#------------------------------------------------------------------------------ #$Date: 2019-05-18 05:06:48 +0300 (Sat, 18 May 2019) $ #$Revision: 215292 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700017.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_7700017 loop_ _publ_author_name 'Zhu, Hongping' 'Chen, Yilin' 'Jiang, Wenjun' 'Li, Bin' 'Fu, Gang' 'Chen, Shimin' _publ_section_title ; Reaction of an N/Al FLP-Based Aluminum Hydride toward Alkyne: Deprotonated Alumination versus Hydroalumination with Regioselective cis-Addition Character ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT00903E _journal_year 2019 _chemical_formula_sum 'C27 H28 Al N S2' _chemical_formula_weight 457.60 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-05-13 deposited with the CCDC. 2019-05-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.0988(9) _cell_length_b 8.7010(3) _cell_length_c 11.4918(5) _cell_measurement_reflns_used 1949 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.0970 _cell_measurement_theta_min 2.5020 _cell_volume 2409.64(16) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 16.1903 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Sapphire 3, Gemini ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_unetI/netI 0.0520 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 7072 _diffrn_reflns_point_group_measured_fraction_full 0.891 _diffrn_reflns_point_group_measured_fraction_max 0.882 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.998 _diffrn_reflns_theta_min 2.449 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_T_max 0.9475 _exptl_absorpt_correction_T_min 0.8989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.empirical' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.214 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr. _refine_ls_matrix_type full _refine_ls_number_parameters 330 _refine_ls_number_reflns 4642 _refine_ls_number_restraints 291 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0457 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.5322P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.1081 _reflns_Friedel_coverage 0.682 _reflns_Friedel_fraction_full 0.772 _reflns_Friedel_fraction_max 0.754 _reflns_number_gt 4115 _reflns_number_total 4642 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00903e2.cif _cod_data_source_block cyl-171129 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7700017 _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_min 0.899 _shelx_estimated_absorpt_t_max 0.948 _shelx_res_file ; cyl-171129.res created by SHELXL-2014/7 TITL cyl-171129 in Pna2(1) CELL 0.71073 24.0988 8.7010 11.4918 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0003 0.0005 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N AL S UNIT 108 112 4 4 8 temp -100 size 0.40 0.20 0.20 omit 0 54 omit 1 1 -4 omit 9 1 -1 omit 8 0 0 omit 0 1 -1 omit 0 1 1 omit 4 0 2 omit 8 2 -3 omit 0 0 -4 simu 0.02 0.02 10 c9 c10 c11 c12 s2 c9a c10a c11a c12a s2a delu 0.01 c9 > s2a free al1 c18 L.S. 18 BOND bond $H acta FMAP 2 PLAN 20 WGHT 0.048800 0.532200 FVAR 5.84885 0.66961 AL1 4 0.161415 0.126367 0.892434 11.00000 0.02303 0.02436 = 0.02321 0.00033 0.00207 0.00362 N1 3 0.191462 -0.085664 0.831134 11.00000 0.02141 0.02116 = 0.01887 0.00044 -0.00069 0.00046 C1 1 0.108660 0.232133 0.794415 11.00000 0.02355 0.02734 = 0.03208 0.00121 0.00329 0.00328 C2 1 0.082162 0.316820 0.731665 11.00000 0.02418 0.02901 = 0.03920 0.00163 0.00338 -0.00074 C3 1 0.054607 0.417031 0.653366 11.00000 0.02651 0.02915 = 0.04001 0.00296 -0.00438 0.00472 C4 1 0.075932 0.477512 0.548188 11.00000 0.03568 0.02616 = 0.02392 0.00043 -0.00130 0.00703 AFIX 43 H4A 2 0.111770 0.456452 0.517664 11.00000 -1.20000 AFIX 0 C5 1 0.035451 0.575308 0.494469 11.00000 0.06398 0.04519 = 0.03522 0.00632 -0.00843 0.00425 AFIX 43 H5A 2 0.041942 0.627680 0.423221 11.00000 -1.20000 AFIX 0 C6 1 -0.011503 0.586182 0.552514 11.00000 0.04653 0.07769 = 0.08899 0.04388 -0.00324 0.02788 AFIX 43 H6A 2 -0.042322 0.645536 0.527268 11.00000 -1.20000 AFIX 0 S1 5 -0.010780 0.482810 0.676822 11.00000 0.04606 0.12852 = 0.10700 0.07557 0.03230 0.04340 C7 1 0.131724 0.120354 1.049377 11.00000 0.03859 0.03566 = 0.02700 -0.00086 0.00547 0.00877 C8 1 0.109389 0.106344 1.142547 11.00000 0.03718 0.03254 = 0.03211 0.00026 0.00569 0.00736 PART 2 C9 1 0.079887 0.077061 1.253038 21.00000 0.03059 0.02792 = 0.02336 0.00678 0.00830 0.01001 C10 1 0.096727 0.128429 1.363617 21.00000 0.05958 0.05371 = 0.03551 0.00136 0.01022 -0.00928 AFIX 43 H10A 2 0.129452 0.184412 1.381718 21.00000 -1.20000 AFIX 0 C11 1 0.053725 0.078339 1.445197 21.00000 0.04139 0.05046 = 0.02657 0.00319 0.00148 0.00175 AFIX 43 H11A 2 0.051562 0.108514 1.524516 21.00000 -1.20000 AFIX 0 C12 1 0.015416 -0.022519 1.388502 21.00000 0.02793 0.03639 = 0.04012 0.00951 -0.00015 -0.00432 AFIX 43 H12A 2 -0.014833 -0.069856 1.427561 21.00000 -1.20000 AFIX 0 S2 5 0.028093 -0.048062 1.254360 21.00000 0.02738 0.04346 = 0.03908 0.00002 0.00404 -0.00853 PART 1 C9A 1 0.082888 0.081877 1.242183 -21.00000 0.04237 0.04060 = 0.02784 -0.00819 0.00689 -0.00502 C10A 1 0.034726 -0.012208 1.246703 -21.00000 0.05362 0.05675 = 0.02888 0.00566 0.00345 -0.01250 AFIX 43 H10B 2 0.015959 -0.064796 1.185877 -21.00000 -1.20000 AFIX 0 C11A 1 0.040010 0.103134 1.439713 -21.00000 0.05144 0.04504 = 0.03308 -0.00101 0.00786 -0.00591 AFIX 43 H11B 2 0.028521 0.148848 1.510815 -21.00000 -1.20000 AFIX 0 C12A 1 0.018667 -0.003686 1.404988 -21.00000 0.04383 0.04703 = 0.02152 -0.00407 0.00967 0.00191 AFIX 43 H12B 2 -0.003086 -0.074687 1.448151 -21.00000 -1.20000 AFIX 0 S2A 5 0.090762 0.175844 1.364567 -21.00000 0.08220 0.06365 = 0.03599 -0.01192 0.02194 -0.02416 PART 0 C13 1 0.240170 0.148113 0.857803 11.00000 0.02325 0.02600 = 0.01965 0.00204 -0.00452 0.00095 C14 1 0.286814 0.243041 0.852014 11.00000 0.03406 0.02755 = 0.02550 0.00272 -0.00905 -0.00256 AFIX 43 H14A 2 0.284263 0.347353 0.875836 11.00000 -1.20000 AFIX 0 C15 1 0.336742 0.185383 0.811629 11.00000 0.02580 0.04506 = 0.03798 0.01169 -0.00321 -0.01084 AFIX 43 H15A 2 0.368476 0.250069 0.809045 11.00000 -1.20000 AFIX 0 C16 1 0.340827 0.035072 0.775158 11.00000 0.01907 0.05050 = 0.04137 0.00808 0.00265 0.00274 AFIX 43 H16A 2 0.375347 -0.002268 0.746976 11.00000 -1.20000 AFIX 0 C17 1 0.295477 -0.062669 0.778840 11.00000 0.02725 0.03221 = 0.03901 0.00212 0.00333 0.00430 AFIX 43 H17A 2 0.298305 -0.166391 0.753713 11.00000 -1.20000 AFIX 0 C18 1 0.245507 -0.003502 0.820728 11.00000 0.02074 0.02550 = 0.02137 0.00191 -0.00153 0.00241 C19 1 0.168810 -0.136983 0.710465 11.00000 0.03042 0.02380 = 0.01909 -0.00031 -0.00347 -0.00119 C20 1 0.196289 -0.288139 0.669711 11.00000 0.03563 0.03144 = 0.02632 -0.00651 0.00018 0.00249 AFIX 23 H20A 2 0.177469 -0.323861 0.598070 11.00000 -1.20000 H20B 2 0.235547 -0.267234 0.649876 11.00000 -1.20000 AFIX 0 C21 1 0.194209 -0.415094 0.759515 11.00000 0.04773 0.02250 = 0.03855 -0.00628 -0.00022 0.00349 AFIX 23 H21A 2 0.214242 -0.506358 0.729817 11.00000 -1.20000 H21B 2 0.155135 -0.444853 0.773644 11.00000 -1.20000 AFIX 0 C22 1 0.220416 -0.362545 0.872663 11.00000 0.04487 0.02252 = 0.03238 0.00386 -0.00124 0.00406 AFIX 23 H22A 2 0.260381 -0.343157 0.859163 11.00000 -1.20000 H22B 2 0.217344 -0.446445 0.930497 11.00000 -1.20000 AFIX 0 C23 1 0.194001 -0.216714 0.923634 11.00000 0.03369 0.02238 = 0.02094 0.00506 -0.00026 -0.00061 C24 1 0.105626 -0.156078 0.716008 11.00000 0.03087 0.03529 = 0.03114 -0.00127 -0.00591 -0.00668 AFIX 137 H24A 2 0.089218 -0.066481 0.754563 11.00000 -1.50000 H24B 2 0.096524 -0.249145 0.760085 11.00000 -1.50000 H24C 2 0.090745 -0.164814 0.636921 11.00000 -1.50000 AFIX 0 C25 1 0.181962 -0.013558 0.619995 11.00000 0.03693 0.03233 = 0.02202 0.00123 -0.00048 0.00061 AFIX 137 H25A 2 0.166012 0.084701 0.644870 11.00000 -1.50000 H25B 2 0.166030 -0.043236 0.544821 11.00000 -1.50000 H25C 2 0.222280 -0.002977 0.612270 11.00000 -1.50000 AFIX 0 C26 1 0.229085 -0.163859 1.027358 11.00000 0.04087 0.03364 = 0.02430 0.00528 -0.00628 0.00606 AFIX 137 H26A 2 0.228952 -0.243789 1.087440 11.00000 -1.50000 H26B 2 0.213478 -0.068818 1.059343 11.00000 -1.50000 H26C 2 0.267265 -0.145161 1.001641 11.00000 -1.50000 AFIX 0 C27 1 0.135356 -0.253749 0.969036 11.00000 0.04032 0.03221 = 0.02763 0.00516 0.00622 -0.00432 AFIX 137 H27A 2 0.138181 -0.313903 1.040889 11.00000 -1.50000 H27B 2 0.115127 -0.313140 0.910292 11.00000 -1.50000 H27C 2 0.115454 -0.157763 0.984807 11.00000 -1.50000 AFIX 0 HKLF 4 REM cyl-171129 in Pna2(1) REM R1 = 0.0457 for 4115 Fo > 4sig(Fo) and 0.0548 for all 4642 data REM 330 parameters refined using 291 restraints END WGHT 0.0469 0.5356 REM Highest difference peak 0.214, deepest hole -0.370, 1-sigma level 0.046 Q1 1 0.0286 0.4585 0.6819 11.00000 0.05 0.21 Q2 1 0.0234 0.4259 0.6491 11.00000 0.05 0.21 Q3 1 -0.0177 0.3732 0.6482 11.00000 0.05 0.21 Q4 1 -0.0273 0.5758 0.6255 11.00000 0.05 0.19 Q5 1 0.0909 0.4857 0.5397 11.00000 0.05 0.19 Q6 1 0.2066 -0.2819 0.8974 11.00000 0.05 0.18 Q7 1 0.0568 0.4464 0.5846 11.00000 0.05 0.18 Q8 1 0.0705 0.4950 0.6095 11.00000 0.05 0.18 Q9 1 0.0014 0.6269 0.6569 11.00000 0.05 0.18 Q10 1 0.1834 -0.2214 0.6936 11.00000 0.05 0.18 Q11 1 0.0622 0.5289 0.5381 11.00000 0.05 0.17 Q12 1 0.1835 -0.1211 0.7694 11.00000 0.05 0.17 Q13 1 0.0025 0.5061 0.5020 11.00000 0.05 0.17 Q14 1 0.1624 -0.2253 0.9405 11.00000 0.05 0.17 Q15 1 0.0799 0.1234 1.3076 11.00000 0.05 0.16 Q16 1 0.0092 0.1627 1.2502 11.00000 0.05 0.16 Q17 1 0.1937 -0.1666 0.8721 11.00000 0.05 0.16 Q18 1 0.1186 0.0606 1.3801 11.00000 0.05 0.16 Q19 1 0.1455 0.0820 0.9806 11.00000 0.05 0.16 Q20 1 0.2126 0.1540 0.8859 11.00000 0.05 0.16 ; _shelx_res_checksum 18896 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.16142(4) 0.12637(11) 0.89243(10) 0.0235(2) Uani 1 1 d . . . . . N1 N 0.19146(11) -0.0857(3) 0.8311(2) 0.0205(6) Uani 1 1 d . . . . . C1 C 0.10866(14) 0.2321(4) 0.7944(3) 0.0277(8) Uani 1 1 d . . . . . C2 C 0.08216(15) 0.3168(4) 0.7317(4) 0.0308(8) Uani 1 1 d . . . . . C3 C 0.05461(15) 0.4170(4) 0.6534(4) 0.0319(8) Uani 1 1 d . . . . . C4 C 0.07593(16) 0.4775(4) 0.5482(3) 0.0286(8) Uani 1 1 d . . . . . H4A H 0.1118 0.4565 0.5177 0.034 Uiso 1 1 calc R U . . . C5 C 0.0355(2) 0.5753(5) 0.4945(4) 0.0481(11) Uani 1 1 d . . . . . H5A H 0.0419 0.6277 0.4232 0.058 Uiso 1 1 calc R U . . . C6 C -0.0115(2) 0.5862(7) 0.5525(6) 0.0711(18) Uani 1 1 d . . . . . H6A H -0.0423 0.6455 0.5273 0.085 Uiso 1 1 calc R U . . . S1 S -0.01078(6) 0.4828(2) 0.67682(18) 0.0939(7) Uani 1 1 d . . . . . C7 C 0.13172(17) 0.1204(4) 1.0494(3) 0.0337(8) Uani 1 1 d . . . . . C8 C 0.10939(16) 0.1063(4) 1.1425(4) 0.0339(9) Uani 1 1 d . . . . . C9 C 0.0799(10) 0.077(3) 1.2530(19) 0.027(2) Uani 0.670(6) 1 d . U P A 2 C10 C 0.0967(9) 0.1284(16) 1.3636(19) 0.050(3) Uani 0.670(6) 1 d . U P A 2 H10A H 0.1295 0.1844 1.3817 0.060 Uiso 0.670(6) 1 calc R U P A 2 C11 C 0.0537(4) 0.0783(16) 1.4452(14) 0.039(2) Uani 0.670(6) 1 d . U P A 2 H11A H 0.0516 0.1085 1.5245 0.047 Uiso 0.670(6) 1 calc R U P A 2 C12 C 0.0154(8) -0.023(2) 1.3885(15) 0.035(3) Uani 0.670(6) 1 d . U P A 2 H12A H -0.0148 -0.0699 1.4276 0.042 Uiso 0.670(6) 1 calc R U P A 2 S2 S 0.02809(12) -0.0481(3) 1.2544(3) 0.0366(6) Uani 0.670(6) 1 d . U P A 2 C9A C 0.083(2) 0.082(7) 1.242(4) 0.037(4) Uani 0.330(6) 1 d . U P A 1 C10A C 0.0347(13) -0.012(3) 1.247(3) 0.046(4) Uani 0.330(6) 1 d . U P A 1 H10B H 0.0160 -0.0648 1.1859 0.056 Uiso 0.330(6) 1 calc R U P A 1 C11A C 0.0400(11) 0.103(4) 1.440(3) 0.043(4) Uani 0.330(6) 1 d . U P A 1 H11B H 0.0285 0.1488 1.5108 0.052 Uiso 0.330(6) 1 calc R U P A 1 C12A C 0.019(2) -0.004(5) 1.405(3) 0.037(4) Uani 0.330(6) 1 d . U P A 1 H12B H -0.0031 -0.0747 1.4482 0.045 Uiso 0.330(6) 1 calc R U P A 1 S2A S 0.0908(5) 0.1758(9) 1.3646(10) 0.061(2) Uani 0.330(6) 1 d . U P A 1 C13 C 0.24017(14) 0.1481(4) 0.8578(3) 0.0230(7) Uani 1 1 d . . . . . C14 C 0.28681(15) 0.2430(4) 0.8520(3) 0.0290(8) Uani 1 1 d . . . . . H14A H 0.2843 0.3474 0.8758 0.035 Uiso 1 1 calc R U . . . C15 C 0.33674(15) 0.1854(5) 0.8116(4) 0.0363(9) Uani 1 1 d . . . . . H15A H 0.3685 0.2501 0.8090 0.044 Uiso 1 1 calc R U . . . C16 C 0.34083(15) 0.0351(5) 0.7752(4) 0.0370(9) Uani 1 1 d . . . . . H16A H 0.3753 -0.0023 0.7470 0.044 Uiso 1 1 calc R U . . . C17 C 0.29548(14) -0.0627(4) 0.7788(4) 0.0328(8) Uani 1 1 d . . . . . H17A H 0.2983 -0.1664 0.7537 0.039 Uiso 1 1 calc R U . . . C18 C 0.24551(14) -0.0035(4) 0.8207(3) 0.0225(7) Uani 1 1 d . . . . . C19 C 0.16881(15) -0.1370(4) 0.7105(3) 0.0244(7) Uani 1 1 d . . . . . C20 C 0.19629(16) -0.2881(4) 0.6697(3) 0.0311(8) Uani 1 1 d . . . . . H20A H 0.1775 -0.3239 0.5981 0.037 Uiso 1 1 calc R U . . . H20B H 0.2355 -0.2672 0.6499 0.037 Uiso 1 1 calc R U . . . C21 C 0.19421(18) -0.4151(4) 0.7595(4) 0.0363(9) Uani 1 1 d . . . . . H21A H 0.2142 -0.5064 0.7298 0.044 Uiso 1 1 calc R U . . . H21B H 0.1551 -0.4449 0.7736 0.044 Uiso 1 1 calc R U . . . C22 C 0.22042(17) -0.3625(4) 0.8727(4) 0.0333(9) Uani 1 1 d . . . . . H22A H 0.2604 -0.3432 0.8592 0.040 Uiso 1 1 calc R U . . . H22B H 0.2173 -0.4464 0.9305 0.040 Uiso 1 1 calc R U . . . C23 C 0.19400(15) -0.2167(4) 0.9236(3) 0.0257(8) Uani 1 1 d . . . . . C24 C 0.10563(15) -0.1561(4) 0.7160(3) 0.0324(8) Uani 1 1 d . . . . . H24A H 0.0892 -0.0665 0.7546 0.049 Uiso 1 1 calc R U . . . H24B H 0.0965 -0.2491 0.7601 0.049 Uiso 1 1 calc R U . . . H24C H 0.0907 -0.1648 0.6369 0.049 Uiso 1 1 calc R U . . . C25 C 0.18196(16) -0.0136(4) 0.6200(3) 0.0304(8) Uani 1 1 d . . . . . H25A H 0.1660 0.0847 0.6449 0.046 Uiso 1 1 calc R U . . . H25B H 0.1660 -0.0432 0.5448 0.046 Uiso 1 1 calc R U . . . H25C H 0.2223 -0.0030 0.6123 0.046 Uiso 1 1 calc R U . . . C26 C 0.22908(17) -0.1639(4) 1.0274(3) 0.0329(8) Uani 1 1 d . . . . . H26A H 0.2290 -0.2438 1.0874 0.049 Uiso 1 1 calc R U . . . H26B H 0.2135 -0.0688 1.0593 0.049 Uiso 1 1 calc R U . . . H26C H 0.2673 -0.1452 1.0016 0.049 Uiso 1 1 calc R U . . . C27 C 0.13536(17) -0.2537(4) 0.9690(3) 0.0334(9) Uani 1 1 d . . . . . H27A H 0.1382 -0.3139 1.0409 0.050 Uiso 1 1 calc R U . . . H27B H 0.1151 -0.3131 0.9103 0.050 Uiso 1 1 calc R U . . . H27C H 0.1155 -0.1578 0.9848 0.050 Uiso 1 1 calc R U . . . 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 0.0230(5) 0.0244(5) 0.0232(5) 0.0003(5) 0.0021(4) 0.0036(4) N1 0.0214(13) 0.0212(12) 0.0189(14) 0.0004(11) -0.0007(11) 0.0005(11) C1 0.0235(16) 0.0273(17) 0.0321(19) 0.0012(15) 0.0033(15) 0.0033(15) C2 0.0242(16) 0.0290(16) 0.039(2) 0.0016(17) 0.0034(16) -0.0007(15) C3 0.0265(18) 0.0291(18) 0.040(2) 0.0030(17) -0.0044(17) 0.0047(15) C4 0.036(2) 0.0262(16) 0.0239(18) 0.0004(15) -0.0013(16) 0.0070(16) C5 0.064(3) 0.045(2) 0.035(2) 0.006(2) -0.008(2) 0.004(2) C6 0.047(3) 0.078(4) 0.089(4) 0.044(4) -0.003(3) 0.028(3) S1 0.0461(7) 0.1285(14) 0.1070(14) 0.0756(12) 0.0323(8) 0.0434(9) C7 0.039(2) 0.0357(19) 0.027(2) -0.0009(17) 0.0055(17) 0.0088(18) C8 0.037(2) 0.0325(19) 0.032(2) 0.0003(17) 0.0057(18) 0.0074(17) C9 0.031(4) 0.028(4) 0.023(5) 0.007(3) 0.008(4) 0.010(3) C10 0.060(5) 0.054(7) 0.036(5) 0.001(5) 0.010(4) -0.009(6) C11 0.041(5) 0.050(5) 0.027(3) 0.003(4) 0.001(4) 0.002(4) C12 0.028(4) 0.036(5) 0.040(6) 0.010(5) 0.000(4) -0.004(3) S2 0.0274(10) 0.0435(13) 0.0391(12) 0.0000(12) 0.0040(9) -0.0085(9) C9A 0.042(8) 0.041(8) 0.028(7) -0.008(7) 0.007(6) -0.005(7) C10A 0.054(8) 0.057(9) 0.029(6) 0.006(7) 0.003(7) -0.012(6) C11A 0.051(8) 0.045(8) 0.033(6) -0.001(6) 0.008(7) -0.006(7) C12A 0.044(8) 0.047(8) 0.022(7) -0.004(6) 0.010(6) 0.002(6) S2A 0.082(4) 0.064(4) 0.036(3) -0.012(3) 0.022(3) -0.024(4) C13 0.0233(16) 0.0260(15) 0.0196(16) 0.0020(13) -0.0045(13) 0.0009(14) C14 0.0341(19) 0.0275(17) 0.0255(18) 0.0027(15) -0.0090(15) -0.0026(16) C15 0.0258(18) 0.045(2) 0.038(2) 0.0117(19) -0.0032(17) -0.0108(18) C16 0.0191(16) 0.050(2) 0.041(2) 0.008(2) 0.0026(16) 0.0027(17) C17 0.0273(18) 0.0322(18) 0.039(2) 0.0021(17) 0.0033(17) 0.0043(16) C18 0.0207(16) 0.0255(15) 0.0214(17) 0.0019(14) -0.0015(13) 0.0024(14) C19 0.0304(17) 0.0238(16) 0.0191(17) -0.0003(14) -0.0035(14) -0.0012(15) C20 0.0356(19) 0.0314(18) 0.0263(19) -0.0065(15) 0.0002(16) 0.0025(17) C21 0.048(2) 0.0225(16) 0.039(2) -0.0063(17) -0.0002(19) 0.0035(17) C22 0.045(2) 0.0225(15) 0.032(2) 0.0039(15) -0.0012(18) 0.0041(16) C23 0.0337(19) 0.0224(16) 0.0209(18) 0.0051(13) -0.0003(14) -0.0006(15) C24 0.0309(18) 0.0353(19) 0.031(2) -0.0013(17) -0.0059(16) -0.0067(17) C25 0.0369(19) 0.0323(18) 0.0220(18) 0.0012(15) -0.0005(16) 0.0006(17) C26 0.041(2) 0.0336(18) 0.0243(19) 0.0053(16) -0.0063(16) 0.0061(17) C27 0.040(2) 0.0322(18) 0.028(2) 0.0052(16) 0.0062(16) -0.0043(17) 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' S S 0.1246 0.1234 '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 C1 Al1 C7 108.18(16) C1 Al1 C13 118.40(15) C7 Al1 C13 123.47(17) C1 Al1 N1 116.69(15) C7 Al1 N1 114.49(14) C13 Al1 N1 71.42(13) C18 N1 C19 111.9(3) C18 N1 C23 111.8(3) C19 N1 C23 114.3(2) C18 N1 Al1 84.66(18) C19 N1 Al1 115.43(19) C23 N1 Al1 115.2(2) C2 C1 Al1 169.3(3) C1 C2 C3 175.9(4) C4 C3 C2 126.9(3) C4 C3 S1 110.3(3) C2 C3 S1 122.8(3) C3 C4 C5 110.0(4) C3 C4 H4A 125.0 C5 C4 H4A 125.0 C6 C5 C4 114.1(4) C6 C5 H5A 122.9 C4 C5 H5A 122.9 C5 C6 S1 112.4(4) C5 C6 H6A 123.8 S1 C6 H6A 123.8 C6 S1 C3 93.1(2) C8 C7 Al1 173.4(4) C7 C8 C9A 176(3) C7 C8 C9 175.2(12) C10 C9 C8 126(2) C10 C9 S2 114.7(15) C8 C9 S2 118.9(17) C9 C10 C11 106.2(17) C9 C10 H10A 126.9 C11 C10 H10A 126.9 C12 C11 C10 110.4(15) C12 C11 H11A 124.8 C10 C11 H11A 124.8 C11 C12 S2 113.8(13) C11 C12 H12A 123.1 S2 C12 H12A 123.1 C12 S2 C9 93.6(10) C8 C9A C10A 121(4) C8 C9A S2A 127(4) C10A C9A S2A 111(3) C9A C10A C12A 101(3) C9A C10A H10B 129.7 C12A C10A H10B 129.7 C12A C11A S2A 118(3) C12A C11A H11B 120.9 S2A C11A H11B 120.9 C11A C12A C10A 106(3) C11A C12A H12B 126.8 C10A C12A H12B 126.8 C11A S2A C9A 100(2) C18 C13 C14 118.1(3) C18 C13 Al1 93.5(2) C14 C13 Al1 148.3(3) C15 C14 C13 120.1(3) C15 C14 H14A 120.0 C13 C14 H14A 120.0 C16 C15 C14 120.6(4) C16 C15 H15A 119.7 C14 C15 H15A 119.7 C15 C16 C17 121.2(4) C15 C16 H16A 119.4 C17 C16 H16A 119.4 C16 C17 C18 117.7(4) C16 C17 H17A 121.1 C18 C17 H17A 121.1 C13 C18 C17 122.3(3) C13 C18 N1 110.4(3) C17 C18 N1 127.2(3) C25 C19 C24 108.1(3) C25 C19 C20 107.6(3) C24 C19 C20 110.2(3) C25 C19 N1 109.4(3) C24 C19 N1 110.0(3) C20 C19 N1 111.4(3) C21 C20 C19 113.6(3) C21 C20 H20A 108.8 C19 C20 H20A 108.8 C21 C20 H20B 108.8 C19 C20 H20B 108.8 H20A C20 H20B 107.7 C20 C21 C22 110.6(3) C20 C21 H21A 109.5 C22 C21 H21A 109.5 C20 C21 H21B 109.5 C22 C21 H21B 109.5 H21A C21 H21B 108.1 C21 C22 C23 113.8(3) C21 C22 H22A 108.8 C23 C22 H22A 108.8 C21 C22 H22B 108.8 C23 C22 H22B 108.8 H22A C22 H22B 107.7 C26 C23 C22 108.4(3) C26 C23 C27 107.8(3) C22 C23 C27 109.7(3) C26 C23 N1 109.4(3) C22 C23 N1 111.1(3) C27 C23 N1 110.3(3) C19 C24 H24A 109.5 C19 C24 H24B 109.5 H24A C24 H24B 109.5 C19 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C19 C25 H25A 109.5 C19 C25 H25B 109.5 H25A C25 H25B 109.5 C19 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C23 C26 H26A 109.5 C23 C26 H26B 109.5 H26A C26 H26B 109.5 C23 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C23 C27 H27A 109.5 C23 C27 H27B 109.5 H27A C27 H27B 109.5 C23 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al1 C1 1.932(4) Al1 C7 1.941(4) Al1 C13 1.948(4) Al1 N1 2.103(3) N1 C18 1.491(4) N1 C19 1.556(4) N1 C23 1.560(4) C1 C2 1.213(5) C2 C3 1.418(5) C3 C4 1.415(6) C3 S1 1.698(4) C4 C5 1.434(6) C4 H4A 0.9500 C5 C6 1.317(7) C5 H5A 0.9500 C6 S1 1.688(6) C6 H6A 0.9500 C7 C8 1.205(5) C8 C9A 1.33(5) C8 C9 1.48(2) C9 C10 1.41(3) C9 S2 1.66(3) C10 C11 1.46(3) C10 H10A 0.9500 C11 C12 1.43(2) C11 H11A 0.9500 C12 S2 1.587(19) C12 H12A 0.9500 C9A C10A 1.42(6) C9A S2A 1.64(6) C10A C12A 1.86(5) C10A H10B 0.9500 C11A C12A 1.13(5) C11A S2A 1.63(3) C11A H11B 0.9500 C12A H12B 0.9500 C13 C18 1.392(5) C13 C14 1.396(5) C14 C15 1.384(6) C14 H14A 0.9500 C15 C16 1.377(6) C15 H15A 0.9500 C16 C17 1.385(5) C16 H16A 0.9500 C17 C18 1.395(5) C17 H17A 0.9500 C19 C25 1.528(5) C19 C24 1.533(5) C19 C20 1.545(5) C20 C21 1.513(5) C20 H20A 0.9900 C20 H20B 0.9900 C21 C22 1.516(6) C21 H21A 0.9900 C21 H21B 0.9900 C22 C23 1.536(5) C22 H22A 0.9900 C22 H22B 0.9900 C23 C26 1.532(5) C23 C27 1.541(5) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 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 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800