#------------------------------------------------------------------------------ #$Date: 2021-10-06 16:57:59 +0300 (Wed, 06 Oct 2021) $ #$Revision: 269648 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/88/7128814.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_7128814 loop_ _publ_author_name 'Morris, Louis J.' 'Carpentier, Ambre' 'Maron, Laurent' 'Okuda, Jun' _publ_section_title ; Reductive elimination of [AlH2]+ from a cationic Ga-Al dihydride. ; _journal_issue 74 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 9454 _journal_page_last 9457 _journal_paper_doi 10.1039/d1cc03706d _journal_volume 57 _journal_year 2021 _chemical_formula_moiety '2(C43 H67 Al2 N6), 2(C32 H36 B), C7 H8' _chemical_formula_sum 'C157 H214 Al4 B2 N12' _chemical_formula_weight 2398.93 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-07-08 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-07-09 deposited with the CCDC. 2021-08-13 downloaded from the CCDC. ; _cell_angle_alpha 96.05(3) _cell_angle_beta 102.03(3) _cell_angle_gamma 108.20(3) _cell_formula_units_Z 1 _cell_length_a 12.130(2) _cell_length_b 16.522(3) _cell_length_c 20.716(4) _cell_measurement_reflns_used 69156 _cell_measurement_temperature 150 _cell_measurement_theta_max 72.43 _cell_measurement_theta_min 2.22 _cell_volume 3791.9(16) _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'Hybrid Pixel Counting Detector' _diffrn_detector_area_resol_mean 5.81 _diffrn_detector_type 'Dectris Pilatus 200K' _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'STOE STADIVARI' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.5 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_polarisn_norm 270 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 94792 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.134 _diffrn_reflns_theta_min 2.218 _diffrn_source 'sealed x-ray tube' _diffrn_source_current 0.600 _diffrn_source_power 0.030 _diffrn_source_target Cu _diffrn_source_type 'Xenocs Cu microfocus tube' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_T_max 0.7511 _exptl_absorpt_correction_T_min 0.2652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Finally a spherical absorption correction was done within STOE LANA. ; _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.051 _exptl_crystal_description Block _exptl_crystal_F_000 1302 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Toluene' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.297 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.266 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef 0.00195(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 860 _refine_ls_number_reflns 14496 _refine_ls_number_restraints 136 _refine_ls_restrained_S_all 0.979 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0481 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1304 _refine_ls_wR_factor_ref 0.1402 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10438 _reflns_number_total 14496 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc03706d2.cif _cod_data_source_block 4Al _cod_depositor_comments 'Adding full bibliography for 7128813--7128817.cif.' _cod_original_cell_volume 3791.8(15) _cod_database_code 7128814 _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_max 0.878 _shelx_estimated_absorpt_t_min 0.745 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C82-C76 1.51 with sigma of 0.02 C76-C77 = C76-C81 = C78-C79 1.39 with sigma of 0.02 C77-C78 = C79-C80 = C80-C81 1.38 with sigma of 0.02 C76-C78 2.42 with sigma of 0.04 C77-C79 2.39 with sigma of 0.04 C76-C80 2.41 with sigma of 0.04 C78-C80 = C79-C81 2.4 with sigma of 0.04 C82-C77 = C82-C81 2.52 with sigma of 0.04 C76-C77 \\sim C77-C78 \\sim C78-C79 \\sim C79-C80 \\sim C80-C81 \\sim C81-C76 with sigma of 0.02 C76-C80 \\sim C76-C78 \\sim C81-C79 \\sim C77-C81 \\sim C78-C80 \\sim C77-C79 with sigma of 0.04 C82-C81 \\sim C82-C77 with sigma of 0.04 3. Restrained planarity C76, C77, C78, C79, C80, C81, C82 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 5. Rigid body (RIGU) restrains C76, C77, C78, C79, C80, C81, C82 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: C76(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) C79(0.5) H79(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5) 7.a Ternary CH refined with riding coordinates: C12(H12), C15(H15), C24(H24), C27(H27) 7.b Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C45(H45), C47(H47), C49(H49), C53(H53), C55(H55), C57(H57), C61(H61), C63(H63), C65(H65), C69(H69), C71(H71), C73(H73), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81) 7.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B, H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A, H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B, H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C66(H66A, H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C82(H82A,H82B,H82C) ; _shelx_res_file ; p-1.res created by SHELXL-2014/7 TITL p-1_a.res in P-1 REM Old TITL P-1 in P-1 REM SHELXT solution in P-1 REM R1 0.169, Rweak 0.010, Alpha 0.054, Orientation as input REM Formula found by SHELXT: C79 B2 N6 Al2 CELL 1.54178 12.1301 16.5216 20.7158 96.048 102.031 108.202 ZERR 1 0.0024 0.0033 0.0041 0.03 0.03 0.03 LATT 1 SFAC C H Al B N UNIT 157 214 4 2 12 DFIX 1.51 C82 C76 DANG 2.42 C76 C78 FLAT C76 C77 C78 C79 C80 C81 C82 DFIX 1.39 C76 C77 C76 C81 C78 C79 DANG 2.39 C77 C79 DFIX 1.38 C77 C78 C79 C80 C80 C81 RIGU C76 > C82 SADI C76 C77 C77 C78 C78 C79 C79 C80 C80 C81 C81 C76 DANG 2.41 C76 C80 SADI 0.04 C76 C80 C76 C78 C81 C79 C77 C81 C78 C80 C77 C79 DANG 2.4 C78 C80 C79 C81 SIMU C76 > C82 SADI 0.04 C82 C81 C82 C77 DANG 2.52 C82 C77 C82 C81 L.S. 16 0 0 PLAN 29 SIZE 0.2 0.297 0.47 TEMP -123(2) CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.094200 EXTI 0.001954 FVAR 0.47881 AL1 3 0.522398 0.419913 0.299672 11.00000 0.04317 0.03746 = 0.03376 0.00408 0.00713 0.01335 H 2 0.409776 0.410055 0.325929 11.00000 0.06202 AL2 3 0.537349 0.277858 0.238981 11.00000 0.04642 0.03923 = 0.04116 0.00239 0.00657 0.01459 HA 2 0.659934 0.285472 0.227882 11.00000 0.05677 N1 5 0.662776 0.480010 0.371274 11.00000 0.04816 0.04054 = 0.03316 0.00139 0.00710 0.01505 N2 5 0.539269 0.517506 0.253921 11.00000 0.04467 0.03832 = 0.03470 0.00420 0.00821 0.01482 N3 5 0.390882 0.136103 0.301991 11.00000 0.05961 0.04801 = 0.05343 0.00497 0.01595 0.01813 N4 5 0.576481 0.149529 0.330609 11.00000 0.06465 0.05010 = 0.05175 0.00769 0.00917 0.02726 N5 5 0.325757 0.225622 0.111781 11.00000 0.05793 0.04107 = 0.04620 0.00627 0.00204 0.01012 N6 5 0.446218 0.156678 0.102895 11.00000 0.07058 0.04144 = 0.04547 0.00253 0.01554 0.01292 C1 1 0.779382 0.606246 0.461684 11.00000 0.07417 0.05203 = 0.04226 -0.00744 0.00006 0.01681 AFIX 137 H1A 2 0.735734 0.590704 0.495952 11.00000 -1.50000 H1B 2 0.809404 0.669418 0.465717 11.00000 -1.50000 H1C 2 0.847097 0.584980 0.468066 11.00000 -1.50000 AFIX 0 C2 1 0.695842 0.565524 0.392666 11.00000 0.05166 0.04641 = 0.03701 -0.00402 0.00705 0.01434 C3 1 0.657581 0.620042 0.354473 11.00000 0.06152 0.03749 = 0.04409 -0.00265 0.00797 0.01505 H3 2 0.686410 0.678007 0.375136 11.00000 0.05273 C4 1 0.593369 0.599142 0.286555 11.00000 0.05402 0.03729 = 0.04388 0.00456 0.01253 0.01551 C5 1 0.591616 0.674144 0.251934 11.00000 0.07699 0.03972 = 0.05612 0.00792 0.00770 0.01747 AFIX 137 H5A 2 0.572118 0.654818 0.203254 11.00000 -1.50000 H5B 2 0.670675 0.719862 0.266822 11.00000 -1.50000 H5C 2 0.530908 0.696779 0.263097 11.00000 -1.50000 AFIX 0 C6 1 0.734197 0.434359 0.405455 11.00000 0.04853 0.04502 = 0.03517 -0.00047 0.00128 0.01593 C7 1 0.700174 0.392588 0.457517 11.00000 0.05819 0.05352 = 0.03756 0.00563 0.00397 0.01855 C8 1 0.772822 0.350314 0.488889 11.00000 0.06992 0.06448 = 0.04647 0.01350 0.00247 0.02514 AFIX 43 H8 2 0.751165 0.320794 0.523774 11.00000 -1.20000 AFIX 0 C9 1 0.875329 0.350243 0.470582 11.00000 0.06631 0.07543 = 0.05705 0.01078 -0.00312 0.03522 AFIX 43 H9 2 0.924336 0.321731 0.493343 11.00000 -1.20000 AFIX 0 C10 1 0.907224 0.391229 0.419507 11.00000 0.05284 0.07508 = 0.05353 0.00325 0.00112 0.02769 AFIX 43 H10 2 0.978505 0.390913 0.407456 11.00000 -1.20000 AFIX 0 C11 1 0.836976 0.433205 0.385104 11.00000 0.04962 0.05272 = 0.04088 -0.00130 0.00160 0.01735 C12 1 0.588092 0.393368 0.479209 11.00000 0.06752 0.06347 = 0.04351 0.01548 0.01753 0.02525 AFIX 13 H12 2 0.560950 0.438359 0.458843 11.00000 -1.20000 AFIX 0 C13 1 0.611550 0.417325 0.555502 11.00000 0.10041 0.11650 = 0.04674 0.00973 0.02336 0.04356 AFIX 137 H13A 2 0.634494 0.372686 0.576736 11.00000 -1.50000 H13B 2 0.538539 0.421289 0.566657 11.00000 -1.50000 H13C 2 0.676627 0.473327 0.571929 11.00000 -1.50000 AFIX 0 C14 1 0.487449 0.305969 0.451832 11.00000 0.06967 0.07670 = 0.06429 0.02284 0.02310 0.01860 AFIX 137 H14A 2 0.470244 0.293905 0.402739 11.00000 -1.50000 H14B 2 0.415126 0.307679 0.465103 11.00000 -1.50000 H14C 2 0.512425 0.260266 0.470095 11.00000 -1.50000 AFIX 0 C15 1 0.872537 0.477218 0.328035 11.00000 0.05043 0.07121 = 0.04357 0.00469 0.00892 0.02187 AFIX 13 H15 2 0.799021 0.483899 0.300228 11.00000 -1.20000 AFIX 0 C16 1 0.965941 0.567147 0.353020 11.00000 0.10373 0.06683 = 0.06125 0.00713 0.02484 0.00967 AFIX 137 H16A 2 0.933908 0.603493 0.378751 11.00000 -1.50000 H16B 2 0.985836 0.592961 0.314613 11.00000 -1.50000 H16C 2 1.038424 0.563085 0.381836 11.00000 -1.50000 AFIX 0 C17 1 0.917312 0.423816 0.282317 11.00000 0.05946 0.08145 = 0.06905 -0.00628 0.02538 0.01393 AFIX 137 H17A 2 0.994822 0.422082 0.306588 11.00000 -1.50000 H17B 2 0.926857 0.450207 0.242704 11.00000 -1.50000 H17C 2 0.859138 0.364711 0.268168 11.00000 -1.50000 AFIX 0 C18 1 0.473402 0.501035 0.184340 11.00000 0.04943 0.03464 = 0.03454 0.00806 0.00653 0.01313 C19 1 0.522392 0.471231 0.134923 11.00000 0.05131 0.03845 = 0.03780 0.00756 0.00974 0.01209 C20 1 0.455669 0.451437 0.068182 11.00000 0.06090 0.05045 = 0.03737 0.00761 0.00810 0.01455 AFIX 43 H20 2 0.486756 0.430768 0.033953 11.00000 -1.20000 AFIX 0 C21 1 0.344813 0.461511 0.051182 11.00000 0.06291 0.05414 = 0.04134 0.01164 0.00011 0.01328 AFIX 43 H21 2 0.300670 0.448138 0.005481 11.00000 -1.20000 AFIX 0 C22 1 0.298359 0.490831 0.100260 11.00000 0.05194 0.05114 = 0.05444 0.01677 0.00183 0.01824 AFIX 43 H22 2 0.222370 0.497800 0.087929 11.00000 -1.20000 AFIX 0 C23 1 0.360920 0.510570 0.167976 11.00000 0.05190 0.04074 = 0.04818 0.01240 0.00952 0.01810 C24 1 0.646474 0.464141 0.153641 11.00000 0.05271 0.05558 = 0.03759 0.00630 0.01244 0.01878 AFIX 13 H24 2 0.655745 0.444974 0.198056 11.00000 -1.20000 AFIX 0 C25 1 0.744702 0.551875 0.163131 11.00000 0.05383 0.06863 = 0.05604 0.00279 0.01727 0.01321 AFIX 137 H25A 2 0.735645 0.574625 0.121262 11.00000 -1.50000 H25B 2 0.823461 0.545121 0.175131 11.00000 -1.50000 H25C 2 0.738161 0.592295 0.199101 11.00000 -1.50000 AFIX 0 C26 1 0.664955 0.396808 0.104344 11.00000 0.06621 0.06773 = 0.04406 0.00830 0.01921 0.02868 AFIX 137 H26A 2 0.598222 0.341836 0.096281 11.00000 -1.50000 H26B 2 0.740554 0.388100 0.123338 11.00000 -1.50000 H26C 2 0.667920 0.417376 0.061847 11.00000 -1.50000 AFIX 0 C27 1 0.303223 0.538335 0.220878 11.00000 0.05797 0.06731 = 0.06280 0.01264 0.01531 0.03569 AFIX 13 H27 2 0.364985 0.558172 0.264929 11.00000 -1.20000 AFIX 0 C28 1 0.260675 0.613492 0.205300 11.00000 0.11435 0.10196 = 0.08692 0.01412 0.01693 0.08002 AFIX 137 H28A 2 0.197322 0.594709 0.163259 11.00000 -1.50000 H28B 2 0.328225 0.661985 0.200733 11.00000 -1.50000 H28C 2 0.229149 0.632057 0.241902 11.00000 -1.50000 AFIX 0 C29 1 0.198658 0.461757 0.227772 11.00000 0.05690 0.11008 = 0.08983 0.02129 0.03245 0.02566 AFIX 137 H29A 2 0.162956 0.480699 0.262196 11.00000 -1.50000 H29B 2 0.228120 0.415443 0.240816 11.00000 -1.50000 H29C 2 0.137921 0.440079 0.184720 11.00000 -1.50000 AFIX 0 C30 1 0.499513 0.180827 0.292549 11.00000 0.05216 0.03886 = 0.04503 0.00139 0.00831 0.01778 C31 1 0.279247 0.149953 0.271292 11.00000 0.05277 0.07148 = 0.06617 0.00598 0.01517 0.01765 AFIX 137 H31A 2 0.295086 0.212085 0.272547 11.00000 -1.50000 H31B 2 0.219363 0.127708 0.296268 11.00000 -1.50000 H31C 2 0.248781 0.119311 0.224571 11.00000 -1.50000 AFIX 0 C32 1 0.400064 0.078860 0.344945 11.00000 0.08991 0.04783 = 0.06852 0.01732 0.03204 0.02514 C33 1 0.292389 0.019631 0.362142 11.00000 0.11640 0.08005 = 0.11211 0.04071 0.06173 0.02712 AFIX 137 H33A 2 0.252944 0.054291 0.383587 11.00000 -1.50000 H33B 2 0.317999 -0.015904 0.393012 11.00000 -1.50000 H33C 2 0.236023 -0.018108 0.321037 11.00000 -1.50000 AFIX 0 C34 1 0.517281 0.087731 0.363523 11.00000 0.09417 0.05729 = 0.06353 0.02155 0.02365 0.03831 C35 1 0.581973 0.044120 0.410382 11.00000 0.14636 0.10954 = 0.10044 0.05740 0.03929 0.07861 AFIX 137 H35A 2 0.628244 0.017755 0.387026 11.00000 -1.50000 H35B 2 0.523398 -0.000924 0.425145 11.00000 -1.50000 H35C 2 0.636444 0.087101 0.449519 11.00000 -1.50000 AFIX 0 C36 1 0.706081 0.176895 0.336005 11.00000 0.05964 0.06822 = 0.06824 0.00445 0.00155 0.03189 AFIX 137 H36A 2 0.726724 0.126793 0.320304 11.00000 -1.50000 H36B 2 0.750402 0.201054 0.382953 11.00000 -1.50000 H36C 2 0.727529 0.221086 0.308354 11.00000 -1.50000 AFIX 0 C37 1 0.426007 0.214634 0.146304 11.00000 0.05432 0.03538 = 0.04061 0.00358 0.00739 0.01186 C38 1 0.264091 0.278904 0.138583 11.00000 0.05515 0.05136 = 0.06563 0.00788 -0.00043 0.01736 AFIX 137 H38A 2 0.184405 0.241806 0.140328 11.00000 -1.50000 H38B 2 0.255654 0.320875 0.109520 11.00000 -1.50000 H38C 2 0.310750 0.309860 0.183922 11.00000 -1.50000 AFIX 0 C39 1 0.285673 0.175956 0.047339 11.00000 0.07108 0.04636 = 0.04090 0.00760 0.00009 0.00237 C40 1 0.178719 0.178290 -0.002383 11.00000 0.09247 0.08514 = 0.05717 0.01281 -0.01558 0.01098 AFIX 137 H40A 2 0.109586 0.164991 0.017153 11.00000 -1.50000 H40B 2 0.160761 0.135255 -0.042955 11.00000 -1.50000 H40C 2 0.195593 0.236155 -0.013989 11.00000 -1.50000 AFIX 0 C41 1 0.360535 0.132045 0.042288 11.00000 0.08469 0.04457 = 0.03956 0.00439 0.01301 0.00515 C42 1 0.356599 0.066363 -0.014171 11.00000 0.12761 0.05805 = 0.04505 -0.00257 0.02348 0.01047 AFIX 137 H42A 2 0.351229 0.011553 0.001322 11.00000 -1.50000 H42B 2 0.429677 0.087109 -0.029759 11.00000 -1.50000 H42C 2 0.286304 0.057274 -0.051171 11.00000 -1.50000 AFIX 0 C43 1 0.547621 0.124802 0.117128 11.00000 0.08408 0.06076 = 0.07425 0.00043 0.02697 0.03086 AFIX 137 H43A 2 0.598016 0.142423 0.086198 11.00000 -1.50000 H43B 2 0.517052 0.061424 0.111211 11.00000 -1.50000 H43C 2 0.595356 0.149322 0.163459 11.00000 -1.50000 AFIX 0 C44 1 0.892791 0.056290 0.259749 11.00000 0.04376 0.03898 = 0.03805 0.00654 0.00797 0.01421 C45 1 0.976970 0.112709 0.316336 11.00000 0.04940 0.04122 = 0.03727 0.00476 0.00467 0.01646 AFIX 43 H45 2 0.997331 0.089927 0.355582 11.00000 -1.20000 AFIX 0 C46 1 1.032280 0.200938 0.317624 11.00000 0.04916 0.03926 = 0.04768 0.00160 0.00424 0.01461 C47 1 1.003266 0.234771 0.260972 11.00000 0.05265 0.03342 = 0.05685 0.00752 0.00882 0.01269 AFIX 43 H47 2 1.042579 0.294301 0.260879 11.00000 -1.20000 AFIX 0 C48 1 0.916960 0.182669 0.203859 11.00000 0.05336 0.04236 = 0.04708 0.01230 0.00932 0.01946 C49 1 0.862682 0.095610 0.204638 11.00000 0.04688 0.04051 = 0.03888 0.00637 0.00448 0.01383 AFIX 43 H49 2 0.802173 0.060665 0.166132 11.00000 -1.20000 AFIX 0 C50 1 1.123180 0.258952 0.380134 11.00000 0.07181 0.04802 = 0.05883 -0.00315 -0.00638 0.01236 AFIX 137 H50A 2 1.081113 0.275065 0.412167 11.00000 -1.50000 H50B 2 1.173030 0.311386 0.368046 11.00000 -1.50000 H50C 2 1.174209 0.227940 0.400633 11.00000 -1.50000 AFIX 0 C51 1 0.885524 0.221131 0.142424 11.00000 0.07072 0.05416 = 0.06038 0.02333 0.00663 0.01932 AFIX 137 H51A 2 0.842166 0.174386 0.103541 11.00000 -1.50000 H51B 2 0.959303 0.258710 0.133846 11.00000 -1.50000 H51C 2 0.834737 0.255212 0.150085 11.00000 -1.50000 AFIX 0 C52 1 0.936456 -0.083978 0.217610 11.00000 0.04688 0.03666 = 0.04489 0.00535 0.00329 0.01174 C53 1 0.994744 -0.041230 0.172854 11.00000 0.04961 0.04297 = 0.04326 0.00608 0.00635 0.01566 AFIX 43 H53 2 0.985258 0.012089 0.164891 11.00000 -1.20000 AFIX 0 C54 1 1.065715 -0.072132 0.139343 11.00000 0.04594 0.05476 = 0.05148 0.00277 0.00785 0.01384 C55 1 1.082209 -0.148556 0.151745 11.00000 0.04694 0.05654 = 0.08157 -0.00236 0.01495 0.01836 AFIX 43 H55 2 1.129793 -0.171109 0.129098 11.00000 -1.20000 AFIX 0 C56 1 1.029481 -0.192692 0.197247 11.00000 0.05569 0.04426 = 0.09930 0.01043 0.01849 0.02042 C57 1 0.956768 -0.160941 0.227800 11.00000 0.05685 0.04283 = 0.07370 0.01662 0.01643 0.01742 AFIX 43 H57 2 0.918553 -0.193081 0.257285 11.00000 -1.20000 AFIX 0 C58 1 1.125078 -0.022114 0.091449 11.00000 0.06710 0.08972 = 0.06448 0.01693 0.02822 0.02920 AFIX 137 H58A 2 1.204106 0.019234 0.116172 11.00000 -1.50000 H58B 2 1.075070 0.009332 0.070533 11.00000 -1.50000 H58C 2 1.134549 -0.062480 0.056590 11.00000 -1.50000 AFIX 0 C59 1 1.054178 -0.273278 0.214501 11.00000 0.09327 0.06196 = 0.18638 0.03905 0.05192 0.04315 AFIX 137 H59A 2 1.023438 -0.318664 0.174255 11.00000 -1.50000 H59B 2 1.014188 -0.293669 0.249217 11.00000 -1.50000 H59C 2 1.140884 -0.259631 0.231192 11.00000 -1.50000 AFIX 0 C60 1 0.848714 -0.077774 0.327565 11.00000 0.06179 0.03616 = 0.04154 0.00770 0.00737 0.01287 C61 1 0.955557 -0.075730 0.371036 11.00000 0.06789 0.05074 = 0.04830 0.01608 0.00315 0.01576 AFIX 43 H61 2 1.027767 -0.056488 0.357097 11.00000 -1.20000 AFIX 0 C62 1 0.961191 -0.100628 0.433973 11.00000 0.09667 0.04932 = 0.04601 0.01467 0.00076 0.02186 C63 1 0.857226 -0.127341 0.454715 11.00000 0.12157 0.04911 = 0.04428 0.01824 0.01848 0.03049 AFIX 43 H63 2 0.859600 -0.144274 0.497265 11.00000 -1.20000 AFIX 0 C64 1 0.749207 -0.129961 0.414626 11.00000 0.10631 0.03960 = 0.05535 0.01347 0.03427 0.02187 C65 1 0.746416 -0.105754 0.351760 11.00000 0.07250 0.03887 = 0.04637 0.00847 0.01804 0.01600 AFIX 43 H65 2 0.671663 -0.108449 0.324280 11.00000 -1.20000 AFIX 0 C66 1 1.079304 -0.099085 0.477709 11.00000 0.12118 0.07777 = 0.06175 0.02455 -0.01324 0.03612 AFIX 137 H66A 2 1.086504 -0.156502 0.469497 11.00000 -1.50000 H66B 2 1.081643 -0.083586 0.525083 11.00000 -1.50000 H66C 2 1.146000 -0.056171 0.466775 11.00000 -1.50000 AFIX 0 C67 1 0.634617 -0.160716 0.437159 11.00000 0.13656 0.06880 = 0.08768 0.03649 0.07104 0.04292 AFIX 137 H67A 2 0.634884 -0.115957 0.472282 11.00000 -1.50000 H67B 2 0.629195 -0.214118 0.454921 11.00000 -1.50000 H67C 2 0.565519 -0.172000 0.398873 11.00000 -1.50000 AFIX 0 C68 1 0.708030 -0.092488 0.205418 11.00000 0.05186 0.03898 = 0.03792 0.00921 0.00953 0.01131 C69 1 0.619817 -0.057023 0.213125 11.00000 0.04969 0.04511 = 0.04821 0.00177 0.00550 0.01014 AFIX 43 H69 2 0.643673 -0.003620 0.243335 11.00000 -1.20000 AFIX 0 C70 1 0.498845 -0.095501 0.179034 11.00000 0.04794 0.05841 = 0.05799 0.00993 0.00492 0.01073 C71 1 0.464702 -0.172029 0.132931 11.00000 0.05209 0.05812 = 0.05194 0.00976 0.00022 0.00273 AFIX 43 H71 2 0.382970 -0.199132 0.108770 11.00000 -1.20000 AFIX 0 C72 1 0.548016 -0.208974 0.121899 11.00000 0.06894 0.04160 = 0.03938 0.00578 0.00420 0.00305 C73 1 0.668070 -0.169132 0.158257 11.00000 0.06034 0.04201 = 0.03747 0.00802 0.00902 0.01250 AFIX 43 H73 2 0.724731 -0.195329 0.150525 11.00000 -1.20000 AFIX 0 C74 1 0.407087 -0.056643 0.192975 11.00000 0.05097 0.08840 = 0.10073 0.00249 0.00861 0.02085 AFIX 137 H74A 2 0.354464 -0.055660 0.150400 11.00000 -1.50000 H74B 2 0.448151 0.002642 0.218277 11.00000 -1.50000 H74C 2 0.359037 -0.091667 0.219305 11.00000 -1.50000 AFIX 0 C75 1 0.511641 -0.291619 0.070822 11.00000 0.09409 0.05262 = 0.05167 -0.00449 0.00175 0.00340 AFIX 137 H75A 2 0.538508 -0.334670 0.092260 11.00000 -1.50000 H75B 2 0.548816 -0.279101 0.033616 11.00000 -1.50000 H75C 2 0.424109 -0.314453 0.053607 11.00000 -1.50000 AFIX 0 B1 4 0.845812 -0.049031 0.253090 11.00000 0.04992 0.03741 = 0.03901 0.00747 0.00704 0.01332 PART -1 C76 1 0.984236 0.469340 0.003223 10.50000 0.05852 0.12927 = 0.06315 0.04370 0.01444 0.02776 C77 1 0.950500 0.520260 0.047672 10.50000 0.05708 0.13829 = 0.05340 0.03260 0.01843 0.02878 AFIX 43 H77 2 0.908374 0.494385 0.078307 10.50000 -1.20000 AFIX 0 C78 1 0.976973 0.606688 0.047927 10.50000 0.06896 0.13456 = 0.06970 0.00891 0.01155 0.03358 AFIX 43 H78 2 0.955868 0.640929 0.079754 10.50000 -1.20000 AFIX 0 C79 1 1.033468 0.644275 0.002869 10.50000 0.07983 0.12569 = 0.11291 0.04758 0.03763 0.04467 AFIX 43 H79 2 1.048565 0.703988 0.001545 10.50000 -1.20000 AFIX 0 C80 1 1.068564 0.594383 -0.040928 10.50000 0.09149 0.14014 = 0.10512 0.06532 0.05422 0.06297 AFIX 43 H80 2 1.112156 0.621042 -0.070726 10.50000 -1.20000 AFIX 0 C81 1 1.042310 0.508974 -0.042231 10.50000 0.07206 0.14290 = 0.06602 0.05246 0.03229 0.06108 AFIX 43 H81 2 1.063572 0.475404 -0.074441 10.50000 -1.20000 AFIX 0 C82 1 0.952343 0.374136 0.000239 10.50000 0.10231 0.12678 = 0.13088 0.04034 0.00126 0.03038 AFIX 137 H82A 2 0.956911 0.361312 0.045646 10.50000 -1.50000 H82B 2 1.008589 0.354051 -0.018953 10.50000 -1.50000 H82C 2 0.870537 0.344384 -0.027941 10.50000 -1.50000 AFIX 0 HKLF 4 REM p-1_a.res in P-1 REM R1 = 0.0481 for 10438 Fo > 4sig(Fo) and 0.0668 for all 14496 data REM 860 parameters refined using 136 restraints END WGHT 0.0942 0.0000 REM Highest difference peak 0.266, deepest hole -0.305, 1-sigma level 0.039 Q1 1 0.4555 0.2380 0.1791 11.00000 0.05 0.27 Q2 1 0.5267 0.3648 0.2598 11.00000 0.05 0.23 Q3 1 0.8930 -0.0605 0.2400 11.00000 0.05 0.21 Q4 1 0.5441 -0.2436 0.1046 11.00000 0.05 0.20 Q5 1 0.5252 0.3254 0.2798 11.00000 0.05 0.20 Q6 1 0.8789 0.0780 0.2373 11.00000 0.05 0.19 Q7 1 0.4938 0.2002 0.2609 11.00000 0.05 0.18 Q8 1 0.4892 -0.2629 0.0311 11.00000 0.05 0.18 Q9 1 0.8404 -0.0653 0.2863 11.00000 0.05 0.18 Q10 1 0.5867 -0.3060 0.0580 11.00000 0.05 0.18 Q11 1 1.1345 -0.1214 0.4421 11.00000 0.05 0.18 Q12 1 0.6106 0.7246 0.2868 11.00000 0.05 0.18 Q13 1 0.5797 -0.1192 0.4366 11.00000 0.05 0.18 Q14 1 1.0616 -0.1469 0.5073 11.00000 0.05 0.18 Q15 1 0.2496 0.1802 0.0560 11.00000 0.05 0.18 Q16 1 0.2633 0.1955 0.3178 11.00000 0.05 0.18 Q17 1 0.2904 0.1971 0.0553 11.00000 0.05 0.17 Q18 1 0.8633 0.0023 0.2594 11.00000 0.05 0.17 Q19 1 0.5177 0.2206 0.2752 11.00000 0.05 0.16 Q20 1 0.5793 -0.2389 0.4127 11.00000 0.05 0.16 Q21 1 0.5643 0.4964 0.2774 11.00000 0.05 0.16 Q22 1 0.4761 0.4674 0.1581 11.00000 0.05 0.16 Q23 1 1.1276 -0.2827 0.1904 11.00000 0.05 0.16 Q24 1 0.9164 0.2008 0.0984 11.00000 0.05 0.15 Q25 1 1.1087 0.3215 0.3844 11.00000 0.05 0.15 Q26 1 0.5163 0.1647 0.2952 11.00000 0.05 0.15 Q27 1 0.2945 0.1426 0.0522 11.00000 0.05 0.15 Q28 1 0.4924 0.4832 0.1062 11.00000 0.05 0.15 Q29 1 0.7080 0.1571 0.2762 11.00000 0.05 0.15 ; _shelx_res_checksum 1431 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.52240(4) 0.41991(3) 0.29967(2) 0.03887(12) Uani 1 1 d . . . . . H H 0.4098(18) 0.4101(13) 0.3259(10) 0.062(6) Uiso 1 1 d . . . . . Al2 Al 0.53735(4) 0.27786(3) 0.23898(2) 0.04342(13) Uani 1 1 d . . . . . HA H 0.6599(18) 0.2855(13) 0.2279(10) 0.057(5) Uiso 1 1 d . . . . . N1 N 0.66278(12) 0.48001(9) 0.37127(6) 0.0416(3) Uani 1 1 d . . . . . N2 N 0.53927(12) 0.51751(9) 0.25392(6) 0.0396(3) Uani 1 1 d . . . . . N3 N 0.39088(14) 0.13610(11) 0.30199(8) 0.0539(4) Uani 1 1 d . . . . . N4 N 0.57648(15) 0.14953(11) 0.33061(8) 0.0547(4) Uani 1 1 d . . . . . N5 N 0.32576(14) 0.22562(10) 0.11178(7) 0.0520(4) Uani 1 1 d . . . . . N6 N 0.44622(15) 0.15668(10) 0.10289(7) 0.0543(4) Uani 1 1 d . . . . . C1 C 0.77938(19) 0.60625(14) 0.46168(9) 0.0609(5) Uani 1 1 d . . . . . H1A H 0.7357 0.5907 0.4960 0.091 Uiso 1 1 calc R U . . . H1B H 0.8094 0.6694 0.4657 0.091 Uiso 1 1 calc R U . . . H1C H 0.8471 0.5850 0.4681 0.091 Uiso 1 1 calc R U . . . C2 C 0.69584(15) 0.56552(12) 0.39267(8) 0.0472(4) Uani 1 1 d . . . . . C3 C 0.65758(17) 0.62004(12) 0.35447(9) 0.0498(4) Uani 1 1 d . . . . . H3 H 0.6864(17) 0.6780(13) 0.3751(10) 0.053(5) Uiso 1 1 d . . . . . C4 C 0.59337(16) 0.59914(11) 0.28655(8) 0.0453(4) Uani 1 1 d . . . . . C5 C 0.5916(2) 0.67414(13) 0.25193(10) 0.0598(5) Uani 1 1 d . . . . . H5A H 0.5721 0.6548 0.2033 0.090 Uiso 1 1 calc R U . . . H5B H 0.6707 0.7199 0.2668 0.090 Uiso 1 1 calc R U . . . H5C H 0.5309 0.6968 0.2631 0.090 Uiso 1 1 calc R U . . . C6 C 0.73420(15) 0.43436(12) 0.40546(7) 0.0450(4) Uani 1 1 d . . . . . C7 C 0.70017(17) 0.39259(13) 0.45752(8) 0.0514(4) Uani 1 1 d . . . . . C8 C 0.77282(19) 0.35031(14) 0.48889(9) 0.0615(5) Uani 1 1 d . . . . . H8 H 0.7512 0.3208 0.5238 0.074 Uiso 1 1 calc R U . . . C9 C 0.8753(2) 0.35024(16) 0.47058(10) 0.0667(6) Uani 1 1 d . . . . . H9 H 0.9243 0.3217 0.4933 0.080 Uiso 1 1 calc R U . . . C10 C 0.90722(18) 0.39123(15) 0.41951(10) 0.0617(5) Uani 1 1 d . . . . . H10 H 0.9785 0.3909 0.4075 0.074 Uiso 1 1 calc R U . . . C11 C 0.83698(16) 0.43320(13) 0.38510(8) 0.0501(4) Uani 1 1 d . . . . . C12 C 0.58809(18) 0.39337(14) 0.47921(9) 0.0565(5) Uani 1 1 d . . . . . H12 H 0.5609 0.4384 0.4588 0.068 Uiso 1 1 calc R U . . . C13 C 0.6116(3) 0.4173(2) 0.55550(11) 0.0860(8) Uani 1 1 d . . . . . H13A H 0.6345 0.3727 0.5767 0.129 Uiso 1 1 calc R U . . . H13B H 0.5385 0.4213 0.5667 0.129 Uiso 1 1 calc R U . . . H13C H 0.6766 0.4733 0.5719 0.129 Uiso 1 1 calc R U . . . C14 C 0.4874(2) 0.30597(16) 0.45183(11) 0.0701(6) Uani 1 1 d . . . . . H14A H 0.4702 0.2939 0.4027 0.105 Uiso 1 1 calc R U . . . H14B H 0.4151 0.3077 0.4651 0.105 Uiso 1 1 calc R U . . . H14C H 0.5124 0.2603 0.4701 0.105 Uiso 1 1 calc R U . . . C15 C 0.87254(17) 0.47722(14) 0.32803(9) 0.0558(5) Uani 1 1 d . . . . . H15 H 0.7990 0.4839 0.3002 0.067 Uiso 1 1 calc R U . . . C16 C 0.9659(3) 0.56715(16) 0.35302(12) 0.0818(7) Uani 1 1 d . . . . . H16A H 0.9339 0.6035 0.3788 0.123 Uiso 1 1 calc R U . . . H16B H 0.9858 0.5930 0.3146 0.123 Uiso 1 1 calc R U . . . H16C H 1.0384 0.5631 0.3818 0.123 Uiso 1 1 calc R U . . . C17 C 0.9173(2) 0.42382(16) 0.28232(11) 0.0726(6) Uani 1 1 d . . . . . H17A H 0.9948 0.4221 0.3066 0.109 Uiso 1 1 calc R U . . . H17B H 0.9269 0.4502 0.2427 0.109 Uiso 1 1 calc R U . . . H17C H 0.8591 0.3647 0.2682 0.109 Uiso 1 1 calc R U . . . C18 C 0.47340(14) 0.50103(11) 0.18434(7) 0.0404(3) Uani 1 1 d . . . . . C19 C 0.52239(15) 0.47123(11) 0.13492(8) 0.0435(4) Uani 1 1 d . . . . . C20 C 0.45567(17) 0.45144(12) 0.06818(8) 0.0514(4) Uani 1 1 d . . . . . H20 H 0.4868 0.4308 0.0340 0.062 Uiso 1 1 calc R U . . . C21 C 0.34481(18) 0.46151(13) 0.05118(9) 0.0563(5) Uani 1 1 d . . . . . H21 H 0.3007 0.4481 0.0055 0.068 Uiso 1 1 calc R U . . . C22 C 0.29836(17) 0.49083(13) 0.10026(9) 0.0537(4) Uani 1 1 d . . . . . H22 H 0.2224 0.4978 0.0879 0.064 Uiso 1 1 calc R U . . . C23 C 0.36092(16) 0.51057(12) 0.16798(8) 0.0466(4) Uani 1 1 d . . . . . C24 C 0.64647(16) 0.46414(12) 0.15364(8) 0.0486(4) Uani 1 1 d . . . . . H24 H 0.6557 0.4450 0.1981 0.058 Uiso 1 1 calc R U . . . C25 C 0.74470(18) 0.55188(14) 0.16313(10) 0.0616(5) Uani 1 1 d . . . . . H25A H 0.7356 0.5746 0.1213 0.092 Uiso 1 1 calc R U . . . H25B H 0.8235 0.5451 0.1751 0.092 Uiso 1 1 calc R U . . . H25C H 0.7382 0.5923 0.1991 0.092 Uiso 1 1 calc R U . . . C26 C 0.66495(18) 0.39681(14) 0.10434(9) 0.0573(5) Uani 1 1 d . . . . . H26A H 0.5982 0.3418 0.0963 0.086 Uiso 1 1 calc R U . . . H26B H 0.7406 0.3881 0.1233 0.086 Uiso 1 1 calc R U . . . H26C H 0.6679 0.4174 0.0618 0.086 Uiso 1 1 calc R U . . . C27 C 0.30322(18) 0.53834(15) 0.22088(10) 0.0592(5) Uani 1 1 d . . . . . H27 H 0.3650 0.5582 0.2649 0.071 Uiso 1 1 calc R U . . . C28 C 0.2607(3) 0.6135(2) 0.20530(14) 0.0923(9) Uani 1 1 d . . . . . H28A H 0.1973 0.5947 0.1633 0.138 Uiso 1 1 calc R U . . . H28B H 0.3282 0.6620 0.2007 0.138 Uiso 1 1 calc R U . . . H28C H 0.2291 0.6321 0.2419 0.138 Uiso 1 1 calc R U . . . C29 C 0.1987(2) 0.46176(19) 0.22777(14) 0.0840(7) Uani 1 1 d . . . . . H29A H 0.1630 0.4807 0.2622 0.126 Uiso 1 1 calc R U . . . H29B H 0.2281 0.4154 0.2408 0.126 Uiso 1 1 calc R U . . . H29C H 0.1379 0.4401 0.1847 0.126 Uiso 1 1 calc R U . . . C30 C 0.49951(15) 0.18083(11) 0.29255(8) 0.0460(4) Uani 1 1 d . . . . . C31 C 0.27925(18) 0.14995(15) 0.27129(11) 0.0649(5) Uani 1 1 d . . . . . H31A H 0.2951 0.2121 0.2725 0.097 Uiso 1 1 calc R U . . . H31B H 0.2194 0.1277 0.2963 0.097 Uiso 1 1 calc R U . . . H31C H 0.2488 0.1193 0.2246 0.097 Uiso 1 1 calc R U . . . C32 C 0.4001(2) 0.07886(14) 0.34495(11) 0.0660(5) Uani 1 1 d . . . . . C33 C 0.2924(3) 0.01963(19) 0.36214(16) 0.0975(9) Uani 1 1 d . . . . . H33A H 0.2529 0.0543 0.3836 0.146 Uiso 1 1 calc R U . . . H33B H 0.3180 -0.0159 0.3930 0.146 Uiso 1 1 calc R U . . . H33C H 0.2360 -0.0181 0.3210 0.146 Uiso 1 1 calc R U . . . C34 C 0.5173(2) 0.08773(15) 0.36352(11) 0.0673(6) Uani 1 1 d . . . . . C35 C 0.5820(3) 0.0441(2) 0.41038(16) 0.1062(10) Uani 1 1 d . . . . . H35A H 0.6282 0.0178 0.3870 0.159 Uiso 1 1 calc R U . . . H35B H 0.5234 -0.0009 0.4251 0.159 Uiso 1 1 calc R U . . . H35C H 0.6364 0.0871 0.4495 0.159 Uiso 1 1 calc R U . . . C36 C 0.70608(18) 0.17690(15) 0.33600(11) 0.0659(5) Uani 1 1 d . . . . . H36A H 0.7267 0.1268 0.3203 0.099 Uiso 1 1 calc R U . . . H36B H 0.7504 0.2011 0.3830 0.099 Uiso 1 1 calc R U . . . H36C H 0.7275 0.2211 0.3084 0.099 Uiso 1 1 calc R U . . . C37 C 0.42601(15) 0.21463(11) 0.14630(8) 0.0453(4) Uani 1 1 d . . . . . C38 C 0.26409(18) 0.27890(14) 0.13858(10) 0.0603(5) Uani 1 1 d . . . . . H38A H 0.1844 0.2418 0.1403 0.090 Uiso 1 1 calc R U . . . H38B H 0.2557 0.3209 0.1095 0.090 Uiso 1 1 calc R U . . . H38C H 0.3108 0.3099 0.1839 0.090 Uiso 1 1 calc R U . . . C39 C 0.28567(19) 0.17596(13) 0.04734(9) 0.0594(5) Uani 1 1 d . . . . . C40 C 0.1787(2) 0.17829(18) -0.00238(12) 0.0885(8) Uani 1 1 d . . . . . H40A H 0.1096 0.1650 0.0172 0.133 Uiso 1 1 calc R U . . . H40B H 0.1608 0.1353 -0.0430 0.133 Uiso 1 1 calc R U . . . H40C H 0.1956 0.2362 -0.0140 0.133 Uiso 1 1 calc R U . . . C41 C 0.3605(2) 0.13204(13) 0.04229(9) 0.0611(5) Uani 1 1 d . . . . . C42 C 0.3566(3) 0.06636(16) -0.01417(10) 0.0828(8) Uani 1 1 d . . . . . H42A H 0.3512 0.0116 0.0013 0.124 Uiso 1 1 calc R U . . . H42B H 0.4297 0.0871 -0.0298 0.124 Uiso 1 1 calc R U . . . H42C H 0.2863 0.0573 -0.0512 0.124 Uiso 1 1 calc R U . . . C43 C 0.5476(2) 0.12480(16) 0.11713(12) 0.0715(6) Uani 1 1 d . . . . . H43A H 0.5980 0.1424 0.0862 0.107 Uiso 1 1 calc R U . . . H43B H 0.5171 0.0614 0.1112 0.107 Uiso 1 1 calc R U . . . H43C H 0.5954 0.1493 0.1635 0.107 Uiso 1 1 calc R U . . . C44 C 0.89279(14) 0.05629(11) 0.25975(7) 0.0407(3) Uani 1 1 d . . . . . C45 C 0.97697(15) 0.11271(11) 0.31634(8) 0.0436(4) Uani 1 1 d . . . . . H45 H 0.9973 0.0899 0.3556 0.052 Uiso 1 1 calc R U . . . C46 C 1.03228(15) 0.20094(12) 0.31762(8) 0.0473(4) Uani 1 1 d . . . . . C47 C 1.00327(16) 0.23477(12) 0.26097(9) 0.0490(4) Uani 1 1 d . . . . . H47 H 1.0426 0.2943 0.2609 0.059 Uiso 1 1 calc R U . . . C48 C 0.91696(16) 0.18267(12) 0.20386(8) 0.0471(4) Uani 1 1 d . . . . . C49 C 0.86268(15) 0.09561(11) 0.20464(8) 0.0435(4) Uani 1 1 d . . . . . H49 H 0.8022 0.0607 0.1661 0.052 Uiso 1 1 calc R U . . . C50 C 1.1232(2) 0.25895(14) 0.38013(10) 0.0662(6) Uani 1 1 d . . . . . H50A H 1.0811 0.2751 0.4122 0.099 Uiso 1 1 calc R U . . . H50B H 1.1730 0.3114 0.3680 0.099 Uiso 1 1 calc R U . . . H50C H 1.1742 0.2279 0.4006 0.099 Uiso 1 1 calc R U . . . C51 C 0.8855(2) 0.22113(14) 0.14242(10) 0.0629(5) Uani 1 1 d . . . . . H51A H 0.8422 0.1744 0.1035 0.094 Uiso 1 1 calc R U . . . H51B H 0.9593 0.2587 0.1338 0.094 Uiso 1 1 calc R U . . . H51C H 0.8347 0.2552 0.1501 0.094 Uiso 1 1 calc R U . . . C52 C 0.93646(15) -0.08398(11) 0.21761(8) 0.0449(4) Uani 1 1 d . . . . . C53 C 0.99474(15) -0.04123(12) 0.17285(8) 0.0464(4) Uani 1 1 d . . . . . H53 H 0.9853 0.0121 0.1649 0.056 Uiso 1 1 calc R U . . . C54 C 1.06571(16) -0.07213(13) 0.13934(9) 0.0528(4) Uani 1 1 d . . . . . C55 C 1.08221(17) -0.14856(14) 0.15175(11) 0.0630(5) Uani 1 1 d . . . . . H55 H 1.1298 -0.1711 0.1291 0.076 Uiso 1 1 calc R U . . . C56 C 1.02948(19) -0.19269(14) 0.19725(13) 0.0660(6) Uani 1 1 d . . . . . C57 C 0.95677(17) -0.16094(13) 0.22780(11) 0.0573(5) Uani 1 1 d . . . . . H57 H 0.9186 -0.1931 0.2573 0.069 Uiso 1 1 calc R U . . . C58 C 1.1251(2) -0.02211(17) 0.09145(11) 0.0712(6) Uani 1 1 d . . . . . H58A H 1.2041 0.0192 0.1162 0.107 Uiso 1 1 calc R U . . . H58B H 1.0751 0.0093 0.0705 0.107 Uiso 1 1 calc R U . . . H58C H 1.1345 -0.0625 0.0566 0.107 Uiso 1 1 calc R U . . . C59 C 1.0542(3) -0.27328(18) 0.2145(2) 0.1060(11) Uani 1 1 d . . . . . H59A H 1.0234 -0.3187 0.1743 0.159 Uiso 1 1 calc R U . . . H59B H 1.0142 -0.2937 0.2492 0.159 Uiso 1 1 calc R U . . . H59C H 1.1409 -0.2596 0.2312 0.159 Uiso 1 1 calc R U . . . C60 C 0.84871(16) -0.07777(12) 0.32757(8) 0.0483(4) Uani 1 1 d . . . . . C61 C 0.95556(19) -0.07573(13) 0.37104(9) 0.0581(5) Uani 1 1 d . . . . . H61 H 1.0278 -0.0565 0.3571 0.070 Uiso 1 1 calc R U . . . C62 C 0.9612(2) -0.10063(14) 0.43397(10) 0.0671(6) Uani 1 1 d . . . . . C63 C 0.8572(3) -0.12734(14) 0.45471(10) 0.0710(6) Uani 1 1 d . . . . . H63 H 0.8596 -0.1443 0.4973 0.085 Uiso 1 1 calc R U . . . C64 C 0.7492(2) -0.12996(13) 0.41463(10) 0.0654(6) Uani 1 1 d . . . . . C65 C 0.74642(19) -0.10575(12) 0.35176(9) 0.0528(4) Uani 1 1 d . . . . . H65 H 0.6717 -0.1084 0.3243 0.063 Uiso 1 1 calc R U . . . C66 C 1.0793(3) -0.09909(18) 0.47771(12) 0.0913(9) Uani 1 1 d . . . . . H66A H 1.0865 -0.1565 0.4695 0.137 Uiso 1 1 calc R U . . . H66B H 1.0816 -0.0836 0.5251 0.137 Uiso 1 1 calc R U . . . H66C H 1.1460 -0.0562 0.4668 0.137 Uiso 1 1 calc R U . . . C67 C 0.6346(3) -0.16072(17) 0.43716(14) 0.0874(8) Uani 1 1 d . . . . . H67A H 0.6349 -0.1160 0.4723 0.131 Uiso 1 1 calc R U . . . H67B H 0.6292 -0.2141 0.4549 0.131 Uiso 1 1 calc R U . . . H67C H 0.5655 -0.1720 0.3989 0.131 Uiso 1 1 calc R U . . . C68 C 0.70803(15) -0.09249(11) 0.20542(8) 0.0441(4) Uani 1 1 d . . . . . C69 C 0.61982(16) -0.05702(12) 0.21312(9) 0.0508(4) Uani 1 1 d . . . . . H69 H 0.6437 -0.0036 0.2433 0.061 Uiso 1 1 calc R U . . . C70 C 0.49885(17) -0.09550(14) 0.17903(10) 0.0580(5) Uani 1 1 d . . . . . C71 C 0.46470(17) -0.17203(14) 0.13293(9) 0.0601(5) Uani 1 1 d . . . . . H71 H 0.3830 -0.1991 0.1088 0.072 Uiso 1 1 calc R U . . . C72 C 0.54802(18) -0.20897(12) 0.12190(8) 0.0555(5) Uani 1 1 d . . . . . C73 C 0.66807(16) -0.16913(12) 0.15826(8) 0.0483(4) Uani 1 1 d . . . . . H73 H 0.7247 -0.1953 0.1505 0.058 Uiso 1 1 calc R U . . . C74 C 0.4071(2) -0.05664(18) 0.19298(14) 0.0836(7) Uani 1 1 d . . . . . H74A H 0.3545 -0.0557 0.1504 0.125 Uiso 1 1 calc R U . . . H74B H 0.4482 0.0026 0.2183 0.125 Uiso 1 1 calc R U . . . H74C H 0.3590 -0.0917 0.2193 0.125 Uiso 1 1 calc R U . . . C75 C 0.5116(2) -0.29162(15) 0.07082(10) 0.0752(7) Uani 1 1 d . . . . . H75A H 0.5385 -0.3347 0.0923 0.113 Uiso 1 1 calc R U . . . H75B H 0.5488 -0.2791 0.0336 0.113 Uiso 1 1 calc R U . . . H75C H 0.4241 -0.3145 0.0536 0.113 Uiso 1 1 calc R U . . . B1 B 0.84581(17) -0.04903(13) 0.25309(9) 0.0432(4) Uani 1 1 d . . . . . C76 C 0.9842(4) 0.4693(4) 0.0032(3) 0.0829(15) Uani 0.5 1 d D U P A -1 C77 C 0.9505(7) 0.5203(5) 0.0477(4) 0.082(2) Uani 0.5 1 d D U P A -1 H77 H 0.9084 0.4944 0.0783 0.099 Uiso 0.5 1 calc R U P A -1 C78 C 0.9770(5) 0.6067(5) 0.0479(3) 0.0932(16) Uani 0.5 1 d D U P A -1 H78 H 0.9559 0.6409 0.0798 0.112 Uiso 0.5 1 calc R U P A -1 C79 C 1.0335(15) 0.6443(8) 0.0029(7) 0.100(3) Uani 0.5 1 d D U P A -1 H79 H 1.0486 0.7040 0.0015 0.120 Uiso 0.5 1 calc R U P A -1 C80 C 1.0686(6) 0.5944(5) -0.0409(3) 0.0987(19) Uani 0.5 1 d D U P A -1 H80 H 1.1122 0.6210 -0.0707 0.118 Uiso 0.5 1 calc R U P A -1 C81 C 1.0423(9) 0.5090(6) -0.0422(5) 0.083(2) Uani 0.5 1 d D U P A -1 H81 H 1.0636 0.4754 -0.0744 0.099 Uiso 0.5 1 calc R U P A -1 C82 C 0.9523(16) 0.3741(8) 0.0002(8) 0.125(5) Uani 0.5 1 d D U P A -1 H82A H 0.9569 0.3613 0.0456 0.188 Uiso 0.5 1 calc R U P A -1 H82B H 1.0086 0.3541 -0.0190 0.188 Uiso 0.5 1 calc R U P A -1 H82C H 0.8705 0.3444 -0.0279 0.188 Uiso 0.5 1 calc R U P A -1 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 0.0432(2) 0.0375(3) 0.0338(2) 0.00408(17) 0.00713(17) 0.01335(19) Al2 0.0464(3) 0.0392(3) 0.0412(2) 0.00239(19) 0.00657(18) 0.0146(2) N1 0.0482(7) 0.0405(8) 0.0332(6) 0.0014(5) 0.0071(5) 0.0150(6) N2 0.0447(7) 0.0383(8) 0.0347(6) 0.0042(5) 0.0082(5) 0.0148(5) N3 0.0596(9) 0.0480(10) 0.0534(8) 0.0050(7) 0.0160(7) 0.0181(7) N4 0.0646(9) 0.0501(10) 0.0517(8) 0.0077(7) 0.0092(7) 0.0273(8) N5 0.0579(8) 0.0411(9) 0.0462(7) 0.0063(6) 0.0020(6) 0.0101(7) N6 0.0706(10) 0.0414(9) 0.0455(7) 0.0025(6) 0.0155(7) 0.0129(7) C1 0.0742(12) 0.0520(12) 0.0423(9) -0.0074(8) 0.0001(8) 0.0168(9) C2 0.0517(9) 0.0464(11) 0.0370(7) -0.0040(7) 0.0070(6) 0.0143(7) C3 0.0615(10) 0.0375(11) 0.0441(8) -0.0026(7) 0.0080(7) 0.0150(8) C4 0.0540(9) 0.0373(10) 0.0439(8) 0.0046(7) 0.0125(7) 0.0155(7) C5 0.0770(13) 0.0397(11) 0.0561(10) 0.0079(8) 0.0077(9) 0.0175(9) C6 0.0485(8) 0.0450(10) 0.0352(7) -0.0005(6) 0.0013(6) 0.0159(7) C7 0.0582(10) 0.0535(12) 0.0376(8) 0.0056(7) 0.0040(7) 0.0185(8) C8 0.0699(12) 0.0645(14) 0.0465(9) 0.0135(8) 0.0025(8) 0.0251(10) C9 0.0663(12) 0.0754(16) 0.0570(11) 0.0108(10) -0.0031(9) 0.0352(11) C10 0.0528(10) 0.0751(15) 0.0535(10) 0.0033(9) 0.0011(8) 0.0277(10) C11 0.0496(9) 0.0527(12) 0.0409(8) -0.0013(7) 0.0016(7) 0.0173(8) C12 0.0675(11) 0.0635(13) 0.0435(9) 0.0155(8) 0.0175(8) 0.0252(9) C13 0.1004(18) 0.116(2) 0.0467(11) 0.0097(12) 0.0234(11) 0.0436(16) C14 0.0697(13) 0.0767(16) 0.0643(12) 0.0228(11) 0.0231(10) 0.0186(11) C15 0.0504(9) 0.0712(14) 0.0436(8) 0.0047(8) 0.0089(7) 0.0219(9) C16 0.1037(19) 0.0668(16) 0.0612(12) 0.0071(11) 0.0248(12) 0.0097(13) C17 0.0595(11) 0.0814(17) 0.0691(13) -0.0063(11) 0.0254(10) 0.0139(11) C18 0.0494(8) 0.0346(9) 0.0345(7) 0.0081(6) 0.0065(6) 0.0131(7) C19 0.0513(9) 0.0385(10) 0.0378(7) 0.0076(6) 0.0097(6) 0.0121(7) C20 0.0609(10) 0.0504(12) 0.0374(8) 0.0076(7) 0.0081(7) 0.0146(8) C21 0.0629(11) 0.0541(12) 0.0413(8) 0.0116(7) 0.0001(7) 0.0133(9) C22 0.0519(9) 0.0511(12) 0.0544(10) 0.0168(8) 0.0018(7) 0.0182(8) C23 0.0519(9) 0.0407(10) 0.0482(8) 0.0124(7) 0.0095(7) 0.0181(7) C24 0.0527(9) 0.0556(12) 0.0376(8) 0.0063(7) 0.0124(7) 0.0188(8) C25 0.0538(10) 0.0686(14) 0.0560(10) 0.0028(9) 0.0173(8) 0.0132(9) C26 0.0662(11) 0.0677(14) 0.0441(9) 0.0083(8) 0.0192(8) 0.0287(10) C27 0.0580(10) 0.0673(14) 0.0628(11) 0.0126(9) 0.0153(8) 0.0357(10) C28 0.114(2) 0.102(2) 0.0869(17) 0.0141(15) 0.0169(15) 0.0800(19) C29 0.0569(12) 0.110(2) 0.0898(17) 0.0213(15) 0.0324(12) 0.0257(13) C30 0.0522(9) 0.0389(10) 0.0450(8) 0.0014(7) 0.0083(7) 0.0178(7) C31 0.0528(10) 0.0715(15) 0.0662(12) 0.0060(10) 0.0152(9) 0.0176(9) C32 0.0899(15) 0.0478(13) 0.0685(12) 0.0173(9) 0.0320(11) 0.0251(11) C33 0.116(2) 0.080(2) 0.112(2) 0.0407(17) 0.0617(19) 0.0271(17) C34 0.0942(16) 0.0573(14) 0.0635(12) 0.0216(10) 0.0237(11) 0.0383(12) C35 0.146(3) 0.110(3) 0.100(2) 0.0574(19) 0.039(2) 0.079(2) C36 0.0596(11) 0.0682(15) 0.0682(12) 0.0044(10) 0.0016(9) 0.0319(10) C37 0.0543(9) 0.0354(10) 0.0406(8) 0.0036(6) 0.0074(7) 0.0119(7) C38 0.0551(10) 0.0514(13) 0.0656(11) 0.0079(9) -0.0004(8) 0.0174(9) C39 0.0711(12) 0.0464(12) 0.0409(9) 0.0076(7) 0.0001(8) 0.0024(9) C40 0.0925(17) 0.0851(19) 0.0572(12) 0.0128(12) -0.0156(12) 0.0110(14) C41 0.0847(14) 0.0446(12) 0.0396(8) 0.0044(7) 0.0130(8) 0.0051(10) C42 0.128(2) 0.0581(15) 0.0451(10) -0.0026(9) 0.0235(12) 0.0105(14) C43 0.0841(15) 0.0608(15) 0.0743(13) 0.0004(11) 0.0270(11) 0.0309(12) C44 0.0438(8) 0.0390(10) 0.0380(7) 0.0065(6) 0.0080(6) 0.0142(7) C45 0.0494(8) 0.0412(10) 0.0373(7) 0.0048(6) 0.0047(6) 0.0165(7) C46 0.0492(9) 0.0393(10) 0.0477(8) 0.0016(7) 0.0042(7) 0.0146(7) C47 0.0527(9) 0.0334(10) 0.0569(9) 0.0075(7) 0.0088(7) 0.0127(7) C48 0.0534(9) 0.0424(11) 0.0471(8) 0.0123(7) 0.0093(7) 0.0195(8) C49 0.0469(8) 0.0405(10) 0.0389(7) 0.0064(6) 0.0045(6) 0.0138(7) C50 0.0718(13) 0.0480(13) 0.0588(11) -0.0032(9) -0.0064(9) 0.0124(10) C51 0.0707(12) 0.0542(13) 0.0604(11) 0.0233(9) 0.0066(9) 0.0193(10) C52 0.0469(8) 0.0367(10) 0.0449(8) 0.0053(6) 0.0033(6) 0.0117(7) C53 0.0496(9) 0.0430(10) 0.0433(8) 0.0061(7) 0.0063(7) 0.0157(7) C54 0.0459(9) 0.0548(12) 0.0515(9) 0.0028(8) 0.0078(7) 0.0138(8) C55 0.0469(9) 0.0565(14) 0.0816(13) -0.0024(10) 0.0149(9) 0.0184(9) C56 0.0557(11) 0.0443(13) 0.0993(16) 0.0104(11) 0.0185(10) 0.0204(9) C57 0.0569(10) 0.0428(12) 0.0737(12) 0.0166(9) 0.0164(9) 0.0174(8) C58 0.0671(12) 0.0897(18) 0.0645(12) 0.0169(11) 0.0282(10) 0.0292(12) C59 0.093(2) 0.0620(18) 0.186(4) 0.039(2) 0.052(2) 0.0432(15) C60 0.0618(10) 0.0362(10) 0.0415(8) 0.0077(6) 0.0074(7) 0.0129(8) C61 0.0679(11) 0.0507(12) 0.0483(9) 0.0161(8) 0.0032(8) 0.0158(9) C62 0.0967(16) 0.0493(13) 0.0460(9) 0.0147(8) 0.0008(10) 0.0219(11) C63 0.122(2) 0.0491(13) 0.0443(9) 0.0182(8) 0.0185(11) 0.0305(12) C64 0.1063(17) 0.0396(12) 0.0553(10) 0.0135(8) 0.0343(11) 0.0219(11) C65 0.0725(11) 0.0389(11) 0.0464(9) 0.0085(7) 0.0180(8) 0.0160(8) C66 0.121(2) 0.0778(18) 0.0618(13) 0.0246(12) -0.0132(13) 0.0361(16) C67 0.137(2) 0.0688(17) 0.0877(16) 0.0365(13) 0.0710(17) 0.0429(16) C68 0.0519(9) 0.0390(10) 0.0379(7) 0.0092(6) 0.0095(6) 0.0113(7) C69 0.0497(9) 0.0451(11) 0.0482(9) 0.0018(7) 0.0055(7) 0.0101(7) C70 0.0479(9) 0.0584(13) 0.0580(10) 0.0099(9) 0.0049(8) 0.0107(8) C71 0.0521(10) 0.0581(13) 0.0519(10) 0.0098(8) 0.0002(8) 0.0027(9) C72 0.0689(11) 0.0416(11) 0.0394(8) 0.0058(7) 0.0042(7) 0.0031(8) C73 0.0603(10) 0.0420(10) 0.0375(7) 0.0080(6) 0.0090(7) 0.0125(8) C74 0.0510(11) 0.0884(19) 0.1007(18) 0.0025(14) 0.0086(11) 0.0208(11) C75 0.0941(16) 0.0526(14) 0.0517(11) -0.0045(9) 0.0018(10) 0.0034(11) B1 0.0499(10) 0.0374(11) 0.0390(8) 0.0075(7) 0.0070(7) 0.0133(8) C76 0.059(3) 0.129(5) 0.063(2) 0.044(3) 0.014(2) 0.028(3) C77 0.057(3) 0.138(5) 0.053(3) 0.033(4) 0.018(2) 0.029(4) C78 0.069(3) 0.135(5) 0.070(3) 0.009(3) 0.012(2) 0.034(3) C79 0.080(5) 0.126(6) 0.113(5) 0.048(5) 0.038(4) 0.045(5) C80 0.091(4) 0.140(5) 0.105(4) 0.065(4) 0.054(3) 0.063(4) C81 0.072(4) 0.143(5) 0.066(4) 0.052(4) 0.032(3) 0.061(4) C82 0.102(10) 0.127(6) 0.131(9) 0.040(6) 0.001(6) 0.030(5) 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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 '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' 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 Al2 Al1 H 116.6(8) . . ? N1 Al1 H 109.2(8) . . ? N1 Al1 Al2 111.10(6) . . ? N1 Al1 N2 93.98(7) . . ? N2 Al1 H 104.8(8) . . ? N2 Al1 Al2 118.66(5) . . ? Al1 Al2 HA 115.3(7) . . ? C30 Al2 Al1 111.33(5) . . ? C30 Al2 HA 104.9(7) . . ? C30 Al2 C37 100.14(8) . . ? C37 Al2 Al1 121.31(6) . . ? C37 Al2 HA 101.6(7) . . ? C2 N1 Al1 120.95(12) . . ? C2 N1 C6 117.78(14) . . ? C6 N1 Al1 121.23(11) . . ? C4 N2 Al1 122.18(11) . . ? C4 N2 C18 119.16(14) . . ? C18 N2 Al1 117.83(11) . . ? C30 N3 C31 123.38(17) . . ? C30 N3 C32 111.63(17) . . ? C32 N3 C31 124.97(18) . . ? C30 N4 C34 111.36(17) . . ? C30 N4 C36 124.60(17) . . ? C34 N4 C36 124.04(18) . . ? C37 N5 C38 125.16(15) . . ? C37 N5 C39 110.71(17) . . ? C39 N5 C38 124.08(17) . . ? C37 N6 C41 111.55(18) . . ? C37 N6 C43 124.97(16) . . ? C41 N6 C43 123.48(17) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 119.62(17) . . ? N1 C2 C3 123.16(15) . . ? C3 C2 C1 117.23(17) . . ? C2 C3 H3 114.9(12) . . ? C2 C3 C4 127.10(17) . . ? C4 C3 H3 117.6(12) . . ? N2 C4 C3 122.32(17) . . ? N2 C4 C5 121.43(15) . . ? C3 C4 C5 116.23(16) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 N1 120.16(16) . . ? C11 C6 N1 118.14(16) . . ? C11 C6 C7 121.70(17) . . ? C6 C7 C12 121.62(17) . . ? C8 C7 C6 117.59(18) . . ? C8 C7 C12 120.79(18) . . ? C7 C8 H8 119.3 . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8 119.3 . . ? C8 C9 H9 119.9 . . ? C10 C9 C8 120.3(2) . . ? C10 C9 H9 119.9 . . ? C9 C10 H10 119.4 . . ? C9 C10 C11 121.2(2) . . ? C11 C10 H10 119.4 . . ? C6 C11 C15 121.61(17) . . ? C10 C11 C6 117.84(18) . . ? C10 C11 C15 120.54(17) . . ? C7 C12 H12 107.6 . . ? C7 C12 C13 112.61(18) . . ? C7 C12 C14 110.15(17) . . ? C13 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C14 C12 C13 110.93(19) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15 107.4 . . ? C16 C15 C11 112.38(16) . . ? C16 C15 H15 107.4 . . ? C16 C15 C17 109.36(18) . . ? C17 C15 C11 112.66(19) . . ? C17 C15 H15 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N2 118.40(14) . . ? C23 C18 N2 119.88(14) . . ? C23 C18 C19 121.64(15) . . ? C18 C19 C24 120.69(14) . . ? C20 C19 C18 118.10(16) . . ? C20 C19 C24 121.17(16) . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.88(17) . . ? C21 C20 H20 119.6 . . ? C20 C21 H21 119.9 . . ? C22 C21 C20 120.18(16) . . ? C22 C21 H21 119.9 . . ? C21 C22 H22 119.4 . . ? C21 C22 C23 121.21(18) . . ? C23 C22 H22 119.4 . . ? C18 C23 C22 117.98(17) . . ? C18 C23 C27 122.60(15) . . ? C22 C23 C27 119.39(17) . . ? C19 C24 H24 106.9 . . ? C19 C24 C25 111.47(16) . . ? C19 C24 C26 113.80(15) . . ? C25 C24 H24 106.9 . . ? C25 C24 C26 110.32(15) . . ? C26 C24 H24 106.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27 108.0 . . ? C23 C27 C28 111.89(19) . . ? C23 C27 C29 110.59(19) . . ? C28 C27 H27 108.0 . . ? C28 C27 C29 110.2(2) . . ? C29 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 Al2 127.47(14) . . ? N4 C30 Al2 128.59(14) . . ? N4 C30 N3 103.81(16) . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 122.3(2) . . ? C34 C32 N3 106.52(19) . . ? C34 C32 C33 131.2(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C35 122.3(2) . . ? C32 C34 N4 106.66(19) . . ? C32 C34 C35 131.0(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 Al2 129.79(13) . . ? N5 C37 N6 104.29(15) . . ? N6 C37 Al2 125.63(13) . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 C40 121.9(2) . . ? C41 C39 N5 107.03(17) . . ? C41 C39 C40 131.1(2) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 C42 123.7(2) . . ? C39 C41 N6 106.41(17) . . ? C39 C41 C42 129.9(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C43 H43A 109.5 . . ? N6 C43 H43B 109.5 . . ? N6 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 115.24(15) . . ? C45 C44 B1 123.04(15) . . ? C49 C44 B1 121.20(14) . . ? C44 C45 H45 118.5 . . ? C46 C45 C44 122.91(16) . . ? C46 C45 H45 118.5 . . ? C45 C46 C50 120.70(17) . . ? C47 C46 C45 119.06(16) . . ? C47 C46 C50 120.24(17) . . ? C46 C47 H47 119.6 . . ? C46 C47 C48 120.80(17) . . ? C48 C47 H47 119.6 . . ? C47 C48 C51 120.03(17) . . ? C49 C48 C47 118.59(16) . . ? C49 C48 C51 121.38(16) . . ? C44 C49 H49 118.4 . . ? C48 C49 C44 123.28(15) . . ? C48 C49 H49 118.4 . . ? C46 C50 H50A 109.5 . . ? C46 C50 H50B 109.5 . . ? C46 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 B1 122.91(16) . . ? C57 C52 C53 114.68(17) . . ? C57 C52 B1 122.35(16) . . ? C52 C53 H53 118.0 . . ? C54 C53 C52 123.91(18) . . ? C54 C53 H53 118.0 . . ? C53 C54 C58 120.57(19) . . ? C55 C54 C53 118.46(18) . . ? C55 C54 C58 120.97(19) . . ? C54 C55 H55 119.9 . . ? C54 C55 C56 120.29(19) . . ? C56 C55 H55 119.9 . . ? C55 C56 C59 120.4(2) . . ? C57 C56 C55 119.2(2) . . ? C57 C56 C59 120.4(2) . . ? C52 C57 H57 118.3 . . ? C56 C57 C52 123.4(2) . . ? C56 C57 H57 118.3 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 B1 121.81(17) . . ? C65 C60 C61 115.10(17) . . ? C65 C60 B1 123.10(16) . . ? C60 C61 H61 118.3 . . ? C62 C61 C60 123.4(2) . . ? C62 C61 H61 118.3 . . ? C61 C62 C66 120.7(2) . . ? C63 C62 C61 118.5(2) . . ? C63 C62 C66 120.9(2) . . ? C62 C63 H63 119.5 . . ? C62 C63 C64 121.03(18) . . ? C64 C63 H63 119.5 . . ? C63 C64 C65 119.1(2) . . ? C63 C64 C67 120.9(2) . . ? C65 C64 C67 120.0(2) . . ? C60 C65 C64 122.9(2) . . ? C60 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C62 C66 H66A 109.5 . . ? C62 C66 H66B 109.5 . . ? C62 C66 H66C 109.5 . . ? H66A C66 H66B 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67B 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 B1 121.03(15) . . ? C73 C68 C69 115.26(16) . . ? C73 C68 B1 123.57(17) . . ? C68 C69 H69 118.1 . . ? C70 C69 C68 123.83(18) . . ? C70 C69 H69 118.1 . . ? C69 C70 C74 121.06(19) . . ? C71 C70 C69 118.1(2) . . ? C71 C70 C74 120.86(18) . . ? C70 C71 H71 119.6 . . ? C72 C71 C70 120.79(18) . . ? C72 C71 H71 119.6 . . ? C71 C72 C73 119.25(18) . . ? C71 C72 C75 121.01(19) . . ? C73 C72 C75 119.7(2) . . ? C68 C73 C72 122.77(19) . . ? C68 C73 H73 118.6 . . ? C72 C73 H73 118.6 . . ? C70 C74 H74A 109.5 . . ? C70 C74 H74B 109.5 . . ? C70 C74 H74C 109.5 . . ? H74A C74 H74B 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75B 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C44 B1 C52 106.71(14) . . ? C44 B1 C60 111.40(14) . . ? C44 B1 C68 110.62(15) . . ? C52 B1 C60 110.14(15) . . ? C68 B1 C52 109.33(13) . . ? C68 B1 C60 108.62(14) . . ? C77 C76 C82 121.9(7) . . ? C81 C76 C77 117.8(6) . . ? C81 C76 C82 120.1(7) . . ? C76 C77 H77 119.5 . . ? C78 C77 C76 120.9(6) . . ? C78 C77 H77 119.5 . . ? C77 C78 H78 119.8 . . ? C79 C78 C77 120.4(7) . . ? C79 C78 H78 119.8 . . ? C78 C79 H79 120.5 . . ? C78 C79 C80 119.0(8) . . ? C80 C79 H79 120.5 . . ? C79 C80 H80 119.4 . . ? C81 C80 C79 121.3(7) . . ? C81 C80 H80 119.4 . . ? C76 C81 H81 119.8 . . ? C80 C81 C76 120.4(7) . . ? C80 C81 H81 119.8 . . ? C76 C82 H82A 109.5 . . ? C76 C82 H82B 109.5 . . ? C76 C82 H82C 109.5 . . ? H82A C82 H82B 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? 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 H 1.54(2) . ? Al1 Al2 2.6194(10) . ? Al1 N1 1.9147(16) . ? Al1 N2 1.9330(15) . ? Al2 HA 1.52(2) . ? Al2 C30 2.035(2) . ? Al2 C37 2.0534(19) . ? N1 C2 1.339(2) . ? N1 C6 1.444(2) . ? N2 C4 1.333(2) . ? N2 C18 1.4462(19) . ? N3 C30 1.360(2) . ? N3 C31 1.468(3) . ? N3 C32 1.379(3) . ? N4 C30 1.357(2) . ? N4 C34 1.384(3) . ? N4 C36 1.470(3) . ? N5 C37 1.351(2) . ? N5 C38 1.457(3) . ? N5 C39 1.393(2) . ? N6 C37 1.357(2) . ? N6 C41 1.381(3) . ? N6 C43 1.471(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.514(2) . ? C2 C3 1.382(3) . ? C3 H3 0.93(2) . ? C3 C4 1.407(2) . ? C4 C5 1.499(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.405(2) . ? C6 C11 1.402(2) . ? C7 C8 1.389(3) . ? C7 C12 1.521(3) . ? C8 H8 0.9500 . ? C8 C9 1.374(3) . ? C9 H9 0.9500 . ? C9 C10 1.373(3) . ? C10 H10 0.9500 . ? C10 C11 1.391(3) . ? C11 C15 1.520(3) . ? C12 H12 1.0000 . ? C12 C13 1.532(3) . ? C12 C14 1.528(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 1.0000 . ? C15 C16 1.517(3) . ? C15 C17 1.519(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.405(2) . ? C18 C23 1.398(2) . ? C19 C20 1.395(2) . ? C19 C24 1.519(2) . ? C20 H20 0.9500 . ? C20 C21 1.384(3) . ? C21 H21 0.9500 . ? C21 C22 1.375(3) . ? C22 H22 0.9500 . ? C22 C23 1.398(2) . ? C23 C27 1.522(3) . ? C24 H24 1.0000 . ? C24 C25 1.524(3) . ? C24 C26 1.531(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27 1.0000 . ? C27 C28 1.526(3) . ? C27 C29 1.530(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.503(3) . ? C32 C34 1.349(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.503(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.493(3) . ? C39 C41 1.341(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.492(3) . ? 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 1.401(2) . ? C44 C49 1.410(2) . ? C44 B1 1.634(3) . ? C45 H45 0.9500 . ? C45 C46 1.396(3) . ? C46 C47 1.379(3) . ? C46 C50 1.515(2) . ? C47 H47 0.9500 . ? C47 C48 1.394(2) . ? C48 C49 1.386(3) . ? C48 C51 1.513(2) . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.399(2) . ? C52 C57 1.397(3) . ? C52 B1 1.651(3) . ? C53 H53 0.9500 . ? C53 C54 1.390(3) . ? C54 C55 1.380(3) . ? C54 C58 1.512(3) . ? C55 H55 0.9500 . ? C55 C56 1.391(3) . ? C56 C57 1.380(3) . ? C56 C59 1.515(3) . ? C57 H57 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.404(3) . ? C60 C65 1.398(3) . ? C60 B1 1.658(2) . ? C61 H61 0.9500 . ? C61 C62 1.403(3) . ? C62 C63 1.374(4) . ? C62 C66 1.518(3) . ? C63 H63 0.9500 . ? C63 C64 1.383(3) . ? C64 C65 1.399(3) . ? C64 C67 1.512(3) . ? C65 H65 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.399(3) . ? C68 C73 1.397(2) . ? C68 B1 1.642(2) . ? C69 H69 0.9500 . ? C69 C70 1.395(2) . ? C70 C71 1.391(3) . ? C70 C74 1.509(3) . ? C71 H71 0.9500 . ? C71 C72 1.378(3) . ? C72 C73 1.400(3) . ? C72 C75 1.518(3) . ? C73 H73 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.390(8) . ? C76 C81 1.389(8) . ? C76 C82 1.489(11) . ? C77 H77 0.9500 . ? C77 C78 1.361(8) . ? C78 H78 0.9500 . ? C78 C79 1.360(9) . ? C79 H79 0.9500 . ? C79 C80 1.381(9) . ? C80 H80 0.9500 . ? C80 C81 1.342(8) . ? C81 H81 0.9500 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? 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 Al1 N1 C2 C1 159.97(14) . . . . ? Al1 N1 C2 C3 -20.2(2) . . . . ? Al1 N1 C6 C7 -82.66(17) . . . . ? Al1 N1 C6 C11 97.30(17) . . . . ? Al1 N2 C4 C3 9.8(2) . . . . ? Al1 N2 C4 C5 -171.88(14) . . . . ? Al1 N2 C18 C19 -82.19(17) . . . . ? Al1 N2 C18 C23 94.52(17) . . . . ? N1 C2 C3 C4 -8.7(3) . . . . ? N1 C6 C7 C8 -179.51(16) . . . . ? N1 C6 C7 C12 0.4(3) . . . . ? N1 C6 C11 C10 178.21(16) . . . . ? N1 C6 C11 C15 -0.9(2) . . . . ? N2 C18 C19 C20 176.93(15) . . . . ? N2 C18 C19 C24 -5.3(2) . . . . ? N2 C18 C23 C22 -177.63(16) . . . . ? N2 C18 C23 C27 0.2(3) . . . . ? N3 C32 C34 N4 -0.8(2) . . . . ? N3 C32 C34 C35 178.6(3) . . . . ? N5 C39 C41 N6 -1.2(2) . . . . ? N5 C39 C41 C42 176.7(2) . . . . ? C1 C2 C3 C4 171.10(19) . . . . ? C2 N1 C6 C7 95.33(19) . . . . ? C2 N1 C6 C11 -84.71(19) . . . . ? C2 C3 C4 N2 14.5(3) . . . . ? C2 C3 C4 C5 -163.96(19) . . . . ? C4 N2 C18 C19 108.01(18) . . . . ? C4 N2 C18 C23 -75.3(2) . . . . ? C6 N1 C2 C1 -18.0(2) . . . . ? C6 N1 C2 C3 161.77(17) . . . . ? C6 C7 C8 C9 1.0(3) . . . . ? C6 C7 C12 C13 -132.1(2) . . . . ? C6 C7 C12 C14 103.5(2) . . . . ? C6 C11 C15 C16 96.9(2) . . . . ? C6 C11 C15 C17 -138.99(18) . . . . ? C7 C6 C11 C10 -1.8(3) . . . . ? C7 C6 C11 C15 179.01(16) . . . . ? C7 C8 C9 C10 -1.1(3) . . . . ? C8 C7 C12 C13 47.8(3) . . . . ? C8 C7 C12 C14 -76.6(2) . . . . ? C8 C9 C10 C11 -0.3(3) . . . . ? C9 C10 C11 C6 1.7(3) . . . . ? C9 C10 C11 C15 -179.15(19) . . . . ? C10 C11 C15 C16 -82.2(2) . . . . ? C10 C11 C15 C17 41.9(2) . . . . ? C11 C6 C7 C8 0.5(3) . . . . ? C11 C6 C7 C12 -179.56(17) . . . . ? C12 C7 C8 C9 -178.9(2) . . . . ? C18 N2 C4 C3 179.11(16) . . . . ? C18 N2 C4 C5 -2.5(2) . . . . ? C18 C19 C20 C21 0.5(3) . . . . ? C18 C19 C24 C25 -80.0(2) . . . . ? C18 C19 C24 C26 154.41(16) . . . . ? C18 C23 C27 C28 129.3(2) . . . . ? C18 C23 C27 C29 -107.4(2) . . . . ? C19 C18 C23 C22 -1.0(3) . . . . ? C19 C18 C23 C27 176.82(17) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? C20 C19 C24 C25 97.6(2) . . . . ? C20 C19 C24 C26 -27.9(2) . . . . ? C20 C21 C22 C23 -0.4(3) . . . . ? C21 C22 C23 C18 1.1(3) . . . . ? C21 C22 C23 C27 -176.85(19) . . . . ? C22 C23 C27 C28 -52.8(3) . . . . ? C22 C23 C27 C29 70.4(2) . . . . ? C23 C18 C19 C20 0.3(3) . . . . ? C23 C18 C19 C24 178.02(16) . . . . ? C24 C19 C20 C21 -177.26(18) . . . . ? C30 N3 C32 C33 -178.2(2) . . . . ? C30 N3 C32 C34 0.3(2) . . . . ? C30 N4 C34 C32 1.0(2) . . . . ? C30 N4 C34 C35 -178.5(2) . . . . ? C31 N3 C30 Al2 2.5(2) . . . . ? C31 N3 C30 N4 178.59(16) . . . . ? C31 N3 C32 C33 3.6(3) . . . . ? C31 N3 C32 C34 -177.96(19) . . . . ? C32 N3 C30 Al2 -175.84(14) . . . . ? C32 N3 C30 N4 0.3(2) . . . . ? C33 C32 C34 N4 177.5(3) . . . . ? C33 C32 C34 C35 -3.1(5) . . . . ? C34 N4 C30 Al2 175.28(14) . . . . ? C34 N4 C30 N3 -0.8(2) . . . . ? C36 N4 C30 Al2 -5.2(3) . . . . ? C36 N4 C30 N3 178.76(17) . . . . ? C36 N4 C34 C32 -178.53(19) . . . . ? C36 N4 C34 C35 2.0(3) . . . . ? C37 N5 C39 C40 -177.84(19) . . . . ? C37 N5 C39 C41 1.4(2) . . . . ? C37 N6 C41 C39 0.6(2) . . . . ? C37 N6 C41 C42 -177.40(19) . . . . ? C38 N5 C37 Al2 -9.4(3) . . . . ? C38 N5 C37 N6 176.56(17) . . . . ? C38 N5 C39 C40 4.6(3) . . . . ? C38 N5 C39 C41 -176.17(18) . . . . ? C39 N5 C37 Al2 173.07(14) . . . . ? C39 N5 C37 N6 -0.9(2) . . . . ? C40 C39 C41 N6 177.9(2) . . . . ? C40 C39 C41 C42 -4.2(4) . . . . ? C41 N6 C37 Al2 -174.14(13) . . . . ? C41 N6 C37 N5 0.2(2) . . . . ? C43 N6 C37 Al2 4.6(3) . . . . ? C43 N6 C37 N5 178.91(18) . . . . ? C43 N6 C41 C39 -178.10(19) . . . . ? C43 N6 C41 C42 3.9(3) . . . . ? C44 C45 C46 C47 0.1(3) . . . . ? C44 C45 C46 C50 -179.72(17) . . . . ? C45 C44 C49 C48 4.0(2) . . . . ? C45 C44 B1 C52 -90.59(18) . . . . ? C45 C44 B1 C60 29.7(2) . . . . ? C45 C44 B1 C68 150.58(15) . . . . ? C45 C46 C47 C48 2.2(3) . . . . ? C46 C47 C48 C49 -1.4(3) . . . . ? C46 C47 C48 C51 179.44(18) . . . . ? C47 C48 C49 C44 -1.9(3) . . . . ? C49 C44 C45 C46 -3.1(2) . . . . ? C49 C44 B1 C52 80.74(18) . . . . ? C49 C44 B1 C60 -159.01(15) . . . . ? C49 C44 B1 C68 -38.1(2) . . . . ? C50 C46 C47 C48 -177.93(18) . . . . ? C51 C48 C49 C44 177.29(17) . . . . ? C52 C53 C54 C55 -1.4(3) . . . . ? C52 C53 C54 C58 179.66(17) . . . . ? C53 C52 C57 C56 0.8(3) . . . . ? C53 C52 B1 C44 -29.5(2) . . . . ? C53 C52 B1 C60 -150.51(15) . . . . ? C53 C52 B1 C68 90.22(19) . . . . ? C53 C54 C55 C56 -0.5(3) . . . . ? C54 C55 C56 C57 2.5(3) . . . . ? C54 C55 C56 C59 -175.9(2) . . . . ? C55 C56 C57 C52 -2.7(3) . . . . ? C57 C52 C53 C54 1.3(2) . . . . ? C57 C52 B1 C44 153.42(16) . . . . ? C57 C52 B1 C60 32.4(2) . . . . ? C57 C52 B1 C68 -86.9(2) . . . . ? C58 C54 C55 C56 178.35(19) . . . . ? C59 C56 C57 C52 175.7(2) . . . . ? C60 C61 C62 C63 -0.9(3) . . . . ? C60 C61 C62 C66 178.4(2) . . . . ? C61 C60 C65 C64 0.1(3) . . . . ? C61 C60 B1 C44 -79.1(2) . . . . ? C61 C60 B1 C52 39.1(2) . . . . ? C61 C60 B1 C68 158.78(17) . . . . ? C61 C62 C63 C64 0.2(3) . . . . ? C62 C63 C64 C65 0.7(3) . . . . ? C62 C63 C64 C67 179.0(2) . . . . ? C63 C64 C65 C60 -0.8(3) . . . . ? C65 C60 C61 C62 0.8(3) . . . . ? C65 C60 B1 C44 101.0(2) . . . . ? C65 C60 B1 C52 -140.80(17) . . . . ? C65 C60 B1 C68 -21.1(2) . . . . ? C66 C62 C63 C64 -179.1(2) . . . . ? C67 C64 C65 C60 -179.2(2) . . . . ? C68 C69 C70 C71 -2.4(3) . . . . ? C68 C69 C70 C74 176.1(2) . . . . ? C69 C68 C73 C72 -1.1(3) . . . . ? C69 C68 B1 C44 -44.9(2) . . . . ? C69 C68 B1 C52 -162.13(15) . . . . ? C69 C68 B1 C60 77.7(2) . . . . ? C69 C70 C71 C72 0.6(3) . . . . ? C70 C71 C72 C73 0.7(3) . . . . ? C70 C71 C72 C75 -178.96(19) . . . . ? C71 C72 C73 C68 -0.4(3) . . . . ? C73 C68 C69 C70 2.5(3) . . . . ? C73 C68 B1 C44 139.52(16) . . . . ? C73 C68 B1 C52 22.3(2) . . . . ? C73 C68 B1 C60 -97.92(19) . . . . ? C74 C70 C71 C72 -177.8(2) . . . . ? C75 C72 C73 C68 179.22(17) . . . . ? B1 C44 C45 C46 168.74(16) . . . . ? B1 C44 C49 C48 -168.00(16) . . . . ? B1 C52 C53 C54 -176.02(15) . . . . ? B1 C52 C57 C56 178.14(18) . . . . ? B1 C60 C61 C62 -179.14(19) . . . . ? B1 C60 C65 C64 180.00(17) . . . . ? B1 C68 C69 C70 -173.38(17) . . . . ? B1 C68 C73 C72 174.70(16) . . . . ? C76 C77 C78 C79 2.3(13) . . . . ? C77 C76 C81 C80 2.5(14) . . . . ? C77 C78 C79 C80 -3.0(19) . . . . ? C78 C79 C80 C81 4(2) . . . . ? C79 C80 C81 C76 -3.4(16) . . . . ? C81 C76 C77 C78 -2.0(13) . . . . ? C82 C76 C77 C78 -177.7(10) . . . . ? C82 C76 C81 C80 178.3(10) . . . . ?