#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:28:56 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267144 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707505.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_7707505 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 'C25 H50 Al N3 Si2' _chemical_formula_sum 'C25 H50 Al N3 Si2' _chemical_formula_weight 475.84 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 110.035(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5020(4) _cell_length_b 16.5369(5) _cell_length_c 15.0602(5) _cell_measurement_reflns_used 16571 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 74.180 _cell_measurement_theta_min 3.763 _cell_volume 2925.19(18) _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 0.992 _diffrn_measured_fraction_theta_max 0.958 _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 0.0504 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 16571 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.958 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.180 _diffrn_reflns_theta_min 3.763 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_correction_T_min 0.854 _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 1.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.143 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.077 _refine_diff_density_max 0.487 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 5699 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0432 _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^)+(0.0630P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1124 _refine_ls_wR_factor_ref 0.1201 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4787 _reflns_number_total 5699 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01454d2.cif _cod_data_source_block FO6949_8a _cod_depositor_comments 'Adding full bibliography for 7707498--7707509.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7707505 _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 0.814 _shelx_estimated_absorpt_t_max 0.893 _shelx_res_file ; TITL rk1817_abs_a.res in P2(1)/c fo6949.res created by SHELXL-2018/3 at 13:32:57 on 21-Apr-2021 CELL 1.54184 12.5020 16.5369 15.0602 90 110.035 90 ZERR 4 0.0004 0.0005 0.0005 0.0 0.004 0.0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Al N Si UNIT 100 200 4 12 8 L.S. 10 0 0 PLAN 20 BOND $H fmap 2 OMIT -5 19 3 OMIT -4 19 3 acta TEMP -150 SIZE 0.143 0.095 0.077 REM COLOR:colourless WGHT 0.063000 0.589100 FVAR 0.47349 AL1 3 0.270570 0.369058 0.283675 11.00000 0.01104 0.01528 = 0.01347 0.00002 0.00454 -0.00032 SI1 5 0.005013 0.314055 0.204474 11.00000 0.01207 0.01993 = 0.02043 -0.00402 0.00524 -0.00198 SI2 5 0.111099 0.411034 0.382099 11.00000 0.01523 0.02074 = 0.01379 0.00002 0.00666 0.00097 N1 4 0.361267 0.283777 0.277473 11.00000 0.01388 0.01884 = 0.01487 0.00116 0.00583 0.00122 N2 4 0.285547 0.411856 0.160446 11.00000 0.01555 0.01728 = 0.01636 0.00277 0.00619 0.00014 N3 4 0.123685 0.358831 0.284972 11.00000 0.01257 0.01702 = 0.01653 0.00094 0.00569 0.00061 C1 1 0.399432 0.284986 0.195927 11.00000 0.01836 0.02167 = 0.02022 -0.00004 0.01057 0.00184 AFIX 23 H1A 2 0.401990 0.229281 0.172657 11.00000 -1.20000 H1B 2 0.476752 0.308546 0.213952 11.00000 -1.20000 AFIX 0 C2 1 0.315608 0.335957 0.119189 11.00000 0.02287 0.02112 = 0.01933 -0.00141 0.01109 0.00090 AFIX 23 H2A 2 0.349671 0.350373 0.070868 11.00000 -1.20000 H2B 2 0.245652 0.304212 0.087912 11.00000 -1.20000 AFIX 0 C3 1 0.427248 0.232950 0.353203 11.00000 0.01274 0.01712 = 0.01610 0.00018 0.00646 0.00055 C4 1 0.393036 0.152098 0.357475 11.00000 0.01362 0.01787 = 0.01690 -0.00197 0.00568 0.00037 C5 1 0.454581 0.103411 0.433231 11.00000 0.01997 0.01867 = 0.02092 0.00202 0.00724 -0.00003 AFIX 43 H5 2 0.430456 0.049362 0.436511 11.00000 -1.20000 AFIX 0 C6 1 0.550344 0.132292 0.503926 11.00000 0.01990 0.02202 = 0.01884 0.00397 0.00308 0.00535 AFIX 43 H6 2 0.591191 0.098534 0.555421 11.00000 -1.20000 AFIX 0 C7 1 0.585758 0.210888 0.498616 11.00000 0.01704 0.02375 = 0.02235 -0.00183 0.00243 0.00088 AFIX 43 H7 2 0.651768 0.230617 0.546707 11.00000 -1.20000 AFIX 0 C8 1 0.526409 0.261765 0.423991 11.00000 0.01236 0.01749 = 0.02270 -0.00188 0.00485 0.00066 C9 1 0.286799 0.119328 0.283290 11.00000 0.01900 0.01647 = 0.02153 0.00014 0.00380 -0.00302 AFIX 13 H9 2 0.265072 0.157861 0.228824 11.00000 -1.20000 AFIX 0 C10 1 0.189339 0.117474 0.322257 11.00000 0.01910 0.04563 = 0.03547 -0.00859 0.00814 -0.00975 AFIX 137 H10A 2 0.208032 0.080001 0.375831 11.00000 -1.50000 H10B 2 0.119591 0.099427 0.272709 11.00000 -1.50000 H10C 2 0.177686 0.171799 0.343302 11.00000 -1.50000 AFIX 0 C11 1 0.303846 0.036388 0.245575 11.00000 0.03402 0.02237 = 0.02679 -0.00636 0.00269 -0.00213 AFIX 137 H11A 2 0.366706 0.039080 0.220765 11.00000 -1.50000 H11B 2 0.233935 0.020246 0.194913 11.00000 -1.50000 H11C 2 0.321836 -0.003385 0.296845 11.00000 -1.50000 AFIX 0 C12 1 0.572528 0.346557 0.422615 11.00000 0.01366 0.01961 = 0.03270 0.00057 0.00003 -0.00247 AFIX 13 H12 2 0.518229 0.375666 0.367248 11.00000 -1.20000 AFIX 0 C13 1 0.579386 0.393789 0.511598 11.00000 0.02647 0.02303 = 0.04578 -0.01120 0.00037 -0.00276 AFIX 137 H13A 2 0.503567 0.396773 0.517001 11.00000 -1.50000 H13B 2 0.607309 0.448571 0.507639 11.00000 -1.50000 H13C 2 0.631681 0.366316 0.567225 11.00000 -1.50000 AFIX 0 C14 1 0.688195 0.344264 0.409025 11.00000 0.01897 0.03437 = 0.05128 0.00621 0.00867 -0.00499 AFIX 137 H14A 2 0.742969 0.315163 0.461864 11.00000 -1.50000 H14B 2 0.715155 0.399624 0.406837 11.00000 -1.50000 H14C 2 0.680605 0.316537 0.349662 11.00000 -1.50000 AFIX 0 C15 1 0.182958 0.449239 0.089426 11.00000 0.02124 0.02953 = 0.01407 0.00534 0.00442 0.00435 AFIX 23 H15A 2 0.117748 0.411640 0.076390 11.00000 -1.20000 H15B 2 0.197737 0.457818 0.029600 11.00000 -1.20000 AFIX 0 C16 1 0.152063 0.529588 0.123357 11.00000 0.02669 0.02698 = 0.02386 0.00752 0.01175 0.00818 AFIX 23 H16A 2 0.083897 0.552233 0.074361 11.00000 -1.20000 H16B 2 0.133323 0.520824 0.181392 11.00000 -1.20000 AFIX 0 C17 1 0.249747 0.589248 0.143853 11.00000 0.03553 0.02220 = 0.03420 0.00751 0.01956 0.00446 AFIX 23 H17A 2 0.230294 0.639580 0.170518 11.00000 -1.20000 H17B 2 0.262795 0.603079 0.084421 11.00000 -1.20000 AFIX 0 C18 1 0.357542 0.552481 0.213832 11.00000 0.02831 0.02077 = 0.03220 -0.00064 0.01611 -0.00361 AFIX 23 H18A 2 0.422551 0.589252 0.221348 11.00000 -1.20000 H18B 2 0.348258 0.546795 0.276229 11.00000 -1.20000 AFIX 0 C19 1 0.383186 0.470160 0.180928 11.00000 0.01943 0.02125 = 0.02617 0.00338 0.01299 -0.00244 AFIX 23 H19A 2 0.402820 0.477257 0.123061 11.00000 -1.20000 H19B 2 0.450389 0.446783 0.230295 11.00000 -1.20000 AFIX 0 C20 1 0.039929 0.252363 0.113341 11.00000 0.02187 0.02942 = 0.02893 -0.01203 0.00898 -0.00516 AFIX 137 H20A 2 0.049230 0.288286 0.064743 11.00000 -1.50000 H20B 2 -0.022032 0.214113 0.084092 11.00000 -1.50000 H20C 2 0.110812 0.222492 0.143622 11.00000 -1.50000 AFIX 0 C21 1 -0.073819 0.242399 0.257403 11.00000 0.02540 0.02610 = 0.04668 -0.00654 0.02019 -0.00600 AFIX 137 H21A 2 -0.020112 0.217461 0.314272 11.00000 -1.50000 H21B 2 -0.110440 0.200208 0.211316 11.00000 -1.50000 H21C 2 -0.131914 0.272252 0.274153 11.00000 -1.50000 AFIX 0 C22 1 -0.101046 0.392113 0.137621 11.00000 0.01622 0.03690 = 0.02499 -0.00082 0.00044 0.00429 AFIX 137 H22A 2 -0.125500 0.424097 0.182021 11.00000 -1.50000 H22B 2 -0.167201 0.365191 0.092377 11.00000 -1.50000 H22C 2 -0.065808 0.427806 0.103562 11.00000 -1.50000 AFIX 0 C23 1 -0.028319 0.394660 0.400163 11.00000 0.02277 0.04080 = 0.02592 -0.00484 0.01492 -0.00085 AFIX 137 H23A 2 -0.090835 0.404743 0.340734 11.00000 -1.50000 H23B 2 -0.034504 0.431886 0.448805 11.00000 -1.50000 H23C 2 -0.032543 0.338787 0.420398 11.00000 -1.50000 AFIX 0 C24 1 0.221267 0.376493 0.494907 11.00000 0.02992 0.03870 = 0.01815 0.00542 0.00680 0.00006 AFIX 137 H24A 2 0.226249 0.317347 0.495095 11.00000 -1.50000 H24B 2 0.199930 0.394347 0.548615 11.00000 -1.50000 H24C 2 0.295279 0.399705 0.500053 11.00000 -1.50000 AFIX 0 C25 1 0.119694 0.523251 0.369476 11.00000 0.02411 0.02326 = 0.02353 -0.00307 0.01011 0.00250 AFIX 137 H25A 2 0.191179 0.537087 0.359883 11.00000 -1.50000 H25B 2 0.117091 0.549759 0.426900 11.00000 -1.50000 H25C 2 0.055311 0.541646 0.315039 11.00000 -1.50000 AFIX 0 H1AL 2 0.330217 0.432257 0.357090 11.00000 0.02574 HKLF 4 REM rk1817_abs_a.res in P2(1)/c REM wR2 = 0.1201, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0432 for 4787 Fo > 4sig(Fo) and 0.0527 for all 5699 data REM 294 parameters refined using 0 restraints END WGHT 0.0630 0.5886 REM Highest difference peak 0.487, deepest hole -0.420, 1-sigma level 0.059 Q1 1 0.1806 0.3587 0.2762 11.00000 0.05 0.49 Q2 1 0.0314 0.4084 0.3844 11.00000 0.05 0.48 Q3 1 0.1420 0.3785 0.4471 11.00000 0.05 0.33 Q4 1 0.1035 0.3205 0.2190 11.00000 0.05 0.32 Q5 1 0.1170 0.3956 0.3053 11.00000 0.05 0.29 Q6 1 0.4852 0.1310 0.4803 11.00000 0.05 0.29 Q7 1 0.2749 0.3823 0.2005 11.00000 0.05 0.28 Q8 1 0.3435 0.1335 0.3216 11.00000 0.05 0.27 Q9 1 0.0076 0.2849 0.1368 11.00000 0.05 0.27 Q10 1 0.4017 0.1873 0.3637 11.00000 0.05 0.26 Q11 1 0.5642 0.1725 0.4978 11.00000 0.05 0.26 Q12 1 0.2932 0.4022 0.3471 11.00000 0.05 0.25 Q13 1 -0.0272 0.3485 0.1418 11.00000 0.05 0.25 Q14 1 -0.0824 0.3166 0.1938 11.00000 0.05 0.24 Q15 1 0.0380 0.3485 0.2766 11.00000 0.05 0.24 Q16 1 0.0982 0.3138 0.2793 11.00000 0.05 0.23 Q17 1 0.4999 0.2335 0.3726 11.00000 0.05 0.23 Q18 1 0.5442 0.2380 0.4725 11.00000 0.05 0.23 Q19 1 -0.0613 0.3717 0.1961 11.00000 0.05 0.23 Q20 1 0.2505 0.3648 0.3599 11.00000 0.05 0.22 ; _shelx_res_checksum 10700 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.27057(4) 0.36906(3) 0.28367(3) 0.01317(13) Uani 1 1 d . . . . . Si1 Si 0.00501(4) 0.31405(3) 0.20447(3) 0.01756(13) Uani 1 1 d . . . . . Si2 Si 0.11110(4) 0.41103(3) 0.38210(3) 0.01615(13) Uani 1 1 d . . . . . N1 N 0.36127(12) 0.28378(9) 0.27747(10) 0.0156(3) Uani 1 1 d . . . . . N2 N 0.28555(12) 0.41186(9) 0.16045(10) 0.0162(3) Uani 1 1 d . . . . . N3 N 0.12368(12) 0.35883(9) 0.28497(10) 0.0152(3) Uani 1 1 d . . . . . C1 C 0.39943(15) 0.28499(11) 0.19593(13) 0.0191(4) Uani 1 1 d . . . . . H1A H 0.401990 0.229281 0.172657 0.023 Uiso 1 1 calc R U . . . H1B H 0.476752 0.308546 0.213952 0.023 Uiso 1 1 calc R U . . . C2 C 0.31561(16) 0.33596(11) 0.11919(13) 0.0201(4) Uani 1 1 d . . . . . H2A H 0.349671 0.350373 0.070868 0.024 Uiso 1 1 calc R U . . . H2B H 0.245652 0.304212 0.087912 0.024 Uiso 1 1 calc R U . . . C3 C 0.42725(14) 0.23295(10) 0.35320(12) 0.0149(3) Uani 1 1 d . . . . . C4 C 0.39304(14) 0.15210(11) 0.35747(12) 0.0160(4) Uani 1 1 d . . . . . C5 C 0.45458(16) 0.10341(11) 0.43323(13) 0.0198(4) Uani 1 1 d . . . . . H5 H 0.430456 0.049362 0.436511 0.024 Uiso 1 1 calc R U . . . C6 C 0.55034(16) 0.13229(11) 0.50393(13) 0.0212(4) Uani 1 1 d . . . . . H6 H 0.591191 0.098534 0.555421 0.025 Uiso 1 1 calc R U . . . C7 C 0.58576(16) 0.21089(12) 0.49862(13) 0.0222(4) Uani 1 1 d . . . . . H7 H 0.651768 0.230617 0.546707 0.027 Uiso 1 1 calc R U . . . C8 C 0.52641(15) 0.26176(11) 0.42399(13) 0.0178(4) Uani 1 1 d . . . . . C9 C 0.28680(15) 0.11933(11) 0.28329(13) 0.0198(4) Uani 1 1 d . . . . . H9 H 0.265072 0.157861 0.228824 0.024 Uiso 1 1 calc R U . . . C10 C 0.18934(17) 0.11747(15) 0.32226(17) 0.0337(5) Uani 1 1 d . . . . . H10A H 0.208032 0.080001 0.375831 0.051 Uiso 1 1 calc R U . . . H10B H 0.119591 0.099427 0.272709 0.051 Uiso 1 1 calc R U . . . H10C H 0.177686 0.171799 0.343302 0.051 Uiso 1 1 calc R U . . . C11 C 0.30385(19) 0.03639(12) 0.24558(15) 0.0297(5) Uani 1 1 d . . . . . H11A H 0.366706 0.039080 0.220765 0.045 Uiso 1 1 calc R U . . . H11B H 0.233935 0.020246 0.194913 0.045 Uiso 1 1 calc R U . . . H11C H 0.321836 -0.003385 0.296845 0.045 Uiso 1 1 calc R U . . . C12 C 0.57253(16) 0.34656(12) 0.42262(15) 0.0240(4) Uani 1 1 d . . . . . H12 H 0.518229 0.375666 0.367248 0.029 Uiso 1 1 calc R U . . . C13 C 0.57939(19) 0.39379(13) 0.51160(17) 0.0349(5) Uani 1 1 d . . . . . H13A H 0.503567 0.396773 0.517001 0.052 Uiso 1 1 calc R U . . . H13B H 0.607309 0.448571 0.507639 0.052 Uiso 1 1 calc R U . . . H13C H 0.631681 0.366316 0.567225 0.052 Uiso 1 1 calc R U . . . C14 C 0.68819(17) 0.34426(14) 0.40903(18) 0.0357(5) Uani 1 1 d . . . . . H14A H 0.742969 0.315163 0.461864 0.054 Uiso 1 1 calc R U . . . H14B H 0.715155 0.399624 0.406837 0.054 Uiso 1 1 calc R U . . . H14C H 0.680605 0.316537 0.349662 0.054 Uiso 1 1 calc R U . . . C15 C 0.18296(16) 0.44924(12) 0.08943(12) 0.0220(4) Uani 1 1 d . . . . . H15A H 0.117748 0.411640 0.076390 0.026 Uiso 1 1 calc R U . . . H15B H 0.197737 0.457818 0.029600 0.026 Uiso 1 1 calc R U . . . C16 C 0.15206(17) 0.52959(12) 0.12336(14) 0.0250(4) Uani 1 1 d . . . . . H16A H 0.083897 0.552233 0.074361 0.030 Uiso 1 1 calc R U . . . H16B H 0.133323 0.520824 0.181392 0.030 Uiso 1 1 calc R U . . . C17 C 0.24975(18) 0.58925(12) 0.14385(15) 0.0287(5) Uani 1 1 d . . . . . H17A H 0.230294 0.639580 0.170518 0.034 Uiso 1 1 calc R U . . . H17B H 0.262795 0.603079 0.084421 0.034 Uiso 1 1 calc R U . . . C18 C 0.35754(17) 0.55248(12) 0.21383(14) 0.0256(4) Uani 1 1 d . . . . . H18A H 0.422551 0.589252 0.221348 0.031 Uiso 1 1 calc R U . . . H18B H 0.348258 0.546795 0.276229 0.031 Uiso 1 1 calc R U . . . C19 C 0.38319(16) 0.47016(11) 0.18093(14) 0.0209(4) Uani 1 1 d . . . . . H19A H 0.402820 0.477257 0.123061 0.025 Uiso 1 1 calc R U . . . H19B H 0.450389 0.446783 0.230295 0.025 Uiso 1 1 calc R U . . . C20 C 0.03993(17) 0.25236(12) 0.11334(14) 0.0267(4) Uani 1 1 d . . . . . H20A H 0.049230 0.288286 0.064743 0.040 Uiso 1 1 calc R U . . . H20B H -0.022032 0.214113 0.084092 0.040 Uiso 1 1 calc R U . . . H20C H 0.110812 0.222492 0.143622 0.040 Uiso 1 1 calc R U . . . C21 C -0.07382(18) 0.24240(13) 0.25740(17) 0.0307(5) Uani 1 1 d . . . . . H21A H -0.020112 0.217461 0.314272 0.046 Uiso 1 1 calc R U . . . H21B H -0.110440 0.200208 0.211316 0.046 Uiso 1 1 calc R U . . . H21C H -0.131914 0.272252 0.274153 0.046 Uiso 1 1 calc R U . . . C22 C -0.10105(16) 0.39211(13) 0.13762(15) 0.0277(4) Uani 1 1 d . . . . . H22A H -0.125500 0.424097 0.182021 0.042 Uiso 1 1 calc R U . . . H22B H -0.167201 0.365191 0.092377 0.042 Uiso 1 1 calc R U . . . H22C H -0.065808 0.427806 0.103562 0.042 Uiso 1 1 calc R U . . . C23 C -0.02832(17) 0.39466(14) 0.40016(15) 0.0281(4) Uani 1 1 d . . . . . H23A H -0.090835 0.404743 0.340734 0.042 Uiso 1 1 calc R U . . . H23B H -0.034504 0.431886 0.448805 0.042 Uiso 1 1 calc R U . . . H23C H -0.032543 0.338787 0.420398 0.042 Uiso 1 1 calc R U . . . C24 C 0.22127(18) 0.37649(14) 0.49491(14) 0.0293(5) Uani 1 1 d . . . . . H24A H 0.226249 0.317347 0.495095 0.044 Uiso 1 1 calc R U . . . H24B H 0.199930 0.394347 0.548615 0.044 Uiso 1 1 calc R U . . . H24C H 0.295279 0.399705 0.500053 0.044 Uiso 1 1 calc R U . . . C25 C 0.11969(16) 0.52325(11) 0.36948(14) 0.0231(4) Uani 1 1 d . . . . . H25A H 0.191179 0.537087 0.359883 0.035 Uiso 1 1 calc R U . . . H25B H 0.117091 0.549759 0.426900 0.035 Uiso 1 1 calc R U . . . H25C H 0.055311 0.541646 0.315039 0.035 Uiso 1 1 calc R U . . . H1AL H 0.3302(18) 0.4323(13) 0.3571(15) 0.026(6) Uiso 1 1 d . . . . . 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 0.0110(2) 0.0153(3) 0.0135(3) 0.00002(18) 0.0045(2) -0.00032(18) Si1 0.0121(2) 0.0199(3) 0.0204(3) -0.00402(19) 0.0052(2) -0.00198(18) Si2 0.0152(2) 0.0207(3) 0.0138(2) 0.00002(18) 0.0067(2) 0.00097(18) N1 0.0139(7) 0.0188(7) 0.0149(7) 0.0012(6) 0.0058(6) 0.0012(6) N2 0.0155(7) 0.0173(7) 0.0164(7) 0.0028(6) 0.0062(6) 0.0001(6) N3 0.0126(7) 0.0170(7) 0.0165(7) 0.0009(6) 0.0057(6) 0.0006(6) C1 0.0184(8) 0.0217(9) 0.0202(9) 0.0000(7) 0.0106(8) 0.0018(7) C2 0.0229(9) 0.0211(9) 0.0193(9) -0.0014(7) 0.0111(8) 0.0009(7) C3 0.0127(8) 0.0171(8) 0.0161(8) 0.0002(7) 0.0065(7) 0.0005(7) C4 0.0136(8) 0.0179(9) 0.0169(9) -0.0020(7) 0.0057(7) 0.0004(7) C5 0.0200(9) 0.0187(9) 0.0209(9) 0.0020(7) 0.0072(8) 0.0000(7) C6 0.0199(9) 0.0220(9) 0.0188(9) 0.0040(7) 0.0031(8) 0.0054(7) C7 0.0170(9) 0.0238(10) 0.0224(9) -0.0018(8) 0.0024(8) 0.0009(7) C8 0.0124(8) 0.0175(9) 0.0227(9) -0.0019(7) 0.0048(7) 0.0007(7) C9 0.0190(9) 0.0165(9) 0.0215(9) 0.0001(7) 0.0038(8) -0.0030(7) C10 0.0191(10) 0.0456(13) 0.0355(12) -0.0086(10) 0.0081(10) -0.0097(9) C11 0.0340(11) 0.0224(10) 0.0268(11) -0.0064(8) 0.0027(9) -0.0021(9) C12 0.0137(8) 0.0196(9) 0.0327(11) 0.0006(8) 0.0000(8) -0.0025(7) C13 0.0265(11) 0.0230(10) 0.0458(14) -0.0112(10) 0.0004(10) -0.0028(9) C14 0.0190(10) 0.0344(12) 0.0513(14) 0.0062(10) 0.0087(10) -0.0050(9) C15 0.0212(9) 0.0295(10) 0.0141(9) 0.0053(7) 0.0044(8) 0.0043(8) C16 0.0267(10) 0.0270(10) 0.0239(10) 0.0075(8) 0.0118(9) 0.0082(8) C17 0.0355(11) 0.0222(10) 0.0342(11) 0.0075(8) 0.0196(10) 0.0045(9) C18 0.0283(10) 0.0208(10) 0.0322(11) -0.0006(8) 0.0161(9) -0.0036(8) C19 0.0194(9) 0.0212(9) 0.0262(10) 0.0034(7) 0.0130(8) -0.0024(7) C20 0.0219(9) 0.0294(11) 0.0289(11) -0.0120(8) 0.0090(9) -0.0052(8) C21 0.0254(10) 0.0261(10) 0.0467(13) -0.0065(9) 0.0202(10) -0.0060(8) C22 0.0162(9) 0.0369(11) 0.0250(10) -0.0008(9) 0.0004(8) 0.0043(8) C23 0.0228(10) 0.0408(12) 0.0259(10) -0.0048(9) 0.0149(9) -0.0009(9) C24 0.0299(11) 0.0387(12) 0.0181(10) 0.0054(8) 0.0068(9) 0.0001(9) C25 0.0241(9) 0.0233(10) 0.0235(9) -0.0031(8) 0.0101(8) 0.0025(8) 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 N3 124.32(7) . . ? N1 Al1 N2 88.26(6) . . ? N3 Al1 N2 116.04(7) . . ? N1 Al1 H1AL 114.1(8) . . ? N3 Al1 H1AL 107.3(8) . . ? N2 Al1 H1AL 104.3(8) . . ? N3 Si1 C22 111.13(8) . . ? N3 Si1 C20 112.76(8) . . ? C22 Si1 C20 106.26(10) . . ? N3 Si1 C21 114.87(9) . . ? C22 Si1 C21 106.48(10) . . ? C20 Si1 C21 104.71(9) . . ? N3 Si2 C25 112.27(8) . . ? N3 Si2 C24 111.03(9) . . ? C25 Si2 C24 110.15(10) . . ? N3 Si2 C23 113.85(8) . . ? C25 Si2 C23 104.28(9) . . ? C24 Si2 C23 104.83(10) . . ? C3 N1 C1 114.40(14) . . ? C3 N1 Al1 127.60(11) . . ? C1 N1 Al1 114.71(11) . . ? C15 N2 C19 108.62(14) . . ? C15 N2 C2 108.92(14) . . ? C19 N2 C2 108.66(14) . . ? C15 N2 Al1 117.90(11) . . ? C19 N2 Al1 110.78(11) . . ? C2 N2 Al1 101.46(10) . . ? Si1 N3 Si2 119.73(8) . . ? Si1 N3 Al1 130.40(9) . . ? Si2 N3 Al1 109.70(8) . . ? N1 C1 C2 107.91(14) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 110.68(14) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C8 119.10(16) . . ? C4 C3 N1 119.48(15) . . ? C8 C3 N1 121.42(15) . . ? C5 C4 C3 119.58(16) . . ? C5 C4 C9 119.78(16) . . ? C3 C4 C9 120.56(15) . . ? C6 C5 C4 121.29(17) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C7 C6 C5 119.23(17) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 121.33(17) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 119.42(16) . . ? C7 C8 C12 117.88(16) . . ? C3 C8 C12 122.70(16) . . ? C4 C9 C10 109.78(16) . . ? C4 C9 C11 113.41(16) . . ? C10 C9 C11 110.93(17) . . ? C4 C9 H9 107.5 . . ? C10 C9 H9 107.5 . . ? C11 C9 H9 107.5 . . ? 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 . . ? C8 C12 C13 111.56(18) . . ? C8 C12 C14 111.09(16) . . ? C13 C12 C14 111.02(17) . . ? C8 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? 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 112.07(15) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 110.93(16) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 109.92(16) . . ? 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 . . ? C19 C18 C17 111.54(17) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C18 113.23(15) . . ? N2 C19 H19A 108.9 . . ? C18 C19 H19A 108.9 . . ? N2 C19 H19B 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 1.8319(15) . ? Al1 N3 1.8509(15) . ? Al1 N2 2.0538(15) . ? Al1 H1AL 1.52(2) . ? Si1 N3 1.7282(15) . ? Si1 C22 1.877(2) . ? Si1 C20 1.8776(19) . ? Si1 C21 1.884(2) . ? Si2 N3 1.7514(15) . ? Si2 C25 1.872(2) . ? Si2 C24 1.873(2) . ? Si2 C23 1.8736(19) . ? N1 C3 1.429(2) . ? N1 C1 1.462(2) . ? N2 C15 1.494(2) . ? N2 C19 1.502(2) . ? N2 C2 1.504(2) . ? C1 C2 1.521(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.412(2) . ? C3 C8 1.412(2) . ? C4 C5 1.393(2) . ? C4 C9 1.513(2) . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 C8 1.396(3) . ? C7 H7 0.9500 . ? C8 C12 1.519(3) . ? C9 C10 1.523(3) . ? C9 C11 1.527(3) . ? C9 H9 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 1.528(3) . ? C12 C14 1.529(3) . ? C12 H12 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 1.520(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.517(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.524(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.520(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ?