#------------------------------------------------------------------------------ #$Date: 2020-04-23 00:57:24 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251058 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557863.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_1557863 loop_ _publ_author_name 'Navarro, Marta' 'S\'ANCHEZ-BARBA MERLO, LUIS FERNANDO' 'Garc\'es Osado, Andr\'es' 'Juan, Fernandez-Baeza' 'Fernandez, Israel' 'Lara, Agustin' 'Rodr\'iguez, Ana Mar\'ia' _publ_section_title ; Bimetallic Scorpionate-based Helical Organoaluminums for the Efficient Carbon Dioxide Fixation into a Variety of Cyclic Carbonates ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D0CY00593B _journal_year 2020 _chemical_formula_moiety 'C30 H40 Al2 N6, 0.5(C7 H8)' _chemical_formula_sum 'C33.5 H44 Al2 N6' _chemical_formula_weight 584.70 _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 geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2020-03-24 deposited with the CCDC. 2020-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 125.3250(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.637(3) _cell_length_b 9.3840(19) _cell_length_c 26.354(4) _cell_measurement_reflns_used 835 _cell_measurement_temperature 240(2) _cell_measurement_theta_max 16.287 _cell_measurement_theta_min 2.213 _cell_volume 3760.4(11) _computing_cell_refinement 'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)' _computing_data_collection 'Bruker APEX' _computing_data_reduction 'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)' _computing_molecular_graphics 'WINGX v2014.1 (Farrugia, 2012)' _computing_publication_material 'WINGX v2014.1 (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2013/4 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013/4 (Sheldrick, 2013)' _diffrn_ambient_temperature 240(2) _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'area detector, APEX' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_unetI/netI 0.1626 _diffrn_reflns_Laue_measured_fraction_full 0.968 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 17044 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.339 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.033 _exptl_crystal_description block _exptl_crystal_F_000 1252 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.635 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef 0.0084(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 412 _refine_ls_number_reflns 6577 _refine_ls_number_restraints 78 _refine_ls_restrained_S_all 0.981 _refine_ls_R_factor_all 0.2079 _refine_ls_R_factor_gt 0.0827 _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^)+(0.1308P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2149 _refine_ls_wR_factor_ref 0.2845 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2554 _reflns_number_total 6577 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy00593b3.cif _cod_data_source_block 8 _cod_original_cell_volume 3760.4(12) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C33.50 H44 Al2 N6' _cod_database_code 1557863 _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 0.981 _shelx_estimated_absorpt_t_max 0.989 _shelxl_version_number 2013-4 _shelx_res_file ; TITL AND_53 in P21/c CELL 0.71073 18.6370 9.3840 26.3540 90.000 125.325 90.000 ZERR 4.00 0.0034 0.0019 0.0040 0.000 0.00117 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N AL UNIT 134 176 24 8 MERG 2 OMIT -2.00 50.00 OMIT -5 1 7 OMIT -5 1 9 OMIT -2 2 6 OMIT -3 1 7 OMIT -2 1 4 OMIT -2 1 3 OMIT -3 0 6 OMIT -2 1 6 OMIT -1 2 2 OMIT -1 2 4 OMIT 0 1 4 OMIT -3 0 4 OMIT -4 3 9 OMIT -4 2 6 OMIT 2 1 1 OMIT -3 2 8 OMIT -2 2 4 OMIT -3 1 5 OMIT -3 3 6 OMIT 0 1 1 OMIT 2 0 0 OMIT 0 0 2 OMIT -1 0 2 OMIT 1 1 0 OMIT 1 0 2 OMIT 0 1 2 OMIT 1 2 3 OMIT -5 0 6 OMIT -2 2 5 OMIT 0 1 5 OMIT -2 2 7 OMIT -5 1 6 OMIT -1 0 4 OMIT -4 2 7 OMIT -2 2 8 OMIT 1 2 1 OMIT -2 1 1 OMIT -3 3 8 OMIT -2 1 5 OMIT -2 1 2 OMIT -4 1 6 OMIT -3 2 9 OMIT -5 3 11 OMIT -4 0 8 OMIT 1 1 2 OMIT -3 0 2 OMIT -1 2 9 OMIT -5 1 10 DFIX 1.53 C31 C37 DFIX 1.53 C41 C47 SADI C31 C32 C32 C33 C33 C34 C34 C35 C35 C36 C36 C31 SADI 0.04 C31 C33 C32 C34 C33 C35 C34 C36 C35 C31 C36 C32 SADI 0.04 C31 C34 C32 C35 C33 C36 SADI 0.04 C36 C37 C32 C37 SADI C41 C42 C42 C43 C43 C44 C44 C45 C45 C46 C46 C41 SADI 0.04 C41 C43 C42 C44 C43 C45 C44 C46 C45 C41 C46 C42 SADI 0.04 C41 C44 C42 C45 C43 C46 SADI 0.04 C46 C47 C42 C47 FLAT C31 > C37 FLAT C41 > C47 DELU 0.005 0.005 C31 > C36 DELU 0.005 0.005 C41 > C46 RIGU C31 > C47 ISOR C36 FMAP 2 PLAN 25 SIZE 0.110 0.160 0.180 ACTA LIST 4 L.S. 15 WGHT 0.130800 EXTI 0.008426 FVAR 0.14617 AL1 4 0.669143 0.277225 0.115857 11.00000 0.05055 0.04892 = 0.04782 0.00648 0.02681 0.00265 AL2 4 0.839948 -0.195509 0.264899 11.00000 0.05585 0.05095 = 0.05449 0.00916 0.03061 0.00711 C1 1 0.646260 -0.106515 0.039563 11.00000 0.04595 0.05929 = 0.04392 -0.01122 0.02346 -0.00668 C2 1 0.585586 -0.042352 -0.015885 11.00000 0.04932 0.06964 = 0.04002 -0.00552 0.01753 -0.00267 AFIX 43 H2 2 0.549961 -0.087674 -0.054166 11.00000 -1.20000 AFIX 0 C3 1 0.586538 0.097530 -0.005295 11.00000 0.04525 0.06045 = 0.04381 0.00107 0.02432 -0.00219 C4 1 0.674568 -0.258262 0.057049 11.00000 0.05882 0.05767 = 0.07117 -0.01435 0.02676 -0.00358 AFIX 137 H4A 2 0.728150 -0.273514 0.060474 11.00000 -1.50000 H4B 2 0.629600 -0.320100 0.025665 11.00000 -1.50000 H4C 2 0.684124 -0.278565 0.096230 11.00000 -1.50000 AFIX 0 C5 1 0.532441 0.214642 -0.049773 11.00000 0.07344 0.07760 = 0.05069 0.01327 0.03245 0.00698 AFIX 137 H5A 2 0.486887 0.174469 -0.089172 11.00000 -1.50000 H5B 2 0.569241 0.274966 -0.055090 11.00000 -1.50000 H5C 2 0.506430 0.269753 -0.033640 11.00000 -1.50000 AFIX 0 C6 1 0.864260 -0.080873 0.127271 11.00000 0.03763 0.06964 = 0.05417 -0.00809 0.02497 -0.00986 C7 1 0.925870 -0.189309 0.151398 11.00000 0.04580 0.07938 = 0.06876 -0.00753 0.03613 0.00321 AFIX 43 H7 2 0.961467 -0.212927 0.138518 11.00000 -1.20000 AFIX 0 C8 1 0.925517 -0.254699 0.196618 11.00000 0.03797 0.06420 = 0.05937 -0.00415 0.02160 0.00746 C9 1 0.838257 0.025154 0.077371 11.00000 0.06217 0.10359 = 0.07398 0.01104 0.04521 0.00223 AFIX 137 H9A 2 0.783093 -0.002413 0.040066 11.00000 -1.50000 H9B 2 0.882489 0.028841 0.069498 11.00000 -1.50000 H9C 2 0.832426 0.117392 0.090379 11.00000 -1.50000 AFIX 0 C10 1 0.980951 -0.376928 0.236926 11.00000 0.05762 0.08095 = 0.09259 -0.00515 0.03165 0.01926 AFIX 137 H10A 2 1.021741 -0.344149 0.278840 11.00000 -1.50000 H10B 2 1.012778 -0.415720 0.221675 11.00000 -1.50000 H10C 2 0.943873 -0.449277 0.236104 11.00000 -1.50000 AFIX 0 C11 1 0.752887 -0.011819 0.146726 11.00000 0.03362 0.05098 = 0.03892 0.00528 0.01668 0.01069 C12 1 0.749340 0.044962 0.193419 11.00000 0.04177 0.04097 = 0.04297 0.00187 0.02634 -0.00221 C13 1 0.647796 0.155268 0.209029 11.00000 0.03977 0.05021 = 0.04270 -0.00235 0.02308 0.00140 C14 1 0.615110 0.035043 0.218741 11.00000 0.06041 0.05115 = 0.06150 -0.00378 0.03810 -0.00224 AFIX 43 H14 2 0.617364 -0.051842 0.202736 11.00000 -1.20000 AFIX 0 C15 1 0.578666 0.041785 0.252254 11.00000 0.06882 0.07569 = 0.09238 0.00794 0.05756 -0.00394 AFIX 43 H15 2 0.558721 -0.041427 0.259427 11.00000 -1.20000 AFIX 0 C16 1 0.571535 0.169316 0.275031 11.00000 0.08391 0.09039 = 0.09142 0.00284 0.06871 0.01316 C17 1 0.602818 0.289955 0.264144 11.00000 0.08606 0.06714 = 0.08290 -0.00699 0.05919 0.01030 AFIX 43 H17 2 0.598794 0.377286 0.279018 11.00000 -1.20000 AFIX 0 C18 1 0.640478 0.283897 0.231218 11.00000 0.05962 0.05113 = 0.06699 -0.00103 0.04379 0.00479 AFIX 43 H18 2 0.660740 0.366939 0.224197 11.00000 -1.20000 AFIX 0 C19 1 0.532624 0.175370 0.311307 11.00000 0.17304 0.14218 = 0.15976 0.04784 0.14514 0.04710 AFIX 137 H19A 2 0.558913 0.252286 0.340678 11.00000 -1.50000 H19B 2 0.543687 0.087103 0.333103 11.00000 -1.50000 H19C 2 0.470338 0.190603 0.283381 11.00000 -1.50000 AFIX 0 C20 1 0.829158 0.089611 0.302728 11.00000 0.03990 0.05902 = 0.03801 -0.00008 0.02255 -0.00025 C21 1 0.856074 0.229812 0.305098 11.00000 0.04720 0.05754 = 0.06082 -0.00324 0.03078 -0.00256 AFIX 43 H21 2 0.858249 0.265493 0.273089 11.00000 -1.20000 AFIX 0 C22 1 0.879410 0.315161 0.355033 11.00000 0.05886 0.06167 = 0.08636 -0.01808 0.03668 -0.01206 AFIX 43 H22 2 0.898249 0.407821 0.356526 11.00000 -1.20000 AFIX 0 C23 1 0.875574 0.266891 0.402764 11.00000 0.09188 0.08622 = 0.06653 -0.01635 0.04729 -0.00540 C24 1 0.850700 0.129959 0.399979 11.00000 0.13670 0.10052 = 0.06278 -0.01881 0.06418 -0.02472 AFIX 43 H24 2 0.849381 0.093451 0.432238 11.00000 -1.20000 AFIX 0 C25 1 0.827172 0.043075 0.350112 11.00000 0.08775 0.06915 = 0.05181 0.00023 0.03816 -0.01309 AFIX 43 H25 2 0.809515 -0.050030 0.349404 11.00000 -1.20000 AFIX 0 C26 1 0.901292 0.367598 0.456645 11.00000 0.16488 0.15877 = 0.10269 -0.07116 0.07801 -0.02458 AFIX 137 H26A 2 0.856725 0.439173 0.442440 11.00000 -1.50000 H26B 2 0.956414 0.412426 0.471396 11.00000 -1.50000 H26C 2 0.906837 0.314233 0.489825 11.00000 -1.50000 AFIX 0 C27 1 0.776841 0.373534 0.138453 11.00000 0.06761 0.06042 = 0.07183 -0.00233 0.04007 -0.00982 AFIX 137 H27A 2 0.788878 0.451497 0.165915 11.00000 -1.50000 H27B 2 0.769580 0.409043 0.101579 11.00000 -1.50000 H27C 2 0.824978 0.307381 0.158966 11.00000 -1.50000 AFIX 0 C28 1 0.566374 0.395629 0.083650 11.00000 0.06854 0.05759 = 0.06358 0.01326 0.02946 0.01313 AFIX 137 H28A 2 0.521522 0.341692 0.082292 11.00000 -1.50000 H28B 2 0.544812 0.427029 0.042474 11.00000 -1.50000 H28C 2 0.581796 0.476916 0.110205 11.00000 -1.50000 AFIX 0 C29 1 0.743731 -0.326706 0.238835 11.00000 0.09155 0.06139 = 0.10935 0.00103 0.07148 -0.00745 AFIX 137 H29A 2 0.727558 -0.321337 0.267382 11.00000 -1.50000 H29B 2 0.761999 -0.422061 0.238369 11.00000 -1.50000 H29C 2 0.694118 -0.301512 0.197884 11.00000 -1.50000 AFIX 0 C30 1 0.951454 -0.229041 0.345825 11.00000 0.08950 0.09851 = 0.07609 0.01409 0.03331 0.03006 AFIX 137 H30A 2 0.995400 -0.165198 0.350862 11.00000 -1.50000 H30B 2 0.969887 -0.325686 0.347923 11.00000 -1.50000 H30C 2 0.943698 -0.212665 0.378331 11.00000 -1.50000 AFIX 0 N1 3 0.645590 0.126584 0.056135 11.00000 0.04628 0.05142 = 0.04250 0.00997 0.02562 0.00644 N2 3 0.681731 -0.004124 0.082230 11.00000 0.03659 0.04941 = 0.04104 0.00451 0.01849 0.00260 N3 3 0.863559 -0.196134 0.201469 11.00000 0.04599 0.04789 = 0.06203 0.00516 0.02916 0.01084 N4 3 0.826656 -0.087691 0.158378 11.00000 0.03721 0.05001 = 0.04842 0.00090 0.02391 0.00605 N5 3 0.686559 0.149573 0.176561 11.00000 0.04353 0.04738 = 0.04813 0.00299 0.03002 0.00421 N6 3 0.806974 -0.003263 0.253285 11.00000 0.04967 0.04713 = 0.03816 -0.00080 0.02295 0.00143 PART 1 C31 1 0.739966 -0.291867 -0.067591 10.25000 0.07015 C32 1 0.824814 -0.276599 -0.032776 10.25000 0.06564 AFIX 41 H32 2 0.850352 -0.201447 -0.039999 10.25000 -1.20000 AFIX 0 C33 1 0.873721 -0.364835 0.011638 10.25000 0.07772 AFIX 41 H33 2 0.934615 -0.356042 0.035508 10.25000 -1.20000 AFIX 0 C34 1 0.836979 -0.467463 0.023014 10.25000 0.03188 AFIX 41 H34 2 0.870884 -0.523055 0.058575 10.25000 -1.20000 AFIX 0 C35 1 0.754097 -0.490866 -0.015100 10.25000 0.06668 AFIX 43 H35 2 0.730003 -0.574053 -0.011736 10.25000 -1.20000 AFIX 0 C36 1 0.703882 -0.399111 -0.058222 10.25000 0.07013 AFIX 41 H36 2 0.643059 -0.409207 -0.082202 10.25000 -1.20000 AFIX 0 C37 1 0.681733 -0.180664 -0.119264 10.25000 0.08587 AFIX 137 H37A 2 0.695917 -0.086796 -0.101514 10.25000 -1.50000 H37B 2 0.620875 -0.200390 -0.137469 10.25000 -1.50000 H37C 2 0.692414 -0.186069 -0.150747 10.25000 -1.50000 AFIX 0 PART 2 C41 1 0.814141 -0.358179 -0.015181 10.25000 0.09344 C42 1 0.818400 -0.251687 -0.046071 10.25000 0.07743 AFIX 41 H42 2 0.872738 -0.216395 -0.034074 10.25000 -1.20000 AFIX 0 C43 1 0.746127 -0.196150 -0.093478 10.25000 0.10159 AFIX 41 H43 2 0.749131 -0.122898 -0.115954 10.25000 -1.20000 AFIX 0 C44 1 0.667081 -0.244155 -0.110141 10.25000 0.10578 AFIX 41 H44 2 0.615569 -0.198469 -0.141069 10.25000 -1.20000 AFIX 0 C45 1 0.664482 -0.356222 -0.081882 10.25000 0.07303 AFIX 41 H45 2 0.610187 -0.393605 -0.094770 10.25000 -1.20000 AFIX 0 C46 1 0.737982 -0.418775 -0.034805 10.25000 0.09127 AFIX 41 H46 2 0.735645 -0.501799 -0.016538 10.25000 -1.20000 AFIX 0 C47 1 0.898251 -0.422547 0.036394 10.25000 0.11276 AFIX 137 H47A 2 0.934748 -0.442024 0.022415 10.25000 -1.50000 H47B 2 0.886368 -0.509765 0.049296 10.25000 -1.50000 H47C 2 0.928006 -0.357458 0.070811 10.25000 -1.50000 AFIX 0 HKLF 4 REM AND_53 in P21/c REM R1 = 0.0827 for 2554 Fo > 4sig(Fo) and 0.2079 for all 6577 data REM 412 parameters refined using 78 restraints END WGHT 0.1307 0.0000 REM Highest difference peak 0.635, deepest hole -0.226, 1-sigma level 0.065 Q1 1 0.6397 -0.2994 -0.1072 11.00000 0.05 0.63 Q2 1 0.8941 -0.3060 -0.0098 11.00000 0.05 0.48 Q3 1 0.7208 -0.3479 -0.0615 11.00000 0.05 0.41 Q4 1 0.7028 -0.4726 -0.0422 11.00000 0.05 0.40 Q5 1 0.8122 -0.5258 0.0184 11.00000 0.05 0.39 Q6 1 0.7935 -0.4378 -0.0026 11.00000 0.05 0.38 Q7 1 0.7952 -0.2123 -0.0786 11.00000 0.05 0.31 Q8 1 0.6599 -0.1099 -0.1131 11.00000 0.05 0.25 Q9 1 0.7805 -0.2687 -0.0540 11.00000 0.05 0.25 Q10 1 0.8426 -0.2580 0.1230 11.00000 0.05 0.25 Q11 1 0.9177 -0.2564 0.3261 11.00000 0.05 0.25 Q12 1 0.8801 0.2845 0.5440 11.00000 0.05 0.24 Q13 1 0.5882 0.1939 -0.0518 11.00000 0.05 0.24 Q14 1 0.8526 -0.4031 0.0167 11.00000 0.05 0.23 Q15 1 0.5687 0.0946 -0.0786 11.00000 0.05 0.22 Q16 1 0.9170 -0.3438 0.1290 11.00000 0.05 0.22 Q17 1 0.5142 0.2025 -0.0959 11.00000 0.05 0.22 Q18 1 0.6464 0.1589 0.0005 11.00000 0.05 0.21 Q19 1 0.7533 -0.0391 0.2461 11.00000 0.05 0.21 Q20 1 0.7171 0.3925 0.1286 11.00000 0.05 0.21 Q21 1 0.7923 -0.4304 0.2906 11.00000 0.05 0.21 Q22 1 0.6228 -0.3712 0.1857 11.00000 0.05 0.20 Q23 1 0.9267 -0.3901 0.1632 11.00000 0.05 0.20 Q24 1 0.4711 0.1982 -0.0664 11.00000 0.05 0.20 Q25 1 0.6778 0.0410 0.0258 11.00000 0.05 0.20 ; _shelx_res_checksum 75285 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 0.66914(11) 0.27722(19) 0.11586(8) 0.0500(5) Uani 1 1 d . . . . . Al2 Al 0.83995(12) -0.1955(2) 0.26490(8) 0.0545(6) Uani 1 1 d . . . . . C1 C 0.6463(4) -0.1065(7) 0.0396(3) 0.0512(15) Uani 1 1 d . . . . . C2 C 0.5856(4) -0.0424(7) -0.0159(3) 0.0578(16) Uani 1 1 d . . . . . H2 H 0.5500 -0.0877 -0.0542 0.069 Uiso 1 1 calc R U . . . C3 C 0.5865(4) 0.0975(7) -0.0053(3) 0.0507(15) Uani 1 1 d . . . . . C4 C 0.6746(4) -0.2583(7) 0.0570(3) 0.0688(19) Uani 1 1 d . . . . . H4A H 0.7282 -0.2735 0.0605 0.103 Uiso 1 1 calc R U . . . H4B H 0.6296 -0.3201 0.0257 0.103 Uiso 1 1 calc R U . . . H4C H 0.6841 -0.2786 0.0962 0.103 Uiso 1 1 calc R U . . . C5 C 0.5324(4) 0.2146(7) -0.0498(3) 0.0692(19) Uani 1 1 d . . . . . H5A H 0.4869 0.1745 -0.0892 0.104 Uiso 1 1 calc R U . . . H5B H 0.5692 0.2750 -0.0551 0.104 Uiso 1 1 calc R U . . . H5C H 0.5064 0.2698 -0.0336 0.104 Uiso 1 1 calc R U . . . C6 C 0.8643(4) -0.0809(7) 0.1273(3) 0.0547(16) Uani 1 1 d . . . . . C7 C 0.9259(4) -0.1893(7) 0.1514(3) 0.0629(18) Uani 1 1 d . . . . . H7 H 0.9615 -0.2129 0.1385 0.075 Uiso 1 1 calc R U . . . C8 C 0.9255(4) -0.2547(7) 0.1966(3) 0.0576(17) Uani 1 1 d . . . . . C9 C 0.8383(4) 0.0252(8) 0.0774(3) 0.077(2) Uani 1 1 d . . . . . H9A H 0.7831 -0.0024 0.0401 0.115 Uiso 1 1 calc R U . . . H9B H 0.8825 0.0288 0.0695 0.115 Uiso 1 1 calc R U . . . H9C H 0.8324 0.1174 0.0904 0.115 Uiso 1 1 calc R U . . . C10 C 0.9810(4) -0.3769(8) 0.2369(3) 0.084(2) Uani 1 1 d . . . . . H10A H 1.0217 -0.3441 0.2788 0.126 Uiso 1 1 calc R U . . . H10B H 1.0128 -0.4157 0.2217 0.126 Uiso 1 1 calc R U . . . H10C H 0.9439 -0.4493 0.2361 0.126 Uiso 1 1 calc R U . . . C11 C 0.7529(3) -0.0118(6) 0.1467(2) 0.0437(14) Uani 1 1 d . . . . . C12 C 0.7493(3) 0.0450(6) 0.1934(2) 0.0408(13) Uani 1 1 d . . . . . C13 C 0.6478(3) 0.1553(6) 0.2090(2) 0.0447(14) Uani 1 1 d . . . . . C14 C 0.6151(4) 0.0350(7) 0.2187(3) 0.0560(16) Uani 1 1 d . . . . . H14 H 0.6174 -0.0518 0.2027 0.067 Uiso 1 1 calc R U . . . C15 C 0.5787(4) 0.0418(8) 0.2523(3) 0.073(2) Uani 1 1 d . . . . . H15 H 0.5587 -0.0414 0.2594 0.087 Uiso 1 1 calc R U . . . C16 C 0.5715(5) 0.1693(9) 0.2750(3) 0.078(2) Uani 1 1 d . . . . . C17 C 0.6028(4) 0.2900(8) 0.2641(3) 0.073(2) Uani 1 1 d . . . . . H17 H 0.5988 0.3773 0.2790 0.087 Uiso 1 1 calc R U . . . C18 C 0.6405(4) 0.2839(7) 0.2312(3) 0.0551(16) Uani 1 1 d . . . . . H18 H 0.6607 0.3669 0.2242 0.066 Uiso 1 1 calc R U . . . C19 C 0.5326(6) 0.1754(10) 0.3113(4) 0.130(4) Uani 1 1 d . . . . . H19A H 0.5589 0.2523 0.3407 0.195 Uiso 1 1 calc R U . . . H19B H 0.5437 0.0871 0.3331 0.195 Uiso 1 1 calc R U . . . H19C H 0.4703 0.1906 0.2834 0.195 Uiso 1 1 calc R U . . . C20 C 0.8292(3) 0.0896(7) 0.3027(2) 0.0456(14) Uani 1 1 d . . . . . C21 C 0.8561(4) 0.2298(7) 0.3051(3) 0.0554(16) Uani 1 1 d . . . . . H21 H 0.8582 0.2655 0.2731 0.067 Uiso 1 1 calc R U . . . C22 C 0.8794(4) 0.3152(8) 0.3550(3) 0.072(2) Uani 1 1 d . . . . . H22 H 0.8982 0.4078 0.3565 0.086 Uiso 1 1 calc R U . . . C23 C 0.8756(5) 0.2669(10) 0.4028(3) 0.081(2) Uani 1 1 d . . . . . C24 C 0.8507(5) 0.1300(10) 0.4000(3) 0.096(3) Uani 1 1 d . . . . . H24 H 0.8494 0.0935 0.4322 0.115 Uiso 1 1 calc R U . . . C25 C 0.8272(4) 0.0431(8) 0.3501(3) 0.0708(19) Uani 1 1 d . . . . . H25 H 0.8095 -0.0500 0.3494 0.085 Uiso 1 1 calc R U . . . C26 C 0.9013(7) 0.3676(11) 0.4566(4) 0.142(4) Uani 1 1 d . . . . . H26A H 0.8567 0.4392 0.4424 0.213 Uiso 1 1 calc R U . . . H26B H 0.9564 0.4124 0.4714 0.213 Uiso 1 1 calc R U . . . H26C H 0.9068 0.3142 0.4898 0.213 Uiso 1 1 calc R U . . . C27 C 0.7768(4) 0.3735(7) 0.1385(3) 0.0668(18) Uani 1 1 d . . . . . H27A H 0.7889 0.4515 0.1659 0.100 Uiso 1 1 calc R U . . . H27B H 0.7696 0.4090 0.1016 0.100 Uiso 1 1 calc R U . . . H27C H 0.8250 0.3074 0.1590 0.100 Uiso 1 1 calc R U . . . C28 C 0.5664(4) 0.3956(7) 0.0837(3) 0.0683(18) Uani 1 1 d . . . . . H28A H 0.5215 0.3417 0.0823 0.102 Uiso 1 1 calc R U . . . H28B H 0.5448 0.4270 0.0425 0.102 Uiso 1 1 calc R U . . . H28C H 0.5818 0.4769 0.1102 0.102 Uiso 1 1 calc R U . . . C29 C 0.7437(4) -0.3267(7) 0.2388(3) 0.080(2) Uani 1 1 d . . . . . H29A H 0.7276 -0.3213 0.2674 0.120 Uiso 1 1 calc R U . . . H29B H 0.7620 -0.4221 0.2384 0.120 Uiso 1 1 calc R U . . . H29C H 0.6941 -0.3015 0.1979 0.120 Uiso 1 1 calc R U . . . C30 C 0.9515(5) -0.2290(9) 0.3458(3) 0.096(3) Uani 1 1 d . . . . . H30A H 0.9954 -0.1652 0.3509 0.145 Uiso 1 1 calc R U . . . H30B H 0.9699 -0.3257 0.3479 0.145 Uiso 1 1 calc R U . . . H30C H 0.9437 -0.2127 0.3783 0.145 Uiso 1 1 calc R U . . . N1 N 0.6456(3) 0.1266(5) 0.0561(2) 0.0468(12) Uani 1 1 d . . . . . N2 N 0.6817(3) -0.0041(5) 0.0822(2) 0.0446(12) Uani 1 1 d . . . . . N3 N 0.8636(3) -0.1961(5) 0.2015(2) 0.0532(13) Uani 1 1 d . . . . . N4 N 0.8267(3) -0.0877(5) 0.1584(2) 0.0457(12) Uani 1 1 d . . . . . N5 N 0.6866(3) 0.1496(5) 0.17656(19) 0.0443(12) Uani 1 1 d . . . . . N6 N 0.8070(3) -0.0033(5) 0.2533(2) 0.0464(12) Uani 1 1 d . . . . . C31 C 0.7400(12) -0.292(2) -0.0676(9) 0.070(7) Uiso 0.25 1 d D . P A 1 C32 C 0.8248(12) -0.277(2) -0.0328(10) 0.066(10) Uiso 0.25 1 d D . P A 1 H32 H 0.8504 -0.2014 -0.0400 0.079 Uiso 0.25 1 calc . U P B 1 C33 C 0.8737(13) -0.365(2) 0.0116(11) 0.078(8) Uiso 0.25 1 d D . P A 1 H33 H 0.9346 -0.3560 0.0355 0.093 Uiso 0.25 1 calc . U P C 1 C34 C 0.8370(10) -0.4675(19) 0.0230(8) 0.032(5) Uiso 0.25 1 d D . P A 1 H34 H 0.8709 -0.5231 0.0586 0.038 Uiso 0.25 1 calc . U P D 1 C35 C 0.7541(12) -0.491(2) -0.0151(10) 0.067(7) Uiso 0.25 1 d D . P A 1 H35 H 0.7300 -0.5741 -0.0117 0.080 Uiso 0.25 1 calc R U P A 1 C36 C 0.7039(14) -0.399(3) -0.0582(12) 0.070(8) Uiso 0.25 1 d D . P A 1 H36 H 0.6431 -0.4092 -0.0822 0.084 Uiso 0.25 1 calc . U P E 1 C37 C 0.6817(17) -0.181(3) -0.1193(12) 0.086(9) Uiso 0.25 1 d D . P A 1 H37A H 0.6959 -0.0868 -0.1015 0.129 Uiso 0.25 1 calc R U P A 1 H37B H 0.6209 -0.2004 -0.1375 0.129 Uiso 0.25 1 calc R U P A 1 H37C H 0.6924 -0.1861 -0.1507 0.129 Uiso 0.25 1 calc R U P A 1 C41 C 0.8141(13) -0.358(3) -0.0152(11) 0.093(10) Uiso 0.25 1 d D . P F 2 C42 C 0.8184(14) -0.252(3) -0.0461(12) 0.077(12) Uiso 0.25 1 d D . P F 2 H42 H 0.8727 -0.2164 -0.0341 0.093 Uiso 0.25 1 calc . U P G 2 C43 C 0.7461(16) -0.196(3) -0.0935(12) 0.102(10) Uiso 0.25 1 d D . P F 2 H43 H 0.7491 -0.1229 -0.1160 0.122 Uiso 0.25 1 calc . U P H 2 C44 C 0.6671(15) -0.244(3) -0.1101(14) 0.106(12) Uiso 0.25 1 d D . P F 2 H44 H 0.6156 -0.1985 -0.1411 0.127 Uiso 0.25 1 calc . U P I 2 C45 C 0.6645(13) -0.356(3) -0.0819(12) 0.073(8) Uiso 0.25 1 d D . P F 2 H45 H 0.6102 -0.3936 -0.0948 0.088 Uiso 0.25 1 calc . U P J 2 C46 C 0.7380(14) -0.419(3) -0.0348(14) 0.091(10) Uiso 0.25 1 d D . P F 2 H46 H 0.7356 -0.5018 -0.0165 0.110 Uiso 0.25 1 calc . U P K 2 C47 C 0.8983(17) -0.423(4) 0.0364(14) 0.113(12) Uiso 0.25 1 d D . P F 2 H47A H 0.9347 -0.4420 0.0224 0.169 Uiso 0.25 1 calc R U P F 2 H47B H 0.8864 -0.5098 0.0493 0.169 Uiso 0.25 1 calc R U P F 2 H47C H 0.9280 -0.3575 0.0708 0.169 Uiso 0.25 1 calc R U P F 2 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 0.0505(10) 0.0489(11) 0.0478(11) 0.0065(9) 0.0268(9) 0.0026(9) Al2 0.0559(11) 0.0510(12) 0.0545(12) 0.0092(9) 0.0306(10) 0.0071(9) C1 0.046(3) 0.059(4) 0.044(4) -0.011(3) 0.023(3) -0.007(3) C2 0.049(4) 0.070(5) 0.040(4) -0.006(3) 0.018(3) -0.003(3) C3 0.045(3) 0.060(4) 0.044(4) 0.001(3) 0.024(3) -0.002(3) C4 0.059(4) 0.058(4) 0.071(5) -0.014(4) 0.027(4) -0.004(3) C5 0.073(4) 0.078(5) 0.051(4) 0.013(4) 0.032(3) 0.007(4) C6 0.038(3) 0.070(5) 0.054(4) -0.008(3) 0.025(3) -0.010(3) C7 0.046(4) 0.079(5) 0.069(5) -0.008(4) 0.036(4) 0.003(4) C8 0.038(3) 0.064(4) 0.059(4) -0.004(3) 0.022(3) 0.007(3) C9 0.062(4) 0.104(6) 0.074(5) 0.011(4) 0.045(4) 0.002(4) C10 0.058(4) 0.081(5) 0.093(5) -0.005(4) 0.032(4) 0.019(4) C11 0.034(3) 0.051(4) 0.039(3) 0.005(3) 0.017(3) 0.011(3) C12 0.042(3) 0.041(3) 0.043(3) 0.002(3) 0.026(3) -0.002(3) C13 0.040(3) 0.050(4) 0.043(3) -0.002(3) 0.023(3) 0.001(3) C14 0.060(4) 0.051(4) 0.062(4) -0.004(3) 0.038(4) -0.002(3) C15 0.069(4) 0.076(5) 0.092(5) 0.008(4) 0.058(4) -0.004(4) C16 0.084(5) 0.090(6) 0.091(6) 0.003(5) 0.069(5) 0.013(4) C17 0.086(5) 0.067(5) 0.083(5) -0.007(4) 0.059(4) 0.010(4) C18 0.060(4) 0.051(4) 0.067(4) -0.001(3) 0.044(4) 0.005(3) C19 0.173(9) 0.142(8) 0.160(9) 0.048(7) 0.145(8) 0.047(7) C20 0.040(3) 0.059(4) 0.038(3) 0.000(3) 0.023(3) 0.000(3) C21 0.047(3) 0.058(4) 0.061(4) -0.003(3) 0.031(3) -0.003(3) C22 0.059(4) 0.062(5) 0.086(6) -0.018(4) 0.037(4) -0.012(4) C23 0.092(5) 0.086(6) 0.067(5) -0.016(4) 0.047(4) -0.005(5) C24 0.137(7) 0.101(7) 0.063(5) -0.019(5) 0.064(5) -0.025(6) C25 0.088(5) 0.069(5) 0.052(4) 0.000(4) 0.038(4) -0.013(4) C26 0.165(9) 0.159(9) 0.103(7) -0.071(7) 0.078(7) -0.025(8) C27 0.068(4) 0.060(4) 0.072(4) -0.002(4) 0.040(4) -0.010(4) C28 0.069(4) 0.058(4) 0.064(4) 0.013(3) 0.029(4) 0.013(4) C29 0.092(5) 0.061(5) 0.109(6) 0.001(4) 0.071(5) -0.007(4) C30 0.090(5) 0.099(6) 0.076(5) 0.014(5) 0.033(4) 0.030(5) N1 0.046(3) 0.051(3) 0.043(3) 0.010(2) 0.026(2) 0.006(2) N2 0.037(2) 0.049(3) 0.041(3) 0.005(3) 0.018(2) 0.003(2) N3 0.046(3) 0.048(3) 0.062(3) 0.005(3) 0.029(3) 0.011(2) N4 0.037(2) 0.050(3) 0.048(3) 0.001(2) 0.024(2) 0.006(2) N5 0.044(3) 0.047(3) 0.048(3) 0.003(2) 0.030(2) 0.004(2) N6 0.050(3) 0.047(3) 0.038(3) -0.001(2) 0.023(2) 0.001(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' 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 N5 Al1 C28 112.4(2) . . ? N5 Al1 C27 113.3(2) . . ? C28 Al1 C27 116.7(3) . . ? N5 Al1 N1 94.1(2) . . ? C28 Al1 N1 110.8(2) . . ? C27 Al1 N1 106.9(2) . . ? N6 Al2 C29 113.8(3) . . ? N6 Al2 N3 94.5(2) . . ? C29 Al2 N3 108.2(3) . . ? N6 Al2 C30 111.9(3) . . ? C29 Al2 C30 117.6(3) . . ? N3 Al2 C30 107.9(3) . . ? N2 C1 C2 106.6(6) . . ? N2 C1 C4 120.9(5) . . ? C2 C1 C4 132.5(6) . . ? C3 C2 C1 107.8(6) . . ? C2 C3 N1 110.4(5) . . ? C2 C3 C5 129.5(6) . . ? N1 C3 C5 120.1(6) . . ? N4 C6 C7 105.6(6) . . ? N4 C6 C9 123.3(6) . . ? C7 C6 C9 131.1(6) . . ? C8 C7 C6 108.4(5) . . ? C7 C8 N3 109.9(6) . . ? C7 C8 C10 128.6(6) . . ? N3 C8 C10 121.4(6) . . ? C12 C11 N4 122.9(5) . . ? C12 C11 N2 123.5(5) . . ? N4 C11 N2 113.6(4) . . ? N6 C12 C11 119.3(5) . . ? N6 C12 N5 123.7(5) . . ? C11 C12 N5 117.0(5) . . ? C14 C13 C18 118.4(5) . . ? C14 C13 N5 121.4(5) . . ? C18 C13 N5 120.2(5) . . ? C13 C14 C15 120.8(6) . . ? C16 C15 C14 121.4(6) . . ? C17 C16 C15 117.6(6) . . ? C17 C16 C19 121.4(7) . . ? C15 C16 C19 121.0(8) . . ? C16 C17 C18 121.4(6) . . ? C13 C18 C17 120.4(6) . . ? C25 C20 C21 117.8(6) . . ? C25 C20 N6 120.3(6) . . ? C21 C20 N6 121.8(5) . . ? C22 C21 C20 119.8(6) . . ? C23 C22 C21 121.8(7) . . ? C24 C23 C22 117.4(7) . . ? C24 C23 C26 123.3(8) . . ? C22 C23 C26 119.3(8) . . ? C23 C24 C25 121.4(7) . . ? C20 C25 C24 121.8(7) . . ? C3 N1 N2 104.0(5) . . ? C3 N1 Al1 138.6(4) . . ? N2 N1 Al1 115.0(3) . . ? C1 N2 N1 111.2(4) . . ? C1 N2 C11 129.4(5) . . ? N1 N2 C11 119.2(4) . . ? C8 N3 N4 105.6(5) . . ? C8 N3 Al2 135.1(4) . . ? N4 N3 Al2 116.7(3) . . ? C6 N4 N3 110.4(5) . . ? C6 N4 C11 128.5(5) . . ? N3 N4 C11 120.7(4) . . ? C12 N5 C13 117.8(4) . . ? C12 N5 Al1 115.1(3) . . ? C13 N5 Al1 126.9(4) . . ? C12 N6 C20 118.2(5) . . ? C12 N6 Al2 118.0(4) . . ? C20 N6 Al2 123.3(4) . . ? C32 C31 C36 120.0(14) . . ? C32 C31 C37 119.6(15) . . ? C36 C31 C37 120.4(15) . . ? C33 C32 C31 120.3(14) . . ? C32 C33 C34 119.4(14) . . ? C35 C34 C33 119.8(13) . . ? C34 C35 C36 120.3(13) . . ? C35 C36 C31 119.1(13) . . ? C42 C41 C46 121.1(13) . . ? C42 C41 C47 117.7(16) . . ? C46 C41 C47 120.5(16) . . ? C43 C42 C41 119.8(13) . . ? C42 C43 C44 120.5(14) . . ? C45 C44 C43 118.5(14) . . ? C44 C45 C46 121.7(13) . . ? C41 C46 C45 117.7(13) . . ? 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 N5 1.871(5) . ? Al1 C28 1.935(6) . ? Al1 C27 1.954(6) . ? Al1 N1 1.967(5) . ? Al2 N6 1.873(5) . ? Al2 C29 1.944(6) . ? Al2 N3 1.959(5) . ? Al2 C30 1.960(7) . ? C1 N2 1.329(7) . ? C1 C2 1.366(8) . ? C1 C4 1.496(8) . ? C2 C3 1.340(8) . ? C3 N1 1.359(6) . ? C3 C5 1.494(8) . ? C6 N4 1.353(7) . ? C6 C7 1.383(8) . ? C6 C9 1.489(8) . ? C7 C8 1.344(8) . ? C8 N3 1.350(7) . ? C8 C10 1.497(9) . ? C11 C12 1.377(7) . ? C11 N4 1.415(6) . ? C11 N2 1.430(6) . ? C12 N6 1.374(6) . ? C12 N5 1.389(6) . ? C13 C14 1.375(8) . ? C13 C18 1.382(8) . ? C13 N5 1.404(6) . ? C14 C15 1.393(8) . ? C15 C16 1.379(9) . ? C16 C17 1.377(9) . ? C16 C19 1.498(9) . ? C17 C18 1.398(8) . ? C20 C25 1.343(8) . ? C20 C21 1.397(8) . ? C20 N6 1.416(7) . ? C21 C22 1.379(8) . ? C22 C23 1.377(9) . ? C23 C24 1.354(10) . ? C23 C26 1.534(10) . ? C24 C25 1.385(9) . ? N1 N2 1.377(6) . ? N3 N4 1.377(6) . ? C31 C32 1.298(16) . ? C31 C36 1.311(16) . ? C31 C37 1.553(18) . ? C32 C33 1.286(16) . ? C33 C34 1.313(16) . ? C34 C35 1.284(15) . ? C35 C36 1.296(17) . ? C41 C42 1.320(17) . ? C41 C46 1.325(17) . ? C41 C47 1.485(18) . ? C42 C43 1.304(17) . ? C43 C44 1.348(17) . ? C44 C45 1.306(17) . ? C45 C46 1.340(17) . ?