#------------------------------------------------------------------------------ #$Date: 2019-11-17 15:43:50 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230958 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/85/1548547.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_1548547 loop_ _publ_author_name 'Yu, Chao' 'Zhang, Pengfei' 'Gao, Fei' 'Zhang, Shaowen' 'Li, Xiaofang' _publ_section_title ; A displacement-type fluorescent probe reveals active species in the coordinative polymerization of olefins ; _journal_issue 5 _journal_name_full 'Polymer Chemistry' _journal_page_first 603 _journal_paper_doi 10.1039/C7PY01915G _journal_volume 9 _journal_year 2018 _chemical_formula_moiety 'C26 H35 Al N2' _chemical_formula_sum 'C26 H35 Al N2' _chemical_formula_weight 402.54 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-05-23 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324) ; _audit_update_record ; 2017-05-26 deposited with the CCDC. 2017-12-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.63(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.8769(16) _cell_length_b 28.840(6) _cell_length_c 10.921(2) _cell_measurement_reflns_used 8272 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 31.5074 _cell_measurement_theta_min 2.1185 _cell_volume 2377.2(9) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 153.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_unetI/netI 0.0490 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 23487 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.506 _diffrn_reflns_theta_min 2.790 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.125 _exptl_crystal_description block _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.344 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 7873 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0581 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.4018P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1509 _refine_ls_wR_factor_ref 0.1597 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6811 _reflns_number_total 7873 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7py01915g2.cif _cod_data_source_block bo4592 _cod_depositor_comments 'Adding full bibliography for 1548544--1548547.cif.' _cod_original_cell_volume 2377.1(9) _cod_database_code 1548547 _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 0.961 _shelx_estimated_absorpt_t_min 0.943 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C23(H23A,H23B), C25(H25A,H25B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C7(H7), C12(H12), C20(H20) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C24(H24A,H24B, H24C), C26(H26A,H26B,H26C) ; _shelx_res_file ; bo4592.res created by SHELXL-2014/7 TITL bo4592 in P2(1)/c CELL 0.71073 7.8769 28.8403 10.9206 90 106.633 90 ZERR 4 0.0016 0.0058 0.0022 0 0.03 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N Al UNIT 104 140 8 4 L.S. 4 PLAN 20 SIZE 0.6 0.43 0.4 TEMP -120 BOND fmap 2 ACTA BOND $H CONF OMIT 2 17 2 OMIT 0 7 4 OMIT 0 2 1 REM REM REM WGHT 0.070300 0.401800 FVAR 6.06196 AL1 4 0.528138 0.179497 0.650907 11.00000 0.03262 0.02760 = 0.02429 -0.00328 0.00704 -0.00332 N1 3 0.636102 0.171007 0.516260 11.00000 0.02715 0.02981 = 0.02929 -0.00397 0.00739 -0.00576 N2 3 0.348485 0.134136 0.587002 11.00000 0.02940 0.02904 = 0.02405 -0.00217 0.00937 -0.00252 C1 1 0.178057 0.013055 -0.089110 11.00000 0.05659 0.06775 = 0.03845 -0.02397 0.01739 -0.02066 AFIX 137 H1A 2 0.207289 0.030246 -0.157798 11.00000 -1.50000 H1B 2 0.049209 0.009583 -0.109435 11.00000 -1.50000 H1C 2 0.233454 -0.017656 -0.080677 11.00000 -1.50000 AFIX 0 C2 1 0.246152 0.039222 0.034978 11.00000 0.03857 0.04212 = 0.03073 -0.01078 0.01554 -0.01318 C3 1 0.380047 0.021295 0.135773 11.00000 0.04235 0.02925 = 0.03815 -0.00769 0.01938 -0.00441 AFIX 43 H3 2 0.431246 -0.007740 0.125461 11.00000 -1.20000 AFIX 0 C4 1 0.441416 0.044715 0.251658 11.00000 0.03241 0.02646 = 0.02979 0.00013 0.01243 0.00099 C5 1 0.365700 0.087481 0.266130 11.00000 0.02430 0.02530 = 0.02367 -0.00121 0.00845 -0.00166 C6 1 0.230630 0.106471 0.165365 11.00000 0.02407 0.02942 = 0.02673 0.00233 0.00828 -0.00226 C7 1 0.173993 0.081971 0.051401 11.00000 0.02840 0.04483 = 0.02308 -0.00079 0.00605 -0.00753 AFIX 43 H7 2 0.083357 0.094787 -0.017295 11.00000 -1.20000 AFIX 0 C8 1 0.586714 0.024125 0.359035 11.00000 0.04453 0.04085 = 0.04068 0.00808 0.01329 0.01639 AFIX 137 H8A 2 0.594579 -0.009267 0.344957 11.00000 -1.50000 H8B 2 0.560298 0.029376 0.440342 11.00000 -1.50000 H8C 2 0.699789 0.038872 0.361660 11.00000 -1.50000 AFIX 0 C9 1 0.147778 0.152459 0.179736 11.00000 0.03175 0.03405 = 0.04019 0.00547 0.00835 0.00581 AFIX 137 H9A 2 0.092553 0.150552 0.249396 11.00000 -1.50000 H9B 2 0.057540 0.160194 0.099897 11.00000 -1.50000 H9C 2 0.239328 0.176555 0.199267 11.00000 -1.50000 AFIX 0 C10 1 0.867840 0.231502 0.593729 11.00000 0.04067 0.04387 = 0.04568 -0.00972 0.00928 -0.01756 AFIX 137 H10A 2 0.799472 0.260388 0.580767 11.00000 -1.50000 H10B 2 0.984626 0.237314 0.581744 11.00000 -1.50000 H10C 2 0.882328 0.220046 0.680609 11.00000 -1.50000 AFIX 0 C11 1 0.771770 0.196009 0.499146 11.00000 0.02780 0.03208 = 0.03658 -0.00153 0.00836 -0.00622 C12 1 0.799585 0.185209 0.381471 11.00000 0.02740 0.03497 = 0.03817 0.00047 0.01237 -0.00535 AFIX 43 H12 2 0.888756 0.198126 0.348833 11.00000 -1.20000 AFIX 0 C13 1 0.675869 0.152687 0.320916 11.00000 0.02558 0.03091 = 0.03153 -0.00027 0.01068 -0.00147 C14 1 0.661205 0.133994 0.190269 11.00000 0.03685 0.04580 = 0.03628 -0.00553 0.01975 -0.00807 AFIX 137 H14A 2 0.744421 0.150421 0.153939 11.00000 -1.50000 H14B 2 0.540112 0.138504 0.135144 11.00000 -1.50000 H14C 2 0.689492 0.100830 0.196276 11.00000 -1.50000 AFIX 0 C15 1 0.570795 0.143364 0.406413 11.00000 0.02551 0.02743 = 0.02622 -0.00205 0.00805 -0.00187 C16 1 0.424413 0.113748 0.389526 11.00000 0.02334 0.02495 = 0.02376 -0.00105 0.00632 -0.00063 C17 1 0.321918 0.107875 0.474657 11.00000 0.02525 0.02558 = 0.02303 -0.00096 0.00715 -0.00166 C18 1 0.173826 0.077485 0.464889 11.00000 0.02695 0.02896 = 0.02660 0.00181 0.00732 -0.00317 C19 1 0.092163 0.041553 0.366504 11.00000 0.03707 0.04023 = 0.03395 -0.00447 0.01217 -0.01545 AFIX 137 H19A 2 0.037164 0.056735 0.284434 11.00000 -1.50000 H19B 2 0.001852 0.024346 0.393602 11.00000 -1.50000 H19C 2 0.184078 0.020082 0.357147 11.00000 -1.50000 AFIX 0 C20 1 0.115382 0.086748 0.569840 11.00000 0.03116 0.03337 = 0.03032 0.00275 0.01258 -0.00416 AFIX 43 H20 2 0.018356 0.072149 0.589616 11.00000 -1.20000 AFIX 0 C21 1 0.223238 0.121303 0.642286 11.00000 0.03471 0.03211 = 0.02709 0.00128 0.01331 -0.00042 C22 1 0.210399 0.141944 0.764746 11.00000 0.05403 0.04528 = 0.03424 -0.00573 0.02393 -0.00594 AFIX 137 H22A 2 0.295586 0.126684 0.836766 11.00000 -1.50000 H22B 2 0.090207 0.137525 0.771820 11.00000 -1.50000 H22C 2 0.236978 0.175166 0.766006 11.00000 -1.50000 AFIX 0 C23 1 0.680463 0.158472 0.818737 11.00000 0.04194 0.05174 = 0.03275 0.00359 0.00075 -0.00619 AFIX 23 H23A 2 0.799978 0.172051 0.832934 11.00000 -1.20000 H23B 2 0.631221 0.170456 0.886405 11.00000 -1.20000 AFIX 0 C24 1 0.698025 0.106146 0.831803 11.00000 0.05411 0.05779 = 0.08837 0.02708 -0.01280 0.00271 AFIX 137 H24A 2 0.754794 0.094134 0.769312 11.00000 -1.50000 H24B 2 0.580183 0.092268 0.816256 11.00000 -1.50000 H24C 2 0.770431 0.098264 0.918276 11.00000 -1.50000 AFIX 0 C25 1 0.419059 0.241630 0.632450 11.00000 0.04789 0.02967 = 0.03820 -0.00194 0.01559 0.00094 AFIX 23 H25A 2 0.331556 0.242709 0.681861 11.00000 -1.20000 H25B 2 0.512039 0.264873 0.669571 11.00000 -1.20000 AFIX 0 C26 1 0.326645 0.254829 0.493778 11.00000 0.07957 0.05896 = 0.04451 0.01638 0.02673 0.02833 AFIX 137 H26A 2 0.414298 0.256533 0.445821 11.00000 -1.50000 H26B 2 0.268991 0.285061 0.491410 11.00000 -1.50000 H26C 2 0.237404 0.231354 0.455207 11.00000 -1.50000 AFIX 0 HKLF 4 REM bo4592 in P2(1)/c REM R1 = 0.0581 for 6811 Fo > 4sig(Fo) and 0.0683 for all 7873 data REM 271 parameters refined using 0 restraints END WGHT 0.0703 0.4018 REM Highest difference peak 0.344, deepest hole -0.398, 1-sigma level 0.047 Q1 1 0.4022 0.1022 0.3303 11.00000 0.05 0.29 Q2 1 0.5029 0.1265 0.3987 11.00000 0.05 0.28 Q3 1 0.4527 0.2113 0.6384 11.00000 0.05 0.28 Q4 1 0.7989 0.1872 0.4404 11.00000 0.05 0.27 Q5 1 0.6221 0.1800 0.5780 11.00000 0.05 0.26 Q6 1 0.7362 0.1691 0.3499 11.00000 0.05 0.25 Q7 1 0.6382 0.1769 0.7468 11.00000 0.05 0.24 Q8 1 0.2761 0.0912 0.4745 11.00000 0.05 0.24 Q9 1 0.2144 0.1331 0.6989 11.00000 0.05 0.24 Q10 1 0.4096 0.0687 0.2575 11.00000 0.05 0.23 Q11 1 0.3909 0.1057 0.4380 11.00000 0.05 0.23 Q12 1 0.6722 0.1417 0.2649 11.00000 0.05 0.23 Q13 1 0.4139 0.0296 0.2009 11.00000 0.05 0.23 Q14 1 0.2970 0.0277 0.0825 11.00000 0.05 0.23 Q15 1 0.4169 0.1533 0.6056 11.00000 0.05 0.23 Q16 1 0.6266 0.0388 0.4263 11.00000 0.05 0.23 Q17 1 0.5952 0.1464 0.3580 11.00000 0.05 0.22 Q18 1 0.8852 0.2615 0.5370 11.00000 0.05 0.22 Q19 1 0.1403 0.0803 0.5165 11.00000 0.05 0.22 Q20 1 0.6255 0.1612 0.6832 11.00000 0.05 0.21 ; _shelx_res_checksum 46077 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Al1 Al 0.52814(6) 0.17950(2) 0.65091(4) 0.02840(11) Uani 1 1 d . N1 N 0.63610(15) 0.17101(4) 0.51626(11) 0.0289(2) Uani 1 1 d . N2 N 0.34849(15) 0.13414(4) 0.58700(10) 0.0271(2) Uani 1 1 d . C1 C 0.1781(3) 0.01305(7) -0.08911(17) 0.0535(5) Uani 1 1 d . H1A H 0.2073 0.0302 -0.1578 0.080 Uiso 1 1 calc GR H1B H 0.0492 0.0096 -0.1094 0.080 Uiso 1 1 calc GR H1C H 0.2335 -0.0177 -0.0807 0.080 Uiso 1 1 calc GR C2 C 0.2462(2) 0.03922(5) 0.03498(14) 0.0360(3) Uani 1 1 d . C3 C 0.3800(2) 0.02129(5) 0.13577(14) 0.0349(3) Uani 1 1 d . H3 H 0.4312 -0.0077 0.1255 0.042 Uiso 1 1 calc R C4 C 0.44142(18) 0.04472(4) 0.25166(13) 0.0288(2) Uani 1 1 d . C5 C 0.36570(16) 0.08748(4) 0.26613(11) 0.0241(2) Uani 1 1 d . C6 C 0.23063(16) 0.10647(4) 0.16536(12) 0.0265(2) Uani 1 1 d . C7 C 0.17399(18) 0.08197(5) 0.05140(12) 0.0324(3) Uani 1 1 d . H7 H 0.0834 0.0948 -0.0173 0.039 Uiso 1 1 calc R C8 C 0.5867(2) 0.02413(6) 0.35903(16) 0.0418(3) Uani 1 1 d . H8A H 0.5946 -0.0093 0.3450 0.063 Uiso 1 1 calc GR H8B H 0.5603 0.0294 0.4403 0.063 Uiso 1 1 calc GR H8C H 0.6998 0.0389 0.3617 0.063 Uiso 1 1 calc GR C9 C 0.14778(19) 0.15246(5) 0.17974(15) 0.0357(3) Uani 1 1 d . H9A H 0.0926 0.1506 0.2494 0.054 Uiso 1 1 calc GR H9B H 0.0575 0.1602 0.0999 0.054 Uiso 1 1 calc GR H9C H 0.2393 0.1766 0.1993 0.054 Uiso 1 1 calc GR C10 C 0.8678(2) 0.23150(6) 0.59373(16) 0.0440(4) Uani 1 1 d . H10A H 0.7995 0.2604 0.5808 0.066 Uiso 1 1 calc GR H10B H 0.9846 0.2373 0.5817 0.066 Uiso 1 1 calc GR H10C H 0.8823 0.2200 0.6806 0.066 Uiso 1 1 calc GR C11 C 0.77177(18) 0.19601(5) 0.49915(14) 0.0323(3) Uani 1 1 d . C12 C 0.79958(18) 0.18521(5) 0.38147(14) 0.0329(3) Uani 1 1 d . H12 H 0.8888 0.1981 0.3488 0.039 Uiso 1 1 calc R C13 C 0.67587(17) 0.15269(5) 0.32092(13) 0.0288(2) Uani 1 1 d . C14 C 0.6612(2) 0.13399(6) 0.19027(14) 0.0377(3) Uani 1 1 d . H14A H 0.7444 0.1504 0.1539 0.057 Uiso 1 1 calc GR H14B H 0.5401 0.1385 0.1351 0.057 Uiso 1 1 calc GR H14C H 0.6895 0.1008 0.1963 0.057 Uiso 1 1 calc GR C15 C 0.57080(16) 0.14336(4) 0.40641(12) 0.0263(2) Uani 1 1 d . C16 C 0.42441(16) 0.11375(4) 0.38953(11) 0.0241(2) Uani 1 1 d . C17 C 0.32192(16) 0.10788(4) 0.47466(11) 0.0246(2) Uani 1 1 d . C18 C 0.17383(17) 0.07749(4) 0.46489(12) 0.0276(2) Uani 1 1 d . C19 C 0.0922(2) 0.04155(5) 0.36650(14) 0.0367(3) Uani 1 1 d . H19A H 0.0372 0.0567 0.2844 0.055 Uiso 1 1 calc GR H19B H 0.0019 0.0243 0.3936 0.055 Uiso 1 1 calc GR H19C H 0.1841 0.0201 0.3571 0.055 Uiso 1 1 calc GR C20 C 0.11538(18) 0.08675(5) 0.56984(13) 0.0308(3) Uani 1 1 d . H20 H 0.0184 0.0721 0.5896 0.037 Uiso 1 1 calc R C21 C 0.22324(19) 0.12130(5) 0.64229(13) 0.0304(3) Uani 1 1 d . C22 C 0.2104(2) 0.14194(6) 0.76475(15) 0.0422(3) Uani 1 1 d . H22A H 0.2956 0.1267 0.8368 0.063 Uiso 1 1 calc GR H22B H 0.0902 0.1375 0.7718 0.063 Uiso 1 1 calc GR H22C H 0.2370 0.1752 0.7660 0.063 Uiso 1 1 calc GR C23 C 0.6805(2) 0.15847(6) 0.81874(15) 0.0442(4) Uani 1 1 d . H23A H 0.8000 0.1721 0.8329 0.053 Uiso 1 1 calc R H23B H 0.6312 0.1705 0.8864 0.053 Uiso 1 1 calc R C24 C 0.6980(3) 0.10615(8) 0.8318(2) 0.0737(7) Uani 1 1 d . H24A H 0.7548 0.0941 0.7693 0.110 Uiso 1 1 calc GR H24B H 0.5802 0.0923 0.8163 0.110 Uiso 1 1 calc GR H24C H 0.7704 0.0983 0.9183 0.110 Uiso 1 1 calc GR C25 C 0.4191(2) 0.24163(5) 0.63245(15) 0.0379(3) Uani 1 1 d . H25A H 0.3316 0.2427 0.6819 0.045 Uiso 1 1 calc R H25B H 0.5120 0.2649 0.6696 0.045 Uiso 1 1 calc R C26 C 0.3266(3) 0.25483(7) 0.49378(18) 0.0592(5) Uani 1 1 d . H26A H 0.4143 0.2565 0.4458 0.089 Uiso 1 1 calc GR H26B H 0.2690 0.2851 0.4914 0.089 Uiso 1 1 calc GR H26C H 0.2374 0.2314 0.4552 0.089 Uiso 1 1 calc GR 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 0.0326(2) 0.0276(2) 0.02429(19) -0.00328(14) 0.00704(15) -0.00332(15) N1 0.0271(5) 0.0298(5) 0.0293(5) -0.0040(4) 0.0074(4) -0.0058(4) N2 0.0294(5) 0.0290(5) 0.0241(5) -0.0022(4) 0.0094(4) -0.0025(4) C1 0.0566(10) 0.0678(12) 0.0385(8) -0.0240(8) 0.0174(7) -0.0207(9) C2 0.0386(7) 0.0421(7) 0.0307(7) -0.0108(5) 0.0155(6) -0.0132(6) C3 0.0423(8) 0.0292(6) 0.0381(7) -0.0077(5) 0.0194(6) -0.0044(5) C4 0.0324(6) 0.0265(5) 0.0298(6) 0.0001(4) 0.0124(5) 0.0010(5) C5 0.0243(5) 0.0253(5) 0.0237(5) -0.0012(4) 0.0085(4) -0.0017(4) C6 0.0241(5) 0.0294(6) 0.0267(6) 0.0023(4) 0.0083(4) -0.0023(4) C7 0.0284(6) 0.0448(7) 0.0231(6) -0.0008(5) 0.0060(5) -0.0075(5) C8 0.0445(8) 0.0408(7) 0.0407(8) 0.0081(6) 0.0133(6) 0.0164(6) C9 0.0317(7) 0.0341(7) 0.0402(7) 0.0055(5) 0.0083(6) 0.0058(5) C10 0.0407(8) 0.0439(8) 0.0457(9) -0.0097(7) 0.0093(7) -0.0176(7) C11 0.0278(6) 0.0321(6) 0.0366(7) -0.0015(5) 0.0084(5) -0.0062(5) C12 0.0274(6) 0.0350(6) 0.0382(7) 0.0005(5) 0.0124(5) -0.0053(5) C13 0.0256(6) 0.0309(6) 0.0315(6) -0.0003(5) 0.0107(5) -0.0015(5) C14 0.0369(7) 0.0458(8) 0.0363(7) -0.0055(6) 0.0197(6) -0.0081(6) C15 0.0255(5) 0.0274(5) 0.0262(5) -0.0020(4) 0.0081(4) -0.0019(4) C16 0.0233(5) 0.0249(5) 0.0238(5) -0.0011(4) 0.0063(4) -0.0006(4) C17 0.0252(5) 0.0256(5) 0.0230(5) -0.0010(4) 0.0071(4) -0.0017(4) C18 0.0270(6) 0.0290(6) 0.0266(6) 0.0018(4) 0.0073(4) -0.0032(4) C19 0.0371(7) 0.0402(7) 0.0340(7) -0.0045(5) 0.0122(6) -0.0154(6) C20 0.0312(6) 0.0334(6) 0.0303(6) 0.0028(5) 0.0126(5) -0.0042(5) C21 0.0347(6) 0.0321(6) 0.0271(6) 0.0013(5) 0.0133(5) -0.0004(5) C22 0.0540(9) 0.0453(8) 0.0342(7) -0.0057(6) 0.0239(7) -0.0059(7) C23 0.0419(8) 0.0517(9) 0.0327(7) 0.0036(6) 0.0007(6) -0.0062(7) C24 0.0541(12) 0.0578(12) 0.0884(16) 0.0271(11) -0.0128(11) 0.0027(9) C25 0.0479(8) 0.0297(6) 0.0382(7) -0.0019(5) 0.0156(6) 0.0009(6) C26 0.0796(14) 0.0590(11) 0.0445(10) 0.0164(8) 0.0267(9) 0.0283(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Al1 C23 112.83(7) N1 Al1 C25 108.31(6) N2 Al1 N1 94.44(5) N2 Al1 C23 108.59(7) N2 Al1 C25 109.27(6) C25 Al1 C23 120.29(7) C11 N1 Al1 125.69(10) C11 N1 C15 107.20(11) C15 N1 Al1 126.32(9) C17 N2 Al1 126.77(9) C21 N2 Al1 125.90(9) C21 N2 C17 107.33(11) 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 C3 C2 C1 121.33(15) C3 C2 C7 118.28(12) C7 C2 C1 120.39(15) C2 C3 H3 119.1 C2 C3 C4 121.81(13) C4 C3 H3 119.1 C3 C4 C5 118.81(12) C3 C4 C8 120.31(13) C5 C4 C8 120.88(12) C4 C5 C6 120.48(11) C4 C5 C16 121.03(11) C6 C5 C16 118.48(11) C5 C6 C9 121.03(12) C7 C6 C5 118.73(12) C7 C6 C9 120.25(12) C2 C7 H7 119.1 C6 C7 C2 121.89(13) C6 C7 H7 119.1 C4 C8 H8A 109.5 C4 C8 H8B 109.5 C4 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C6 C9 H9A 109.5 C6 C9 H9B 109.5 C6 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C11 C10 H10A 109.5 C11 C10 H10B 109.5 C11 C10 H10C 109.5 N1 C11 C10 122.37(13) N1 C11 C12 110.34(12) C12 C11 C10 127.23(13) C11 C12 H12 125.8 C13 C12 C11 108.50(12) C13 C12 H12 125.8 C12 C13 C14 123.59(13) C12 C13 C15 105.96(12) C15 C13 C14 130.43(12) C13 C14 H14A 109.5 C13 C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N1 C15 C13 108.00(11) C16 C15 N1 122.81(11) C16 C15 C13 129.17(12) C15 C16 C5 117.13(11) C15 C16 C17 126.31(11) C17 C16 C5 116.49(10) N2 C17 C18 107.94(11) C16 C17 N2 122.85(11) C16 C17 C18 129.18(11) C17 C18 C19 130.31(12) C20 C18 C17 106.09(11) C20 C18 C19 123.59(12) C18 C19 H19A 109.5 C18 C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C18 C20 H20 125.8 C18 C20 C21 108.37(12) C21 C20 H20 125.8 N2 C21 C20 110.27(12) N2 C21 C22 122.52(13) C20 C21 C22 127.21(13) C21 C22 H22A 109.5 C21 C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 Al1 C23 H23A 108.8 Al1 C23 H23B 108.8 H23A C23 H23B 107.6 C24 C23 Al1 114.00(13) C24 C23 H23A 108.8 C24 C23 H23B 108.8 C23 C24 H24A 109.5 C23 C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 Al1 C25 H25A 108.9 Al1 C25 H25B 108.9 H25A C25 H25B 107.7 C26 C25 Al1 113.42(11) C26 C25 H25A 108.9 C26 C25 H25B 108.9 C25 C26 H26A 109.5 C25 C26 H26B 109.5 C25 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 N1 1.9134(13) Al1 N2 1.9067(12) Al1 C23 1.9768(17) Al1 C25 1.9725(15) N1 C11 1.3458(17) N1 C15 1.4092(16) N2 C17 1.4056(15) N2 C21 1.3475(17) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C1 C2 1.509(2) C2 C3 1.388(2) C2 C7 1.391(2) C3 H3 0.9500 C3 C4 1.3933(19) C4 C5 1.3985(17) C4 C8 1.506(2) C5 C6 1.4045(17) C5 C16 1.4990(16) C6 C7 1.3890(18) C6 C9 1.5061(19) C7 H7 0.9500 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C10 C11 1.497(2) C11 C12 1.399(2) C12 H12 0.9500 C12 C13 1.3776(19) C13 C14 1.4984(19) C13 C15 1.4393(18) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.4040(17) C16 C17 1.4052(17) C17 C18 1.4384(17) C18 C19 1.4988(19) C18 C20 1.3780(19) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20 0.9500 C20 C21 1.3986(19) C21 C22 1.4935(19) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.518(3) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9900 C25 H25B 0.9900 C25 C26 1.529(2) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 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 Al1 N1 C11 C10 6.1(2) Al1 N1 C11 C12 -171.12(10) Al1 N1 C15 C13 170.71(9) Al1 N1 C15 C16 -7.65(18) Al1 N2 C17 C16 -3.08(17) Al1 N2 C17 C18 179.01(9) Al1 N2 C21 C20 -179.19(9) Al1 N2 C21 C22 0.0(2) N1 C11 C12 C13 0.83(17) N1 C15 C16 C5 178.10(11) N1 C15 C16 C17 1.3(2) N2 C17 C18 C19 -178.30(13) N2 C17 C18 C20 0.69(14) C1 C2 C3 C4 -178.67(14) C1 C2 C7 C6 178.47(14) C2 C3 C4 C5 -0.1(2) C2 C3 C4 C8 179.86(14) C3 C2 C7 C6 -0.8(2) C3 C4 C5 C6 -0.20(19) C3 C4 C5 C16 178.89(12) C4 C5 C6 C7 0.00(18) C4 C5 C6 C9 179.91(12) C4 C5 C16 C15 86.66(15) C4 C5 C16 C17 -96.21(14) C5 C6 C7 C2 0.5(2) C5 C16 C17 N2 -172.58(11) C5 C16 C17 C18 4.86(19) C6 C5 C16 C15 -94.23(14) C6 C5 C16 C17 82.90(14) C7 C2 C3 C4 0.6(2) C8 C4 C5 C6 179.82(13) C8 C4 C5 C16 -1.08(19) C9 C6 C7 C2 -179.39(13) C10 C11 C12 C13 -176.26(15) C11 N1 C15 C13 0.43(15) C11 N1 C15 C16 -177.92(12) C11 C12 C13 C14 177.87(13) C11 C12 C13 C15 -0.52(15) C12 C13 C15 N1 0.06(15) C12 C13 C15 C16 178.28(13) C13 C15 C16 C5 0.1(2) C13 C15 C16 C17 -176.70(13) C14 C13 C15 N1 -178.18(14) C14 C13 C15 C16 0.0(2) C15 N1 C11 C10 176.49(13) C15 N1 C11 C12 -0.77(16) C15 C16 C17 N2 4.3(2) C15 C16 C17 C18 -178.31(13) C16 C5 C6 C7 -179.12(11) C16 C5 C6 C9 0.80(18) C16 C17 C18 C19 4.0(2) C16 C17 C18 C20 -177.05(13) C17 N2 C21 C20 0.65(15) C17 N2 C21 C22 179.81(13) C17 C18 C20 C21 -0.30(15) C18 C20 C21 N2 -0.22(16) C18 C20 C21 C22 -179.33(14) C19 C18 C20 C21 178.77(13) C21 N2 C17 C16 177.09(12) C21 N2 C17 C18 -0.82(14)