#------------------------------------------------------------------------------ #$Date: 2019-05-17 04:34:17 +0300 (Fri, 17 May 2019) $ #$Revision: 215230 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700010.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_7700010 loop_ _publ_author_name 'Koner, Abhishek' 'Gabidullin, Bulat M.' 'Kelemen, Zsolt' 'Nyul\'aszi, L\'aszl\'o' 'Nikonov, Georgii I.' 'Streubel, Rainer' _publ_section_title ; 7-Metalla-1,4-diphosphanorbornadienes: cycloaddition of monovalent group 13 NacNac complexes to a stable 1,4-diphosphinine ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01425J _journal_year 2019 _chemical_formula_sum 'C51 H77 Al N6 P2 S2' _chemical_formula_weight 927.22 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-02-28 deposited with the CCDC. 2019-04-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.880(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.3978(5) _cell_length_b 20.1923(9) _cell_length_c 21.8157(11) _cell_measurement_reflns_used 5144 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 23.39 _cell_measurement_theta_min 2.62 _cell_volume 5363.2(4) _computing_cell_refinement 'APEX II (Bruker, 2009)' _computing_data_collection 'APEX II (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.933 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0786 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.933 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 41871 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.933 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.088 _diffrn_reflns_theta_min 1.386 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.6815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.148 _exptl_crystal_description plate _exptl_crystal_F_000 2000 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ether' _exptl_crystal_size_max 0.737 _exptl_crystal_size_mid 0.583 _exptl_crystal_size_min 0.104 _refine_diff_density_max 0.517 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 563 _refine_ls_number_reflns 14732 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0607 _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^)+(0.0743P)^2^+0.4415P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1368 _refine_ls_wR_factor_ref 0.1638 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8445 _reflns_number_total 14732 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01425j2.cif _cod_data_source_block shelx _cod_database_code 7700010 _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 0.858 _shelx_estimated_absorpt_t_max 0.978 _shelx_res_file ; TITL gn232 in P2(1)/n shelx.res created by SHELXL-2018/3 at 19:55:09 on 17-May-2018 CELL 0.71073 12.3978 20.1923 21.8157 90.000 100.880 90.000 ZERR 4.00 0.0005 0.0009 0.0011 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N AL P S UNIT 204 308 24 4 8 8 MERG 2 OMIT -3.00 180.00 EQIV $1 x+1/2, -y+1/2, z+1/2 HTAB C3 S1_$1 HTAB C41 S1 HTAB C45 S2 HTAB C3 S1_$1 HTAB C41 S1 HTAB C45 S2 FMAP 2 PLAN 3 SIZE 0.104 0.583 0.737 ACTA BOND $H CONF L.S. 10 TEMP -73.15 WGHT 0.074300 0.441500 FVAR 0.25753 0.18995 0.42826 AL 4 0.252636 0.287460 0.623736 11.00000 0.02778 0.03242 = 0.02611 0.00208 0.00575 -0.00314 P1 5 0.189918 0.325704 0.517762 11.00000 0.03623 0.03016 = 0.02976 0.00194 0.00629 -0.00163 P2 5 0.303320 0.183901 0.576060 11.00000 0.02985 0.03290 = 0.03429 0.00568 0.00489 -0.00258 S1 6 -0.115897 0.123229 0.438868 11.00000 0.03806 0.05904 = 0.04297 -0.00007 -0.00064 -0.01718 S2 6 0.587955 0.298530 0.432498 11.00000 0.05209 0.06257 = 0.05868 -0.00206 0.03029 -0.01373 N1 3 0.359527 0.338615 0.676339 11.00000 0.03121 0.03263 = 0.02748 0.00309 0.00568 -0.00332 N2 3 0.148817 0.289155 0.676809 11.00000 0.02988 0.03996 = 0.02741 0.00456 0.00627 -0.00062 N3 3 0.017225 0.230735 0.469270 11.00000 0.03049 0.03699 = 0.03125 0.00385 0.00344 -0.00152 N4 3 0.093523 0.137484 0.504213 11.00000 0.03365 0.03197 = 0.03462 0.00298 0.00443 -0.00818 N5 3 0.463137 0.228684 0.501078 11.00000 0.03431 0.03822 = 0.03880 0.00071 0.01230 -0.00503 N6 3 0.391221 0.323075 0.466540 11.00000 0.04183 0.03312 = 0.03476 0.00026 0.01215 -0.01013 C1 1 0.087614 0.297382 0.778285 11.00000 0.04757 0.07505 = 0.03729 0.00134 0.01721 -0.00094 AFIX 137 H1A 2 0.014217 0.294830 0.752120 11.00000 -1.50000 H1B 2 0.091254 0.335560 0.806337 11.00000 -1.50000 H1C 2 0.102421 0.256744 0.803000 11.00000 -1.50000 AFIX 0 C2 1 0.172351 0.305113 0.737260 11.00000 0.03867 0.04348 = 0.03037 0.00541 0.00996 0.00368 C3 1 0.273714 0.330133 0.766007 11.00000 0.04352 0.05143 = 0.02424 -0.00006 0.00648 0.00078 AFIX 43 H3A 2 0.285886 0.334281 0.810154 11.00000 -1.20000 AFIX 0 C4 1 0.359381 0.349780 0.736998 11.00000 0.03978 0.03686 = 0.03036 0.00031 0.00243 0.00066 C5 1 0.453253 0.386095 0.776784 11.00000 0.05154 0.05483 = 0.03179 -0.00682 0.00307 -0.01289 AFIX 137 H5A 2 0.485906 0.416861 0.750706 11.00000 -1.50000 H5B 2 0.508904 0.354170 0.796179 11.00000 -1.50000 H5C 2 0.426089 0.410904 0.809378 11.00000 -1.50000 AFIX 0 C6 1 0.443957 0.368048 0.647360 11.00000 0.03580 0.03587 = 0.02950 -0.00328 0.00457 -0.01096 C7 1 0.417133 0.426172 0.611896 11.00000 0.04619 0.03052 = 0.03506 -0.00254 0.00546 -0.01135 C8 1 0.492948 0.448824 0.577858 11.00000 0.06184 0.04231 = 0.04819 0.00562 0.01202 -0.01944 AFIX 43 H8A 2 0.477138 0.487719 0.553305 11.00000 -1.20000 AFIX 0 C9 1 0.590683 0.416459 0.578654 11.00000 0.05716 0.06993 = 0.05714 0.00404 0.02342 -0.02523 AFIX 43 H9A 2 0.639890 0.431866 0.553292 11.00000 -1.20000 AFIX 0 C10 1 0.617321 0.362133 0.615853 11.00000 0.04034 0.06427 = 0.06485 -0.00221 0.01929 -0.01035 AFIX 43 H10A 2 0.686335 0.341229 0.617049 11.00000 -1.20000 AFIX 0 C11 1 0.545990 0.336824 0.651876 11.00000 0.03475 0.04548 = 0.04081 -0.00282 0.00637 -0.00830 C12 1 0.582391 0.279059 0.695884 11.00000 0.03399 0.05796 = 0.04671 0.00657 0.00286 0.00300 AFIX 13 H12A 2 0.524752 0.271968 0.721691 11.00000 -1.20000 AFIX 0 C13 1 0.690853 0.295235 0.740508 11.00000 0.05080 0.09647 = 0.07564 0.00040 -0.01718 0.00201 AFIX 33 H13A 2 0.682559 0.336509 0.762794 11.00000 -1.50000 H13B 2 0.709443 0.259117 0.770658 11.00000 -1.50000 H13C 2 0.749625 0.300379 0.716490 11.00000 -1.50000 AFIX 0 C14 1 0.594060 0.215105 0.660973 11.00000 0.05255 0.05709 = 0.06145 0.00231 0.00608 0.00446 AFIX 33 H14A 2 0.617513 0.179452 0.691014 11.00000 -1.50000 H14B 2 0.523225 0.203550 0.634913 11.00000 -1.50000 H14C 2 0.648966 0.221077 0.634482 11.00000 -1.50000 AFIX 0 C15 1 0.313353 0.464674 0.613996 11.00000 0.06006 0.03235 = 0.04657 0.00364 0.01089 -0.00115 AFIX 13 H15A 2 0.254711 0.431797 0.617910 11.00000 -1.20000 AFIX 0 C16 1 0.270818 0.507022 0.556991 11.00000 0.08641 0.04970 = 0.05306 0.00543 0.00310 0.01084 AFIX 33 H16A 2 0.203718 0.529918 0.562698 11.00000 -1.50000 H16B 2 0.326685 0.539731 0.551614 11.00000 -1.50000 H16C 2 0.254614 0.478731 0.519890 11.00000 -1.50000 AFIX 0 C17 1 0.327023 0.509391 0.670565 11.00000 0.17356 0.09637 = 0.05340 -0.02363 -0.00663 0.06850 AFIX 33 H17A 2 0.258482 0.533578 0.670535 11.00000 -1.50000 H17B 2 0.344897 0.482587 0.708579 11.00000 -1.50000 H17C 2 0.386547 0.540980 0.669231 11.00000 -1.50000 AFIX 0 C18 1 0.036882 0.274353 0.646142 11.00000 0.02828 0.05452 = 0.03000 0.00258 0.01081 -0.00046 C19 1 -0.024542 0.326190 0.612623 11.00000 0.03348 0.06654 = 0.03388 0.00549 0.01450 0.01004 C20 1 -0.123356 0.309194 0.574481 11.00000 0.02883 0.09962 = 0.04078 0.01263 0.01097 0.01301 AFIX 43 H20A 2 -0.166871 0.342776 0.551365 11.00000 -1.20000 AFIX 0 C21 1 -0.159519 0.244634 0.569498 11.00000 0.02885 0.11876 = 0.04520 -0.00044 0.00480 -0.01374 AFIX 43 H21A 2 -0.224271 0.233599 0.540505 11.00000 -1.20000 AFIX 0 C22 1 -0.103291 0.196599 0.605734 11.00000 0.04314 0.08647 = 0.04877 0.00131 0.01330 -0.02506 AFIX 43 H22A 2 -0.132176 0.152911 0.603768 11.00000 -1.20000 AFIX 0 C23 1 -0.003944 0.210039 0.645817 11.00000 0.03562 0.06341 = 0.03589 0.00200 0.01300 -0.00899 C24 1 0.050701 0.157053 0.690907 11.00000 0.04783 0.05359 = 0.04789 0.00371 0.01688 -0.01103 AFIX 13 H24A 2 0.116161 0.177550 0.718095 11.00000 -1.20000 AFIX 0 C25 1 -0.030666 0.136136 0.733406 11.00000 0.07730 0.09015 = 0.07155 0.02575 0.03680 -0.00890 AFIX 33 H25A 2 -0.055156 0.175496 0.753228 11.00000 -1.50000 H25B 2 -0.094299 0.114050 0.708170 11.00000 -1.50000 H25C 2 0.006078 0.105653 0.765657 11.00000 -1.50000 AFIX 0 C26 1 0.089796 0.097256 0.659733 11.00000 0.08015 0.05791 = 0.06032 0.00751 0.02178 -0.01415 AFIX 33 H26A 2 0.123813 0.065597 0.691647 11.00000 -1.50000 H26B 2 0.027163 0.076265 0.632552 11.00000 -1.50000 H26C 2 0.143786 0.111093 0.634766 11.00000 -1.50000 AFIX 0 C27 1 0.011662 0.397746 0.620809 11.00000 0.05106 0.06185 = 0.05393 0.00806 0.01268 0.02010 AFIX 13 H27A 2 0.093771 0.398399 0.630619 11.00000 -1.20000 AFIX 0 C28 1 -0.029535 0.428883 0.675713 11.00000 0.14492 0.07878 = 0.06411 -0.00182 0.02936 0.03335 AFIX 33 H28A 2 -0.005412 0.475132 0.680352 11.00000 -1.50000 H28B 2 -0.109953 0.427101 0.668124 11.00000 -1.50000 H28C 2 0.000263 0.404440 0.713975 11.00000 -1.50000 AFIX 0 C29 1 -0.025281 0.440888 0.563630 11.00000 0.09615 0.07491 = 0.06314 0.02246 0.02288 0.02823 AFIX 33 H29A 2 0.001261 0.486222 0.572626 11.00000 -1.50000 H29B 2 0.004754 0.423246 0.528507 11.00000 -1.50000 H29C 2 -0.105684 0.441018 0.552882 11.00000 -1.50000 AFIX 0 C30 1 -0.000507 0.164242 0.470293 11.00000 0.03379 0.04324 = 0.02963 0.00132 0.00743 -0.00512 C31 1 0.120604 0.245878 0.503798 11.00000 0.02973 0.03623 = 0.02743 0.00038 0.00447 -0.00330 C32 1 0.167616 0.187910 0.525987 11.00000 0.03133 0.03000 = 0.03081 0.00109 0.00584 -0.00584 C33 1 0.479364 0.282984 0.466400 11.00000 0.04132 0.04075 = 0.03998 -0.00513 0.01192 -0.01057 C34 1 0.320640 0.294882 0.502187 11.00000 0.03591 0.03046 = 0.03042 -0.00077 0.01016 -0.00766 C35 1 0.366431 0.236971 0.524247 11.00000 0.03104 0.03570 = 0.03232 -0.00084 0.00880 -0.00479 C36 1 -0.060491 0.278298 0.435244 11.00000 0.03345 0.04285 = 0.03672 0.00011 0.00304 0.00451 AFIX 23 H36A 2 -0.052152 0.321119 0.457744 11.00000 -1.20000 H36B 2 -0.136172 0.262205 0.434449 11.00000 -1.20000 AFIX 0 C37 1 -0.044716 0.289282 0.369219 11.00000 0.04096 0.04228 = 0.03462 0.00345 0.00363 0.00460 AFIX 23 H37A 2 -0.054916 0.246835 0.346140 11.00000 -1.20000 H37B 2 0.031183 0.304794 0.369677 11.00000 -1.20000 AFIX 0 C38 1 -0.125792 0.340169 0.335867 11.00000 0.06508 0.05674 = 0.04578 0.00621 0.00303 0.01399 AFIX 23 H38A 2 -0.201205 0.325870 0.338404 11.00000 -1.20000 H38B 2 -0.112238 0.383063 0.357957 11.00000 -1.20000 AFIX 0 C39 1 -0.119106 0.350302 0.268468 11.00000 0.07193 0.07556 = 0.04960 0.02249 0.00473 0.01084 AFIX 33 H39A 2 -0.173306 0.383519 0.250093 11.00000 -1.50000 H39B 2 -0.045286 0.365632 0.265460 11.00000 -1.50000 H39C 2 -0.134365 0.308366 0.245883 11.00000 -1.50000 AFIX 0 C40 1 0.115165 0.066181 0.509789 11.00000 0.04635 0.03247 = 0.04408 0.00572 0.00756 -0.00657 AFIX 23 H40A 2 0.051840 0.043957 0.522676 11.00000 -1.20000 H40B 2 0.180517 0.058495 0.542848 11.00000 -1.20000 AFIX 0 C41 1 0.134554 0.035611 0.449642 11.00000 0.07742 0.04163 = 0.06757 -0.00183 0.02110 -0.00192 AFIX 23 H41A 2 0.149920 -0.012142 0.456962 11.00000 -1.20000 H41B 2 0.065976 0.039335 0.418146 11.00000 -1.20000 AFIX 0 C42 1 0.224161 0.064599 0.423552 11.00000 0.10053 0.07644 = 0.08073 -0.01223 0.04441 -0.01072 AFIX 23 H42A 2 0.292764 0.062370 0.455186 11.00000 -1.20000 H42B 2 0.207728 0.111878 0.414028 11.00000 -1.20000 AFIX 0 C43 1 0.242180 0.029350 0.363923 11.00000 0.10599 0.10762 = 0.07763 -0.02466 0.04064 0.00009 AFIX 33 H43A 2 0.302846 0.050602 0.348413 11.00000 -1.50000 H43B 2 0.260125 -0.017283 0.373236 11.00000 -1.50000 H43C 2 0.175066 0.032237 0.332067 11.00000 -1.50000 AFIX 0 C44 1 0.532379 0.169471 0.506398 11.00000 0.03322 0.04836 = 0.05198 0.00002 0.00971 0.00163 AFIX 23 H44A 2 0.513666 0.140651 0.539586 11.00000 -1.20000 H44B 2 0.610143 0.182940 0.519269 11.00000 -1.20000 AFIX 0 C45 1 0.520160 0.130233 0.446758 11.00000 0.05518 0.04859 = 0.06553 -0.00376 0.01721 0.00795 AFIX 23 H45A 2 0.541571 0.158280 0.413804 11.00000 -1.20000 H45B 2 0.442151 0.117663 0.433034 11.00000 -1.20000 AFIX 0 C46 1 0.590342 0.068160 0.454729 11.00000 0.05591 0.05451 = 0.10430 0.00200 0.02906 0.01008 AFIX 23 H46A 2 0.667621 0.081012 0.470624 11.00000 -1.20000 H46B 2 0.566594 0.039708 0.486680 11.00000 -1.20000 AFIX 0 C47 1 0.585366 0.028251 0.395860 11.00000 0.13182 0.07661 = 0.12815 -0.02236 0.03339 0.03963 AFIX 33 H47A 2 0.632626 -0.010810 0.404830 11.00000 -1.50000 H47B 2 0.509522 0.014123 0.380282 11.00000 -1.50000 H47C 2 0.610715 0.055494 0.364200 11.00000 -1.50000 AFIX 0 C48 1 0.370163 0.383901 0.430834 11.00000 0.05872 0.03196 = 0.04532 0.00333 0.02113 -0.00914 AFIX 23 H48A 2 0.441050 0.402910 0.424845 11.00000 -1.20000 H48B 2 0.335074 0.416229 0.455008 11.00000 -1.20000 AFIX 0 C49 1 0.297513 0.374065 0.368005 11.00000 0.06207 0.04988 = 0.04444 0.00445 0.01296 -0.00431 AFIX 23 H49A 2 0.227583 0.353298 0.373418 11.00000 -1.20000 H49B 2 0.334047 0.343932 0.342501 11.00000 -1.20000 AFIX 0 C50 1 0.273722 0.440319 0.334264 11.00000 0.08714 0.06081 = 0.05421 0.00151 0.00636 0.00257 AFIX 23 H50A 2 0.241710 0.470933 0.361444 11.00000 -1.20000 H50B 2 0.343999 0.459717 0.327703 11.00000 -1.20000 AFIX 0 C51 1 0.198528 0.435695 0.273616 11.00000 0.09454 0.09344 = 0.06744 0.00370 0.01132 0.01501 AFIX 33 H51A 2 0.187274 0.479871 0.254897 11.00000 -1.50000 H51B 2 0.230319 0.406450 0.245873 11.00000 -1.50000 H51C 2 0.127883 0.417683 0.279663 11.00000 -1.50000 AFIX 0 HKLF 4 REM gn232 in P2(1)/n REM wR2 = 0.1638, GooF = S = 1.021, Restrained GooF = 1.021 for all data REM R1 = 0.0607 for 8445 Fo > 4sig(Fo) and 0.1190 for all 14732 data REM 563 parameters refined using 0 restraints END WGHT 0.0743 0.4416 REM Highest difference peak 0.517, deepest hole -0.271, 1-sigma level 0.059 Q1 1 0.1406 0.0562 0.4003 11.00000 0.05 0.52 Q2 1 0.5401 0.3189 0.4063 11.00000 0.05 0.48 Q3 1 0.2057 0.0494 0.4691 11.00000 0.05 0.45 ; _shelx_res_checksum 58284 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Al Al 0.25264(5) 0.28746(3) 0.62374(3) 0.02869(16) Uani 1 1 d . . P1 P 0.18992(5) 0.32570(3) 0.51776(3) 0.03204(14) Uani 1 1 d . . P2 P 0.30332(5) 0.18390(3) 0.57606(3) 0.03250(15) Uani 1 1 d . . S1 S -0.11590(5) 0.12323(4) 0.43887(3) 0.04777(18) Uani 1 1 d . . S2 S 0.58796(6) 0.29853(4) 0.43250(4) 0.0552(2) Uani 1 1 d . . N1 N 0.35953(14) 0.33861(9) 0.67634(8) 0.0304(4) Uani 1 1 d . . N2 N 0.14882(14) 0.28916(9) 0.67681(8) 0.0323(4) Uani 1 1 d . . N3 N 0.01723(14) 0.23074(10) 0.46927(8) 0.0332(4) Uani 1 1 d . . N4 N 0.09352(14) 0.13748(9) 0.50421(9) 0.0337(4) Uani 1 1 d . . N5 N 0.46314(15) 0.22868(10) 0.50108(9) 0.0364(4) Uani 1 1 d . . N6 N 0.39122(16) 0.32307(9) 0.46654(9) 0.0359(4) Uani 1 1 d . . C1 C 0.0876(2) 0.29738(15) 0.77828(12) 0.0521(7) Uani 1 1 d . . H1A H 0.014217 0.294830 0.752120 0.078 Uiso 1 1 calc R U H1B H 0.091254 0.335560 0.806337 0.078 Uiso 1 1 calc R U H1C H 0.102421 0.256744 0.803000 0.078 Uiso 1 1 calc R U C2 C 0.17235(19) 0.30511(12) 0.73726(11) 0.0371(5) Uani 1 1 d . . C3 C 0.27371(19) 0.33013(13) 0.76601(10) 0.0397(6) Uani 1 1 d . . H3A H 0.285886 0.334281 0.810154 0.048 Uiso 1 1 calc R U C4 C 0.35938(19) 0.34978(12) 0.73700(10) 0.0362(5) Uani 1 1 d . . C5 C 0.4533(2) 0.38609(14) 0.77678(11) 0.0467(6) Uani 1 1 d . . H5A H 0.485906 0.416861 0.750706 0.070 Uiso 1 1 calc R U H5B H 0.508904 0.354170 0.796179 0.070 Uiso 1 1 calc R U H5C H 0.426089 0.410904 0.809378 0.070 Uiso 1 1 calc R U C6 C 0.44396(18) 0.36805(12) 0.64736(10) 0.0339(5) Uani 1 1 d . . C7 C 0.41713(19) 0.42617(12) 0.61190(11) 0.0375(5) Uani 1 1 d . . C8 C 0.4929(2) 0.44882(14) 0.57786(12) 0.0506(7) Uani 1 1 d . . H8A H 0.477138 0.487719 0.553305 0.061 Uiso 1 1 calc R U C9 C 0.5907(2) 0.41646(16) 0.57865(14) 0.0598(8) Uani 1 1 d . . H9A H 0.639890 0.431866 0.553292 0.072 Uiso 1 1 calc R U C10 C 0.6173(2) 0.36213(15) 0.61585(14) 0.0553(7) Uani 1 1 d . . H10A H 0.686335 0.341229 0.617049 0.066 Uiso 1 1 calc R U C11 C 0.54599(19) 0.33682(13) 0.65188(11) 0.0404(6) Uani 1 1 d . . C12 C 0.5824(2) 0.27906(14) 0.69588(12) 0.0468(6) Uani 1 1 d . . H12A H 0.524752 0.271968 0.721691 0.056 Uiso 1 1 calc R U C13 C 0.6909(2) 0.29524(19) 0.74051(17) 0.0781(10) Uani 1 1 d . . H13A H 0.682559 0.336509 0.762794 0.117 Uiso 1 1 calc R U H13B H 0.709443 0.259117 0.770658 0.117 Uiso 1 1 calc R U H13C H 0.749625 0.300379 0.716490 0.117 Uiso 1 1 calc R U C14 C 0.5941(2) 0.21510(15) 0.66097(14) 0.0576(7) Uani 1 1 d . . H14A H 0.617513 0.179452 0.691014 0.086 Uiso 1 1 calc R U H14B H 0.523225 0.203550 0.634913 0.086 Uiso 1 1 calc R U H14C H 0.648966 0.221077 0.634482 0.086 Uiso 1 1 calc R U C15 C 0.3134(2) 0.46467(13) 0.61400(12) 0.0462(6) Uani 1 1 d . . H15A H 0.254711 0.431797 0.617910 0.055 Uiso 1 1 calc R U C16 C 0.2708(3) 0.50702(15) 0.55699(14) 0.0644(8) Uani 1 1 d . . H16A H 0.203718 0.529918 0.562698 0.097 Uiso 1 1 calc R U H16B H 0.326685 0.539731 0.551614 0.097 Uiso 1 1 calc R U H16C H 0.254614 0.478731 0.519890 0.097 Uiso 1 1 calc R U C17 C 0.3270(4) 0.5094(2) 0.67057(16) 0.1114(17) Uani 1 1 d . . H17A H 0.258482 0.533578 0.670535 0.167 Uiso 1 1 calc R U H17B H 0.344897 0.482587 0.708579 0.167 Uiso 1 1 calc R U H17C H 0.386547 0.540980 0.669231 0.167 Uiso 1 1 calc R U C18 C 0.03688(17) 0.27435(13) 0.64614(10) 0.0369(5) Uani 1 1 d . . C19 C -0.02454(19) 0.32619(14) 0.61262(11) 0.0436(6) Uani 1 1 d . . C20 C -0.1234(2) 0.30919(18) 0.57448(12) 0.0558(8) Uani 1 1 d . . H20A H -0.166871 0.342776 0.551365 0.067 Uiso 1 1 calc R U C21 C -0.1595(2) 0.2446(2) 0.56950(14) 0.0646(9) Uani 1 1 d . . H21A H -0.224271 0.233599 0.540505 0.077 Uiso 1 1 calc R U C22 C -0.1033(2) 0.19660(17) 0.60573(13) 0.0589(8) Uani 1 1 d . . H22A H -0.132176 0.152911 0.603768 0.071 Uiso 1 1 calc R U C23 C -0.00394(19) 0.21004(14) 0.64582(11) 0.0442(6) Uani 1 1 d . . C24 C 0.0507(2) 0.15705(14) 0.69091(13) 0.0487(7) Uani 1 1 d . . H24A H 0.116161 0.177550 0.718095 0.058 Uiso 1 1 calc R U C25 C -0.0307(3) 0.13614(19) 0.73341(16) 0.0767(10) Uani 1 1 d . . H25A H -0.055156 0.175496 0.753228 0.115 Uiso 1 1 calc R U H25B H -0.094299 0.114050 0.708170 0.115 Uiso 1 1 calc R U H25C H 0.006078 0.105653 0.765657 0.115 Uiso 1 1 calc R U C26 C 0.0898(3) 0.09726(16) 0.65973(14) 0.0650(8) Uani 1 1 d . . H26A H 0.123813 0.065597 0.691647 0.098 Uiso 1 1 calc R U H26B H 0.027163 0.076265 0.632552 0.098 Uiso 1 1 calc R U H26C H 0.143786 0.111093 0.634766 0.098 Uiso 1 1 calc R U C27 C 0.0117(2) 0.39775(15) 0.62081(13) 0.0553(7) Uani 1 1 d . . H27A H 0.093771 0.398399 0.630619 0.066 Uiso 1 1 calc R U C28 C -0.0295(4) 0.4289(2) 0.67571(17) 0.0947(13) Uani 1 1 d . . H28A H -0.005412 0.475132 0.680352 0.142 Uiso 1 1 calc R U H28B H -0.109953 0.427101 0.668124 0.142 Uiso 1 1 calc R U H28C H 0.000263 0.404440 0.713975 0.142 Uiso 1 1 calc R U C29 C -0.0253(3) 0.44089(18) 0.56363(15) 0.0770(10) Uani 1 1 d . . H29A H 0.001261 0.486222 0.572626 0.116 Uiso 1 1 calc R U H29B H 0.004754 0.423246 0.528507 0.116 Uiso 1 1 calc R U H29C H -0.105684 0.441018 0.552882 0.116 Uiso 1 1 calc R U C30 C -0.00051(18) 0.16424(12) 0.47029(10) 0.0354(5) Uani 1 1 d . . C31 C 0.12060(17) 0.24588(11) 0.50380(10) 0.0312(5) Uani 1 1 d . . C32 C 0.16762(17) 0.18791(11) 0.52599(10) 0.0307(5) Uani 1 1 d . . C33 C 0.47936(19) 0.28298(12) 0.46640(11) 0.0401(6) Uani 1 1 d . . C34 C 0.32064(18) 0.29488(11) 0.50219(10) 0.0318(5) Uani 1 1 d . . C35 C 0.36643(17) 0.23697(11) 0.52425(10) 0.0327(5) Uani 1 1 d . . C36 C -0.06049(18) 0.27830(13) 0.43524(11) 0.0381(5) Uani 1 1 d . . H36A H -0.052152 0.321119 0.457744 0.046 Uiso 1 1 calc R U H36B H -0.136172 0.262205 0.434449 0.046 Uiso 1 1 calc R U C37 C -0.04472(19) 0.28928(13) 0.36922(11) 0.0397(6) Uani 1 1 d . . H37A H -0.054916 0.246835 0.346140 0.048 Uiso 1 1 calc R U H37B H 0.031183 0.304794 0.369677 0.048 Uiso 1 1 calc R U C38 C -0.1258(2) 0.34017(15) 0.33587(13) 0.0568(7) Uani 1 1 d . . H38A H -0.201205 0.325870 0.338404 0.068 Uiso 1 1 calc R U H38B H -0.112238 0.383063 0.357957 0.068 Uiso 1 1 calc R U C39 C -0.1191(3) 0.35030(17) 0.26847(13) 0.0666(9) Uani 1 1 d . . H39A H -0.173306 0.383519 0.250093 0.100 Uiso 1 1 calc R U H39B H -0.045286 0.365632 0.265460 0.100 Uiso 1 1 calc R U H39C H -0.134365 0.308366 0.245883 0.100 Uiso 1 1 calc R U C40 C 0.1152(2) 0.06618(12) 0.50979(11) 0.0411(6) Uani 1 1 d . . H40A H 0.051840 0.043957 0.522676 0.049 Uiso 1 1 calc R U H40B H 0.180517 0.058495 0.542848 0.049 Uiso 1 1 calc R U C41 C 0.1346(3) 0.03561(15) 0.44964(14) 0.0612(8) Uani 1 1 d . . H41A H 0.149920 -0.012142 0.456962 0.073 Uiso 1 1 calc R U H41B H 0.065976 0.039335 0.418146 0.073 Uiso 1 1 calc R U C42 C 0.2242(3) 0.06460(19) 0.42355(17) 0.0823(11) Uani 1 1 d . . H42A H 0.292764 0.062370 0.455186 0.099 Uiso 1 1 calc R U H42B H 0.207728 0.111878 0.414028 0.099 Uiso 1 1 calc R U C43 C 0.2422(3) 0.0294(2) 0.36392(17) 0.0940(12) Uani 1 1 d . . H43A H 0.302846 0.050602 0.348413 0.141 Uiso 1 1 calc R U H43B H 0.260125 -0.017283 0.373236 0.141 Uiso 1 1 calc R U H43C H 0.175066 0.032237 0.332067 0.141 Uiso 1 1 calc R U C44 C 0.53238(19) 0.16947(13) 0.50640(12) 0.0443(6) Uani 1 1 d . . H44A H 0.513666 0.140651 0.539586 0.053 Uiso 1 1 calc R U H44B H 0.610143 0.182940 0.519269 0.053 Uiso 1 1 calc R U C45 C 0.5202(2) 0.13023(14) 0.44676(14) 0.0557(7) Uani 1 1 d . . H45A H 0.541571 0.158280 0.413804 0.067 Uiso 1 1 calc R U H45B H 0.442151 0.117663 0.433034 0.067 Uiso 1 1 calc R U C46 C 0.5903(3) 0.06816(16) 0.45473(17) 0.0698(9) Uani 1 1 d . . H46A H 0.667621 0.081012 0.470624 0.084 Uiso 1 1 calc R U H46B H 0.566594 0.039708 0.486680 0.084 Uiso 1 1 calc R U C47 C 0.5854(4) 0.0283(2) 0.3959(2) 0.1110(15) Uani 1 1 d . . H47A H 0.632626 -0.010810 0.404830 0.167 Uiso 1 1 calc R U H47B H 0.509522 0.014123 0.380282 0.167 Uiso 1 1 calc R U H47C H 0.610715 0.055494 0.364200 0.167 Uiso 1 1 calc R U C48 C 0.3702(2) 0.38390(12) 0.43083(12) 0.0439(6) Uani 1 1 d . . H48A H 0.441050 0.402910 0.424845 0.053 Uiso 1 1 calc R U H48B H 0.335074 0.416229 0.455008 0.053 Uiso 1 1 calc R U C49 C 0.2975(2) 0.37407(14) 0.36800(12) 0.0517(7) Uani 1 1 d . . H49A H 0.227583 0.353298 0.373418 0.062 Uiso 1 1 calc R U H49B H 0.334047 0.343932 0.342501 0.062 Uiso 1 1 calc R U C50 C 0.2737(3) 0.44032(16) 0.33426(15) 0.0683(9) Uani 1 1 d . . H50A H 0.241710 0.470933 0.361444 0.082 Uiso 1 1 calc R U H50B H 0.343999 0.459717 0.327703 0.082 Uiso 1 1 calc R U C51 C 0.1985(3) 0.4357(2) 0.27362(16) 0.0857(11) Uani 1 1 d . . H51A H 0.187274 0.479871 0.254897 0.128 Uiso 1 1 calc R U H51B H 0.230319 0.406450 0.245873 0.128 Uiso 1 1 calc R U H51C H 0.127883 0.417683 0.279663 0.128 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 Al 0.0278(3) 0.0324(4) 0.0261(3) 0.0021(3) 0.0058(3) -0.0031(3) P1 0.0362(3) 0.0302(3) 0.0298(3) 0.0019(2) 0.0063(2) -0.0016(2) P2 0.0299(3) 0.0329(3) 0.0343(3) 0.0057(2) 0.0049(2) -0.0026(2) S1 0.0381(3) 0.0590(5) 0.0430(4) -0.0001(3) -0.0006(3) -0.0172(3) S2 0.0521(4) 0.0626(5) 0.0587(4) -0.0021(3) 0.0303(3) -0.0137(3) N1 0.0312(9) 0.0326(11) 0.0275(9) 0.0031(8) 0.0057(7) -0.0033(8) N2 0.0299(9) 0.0400(12) 0.0274(9) 0.0046(8) 0.0063(8) -0.0006(8) N3 0.0305(9) 0.0370(12) 0.0312(10) 0.0039(8) 0.0034(8) -0.0015(8) N4 0.0336(10) 0.0320(11) 0.0346(10) 0.0030(8) 0.0044(8) -0.0082(8) N5 0.0343(10) 0.0382(12) 0.0388(11) 0.0007(9) 0.0123(9) -0.0050(9) N6 0.0418(11) 0.0331(11) 0.0348(10) 0.0003(8) 0.0122(9) -0.0101(9) C1 0.0476(15) 0.075(2) 0.0373(14) 0.0013(13) 0.0172(12) -0.0009(14) C2 0.0387(12) 0.0435(15) 0.0304(12) 0.0054(10) 0.0100(10) 0.0037(11) C3 0.0435(13) 0.0514(16) 0.0242(11) -0.0001(10) 0.0065(10) 0.0008(11) C4 0.0398(13) 0.0369(14) 0.0304(12) 0.0003(10) 0.0024(10) 0.0007(10) C5 0.0515(15) 0.0548(17) 0.0318(13) -0.0068(11) 0.0031(11) -0.0129(13) C6 0.0358(12) 0.0359(13) 0.0295(11) -0.0033(9) 0.0046(9) -0.0110(10) C7 0.0462(13) 0.0305(13) 0.0351(12) -0.0025(10) 0.0055(10) -0.0113(10) C8 0.0618(17) 0.0423(16) 0.0482(16) 0.0056(12) 0.0120(13) -0.0194(13) C9 0.0572(17) 0.070(2) 0.0571(18) 0.0040(15) 0.0234(14) -0.0252(16) C10 0.0403(14) 0.064(2) 0.0649(19) -0.0022(15) 0.0193(13) -0.0103(13) C11 0.0348(12) 0.0455(15) 0.0408(13) -0.0028(11) 0.0064(10) -0.0083(11) C12 0.0340(12) 0.0580(18) 0.0467(15) 0.0066(13) 0.0029(11) 0.0030(12) C13 0.0508(18) 0.096(3) 0.076(2) 0.000(2) -0.0172(16) 0.0020(18) C14 0.0526(16) 0.0571(19) 0.0614(18) 0.0023(14) 0.0061(14) 0.0045(14) C15 0.0601(16) 0.0324(15) 0.0466(15) 0.0036(11) 0.0109(13) -0.0012(12) C16 0.086(2) 0.0497(19) 0.0531(17) 0.0054(14) 0.0031(16) 0.0108(16) C17 0.174(4) 0.096(3) 0.053(2) -0.024(2) -0.007(2) 0.069(3) C18 0.0283(11) 0.0545(16) 0.0300(12) 0.0026(10) 0.0108(9) -0.0005(11) C19 0.0335(12) 0.0665(19) 0.0339(13) 0.0055(12) 0.0145(10) 0.0100(12) C20 0.0288(12) 0.100(3) 0.0408(15) 0.0126(15) 0.0110(11) 0.0130(15) C21 0.0288(13) 0.119(3) 0.0452(16) -0.0004(18) 0.0048(12) -0.0137(16) C22 0.0431(15) 0.086(2) 0.0488(17) 0.0013(15) 0.0133(13) -0.0251(15) C23 0.0356(12) 0.0634(18) 0.0359(13) 0.0020(12) 0.0130(11) -0.0090(12) C24 0.0478(15) 0.0536(17) 0.0479(15) 0.0037(13) 0.0169(12) -0.0110(13) C25 0.077(2) 0.090(3) 0.072(2) 0.0257(19) 0.0368(18) -0.0089(19) C26 0.080(2) 0.058(2) 0.0603(19) 0.0075(15) 0.0218(17) -0.0142(16) C27 0.0511(16) 0.062(2) 0.0539(17) 0.0081(14) 0.0127(13) 0.0201(14) C28 0.145(4) 0.079(3) 0.064(2) -0.0018(19) 0.029(2) 0.033(3) C29 0.096(3) 0.075(2) 0.063(2) 0.0225(17) 0.0229(18) 0.028(2) C30 0.0338(12) 0.0432(15) 0.0296(12) 0.0013(10) 0.0074(9) -0.0051(10) C31 0.0297(11) 0.0362(13) 0.0274(11) 0.0004(9) 0.0045(9) -0.0033(9) C32 0.0313(11) 0.0300(13) 0.0308(11) 0.0011(9) 0.0058(9) -0.0058(9) C33 0.0413(13) 0.0407(15) 0.0400(13) -0.0051(11) 0.0119(11) -0.0106(11) C34 0.0359(11) 0.0305(13) 0.0304(11) -0.0008(9) 0.0102(9) -0.0077(10) C35 0.0310(11) 0.0357(13) 0.0323(12) -0.0008(10) 0.0088(9) -0.0048(10) C36 0.0334(12) 0.0429(15) 0.0367(13) 0.0001(10) 0.0030(10) 0.0045(10) C37 0.0410(13) 0.0423(15) 0.0346(13) 0.0035(11) 0.0036(10) 0.0046(11) C38 0.0651(18) 0.0567(19) 0.0458(16) 0.0062(13) 0.0030(14) 0.0140(15) C39 0.072(2) 0.076(2) 0.0496(17) 0.0225(16) 0.0047(15) 0.0108(17) C40 0.0464(14) 0.0325(14) 0.0441(14) 0.0057(11) 0.0076(11) -0.0066(11) C41 0.077(2) 0.0416(17) 0.068(2) -0.0018(14) 0.0211(16) -0.0019(15) C42 0.101(3) 0.076(3) 0.081(2) -0.0122(19) 0.044(2) -0.011(2) C43 0.106(3) 0.108(3) 0.078(3) -0.025(2) 0.041(2) 0.000(2) C44 0.0332(12) 0.0484(16) 0.0520(15) 0.0000(12) 0.0097(11) 0.0016(11) C45 0.0552(17) 0.0486(18) 0.0655(19) -0.0038(14) 0.0172(14) 0.0079(13) C46 0.0559(18) 0.055(2) 0.104(3) 0.0020(18) 0.0291(18) 0.0101(15) C47 0.132(4) 0.077(3) 0.128(4) -0.022(3) 0.033(3) 0.040(3) C48 0.0587(15) 0.0320(14) 0.0453(15) 0.0033(11) 0.0211(12) -0.0091(12) C49 0.0621(17) 0.0499(17) 0.0444(15) 0.0045(12) 0.0130(13) -0.0043(14) C50 0.087(2) 0.061(2) 0.0542(19) 0.0015(15) 0.0064(17) 0.0026(18) C51 0.095(3) 0.093(3) 0.067(2) 0.004(2) 0.011(2) 0.015(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 '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 N2 Al N1 95.68(8) N2 Al P1 116.52(6) N1 Al P1 117.88(6) N2 Al P2 122.08(7) N1 Al P2 120.93(6) P1 Al P2 85.95(3) C31 P1 C34 94.26(10) C31 P1 Al 86.21(7) C34 P1 Al 86.14(7) C32 P2 C35 93.29(10) C32 P2 Al 86.30(7) C35 P2 Al 86.39(8) C4 N1 C6 119.78(18) C4 N1 Al 124.02(15) C6 N1 Al 116.18(14) C2 N2 C18 121.06(17) C2 N2 Al 124.28(15) C18 N2 Al 114.61(13) C30 N3 C31 110.04(18) C30 N3 C36 124.33(19) C31 N3 C36 125.61(19) C30 N4 C32 109.59(19) C30 N4 C40 123.83(19) C32 N4 C40 126.23(19) C33 N5 C35 109.27(19) C33 N5 C44 123.58(19) C35 N5 C44 126.87(19) C33 N6 C34 110.28(19) C33 N6 C48 124.44(19) C34 N6 C48 125.1(2) C2 C1 H1A 109.5 C2 C1 H1B 109.5 H1A C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 N2 C2 C3 123.0(2) N2 C2 C1 120.9(2) C3 C2 C1 116.2(2) C2 C3 C4 126.9(2) C2 C3 H3A 116.5 C4 C3 H3A 116.5 N1 C4 C3 122.9(2) N1 C4 C5 120.4(2) C3 C4 C5 116.7(2) C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C11 C6 C7 122.0(2) C11 C6 N1 120.1(2) C7 C6 N1 117.8(2) C8 C7 C6 117.2(2) C8 C7 C15 121.0(2) C6 C7 C15 121.7(2) C9 C8 C7 121.6(3) C9 C8 H8A 119.2 C7 C8 H8A 119.2 C10 C9 C8 120.2(2) C10 C9 H9A 119.9 C8 C9 H9A 119.9 C9 C10 C11 121.6(3) C9 C10 H10A 119.2 C11 C10 H10A 119.2 C10 C11 C6 117.3(2) C10 C11 C12 119.6(2) C6 C11 C12 123.0(2) C14 C12 C11 112.3(2) C14 C12 C13 110.1(2) C11 C12 C13 110.8(2) C14 C12 H12A 107.8 C11 C12 H12A 107.8 C13 C12 H12A 107.8 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 C7 C15 C17 111.5(3) C7 C15 C16 115.5(2) C17 C15 C16 107.5(2) C7 C15 H15A 107.3 C17 C15 H15A 107.3 C16 C15 H15A 107.3 C15 C16 H16A 109.5 C15 C16 H16B 109.5 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C15 C17 H17A 109.5 C15 C17 H17B 109.5 H17A C17 H17B 109.5 C15 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C23 C18 C19 121.8(2) C23 C18 N2 120.6(2) C19 C18 N2 117.4(2) C20 C19 C18 117.1(3) C20 C19 C27 121.0(3) C18 C19 C27 121.8(2) C21 C20 C19 121.3(3) C21 C20 H20A 119.4 C19 C20 H20A 119.4 C22 C21 C20 120.5(3) C22 C21 H21A 119.8 C20 C21 H21A 119.8 C21 C22 C23 121.4(3) C21 C22 H22A 119.3 C23 C22 H22A 119.3 C18 C23 C22 117.5(3) C18 C23 C24 122.3(2) C22 C23 C24 120.0(3) C26 C24 C23 114.4(2) C26 C24 C25 110.6(2) C23 C24 C25 108.5(2) C26 C24 H24A 107.7 C23 C24 H24A 107.7 C25 C24 H24A 107.7 C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 H26A C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C19 C27 C29 114.4(3) C19 C27 C28 110.5(3) C29 C27 C28 108.4(3) C19 C27 H27A 107.8 C29 C27 H27A 107.8 C28 C27 H27A 107.8 C27 C28 H28A 109.5 C27 C28 H28B 109.5 H28A C28 H28B 109.5 C27 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C27 C29 H29A 109.5 C27 C29 H29B 109.5 H29A C29 H29B 109.5 C27 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 N3 C30 N4 105.93(18) N3 C30 S1 127.31(18) N4 C30 S1 126.72(18) C32 C31 N3 107.06(19) C32 C31 P1 123.08(16) N3 C31 P1 129.83(17) C31 C32 N4 107.33(19) C31 C32 P2 122.49(17) N4 C32 P2 130.17(17) N6 C33 N5 105.88(18) N6 C33 S2 126.82(19) N5 C33 S2 127.27(19) C35 C34 N6 106.64(19) C35 C34 P1 123.89(16) N6 C34 P1 129.47(17) C34 C35 N5 107.89(19) C34 C35 P2 121.75(16) N5 C35 P2 130.36(17) N3 C36 C37 113.00(19) N3 C36 H36A 109.0 C37 C36 H36A 109.0 N3 C36 H36B 109.0 C37 C36 H36B 109.0 H36A C36 H36B 107.8 C36 C37 C38 111.3(2) C36 C37 H37A 109.4 C38 C37 H37A 109.4 C36 C37 H37B 109.4 C38 C37 H37B 109.4 H37A C37 H37B 108.0 C39 C38 C37 114.0(2) C39 C38 H38A 108.8 C37 C38 H38A 108.8 C39 C38 H38B 108.8 C37 C38 H38B 108.8 H38A C38 H38B 107.7 C38 C39 H39A 109.5 C38 C39 H39B 109.5 H39A C39 H39B 109.5 C38 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 N4 C40 C41 112.7(2) N4 C40 H40A 109.0 C41 C40 H40A 109.0 N4 C40 H40B 109.0 C41 C40 H40B 109.0 H40A C40 H40B 107.8 C42 C41 C40 115.6(3) C42 C41 H41A 108.4 C40 C41 H41A 108.4 C42 C41 H41B 108.4 C40 C41 H41B 108.4 H41A C41 H41B 107.4 C41 C42 C43 112.8(3) C41 C42 H42A 109.0 C43 C42 H42A 109.0 C41 C42 H42B 109.0 C43 C42 H42B 109.0 H42A C42 H42B 107.8 C42 C43 H43A 109.5 C42 C43 H43B 109.5 H43A C43 H43B 109.5 C42 C43 H43C 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 N5 C44 C45 113.5(2) N5 C44 H44A 108.9 C45 C44 H44A 108.9 N5 C44 H44B 108.9 C45 C44 H44B 108.9 H44A C44 H44B 107.7 C44 C45 C46 111.9(3) C44 C45 H45A 109.2 C46 C45 H45A 109.2 C44 C45 H45B 109.2 C46 C45 H45B 109.2 H45A C45 H45B 107.9 C47 C46 C45 114.4(3) C47 C46 H46A 108.7 C45 C46 H46A 108.7 C47 C46 H46B 108.7 C45 C46 H46B 108.7 H46A C46 H46B 107.6 C46 C47 H47A 109.5 C46 C47 H47B 109.5 H47A C47 H47B 109.5 C46 C47 H47C 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 N6 C48 C49 113.2(2) N6 C48 H48A 108.9 C49 C48 H48A 108.9 N6 C48 H48B 108.9 C49 C48 H48B 108.9 H48A C48 H48B 107.8 C48 C49 C50 110.6(2) C48 C49 H49A 109.5 C50 C49 H49A 109.5 C48 C49 H49B 109.5 C50 C49 H49B 109.5 H49A C49 H49B 108.1 C51 C50 C49 114.2(3) C51 C50 H50A 108.7 C49 C50 H50A 108.7 C51 C50 H50B 108.7 C49 C50 H50B 108.7 H50A C50 H50B 107.6 C50 C51 H51A 109.5 C50 C51 H51B 109.5 H51A C51 H51B 109.5 C50 C51 H51C 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Al N2 1.8871(18) Al N1 1.8884(19) Al P1 2.4222(8) Al P2 2.4690(9) P1 C31 1.825(2) P1 C34 1.827(2) P2 C32 1.827(2) P2 C35 1.836(2) S1 C30 1.683(2) S2 C33 1.683(2) N1 C4 1.343(3) N1 C6 1.449(3) N2 C2 1.335(3) N2 C18 1.453(3) N3 C30 1.361(3) N3 C31 1.393(3) N3 C36 1.460(3) N4 C30 1.369(3) N4 C32 1.393(3) N4 C40 1.465(3) N5 C33 1.368(3) N5 C35 1.396(3) N5 C44 1.464(3) N6 C33 1.360(3) N6 C34 1.397(3) N6 C48 1.451(3) C1 C2 1.511(3) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 C3 1.389(3) C3 C4 1.393(3) C3 H3A 0.9500 C4 C5 1.505(3) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 C11 1.400(3) C6 C7 1.411(3) C7 C8 1.381(3) C7 C15 1.511(3) C8 C9 1.374(4) C8 H8A 0.9500 C9 C10 1.367(4) C9 H9A 0.9500 C10 C11 1.387(3) C10 H10A 0.9500 C11 C12 1.524(4) C12 C14 1.520(4) C12 C13 1.539(4) 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 C17 1.513(4) C15 C16 1.519(4) C15 H15A 1.0000 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 C23 1.393(4) C18 C19 1.414(3) C19 C20 1.388(4) C19 C27 1.514(4) C20 C21 1.376(5) C20 H20A 0.9500 C21 C22 1.358(4) C21 H21A 0.9500 C22 C23 1.396(4) C22 H22A 0.9500 C23 C24 1.523(4) C24 C26 1.510(4) C24 C25 1.552(4) C24 H24A 1.0000 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 C29 1.520(4) C27 C28 1.524(4) C27 H27A 1.0000 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C31 C32 1.356(3) C34 C35 1.348(3) C36 C37 1.506(3) C36 H36A 0.9900 C36 H36B 0.9900 C37 C38 1.523(3) C37 H37A 0.9900 C37 H37B 0.9900 C38 C39 1.502(4) C38 H38A 0.9900 C38 H38B 0.9900 C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 C41 1.510(4) C40 H40A 0.9900 C40 H40B 0.9900 C41 C42 1.463(4) C41 H41A 0.9900 C41 H41B 0.9900 C42 C43 1.536(4) C42 H42A 0.9900 C42 H42B 0.9900 C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C44 C45 1.506(4) C44 H44A 0.9900 C44 H44B 0.9900 C45 C46 1.517(4) C45 H45A 0.9900 C45 H45B 0.9900 C46 C47 1.508(5) C46 H46A 0.9900 C46 H46B 0.9900 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C48 C49 1.504(4) C48 H48A 0.9900 C48 H48B 0.9900 C49 C50 1.529(4) C49 H49A 0.9900 C49 H49B 0.9900 C50 C51 1.471(4) C50 H50A 0.9900 C50 H50B 0.9900 C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C3 H3A S1 0.95 2.97 3.877(2) 160.5 4_666 yes C41 H41B S1 0.99 2.92 3.543(3) 121.5 . yes C45 H45A S2 0.99 2.90 3.529(3) 121.9 . yes C3 H3A S1 0.95 2.97 3.877(2) 160.5 4_666 yes C41 H41B S1 0.99 2.92 3.543(3) 121.5 . yes C45 H45A S2 0.99 2.90 3.529(3) 121.9 . yes 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 N2 Al N1 C4 16.5(2) P1 Al N1 C4 140.53(17) P2 Al N1 C4 -116.53(17) N2 Al N1 C6 -162.03(16) P1 Al N1 C6 -37.95(17) P2 Al N1 C6 64.98(17) N1 Al N2 C2 -17.2(2) P1 Al N2 C2 -142.32(17) P2 Al N2 C2 114.99(18) N1 Al N2 C18 160.09(16) P1 Al N2 C18 35.00(18) P2 Al N2 C18 -67.69(17) C18 N2 C2 C3 -169.0(2) Al N2 C2 C3 8.1(3) C18 N2 C2 C1 10.2(3) Al N2 C2 C1 -172.62(19) N2 C2 C3 C4 8.3(4) C1 C2 C3 C4 -171.0(2) C6 N1 C4 C3 171.8(2) Al N1 C4 C3 -6.7(3) C6 N1 C4 C5 -7.0(3) Al N1 C4 C5 174.56(18) C2 C3 C4 N1 -9.1(4) C2 C3 C4 C5 169.7(2) C4 N1 C6 C11 84.3(3) Al N1 C6 C11 -97.1(2) C4 N1 C6 C7 -99.4(2) Al N1 C6 C7 79.2(2) C11 C6 C7 C8 4.5(3) N1 C6 C7 C8 -171.7(2) C11 C6 C7 C15 -171.7(2) N1 C6 C7 C15 12.1(3) C6 C7 C8 C9 -0.3(4) C15 C7 C8 C9 175.9(2) C7 C8 C9 C10 -3.0(4) C8 C9 C10 C11 2.3(5) C9 C10 C11 C6 1.7(4) C9 C10 C11 C12 -175.9(3) C7 C6 C11 C10 -5.2(4) N1 C6 C11 C10 170.9(2) C7 C6 C11 C12 172.4(2) N1 C6 C11 C12 -11.5(3) C10 C11 C12 C14 -68.9(3) C6 C11 C12 C14 113.6(3) C10 C11 C12 C13 54.7(3) C6 C11 C12 C13 -122.9(3) C8 C7 C15 C17 -95.0(3) C6 C7 C15 C17 81.1(3) C8 C7 C15 C16 28.1(4) C6 C7 C15 C16 -155.8(2) C2 N2 C18 C23 -88.4(3) Al N2 C18 C23 94.2(2) C2 N2 C18 C19 96.8(3) Al N2 C18 C19 -80.6(2) C23 C18 C19 C20 -5.9(3) N2 C18 C19 C20 168.80(19) C23 C18 C19 C27 170.3(2) N2 C18 C19 C27 -15.0(3) C18 C19 C20 C21 -0.2(3) C27 C19 C20 C21 -176.4(2) C19 C20 C21 C22 5.2(4) C20 C21 C22 C23 -4.4(4) C19 C18 C23 C22 6.8(3) N2 C18 C23 C22 -167.8(2) C19 C18 C23 C24 -168.0(2) N2 C18 C23 C24 17.4(3) C21 C22 C23 C18 -1.6(4) C21 C22 C23 C24 173.3(3) C18 C23 C24 C26 -119.6(3) C22 C23 C24 C26 65.8(3) C18 C23 C24 C25 116.5(3) C22 C23 C24 C25 -58.1(3) C20 C19 C27 C29 -32.4(3) C18 C19 C27 C29 151.5(2) C20 C19 C27 C28 90.3(3) C18 C19 C27 C28 -85.8(3) C31 N3 C30 N4 -1.6(2) C36 N3 C30 N4 176.79(18) C31 N3 C30 S1 176.17(16) C36 N3 C30 S1 -5.4(3) C32 N4 C30 N3 2.2(2) C40 N4 C30 N3 -171.45(19) C32 N4 C30 S1 -175.66(17) C40 N4 C30 S1 10.7(3) C30 N3 C31 C32 0.5(2) C36 N3 C31 C32 -177.91(19) C30 N3 C31 P1 178.69(16) C36 N3 C31 P1 0.3(3) C34 P1 C31 C32 43.6(2) Al P1 C31 C32 -42.24(18) C34 P1 C31 N3 -134.3(2) Al P1 C31 N3 139.82(19) N3 C31 C32 N4 0.8(2) P1 C31 C32 N4 -177.50(14) N3 C31 C32 P2 -178.25(14) P1 C31 C32 P2 3.4(3) C30 N4 C32 C31 -1.9(2) C40 N4 C32 C31 171.5(2) C30 N4 C32 P2 177.10(17) C40 N4 C32 P2 -9.5(3) C35 P2 C32 C31 -49.2(2) Al P2 C32 C31 36.95(18) C35 P2 C32 N4 131.9(2) Al P2 C32 N4 -141.9(2) C34 N6 C33 N5 1.2(3) C48 N6 C33 N5 -174.6(2) C34 N6 C33 S2 -176.91(18) C48 N6 C33 S2 7.3(3) C35 N5 C33 N6 -2.1(2) C44 N5 C33 N6 172.2(2) C35 N5 C33 S2 175.99(18) C44 N5 C33 S2 -9.7(3) C33 N6 C34 C35 0.2(3) C48 N6 C34 C35 175.9(2) C33 N6 C34 P1 -179.02(18) C48 N6 C34 P1 -3.3(3) C31 P1 C34 C35 -44.1(2) Al P1 C34 C35 41.82(19) C31 P1 C34 N6 135.0(2) Al P1 C34 N6 -139.1(2) N6 C34 C35 N5 -1.5(2) P1 C34 C35 N5 177.79(15) N6 C34 C35 P2 178.00(15) P1 C34 C35 P2 -2.7(3) C33 N5 C35 C34 2.3(3) C44 N5 C35 C34 -171.8(2) C33 N5 C35 P2 -177.14(18) C44 N5 C35 P2 8.8(3) C32 P2 C35 C34 48.7(2) Al P2 C35 C34 -37.37(19) C32 P2 C35 N5 -132.0(2) Al P2 C35 N5 142.0(2) C30 N3 C36 C37 -89.3(3) C31 N3 C36 C37 88.9(3) N3 C36 C37 C38 -178.9(2) C36 C37 C38 C39 -176.4(3) C30 N4 C40 C41 69.8(3) C32 N4 C40 C41 -102.7(3) N4 C40 C41 C42 57.1(4) C40 C41 C42 C43 177.7(3) C33 N5 C44 C45 -68.8(3) C35 N5 C44 C45 104.4(3) N5 C44 C45 C46 -178.1(2) C44 C45 C46 C47 -177.5(3) C33 N6 C48 C49 93.0(3) C34 N6 C48 C49 -82.1(3) N6 C48 C49 C50 177.1(2) C48 C49 C50 C51 -177.1(3)