#------------------------------------------------------------------------------ #$Date: 2017-12-26 07:21:00 +0200 (Tue, 26 Dec 2017) $ #$Revision: 204518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/85/1548545.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_1548545 loop_ _publ_author_name 'Yu, Chao' 'Zhang, Pengfei' 'Gao, Fei' 'Zhang, Shaowen' 'Li, Xiaofang' _publ_section_title ; Displacement Type Fluorescent Probe Reveals Active Species in Coordinative Polymerization of Olefin ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/C7PY01915G _journal_year 2017 _chemical_formula_moiety 'C30 H43 Al N2' _chemical_formula_sum 'C30 H43 Al N2' _chemical_formula_weight 458.64 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _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 94.73(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.6985(17) _cell_length_b 11.354(2) _cell_length_c 28.622(6) _cell_measurement_reflns_used 10241 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 31.5074 _cell_measurement_theta_min 1.9306 _cell_volume 2817.2(10) _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 0.998 _diffrn_measured_fraction_theta_max 0.996 _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 0.0254 _diffrn_reflns_av_unetI/netI 0.0224 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 41434 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.501 _diffrn_reflns_theta_min 2.293 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.081 _exptl_crystal_description block _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.33 _refine_diff_density_max 0.382 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 9322 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0509 _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^)+(0.0722P)^2^+0.6883P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1359 _refine_ls_wR_factor_ref 0.1411 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8493 _reflns_number_total 9322 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7py01915g2.cif _cod_data_source_block bo4475 _cod_original_cell_volume 2817.1(10) _cod_database_code 1548545 _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 0.971 _shelx_estimated_absorpt_t_min 0.959 _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 Riding coordinates: C7(H7A,H7B,H7C) 2.b Ternary CH refined with riding coordinates: C25(H25), C29(H29) 2.c Secondary CH2 refined with riding coordinates: C23(H23A,H23B), C27(H27A,H27B) 2.d Aromatic/amide H refined with riding coordinates: C2(H2), C6(H6), C12(H12), C19(H19) 2.e Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B, H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C) ; _shelx_res_file ; bo4475.res created by SHELXL-2014/7 TITL bo4475 in P2(1)/n CELL 0.71073 8.6985 11.3538 28.6217 90 94.726 90 ZERR 4 0.0017 0.0023 0.0057 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Al UNIT 120 172 8 4 L.S. 4 PLAN 20 SIZE 0.46 0.34 0.33 TEMP -120 BOND BOND $H CONF fmap 2 acta OMIT -4 3 3 OMIT 1 3 9 REM REM REM WGHT 0.072200 0.688300 FVAR 4.66354 AL1 4 0.420706 0.563356 0.184396 11.00000 0.02049 0.02009 = 0.02076 -0.00217 -0.00106 0.00015 N1 3 0.256225 0.451739 0.177107 11.00000 0.02056 0.02066 = 0.02042 -0.00220 0.00191 0.00028 N2 3 0.523457 0.501790 0.133264 11.00000 0.02162 0.02486 = 0.02466 -0.00290 0.00231 -0.00240 C1 1 0.237214 0.073967 0.004921 11.00000 0.03256 0.02701 = 0.02991 -0.00886 -0.00168 0.00247 C2 1 0.167060 0.184100 0.000200 11.00000 0.03108 0.03045 = 0.02541 -0.00535 -0.00543 0.00445 AFIX 43 H2 2 0.097889 0.199342 -0.026556 11.00000 -1.20000 AFIX 0 C3 1 0.195273 0.272489 0.033510 11.00000 0.02635 0.02292 = 0.02240 -0.00111 -0.00172 0.00400 C4 1 0.298913 0.250384 0.072686 11.00000 0.02437 0.01913 = 0.01985 -0.00189 -0.00007 0.00224 C5 1 0.369691 0.139686 0.078491 11.00000 0.02720 0.02161 = 0.02382 -0.00105 -0.00056 0.00376 C6 1 0.337826 0.053492 0.044441 11.00000 0.03221 0.02140 = 0.03015 -0.00426 -0.00019 0.00510 AFIX 43 H6 2 0.386099 -0.021326 0.048303 11.00000 -1.20000 AFIX 0 C7 1 0.203174 -0.020494 -0.031508 11.00000 0.04909 0.03792 = 0.04449 -0.02039 -0.00745 0.00545 AFIX 3 H7A 2 0.098614 -0.009624 -0.046408 11.00000 -1.50000 H7B 2 0.211114 -0.098074 -0.016498 11.00000 -1.50000 H7C 2 0.277694 -0.015174 -0.055308 11.00000 -1.50000 AFIX 0 C8 1 0.115047 0.389669 0.027466 11.00000 0.03717 0.02678 = 0.02954 -0.00061 -0.00629 0.01001 AFIX 137 H8A 2 0.049703 0.390035 -0.002110 11.00000 -1.50000 H8B 2 0.192170 0.452480 0.026967 11.00000 -1.50000 H8C 2 0.051052 0.402761 0.053607 11.00000 -1.50000 AFIX 0 C9 1 0.479655 0.113741 0.120758 11.00000 0.04155 0.02853 = 0.02974 -0.00075 -0.00878 0.01016 AFIX 137 H9A 2 0.572052 0.162771 0.119769 11.00000 -1.50000 H9B 2 0.509043 0.030424 0.120603 11.00000 -1.50000 H9C 2 0.429325 0.131169 0.149367 11.00000 -1.50000 AFIX 0 C10 1 0.025404 0.192110 0.127589 11.00000 0.03670 0.02868 = 0.03965 -0.00799 0.00862 -0.01257 AFIX 137 H10A 2 -0.059560 0.163596 0.145011 11.00000 -1.50000 H10B 2 0.101582 0.129165 0.125432 11.00000 -1.50000 H10C 2 -0.014808 0.215749 0.095987 11.00000 -1.50000 AFIX 0 C11 1 0.100374 0.295883 0.152587 11.00000 0.02503 0.02122 = 0.02739 -0.00054 0.00277 -0.00224 C12 1 0.043681 0.348139 0.191199 11.00000 0.02600 0.02536 = 0.03156 -0.00173 0.00831 -0.00381 AFIX 43 H12 2 -0.045400 0.324056 0.205775 11.00000 -1.20000 AFIX 0 C13 1 0.140366 0.443055 0.205233 11.00000 0.02424 0.02310 = 0.02400 -0.00127 0.00405 0.00116 C14 1 0.122934 0.525608 0.245137 11.00000 0.03219 0.03125 = 0.02915 -0.00660 0.00883 0.00055 AFIX 137 H14A 2 0.151151 0.484984 0.274820 11.00000 -1.50000 H14B 2 0.015570 0.552174 0.244414 11.00000 -1.50000 H14C 2 0.190653 0.593787 0.242338 11.00000 -1.50000 AFIX 0 C15 1 0.236471 0.361616 0.143377 11.00000 0.02169 0.01851 = 0.02078 -0.00136 0.00052 0.00029 C16 1 0.335925 0.346317 0.107705 11.00000 0.02205 0.01840 = 0.01938 -0.00039 -0.00054 0.00260 C17 1 0.469186 0.413421 0.101623 11.00000 0.02292 0.02159 = 0.02141 -0.00091 0.00222 0.00204 C18 1 0.574364 0.405385 0.065560 11.00000 0.02774 0.02923 = 0.02617 -0.00055 0.00762 0.00252 C19 1 0.689486 0.486711 0.077175 11.00000 0.02782 0.03937 = 0.03499 -0.00236 0.01145 -0.00383 AFIX 43 H19 2 0.776825 0.501154 0.060151 11.00000 -1.20000 AFIX 0 C20 1 0.655223 0.544123 0.118342 11.00000 0.02454 0.03364 = 0.03288 -0.00199 0.00470 -0.00477 C21 1 0.569099 0.331951 0.021925 11.00000 0.04434 0.03961 = 0.03185 -0.00738 0.01692 -0.00152 AFIX 137 H21A 2 0.566847 0.248349 0.030358 11.00000 -1.50000 H21B 2 0.660758 0.347950 0.005210 11.00000 -1.50000 H21C 2 0.476248 0.351551 0.001682 11.00000 -1.50000 AFIX 0 C22 1 0.747013 0.639868 0.143348 11.00000 0.03554 0.05034 = 0.04876 -0.01170 0.00903 -0.01986 AFIX 137 H22A 2 0.722023 0.715509 0.128069 11.00000 -1.50000 H22B 2 0.857308 0.623574 0.142288 11.00000 -1.50000 H22C 2 0.721846 0.643251 0.176071 11.00000 -1.50000 AFIX 0 C23 1 0.340373 0.724981 0.172397 11.00000 0.02792 0.02032 = 0.02865 -0.00187 -0.00323 -0.00023 AFIX 23 H23A 2 0.318709 0.759869 0.202868 11.00000 -1.20000 H23B 2 0.423485 0.772367 0.160008 11.00000 -1.20000 AFIX 0 C24 1 0.226233 0.696935 0.089936 11.00000 0.11696 0.05531 = 0.03811 -0.01858 -0.03409 0.04890 AFIX 137 H24A 2 0.308361 0.744776 0.078084 11.00000 -1.50000 H24B 2 0.131906 0.705073 0.068981 11.00000 -1.50000 H24C 2 0.258050 0.614119 0.091240 11.00000 -1.50000 AFIX 0 C25 1 0.195798 0.738569 0.138812 11.00000 0.03189 0.02475 = 0.03527 0.00104 -0.00690 0.00220 AFIX 13 H25 2 0.113253 0.687578 0.150401 11.00000 -1.20000 AFIX 0 C26 1 0.135920 0.865199 0.136228 11.00000 0.04321 0.03232 = 0.03818 0.00324 0.00112 0.01299 AFIX 137 H26A 2 0.115234 0.891832 0.167671 11.00000 -1.50000 H26B 2 0.040522 0.868499 0.115516 11.00000 -1.50000 H26C 2 0.213623 0.916435 0.123842 11.00000 -1.50000 AFIX 0 C27 1 0.548068 0.543322 0.244369 11.00000 0.02540 0.02585 = 0.02397 -0.00374 -0.00280 0.00197 AFIX 23 H27A 2 0.605042 0.617723 0.251046 11.00000 -1.20000 H27B 2 0.477290 0.532798 0.269419 11.00000 -1.20000 AFIX 0 C28 1 0.587852 0.322721 0.239507 11.00000 0.04355 0.02802 = 0.04761 -0.00264 -0.00883 0.00664 AFIX 137 H28A 2 0.509922 0.310893 0.261912 11.00000 -1.50000 H28B 2 0.665493 0.260179 0.243416 11.00000 -1.50000 H28C 2 0.538305 0.320428 0.207504 11.00000 -1.50000 AFIX 0 C29 1 0.665449 0.442089 0.248365 11.00000 0.02389 0.03118 = 0.02781 0.00148 -0.00156 0.00323 AFIX 13 H29 2 0.739114 0.454197 0.223755 11.00000 -1.20000 AFIX 0 C30 1 0.758630 0.442206 0.296058 11.00000 0.02830 0.04905 = 0.03498 0.00893 -0.00740 0.00050 AFIX 137 H30A 2 0.807335 0.519365 0.301510 11.00000 -1.50000 H30B 2 0.838436 0.381201 0.296483 11.00000 -1.50000 H30C 2 0.689842 0.426126 0.320747 11.00000 -1.50000 AFIX 0 HKLF 4 REM bo4475 in P2(1)/n REM R1 = 0.0509 for 8493 Fo > 4sig(Fo) and 0.0564 for all 9322 data REM 308 parameters refined using 0 restraints END WGHT 0.0722 0.6883 REM Highest difference peak 0.382, deepest hole -0.302, 1-sigma level 0.049 Q1 1 0.6441 0.4395 0.0712 11.00000 0.05 0.38 Q2 1 0.2530 0.2665 0.0532 11.00000 0.05 0.37 Q3 1 0.3323 0.2018 0.0766 11.00000 0.05 0.35 Q4 1 0.2156 0.1362 0.0010 11.00000 0.05 0.34 Q5 1 0.8180 0.6787 0.1241 11.00000 0.05 0.34 Q6 1 0.3138 0.2986 0.0901 11.00000 0.05 0.34 Q7 1 0.3745 0.6623 0.1760 11.00000 0.05 0.33 Q8 1 0.2941 -0.0720 -0.0342 11.00000 0.05 0.33 Q9 1 0.4046 0.3806 0.1045 11.00000 0.05 0.32 Q10 1 0.4938 0.5486 0.2178 11.00000 0.05 0.31 Q11 1 0.0854 0.4003 0.1982 11.00000 0.05 0.31 Q12 1 0.3480 0.0954 0.0618 11.00000 0.05 0.31 Q13 1 0.3235 0.4962 0.1792 11.00000 0.05 0.30 Q14 1 0.1442 0.4817 0.2248 11.00000 0.05 0.29 Q15 1 0.2651 0.7385 0.1551 11.00000 0.05 0.28 Q16 1 0.6746 0.5185 0.0965 11.00000 0.05 0.28 Q17 1 0.4945 0.5361 0.1538 11.00000 0.05 0.27 Q18 1 0.0717 0.3160 0.1717 11.00000 0.05 0.27 Q19 1 0.2766 0.3576 0.1247 11.00000 0.05 0.26 Q20 1 0.1713 0.3248 0.1479 11.00000 0.05 0.26 ; _shelx_res_checksum 58025 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Al1 Al 0.42071(3) 0.56336(3) 0.18440(2) 0.02060(8) Uani 1 1 d . N1 N 0.25623(10) 0.45174(7) 0.17711(3) 0.02054(16) Uani 1 1 d . N2 N 0.52346(10) 0.50179(8) 0.13326(3) 0.02369(17) Uani 1 1 d . C1 C 0.23721(14) 0.07397(10) 0.00492(4) 0.0301(2) Uani 1 1 d . C2 C 0.16706(13) 0.18410(10) 0.00020(4) 0.0294(2) Uani 1 1 d . H2 H 0.0979 0.1993 -0.0266 0.035 Uiso 1 1 calc R C3 C 0.19527(12) 0.27249(9) 0.03351(3) 0.02409(19) Uani 1 1 d . C4 C 0.29891(12) 0.25038(8) 0.07269(3) 0.02122(18) Uani 1 1 d . C5 C 0.36969(12) 0.13969(9) 0.07849(4) 0.02436(19) Uani 1 1 d . C6 C 0.33783(14) 0.05349(9) 0.04444(4) 0.0281(2) Uani 1 1 d . H6 H 0.3861 -0.0213 0.0483 0.034 Uiso 1 1 calc R C7 C 0.20317(18) -0.02049(13) -0.03151(5) 0.0445(3) Uani 1 1 d . H7A H 0.0986 -0.0096 -0.0464 0.067 Uiso 1 1 d R H7B H 0.2111 -0.0981 -0.0165 0.067 Uiso 1 1 d R H7C H 0.2777 -0.0152 -0.0553 0.067 Uiso 1 1 d R C8 C 0.11505(14) 0.38967(10) 0.02747(4) 0.0317(2) Uani 1 1 d . H8A H 0.0497 0.3900 -0.0021 0.047 Uiso 1 1 calc GR H8B H 0.1922 0.4525 0.0270 0.047 Uiso 1 1 calc GR H8C H 0.0511 0.4028 0.0536 0.047 Uiso 1 1 calc GR C9 C 0.47966(15) 0.11374(11) 0.12076(4) 0.0339(3) Uani 1 1 d . H9A H 0.5721 0.1628 0.1198 0.051 Uiso 1 1 calc GR H9B H 0.5090 0.0304 0.1206 0.051 Uiso 1 1 calc GR H9C H 0.4293 0.1312 0.1494 0.051 Uiso 1 1 calc GR C10 C 0.02540(15) 0.19211(11) 0.12759(5) 0.0347(3) Uani 1 1 d . H10A H -0.0596 0.1636 0.1450 0.052 Uiso 1 1 calc GR H10B H 0.1016 0.1292 0.1254 0.052 Uiso 1 1 calc GR H10C H -0.0148 0.2157 0.0960 0.052 Uiso 1 1 calc GR C11 C 0.10037(12) 0.29588(9) 0.15259(4) 0.02452(19) Uani 1 1 d . C12 C 0.04368(13) 0.34814(10) 0.19120(4) 0.0273(2) Uani 1 1 d . H12 H -0.0454 0.3241 0.2058 0.033 Uiso 1 1 calc R C13 C 0.14037(12) 0.44306(9) 0.20523(4) 0.02367(19) Uani 1 1 d . C14 C 0.12293(14) 0.52561(11) 0.24514(4) 0.0305(2) Uani 1 1 d . H14A H 0.1512 0.4850 0.2748 0.046 Uiso 1 1 calc GR H14B H 0.0156 0.5522 0.2444 0.046 Uiso 1 1 calc GR H14C H 0.1907 0.5938 0.2423 0.046 Uiso 1 1 calc GR C15 C 0.23647(11) 0.36162(8) 0.14338(3) 0.02039(17) Uani 1 1 d . C16 C 0.33593(11) 0.34632(8) 0.10770(3) 0.02007(17) Uani 1 1 d . C17 C 0.46919(12) 0.41342(9) 0.10162(3) 0.02195(18) Uani 1 1 d . C18 C 0.57436(13) 0.40539(10) 0.06556(4) 0.0274(2) Uani 1 1 d . C19 C 0.68949(14) 0.48671(12) 0.07718(4) 0.0336(2) Uani 1 1 d . H19 H 0.7768 0.5012 0.0602 0.040 Uiso 1 1 calc R C20 C 0.65522(13) 0.54412(11) 0.11834(4) 0.0302(2) Uani 1 1 d . C21 C 0.56910(17) 0.33195(12) 0.02192(4) 0.0378(3) Uani 1 1 d . H21A H 0.5668 0.2483 0.0304 0.057 Uiso 1 1 calc GR H21B H 0.6608 0.3479 0.0052 0.057 Uiso 1 1 calc GR H21C H 0.4762 0.3516 0.0017 0.057 Uiso 1 1 calc GR C22 C 0.74701(16) 0.63987(14) 0.14335(5) 0.0446(3) Uani 1 1 d . H22A H 0.7220 0.7155 0.1281 0.067 Uiso 1 1 calc GR H22B H 0.8573 0.6236 0.1423 0.067 Uiso 1 1 calc GR H22C H 0.7218 0.6433 0.1761 0.067 Uiso 1 1 calc GR C23 C 0.34037(13) 0.72498(9) 0.17240(4) 0.0259(2) Uani 1 1 d . H23A H 0.3187 0.7599 0.2029 0.031 Uiso 1 1 calc R H23B H 0.4235 0.7724 0.1600 0.031 Uiso 1 1 calc R C24 C 0.2262(3) 0.69693(16) 0.08994(6) 0.0724(7) Uani 1 1 d . H24A H 0.3084 0.7448 0.0781 0.109 Uiso 1 1 calc GR H24B H 0.1319 0.7051 0.0690 0.109 Uiso 1 1 calc GR H24C H 0.2580 0.6141 0.0912 0.109 Uiso 1 1 calc GR C25 C 0.19580(14) 0.73857(10) 0.13881(4) 0.0312(2) Uani 1 1 d . H25 H 0.1133 0.6876 0.1504 0.037 Uiso 1 1 calc R C26 C 0.13592(17) 0.86520(11) 0.13623(5) 0.0380(3) Uani 1 1 d . H26A H 0.1152 0.8918 0.1677 0.057 Uiso 1 1 calc GR H26B H 0.0405 0.8685 0.1155 0.057 Uiso 1 1 calc GR H26C H 0.2136 0.9164 0.1238 0.057 Uiso 1 1 calc GR C27 C 0.54807(12) 0.54332(9) 0.24437(4) 0.0253(2) Uani 1 1 d . H27A H 0.6050 0.6177 0.2510 0.030 Uiso 1 1 calc R H27B H 0.4773 0.5328 0.2694 0.030 Uiso 1 1 calc R C28 C 0.58785(17) 0.32272(11) 0.23951(5) 0.0404(3) Uani 1 1 d . H28A H 0.5099 0.3109 0.2619 0.061 Uiso 1 1 calc GR H28B H 0.6655 0.2602 0.2434 0.061 Uiso 1 1 calc GR H28C H 0.5383 0.3204 0.2075 0.061 Uiso 1 1 calc GR C29 C 0.66545(13) 0.44209(10) 0.24836(4) 0.0278(2) Uani 1 1 d . H29 H 0.7391 0.4542 0.2238 0.033 Uiso 1 1 calc R C30 C 0.75863(15) 0.44221(13) 0.29606(5) 0.0380(3) Uani 1 1 d . H30A H 0.8073 0.5194 0.3015 0.057 Uiso 1 1 calc GR H30B H 0.8384 0.3812 0.2965 0.057 Uiso 1 1 calc GR H30C H 0.6898 0.4261 0.3207 0.057 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 0.02049(15) 0.02009(14) 0.02076(14) -0.00217(10) -0.00106(11) 0.00015(10) N1 0.0206(4) 0.0207(4) 0.0204(3) -0.0022(3) 0.0019(3) 0.0003(3) N2 0.0216(4) 0.0249(4) 0.0247(4) -0.0029(3) 0.0023(3) -0.0024(3) C1 0.0326(5) 0.0270(5) 0.0299(5) -0.0089(4) -0.0017(4) 0.0025(4) C2 0.0311(5) 0.0304(5) 0.0254(5) -0.0053(4) -0.0054(4) 0.0045(4) C3 0.0263(5) 0.0229(4) 0.0224(4) -0.0011(3) -0.0017(3) 0.0040(4) C4 0.0244(4) 0.0191(4) 0.0199(4) -0.0019(3) -0.0001(3) 0.0022(3) C5 0.0272(5) 0.0216(4) 0.0238(4) -0.0010(3) -0.0006(4) 0.0038(4) C6 0.0322(5) 0.0214(4) 0.0301(5) -0.0043(4) -0.0002(4) 0.0051(4) C7 0.0491(8) 0.0379(7) 0.0445(7) -0.0204(6) -0.0074(6) 0.0055(6) C8 0.0372(6) 0.0268(5) 0.0295(5) -0.0006(4) -0.0063(4) 0.0100(4) C9 0.0415(6) 0.0285(5) 0.0297(5) -0.0008(4) -0.0088(5) 0.0102(5) C10 0.0367(6) 0.0287(5) 0.0397(6) -0.0080(4) 0.0086(5) -0.0126(5) C11 0.0250(5) 0.0212(4) 0.0274(5) -0.0005(3) 0.0028(4) -0.0022(3) C12 0.0260(5) 0.0254(5) 0.0316(5) -0.0017(4) 0.0083(4) -0.0038(4) C13 0.0242(5) 0.0231(4) 0.0240(4) -0.0013(3) 0.0040(3) 0.0012(3) C14 0.0322(5) 0.0313(5) 0.0291(5) -0.0066(4) 0.0088(4) 0.0006(4) C15 0.0217(4) 0.0185(4) 0.0208(4) -0.0014(3) 0.0005(3) 0.0003(3) C16 0.0220(4) 0.0184(4) 0.0194(4) -0.0004(3) -0.0005(3) 0.0026(3) C17 0.0229(4) 0.0216(4) 0.0214(4) -0.0009(3) 0.0022(3) 0.0020(3) C18 0.0277(5) 0.0292(5) 0.0262(5) -0.0005(4) 0.0076(4) 0.0025(4) C19 0.0278(5) 0.0394(6) 0.0350(6) -0.0024(5) 0.0115(4) -0.0038(5) C20 0.0245(5) 0.0336(5) 0.0329(5) -0.0020(4) 0.0047(4) -0.0048(4) C21 0.0443(7) 0.0396(6) 0.0318(6) -0.0074(5) 0.0169(5) -0.0015(5) C22 0.0355(7) 0.0503(8) 0.0488(8) -0.0117(6) 0.0090(6) -0.0199(6) C23 0.0279(5) 0.0203(4) 0.0287(5) -0.0019(3) -0.0032(4) -0.0002(4) C24 0.1170(17) 0.0553(10) 0.0381(7) -0.0186(7) -0.0341(9) 0.0489(11) C25 0.0319(5) 0.0247(5) 0.0353(5) 0.0010(4) -0.0069(4) 0.0022(4) C26 0.0432(7) 0.0323(6) 0.0382(6) 0.0032(5) 0.0011(5) 0.0130(5) C27 0.0254(5) 0.0258(4) 0.0240(4) -0.0037(3) -0.0028(4) 0.0020(4) C28 0.0435(7) 0.0280(5) 0.0476(7) -0.0026(5) -0.0088(6) 0.0066(5) C29 0.0239(5) 0.0312(5) 0.0278(5) 0.0015(4) -0.0016(4) 0.0032(4) C30 0.0283(6) 0.0491(7) 0.0350(6) 0.0089(5) -0.0074(5) 0.0005(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 110.18(4) N1 Al1 C27 112.30(5) N2 Al1 N1 93.85(4) N2 Al1 C23 112.74(5) N2 Al1 C27 111.04(5) C27 Al1 C23 114.89(5) C13 N1 Al1 125.11(7) C13 N1 C15 107.59(8) C15 N1 Al1 127.25(7) C17 N2 Al1 126.95(7) C20 N2 Al1 125.30(8) C20 N2 C17 107.46(9) C2 C1 C7 120.78(11) C6 C1 C2 118.03(10) C6 C1 C7 121.18(11) C1 C2 H2 119.0 C3 C2 C1 121.98(10) C3 C2 H2 119.0 C2 C3 C4 118.95(9) C2 C3 C8 120.29(9) C4 C3 C8 120.75(9) C3 C4 C5 120.12(9) C3 C4 C16 119.59(9) C5 C4 C16 120.28(8) C4 C5 C9 120.86(9) C6 C5 C4 119.10(9) C6 C5 C9 120.04(9) C1 C6 C5 121.80(10) C1 C6 H6 119.1 C5 C6 H6 119.1 C1 C7 H7A 109.5 C1 C7 H7B 109.5 C1 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C3 C8 H8A 109.5 C3 C8 H8B 109.5 C3 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C5 C9 H9A 109.5 C5 C9 H9B 109.5 C5 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 C12 C11 C10 123.34(10) C12 C11 C15 106.06(9) C15 C11 C10 130.60(10) C11 C12 H12 125.9 C11 C12 C13 108.27(10) C13 C12 H12 125.9 N1 C13 C12 110.22(9) N1 C13 C14 122.67(10) C12 C13 C14 127.11(10) 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 C11 107.85(9) C16 C15 N1 122.80(9) C16 C15 C11 129.34(9) C15 C16 C4 117.78(9) C15 C16 C17 125.86(9) C17 C16 C4 116.37(9) N2 C17 C16 122.79(9) N2 C17 C18 107.93(9) C16 C17 C18 129.25(10) C17 C18 C21 130.99(11) C19 C18 C17 106.03(10) C19 C18 C21 122.93(10) C18 C19 H19 125.9 C18 C19 C20 108.25(10) C20 C19 H19 125.9 N2 C20 C19 110.31(10) N2 C20 C22 122.90(11) C19 C20 C22 126.79(11) C18 C21 H21A 109.5 C18 C21 H21B 109.5 C18 C21 H21C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 Al1 C23 H23A 107.9 Al1 C23 H23B 107.9 H23A C23 H23B 107.2 C25 C23 Al1 117.57(7) C25 C23 H23A 107.9 C25 C23 H23B 107.9 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C25 C24 H24A 109.5 C25 C24 H24B 109.5 C25 C24 H24C 109.5 C23 C25 H25 108.0 C23 C25 C26 112.66(10) C24 C25 C23 110.56(12) C24 C25 H25 108.0 C24 C25 C26 109.41(11) C26 C25 H25 108.0 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 Al1 C27 H27A 107.8 Al1 C27 H27B 107.8 H27A C27 H27B 107.1 C29 C27 Al1 118.18(7) C29 C27 H27A 107.8 C29 C27 H27B 107.8 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C29 C28 H28A 109.5 C29 C28 H28B 109.5 C29 C28 H28C 109.5 C27 C29 H29 107.8 C28 C29 C27 111.72(9) C28 C29 H29 107.8 C28 C29 C30 110.11(10) C30 C29 C27 111.48(10) C30 C29 H29 107.8 C29 C30 H30A 109.5 C29 C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 N1 1.9098(9) Al1 N2 1.9091(10) Al1 C23 1.9835(11) Al1 C27 1.9779(12) N1 C13 1.3443(14) N1 C15 1.4076(12) N2 C17 1.4068(13) N2 C20 1.3445(14) C1 C2 1.3931(16) C1 C6 1.3915(16) C1 C7 1.5081(16) C2 H2 0.9500 C2 C3 1.3920(14) C3 C4 1.4023(14) C3 C8 1.5057(15) C4 C5 1.4034(14) C4 C16 1.4971(13) C5 C6 1.3928(14) C5 C9 1.5082(15) C6 H6 0.9500 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9801 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 1.4995(15) C11 C12 1.3807(15) C11 C15 1.4420(14) C12 H12 0.9500 C12 C13 1.4051(15) C13 C14 1.4948(15) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.4023(14) C16 C17 1.4099(14) C17 C18 1.4375(15) C18 C19 1.3824(17) C18 C21 1.4992(16) C19 H19 0.9500 C19 C20 1.4000(17) C20 C22 1.4958(17) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9900 C23 H23B 0.9900 C23 C25 1.5265(16) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C24 C25 1.520(2) C25 H25 1.0000 C25 C26 1.5289(17) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9900 C27 H27B 0.9900 C27 C29 1.5354(15) C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C28 C29 1.5259(18) C29 H29 1.0000 C29 C30 1.5291(16) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 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 C13 C12 -177.19(7) Al1 N1 C13 C14 2.96(14) Al1 N1 C15 C11 177.34(7) Al1 N1 C15 C16 -3.74(13) Al1 N2 C17 C16 -8.75(14) Al1 N2 C17 C18 172.88(7) Al1 N2 C20 C19 -173.61(8) Al1 N2 C20 C22 5.92(17) Al1 C23 C25 C24 -63.03(14) Al1 C23 C25 C26 174.20(9) Al1 C27 C29 C28 -58.71(13) Al1 C27 C29 C30 177.62(8) N1 C15 C16 C4 -177.43(8) N1 C15 C16 C17 2.63(15) N2 C17 C18 C19 1.31(12) N2 C17 C18 C21 -176.15(12) C1 C2 C3 C4 0.81(18) C1 C2 C3 C8 -179.00(11) C2 C1 C6 C5 -0.42(19) C2 C3 C4 C5 -1.51(16) C2 C3 C4 C16 177.24(10) C3 C4 C5 C6 1.26(16) C3 C4 C5 C9 -179.10(11) C3 C4 C16 C15 85.18(12) C3 C4 C16 C17 -94.88(12) C4 C5 C6 C1 -0.28(18) C4 C16 C17 N2 -176.18(9) C4 C16 C17 C18 1.81(15) C5 C4 C16 C15 -96.06(12) C5 C4 C16 C17 83.88(12) C6 C1 C2 C3 0.15(19) C7 C1 C2 C3 179.38(13) C7 C1 C6 C5 -179.65(13) C8 C3 C4 C5 178.29(10) C8 C3 C4 C16 -2.95(16) C9 C5 C6 C1 -179.93(12) C10 C11 C12 C13 -179.26(10) C10 C11 C15 N1 179.46(11) C10 C11 C15 C16 0.63(19) C11 C12 C13 N1 -0.48(13) C11 C12 C13 C14 179.37(11) C11 C15 C16 C4 1.25(15) C11 C15 C16 C17 -178.69(10) C12 C11 C15 N1 -0.08(11) C12 C11 C15 C16 -178.92(10) C13 N1 C15 C11 -0.21(11) C13 N1 C15 C16 178.72(9) C15 N1 C13 C12 0.42(12) C15 N1 C13 C14 -179.43(10) C15 C11 C12 C13 0.33(12) C15 C16 C17 N2 3.75(15) C15 C16 C17 C18 -178.25(10) C16 C4 C5 C6 -177.49(10) C16 C4 C5 C9 2.16(16) C16 C17 C18 C19 -176.92(11) C16 C17 C18 C21 5.6(2) C17 N2 C20 C19 0.53(13) C17 N2 C20 C22 -179.93(12) C17 C18 C19 C20 -0.99(14) C18 C19 C20 N2 0.31(15) C18 C19 C20 C22 -179.21(13) C20 N2 C17 C16 177.23(10) C20 N2 C17 C18 -1.14(12) C21 C18 C19 C20 176.73(12)