#------------------------------------------------------------------------------ #$Date: 2017-12-26 07:21:00 +0200 (Tue, 26 Dec 2017) $ #$Revision: 204518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/85/1548544.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_1548544 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 'C24 H31 Al N2' _chemical_formula_sum 'C24 H31 Al N2' _chemical_formula_weight 374.49 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-04-13 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324) ; _audit_update_record ; 2017-04-13 deposited with the CCDC. 2017-12-26 downloaded from the CCDC. ; _cell_angle_alpha 76.92(3) _cell_angle_beta 86.12(3) _cell_angle_gamma 85.20(3) _cell_formula_units_Z 2 _cell_length_a 7.0719(14) _cell_length_b 11.897(2) _cell_length_c 15.148(3) _cell_measurement_reflns_used 15490 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 31.507 _cell_measurement_theta_min 1.983 _cell_volume 1235.5(4) _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 293.15 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.971 _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 0.0311 _diffrn_reflns_av_unetI/netI 0.0672 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 15469 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.507 _diffrn_reflns_theta_min 1.983 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.007 _exptl_crystal_description block _exptl_crystal_F_000 404 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.317 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 7995 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.951 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0478 _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^)+(0.0665P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1236 _refine_ls_wR_factor_ref 0.1336 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4851 _reflns_number_total 7995 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7py01915g2.cif _cod_data_source_block bo4474 _cod_original_cell_volume 1235.5(5) _cod_database_code 1548544 _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 0.986 _shelx_estimated_absorpt_t_min 0.981 _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.a Aromatic/amide H refined with riding coordinates: C3(H3), C10(H10), C12(H12), C20(H20) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B, H23C), C24(H24A,H24B,H24C) ; _shelx_res_file ; bo4474.res created by SHELXL-2014/7 TITL bo4474 in P-1 CELL 0.71073 7.0719 11.8969 15.1483 76.924 86.12 85.202 ZERR 2 0.0014 0.0024 0.003 0.03 0.03 0.03 LATT 1 SFAC C H N Al UNIT 48 62 4 2 L.S. 4 PLAN 20 SIZE 0.21 0.18 0.15 TEMP 20 BOND BOND $H CONF fmap 2 acta OMIT 0 2 4 OMIT 1 -3 2 OMIT 2 1 5 OMIT 2 -1 2 OMIT 0 -3 6 OMIT 0 -3 1 REM REM REM WGHT 0.066500 FVAR 66.03095 AL1 4 0.593403 0.411457 0.265400 11.00000 0.03300 0.02146 = 0.03008 -0.00556 -0.00202 -0.00001 N1 3 0.581860 0.534027 0.159889 11.00000 0.02614 0.02335 = 0.02917 -0.00830 0.00078 -0.00058 N2 3 0.425288 0.492219 0.337349 11.00000 0.03022 0.02433 = 0.02653 -0.00323 -0.00006 -0.00330 C1 1 0.788859 0.427192 0.062149 11.00000 0.03911 0.03333 = 0.04342 -0.01666 0.00580 0.00095 AFIX 137 H1A 2 0.902620 0.416970 0.095094 11.00000 -1.50000 H1B 2 0.821858 0.437376 -0.001551 11.00000 -1.50000 H1C 2 0.717214 0.360174 0.082116 11.00000 -1.50000 AFIX 0 C2 1 0.672349 0.531198 0.078880 11.00000 0.02587 0.02931 = 0.03013 -0.01136 0.00142 -0.00265 C3 1 0.640450 0.637775 0.018163 11.00000 0.02985 0.03384 = 0.02363 -0.00714 0.00186 -0.00440 AFIX 43 H3 2 0.687013 0.656475 -0.041861 11.00000 -1.20000 AFIX 0 C4 1 0.528077 0.710488 0.062503 11.00000 0.02634 0.02752 = 0.02553 -0.00459 -0.00200 -0.00287 C5 1 0.471389 0.834068 0.018677 11.00000 0.04451 0.03399 = 0.02983 0.00149 0.00361 0.00374 AFIX 137 H5A 2 0.518672 0.884418 0.052149 11.00000 -1.50000 H5B 2 0.335373 0.845132 0.018480 11.00000 -1.50000 H5C 2 0.523911 0.851593 -0.042593 11.00000 -1.50000 AFIX 0 C6 1 0.488178 0.644284 0.152750 11.00000 0.02449 0.02234 = 0.02529 -0.00664 -0.00176 -0.00091 C7 1 0.374261 0.675801 0.224289 11.00000 0.02166 0.02213 = 0.02621 -0.00663 -0.00205 -0.00246 C8 1 0.274845 0.793919 0.204257 11.00000 0.02514 0.02373 = 0.02384 -0.00617 0.00338 -0.00181 C9 1 0.098883 0.810322 0.164687 11.00000 0.02636 0.02772 = 0.02967 -0.00848 -0.00055 0.00069 C10 1 0.013043 0.921785 0.141315 11.00000 0.02769 0.03493 = 0.03711 -0.00675 -0.00184 0.00531 AFIX 43 H10 2 -0.102816 0.933055 0.113852 11.00000 -1.20000 AFIX 0 C11 1 0.094649 1.016637 0.157646 11.00000 0.04027 0.02562 = 0.04025 -0.00440 0.00396 0.00576 C12 1 0.267381 0.997754 0.199160 11.00000 0.04044 0.02239 = 0.03712 -0.00727 0.00313 -0.00358 AFIX 43 H12 2 0.322969 1.060308 0.211479 11.00000 -1.20000 AFIX 0 C13 1 0.359602 0.887903 0.222837 11.00000 0.03011 0.02478 = 0.02787 -0.00701 0.00244 -0.00313 C14 1 0.002341 0.709523 0.147363 11.00000 0.03089 0.03932 = 0.05049 -0.01763 -0.00835 -0.00043 AFIX 137 H14A 2 0.077411 0.676285 0.103231 11.00000 -1.50000 H14B 2 -0.121052 0.735914 0.124924 11.00000 -1.50000 H14C 2 -0.010760 0.652239 0.202910 11.00000 -1.50000 AFIX 0 C15 1 0.000672 1.136974 0.131211 11.00000 0.05923 0.03267 = 0.06676 -0.00214 -0.00387 0.01441 AFIX 137 H15A 2 0.030567 1.168817 0.068206 11.00000 -1.50000 H15B 2 0.046041 1.184839 0.167317 11.00000 -1.50000 H15C 2 -0.134483 1.133958 0.141262 11.00000 -1.50000 AFIX 0 C16 1 0.546262 0.871362 0.268256 11.00000 0.03751 0.03387 = 0.04503 -0.01194 -0.00530 -0.00792 AFIX 137 H16A 2 0.524247 0.845122 0.332598 11.00000 -1.50000 H16B 2 0.605084 0.943531 0.255761 11.00000 -1.50000 H16C 2 0.628317 0.814902 0.245331 11.00000 -1.50000 AFIX 0 C17 1 0.341223 0.605475 0.310812 11.00000 0.02654 0.02331 = 0.02686 -0.00607 0.00004 -0.00217 C18 1 0.219617 0.629863 0.385262 11.00000 0.03150 0.03226 = 0.02748 -0.00940 0.00284 -0.00422 C19 1 0.097951 0.737007 0.394268 11.00000 0.04614 0.04433 = 0.03544 -0.01246 0.00960 0.00446 AFIX 137 H19A 2 0.175532 0.801689 0.383576 11.00000 -1.50000 H19B 2 0.039209 0.726005 0.454331 11.00000 -1.50000 H19C 2 0.001471 0.751700 0.350643 11.00000 -1.50000 AFIX 0 C20 1 0.234094 0.531512 0.453614 11.00000 0.03701 0.03981 = 0.02604 -0.00631 0.00617 -0.00895 AFIX 43 H20 2 0.171856 0.521553 0.510638 11.00000 -1.20000 AFIX 0 C21 1 0.358646 0.448871 0.422656 11.00000 0.03540 0.03107 = 0.02799 -0.00298 -0.00075 -0.00797 C22 1 0.410625 0.328974 0.472687 11.00000 0.05011 0.03555 = 0.03528 0.00301 -0.00051 -0.00726 AFIX 137 H22A 2 0.325521 0.277322 0.458798 11.00000 -1.50000 H22B 2 0.401467 0.325661 0.536732 11.00000 -1.50000 H22C 2 0.538492 0.306425 0.454877 11.00000 -1.50000 AFIX 0 C23 1 0.853028 0.387116 0.309238 11.00000 0.04099 0.04266 = 0.04129 -0.00994 -0.00580 0.00593 AFIX 137 H23A 2 0.937059 0.356585 0.266540 11.00000 -1.50000 H23B 2 0.853564 0.333412 0.367030 11.00000 -1.50000 H23C 2 0.894912 0.459496 0.315495 11.00000 -1.50000 AFIX 0 C24 1 0.472212 0.275904 0.247302 11.00000 0.05470 0.02990 = 0.03939 -0.00698 -0.00079 -0.00901 AFIX 137 H24A 2 0.343928 0.298405 0.230201 11.00000 -1.50000 H24B 2 0.471708 0.217616 0.302690 11.00000 -1.50000 H24C 2 0.541885 0.245570 0.200187 11.00000 -1.50000 AFIX 0 HKLF 4 REM bo4474 in P-1 REM R1 = 0.0478 for 4851 Fo > 4sig(Fo) and 0.0737 for all 7995 data REM 253 parameters refined using 0 restraints END WGHT 0.0667 0.0000 REM Highest difference peak 0.317, deepest hole -0.174, 1-sigma level 0.050 Q1 1 0.3172 0.7407 0.2126 11.00000 0.05 0.32 Q2 1 0.5596 0.6694 0.0422 11.00000 0.05 0.28 Q3 1 0.2868 0.6318 0.3400 11.00000 0.05 0.28 Q4 1 0.5496 0.3286 0.2635 11.00000 0.05 0.27 Q5 1 0.4852 0.6814 0.1178 11.00000 0.05 0.26 Q6 1 0.6514 0.5843 0.0510 11.00000 0.05 0.26 Q7 1 0.7501 0.3789 0.2688 11.00000 0.05 0.26 Q8 1 0.3755 0.5434 0.3292 11.00000 0.05 0.24 Q9 1 0.5821 0.1992 0.2791 11.00000 0.05 0.24 Q10 1 0.4883 0.4550 0.3096 11.00000 0.05 0.23 Q11 1 0.4935 0.7616 0.0462 11.00000 0.05 0.23 Q12 1 0.3313 0.8372 0.2085 11.00000 0.05 0.23 Q13 1 0.8303 0.3646 0.1187 11.00000 0.05 0.23 Q14 1 0.5436 0.5924 0.1567 11.00000 0.05 0.22 Q15 1 0.7286 0.4830 0.0789 11.00000 0.05 0.22 Q16 1 0.2325 0.5901 0.4205 11.00000 0.05 0.22 Q17 1 0.0564 0.8591 0.1470 11.00000 0.05 0.22 Q18 1 0.3850 0.4764 0.3517 11.00000 0.05 0.22 Q19 1 0.3126 0.9415 0.2142 11.00000 0.05 0.22 Q20 1 0.6817 0.6428 0.0033 11.00000 0.05 0.21 ; _shelx_res_checksum 45291 _platon_squeeze_void_probe_radius 1.20 _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 Al1 Al 0.59340(6) 0.41146(3) 0.26540(3) 0.02829(11) Uani 1 1 d . N1 N 0.58186(14) 0.53403(8) 0.15989(7) 0.0260(2) Uani 1 1 d . N2 N 0.42529(14) 0.49222(9) 0.33735(7) 0.0274(2) Uani 1 1 d . C1 C 0.7889(2) 0.42719(12) 0.06215(10) 0.0379(3) Uani 1 1 d . H1A H 0.9026 0.4170 0.0951 0.057 Uiso 1 1 calc GR H1B H 0.8219 0.4374 -0.0016 0.057 Uiso 1 1 calc GR H1C H 0.7172 0.3602 0.0821 0.057 Uiso 1 1 calc GR C2 C 0.67235(17) 0.53120(11) 0.07888(9) 0.0278(3) Uani 1 1 d . C3 C 0.64045(18) 0.63778(11) 0.01816(9) 0.0290(3) Uani 1 1 d . H3 H 0.6870 0.6565 -0.0419 0.035 Uiso 1 1 calc R C4 C 0.52808(17) 0.71049(11) 0.06250(8) 0.0266(3) Uani 1 1 d . C5 C 0.4714(2) 0.83407(12) 0.01868(10) 0.0381(3) Uani 1 1 d . H5A H 0.5187 0.8844 0.0521 0.057 Uiso 1 1 calc GR H5B H 0.3354 0.8451 0.0185 0.057 Uiso 1 1 calc GR H5C H 0.5239 0.8516 -0.0426 0.057 Uiso 1 1 calc GR C6 C 0.48818(16) 0.64428(10) 0.15275(8) 0.0238(2) Uani 1 1 d . C7 C 0.37426(16) 0.67580(10) 0.22429(8) 0.0230(2) Uani 1 1 d . C8 C 0.27485(17) 0.79392(10) 0.20426(8) 0.0243(2) Uani 1 1 d . C9 C 0.09888(17) 0.81032(11) 0.16469(9) 0.0278(3) Uani 1 1 d . C10 C 0.01304(19) 0.92178(12) 0.14132(10) 0.0339(3) Uani 1 1 d . H10 H -0.1028 0.9331 0.1139 0.041 Uiso 1 1 calc R C11 C 0.0946(2) 1.01664(11) 0.15765(10) 0.0366(3) Uani 1 1 d . C12 C 0.26738(19) 0.99775(11) 0.19916(9) 0.0334(3) Uani 1 1 d . H12 H 0.3230 1.0603 0.2115 0.040 Uiso 1 1 calc R C13 C 0.35960(17) 0.88790(10) 0.22284(9) 0.0275(3) Uani 1 1 d . C14 C 0.00234(19) 0.70952(13) 0.14736(11) 0.0388(3) Uani 1 1 d . H14A H 0.0774 0.6763 0.1032 0.058 Uiso 1 1 calc GR H14B H -0.1211 0.7359 0.1249 0.058 Uiso 1 1 calc GR H14C H -0.0108 0.6522 0.2029 0.058 Uiso 1 1 calc GR C15 C 0.0007(2) 1.13697(13) 0.13121(13) 0.0553(5) Uani 1 1 d . H15A H 0.0306 1.1688 0.0682 0.083 Uiso 1 1 calc GR H15B H 0.0460 1.1848 0.1673 0.083 Uiso 1 1 calc GR H15C H -0.1345 1.1340 0.1413 0.083 Uiso 1 1 calc GR C16 C 0.54626(19) 0.87136(12) 0.26826(10) 0.0378(3) Uani 1 1 d . H16A H 0.5242 0.8451 0.3326 0.057 Uiso 1 1 calc GR H16B H 0.6051 0.9435 0.2558 0.057 Uiso 1 1 calc GR H16C H 0.6283 0.8149 0.2453 0.057 Uiso 1 1 calc GR C17 C 0.34122(17) 0.60548(10) 0.31081(8) 0.0255(3) Uani 1 1 d . C18 C 0.21962(18) 0.62986(11) 0.38526(9) 0.0301(3) Uani 1 1 d . C19 C 0.0980(2) 0.73701(13) 0.39427(10) 0.0424(4) Uani 1 1 d . H19A H 0.1755 0.8017 0.3836 0.064 Uiso 1 1 calc GR H19B H 0.0392 0.7260 0.4543 0.064 Uiso 1 1 calc GR H19C H 0.0015 0.7517 0.3506 0.064 Uiso 1 1 calc GR C20 C 0.2341(2) 0.53151(12) 0.45361(9) 0.0344(3) Uani 1 1 d . H20 H 0.1719 0.5216 0.5106 0.041 Uiso 1 1 calc R C21 C 0.35865(19) 0.44887(11) 0.42266(9) 0.0318(3) Uani 1 1 d . C22 C 0.4106(2) 0.32897(12) 0.47269(10) 0.0419(4) Uani 1 1 d . H22A H 0.3255 0.2773 0.4588 0.063 Uiso 1 1 calc GR H22B H 0.4015 0.3257 0.5367 0.063 Uiso 1 1 calc GR H22C H 0.5385 0.3064 0.4549 0.063 Uiso 1 1 calc GR C23 C 0.8530(2) 0.38712(13) 0.30924(11) 0.0419(3) Uani 1 1 d . H23A H 0.9371 0.3566 0.2665 0.063 Uiso 1 1 calc GR H23B H 0.8536 0.3334 0.3670 0.063 Uiso 1 1 calc GR H23C H 0.8949 0.4595 0.3155 0.063 Uiso 1 1 calc GR C24 C 0.4722(2) 0.27590(12) 0.24730(10) 0.0412(3) Uani 1 1 d . H24A H 0.3439 0.2984 0.2302 0.062 Uiso 1 1 calc GR H24B H 0.4717 0.2176 0.3027 0.062 Uiso 1 1 calc GR H24C H 0.5419 0.2456 0.2002 0.062 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 0.0330(2) 0.02146(18) 0.0301(2) -0.00556(14) -0.00202(16) -0.00001(15) N1 0.0261(5) 0.0233(5) 0.0292(6) -0.0083(4) 0.0008(4) -0.0006(4) N2 0.0302(6) 0.0243(5) 0.0265(5) -0.0032(4) -0.0001(4) -0.0033(4) C1 0.0391(8) 0.0333(7) 0.0434(8) -0.0167(6) 0.0058(6) 0.0010(6) C2 0.0259(6) 0.0293(6) 0.0301(7) -0.0114(5) 0.0014(5) -0.0027(5) C3 0.0298(6) 0.0338(7) 0.0236(6) -0.0071(5) 0.0019(5) -0.0044(5) C4 0.0263(6) 0.0275(6) 0.0255(6) -0.0046(5) -0.0020(5) -0.0029(5) C5 0.0445(8) 0.0340(7) 0.0298(7) 0.0015(5) 0.0036(6) 0.0037(6) C6 0.0245(6) 0.0223(5) 0.0253(6) -0.0066(4) -0.0018(5) -0.0009(4) C7 0.0217(5) 0.0221(5) 0.0262(6) -0.0066(4) -0.0021(5) -0.0025(4) C8 0.0251(6) 0.0237(5) 0.0238(6) -0.0062(4) 0.0034(5) -0.0018(5) C9 0.0264(6) 0.0277(6) 0.0297(6) -0.0085(5) -0.0005(5) 0.0007(5) C10 0.0277(6) 0.0349(7) 0.0371(8) -0.0068(6) -0.0018(6) 0.0053(5) C11 0.0403(8) 0.0256(6) 0.0403(8) -0.0044(5) 0.0040(6) 0.0058(6) C12 0.0404(8) 0.0224(6) 0.0371(8) -0.0073(5) 0.0031(6) -0.0036(5) C13 0.0301(6) 0.0248(6) 0.0279(6) -0.0070(5) 0.0024(5) -0.0031(5) C14 0.0309(7) 0.0393(8) 0.0505(9) -0.0176(7) -0.0084(6) -0.0004(6) C15 0.0592(10) 0.0327(8) 0.0668(12) -0.0021(7) -0.0039(9) 0.0144(7) C16 0.0375(8) 0.0339(7) 0.0450(9) -0.0119(6) -0.0053(6) -0.0079(6) C17 0.0265(6) 0.0233(5) 0.0269(6) -0.0061(5) 0.0000(5) -0.0022(5) C18 0.0315(7) 0.0323(6) 0.0275(7) -0.0094(5) 0.0028(5) -0.0042(5) C19 0.0461(9) 0.0443(8) 0.0354(8) -0.0125(6) 0.0096(7) 0.0045(7) C20 0.0370(7) 0.0398(7) 0.0260(7) -0.0063(5) 0.0062(6) -0.0090(6) C21 0.0354(7) 0.0311(6) 0.0280(7) -0.0030(5) -0.0007(5) -0.0080(6) C22 0.0501(9) 0.0356(7) 0.0353(8) 0.0030(6) -0.0005(7) -0.0073(7) C23 0.0410(8) 0.0427(8) 0.0413(8) -0.0099(6) -0.0058(7) 0.0059(6) C24 0.0547(9) 0.0299(7) 0.0394(8) -0.0070(6) -0.0008(7) -0.0090(6) 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 N2 94.12(5) N1 Al1 C23 110.03(6) N1 Al1 C24 111.10(6) N2 Al1 C23 111.98(6) N2 Al1 C24 109.24(6) C24 Al1 C23 117.85(7) C2 N1 Al1 125.18(9) C2 N1 C6 107.69(11) C6 N1 Al1 127.06(9) C17 N2 Al1 126.99(8) C21 N2 Al1 125.80(9) C21 N2 C17 107.17(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 N1 C2 C1 122.38(12) N1 C2 C3 109.92(12) C3 C2 C1 127.69(13) C2 C3 H3 125.8 C4 C3 C2 108.40(11) C4 C3 H3 125.8 C3 C4 C5 122.95(12) C3 C4 C6 106.22(11) C6 C4 C5 130.81(12) 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 N1 C6 C4 107.76(11) N1 C6 C7 122.76(11) C7 C6 C4 129.46(11) C6 C7 C8 116.31(11) C17 C7 C6 126.05(11) C17 C7 C8 117.60(11) C9 C8 C7 119.35(11) C9 C8 C13 120.35(11) C13 C8 C7 120.28(11) C8 C9 C14 121.04(12) C10 C9 C8 118.83(12) C10 C9 C14 120.12(12) C9 C10 H10 118.9 C11 C10 C9 122.11(13) C11 C10 H10 118.9 C10 C11 C12 117.99(12) C10 C11 C15 121.47(14) C12 C11 C15 120.54(13) C11 C12 H12 119.0 C11 C12 C13 121.91(12) C13 C12 H12 119.0 C8 C13 C16 121.14(12) C12 C13 C8 118.76(12) C12 C13 C16 120.10(12) C9 C14 H14A 109.5 C9 C14 H14B 109.5 C9 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C11 C15 H15A 109.5 C11 C15 H15B 109.5 C11 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C13 C16 H16A 109.5 C13 C16 H16B 109.5 C13 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 N2 C17 C18 108.20(11) C7 C17 N2 122.82(11) C7 C17 C18 128.97(12) C17 C18 C19 130.70(12) C20 C18 C17 105.92(12) C20 C18 C19 123.37(13) 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 108.47(12) C21 C20 H20 125.8 N2 C21 C20 110.24(12) N2 C21 C22 122.84(13) C20 C21 C22 126.91(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 109.5 Al1 C23 H23B 109.5 Al1 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 Al1 C24 H24A 109.5 Al1 C24 H24B 109.5 Al1 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 N1 1.9055(13) Al1 N2 1.9058(13) Al1 C23 1.9710(15) Al1 C24 1.9681(15) N1 C2 1.3511(16) N1 C6 1.4040(16) N2 C17 1.4085(16) N2 C21 1.3471(16) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C1 C2 1.4890(18) C2 C3 1.3989(18) C3 H3 0.9300 C3 C4 1.3808(18) C4 C5 1.5029(18) C4 C6 1.4376(17) C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 C6 C7 1.4068(17) C7 C8 1.4939(17) C7 C17 1.4027(17) C8 C9 1.3976(18) C8 C13 1.4021(17) C9 C10 1.3908(18) C9 C14 1.5089(19) C10 H10 0.9300 C10 C11 1.386(2) C11 C12 1.390(2) C11 C15 1.506(2) C12 H12 0.9300 C12 C13 1.3924(18) C13 C16 1.5076(19) C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 C18 1.4390(18) C18 C19 1.504(2) C18 C20 1.3776(19) C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 H20 0.9300 C20 C21 1.404(2) C21 C22 1.4849(19) C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 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 C2 C1 2.24(17) Al1 N1 C2 C3 -176.94(8) Al1 N1 C6 C4 176.20(8) Al1 N1 C6 C7 -5.23(16) Al1 N2 C17 C7 -0.54(17) Al1 N2 C17 C18 177.99(8) Al1 N2 C21 C20 -178.31(9) Al1 N2 C21 C22 0.26(18) N1 C2 C3 C4 0.65(14) N1 C6 C7 C8 -176.46(10) N1 C6 C7 C17 1.31(19) N2 C17 C18 C19 179.44(13) N2 C17 C18 C20 -0.01(14) C1 C2 C3 C4 -178.47(12) C2 N1 C6 C4 -0.74(13) C2 N1 C6 C7 177.83(11) C2 C3 C4 C5 177.65(12) C2 C3 C4 C6 -1.08(13) C3 C4 C6 N1 1.12(13) C3 C4 C6 C7 -177.32(12) C4 C6 C7 C8 1.79(18) C4 C6 C7 C17 179.55(12) C5 C4 C6 N1 -177.47(13) C5 C4 C6 C7 4.1(2) C6 N1 C2 C1 179.25(11) C6 N1 C2 C3 0.07(14) C6 C7 C8 C9 85.71(14) C6 C7 C8 C13 -92.65(14) C6 C7 C17 N2 1.64(19) C6 C7 C17 C18 -176.56(12) C7 C8 C9 C10 -176.16(11) C7 C8 C9 C14 3.88(18) C7 C8 C13 C12 176.84(11) C7 C8 C13 C16 -3.66(18) C7 C17 C18 C19 -2.1(2) C7 C17 C18 C20 178.40(13) C8 C7 C17 N2 179.38(10) C8 C7 C17 C18 1.18(19) C8 C9 C10 C11 -1.3(2) C9 C8 C13 C12 -1.51(18) C9 C8 C13 C16 177.99(11) C9 C10 C11 C12 -0.3(2) C9 C10 C11 C15 179.48(14) C10 C11 C12 C13 1.0(2) C11 C12 C13 C8 -0.14(19) C11 C12 C13 C16 -179.65(12) C13 C8 C9 C10 2.21(18) C13 C8 C9 C14 -177.75(12) C14 C9 C10 C11 178.67(13) C15 C11 C12 C13 -178.75(14) C17 N2 C21 C20 -0.75(14) C17 N2 C21 C22 177.82(12) C17 C7 C8 C9 -92.24(14) C17 C7 C8 C13 89.39(14) C17 C18 C20 C21 -0.44(15) C18 C20 C21 N2 0.76(16) C18 C20 C21 C22 -177.74(13) C19 C18 C20 C21 -179.94(12) C21 N2 C17 C7 -178.06(11) C21 N2 C17 C18 0.46(14) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.029 0.000 0.500 218 43 ' ' 2 0.166 0.457 0.149 13 0 ' ' 3 0.230 0.364 0.658 12 -1 ' ' 4 0.769 0.636 0.342 11 -1 ' ' 5 0.833 0.543 0.851 13 0 ' '