#------------------------------------------------------------------------------ #$Date: 2019-12-03 12:35:34 +0200 (Tue, 03 Dec 2019) $ #$Revision: 244885 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556418.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_1556418 loop_ _publ_author_name 'Weetman, C.' 'Ito, N.' 'Unno, M.' 'Hanusch, F.' 'Inoue, S.' _publ_section_title ; NHI- and NHC-Supported Al(III) Hydrides for Amine-Borane Dehydrocoupling Catalysis ; _journal_name_full Inorganics _journal_page_first 92 _journal_paper_doi 10.3390/inorganics7080092 _journal_volume 7 _journal_year 2019 _chemical_compound_source 'see text' _chemical_formula_moiety 'C31 H55 Al B2 N4' _chemical_formula_sum 'C31 H55 Al B2 N4' _chemical_formula_weight 532.39 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 104.73(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.135(9) _cell_length_b 18.687(14) _cell_length_c 19.155(15) _cell_measurement_reflns_used 8820 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.1718 _cell_measurement_theta_min 2.1678 _cell_volume 3509(5) _computing_cell_refinement 'SAINT (Bruker, 2017)' _computing_data_collection 'APEX III Control Software (Bruker, 2016)' _computing_data_reduction 'SAINT (Bruker, 2017)' _computing_molecular_graphics 'PLATON (Spek, 2011)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2014)' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector ' CMOS plate ' _diffrn_detector_area_resol_mean 16 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker Photon CMOS ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_radiation_monochromator 'Helios optic' _diffrn_radiation_probe x-ray _diffrn_radiation_source 'TXS rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1316 _diffrn_reflns_av_unetI/netI 0.0500 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 87849 _diffrn_reflns_reduction_process ; ; _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 25.62 _diffrn_reflns_theta_min 2.18 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 0.735 _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2016/2, Bruker, 2016' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.008 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description plate _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.313 _exptl_crystal_size_mid 0.252 _exptl_crystal_size_min 0.178 _refine_diff_density_max 0.265 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.049 _refine_ls_abs_structure_Flack . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 443 _refine_ls_number_reflns 6558 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0574 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'W=1/[\S^2^(FO^2^)+(0.0494P)^2^+1.8193P] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.1319 _reflns_number_gt 4722 _reflns_number_total 6558 _reflns_threshold_expression I>2\s(I) _cod_data_source_file Inorganics-2019-7-92.cif _cod_data_source_block itono1_fine _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1556418 _shelx_res_file ; TITL ItoNo1_0m_a.res in P2(1)/c ItoNo1_fine.res created by SHELXL-2016/6 at 18:14:00 on 25-Jun-2019 CELL 0.71073 10.1347 18.6867 19.1547 90.000 104.729 90.000 ZERR 4.00 0.0087 0.0140 0.0152 0.000 0.024 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N AL B UNIT 124 220 16 4 8 LIST 4 TEMP -173.000 ACTA L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF OMIT 0 0 2 ! affected by beamstop REM NHC WGHT 0.049400 1.819300 FVAR 0.43011 0.84052 0.85384 N1 3 0.582146 0.564175 0.296963 11.00000 0.02199 0.02491 = 0.02020 -0.00183 0.00895 -0.00493 N2 3 0.405589 0.631188 0.261883 11.00000 0.02679 0.02246 = 0.01661 -0.00149 0.00357 -0.00322 C1 1 0.449043 0.562721 0.259140 11.00000 0.02342 0.02409 = 0.01519 0.00215 0.00886 -0.00098 C2 1 0.620107 0.632228 0.321956 11.00000 0.02708 0.03162 = 0.02270 -0.00464 0.00658 -0.00861 AFIX 43 H2 2 0.707740 0.646661 0.349575 11.00000 -1.20000 AFIX 0 C3 1 0.510219 0.674150 0.299976 11.00000 0.03922 0.02274 = 0.02261 -0.00430 0.00780 -0.00937 AFIX 43 H3 2 0.505175 0.723959 0.308885 11.00000 -1.20000 AFIX 0 C4 1 0.677805 0.505129 0.306584 11.00000 0.01629 0.02982 = 0.02991 -0.00230 0.00915 -0.00388 C5 1 0.726098 0.483935 0.246939 11.00000 0.02088 0.03797 = 0.03288 -0.00765 0.01439 -0.00892 C6 1 0.817725 0.427615 0.258050 11.00000 0.03060 0.04285 = 0.04770 -0.00973 0.02355 -0.00430 AFIX 43 H6 2 0.849866 0.410419 0.218694 11.00000 -1.20000 AFIX 0 C7 1 0.863554 0.395825 0.324774 11.00000 0.03181 0.03852 = 0.06817 0.00154 0.02359 0.00764 AFIX 43 H7 2 0.927312 0.357615 0.330945 11.00000 -1.20000 AFIX 0 C8 1 0.817360 0.419186 0.382570 11.00000 0.03304 0.04475 = 0.04751 0.01120 0.01536 0.00695 AFIX 43 H8 2 0.850599 0.397227 0.428412 11.00000 -1.20000 AFIX 0 C9 1 0.722716 0.474484 0.374765 11.00000 0.02373 0.03638 = 0.03143 0.00284 0.00986 -0.00002 C10 1 0.684635 0.522460 0.175134 11.00000 0.02806 0.05068 = 0.02807 -0.00713 0.01557 -0.00832 AFIX 13 H10 2 0.588947 0.539718 0.168938 11.00000 -1.20000 AFIX 0 C11 1 0.685624 0.474971 0.110738 11.00000 0.05554 0.07127 = 0.03596 -0.01612 0.02324 -0.01488 AFIX 137 H11A 2 0.633346 0.431312 0.113080 11.00000 -1.50000 H11B 2 0.779888 0.462271 0.111697 11.00000 -1.50000 H11C 2 0.644275 0.500745 0.065962 11.00000 -1.50000 AFIX 0 C12 1 0.774074 0.588231 0.175361 11.00000 0.04656 0.05548 = 0.03610 0.00398 0.01665 -0.01247 AFIX 137 H12A 2 0.868749 0.573138 0.180763 11.00000 -1.50000 H12B 2 0.769131 0.619521 0.215677 11.00000 -1.50000 H12C 2 0.741763 0.614257 0.129789 11.00000 -1.50000 AFIX 0 C13 1 0.676338 0.500328 0.440165 11.00000 0.03474 0.04683 = 0.02590 0.00580 0.00984 0.00669 AFIX 13 H13 2 0.596674 0.532992 0.422498 11.00000 -1.20000 AFIX 0 C14 1 0.629719 0.438274 0.480526 11.00000 0.05013 0.05757 = 0.03453 0.01581 0.01866 0.01166 AFIX 137 H14A 2 0.597985 0.457156 0.521141 11.00000 -1.50000 H14B 2 0.706294 0.405527 0.498675 11.00000 -1.50000 H14C 2 0.555084 0.412479 0.447557 11.00000 -1.50000 AFIX 0 C15 1 0.789686 0.543228 0.490882 11.00000 0.05829 0.06939 = 0.03382 -0.00652 0.00690 -0.00060 AFIX 137 H15A 2 0.868405 0.512060 0.509865 11.00000 -1.50000 H15B 2 0.756336 0.562084 0.530982 11.00000 -1.50000 H15C 2 0.816954 0.583031 0.464301 11.00000 -1.50000 AFIX 0 C16 1 0.275449 0.659983 0.221719 11.00000 0.03461 0.01673 = 0.02226 -0.00155 -0.00075 -0.00098 C17 1 0.174869 0.675137 0.257775 11.00000 0.03476 0.02033 = 0.02663 -0.00495 0.00157 0.00271 C18 1 0.052517 0.702751 0.216795 11.00000 0.03567 0.02660 = 0.04298 -0.00382 0.00083 0.00375 AFIX 43 H18 2 -0.017638 0.714373 0.239644 11.00000 -1.20000 AFIX 0 C19 1 0.030757 0.713660 0.143504 11.00000 0.04304 0.02954 = 0.04110 0.00174 -0.01160 0.00349 AFIX 43 H19 2 -0.055332 0.730449 0.116083 11.00000 -1.20000 AFIX 0 C20 1 0.133594 0.700275 0.109867 11.00000 0.05669 0.02934 = 0.02504 0.00245 -0.00896 -0.00372 AFIX 43 H20 2 0.117882 0.708988 0.059557 11.00000 -1.20000 AFIX 0 C21 1 0.259262 0.674378 0.148102 11.00000 0.04573 0.02106 = 0.02223 -0.00154 0.00217 -0.00439 C22 1 0.197258 0.665120 0.338700 11.00000 0.03612 0.03652 = 0.02724 -0.00569 0.00663 0.01057 AFIX 13 H22 2 0.272804 0.629767 0.355314 11.00000 -1.20000 AFIX 0 C23 1 0.071030 0.636615 0.359779 11.00000 0.04537 0.05102 = 0.03607 -0.00376 0.01583 0.01133 AFIX 137 H23A 2 0.094127 0.626715 0.411719 11.00000 -1.50000 H23B 2 0.040059 0.592436 0.333056 11.00000 -1.50000 H23C 2 -0.001862 0.672457 0.348050 11.00000 -1.50000 AFIX 0 C24 1 0.242039 0.736347 0.377762 11.00000 0.05450 0.05165 = 0.04237 -0.02152 0.00731 0.00329 AFIX 137 H24A 2 0.263119 0.728790 0.430064 11.00000 -1.50000 H24B 2 0.168173 0.771415 0.363528 11.00000 -1.50000 H24C 2 0.323365 0.754228 0.364589 11.00000 -1.50000 AFIX 0 C25 1 0.376546 0.667512 0.112620 11.00000 0.05906 0.03356 = 0.02134 0.00530 0.00974 -0.00535 AFIX 13 H25 2 0.450071 0.638708 0.145322 11.00000 -1.20000 AFIX 0 C26 1 0.335812 0.629598 0.039540 11.00000 0.09271 0.04160 = 0.02836 -0.00331 0.02178 -0.01249 AFIX 137 H26A 2 0.299819 0.581977 0.045658 11.00000 -1.50000 H26B 2 0.415931 0.624872 0.020060 11.00000 -1.50000 H26C 2 0.265579 0.657644 0.006064 11.00000 -1.50000 AFIX 0 C27 1 0.434476 0.742087 0.104500 11.00000 0.07752 0.04749 = 0.03728 -0.00194 0.01572 -0.02218 AFIX 137 H27A 2 0.463691 0.764876 0.152017 11.00000 -1.50000 H27B 2 0.363932 0.771437 0.072769 11.00000 -1.50000 H27C 2 0.512780 0.737549 0.083531 11.00000 -1.50000 AFIX 0 REM BH2 Gruppe B1 5 0.372936 0.495740 0.211010 11.00000 0.02584 0.02431 = 0.02006 -0.00111 0.00823 -0.00202 HB11 2 0.452904 0.458365 0.206022 11.00000 0.02204 HB12 2 0.320541 0.516752 0.158412 11.00000 0.02891 REM NMe2 Gruppe Part 1 21.000 SIMU 0.05 N3 C28 C29 DELU 0.05 N3 C28 C29 N3 3 0.270933 0.453293 0.243689 21.00000 0.04116 0.01873 = 0.03717 -0.01506 0.02934 -0.01044 C28 1 0.147417 0.488289 0.244933 21.00000 0.04597 0.04358 = 0.12816 -0.03655 0.05741 -0.01435 AFIX 137 H28A 2 0.167904 0.532048 0.273866 21.00000 -1.50000 H28B 2 0.091488 0.456416 0.266249 21.00000 -1.50000 H28C 2 0.097488 0.500590 0.195546 21.00000 -1.50000 AFIX 0 C29 1 0.343229 0.429732 0.320608 21.00000 0.10047 0.04249 = 0.02234 -0.00821 0.02751 -0.03292 AFIX 137 H29A 2 0.286711 0.394497 0.337492 21.00000 -1.50000 H29B 2 0.357664 0.471408 0.352715 21.00000 -1.50000 H29C 2 0.431504 0.408236 0.320763 21.00000 -1.50000 AFIX 0 Part 2 -21.000 SIMU 0.001 N3B C28B C29B DELU 0.001 N3B C28B C29B N3B 3 0.274702 0.436567 0.238838 -21.00000 0.02627 0.03410 = 0.05706 -0.00777 0.02153 0.00201 C28B 1 0.120401 0.499944 0.207666 -21.00000 0.02528 0.03375 = 0.05667 -0.00837 0.02216 0.00172 AFIX 137 H28D 2 0.139014 0.545099 0.234384 -21.00000 -1.50000 H28E 2 0.039114 0.477487 0.216917 -21.00000 -1.50000 H28F 2 0.104776 0.509406 0.155881 -21.00000 -1.50000 AFIX 0 C29B 1 0.278351 0.448011 0.307391 -21.00000 0.02807 0.03472 = 0.05693 -0.00793 0.02081 0.00166 AFIX 137 H29D 2 0.250891 0.497435 0.313462 -21.00000 -1.50000 H29E 2 0.371256 0.440082 0.337142 -21.00000 -1.50000 H29F 2 0.215612 0.415003 0.322403 -21.00000 -1.50000 AFIX 0 Part 0 REM AlH2 Gruppe AL1 4 0.235562 0.357720 0.192462 11.00000 0.04200 0.02226 = 0.02825 0.00027 0.01203 -0.00523 HA1 2 0.366032 0.321539 0.219254 11.00000 0.04771 HA2 2 0.106172 0.334669 0.217290 11.00000 0.05820 REM NMe2-BH3 Gruppe Part 1 31.0000 N4 3 0.197792 0.366402 0.087916 31.00000 0.02881 0.02762 = 0.01638 0.00391 -0.00119 -0.00331 C30 1 0.097019 0.419823 0.051094 31.00000 0.05396 0.03395 = 0.04845 0.01747 -0.02030 -0.00638 AFIX 137 H30A 2 0.072425 0.410548 -0.000972 31.00000 -1.50000 H30B 2 0.136344 0.467865 0.060388 31.00000 -1.50000 H30C 2 0.015260 0.416589 0.069376 31.00000 -1.50000 AFIX 0 C31 1 0.324215 0.375245 0.063230 31.00000 0.05467 0.06165 = 0.02638 -0.01181 0.01879 -0.01764 AFIX 137 H31A 2 0.303313 0.368620 0.010806 31.00000 -1.50000 H31B 2 0.391668 0.339578 0.086983 31.00000 -1.50000 H31C 2 0.361183 0.423380 0.075595 31.00000 -1.50000 AFIX 0 Part 2 -31.0000 SAME N4 C30 C31 SIMU 0.005 N4B C30B C31B DELU 0.005 N4B C30B C31B N4B 3 0.189446 0.369514 0.104476 -31.00000 0.06421 0.03458 = 0.04481 -0.00438 0.02251 -0.00002 C30B 1 0.060828 0.410371 0.074653 -31.00000 0.07131 0.04511 = 0.05137 0.00913 0.01794 0.00561 AFIX 137 H30D 2 0.074868 0.460715 0.088945 -31.00000 -1.50000 H30E 2 -0.012481 0.390336 0.093572 -31.00000 -1.50000 H30F 2 0.035685 0.406878 0.021870 -31.00000 -1.50000 AFIX 0 C31B 1 0.280060 0.392870 0.059034 -31.00000 0.07109 0.02967 = 0.03788 -0.01165 0.01995 -0.00794 AFIX 137 H31D 2 0.236680 0.382157 0.008303 -31.00000 -1.50000 H31E 2 0.367238 0.367398 0.073925 -31.00000 -1.50000 H31F 2 0.296158 0.444495 0.064837 -31.00000 -1.50000 AFIX 0 Part 0 B2 5 0.141247 0.286730 0.070770 11.00000 0.05880 0.03185 = 0.03773 0.00068 -0.00180 -0.00829 HB21 2 0.198021 0.253251 0.114923 11.00000 0.04507 HB22 2 0.032633 0.286976 0.070261 11.00000 0.05903 HB23 2 0.163056 0.267765 0.019497 11.00000 0.06582 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM ItoNo1_0m_a.res in P2(1)/c REM R1 = 0.0574 for 4722 Fo > 4sig(Fo) and 0.0877 for all 6558 data REM 443 parameters refined using 48 restraints END WGHT 0.0490 1.8405 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.265, deepest hole -0.321, 1-sigma level 0.049 Q1 1 0.3358 0.3566 0.2024 11.00000 0.05 0.26 Q2 1 0.4235 0.3218 0.2063 11.00000 0.05 0.21 Q3 1 0.7286 0.6269 0.3383 11.00000 0.05 0.20 Q4 1 0.5060 0.5567 0.2914 11.00000 0.05 0.18 Q5 1 0.4599 0.8606 0.2212 11.00000 0.05 0.18 ; _shelx_res_checksum 80711 _shelx_hkl_file ; -2 0 0 9539.83 572.892 2 -2 0 0 9999.99 572.190 4 -2 0 0 9353.39 570.987 6 2 0 0 9765.90 571.871 4 2 0 0 9827.97 571.043 6 -3 0 0 87.8268 11.3815 2 -3 0 0 117.894 7.35201 6 -3 0 0 95.5827 7.19824 6 -3 0 0 86.3944 9.07948 4 3 0 0 104.403 7.07176 6 3 0 0 81.2397 9.50749 4 3 0 0 110.909 7.42449 6 -4 0 0 1.48983 4.84755 2 -4 0 0 1.43809 6.07985 4 -4 0 0 6.37811 3.29502 6 -4 0 0 4.83329 3.16700 6 4 0 0 -0.1362 7.11571 4 4 0 0 4.56951 3.34191 6 4 0 0 0.33898 2.91649 6 -5 0 0 48.5180 7.49220 6 -5 0 0 71.4028 7.78589 6 -5 0 0 64.7242 9.66498 4 5 0 0 58.1755 6.79974 6 5 0 0 53.9285 10.7166 4 5 0 0 68.8346 8.17212 6 -6 0 0 56.9151 6.64230 6 -6 0 0 45.5060 8.85647 4 -6 0 0 28.7973 7.07736 2 6 0 0 40.7236 9.79358 4 6 0 0 43.2750 5.94703 6 -7 0 0 26.0541 4.64517 6 -7 0 0 37.7933 9.35442 4 -7 0 0 25.0412 6.95813 2 7 0 0 27.0997 4.28060 6 7 0 0 14.2824 10.5534 4 -8 0 0 7.88001 7.89114 2 -8 0 0 4.59288 4.45995 6 -8 0 0 -1.3115 10.2325 4 -8 0 0 6.93395 5.45474 6 8 0 0 7.59732 12.8187 4 8 0 0 7.11789 5.77011 6 8 0 0 7.15669 4.43635 6 -9 0 0 16.5406 4.91681 6 -9 0 0 15.8535 9.79338 2 -9 0 0 15.8401 13.7915 4 -9 0 0 17.7472 6.29367 6 9 0 0 11.2642 15.2235 4 9 0 0 15.9536 6.49302 6 9 0 0 21.5938 4.86980 6 -10 0 0 6.59695 12.9231 4 -10 0 0 -8.0816 9.51930 2 -10 0 0 4.62040 4.65238 6 10 0 0 -3.0367 17.4977 4 10 0 0 -0.0316 6.52359 6 10 0 0 5.10250 4.38113 6 -11 0 0 24.1906 5.30536 6 -11 0 0 17.6196 14.1928 4 -11 0 0 -3.9603 11.2375 2 -11 0 0 16.5938 7.16664 6 11 0 0 12.4381 19.7852 4 11 -1 0 13.1934 20.4203 4 11 -1 0 19.7694 4.87889 6 11 -1 0 -1.7324 7.47174 6 -11 1 0 18.3359 5.17911 6 -11 1 0 14.6228 14.0159 4 10 -1 0 25.9292 7.70051 6 10 -1 0 59.7620 7.91824 6 10 -1 0 39.0109 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10.1033 6 3 -5 -22 9.29025 11.6350 4 3 -5 -22 14.6544 16.8036 3 -3 5 22 -6.0514 10.6876 6 -3 5 22 19.7445 16.8160 5 -3 5 22 3.45870 14.5426 3 -3 5 22 28.7744 9.59291 6 2 -5 -22 15.8402 8.97167 6 2 -5 -22 -5.5101 15.9896 3 2 -5 -22 8.98850 11.2109 4 2 -5 -22 -0.1675 12.2247 6 -2 5 22 -5.5277 14.4525 3 -2 5 22 35.9207 9.31970 6 -2 5 22 -1.4810 9.80366 6 -2 5 22 9.36882 16.6701 5 1 -5 -22 5.38532 15.7086 3 1 -5 -22 18.0425 9.37459 6 1 -5 -22 -19.458 9.77444 4 -1 5 22 -4.6381 16.0744 3 -1 5 22 -17.545 8.21726 6 -1 5 22 53.0137 18.1654 5 5 -6 -22 15.7115 13.3652 4 4 -6 -22 31.2516 10.5152 6 4 -6 -22 -17.970 17.1132 3 4 -6 -22 -0.9268 13.3060 6 4 -6 -22 6.63010 12.5375 4 -4 6 22 -15.063 10.7191 6 -4 6 22 21.0956 10.1589 6 -4 6 22 -3.7607 15.5967 3 -4 6 22 29.4157 17.1800 5 3 -6 -22 -3.8837 11.1429 4 3 -6 -22 20.0619 13.2416 6 3 -6 -22 33.8850 10.2111 6 3 -6 -22 24.9116 17.2460 3 -3 6 22 15.7350 11.8438 6 -3 6 22 20.5696 9.43426 6 -3 6 22 1.28502 14.9944 3 -3 6 22 23.5989 18.2615 5 2 -6 -22 -10.177 10.5465 4 2 -6 -22 20.4971 8.77337 6 2 -6 -22 0.51512 16.8354 3 2 -6 -22 6.81675 12.9033 6 -2 6 22 38.8314 16.8924 5 -2 6 22 20.8542 9.65133 6 -2 6 22 -5.3197 9.85965 6 -2 6 22 2.83213 14.8340 3 1 -6 -22 -15.547 10.1053 4 3 -7 -22 1.87253 11.7631 4 4 2 -23 5.85024 12.5115 4 3 2 -23 10.6266 15.8337 5 3 2 -23 17.2219 12.1332 4 -3 -2 23 25.2634 20.6586 5 -4 -1 23 56.6847 20.6429 5 3 1 -23 26.6195 15.5473 5 3 1 -23 -18.195 12.3993 6 3 1 -23 11.4745 12.2153 4 3 1 -23 17.6140 11.1059 6 3 1 -23 3.19069 14.4097 3 -3 -1 23 14.7211 10.9463 6 -3 -1 23 44.3851 19.8547 5 -3 -1 23 10.8570 10.6175 6 2 1 -23 12.3157 12.9842 4 -2 -1 23 51.4950 22.0999 5 4 0 -23 -11.773 13.9858 3 4 0 -23 -21.784 12.1278 6 4 0 -23 8.68328 12.3952 4 -4 0 23 21.3039 19.3558 5 -4 0 23 11.6713 10.8104 6 3 0 -23 10.6443 10.6945 6 3 0 -23 -8.8982 14.5351 3 3 0 -23 19.5538 12.1492 4 3 0 -23 1.86159 14.5088 5 -3 0 23 14.6143 10.8314 6 -3 0 23 2.59752 18.6479 5 -3 0 23 -3.9563 10.0223 6 2 0 -23 21.3783 11.8346 4 2 0 -23 17.0870 15.8528 5 -2 0 23 28.0210 20.9360 5 4 -1 -23 9.71425 12.4855 4 -4 1 23 48.5887 20.5702 5 3 -1 -23 27.2724 11.2564 6 3 -1 -23 8.11088 12.2102 4 3 -1 -23 -2.8000 14.5631 3 -3 1 23 33.9949 10.6839 6 -3 1 23 21.5917 10.6116 6 -3 1 23 33.3615 19.7920 5 2 -1 -23 24.8543 12.7520 4 -2 1 23 47.7478 20.6171 5 4 -2 -23 24.9976 13.3827 4 3 -2 -23 10.4568 12.8148 4 -3 2 23 47.4773 19.6883 5 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7355 _exptl_absorpt_correction_T_min 0.6619 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71108 10.161 18.703 19.170 90.073 104.717 89.979 ) ; _shelx_hkl_checksum 9880 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z 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 0.0420(4) 0.0223(3) 0.0282(3) 0.0003(3) 0.0120(3) -0.0052(3) N1 0.0220(9) 0.0249(9) 0.0202(8) -0.0018(7) 0.0089(7) -0.0049(7) N2 0.0268(9) 0.0225(9) 0.0166(8) -0.0015(6) 0.0036(7) -0.0032(7) N3 0.0412(17) 0.019(2) 0.0372(17) -0.0151(15) 0.0293(12) -0.0104(16) N3B 0.026(6) 0.034(7) 0.057(8) -0.008(6) 0.022(6) 0.002(5) N4 0.0288(16) 0.0276(16) 0.0164(18) 0.0039(14) -0.0012(13) -0.0033(12) N4B 0.064(11) 0.035(9) 0.045(11) -0.004(8) 0.023(9) 0.000(7) C1 0.0234(10) 0.0241(10) 0.0152(9) 0.0021(8) 0.0089(8) -0.0010(8) C2 0.0271(11) 0.0316(12) 0.0227(10) -0.0046(9) 0.0066(9) -0.0086(9) C3 0.0392(13) 0.0227(11) 0.0226(10) -0.0043(8) 0.0078(9) -0.0094(9) C4 0.0163(10) 0.0298(11) 0.0299(11) -0.0023(9) 0.0091(8) -0.0039(8) C5 0.0209(10) 0.0380(12) 0.0329(11) -0.0077(9) 0.0144(9) -0.0089(9) C6 0.0306(12) 0.0428(14) 0.0477(14) -0.0097(11) 0.0236(11) -0.0043(10) C7 0.0318(13) 0.0385(14) 0.0682(18) 0.0015(12) 0.0236(13) 0.0076(11) C8 0.0330(13) 0.0448(14) 0.0475(14) 0.0112(11) 0.0154(11) 0.0070(11) C9 0.0237(11) 0.0364(12) 0.0314(11) 0.0028(9) 0.0099(9) 0.0000(9) C10 0.0281(12) 0.0507(14) 0.0281(11) -0.0071(10) 0.0156(9) -0.0083(10) C11 0.0555(17) 0.0713(19) 0.0360(13) -0.0161(13) 0.0232(12) -0.0149(14) C12 0.0466(15) 0.0555(16) 0.0361(13) 0.0040(11) 0.0167(12) -0.0125(12) C13 0.0347(13) 0.0468(14) 0.0259(11) 0.0058(10) 0.0098(10) 0.0067(10) C14 0.0501(15) 0.0576(16) 0.0345(13) 0.0158(12) 0.0187(11) 0.0117(13) C15 0.0583(17) 0.0694(19) 0.0338(13) -0.0065(13) 0.0069(12) -0.0006(14) C16 0.0346(12) 0.0167(10) 0.0223(10) -0.0016(8) -0.0007(9) -0.0010(8) C17 0.0348(12) 0.0203(10) 0.0266(11) -0.0050(8) 0.0016(9) 0.0027(9) C18 0.0357(13) 0.0266(12) 0.0430(14) -0.0038(10) 0.0008(11) 0.0037(10) C19 0.0430(15) 0.0295(12) 0.0411(14) 0.0017(10) -0.0116(12) 0.0035(10) C20 0.0567(16) 0.0293(12) 0.0250(11) 0.0024(9) -0.0090(11) -0.0037(11) C21 0.0457(14) 0.0211(11) 0.0222(10) -0.0015(8) 0.0022(10) -0.0044(9) C22 0.0361(13) 0.0365(13) 0.0272(11) -0.0057(9) 0.0066(10) 0.0106(10) C23 0.0454(15) 0.0510(15) 0.0361(13) -0.0038(11) 0.0158(11) 0.0113(12) C24 0.0545(17) 0.0516(16) 0.0424(14) -0.0215(12) 0.0073(13) 0.0033(13) C25 0.0591(16) 0.0336(13) 0.0213(11) 0.0053(9) 0.0097(10) -0.0054(11) C26 0.093(2) 0.0416(15) 0.0284(13) -0.0033(11) 0.0218(13) -0.0125(14) C27 0.078(2) 0.0475(16) 0.0373(14) -0.0019(12) 0.0157(14) -0.0222(14) C28 0.046(3) 0.044(2) 0.128(6) -0.037(3) 0.057(3) -0.014(2) C29 0.100(5) 0.042(2) 0.0223(17) -0.0082(15) 0.028(2) -0.033(3) C29B 0.028(6) 0.035(7) 0.057(8) -0.008(6) 0.021(6) 0.002(5) C30 0.054(3) 0.0339(18) 0.048(3) 0.0175(17) -0.020(2) -0.0064(17) C30B 0.071(12) 0.045(11) 0.051(12) 0.009(9) 0.018(10) 0.006(8) C31 0.055(3) 0.062(4) 0.0264(19) -0.012(2) 0.019(2) -0.018(2) C31B 0.071(12) 0.030(10) 0.038(10) -0.012(8) 0.020(10) -0.008(9) B1 0.0258(12) 0.0243(12) 0.0201(11) -0.0011(9) 0.0082(10) -0.0020(10) B2 0.059(2) 0.0318(15) 0.0377(16) 0.0007(12) -0.0018(15) -0.0083(14) C28B 0.025(6) 0.034(7) 0.057(8) -0.008(6) 0.022(6) 0.002(5) loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al Uani 0.23556(7) 0.35772(3) 0.19246(3) 1.000 0.0303(2) d . . . N1 N Uani 0.58215(16) 0.56418(8) 0.29696(8) 1.000 0.0217(5) d . . . N2 N Uani 0.40559(16) 0.63119(8) 0.26188(8) 1.000 0.0223(5) d . . . N3 N Uani 0.2709(6) 0.4533(2) 0.2437(3) 0.841(15) 0.0290(10) d UP A 1 N3B N Uani 0.275(3) 0.4366(16) 0.239(2) 0.159(15) 0.037(4) d UP A 2 N4 N Uani 0.1978(5) 0.3664(3) 0.0879(3) 0.85(2) 0.0255(10) d DP A 1 N4B N Uani 0.189(3) 0.370(2) 0.104(2) 0.15(2) 0.046(6) d DUP A 2 C1 C Uani 0.44904(19) 0.56272(10) 0.25914(9) 1.000 0.0202(6) d . . . C2 C Uani 0.6201(2) 0.63223(11) 0.32196(10) 1.000 0.0271(6) d . . . C3 C Uani 0.5102(2) 0.67415(11) 0.29998(10) 1.000 0.0282(7) d . . . C4 C Uani 0.67780(19) 0.50513(11) 0.30658(11) 1.000 0.0248(6) d . . . C5 C Uani 0.7261(2) 0.48393(11) 0.24694(11) 1.000 0.0292(6) d . . . C6 C Uani 0.8177(2) 0.42761(13) 0.25805(13) 1.000 0.0379(8) d . . . C7 C Uani 0.8636(2) 0.39582(13) 0.32477(14) 1.000 0.0442(9) d . . . C8 C Uani 0.8174(2) 0.41919(13) 0.38257(14) 1.000 0.0408(8) d . . . C9 C Uani 0.7227(2) 0.47448(12) 0.37477(11) 1.000 0.0300(7) d . . . C10 C Uani 0.6846(2) 0.52246(13) 0.17513(11) 1.000 0.0341(7) d . . . C11 C Uani 0.6856(3) 0.47497(15) 0.11074(13) 1.000 0.0522(10) d . . . C12 C Uani 0.7741(3) 0.58823(14) 0.17536(13) 1.000 0.0450(8) d . . . C13 C Uani 0.6763(2) 0.50033(13) 0.44016(11) 1.000 0.0354(7) d . . . C14 C Uani 0.6297(3) 0.43827(14) 0.48053(13) 1.000 0.0460(8) d . . . C15 C Uani 0.7897(3) 0.54323(16) 0.49088(14) 1.000 0.0547(10) d . . . C16 C Uani 0.2754(2) 0.65998(10) 0.22172(10) 1.000 0.0260(6) d . . . C17 C Uani 0.1749(2) 0.67514(10) 0.25778(11) 1.000 0.0284(6) d . . . C18 C Uani 0.0525(2) 0.70275(11) 0.21679(12) 1.000 0.0368(8) d . . . C19 C Uani 0.0308(3) 0.71366(12) 0.14350(13) 1.000 0.0419(8) d . . . C20 C Uani 0.1336(3) 0.70028(12) 0.10987(12) 1.000 0.0405(8) d . . . C21 C Uani 0.2593(2) 0.67438(11) 0.14810(11) 1.000 0.0308(7) d . . . C22 C Uani 0.1973(2) 0.66512(12) 0.33870(11) 1.000 0.0335(7) d . . . C23 C Uani 0.0710(2) 0.63662(14) 0.35978(13) 1.000 0.0432(8) d . . . C24 C Uani 0.2420(3) 0.73635(14) 0.37776(14) 1.000 0.0504(9) d . . . C25 C Uani 0.3765(3) 0.66751(12) 0.11262(11) 1.000 0.0381(8) d . . . C26 C Uani 0.3358(3) 0.62960(14) 0.03954(12) 1.000 0.0532(9) d . . . C27 C Uani 0.4345(3) 0.74209(14) 0.10450(14) 1.000 0.0541(10) d . . . C28 C Uani 0.1474(5) 0.4883(3) 0.2449(5) 0.841(15) 0.066(2) d UP A 1 C29 C Uani 0.3432(9) 0.4297(3) 0.32061(18) 0.841(15) 0.0525(19) d UP A 1 C29B C Uani 0.278(2) 0.4480(13) 0.3074(14) 0.159(15) 0.038(4) d UP A 2 C30 C Uani 0.0970(7) 0.4198(2) 0.0511(4) 0.85(2) 0.0513(15) d DP A 1 C30B C Uani 0.061(3) 0.410(2) 0.075(2) 0.15(2) 0.055(7) d DUP A 2 C31 C Uani 0.3242(7) 0.3752(4) 0.0632(3) 0.85(2) 0.0462(18) d DP A 1 C31B C Uani 0.280(4) 0.3929(18) 0.059(2) 0.15(2) 0.045(6) d DUP A 2 B1 B Uani 0.3729(2) 0.49574(12) 0.21101(12) 1.000 0.0230(7) d . . . B2 B Uani 0.1412(4) 0.28673(15) 0.07077(16) 1.000 0.0454(10) d . . . C28B C Uani 0.120(2) 0.4999(13) 0.2077(13) 0.159(15) 0.037(4) d UP A 2 Hb11 H Uiso 0.453(2) 0.4584(10) 0.2060(10) 1.000 0.022(5) d . . . H2 H Uiso 0.70774 0.64666 0.34958 1.000 0.0330 c RU . . Hb12 H Uiso 0.321(2) 0.5168(11) 0.1584(11) 1.000 0.029(5) d . . . H3 H Uiso 0.50517 0.72396 0.30889 1.000 0.0340 c RU . . Ha1 H Uiso 0.366(2) 0.3215(12) 0.2193(12) 1.000 0.048(7) d . . . Ha2 H Uiso 0.106(3) 0.3347(14) 0.2173(13) 1.000 0.058(8) d . . . Hb21 H Uiso 0.198(2) 0.2533(13) 0.1149(13) 1.000 0.045(7) d . . . H6 H Uiso 0.84987 0.41042 0.21869 1.000 0.0460 c RU . . Hb22 H Uiso 0.033(3) 0.2870(14) 0.0703(14) 1.000 0.059(8) d . . . H7 H Uiso 0.92731 0.35761 0.33094 1.000 0.0530 c RU . . Hb23 H Uiso 0.163(3) 0.2678(15) 0.0195(15) 1.000 0.066(8) d . . . H8 H Uiso 0.85060 0.39723 0.42841 1.000 0.0490 c RU . . H10 H Uiso 0.58895 0.53972 0.16894 1.000 0.0410 c RU . . H11A H Uiso 0.63335 0.43131 0.11308 1.000 0.0780 c RU . . H11B H Uiso 0.77989 0.46227 0.11170 1.000 0.0780 c RU . . H11C H Uiso 0.64428 0.50074 0.06596 1.000 0.0780 c RU . . H12A H Uiso 0.86875 0.57314 0.18076 1.000 0.0670 c RU . . H12B H Uiso 0.76913 0.61952 0.21568 1.000 0.0670 c RU . . H12C H Uiso 0.74176 0.61426 0.12979 1.000 0.0670 c RU . . H13 H Uiso 0.59667 0.53299 0.42250 1.000 0.0430 c RU . . H14A H Uiso 0.59799 0.45716 0.52114 1.000 0.0690 c RU . . H14B H Uiso 0.70629 0.40553 0.49867 1.000 0.0690 c RU . . H14C H Uiso 0.55508 0.41248 0.44756 1.000 0.0690 c RU . . H15A H Uiso 0.86840 0.51206 0.50986 1.000 0.0820 c RU . . H15B H Uiso 0.75634 0.56208 0.53098 1.000 0.0820 c RU . . H15C H Uiso 0.81695 0.58303 0.46430 1.000 0.0820 c RU . . H18 H Uiso -0.01764 0.71437 0.23964 1.000 0.0440 c RU . . H19 H Uiso -0.05533 0.73045 0.11608 1.000 0.0500 c RU . . H20 H Uiso 0.11788 0.70899 0.05956 1.000 0.0490 c RU . . H22 H Uiso 0.27280 0.62977 0.35531 1.000 0.0400 c RU . . H23A H Uiso 0.09413 0.62672 0.41172 1.000 0.0650 c RU . . H23B H Uiso 0.04006 0.59244 0.33306 1.000 0.0650 c RU . . H23C H Uiso -0.00186 0.67246 0.34805 1.000 0.0650 c RU . . H24A H Uiso 0.26312 0.72879 0.43006 1.000 0.0760 c RU . . H24B H Uiso 0.16817 0.77141 0.36353 1.000 0.0760 c RU . . H24C H Uiso 0.32337 0.75423 0.36459 1.000 0.0760 c RU . . H25 H Uiso 0.45007 0.63871 0.14532 1.000 0.0460 c RU . . H26A H Uiso 0.29982 0.58198 0.04566 1.000 0.0800 c RU . . H26B H Uiso 0.41593 0.62487 0.02006 1.000 0.0800 c RU . . H26C H Uiso 0.26558 0.65764 0.00606 1.000 0.0800 c RU . . H27A H Uiso 0.46369 0.76488 0.15202 1.000 0.0810 c RU . . H27B H Uiso 0.36393 0.77144 0.07277 1.000 0.0810 c RU . . H27C H Uiso 0.51278 0.73755 0.08353 1.000 0.0810 c RU . . H28A H Uiso 0.16790 0.53205 0.27387 0.841(15) 0.0990 c RUP A 1 H28B H Uiso 0.09149 0.45642 0.26625 0.841(15) 0.0990 c RUP A 1 H28C H Uiso 0.09749 0.50059 0.19555 0.841(15) 0.0990 c RUP A 1 H29A H Uiso 0.28671 0.39450 0.33749 0.841(15) 0.0790 c RUP A 1 H29B H Uiso 0.35766 0.47141 0.35271 0.841(15) 0.0790 c RUP A 1 H29C H Uiso 0.43150 0.40824 0.32076 0.841(15) 0.0790 c RUP A 1 H29D H Uiso 0.25089 0.49744 0.31346 0.159(15) 0.0570 c RUP A 2 H29E H Uiso 0.37126 0.44008 0.33714 0.159(15) 0.0570 c RUP A 2 H29F H Uiso 0.21561 0.41500 0.32240 0.159(15) 0.0570 c RUP A 2 H30A H Uiso 0.07243 0.41055 -0.00097 0.85(2) 0.0770 c RUP A 1 H30B H Uiso 0.13634 0.46786 0.06039 0.85(2) 0.0770 c RUP A 1 H30C H Uiso 0.01526 0.41659 0.06938 0.85(2) 0.0770 c RUP A 1 H30D H Uiso 0.07487 0.46071 0.08895 0.15(2) 0.0830 c RUP A 2 H30E H Uiso -0.01248 0.39034 0.09357 0.15(2) 0.0830 c RUP A 2 H30F H Uiso 0.03568 0.40688 0.02187 0.15(2) 0.0830 c RUP A 2 H31A H Uiso 0.30331 0.36862 0.01081 0.85(2) 0.0690 c RUP A 1 H31B H Uiso 0.39167 0.33958 0.08698 0.85(2) 0.0690 c RUP A 1 H31C H Uiso 0.36118 0.42338 0.07559 0.85(2) 0.0690 c RUP A 1 H31D H Uiso 0.23668 0.38216 0.00830 0.15(2) 0.0680 c RUP A 2 H31E H Uiso 0.36724 0.36740 0.07393 0.15(2) 0.0680 c RUP A 2 H31F H Uiso 0.29616 0.44449 0.06484 0.15(2) 0.0680 c RUP A 2 H28D H Uiso 0.13901 0.54510 0.23438 0.159(15) 0.0550 c RUP A 2 H28E H Uiso 0.03911 0.47749 0.21692 0.159(15) 0.0550 c RUP A 2 H28F H Uiso 0.10478 0.50941 0.15588 0.159(15) 0.0550 c RUP A 2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ha1 Al1 Ha2 121.4(13) . . . no N3 Al1 Ha2 98.8(10) . . . no N4 Al1 Ha1 109.0(9) . . . no N4 Al1 Ha2 112.0(9) . . . no N3B Al1 Ha1 98.3(14) . . . no N3B Al1 Ha2 100.4(14) . . . no N4B Al1 Ha1 115.0(14) . . . no N3 Al1 Ha1 101.9(9) . . . no N4B Al1 Ha2 107.8(14) . . . no C2 N1 C4 122.66(17) . . . yes C1 N1 C4 126.40(16) . . . yes C1 N1 C2 110.79(16) . . . yes C1 N2 C3 110.80(16) . . . yes C1 N2 C16 126.06(16) . . . yes C3 N2 C16 122.48(16) . . . yes Al1 N3 C28 111.5(4) . . . yes C28 N3 C29 109.0(6) . . . yes Al1 N3 C29 101.2(3) . . . yes Al1 N3 B1 108.0(3) . . . yes C28 N3 B1 116.8(4) . . . yes C29 N3 B1 109.2(5) . . . yes C29B N3B B1 110(2) . . . yes Al1 N3B C29B 127(2) . . . yes Al1 N3B B1 119(2) . . . yes C31 N4 B2 109.4(5) . . . yes C30 N4 C31 108.8(5) . . . yes C30 N4 B2 111.3(4) . . . yes Al1 N4 C30 118.7(4) . . . yes Al1 N4 B2 95.7(3) . . . yes Al1 N4 C31 112.2(4) . . . yes C31B N4B B2 102(2) . . . yes C30B N4B C31B 105(3) . . . yes C30B N4B B2 101(2) . . . yes Al1 N4B C30B 117(3) . . . yes Al1 N4B C31B 125(3) . . . yes Al1 N4B B2 104(2) . . . yes N1 C1 B1 125.48(17) . . . yes N1 C1 N2 104.36(16) . . . yes N2 C1 B1 129.37(17) . . . yes N1 C2 C3 107.10(18) . . . yes N2 C3 C2 106.95(18) . . . yes C5 C4 C9 123.14(19) . . . no N1 C4 C5 118.03(17) . . . yes N1 C4 C9 118.75(18) . . . yes C4 C5 C10 121.95(19) . . . no C4 C5 C6 116.55(19) . . . no C6 C5 C10 121.46(19) . . . no C5 C6 C7 121.7(2) . . . no C6 C7 C8 120.3(2) . . . no C7 C8 C9 121.0(2) . . . no C4 C9 C13 123.02(19) . . . no C8 C9 C13 119.7(2) . . . no C4 C9 C8 117.3(2) . . . no C11 C10 C12 110.2(2) . . . no C5 C10 C11 113.7(2) . . . no C5 C10 C12 110.64(18) . . . no C14 C13 C15 110.74(19) . . . no C9 C13 C14 111.9(2) . . . no C9 C13 C15 110.43(19) . . . no N2 C16 C17 119.47(17) . . . yes N2 C16 C21 117.47(18) . . . yes C17 C16 C21 122.99(19) . . . no C16 C17 C18 117.05(19) . . . no C18 C17 C22 120.20(19) . . . no C16 C17 C22 122.72(18) . . . no C17 C18 C19 121.3(2) . . . no C18 C19 C20 120.3(2) . . . no C19 C20 C21 121.2(2) . . . no C16 C21 C20 117.0(2) . . . no C16 C21 C25 121.99(19) . . . no C20 C21 C25 120.8(2) . . . no C17 C22 C24 109.80(18) . . . no C17 C22 C23 113.16(18) . . . no C23 C22 C24 109.6(2) . . . no C21 C25 C27 109.4(2) . . . no C26 C25 C27 110.42(19) . . . no C21 C25 C26 112.9(2) . . . no N3B B1 C1 124.4(12) . . . yes N3 B1 C1 115.6(2) . . . yes N1 C2 H2 126.00 . . . no C3 C2 H2 126.00 . . . no N2 C3 H3 127.00 . . . no C2 C3 H3 127.00 . . . no C5 C6 H6 119.00 . . . no C7 C6 H6 119.00 . . . no C6 C7 H7 120.00 . . . no C8 C7 H7 120.00 . . . no C7 C8 H8 120.00 . . . no C9 C8 H8 119.00 . . . no C5 C10 H10 107.00 . . . no C11 C10 H10 107.00 . . . no C12 C10 H10 107.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 109.00 . . . no C10 C11 H11C 109.00 . . . no H11A C11 H11B 109.00 . . . no H11A C11 H11C 109.00 . . . no H11B C11 H11C 109.00 . . . no C10 C12 H12A 109.00 . . . no C10 C12 H12B 109.00 . . . no C10 C12 H12C 109.00 . . . no H12A C12 H12B 109.00 . . . no H12A C12 H12C 109.00 . . . no H12B C12 H12C 109.00 . . . no C9 C13 H13 108.00 . . . no C14 C13 H13 108.00 . . . no C15 C13 H13 108.00 . . . no C13 C14 H14A 109.00 . . . no C13 C14 H14B 109.00 . . . no C13 C14 H14C 109.00 . . . no H14A C14 H14B 109.00 . . . no H14A C14 H14C 109.00 . . . no H14B C14 H14C 109.00 . . . no C13 C15 H15A 109.00 . . . no C13 C15 H15B 109.00 . . . no C13 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 109.00 . . . no H15B C15 H15C 109.00 . . . no C17 C18 H18 119.00 . . . no C19 C18 H18 119.00 . . . no C18 C19 H19 120.00 . . . no C20 C19 H19 120.00 . . . no C19 C20 H20 119.00 . . . no C21 C20 H20 119.00 . . . no C17 C22 H22 108.00 . . . no C23 C22 H22 108.00 . . . no C24 C22 H22 108.00 . . . no C22 C23 H23A 109.00 . . . no C22 C23 H23B 109.00 . . . no C22 C23 H23C 109.00 . . . no H23A C23 H23B 109.00 . . . no H23A C23 H23C 109.00 . . . no H23B C23 H23C 109.00 . . . no C22 C24 H24A 109.00 . . . no C22 C24 H24B 110.00 . . . no C22 C24 H24C 109.00 . . . no H24A C24 H24B 109.00 . . . no H24A C24 H24C 109.00 . . . no H24B C24 H24C 109.00 . . . no C21 C25 H25 108.00 . . . no C26 C25 H25 108.00 . . . no C27 C25 H25 108.00 . . . no C25 C26 H26A 109.00 . . . no C25 C26 H26B 109.00 . . . no C25 C26 H26C 109.00 . . . no H26A C26 H26B 109.00 . . . no H26A C26 H26C 109.00 . . . no H26B C26 H26C 109.00 . . . no C25 C27 H27A 109.00 . . . no C25 C27 H27B 109.00 . . . no C25 C27 H27C 109.00 . . . no H27A C27 H27B 109.00 . . . no H27A C27 H27C 109.00 . . . no H27B C27 H27C 109.00 . . . no N3 C28 H28A 109.00 . . . no N3 C28 H28B 109.00 . . . no N3 C28 H28C 110.00 . . . no H28A C28 H28B 109.00 . . . no H28A C28 H28C 110.00 . . . no H28B C28 H28C 109.00 . . . no N3 C29 H29A 109.00 . . . no N3 C29 H29B 109.00 . . . no N3 C29 H29C 109.00 . . . no H29A C29 H29B 109.00 . . . no H29A C29 H29C 110.00 . . . no H29B C29 H29C 109.00 . . . no H29D C29B H29E 109.00 . . . no H29D C29B H29F 110.00 . . . no H29E C29B H29F 109.00 . . . no N3B C29B H29D 109.00 . . . no N3B C29B H29E 109.00 . . . no N3B C29B H29F 110.00 . . . no H30A C30 H30B 109.00 . . . no H30A C30 H30C 109.00 . . . no H30B C30 H30C 109.00 . . . no N4 C30 H30A 109.00 . . . no N4 C30 H30B 109.00 . . . no N4 C30 H30C 110.00 . . . no N4B C30B H30D 109.00 . . . no H30D C30B H30E 109.00 . . . no H30D C30B H30F 109.00 . . . no H30E C30B H30F 109.00 . . . no N4B C30B H30E 111.00 . . . no N4B C30B H30F 109.00 . . . no H31A C31 H31B 110.00 . . . no N4 C31 H31A 109.00 . . . no H31A C31 H31C 109.00 . . . no H31B C31 H31C 109.00 . . . no N4 C31 H31B 109.00 . . . no N4 C31 H31C 109.00 . . . no H31D C31B H31E 109.00 . . . no N4B C31B H31D 109.00 . . . no N4B C31B H31E 110.00 . . . no N4B C31B H31F 109.00 . . . no H31D C31B H31F 110.00 . . . no H31E C31B H31F 109.00 . . . no C1 B1 Hb12 107.2(11) . . . no N3B B1 Hb11 97.0(15) . . . no N3B B1 Hb12 110.6(17) . . . no Hb11 B1 Hb12 110.2(15) . . . no N3 B1 Hb12 110.1(11) . . . no C1 B1 Hb11 106.6(10) . . . no N3 B1 Hb11 107.1(10) . . . no N4 B2 Hb21 106.5(13) . . . no N4 B2 Hb22 107.7(14) . . . no N4B B2 Hb23 121.1(19) . . . no Hb21 B2 Hb22 109.8(18) . . . no Hb21 B2 Hb23 108.5(19) . . . no Hb22 B2 Hb23 115(2) . . . no N4 B2 Hb23 109.5(15) . . . no N4B B2 Hb21 100.9(18) . . . no N4B B2 Hb22 100.8(18) . . . no H28D C28B H28E 110.00 . . . no H28D C28B H28F 109.00 . . . no H28E C28B H28F 110.00 . . . no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N3 2.026(5) . . yes Al1 N4 1.948(6) . . yes Al1 N3B 1.72(3) . . yes Al1 N4B 1.66(4) . . yes Al1 Ha2 1.57(3) . . no Al1 Ha1 1.46(2) . . no N1 C2 1.379(3) . . yes N1 C1 1.360(3) . . yes N1 C4 1.449(3) . . yes N2 C3 1.381(3) . . yes N2 C1 1.359(3) . . yes N2 C16 1.451(3) . . yes N3 C29 1.534(7) . . yes N3 B1 1.555(6) . . yes N3 C28 1.418(8) . . yes N3B C29B 1.32(4) . . yes N3B B1 1.66(3) . . yes N4 B2 1.599(6) . . yes N4 C30 1.473(8) . . yes N4 C31 1.483(9) . . yes N4B B2 1.70(4) . . yes N4B C31B 1.48(5) . . yes N4B C30B 1.48(5) . . yes C1 B1 1.628(3) . . yes C2 C3 1.339(3) . . no C4 C9 1.393(3) . . no C4 C5 1.409(3) . . no C5 C6 1.384(3) . . no C5 C10 1.514(3) . . no C6 C7 1.379(4) . . no C7 C8 1.378(4) . . no C8 C9 1.392(3) . . no C9 C13 1.524(3) . . no C10 C11 1.522(4) . . no C10 C12 1.527(4) . . no C13 C15 1.530(4) . . no C13 C14 1.534(4) . . no C16 C17 1.397(3) . . no C16 C21 1.404(3) . . no C17 C22 1.520(3) . . no C17 C18 1.388(3) . . no C18 C19 1.380(3) . . no C19 C20 1.380(4) . . no C20 C21 1.385(4) . . no C21 C25 1.517(4) . . no C22 C23 1.532(3) . . no C22 C24 1.538(4) . . no C25 C26 1.529(3) . . no C25 C27 1.536(4) . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C10 H10 1.0000 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no C12 H12A 0.9800 . . no C12 H12B 0.9800 . . no C12 H12C 0.9800 . . no C13 H13 1.0000 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C14 H14C 0.9800 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C18 H18 0.9500 . . no C19 H19 0.9500 . . no C20 H20 0.9500 . . no C22 H22 1.0000 . . no C23 H23A 0.9800 . . no C23 H23B 0.9800 . . no C23 H23C 0.9800 . . no C24 H24A 0.9800 . . no C24 H24B 0.9800 . . no C24 H24C 0.9800 . . no C25 H25 1.0000 . . no C26 H26A 0.9800 . . no C26 H26B 0.9800 . . no C26 H26C 0.9800 . . no C27 H27A 0.9800 . . no C27 H27B 0.9800 . . no C27 H27C 0.9800 . . no C28 H28A 0.9800 . . no C28 H28B 0.9800 . . no C28 H28C 0.9800 . . no C29 H29A 0.9800 . . no C29 H29B 0.9800 . . no C29 H29C 0.9800 . . no C29B H29F 0.9800 . . no C29B H29D 0.9800 . . no C29B H29E 0.9800 . . no C30 H30A 0.9800 . . no C30 H30B 0.9800 . . no C30 H30C 0.9800 . . no C30B H30F 0.9900 . . no C30B H30D 0.9800 . . no C30B H30E 0.9800 . . no C31 H31A 0.9800 . . no C31 H31B 0.9800 . . no C31 H31C 0.9800 . . no C31B H31D 0.9800 . . no C31B H31F 0.9800 . . no C31B H31E 0.9800 . . no B1 Hb12 1.09(2) . . no B1 Hb11 1.09(2) . . no B2 Hb23 1.12(3) . . no B2 Hb21 1.09(2) . . no B2 Hb22 1.09(3) . . no C28B H28D 0.9800 . . no C28B H28E 0.9800 . . no C28B H28F 0.9800 . . no 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 _geom_hbond_publ_flag C2 H2 Hb21 0.9500 2.2400 2.97(2) 133.00 2_655 yes C10 H10 N1 1.0000 2.5100 2.892(4) 102.00 . yes C13 H13 N1 1.0000 2.4400 2.920(4) 109.00 . yes C22 H22 N2 1.0000 2.5000 2.933(4) 106.00 . yes C25 H25 N2 1.0000 2.3900 2.880(4) 109.00 . yes 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 N4 Al1 N3 B1 -46.8(4) . . . . no N3 Al1 N4 C30 -48.4(5) . . . . no N4 Al1 N3 C28 82.8(5) . . . . no N4 Al1 N3 C29 -161.5(4) . . . . no N3 Al1 N4 B2 -166.6(3) . . . . no N3 Al1 N4 C31 79.8(5) . . . . no C4 N1 C1 N2 -176.10(17) . . . . no C2 N1 C1 B1 170.14(17) . . . . no C2 N1 C4 C5 -102.7(2) . . . . no C4 N1 C1 B1 -5.5(3) . . . . no C2 N1 C1 N2 -0.5(2) . . . . no C1 N1 C2 C3 0.1(2) . . . . no C2 N1 C4 C9 74.1(2) . . . . no C1 N1 C4 C5 72.4(3) . . . . no C1 N1 C4 C9 -110.7(2) . . . . no C4 N1 C2 C3 175.98(17) . . . . no C3 N2 C1 N1 0.6(2) . . . . no C1 N2 C16 C17 106.9(2) . . . . no C3 N2 C16 C17 -83.4(2) . . . . no C3 N2 C16 C21 93.8(2) . . . . no C1 N2 C16 C21 -76.0(2) . . . . no C1 N2 C3 C2 -0.6(2) . . . . no C16 N2 C3 C2 -171.69(17) . . . . no C3 N2 C1 B1 -169.48(18) . . . . no C16 N2 C1 N1 171.37(16) . . . . no C16 N2 C1 B1 1.3(3) . . . . no Al1 N3 B1 C1 -162.70(19) . . . . no C28 N3 B1 C1 70.7(6) . . . . no C29 N3 B1 C1 -53.5(4) . . . . no N1 C1 B1 N3 107.1(3) . . . . no N2 C1 B1 N3 -84.7(3) . . . . no N1 C2 C3 N2 0.2(2) . . . . no N1 C4 C5 C6 179.73(18) . . . . no N1 C4 C5 C10 2.1(3) . . . . no C9 C4 C5 C6 3.0(3) . . . . no C9 C4 C5 C10 -174.6(2) . . . . no N1 C4 C9 C8 -178.27(19) . . . . no N1 C4 C9 C13 -0.2(3) . . . . no C5 C4 C9 C8 -1.6(3) . . . . no C5 C4 C9 C13 176.5(2) . . . . no C4 C5 C6 C7 -2.6(3) . . . . no C10 C5 C6 C7 175.1(2) . . . . no C4 C5 C10 C11 -151.6(2) . . . . no C4 C5 C10 C12 83.7(3) . . . . no C6 C5 C10 C11 30.8(3) . . . . no C6 C5 C10 C12 -93.8(3) . . . . no C5 C6 C7 C8 0.8(4) . . . . no C6 C7 C8 C9 0.8(4) . . . . no C7 C8 C9 C4 -0.4(3) . . . . no C7 C8 C9 C13 -178.5(2) . . . . no C4 C9 C13 C14 131.1(2) . . . . no C4 C9 C13 C15 -105.0(2) . . . . no C8 C9 C13 C14 -50.9(3) . . . . no C8 C9 C13 C15 73.0(3) . . . . no N2 C16 C17 C18 179.84(17) . . . . no N2 C16 C17 C22 2.1(3) . . . . no C21 C16 C17 C18 2.9(3) . . . . no C21 C16 C17 C22 -174.83(19) . . . . no N2 C16 C21 C20 178.54(18) . . . . no N2 C16 C21 C25 -6.0(3) . . . . no C17 C16 C21 C20 -4.5(3) . . . . no C17 C16 C21 C25 171.02(19) . . . . no C16 C17 C18 C19 0.9(3) . . . . no C22 C17 C18 C19 178.7(2) . . . . no C16 C17 C22 C23 -142.1(2) . . . . no C16 C17 C22 C24 95.2(2) . . . . no C18 C17 C22 C23 40.3(3) . . . . no C18 C17 C22 C24 -82.5(2) . . . . no C17 C18 C19 C20 -3.0(3) . . . . no C18 C19 C20 C21 1.3(4) . . . . no C19 C20 C21 C16 2.3(3) . . . . no C19 C20 C21 C25 -173.3(2) . . . . no C16 C21 C25 C26 135.8(2) . . . . no C16 C21 C25 C27 -100.8(2) . . . . no C20 C21 C25 C26 -48.9(3) . . . . no C20 C21 C25 C27 74.5(3) . . . . no