0046(18) -0.0018(19) C34 0.037(3) 0.042(3) 0.049(3) 0.003(3) -0.018(2) -0.007(2) C35 0.037(3) 0.037(3) 0.037(3) 0.002(2) -0.007(2) 0.010(2) C36 0.030(2) 0.025(2) 0.032(2) 0.001(2) -0.001(2) -0.0080(19) C37 0.058(3) 0.030(3) 0.048(3) 0.009(2) -0.010(3) -0.008(3) C38 0.032(3) 0.043(3) 0.041(3) -0.004(2) -0.004(2) -0.013(2) C39 0.035(3) 0.031(3) 0.033(3) 0.003(2) -0.004(2) -0.003(2) C40 0.032(3) 0.064(4) 0.039(3) 0.002(3) 0.004(2) -0.010(2) N1 0.0243(18) 0.024(2) 0.0252(19) -0.0034(16) 0.0029(15) -0.0031(15) N2 0.0177(16) 0.029(2) 0.0225(19) -0.0010(16) 0.0008(14) -0.0017(15) N3 0.0163(16) 0.0257(19) 0.0258(19) 0.0029(16) 0.0010(15) 0.0030(14) N4 0.0216(17) 0.030(2) 0.036(2) 0.0051(17) -0.0001(17) 0.0073(15) N5 0.0148(16) 0.0202(18) 0.0275(19) -0.0033(15) 0.0039(14) -0.0038(13) N6 0.0246(17) 0.0163(17) 0.0256(19) 0.0055(15) -0.0012(15) -0.0009(14) N7 0.0226(19) 0.041(2) 0.0243(19) 0.0005(17) 0.0034(16) 0.0039(17) N8 0.0257(18) 0.028(2) 0.0236(19) -0.0013(16) 0.0021(15) 0.0029(15) N9 0.0285(18) 0.0196(19) 0.0231(18) 0.0006(16) 0.0022(16) -0.0027(15) N10 0.0291(18) 0.024(2) 0.028(2) -0.0010(16) 0.0043(16) -0.0039(16) N11 0.0268(19) 0.0229(19) 0.0224(18) 0.0003(15) 0.0016(15) -0.0056(16) N12 0.0243(18) 0.0266(19) 0.0155(17) -0.0027(15) 0.0003(14) 0.0033(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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 N5 Al1 N1 95.65(14) . . ? N5 Al1 C19 114.00(18) . . ? N1 Al1 C19 109.29(18) . . ? N5 Al1 C20 115.24(18) . . ? N1 Al1 C20 105.86(18) . . ? C19 Al1 C20 114.5(2) . . ? N11 Al2 C39 111.26(18) . . ? N11 Al2 C40 116.8(2) . . ? C39 Al2 C40 114.9(2) . . ? N11 Al2 N7 94.36(16) . . ? C39 Al2 N7 109.81(19) . . ? C40 Al2 N7 107.6(2) . . ? C2 C1 N2 123.0(3) . . ? C2 C1 N3 122.7(4) . . ? N2 C1 N3 114.0(3) . . ? N5 C2 C1 122.3(4) . . ? N5 C2 N6 119.7(3) . . ? C1 C2 N6 118.0(3) . . ? N1 C3 C4 109.3(4) . . ? N1 C3 C6 121.9(4) . . ? C4 C3 C6 128.8(4) . . ? C5 C4 C3 107.4(4) . . ? C5 C4 H4 126.3 . . ? C3 C4 H4 126.3 . . ? N2 C5 C4 106.7(4) . . ? N2 C5 C7 122.3(4) . . ? C4 C5 C7 131.0(4) . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 105.9(4) . . ? N3 C8 C11 122.3(4) . . ? C9 C8 C11 131.8(4) . . ? C8 C9 C10 106.6(4) . . ? C8 C9 H9 126.7 . . ? C10 C9 H9 126.7 . . ? N4 C10 C9 111.2(4) . . ? N4 C10 C12 119.8(4) . . ? C9 C10 C12 129.0(4) . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 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 . . ? N6 C13 C15 108.9(3) . . ? N6 C13 C14 111.2(3) . . ? C15 C13 C14 112.3(4) . . ? N6 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 C18 110.3(3) . . ? N5 C16 C17 110.0(3) . . ? C18 C16 C17 111.6(4) . . ? N5 C16 H16 108.3 . . ? C18 C16 H16 108.3 . . ? C17 C16 H16 108.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N8 123.4(4) . . ? C22 C21 N9 122.4(3) . . ? N8 C21 N9 114.0(3) . . ? C21 C22 N11 121.9(4) . . ? C21 C22 N12 118.7(3) . . ? N11 C22 N12 119.4(4) . . ? N7 C23 C24 110.2(4) . . ? N7 C23 C26 121.1(4) . . ? C24 C23 C26 128.7(4) . . ? C23 C24 C25 107.1(4) . . ? C23 C24 H24 126.4 . . ? C25 C24 H24 126.4 . . ? N8 C25 C24 106.7(4) . . ? N8 C25 C27 123.6(4) . . ? C24 C25 C27 129.7(4) . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N9 C28 C29 106.0(4) . . ? N9 C28 C31 121.6(4) . . ? C29 C28 C31 132.4(4) . . ? C28 C29 C30 106.5(4) . . ? C28 C29 H29 126.7 . . ? C30 C29 H29 126.7 . . ? N10 C30 C29 111.0(4) . . ? N10 C30 C32 121.3(4) . . ? C29 C30 C32 127.7(4) . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 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 . . ? N12 C33 C35 110.7(3) . . ? N12 C33 C34 109.9(4) . . ? C35 C33 C34 112.0(4) . . ? N12 C33 H33 108.0 . . ? C35 C33 H33 108.0 . . ? C34 C33 H33 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N11 C36 C38 110.2(4) . . ? N11 C36 C37 111.7(4) . . ? C38 C36 C37 111.2(4) . . ? N11 C36 H36 107.9 . . ? C38 C36 H36 107.9 . . ? C37 C36 H36 107.9 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Al2 C39 H39A 109.5 . . ? Al2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Al2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Al2 C40 H40A 109.5 . . ? Al2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Al2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C3 N1 N2 107.0(3) . . ? C3 N1 Al1 130.8(3) . . ? N2 N1 Al1 118.4(2) . . ? C5 N2 N1 109.6(3) . . ? C5 N2 C1 128.7(4) . . ? N1 N2 C1 121.0(3) . . ? C8 N3 N4 112.2(3) . . ? C8 N3 C1 127.3(3) . . ? N4 N3 C1 120.4(3) . . ? C10 N4 N3 104.1(3) . . ? C2 N5 C16 118.6(3) . . ? C2 N5 Al1 119.6(2) . . ? C16 N5 Al1 121.5(2) . . ? C2 N6 C13 118.6(3) . . ? C2 N6 H6 120.7 . . ? C13 N6 H6 120.7 . . ? C23 N7 N8 105.6(4) . . ? C23 N7 Al2 135.3(3) . . ? N8 N7 Al2 117.2(3) . . ? C25 N8 N7 110.4(3) . . ? C25 N8 C21 129.6(4) . . ? N7 N8 C21 119.5(3) . . ? C28 N9 N10 111.7(3) . . ? C28 N9 C21 127.3(3) . . ? N10 N9 C21 121.0(3) . . ? C30 N10 N9 104.7(3) . . ? C22 N11 C36 117.8(3) . . ? C22 N11 Al2 114.1(3) . . ? C36 N11 Al2 127.9(3) . . ? C22 N12 C33 118.0(3) . . ? C22 N12 H12 121.0 . . ? C33 N12 H12 121.0 . . ? 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 N5 1.878(3) . ? Al1 N1 1.950(3) . ? Al1 C19 1.959(5) . ? Al1 C20 1.963(4) . ? Al2 N11 1.866(4) . ? Al2 C39 1.950(4) . ? Al2 C40 1.961(5) . ? Al2 N7 1.975(4) . ? C1 C2 1.367(5) . ? C1 N2 1.417(5) . ? C1 N3 1.418(5) . ? C2 N5 1.360(5) . ? C2 N6 1.402(5) . ? C3 N1 1.339(5) . ? C3 C4 1.381(7) . ? C3 C6 1.494(7) . ? C4 C5 1.376(7) . ? C4 H4 0.9500 . ? C5 N2 1.361(5) . ? C5 C7 1.481(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N3 1.358(5) . ? C8 C9 1.372(6) . ? C8 C11 1.482(6) . ? C9 C10 1.400(6) . ? C9 H9 0.9500 . ? C10 N4 1.336(5) . ? C10 C12 1.483(6) . ? 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 N6 1.475(5) . ? C13 C15 1.504(6) . ? C13 C14 1.515(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N5 1.478(5) . ? C16 C18 1.519(6) . ? C16 C17 1.530(6) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.359(6) . ? C21 N8 1.418(5) . ? C21 N9 1.418(5) . ? C22 N11 1.365(5) . ? C22 N12 1.394(5) . ? C23 N7 1.342(6) . ? C23 C24 1.376(7) . ? C23 C26 1.506(7) . ? C24 C25 1.377(6) . ? C24 H24 0.9500 . ? C25 N8 1.352(5) . ? C25 C27 1.485(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N9 1.358(5) . ? C28 C29 1.374(6) . ? C28 C31 1.485(6) . ? C29 C30 1.394(7) . ? C29 H29 0.9500 . ? C30 N10 1.331(5) . ? C30 C32 1.487(6) . ? 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 N12 1.485(5) . ? C33 C35 1.508(6) . ? C33 C34 1.519(6) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N11 1.479(5) . ? C36 C38 1.525(6) . ? C36 C37 1.532(6) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 N2 1.372(5) . ? N3 N4 1.384(5) . ? N6 H6 0.8800 . ? N7 N8 1.383(5) . ? N9 N10 1.378(5) . ? N12 H12 0.8800 . ? 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 _geom_hbond_site_symmetry_A C16 H16 N6 1.00 2.32 2.824(5) 110.1 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 N5 -10.5(6) . . . . ? N3 C1 C2 N5 162.0(4) . . . . ? N2 C1 C2 N6 169.7(4) . . . . ? N3 C1 C2 N6 -17.8(6) . . . . ? N1 C3 C4 C5 1.0(5) . . . . ? C6 C3 C4 C5 -179.2(5) . . . . ? C3 C4 C5 N2 -0.7(5) . . . . ? C3 C4 C5 C7 -180.0(4) . . . . ? N3 C8 C9 C10 -0.5(5) . . . . ? C11 C8 C9 C10 -179.4(5) . . . . ? C8 C9 C10 N4 1.5(5) . . . . ? C8 C9 C10 C12 -178.2(5) . . . . ? N8 C21 C22 N11 8.3(6) . . . . ? N9 C21 C22 N11 -166.0(4) . . . . ? N8 C21 C22 N12 -171.8(3) . . . . ? N9 C21 C22 N12 13.9(6) . . . . ? N7 C23 C24 C25 0.2(6) . . . . ? C26 C23 C24 C25 179.4(5) . . . . ? C23 C24 C25 N8 -0.6(5) . . . . ? C23 C24 C25 C27 178.3(5) . . . . ? N9 C28 C29 C30 1.0(5) . . . . ? C31 C28 C29 C30 -178.6(5) . . . . ? C28 C29 C30 N10 -1.5(5) . . . . ? C28 C29 C30 C32 179.4(4) . . . . ? C4 C3 N1 N2 -0.9(4) . . . . ? C6 C3 N1 N2 179.3(4) . . . . ? C4 C3 N1 Al1 -158.0(3) . . . . ? C6 C3 N1 Al1 22.2(6) . . . . ? C4 C5 N2 N1 0.1(4) . . . . ? C7 C5 N2 N1 179.5(4) . . . . ? C4 C5 N2 C1 -170.7(4) . . . . ? C7 C5 N2 C1 8.6(6) . . . . ? C3 N1 N2 C5 0.5(4) . . . . ? Al1 N1 N2 C5 160.9(3) . . . . ? C3 N1 N2 C1 172.2(4) . . . . ? Al1 N1 N2 C1 -27.4(4) . . . . ? C2 C1 N2 C5 -146.2(4) . . . . ? N3 C1 N2 C5 40.6(5) . . . . ? C2 C1 N2 N1 43.8(6) . . . . ? N3 C1 N2 N1 -129.3(3) . . . . ? C9 C8 N3 N4 -0.7(5) . . . . ? C11 C8 N3 N4 178.4(4) . . . . ? C9 C8 N3 C1 -178.1(4) . . . . ? C11 C8 N3 C1 1.0(6) . . . . ? C2 C1 N3 C8 -115.4(5) . . . . ? N2 C1 N3 C8 57.7(5) . . . . ? C2 C1 N3 N4 67.4(5) . . . . ? N2 C1 N3 N4 -119.5(4) . . . . ? C9 C10 N4 N3 -1.9(5) . . . . ? C12 C10 N4 N3 177.9(4) . . . . ? C8 N3 N4 C10 1.6(4) . . . . ? C1 N3 N4 C10 179.2(3) . . . . ? C1 C2 N5 C16 153.8(4) . . . . ? N6 C2 N5 C16 -26.5(5) . . . . ? C1 C2 N5 Al1 -32.0(5) . . . . ? N6 C2 N5 Al1 147.8(3) . . . . ? C18 C16 N5 C2 132.0(4) . . . . ? C17 C16 N5 C2 -104.4(4) . . . . ? C18 C16 N5 Al1 -42.1(4) . . . . ? C17 C16 N5 Al1 81.5(4) . . . . ? N1 Al1 N5 C2 36.3(3) . . . . ? C19 Al1 N5 C2 -77.8(3) . . . . ? C20 Al1 N5 C2 146.8(3) . . . . ? N1 Al1 N5 C16 -149.7(3) . . . . ? C19 Al1 N5 C16 96.3(3) . . . . ? C20 Al1 N5 C16 -39.2(4) . . . . ? N5 C2 N6 C13 -60.8(5) . . . . ? C1 C2 N6 C13 118.9(4) . . . . ? C15 C13 N6 C2 172.7(4) . . . . ? C14 C13 N6 C2 -63.0(5) . . . . ? C24 C23 N7 N8 0.2(5) . . . . ? C26 C23 N7 N8 -179.0(4) . . . . ? C24 C23 N7 Al2 162.9(4) . . . . ? C26 C23 N7 Al2 -16.4(8) . . . . ? C24 C25 N8 N7 0.8(5) . . . . ? C27 C25 N8 N7 -178.2(4) . . . . ? C24 C25 N8 C21 172.0(4) . . . . ? C27 C25 N8 C21 -6.9(7) . . . . ? C23 N7 N8 C25 -0.6(5) . . . . ? Al2 N7 N8 C25 -167.0(3) . . . . ? C23 N7 N8 C21 -172.9(4) . . . . ? Al2 N7 N8 C21 20.8(5) . . . . ? C22 C21 N8 C25 145.2(4) . . . . ? N9 C21 N8 C25 -40.1(6) . . . . ? C22 C21 N8 N7 -44.2(6) . . . . ? N9 C21 N8 N7 130.5(4) . . . . ? C29 C28 N9 N10 -0.2(5) . . . . ? C31 C28 N9 N10 179.5(4) . . . . ? C29 C28 N9 C21 179.7(4) . . . . ? C31 C28 N9 C21 -0.6(7) . . . . ? C22 C21 N9 C28 115.0(5) . . . . ? N8 C21 N9 C28 -59.8(5) . . . . ? C22 C21 N9 N10 -65.2(5) . . . . ? N8 C21 N9 N10 120.0(4) . . . . ? C29 C30 N10 N9 1.4(5) . . . . ? C32 C30 N10 N9 -179.5(4) . . . . ? C28 N9 N10 C30 -0.8(4) . . . . ? C21 N9 N10 C30 179.4(4) . . . . ? C21 C22 N11 C36 -142.1(4) . . . . ? N12 C22 N11 C36 38.0(5) . . . . ? C21 C22 N11 Al2 43.0(5) . . . . ? N12 C22 N11 Al2 -136.9(3) . . . . ? C38 C36 N11 C22 107.0(4) . . . . ? C37 C36 N11 C22 -128.9(4) . . . . ? C38 C36 N11 Al2 -78.9(4) . . . . ? C37 C36 N11 Al2 45.2(5) . . . . ? C39 Al2 N11 C22 63.5(3) . . . . ? C40 Al2 N11 C22 -162.0(3) . . . . ? N7 Al2 N11 C22 -49.8(3) . . . . ? C39 Al2 N11 C36 -110.8(4) . . . . ? C40 Al2 N11 C36 23.7(4) . . . . ? N7 Al2 N11 C36 135.9(3) . . . . ? C21 C22 N12 C33 -119.8(4) . . . . ? N11 C22 N12 C33 60.1(5) . . . . ? C35 C33 N12 C22 -139.6(4) . . . . ? C34 C33 N12 C22 96.2(4) . . . . ?