#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:28:56 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267144 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707507.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_7707507 loop_ _publ_author_name 'Dehmel, Maximilian' 'K\"ohler, Angelina' 'G\"orls, Helmar' 'Kretschmer, Robert' _publ_section_title ; Synthesis, characterization, and reactivity of group 13 hydride complexes based on amido-amine ligands. ; _journal_issue 24 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8434 _journal_page_last 8445 _journal_paper_doi 10.1039/d1dt01454d _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C19 H32 Al Cl N2' _chemical_formula_sum 'C19 H32 Al Cl N2' _chemical_formula_weight 350.89 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-04-21 deposited with the CCDC. 2021-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.7757(2) _cell_length_b 14.2425(2) _cell_length_c 7.5367(1) _cell_measurement_reflns_used 25371 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 74.458 _cell_measurement_theta_min 3.825 _cell_volume 2122.75(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Xcalibur, AtlasS2, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 25371 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.458 _diffrn_reflns_theta_min 3.825 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.985 _exptl_absorpt_correction_T_max 0.830 _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.362 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.105 _refine_diff_density_max 0.978 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.086 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.08(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 228 _refine_ls_number_reflns 4281 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0601 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+1.3506P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1827 _refine_ls_wR_factor_ref 0.1850 _reflns_Friedel_coverage 0.731 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.974 _reflns_number_gt 4077 _reflns_number_total 4281 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01454d2.cif _cod_data_source_block FO6946_7a _cod_depositor_comments 'Adding full bibliography for 7707498--7707509.cif.' _cod_database_code 7707507 _shelx_shelxl_version_number 2018/3 _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 0.533 _shelx_estimated_absorpt_t_max 0.819 _shelx_res_file ; TITL rk1772_abs_a.res in P2(1)2(1)2(1) fo6946.res created by SHELXL-2018/3 at 16:53:18 on 20-Apr-2021 CELL 1.54184 19.7757 14.2425 7.5367 90 90 90 ZERR 4 0.0002 0.0002 0.0001 0.0 0.0 0.0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Al Cl N UNIT 76 128 4 4 8 DFIX 1.5 0.0002 H1C1 Al1 DFIX 1.5 0.0002 H1C2 Al1 DFIX 1.5 0.0002 Al1 H1C1 Al1 H1C2 L.S. 4 PLAN 20 BOND $H TWIN fmap 2 acta TEMP -150 SIZE 0.362 0.153 0.105 REM COLOR:colourless WGHT 0.114400 1.350600 BASF 0.08084 FVAR 0.84569 AL1 3 0.608380 0.161453 0.295345 11.00000 0.04477 0.02719 = 0.02976 0.00268 0.00718 0.00577 PART 1 CL1 4 0.689581 0.159573 0.460903 10.34000 0.02330 0.02986 = 0.02077 -0.00097 -0.01017 0.01264 H1C1 2 0.577504 0.066961 0.329429 10.34000 -1.50000 PART 2 CL2 4 0.557943 0.029432 0.322194 10.66000 0.04318 0.00900 = 0.04096 0.00507 0.02534 -0.00240 H1C2 2 0.669030 0.156550 0.414509 10.66000 -1.50000 PART 0 N1 5 0.559552 0.267970 0.296976 11.00000 0.03800 0.02918 = 0.02430 -0.00015 0.00078 0.00370 N2 5 0.621694 0.176116 0.034712 11.00000 0.04726 0.02736 = 0.02842 -0.00286 0.00645 -0.00126 C1 1 0.540251 0.301329 0.121049 11.00000 0.05567 0.03470 = 0.02796 -0.00046 -0.00376 0.01386 AFIX 23 H1A 2 0.565794 0.358926 0.090787 11.00000 -1.20000 H1B 2 0.491343 0.316076 0.118006 11.00000 -1.20000 AFIX 0 C2 1 0.556515 0.223411 -0.010730 11.00000 0.06087 0.04215 = 0.02627 -0.00512 -0.00477 0.00796 AFIX 23 H2A 2 0.519541 0.176549 -0.010131 11.00000 -1.20000 H2B 2 0.559572 0.250212 -0.131664 11.00000 -1.20000 AFIX 0 C3 1 0.537533 0.322941 0.444642 11.00000 0.03669 0.02334 = 0.02701 0.00480 -0.00259 0.00476 C4 1 0.579331 0.395464 0.509838 11.00000 0.04020 0.02833 = 0.03147 -0.00201 -0.00236 0.00506 C5 1 0.557747 0.445569 0.660486 11.00000 0.04969 0.02969 = 0.03539 -0.00491 -0.00424 0.00337 AFIX 43 H5A 2 0.585641 0.493962 0.707052 11.00000 -1.20000 AFIX 0 C6 1 0.497409 0.426006 0.741247 11.00000 0.05657 0.03361 = 0.02921 -0.00437 0.00177 0.01346 AFIX 43 H6A 2 0.484180 0.459913 0.844097 11.00000 -1.20000 AFIX 0 C7 1 0.455616 0.356833 0.673198 11.00000 0.04229 0.03327 = 0.03162 0.00365 0.00370 0.00853 AFIX 43 H7A 2 0.413239 0.344857 0.728081 11.00000 -1.20000 AFIX 0 C8 1 0.474911 0.304372 0.524851 11.00000 0.03605 0.02637 = 0.02996 0.00489 0.00023 0.00801 C9 1 0.644363 0.423880 0.421227 11.00000 0.04299 0.03693 = 0.04028 -0.00104 -0.00240 -0.00324 AFIX 13 H9A 2 0.651801 0.380890 0.318154 11.00000 -1.20000 AFIX 0 C10 1 0.705885 0.417128 0.541199 11.00000 0.04258 0.09908 = 0.07169 0.00902 -0.00761 -0.01070 AFIX 137 H10A 2 0.746039 0.438458 0.476527 11.00000 -1.50000 H10B 2 0.712224 0.351802 0.578500 11.00000 -1.50000 H10C 2 0.699088 0.456768 0.645976 11.00000 -1.50000 AFIX 0 C11 1 0.637861 0.524918 0.348257 11.00000 0.07124 0.05438 = 0.10457 0.02609 0.02566 -0.00741 AFIX 137 H11A 2 0.679866 0.542552 0.287848 11.00000 -1.50000 H11B 2 0.629445 0.568399 0.446587 11.00000 -1.50000 H11C 2 0.600150 0.527855 0.264079 11.00000 -1.50000 AFIX 0 C12 1 0.427628 0.229954 0.453322 11.00000 0.03958 0.02863 = 0.03940 0.00428 0.00130 0.00045 AFIX 13 H12A 2 0.450900 0.198521 0.351597 11.00000 -1.20000 AFIX 0 C13 1 0.363115 0.273120 0.383196 11.00000 0.04425 0.04462 = 0.06403 0.00304 -0.01387 -0.00086 AFIX 137 H13A 2 0.333543 0.223495 0.337453 11.00000 -1.50000 H13B 2 0.373951 0.317184 0.287461 11.00000 -1.50000 H13C 2 0.340027 0.306665 0.479212 11.00000 -1.50000 AFIX 0 C14 1 0.412930 0.155331 0.592010 11.00000 0.05886 0.04035 = 0.05226 0.01291 -0.00326 -0.00754 AFIX 137 H14A 2 0.455319 0.125228 0.628074 11.00000 -1.50000 H14B 2 0.382401 0.108064 0.541888 11.00000 -1.50000 H14C 2 0.391586 0.184551 0.695560 11.00000 -1.50000 AFIX 0 C15 1 0.627413 0.087393 -0.071987 11.00000 0.06229 0.02645 = 0.03701 -0.00624 0.01296 -0.00241 AFIX 23 H15A 2 0.623942 0.102355 -0.199941 11.00000 -1.20000 H15B 2 0.589808 0.044558 -0.040909 11.00000 -1.20000 AFIX 0 C16 1 0.694778 0.039099 -0.035119 11.00000 0.06388 0.03460 = 0.06066 -0.00363 0.02001 0.00837 AFIX 23 H16A 2 0.696918 0.021162 0.091665 11.00000 -1.20000 H16B 2 0.697741 -0.019032 -0.106719 11.00000 -1.20000 AFIX 0 C17 1 0.754300 0.102001 -0.078930 11.00000 0.06103 0.04615 = 0.08030 -0.00775 0.03221 0.00279 AFIX 23 H17A 2 0.755638 0.113963 -0.208280 11.00000 -1.20000 H17B 2 0.796965 0.070480 -0.044669 11.00000 -1.20000 AFIX 0 C18 1 0.747787 0.194622 0.020303 11.00000 0.04849 0.05270 = 0.06664 -0.01148 0.02484 -0.01351 AFIX 23 H18A 2 0.784076 0.237799 -0.018820 11.00000 -1.20000 H18B 2 0.753618 0.183320 0.149006 11.00000 -1.20000 AFIX 0 C19 1 0.679313 0.240409 -0.012178 11.00000 0.05999 0.02997 = 0.04274 -0.00072 0.01875 -0.00699 AFIX 23 H19A 2 0.675965 0.298416 0.059666 11.00000 -1.20000 H19B 2 0.675725 0.258308 -0.138756 11.00000 -1.20000 AFIX 0 HKLF 4 REM rk1772_abs_a.res in P2(1)2(1)2(1) REM wR2 = 0.1850, GooF = S = 1.101, Restrained GooF = 1.100 for all data REM R1 = 0.0601 for 4077 Fo > 4sig(Fo) and 0.0622 for all 4281 data REM 228 parameters refined using 4 restraints END WGHT 0.1144 1.3506 REM Highest difference peak 0.978, deepest hole -0.490, 1-sigma level 0.086 Q1 1 0.5712 0.0336 0.3640 11.00000 0.05 0.92 Q2 1 0.5720 -0.0647 0.3464 11.00000 0.05 0.29 Q3 1 0.5504 -0.0749 0.2794 11.00000 0.05 0.28 Q4 1 0.5717 0.0582 -0.3603 11.00000 0.05 0.26 Q5 1 0.6875 0.1629 0.6698 11.00000 0.05 0.22 Q6 1 0.5649 0.1820 0.5223 11.00000 0.05 0.22 Q7 1 0.5546 0.1224 0.3114 11.00000 0.05 0.22 Q8 1 0.6741 0.6609 0.4616 11.00000 0.05 0.22 Q9 1 0.6878 0.1938 -0.2828 11.00000 0.05 0.21 Q10 1 0.6798 0.2990 0.5176 11.00000 0.05 0.21 Q11 1 0.6537 0.1945 0.6246 11.00000 0.05 0.20 Q12 1 0.5540 0.0634 -0.2698 11.00000 0.05 0.20 Q13 1 0.5465 0.0168 0.0595 11.00000 0.05 0.19 Q14 1 0.3374 0.1312 0.3426 11.00000 0.05 0.19 Q15 1 0.5758 0.0600 0.5239 11.00000 0.05 0.19 Q16 1 0.3105 0.1779 0.8114 11.00000 0.05 0.19 Q17 1 0.6615 0.5340 0.1740 11.00000 0.05 0.19 Q18 1 0.4637 0.3889 0.3180 11.00000 0.05 0.19 Q19 1 0.3219 0.2164 0.7680 11.00000 0.05 0.18 Q20 1 0.4568 0.1750 0.1934 11.00000 0.05 0.18 ; _shelx_res_checksum 44261 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.60838(7) 0.16145(9) 0.29535(17) 0.0339(4) Uani 1 1 d D . . . . Cl1 Cl 0.68958(12) 0.1596(2) 0.4609(3) 0.0246(5) Uani 0.34 1 d . . P A 1 H1C1 H 0.5775(7) 0.0670(5) 0.329(5) 0.037 Uiso 0.34 1 d D U P B 1 Cl2 Cl 0.55794(8) 0.02943(8) 0.3222(2) 0.0310(4) Uani 0.66 1 d . . P A 2 H1C2 H 0.6690(4) 0.157(6) 0.4145(12) 0.047 Uiso 0.66 1 d D U P C 2 N1 N 0.55955(19) 0.2680(2) 0.2970(5) 0.0305(8) Uani 1 1 d . . . . . N2 N 0.6217(2) 0.1761(3) 0.0347(5) 0.0343(8) Uani 1 1 d . . . . . C1 C 0.5403(3) 0.3013(3) 0.1210(6) 0.0394(11) Uani 1 1 d . . . . . H1A H 0.565794 0.358926 0.090787 0.047 Uiso 1 1 calc R U . . . H1B H 0.491343 0.316076 0.118006 0.047 Uiso 1 1 calc R U . . . C2 C 0.5565(3) 0.2234(4) -0.0107(6) 0.0431(12) Uani 1 1 d . . . . . H2A H 0.519541 0.176549 -0.010131 0.052 Uiso 1 1 calc R U . . . H2B H 0.559572 0.250212 -0.131664 0.052 Uiso 1 1 calc R U . . . C3 C 0.5375(2) 0.3229(3) 0.4446(6) 0.0290(9) Uani 1 1 d . . . . . C4 C 0.5793(2) 0.3955(3) 0.5098(6) 0.0333(9) Uani 1 1 d . . . . . C5 C 0.5577(3) 0.4456(3) 0.6605(7) 0.0383(10) Uani 1 1 d . . . . . H5A H 0.585641 0.493962 0.707052 0.046 Uiso 1 1 calc R U . . . C6 C 0.4974(3) 0.4260(4) 0.7412(7) 0.0398(11) Uani 1 1 d . . . . . H6A H 0.484180 0.459913 0.844097 0.048 Uiso 1 1 calc R U . . . C7 C 0.4556(2) 0.3568(3) 0.6732(6) 0.0357(10) Uani 1 1 d . . . . . H7A H 0.413239 0.344857 0.728081 0.043 Uiso 1 1 calc R U . . . C8 C 0.4749(2) 0.3044(3) 0.5249(6) 0.0308(9) Uani 1 1 d . . . . . C9 C 0.6444(3) 0.4239(3) 0.4212(7) 0.0401(11) Uani 1 1 d . . . . . H9A H 0.651801 0.380890 0.318154 0.048 Uiso 1 1 calc R U . . . C10 C 0.7059(3) 0.4171(6) 0.5412(11) 0.071(2) Uani 1 1 d . . . . . H10A H 0.746039 0.438458 0.476527 0.107 Uiso 1 1 calc R U . . . H10B H 0.712224 0.351802 0.578500 0.107 Uiso 1 1 calc R U . . . H10C H 0.699088 0.456768 0.645976 0.107 Uiso 1 1 calc R U . . . C11 C 0.6379(4) 0.5249(5) 0.3483(12) 0.077(2) Uani 1 1 d . . . . . H11A H 0.679866 0.542552 0.287848 0.115 Uiso 1 1 calc R U . . . H11B H 0.629445 0.568399 0.446587 0.115 Uiso 1 1 calc R U . . . H11C H 0.600150 0.527855 0.264079 0.115 Uiso 1 1 calc R U . . . C12 C 0.4276(2) 0.2300(3) 0.4533(7) 0.0359(10) Uani 1 1 d . . . . . H12A H 0.450900 0.198521 0.351597 0.043 Uiso 1 1 calc R U . . . C13 C 0.3631(3) 0.2731(4) 0.3832(9) 0.0510(13) Uani 1 1 d . . . . . H13A H 0.333543 0.223495 0.337453 0.076 Uiso 1 1 calc R U . . . H13B H 0.373951 0.317184 0.287461 0.076 Uiso 1 1 calc R U . . . H13C H 0.340027 0.306665 0.479212 0.076 Uiso 1 1 calc R U . . . C14 C 0.4129(3) 0.1553(4) 0.5920(8) 0.0505(13) Uani 1 1 d . . . . . H14A H 0.455319 0.125228 0.628074 0.076 Uiso 1 1 calc R U . . . H14B H 0.382401 0.108064 0.541888 0.076 Uiso 1 1 calc R U . . . H14C H 0.391586 0.184551 0.695560 0.076 Uiso 1 1 calc R U . . . C15 C 0.6274(3) 0.0874(3) -0.0720(7) 0.0419(12) Uani 1 1 d . . . . . H15A H 0.623942 0.102355 -0.199941 0.050 Uiso 1 1 calc R U . . . H15B H 0.589808 0.044558 -0.040909 0.050 Uiso 1 1 calc R U . . . C16 C 0.6948(3) 0.0391(4) -0.0351(9) 0.0530(14) Uani 1 1 d . . . . . H16A H 0.696918 0.021162 0.091665 0.064 Uiso 1 1 calc R U . . . H16B H 0.697741 -0.019032 -0.106719 0.064 Uiso 1 1 calc R U . . . C17 C 0.7543(3) 0.1020(4) -0.0789(11) 0.0625(18) Uani 1 1 d . . . . . H17A H 0.755638 0.113963 -0.208280 0.075 Uiso 1 1 calc R U . . . H17B H 0.796965 0.070480 -0.044669 0.075 Uiso 1 1 calc R U . . . C18 C 0.7478(3) 0.1946(4) 0.0203(9) 0.0559(16) Uani 1 1 d . . . . . H18A H 0.784076 0.237799 -0.018820 0.067 Uiso 1 1 calc R U . . . H18B H 0.753618 0.183320 0.149006 0.067 Uiso 1 1 calc R U . . . C19 C 0.6793(3) 0.2404(4) -0.0122(7) 0.0442(12) Uani 1 1 d . . . . . H19A H 0.675965 0.298416 0.059666 0.053 Uiso 1 1 calc R U . . . H19B H 0.675725 0.258308 -0.138756 0.053 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 0.0448(7) 0.0272(7) 0.0298(6) 0.0027(5) 0.0072(5) 0.0058(5) Cl1 0.0233(11) 0.0299(13) 0.0208(11) -0.0010(10) -0.0102(9) 0.0126(11) Cl2 0.0432(8) 0.0090(5) 0.0410(8) 0.0051(5) 0.0253(6) -0.0024(5) N1 0.0380(19) 0.0292(17) 0.0243(17) -0.0002(14) 0.0008(15) 0.0037(15) N2 0.047(2) 0.0274(19) 0.0284(18) -0.0029(15) 0.0065(15) -0.0013(15) C1 0.056(3) 0.035(2) 0.028(2) -0.0005(18) -0.004(2) 0.014(2) C2 0.061(3) 0.042(3) 0.026(2) -0.0051(19) -0.005(2) 0.008(2) C3 0.037(2) 0.0233(19) 0.0270(19) 0.0048(16) -0.0026(16) 0.0048(16) C4 0.040(2) 0.028(2) 0.031(2) -0.0020(17) -0.0024(18) 0.0051(18) C5 0.050(3) 0.030(2) 0.035(2) -0.0049(18) -0.004(2) 0.0034(19) C6 0.057(3) 0.034(2) 0.029(2) -0.0044(19) 0.002(2) 0.013(2) C7 0.042(2) 0.033(2) 0.032(2) 0.0037(19) 0.0037(18) 0.0085(18) C8 0.036(2) 0.026(2) 0.030(2) 0.0049(17) 0.0002(17) 0.0080(17) C9 0.043(3) 0.037(2) 0.040(2) -0.001(2) -0.002(2) -0.003(2) C10 0.043(3) 0.099(6) 0.072(4) 0.009(4) -0.008(3) -0.011(3) C11 0.071(4) 0.054(4) 0.105(6) 0.026(4) 0.026(4) -0.007(3) C12 0.040(2) 0.029(2) 0.039(2) 0.0043(19) 0.0013(19) 0.0005(18) C13 0.044(3) 0.045(3) 0.064(3) 0.003(3) -0.014(3) -0.001(2) C14 0.059(3) 0.040(3) 0.052(3) 0.013(3) -0.003(2) -0.008(2) C15 0.062(3) 0.026(2) 0.037(2) -0.0062(19) 0.013(2) -0.002(2) C16 0.064(3) 0.035(3) 0.061(3) -0.004(2) 0.020(3) 0.008(2) C17 0.061(3) 0.046(3) 0.080(5) -0.008(3) 0.032(3) 0.003(3) C18 0.048(3) 0.053(3) 0.067(4) -0.011(3) 0.025(3) -0.014(3) C19 0.060(3) 0.030(2) 0.043(3) -0.001(2) 0.019(2) -0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 N2 89.39(17) . . ? N1 Al1 Cl1 115.52(16) . . ? N2 Al1 Cl1 120.12(16) . . ? N1 Al1 Cl2 119.39(14) . . ? N2 Al1 Cl2 104.30(13) . . ? N1 Al1 H1C1 122.5(6) . . ? N2 Al1 H1C1 108.5(13) . . ? Cl1 Al1 H1C1 101.8(11) . . ? N1 Al1 H1C2 118(3) . . ? N2 Al1 H1C2 119.3(5) . . ? Cl2 Al1 H1C2 106(3) . . ? C3 N1 C1 116.7(3) . . ? C3 N1 Al1 129.1(3) . . ? C1 N1 Al1 114.1(3) . . ? C2 N2 C15 108.8(4) . . ? C2 N2 C19 109.0(4) . . ? C15 N2 C19 109.2(4) . . ? C2 N2 Al1 99.2(3) . . ? C15 N2 Al1 116.7(3) . . ? C19 N2 Al1 113.3(3) . . ? N1 C1 C2 107.5(4) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 111.2(4) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C8 C3 C4 120.3(4) . . ? C8 C3 N1 120.1(4) . . ? C4 C3 N1 119.6(4) . . ? C5 C4 C3 118.3(4) . . ? C5 C4 C9 118.7(4) . . ? C3 C4 C9 122.9(4) . . ? C6 C5 C4 121.3(5) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C8 120.9(4) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C7 C8 C3 119.0(4) . . ? C7 C8 C12 119.4(4) . . ? C3 C8 C12 121.6(4) . . ? C4 C9 C10 113.8(5) . . ? C4 C9 C11 109.7(5) . . ? C10 C9 C11 109.7(6) . . ? C4 C9 H9A 107.8 . . ? C10 C9 H9A 107.8 . . ? C11 C9 H9A 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C8 111.2(4) . . ? C13 C12 C14 111.3(4) . . ? C8 C12 C14 111.3(4) . . ? C13 C12 H12A 107.6 . . ? C8 C12 H12A 107.6 . . ? C14 C12 H12A 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 110.3(4) . . ? N2 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N2 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 111.8(5) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 109.9(5) . . ? C16 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C17 C18 C19 111.6(5) . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C18 112.0(4) . . ? N2 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? N2 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.798(4) . ? Al1 N2 1.993(4) . ? Al1 Cl1 2.034(3) . ? Al1 Cl2 2.1381(18) . ? Al1 H1C1 1.5000(2) . ? Al1 H1C2 1.5000(3) . ? N1 C3 1.429(6) . ? N1 C1 1.459(6) . ? N2 C2 1.494(7) . ? N2 C15 1.502(6) . ? N2 C19 1.504(6) . ? C1 C2 1.524(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.403(6) . ? C3 C4 1.411(6) . ? C4 C5 1.407(6) . ? C4 C9 1.505(7) . ? C5 C6 1.368(8) . ? C5 H5A 0.9500 . ? C6 C7 1.384(7) . ? C6 H6A 0.9500 . ? C7 C8 1.398(6) . ? C7 H7A 0.9500 . ? C8 C12 1.513(7) . ? C9 C10 1.519(8) . ? C9 C11 1.546(8) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.512(7) . ? C12 C14 1.519(7) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.525(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.516(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.522(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.523(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ?