#------------------------------------------------------------------------------ #$Date: 2017-04-22 05:10:45 +0300 (Sat, 22 Apr 2017) $ #$Revision: 195683 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042752.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_7042752 loop_ _publ_author_name 'Huerta-Lavorie, Ra\'ul' 'B\'aez-Rodr\'iguez, Dana V.' 'Garc\'ia-R\'ios, Jessica' 'Mart\'inez-Vollbert, Emiliano' 'Mart\'inez-Otero, Diego' 'Jancik, Vojtech' _publ_section_title ; Molecular rare earth metal alumosilicates ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00874K _journal_year 2017 _chemical_formula_moiety 'C52 H76 Al N2 Ce O5 Si, 0.5(C7 H8)' _chemical_formula_sum 'C55.5 H80 Al Ce N2 O5 Si' _chemical_formula_weight 1050.40 _chemical_properties_physical ', Moisture-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary intrinsic-phasing _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-03-10 deposited with the CCDC. 2017-04-05 downloaded from the CCDC. ; _cell_angle_alpha 66.9864(7) _cell_angle_beta 77.5958(7) _cell_angle_gamma 63.1834(6) _cell_formula_units_Z 2 _cell_length_a 14.3084(5) _cell_length_b 14.3951(5) _cell_length_c 16.1187(6) _cell_measurement_reflns_used 9425 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 3.19 _cell_volume 2724.13(17) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014 (Sheldrick 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_unetI/netI 0.0140 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 83315 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.878 _diffrn_reflns_theta_min 2.507 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_T_max 0.6663 _exptl_absorpt_correction_T_min 0.6193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.281 _exptl_crystal_description prism _exptl_crystal_F_000 1104 _exptl_crystal_size_max 0.364 _exptl_crystal_size_mid 0.224 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.971 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 756 _refine_ls_number_reflns 12948 _refine_ls_number_restraints 578 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0196 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.5246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0491 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12441 _reflns_number_total 12948 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00874k2.cif _cod_data_source_block Comp2 _cod_original_cell_volume 2724.14(17) _cod_original_formula_sum 'C55.50 H80 Al Ce N2 O5 Si' _cod_database_code 7042752 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.731 _shelx_estimated_absorpt_t_max 0.830 _shelx_res_file ; mo_036JAV10_0m.res created by SHELXL-2014/7 TITL mo_036JAV10_0m in P-1 CELL 0.71073 14.3084 14.3951 16.1187 66.9864 77.5958 63.1834 ZERR 2.00 0.0005 0.0005 0.0006 0.0007 0.0007 0.0006 LATT 1 SFAC C H N O AL SI CE UNIT 111 160 4 10 2 2 2 LIST 4 TEMP -173 L.S. 15 BOND FMAP 2 PLAN 20 size 0.210 0.224 0.364 acta dfix 0.84 0.01 o2 h2 o5 h5 omit 1 0 0 omit 0 0 1 omit -5 -3 2 omit -5 3 8 omit -5 1 6 omit -2 1 3 omit 11 5 8 omit -6 -2 4 omit -4 -3 1 omit 5 -1 1 omit -4 -5 6 htab o2 o5 bind o5 h5 bind o2 h2 WGHT 0.021100 1.524600 FVAR 0.18388 0.72199 0.61344 CE1 7 0.566944 0.697571 0.125241 11.00000 0.01539 0.01321 = 0.01613 -0.00660 -0.00216 -0.00433 SI1 6 0.766494 0.391938 0.256102 11.00000 0.01360 0.01356 = 0.01310 -0.00450 -0.00221 -0.00646 AL1 5 0.708308 0.227757 0.225577 11.00000 0.01118 0.01180 = 0.01185 -0.00470 -0.00029 -0.00512 O1 4 0.763653 0.274096 0.277789 11.00000 0.01470 0.01363 = 0.01483 -0.00458 -0.00254 -0.00639 O2 4 0.663793 0.488427 0.194385 11.00000 0.01589 0.01364 = 0.01814 -0.00559 -0.00427 -0.00577 H2 2 0.642785 0.460095 0.170315 11.00000 -1.50000 O3 4 0.761502 0.421079 0.344498 11.00000 0.02730 0.02002 = 0.01475 -0.00672 -0.00194 -0.01369 O4 4 0.866795 0.407639 0.192993 11.00000 0.01362 0.02015 = 0.01936 -0.00525 -0.00192 -0.00881 O5 4 0.632172 0.347952 0.145468 11.00000 0.01590 0.01531 = 0.01573 -0.00517 -0.00440 -0.00582 H5 2 0.596679 0.348640 0.111475 11.00000 -1.50000 N1 3 0.625977 0.150880 0.298468 11.00000 0.01312 0.01443 = 0.01306 -0.00511 0.00014 -0.00651 N2 3 0.805869 0.117340 0.178422 11.00000 0.01185 0.01500 = 0.01525 -0.00696 0.00063 -0.00524 C1 1 0.527744 0.041586 0.310829 11.00000 0.02447 0.02467 = 0.02493 -0.01208 0.00563 -0.01722 AFIX 137 H1A 2 0.516747 0.032255 0.375235 11.00000 -1.50000 H1B 2 0.546270 -0.029052 0.303167 11.00000 -1.50000 H1C 2 0.463244 0.097075 0.279825 11.00000 -1.50000 AFIX 0 C2 1 0.615371 0.079238 0.271237 11.00000 0.01680 0.01445 = 0.01591 -0.00367 -0.00224 -0.00775 C3 1 0.683391 0.034891 0.206883 11.00000 0.01807 0.01505 = 0.01898 -0.00767 -0.00174 -0.00762 AFIX 43 H3 2 0.663927 -0.007768 0.187071 11.00000 -1.20000 AFIX 0 C4 1 0.776739 0.046021 0.168287 11.00000 0.01599 0.01427 = 0.01576 -0.00593 -0.00230 -0.00417 C5 1 0.846497 -0.028041 0.114792 11.00000 0.02182 0.02578 = 0.03207 -0.02018 0.00510 -0.00881 AFIX 137 H5A 2 0.808944 -0.065690 0.105844 11.00000 -1.50000 H5B 2 0.909831 -0.083108 0.147689 11.00000 -1.50000 H5C 2 0.866136 0.016453 0.056012 11.00000 -1.50000 AFIX 0 C6 1 0.560840 0.180531 0.374405 11.00000 0.01697 0.01704 = 0.01460 -0.00654 0.00200 -0.01114 C7 1 0.459130 0.264528 0.361682 11.00000 0.01668 0.02005 = 0.01653 -0.00793 0.00160 -0.01087 C8 1 0.401974 0.294197 0.436277 11.00000 0.01901 0.02466 = 0.02228 -0.01328 0.00351 -0.01034 AFIX 43 H8 2 0.333515 0.351918 0.428751 11.00000 -1.20000 AFIX 0 C9 1 0.443403 0.240985 0.520653 11.00000 0.02648 0.02976 = 0.01904 -0.01497 0.00689 -0.01652 AFIX 43 H9 2 0.403182 0.261612 0.570651 11.00000 -1.20000 AFIX 0 C10 1 0.543531 0.157620 0.532279 11.00000 0.02837 0.02478 = 0.01419 -0.00624 0.00084 -0.01729 AFIX 43 H10 2 0.571325 0.121890 0.590528 11.00000 -1.20000 AFIX 0 C11 1 0.604633 0.124812 0.460432 11.00000 0.01955 0.01797 = 0.01523 -0.00401 -0.00003 -0.01218 C12 1 0.714414 0.031983 0.475079 11.00000 0.02161 0.02227 = 0.01662 -0.00237 -0.00283 -0.00970 AFIX 13 H12 2 0.762019 0.056662 0.424979 11.00000 -1.20000 AFIX 0 C13 1 0.758589 0.004832 0.564289 11.00000 0.03156 0.03449 = 0.02107 -0.00198 -0.00891 -0.01336 AFIX 137 H13A 2 0.719792 -0.030131 0.614708 11.00000 -1.50000 H13B 2 0.751375 0.073114 0.570000 11.00000 -1.50000 H13C 2 0.832851 -0.045850 0.565212 11.00000 -1.50000 AFIX 0 C14 1 0.718868 -0.075470 0.471856 11.00000 0.03763 0.01956 = 0.02625 -0.00400 -0.00692 -0.00617 AFIX 137 H14A 2 0.666220 -0.096490 0.515126 11.00000 -1.50000 H14B 2 0.788747 -0.134621 0.487452 11.00000 -1.50000 H14C 2 0.704470 -0.063676 0.410939 11.00000 -1.50000 AFIX 0 C15 1 0.406614 0.324527 0.271478 11.00000 0.01317 0.02377 = 0.01704 -0.00864 0.00028 -0.00618 AFIX 13 H15 2 0.454518 0.289593 0.226857 11.00000 -1.20000 AFIX 0 C16 1 0.387447 0.447162 0.236019 11.00000 0.02211 0.02225 = 0.02672 -0.00734 -0.00034 -0.00431 AFIX 137 H16A 2 0.454145 0.453334 0.230492 11.00000 -1.50000 H16B 2 0.339113 0.483286 0.278178 11.00000 -1.50000 H16C 2 0.356854 0.483100 0.176765 11.00000 -1.50000 AFIX 0 C17 1 0.302280 0.314794 0.279137 11.00000 0.01692 0.04512 = 0.02486 -0.01717 0.00129 -0.01364 AFIX 137 H17A 2 0.253275 0.351211 0.320870 11.00000 -1.50000 H17B 2 0.314521 0.236551 0.301862 11.00000 -1.50000 H17C 2 0.272480 0.350409 0.219566 11.00000 -1.50000 AFIX 0 C18 1 0.913096 0.105562 0.151173 11.00000 0.01202 0.01658 = 0.01937 -0.00951 0.00150 -0.00496 C19 1 0.992832 0.022011 0.210082 11.00000 0.01643 0.01763 = 0.02206 -0.00705 -0.00115 -0.00551 C20 1 1.095897 0.010168 0.183316 11.00000 0.01361 0.02095 = 0.03024 -0.00815 -0.00312 -0.00255 AFIX 43 H20 2 1.151014 -0.046152 0.221697 11.00000 -1.20000 AFIX 0 C21 1 1.119043 0.079194 0.101739 11.00000 0.01284 0.02594 = 0.03234 -0.01296 0.00368 -0.00694 AFIX 43 H21 2 1.189653 0.070024 0.084668 11.00000 -1.20000 AFIX 0 C22 1 1.039940 0.161358 0.045030 11.00000 0.01802 0.02229 = 0.02225 -0.00983 0.00541 -0.00935 AFIX 43 H22 2 1.056849 0.208628 -0.010527 11.00000 -1.20000 AFIX 0 C23 1 0.935289 0.176243 0.067938 11.00000 0.01525 0.01793 = 0.01830 -0.00935 0.00098 -0.00527 C24 1 0.851889 0.265501 0.001139 11.00000 0.01828 0.02288 = 0.01576 -0.00586 -0.00004 -0.00700 AFIX 13 H24 2 0.782283 0.264897 0.028131 11.00000 -1.20000 AFIX 0 C25 1 0.847061 0.380304 -0.017714 11.00000 0.03495 0.02072 = 0.02433 -0.00421 -0.00669 -0.00702 AFIX 137 H25A 2 0.833297 0.395117 0.039107 11.00000 -1.50000 H25B 2 0.790695 0.436177 -0.058606 11.00000 -1.50000 H25C 2 0.914099 0.383141 -0.045715 11.00000 -1.50000 AFIX 0 C26 1 0.872114 0.242766 -0.087859 11.00000 0.03187 0.03514 = 0.02213 -0.01295 -0.00449 -0.00933 AFIX 137 H26A 2 0.873782 0.169848 -0.075858 11.00000 -1.50000 H26B 2 0.939536 0.244373 -0.115938 11.00000 -1.50000 H26C 2 0.815947 0.299549 -0.128650 11.00000 -1.50000 AFIX 0 C27 1 0.971162 -0.053510 0.302135 11.00000 0.01906 0.02083 = 0.02255 -0.00216 -0.00461 -0.00715 AFIX 13 H27 2 0.896797 -0.043592 0.305428 11.00000 -1.20000 AFIX 0 C28 1 0.983866 -0.020487 0.377165 11.00000 0.02304 0.02671 = 0.02481 -0.00709 -0.00285 -0.00707 AFIX 137 H28A 2 0.968955 -0.068952 0.435938 11.00000 -1.50000 H28B 2 0.934905 0.056368 0.369375 11.00000 -1.50000 H28C 2 1.055870 -0.027738 0.374212 11.00000 -1.50000 AFIX 0 C29 1 1.042421 -0.175974 0.316241 11.00000 0.04664 0.02047 = 0.02948 -0.00403 -0.00577 -0.01017 AFIX 137 H29A 2 1.023821 -0.221962 0.374696 11.00000 -1.50000 H29B 2 1.115733 -0.188051 0.315061 11.00000 -1.50000 H29C 2 1.033134 -0.195974 0.267957 11.00000 -1.50000 AFIX 0 C30 1 0.724089 0.384114 0.437044 11.00000 0.03737 0.02228 = 0.01227 -0.00613 -0.00295 -0.01437 C31 1 0.729485 0.458024 0.480600 11.00000 0.06697 0.04149 = 0.02380 -0.01816 -0.00066 -0.03095 AFIX 137 H31A 2 0.706828 0.435668 0.544476 11.00000 -1.50000 H31B 2 0.683376 0.535073 0.450018 11.00000 -1.50000 H31C 2 0.801726 0.450965 0.475375 11.00000 -1.50000 AFIX 0 C32 1 0.612823 0.396251 0.440433 11.00000 0.04348 0.05119 = 0.03045 -0.02297 0.01443 -0.03062 AFIX 137 H32A 2 0.588232 0.371204 0.503461 11.00000 -1.50000 H32B 2 0.610732 0.351370 0.408777 11.00000 -1.50000 H32C 2 0.567405 0.474043 0.411257 11.00000 -1.50000 AFIX 0 C33 1 0.796913 0.264740 0.481914 11.00000 0.07605 0.02646 = 0.02495 -0.00094 -0.02125 -0.01032 AFIX 137 H33A 2 0.774634 0.239779 0.545658 11.00000 -1.50000 H33B 2 0.868689 0.258811 0.477246 11.00000 -1.50000 H33C 2 0.794494 0.218461 0.451845 11.00000 -1.50000 AFIX 0 C34 1 0.975955 0.363761 0.213183 11.00000 0.01398 0.02434 = 0.02855 -0.00907 -0.00287 -0.00832 C35 1 1.013558 0.241863 0.269428 11.00000 0.01952 0.02711 = 0.03655 -0.00442 -0.00677 -0.00561 AFIX 137 H35A 2 0.975248 0.233160 0.328229 11.00000 -1.50000 H35B 2 1.088753 0.211158 0.278204 11.00000 -1.50000 H35C 2 1.000947 0.202575 0.238160 11.00000 -1.50000 AFIX 0 C36 1 1.036058 0.379543 0.122185 11.00000 0.01958 0.03578 = 0.03634 -0.01325 0.00454 -0.01495 AFIX 137 H36A 2 1.110419 0.353853 0.131346 11.00000 -1.50000 H36B 2 1.008049 0.458087 0.085297 11.00000 -1.50000 H36C 2 1.028407 0.336851 0.091317 11.00000 -1.50000 AFIX 0 C37 1 0.987428 0.429175 0.262074 11.00000 0.02041 0.04490 = 0.04839 -0.02561 -0.00352 -0.01543 AFIX 137 H37A 2 1.061065 0.399710 0.275564 11.00000 -1.50000 H37B 2 0.944325 0.422919 0.318485 11.00000 -1.50000 H37C 2 0.964291 0.507077 0.223698 11.00000 -1.50000 AFIX 0 C38 1 0.522759 0.788334 -0.057744 11.00000 0.05362 0.02412 = 0.01850 -0.00009 -0.01069 -0.01589 AFIX 43 H38 2 0.522294 0.860069 -0.086703 11.00000 -1.20000 AFIX 0 C39 1 0.436533 0.764453 -0.014274 11.00000 0.03854 0.04218 = 0.02612 -0.00322 -0.01838 -0.01264 AFIX 43 H39 2 0.367181 0.817028 -0.008751 11.00000 -1.20000 AFIX 0 C40 1 0.470781 0.648282 0.019993 11.00000 0.05826 0.04860 = 0.02086 -0.00357 -0.01358 -0.03635 AFIX 43 H40 2 0.428818 0.608765 0.053178 11.00000 -1.20000 AFIX 0 C41 1 0.577585 0.601975 -0.003751 11.00000 0.06672 0.02598 = 0.01702 -0.00784 -0.00968 -0.01835 AFIX 43 H41 2 0.620591 0.525204 0.010029 11.00000 -1.20000 AFIX 0 C42 1 0.610532 0.687483 -0.051149 11.00000 0.04694 0.03513 = 0.01628 -0.00948 0.00084 -0.01679 AFIX 43 H42 2 0.679606 0.679137 -0.074672 11.00000 -1.20000 AFIX 0 simu 0.01 c43 > c47a delu 0.005 c43 > c47a same c44 > c47 c43 part 1 C43 1 0.423068 0.829874 0.225819 31.00000 0.03604 0.03944 = 0.05138 -0.03618 0.00387 -0.00500 AFIX 43 H43 2 0.435847 0.892054 0.218283 31.00000 -1.20000 AFIX 0 C44 1 0.463607 0.724718 0.293413 31.00000 0.03395 0.04506 = 0.03144 -0.03032 0.01121 -0.01478 AFIX 43 H44 2 0.505067 0.704668 0.341436 31.00000 -1.20000 AFIX 0 C45 1 0.430757 0.654867 0.276045 31.00000 0.02909 0.05000 = 0.02558 -0.02530 0.01122 -0.01913 AFIX 43 H45 2 0.450672 0.578042 0.307922 31.00000 -1.20000 AFIX 0 C46 1 0.363899 0.718634 0.203808 31.00000 0.01839 0.04499 = 0.04711 -0.02908 0.00777 -0.00878 AFIX 43 H46 2 0.327138 0.694129 0.180286 31.00000 -1.20000 AFIX 0 C47 1 0.361316 0.826099 0.172465 31.00000 0.02136 0.03771 = 0.05557 -0.03193 -0.00104 0.00401 AFIX 43 H47 2 0.323450 0.886123 0.122886 31.00000 -1.20000 AFIX 0 part 2 same 0.01 0.01 c43 > c47 C43A 1 0.446207 0.821926 0.239495 -31.00000 0.02920 0.04432 = 0.04051 -0.03305 0.00371 -0.01020 AFIX 43 H43A 2 0.466046 0.875178 0.242551 -31.00000 -1.20000 AFIX 0 C44A 1 0.483861 0.708563 0.293259 -31.00000 0.03555 0.04216 = 0.02563 -0.02614 0.00967 -0.01322 AFIX 43 H44A 2 0.539858 0.669342 0.333098 -31.00000 -1.20000 AFIX 0 C45A 1 0.421336 0.664953 0.275877 -31.00000 0.02860 0.04797 = 0.03478 -0.02399 0.01341 -0.01561 AFIX 43 H45A 2 0.420838 0.594130 0.308690 -31.00000 -1.20000 AFIX 0 C46A 1 0.360534 0.744593 0.201910 -31.00000 0.01903 0.04787 = 0.04888 -0.03089 0.00318 -0.00778 AFIX 43 H46A 2 0.317544 0.734878 0.171337 -31.00000 -1.20000 AFIX 0 C47A 1 0.375313 0.841499 0.181634 -31.00000 0.02499 0.03587 = 0.05799 -0.03209 -0.00139 0.00054 AFIX 43 H47A 2 0.341956 0.909661 0.135530 -31.00000 -1.20000 AFIX 0 part 0 C48 1 0.749143 0.681326 0.180526 11.00000 0.03173 0.02803 = 0.04911 -0.00590 -0.01447 -0.01780 AFIX 43 H48 2 0.779152 0.619173 0.232175 11.00000 -1.20000 AFIX 0 C49 1 0.674479 0.785774 0.180829 11.00000 0.04761 0.02832 = 0.04767 -0.01274 -0.01476 -0.02066 AFIX 43 H49 2 0.645427 0.807247 0.232639 11.00000 -1.20000 AFIX 0 C50 1 0.649827 0.853850 0.090345 11.00000 0.04985 0.02161 = 0.05525 -0.00219 -0.01942 -0.02156 AFIX 43 H50 2 0.600396 0.928644 0.070570 11.00000 -1.20000 AFIX 0 C51 1 0.711513 0.790909 0.035385 11.00000 0.04921 0.04554 = 0.04047 -0.00367 0.00076 -0.03799 AFIX 43 H51 2 0.712165 0.816318 -0.028633 11.00000 -1.20000 AFIX 0 C52 1 0.772074 0.684385 0.090258 11.00000 0.02508 0.03759 = 0.05627 -0.01298 0.00373 -0.02111 AFIX 43 H52 2 0.820100 0.624732 0.070250 11.00000 -1.20000 AFIX 0 part -1 same c54 > c58 c53 same c53 c58 < c54 c59 simu 0.02 c53 > c59a delu 0.01 c53 > c59a isor 0.015 c53 > c59a C53 1 0.061154 0.392299 0.584853 20.50000 0.04971 0.06249 = 0.06583 -0.03258 0.00733 -0.03916 C54 1 0.102192 0.407288 0.496437 20.50000 0.03196 0.04786 = 0.06430 -0.02563 0.00829 -0.02442 AFIX 43 H54 2 0.169286 0.354596 0.485541 20.50000 -1.20000 AFIX 0 C55 1 0.048976 0.496206 0.423485 20.50000 0.04687 0.05862 = 0.05023 -0.03794 0.01581 -0.03064 AFIX 43 H55 2 0.078814 0.502014 0.363991 20.50000 -1.20000 AFIX 0 C56 1 -0.048044 0.576896 0.437337 20.50000 0.04228 0.05130 = 0.05958 -0.03007 -0.00493 -0.02628 AFIX 43 H56 2 -0.085929 0.637255 0.387928 20.50000 -1.20000 AFIX 0 C57 1 -0.087593 0.566508 0.525216 20.50000 0.03770 0.05461 = 0.05968 -0.04337 0.01186 -0.02007 AFIX 43 H57 2 -0.151324 0.622890 0.536780 20.50000 -1.20000 AFIX 0 C58 1 -0.034390 0.473416 0.597417 20.50000 0.04915 0.06117 = 0.05066 -0.03311 0.00698 -0.03443 AFIX 43 H58 2 -0.065196 0.466110 0.656766 20.50000 -1.20000 AFIX 0 C59 1 0.118916 0.313093 0.648159 20.50000 0.06847 0.08305 = 0.08321 -0.03134 -0.02137 -0.04013 AFIX 137 H59A 2 0.146232 0.244068 0.635205 20.50000 -1.50000 H59B 2 0.077408 0.305919 0.705412 20.50000 -1.50000 H59C 2 0.177493 0.328432 0.652503 20.50000 -1.50000 AFIX 0 part -2 same 0.01 0.01 c53 > c59 C53A 1 0.032100 0.472898 0.518498 -20.50000 0.04986 0.05444 = 0.05996 -0.03598 0.00495 -0.03141 C54A 1 0.070559 0.494711 0.429274 -20.50000 0.04933 0.05521 = 0.05799 -0.03972 0.00681 -0.01711 AFIX 43 H54A 2 0.139915 0.447830 0.416110 -20.50000 -1.20000 AFIX 0 C55A 1 0.011582 0.582364 0.358578 -20.50000 0.06758 0.05885 = 0.06303 -0.03631 -0.00162 -0.02854 AFIX 43 H55A 2 0.041933 0.595789 0.298887 -20.50000 -1.20000 AFIX 0 C56A 1 -0.091902 0.650847 0.374571 -20.50000 0.05711 0.05577 = 0.05955 -0.01577 -0.03113 -0.02390 AFIX 43 H56A 2 -0.135787 0.705291 0.326325 -20.50000 -1.20000 AFIX 0 C57A 1 -0.127902 0.636081 0.463727 -20.50000 0.04526 0.06296 = 0.07348 -0.03007 0.00406 -0.02707 AFIX 43 H57A 2 -0.192045 0.689889 0.478007 -20.50000 -1.20000 AFIX 0 C58A 1 -0.069972 0.541775 0.533315 -20.50000 0.05364 0.06162 = 0.05889 -0.02653 0.01002 -0.02742 AFIX 43 H58A 2 -0.102100 0.525108 0.592147 -20.50000 -1.20000 AFIX 0 C59A 1 0.090586 0.388689 0.579343 -20.50000 0.06527 0.06448 = 0.07164 -0.02697 0.00170 -0.04830 AFIX 137 H59D 2 0.118573 0.323487 0.560749 -20.50000 -1.50000 H59E 2 0.049265 0.375852 0.636347 -20.50000 -1.50000 H59F 2 0.148686 0.402275 0.587503 -20.50000 -1.50000 AFIX 0 HKLF 4 REM mo_036JAV10_0m in P-1 REM R1 = 0.0196 for 12441 Fo > 4sig(Fo) and 0.0207 for all 12948 data REM 756 parameters refined using 578 restraints END WGHT 0.0211 1.5246 REM Highest difference peak 0.971, deepest hole -0.469, 1-sigma level 0.050 Q1 1 0.5523 0.7407 0.0788 11.00000 0.05 0.97 Q2 1 0.8976 0.2158 0.0355 11.00000 0.05 0.41 Q3 1 0.9814 -0.0129 0.2544 11.00000 0.05 0.39 Q4 1 0.4316 0.2904 0.3173 11.00000 0.05 0.39 Q5 1 1.1030 0.0644 0.1528 11.00000 0.05 0.36 Q6 1 0.4846 0.1873 0.5268 11.00000 0.05 0.35 Q7 1 1.0415 0.0223 0.1993 11.00000 0.05 0.35 Q8 1 0.5833 0.1536 0.4160 11.00000 0.05 0.35 Q9 1 0.7218 0.4212 0.4569 11.00000 0.05 0.34 Q10 1 0.8127 0.0088 0.1410 11.00000 0.05 0.34 Q11 1 0.3567 0.3162 0.2754 11.00000 0.05 0.34 Q12 1 0.9841 0.1756 0.0617 11.00000 0.05 0.34 Q13 1 0.9209 0.1555 0.1122 11.00000 0.05 0.34 Q14 1 0.5780 0.0593 0.2919 11.00000 0.05 0.34 Q15 1 0.8235 0.3958 0.2201 11.00000 0.05 0.34 Q16 1 0.6579 0.0789 0.4682 11.00000 0.05 0.34 Q17 1 0.3943 0.3850 0.2527 11.00000 0.05 0.33 Q18 1 0.5070 0.2163 0.3718 11.00000 0.05 0.33 Q19 1 0.8573 0.1165 0.1623 11.00000 0.05 0.33 Q20 1 0.6403 0.0747 0.2264 11.00000 0.05 0.33 ; _shelx_res_checksum 76390 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.56694(2) 0.69757(2) 0.12524(2) 0.01471(3) Uani 1 1 d . . . . . Si1 Si 0.76649(3) 0.39194(3) 0.25610(2) 0.01278(7) Uani 1 1 d . . . . . Al1 Al 0.70831(3) 0.22776(3) 0.22558(2) 0.01123(7) Uani 1 1 d . . . . . O1 O 0.76365(7) 0.27410(7) 0.27779(6) 0.01390(17) Uani 1 1 d . . . . . O2 O 0.66379(7) 0.48843(7) 0.19439(6) 0.01531(18) Uani 1 1 d D . . . . H2 H 0.6428(13) 0.4601(13) 0.1703(11) 0.023 Uiso 1 1 d D U . . . O3 O 0.76150(8) 0.42108(8) 0.34450(6) 0.01862(19) Uani 1 1 d . . . . . O4 O 0.86679(7) 0.40764(8) 0.19299(6) 0.01722(18) Uani 1 1 d . . . . . O5 O 0.63217(7) 0.34795(7) 0.14547(6) 0.01525(17) Uani 1 1 d D . . . . H5 H 0.5967(12) 0.3486(14) 0.1115(10) 0.023 Uiso 1 1 d D U . . . N1 N 0.62598(8) 0.15088(9) 0.29847(7) 0.0132(2) Uani 1 1 d . . . . . N2 N 0.80587(8) 0.11734(9) 0.17842(7) 0.0137(2) Uani 1 1 d . . . . . C1 C 0.52774(11) 0.04159(12) 0.31083(10) 0.0217(3) Uani 1 1 d . . . . . H1A H 0.5167 0.0323 0.3752 0.033 Uiso 1 1 calc R U . . . H1B H 0.5463 -0.0291 0.3032 0.033 Uiso 1 1 calc R U . . . H1C H 0.4632 0.0971 0.2798 0.033 Uiso 1 1 calc R U . . . C2 C 0.61537(10) 0.07924(10) 0.27124(9) 0.0154(2) Uani 1 1 d . . . . . C3 C 0.68339(10) 0.03489(11) 0.20688(9) 0.0162(2) Uani 1 1 d . . . . . H3 H 0.6639 -0.0078 0.1871 0.019 Uiso 1 1 calc R U . . . C4 C 0.77674(10) 0.04602(10) 0.16829(9) 0.0156(2) Uani 1 1 d . . . . . C5 C 0.84650(11) -0.02804(13) 0.11479(11) 0.0245(3) Uani 1 1 d . . . . . H5A H 0.8089 -0.0657 0.1058 0.037 Uiso 1 1 calc R U . . . H5B H 0.9098 -0.0831 0.1477 0.037 Uiso 1 1 calc R U . . . H5C H 0.8661 0.0165 0.0560 0.037 Uiso 1 1 calc R U . . . C6 C 0.56084(10) 0.18053(11) 0.37441(8) 0.0146(2) Uani 1 1 d . . . . . C7 C 0.45913(10) 0.26453(11) 0.36168(9) 0.0162(2) Uani 1 1 d . . . . . C8 C 0.40197(11) 0.29420(12) 0.43628(10) 0.0204(3) Uani 1 1 d . . . . . H8 H 0.3335 0.3519 0.4288 0.024 Uiso 1 1 calc R U . . . C9 C 0.44340(12) 0.24099(12) 0.52065(10) 0.0222(3) Uani 1 1 d . . . . . H9 H 0.4032 0.2616 0.5707 0.027 Uiso 1 1 calc R U . . . C10 C 0.54353(11) 0.15762(12) 0.53228(9) 0.0203(3) Uani 1 1 d . . . . . H10 H 0.5713 0.1219 0.5905 0.024 Uiso 1 1 calc R U . . . C11 C 0.60463(10) 0.12481(11) 0.46043(9) 0.0164(2) Uani 1 1 d . . . . . C12 C 0.71441(11) 0.03198(12) 0.47508(9) 0.0209(3) Uani 1 1 d . . . . . H12 H 0.7620 0.0567 0.4250 0.025 Uiso 1 1 calc R U . . . C13 C 0.75859(13) 0.00483(14) 0.56429(10) 0.0302(3) Uani 1 1 d . . . . . H13A H 0.7198 -0.0301 0.6147 0.045 Uiso 1 1 calc R U . . . H13B H 0.7514 0.0731 0.5700 0.045 Uiso 1 1 calc R U . . . H13C H 0.8329 -0.0459 0.5652 0.045 Uiso 1 1 calc R U . . . C14 C 0.71887(14) -0.07547(13) 0.47186(11) 0.0303(3) Uani 1 1 d . . . . . H14A H 0.6662 -0.0965 0.5151 0.046 Uiso 1 1 calc R U . . . H14B H 0.7887 -0.1346 0.4875 0.046 Uiso 1 1 calc R U . . . H14C H 0.7045 -0.0637 0.4109 0.046 Uiso 1 1 calc R U . . . C15 C 0.40661(10) 0.32453(11) 0.27148(9) 0.0181(3) Uani 1 1 d . . . . . H15 H 0.4545 0.2896 0.2269 0.022 Uiso 1 1 calc R U . . . C16 C 0.38745(12) 0.44716(12) 0.23602(11) 0.0261(3) Uani 1 1 d . . . . . H16A H 0.4541 0.4533 0.2305 0.039 Uiso 1 1 calc R U . . . H16B H 0.3391 0.4833 0.2782 0.039 Uiso 1 1 calc R U . . . H16C H 0.3569 0.4831 0.1768 0.039 Uiso 1 1 calc R U . . . C17 C 0.30228(11) 0.31479(15) 0.27914(10) 0.0272(3) Uani 1 1 d . . . . . H17A H 0.2533 0.3512 0.3209 0.041 Uiso 1 1 calc R U . . . H17B H 0.3145 0.2366 0.3019 0.041 Uiso 1 1 calc R U . . . H17C H 0.2725 0.3504 0.2196 0.041 Uiso 1 1 calc R U . . . C18 C 0.91310(10) 0.10556(11) 0.15117(9) 0.0156(2) Uani 1 1 d . . . . . C19 C 0.99283(10) 0.02201(11) 0.21008(9) 0.0191(3) Uani 1 1 d . . . . . C20 C 1.09590(11) 0.01017(12) 0.18332(10) 0.0232(3) Uani 1 1 d . . . . . H20 H 1.1510 -0.0462 0.2217 0.028 Uiso 1 1 calc R U . . . C21 C 1.11904(11) 0.07919(12) 0.10174(11) 0.0239(3) Uani 1 1 d . . . . . H21 H 1.1897 0.0700 0.0847 0.029 Uiso 1 1 calc R U . . . C22 C 1.03994(11) 0.16136(12) 0.04503(10) 0.0207(3) Uani 1 1 d . . . . . H22 H 1.0568 0.2086 -0.0105 0.025 Uiso 1 1 calc R U . . . C23 C 0.93529(10) 0.17624(11) 0.06794(9) 0.0170(2) Uani 1 1 d . . . . . C24 C 0.85189(11) 0.26550(12) 0.00114(9) 0.0199(3) Uani 1 1 d . . . . . H24 H 0.7823 0.2649 0.0281 0.024 Uiso 1 1 calc R U . . . C25 C 0.84706(13) 0.38030(12) -0.01771(11) 0.0286(3) Uani 1 1 d . . . . . H25A H 0.8333 0.3951 0.0391 0.043 Uiso 1 1 calc R U . . . H25B H 0.7907 0.4362 -0.0586 0.043 Uiso 1 1 calc R U . . . H25C H 0.9141 0.3831 -0.0457 0.043 Uiso 1 1 calc R U . . . C26 C 0.87211(13) 0.24277(14) -0.08786(10) 0.0298(3) Uani 1 1 d . . . . . H26A H 0.8738 0.1698 -0.0759 0.045 Uiso 1 1 calc R U . . . H26B H 0.9395 0.2444 -0.1159 0.045 Uiso 1 1 calc R U . . . H26C H 0.8159 0.2995 -0.1287 0.045 Uiso 1 1 calc R U . . . C27 C 0.97116(11) -0.05351(12) 0.30214(10) 0.0223(3) Uani 1 1 d . . . . . H27 H 0.8968 -0.0436 0.3054 0.027 Uiso 1 1 calc R U . . . C28 C 0.98387(12) -0.02049(13) 0.37716(10) 0.0263(3) Uani 1 1 d . . . . . H28A H 0.9690 -0.0690 0.4359 0.039 Uiso 1 1 calc R U . . . H28B H 0.9349 0.0564 0.3694 0.039 Uiso 1 1 calc R U . . . H28C H 1.0559 -0.0277 0.3742 0.039 Uiso 1 1 calc R U . . . C29 C 1.04242(15) -0.17597(13) 0.31624(12) 0.0344(4) Uani 1 1 d . . . . . H29A H 1.0238 -0.2220 0.3747 0.052 Uiso 1 1 calc R U . . . H29B H 1.1157 -0.1881 0.3151 0.052 Uiso 1 1 calc R U . . . H29C H 1.0331 -0.1960 0.2680 0.052 Uiso 1 1 calc R U . . . C30 C 0.72409(13) 0.38411(12) 0.43704(9) 0.0227(3) Uani 1 1 d . . . . . C31 C 0.72948(17) 0.45802(16) 0.48060(11) 0.0384(4) Uani 1 1 d . . . . . H31A H 0.7068 0.4357 0.5445 0.058 Uiso 1 1 calc R U . . . H31B H 0.6834 0.5351 0.4500 0.058 Uiso 1 1 calc R U . . . H31C H 0.8017 0.4510 0.4754 0.058 Uiso 1 1 calc R U . . . C32 C 0.61282(15) 0.39625(17) 0.44043(12) 0.0369(4) Uani 1 1 d . . . . . H32A H 0.5882 0.3712 0.5035 0.055 Uiso 1 1 calc R U . . . H32B H 0.6107 0.3514 0.4088 0.055 Uiso 1 1 calc R U . . . H32C H 0.5674 0.4740 0.4113 0.055 Uiso 1 1 calc R U . . . C33 C 0.79691(19) 0.26474(15) 0.48191(12) 0.0461(5) Uani 1 1 d . . . . . H33A H 0.7746 0.2398 0.5457 0.069 Uiso 1 1 calc R U . . . H33B H 0.8687 0.2588 0.4772 0.069 Uiso 1 1 calc R U . . . H33C H 0.7945 0.2185 0.4518 0.069 Uiso 1 1 calc R U . . . C34 C 0.97596(11) 0.36376(12) 0.21318(10) 0.0217(3) Uani 1 1 d . . . . . C35 C 1.01356(12) 0.24186(13) 0.26943(12) 0.0305(3) Uani 1 1 d . . . . . H35A H 0.9752 0.2332 0.3282 0.046 Uiso 1 1 calc R U . . . H35B H 1.0888 0.2112 0.2782 0.046 Uiso 1 1 calc R U . . . H35C H 1.0009 0.2026 0.2382 0.046 Uiso 1 1 calc R U . . . C36 C 1.03606(12) 0.37954(14) 0.12218(11) 0.0298(3) Uani 1 1 d . . . . . H36A H 1.1104 0.3539 0.1313 0.045 Uiso 1 1 calc R U . . . H36B H 1.0080 0.4581 0.0853 0.045 Uiso 1 1 calc R U . . . H36C H 1.0284 0.3369 0.0913 0.045 Uiso 1 1 calc R U . . . C37 C 0.98743(12) 0.42918(15) 0.26207(13) 0.0334(4) Uani 1 1 d . . . . . H37A H 1.0611 0.3997 0.2756 0.050 Uiso 1 1 calc R U . . . H37B H 0.9443 0.4229 0.3185 0.050 Uiso 1 1 calc R U . . . H37C H 0.9643 0.5071 0.2237 0.050 Uiso 1 1 calc R U . . . C38 C 0.52276(15) 0.78833(13) -0.05774(10) 0.0329(4) Uani 1 1 d . . . . . H38 H 0.5223 0.8601 -0.0867 0.039 Uiso 1 1 calc R U . . . C39 C 0.43653(15) 0.76445(16) -0.01427(11) 0.0370(4) Uani 1 1 d . . . . . H39 H 0.3672 0.8170 -0.0088 0.044 Uiso 1 1 calc R U . . . C40 C 0.47078(16) 0.64828(16) 0.01999(11) 0.0374(4) Uani 1 1 d . . . . . H40 H 0.4288 0.6088 0.0532 0.045 Uiso 1 1 calc R U . . . C41 C 0.57758(16) 0.60198(14) -0.00375(10) 0.0353(4) Uani 1 1 d . . . . . H41 H 0.6206 0.5252 0.0100 0.042 Uiso 1 1 calc R U . . . C42 C 0.61053(15) 0.68748(14) -0.05115(10) 0.0329(4) Uani 1 1 d . . . . . H42 H 0.6796 0.6791 -0.0747 0.039 Uiso 1 1 calc R U . . . C43 C 0.4231(8) 0.8299(5) 0.2258(6) 0.0405(13) Uani 0.61(3) 1 d D U P A 1 H43 H 0.4358 0.8921 0.2183 0.049 Uiso 0.61(3) 1 calc R U P A 1 C44 C 0.4636(8) 0.7247(7) 0.2934(6) 0.0337(12) Uani 0.61(3) 1 d D U P A 1 H44 H 0.5051 0.7047 0.3414 0.040 Uiso 0.61(3) 1 calc R U P A 1 C45 C 0.4308(11) 0.6549(6) 0.2760(8) 0.0316(12) Uani 0.61(3) 1 d D U P A 1 H45 H 0.4507 0.5780 0.3079 0.038 Uiso 0.61(3) 1 calc R U P A 1 C46 C 0.3639(7) 0.7186(8) 0.2038(6) 0.0356(11) Uani 0.61(3) 1 d D U P A 1 H46 H 0.3271 0.6941 0.1803 0.043 Uiso 0.61(3) 1 calc R U P A 1 C47 C 0.3613(6) 0.8261(6) 0.1725(5) 0.0393(14) Uani 0.61(3) 1 d D U P A 1 H47 H 0.3234 0.8861 0.1229 0.047 Uiso 0.61(3) 1 calc R U P A 1 C43A C 0.4462(11) 0.8219(9) 0.2395(9) 0.0346(15) Uani 0.39(3) 1 d D U P A 2 H43A H 0.4660 0.8752 0.2426 0.041 Uiso 0.39(3) 1 calc R U P A 2 C44A C 0.4839(12) 0.7086(11) 0.2933(8) 0.0325(17) Uani 0.39(3) 1 d D U P A 2 H44A H 0.5399 0.6693 0.3331 0.039 Uiso 0.39(3) 1 calc R U P A 2 C45A C 0.4213(18) 0.6650(10) 0.2759(14) 0.036(2) Uani 0.39(3) 1 d D U P A 2 H45A H 0.4208 0.5941 0.3087 0.044 Uiso 0.39(3) 1 calc R U P A 2 C46A C 0.3605(11) 0.7446(12) 0.2019(11) 0.0369(17) Uani 0.39(3) 1 d D U P A 2 H46A H 0.3175 0.7349 0.1713 0.044 Uiso 0.39(3) 1 calc R U P A 2 C47A C 0.3753(11) 0.8415(9) 0.1816(8) 0.0394(19) Uani 0.39(3) 1 d D U P A 2 H47A H 0.3420 0.9097 0.1355 0.047 Uiso 0.39(3) 1 calc R U P A 2 C48 C 0.74914(13) 0.68133(14) 0.18053(13) 0.0342(4) Uani 1 1 d . . . . . H48 H 0.7792 0.6192 0.2322 0.041 Uiso 1 1 calc R U . . . C49 C 0.67448(15) 0.78577(14) 0.18083(13) 0.0370(4) Uani 1 1 d . . . . . H49 H 0.6454 0.8072 0.2326 0.044 Uiso 1 1 calc R U . . . C50 C 0.64983(16) 0.85385(14) 0.09034(14) 0.0401(4) Uani 1 1 d . . . . . H50 H 0.6004 0.9286 0.0706 0.048 Uiso 1 1 calc R U . . . C51 C 0.71151(16) 0.79091(17) 0.03538(14) 0.0418(4) Uani 1 1 d . . . . . H51 H 0.7122 0.8163 -0.0286 0.050 Uiso 1 1 calc R U . . . C52 C 0.77207(13) 0.68439(16) 0.09026(14) 0.0383(4) Uani 1 1 d . . . . . H52 H 0.8201 0.6247 0.0703 0.046 Uiso 1 1 calc R U . . . C53 C 0.0612(12) 0.3923(14) 0.5849(11) 0.051(3) Uani 0.361(4) 1 d D U P B -1 C54 C 0.1022(10) 0.4073(11) 0.4964(8) 0.044(2) Uani 0.361(4) 1 d D U P B -1 H54 H 0.1693 0.3546 0.4855 0.053 Uiso 0.361(4) 1 calc R U P B -1 C55 C 0.0490(12) 0.4962(14) 0.4235(9) 0.045(3) Uani 0.361(4) 1 d D U P B -1 H55 H 0.0788 0.5020 0.3640 0.054 Uiso 0.361(4) 1 calc R U P B -1 C56 C -0.0480(10) 0.5769(10) 0.4373(8) 0.044(2) Uani 0.361(4) 1 d D U P B -1 H56 H -0.0859 0.6373 0.3879 0.053 Uiso 0.361(4) 1 calc R U P B -1 C57 C -0.0876(11) 0.5665(12) 0.5252(8) 0.045(3) Uani 0.361(4) 1 d D U P B -1 H57 H -0.1513 0.6229 0.5368 0.053 Uiso 0.361(4) 1 calc R U P B -1 C58 C -0.0344(11) 0.4734(11) 0.5974(8) 0.046(2) Uani 0.361(4) 1 d D U P B -1 H58 H -0.0652 0.4661 0.6568 0.055 Uiso 0.361(4) 1 calc R U P B -1 C59 C 0.1189(7) 0.3131(9) 0.6482(7) 0.070(2) Uani 0.361(4) 1 d D U P B -1 H59A H 0.1462 0.2441 0.6352 0.105 Uiso 0.361(4) 1 calc R U P B -1 H59B H 0.0774 0.3059 0.7054 0.105 Uiso 0.361(4) 1 calc R U P B -1 H59C H 0.1775 0.3284 0.6525 0.105 Uiso 0.361(4) 1 calc R U P B -1 C53A C 0.0321(11) 0.4729(13) 0.5185(10) 0.046(3) Uani 0.139(4) 1 d D U P B -2 C54A C 0.0706(16) 0.495(3) 0.4293(12) 0.051(6) Uani 0.139(4) 1 d D U P B -2 H54A H 0.1399 0.4478 0.4161 0.061 Uiso 0.139(4) 1 calc R U P B -2 C55A C 0.0116(13) 0.5824(15) 0.3586(10) 0.057(4) Uani 0.139(4) 1 d D U P B -2 H55A H 0.0419 0.5958 0.2989 0.068 Uiso 0.139(4) 1 calc R U P B -2 C56A C -0.0919(15) 0.6508(19) 0.3746(13) 0.053(4) Uani 0.139(4) 1 d D U P B -2 H56A H -0.1358 0.7053 0.3263 0.064 Uiso 0.139(4) 1 calc R U P B -2 C57A C -0.1279(12) 0.6361(16) 0.4637(14) 0.057(4) Uani 0.139(4) 1 d D U P B -2 H57A H -0.1920 0.6899 0.4780 0.069 Uiso 0.139(4) 1 calc R U P B -2 C58A C -0.070(2) 0.542(3) 0.5333(14) 0.057(6) Uani 0.139(4) 1 d D U P B -2 H58A H -0.1021 0.5251 0.5921 0.068 Uiso 0.139(4) 1 calc R U P B -2 C59A C 0.0906(18) 0.389(3) 0.5793(18) 0.058(6) Uani 0.139(4) 1 d D U P B -2 H59D H 0.1186 0.3235 0.5607 0.087 Uiso 0.139(4) 1 calc R U P B -2 H59E H 0.0493 0.3759 0.6363 0.087 Uiso 0.139(4) 1 calc R U P B -2 H59F H 0.1487 0.4023 0.5875 0.087 Uiso 0.139(4) 1 calc R U P B -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 Ce1 0.01539(4) 0.01321(4) 0.01613(4) -0.00660(3) -0.00216(3) -0.00433(3) Si1 0.01360(15) 0.01356(15) 0.01310(16) -0.00450(12) -0.00221(12) -0.00646(13) Al1 0.01118(16) 0.01180(16) 0.01185(17) -0.00470(13) -0.00029(13) -0.00512(13) O1 0.0147(4) 0.0136(4) 0.0148(4) -0.0046(3) -0.0025(3) -0.0064(3) O2 0.0159(4) 0.0136(4) 0.0181(4) -0.0056(3) -0.0043(3) -0.0058(3) O3 0.0273(5) 0.0200(5) 0.0148(4) -0.0067(4) -0.0019(4) -0.0137(4) O4 0.0136(4) 0.0202(5) 0.0194(5) -0.0053(4) -0.0019(3) -0.0088(4) O5 0.0159(4) 0.0153(4) 0.0157(4) -0.0052(3) -0.0044(3) -0.0058(4) N1 0.0131(5) 0.0144(5) 0.0131(5) -0.0051(4) 0.0001(4) -0.0065(4) N2 0.0119(5) 0.0150(5) 0.0153(5) -0.0070(4) 0.0006(4) -0.0052(4) C1 0.0245(7) 0.0247(7) 0.0249(7) -0.0121(6) 0.0056(5) -0.0172(6) C2 0.0168(6) 0.0144(6) 0.0159(6) -0.0037(5) -0.0022(5) -0.0078(5) C3 0.0181(6) 0.0151(6) 0.0190(6) -0.0077(5) -0.0017(5) -0.0076(5) C4 0.0160(6) 0.0143(6) 0.0158(6) -0.0059(5) -0.0023(5) -0.0042(5) C5 0.0218(7) 0.0258(7) 0.0321(8) -0.0202(6) 0.0051(6) -0.0088(6) C6 0.0170(6) 0.0170(6) 0.0146(6) -0.0065(5) 0.0020(5) -0.0111(5) C7 0.0167(6) 0.0201(6) 0.0165(6) -0.0079(5) 0.0016(5) -0.0109(5) C8 0.0190(6) 0.0247(7) 0.0223(7) -0.0133(6) 0.0035(5) -0.0103(5) C9 0.0265(7) 0.0298(7) 0.0190(7) -0.0150(6) 0.0069(5) -0.0165(6) C10 0.0284(7) 0.0248(7) 0.0142(6) -0.0062(5) 0.0008(5) -0.0173(6) C11 0.0196(6) 0.0180(6) 0.0152(6) -0.0040(5) 0.0000(5) -0.0122(5) C12 0.0216(7) 0.0223(7) 0.0166(6) -0.0024(5) -0.0028(5) -0.0097(6) C13 0.0316(8) 0.0345(8) 0.0211(7) -0.0020(6) -0.0089(6) -0.0134(7) C14 0.0376(9) 0.0196(7) 0.0262(8) -0.0040(6) -0.0069(6) -0.0062(6) C15 0.0132(6) 0.0238(7) 0.0170(6) -0.0086(5) 0.0003(5) -0.0062(5) C16 0.0221(7) 0.0223(7) 0.0267(7) -0.0073(6) -0.0003(6) -0.0043(6) C17 0.0169(7) 0.0451(9) 0.0249(7) -0.0172(7) 0.0013(5) -0.0136(6) C18 0.0120(6) 0.0166(6) 0.0194(6) -0.0095(5) 0.0015(5) -0.0050(5) C19 0.0164(6) 0.0176(6) 0.0221(7) -0.0070(5) -0.0011(5) -0.0055(5) C20 0.0136(6) 0.0210(7) 0.0302(8) -0.0081(6) -0.0031(5) -0.0025(5) C21 0.0128(6) 0.0259(7) 0.0323(8) -0.0130(6) 0.0037(5) -0.0069(5) C22 0.0180(6) 0.0223(7) 0.0223(7) -0.0098(5) 0.0054(5) -0.0093(5) C23 0.0152(6) 0.0179(6) 0.0183(6) -0.0093(5) 0.0010(5) -0.0053(5) C24 0.0183(6) 0.0229(7) 0.0158(6) -0.0059(5) 0.0000(5) -0.0070(5) C25 0.0350(8) 0.0207(7) 0.0243(7) -0.0042(6) -0.0067(6) -0.0070(6) C26 0.0319(8) 0.0351(8) 0.0221(7) -0.0129(6) -0.0045(6) -0.0093(7) C27 0.0191(6) 0.0208(7) 0.0226(7) -0.0022(5) -0.0046(5) -0.0071(5) C28 0.0230(7) 0.0267(7) 0.0248(7) -0.0071(6) -0.0029(6) -0.0071(6) C29 0.0466(10) 0.0205(7) 0.0295(8) -0.0040(6) -0.0058(7) -0.0102(7) C30 0.0374(8) 0.0223(7) 0.0123(6) -0.0061(5) -0.0030(5) -0.0144(6) C31 0.0670(13) 0.0415(10) 0.0238(8) -0.0182(7) -0.0007(8) -0.0310(9) C32 0.0435(10) 0.0512(11) 0.0305(9) -0.0230(8) 0.0144(7) -0.0306(9) C33 0.0761(15) 0.0265(9) 0.0249(8) -0.0009(7) -0.0213(9) -0.0103(9) C34 0.0140(6) 0.0243(7) 0.0286(7) -0.0091(6) -0.0029(5) -0.0083(5) C35 0.0195(7) 0.0271(8) 0.0365(9) -0.0044(7) -0.0068(6) -0.0056(6) C36 0.0196(7) 0.0358(9) 0.0363(9) -0.0133(7) 0.0045(6) -0.0150(6) C37 0.0204(7) 0.0449(10) 0.0484(10) -0.0256(8) -0.0035(7) -0.0154(7) C38 0.0536(11) 0.0241(8) 0.0185(7) -0.0001(6) -0.0107(7) -0.0159(7) C39 0.0385(9) 0.0422(10) 0.0261(8) -0.0032(7) -0.0184(7) -0.0126(8) C40 0.0583(12) 0.0486(10) 0.0209(8) -0.0036(7) -0.0136(7) -0.0364(9) C41 0.0667(12) 0.0260(8) 0.0170(7) -0.0078(6) -0.0097(7) -0.0184(8) C42 0.0469(10) 0.0351(9) 0.0163(7) -0.0095(6) 0.0008(6) -0.0168(8) C43 0.036(3) 0.0394(17) 0.051(3) -0.0362(17) 0.004(2) -0.0050(19) C44 0.034(3) 0.045(2) 0.0314(17) -0.0303(16) 0.0112(17) -0.015(2) C45 0.029(3) 0.050(2) 0.0256(18) -0.0253(17) 0.0112(18) -0.019(2) C46 0.0184(16) 0.045(3) 0.0471(19) -0.029(2) 0.0078(13) -0.009(2) C47 0.021(2) 0.038(2) 0.056(2) -0.0319(17) -0.0010(14) 0.0040(16) C43A 0.029(4) 0.044(3) 0.041(3) -0.033(2) 0.004(2) -0.010(2) C44A 0.036(4) 0.042(3) 0.026(2) -0.026(2) 0.010(2) -0.013(3) C45A 0.029(3) 0.048(3) 0.035(3) -0.024(3) 0.013(3) -0.016(3) C46A 0.019(2) 0.048(4) 0.049(3) -0.031(3) 0.0032(19) -0.008(3) C47A 0.025(3) 0.036(3) 0.058(3) -0.032(2) -0.001(2) 0.001(2) C48 0.0317(8) 0.0280(8) 0.0491(10) -0.0059(7) -0.0145(7) -0.0178(7) C49 0.0476(10) 0.0283(8) 0.0477(10) -0.0127(7) -0.0148(8) -0.0207(8) C50 0.0499(11) 0.0216(8) 0.0552(11) -0.0022(7) -0.0194(9) -0.0216(8) C51 0.0492(11) 0.0455(11) 0.0405(10) -0.0037(8) 0.0008(8) -0.0380(9) C52 0.0251(8) 0.0376(9) 0.0563(12) -0.0130(8) 0.0037(7) -0.0211(7) C53 0.050(6) 0.062(6) 0.066(5) -0.033(4) 0.007(5) -0.039(4) C54 0.032(4) 0.048(5) 0.064(5) -0.026(4) 0.008(4) -0.024(4) C55 0.047(5) 0.059(6) 0.050(5) -0.038(4) 0.016(4) -0.031(4) C56 0.042(4) 0.051(5) 0.060(5) -0.030(4) -0.005(4) -0.026(4) C57 0.038(5) 0.055(6) 0.060(5) -0.043(5) 0.012(4) -0.020(4) C58 0.049(5) 0.061(6) 0.051(5) -0.033(4) 0.007(4) -0.034(4) C59 0.068(5) 0.083(7) 0.083(5) -0.031(5) -0.021(4) -0.040(4) C53A 0.050(5) 0.054(6) 0.060(6) -0.036(5) 0.005(5) -0.031(5) C54A 0.049(7) 0.055(7) 0.058(7) -0.040(6) 0.007(6) -0.017(6) C55A 0.068(7) 0.059(7) 0.063(6) -0.036(5) -0.002(6) -0.029(6) C56A 0.057(7) 0.056(9) 0.060(7) -0.016(7) -0.031(7) -0.024(6) C57A 0.045(7) 0.063(8) 0.073(7) -0.030(6) 0.004(6) -0.027(5) C58A 0.054(7) 0.062(8) 0.059(7) -0.027(7) 0.010(6) -0.027(6) C59A 0.065(11) 0.064(10) 0.072(10) -0.027(8) 0.002(10) -0.048(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' O O 0.0106 0.0060 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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 O2 Ce1 C44A 89.9(3) O2 Ce1 C52 81.78(4) C44A Ce1 C52 113.9(3) O2 Ce1 C38 118.51(4) C44A Ce1 C38 143.5(3) C52 Ce1 C38 93.72(6) O2 Ce1 C51 109.66(5) C44A Ce1 C51 119.8(3) C52 Ce1 C51 28.88(6) C38 Ce1 C51 74.12(6) O2 Ce1 C47 126.05(17) C52 Ce1 C47 143.8(2) C38 Ce1 C47 91.55(16) C51 Ce1 C47 121.8(2) O2 Ce1 C47A 129.5(2) C44A Ce1 C47A 48.1(2) C52 Ce1 C47A 135.3(3) C38 Ce1 C47A 95.5(2) C51 Ce1 C47A 115.3(3) O2 Ce1 C50 125.86(4) C44A Ce1 C50 93.8(3) C52 Ce1 C50 47.75(6) C38 Ce1 C50 87.46(5) C51 Ce1 C50 28.81(6) C47 Ce1 C50 96.8(2) C47A Ce1 C50 89.1(3) O2 Ce1 C48 79.07(4) C44A Ce1 C48 84.9(3) C52 Ce1 C48 29.05(6) C38 Ce1 C48 120.69(6) C51 Ce1 C48 47.56(6) C47 Ce1 C48 124.7(2) C47A Ce1 C48 116.0(3) C50 Ce1 C48 47.70(5) O2 Ce1 C43 122.71(16) C52 Ce1 C43 119.5(2) C38 Ce1 C43 112.6(2) C51 Ce1 C43 107.55(18) C47 Ce1 C43 28.59(11) C50 Ce1 C43 78.87(18) C48 Ce1 C43 96.4(2) O2 Ce1 C39 113.82(4) C44A Ce1 C39 121.1(3) C52 Ce1 C39 122.08(6) C38 Ce1 C39 28.79(5) C51 Ce1 C39 102.30(6) C47 Ce1 C39 71.6(2) C47A Ce1 C39 78.3(3) C50 Ce1 C39 109.88(5) C48 Ce1 C39 149.45(6) C43 Ce1 C39 98.6(2) O2 Ce1 C45 79.99(19) C52 Ce1 C45 138.28(18) C38 Ce1 C45 127.93(18) C51 Ce1 C45 149.44(19) C47 Ce1 C45 47.47(18) C50 Ce1 C45 122.28(19) C48 Ce1 C45 110.14(18) C43 Ce1 C45 47.75(19) C39 Ce1 C45 99.61(18) O1 Si1 O3 114.27(5) O1 Si1 O4 114.36(5) O3 Si1 O4 107.30(5) O1 Si1 O2 107.26(5) O3 Si1 O2 108.98(5) O4 Si1 O2 104.10(5) O1 Al1 O5 103.31(5) O1 Al1 N2 114.36(5) O5 Al1 N2 114.26(5) O1 Al1 N1 117.48(5) O5 Al1 N1 110.01(5) N2 Al1 N1 97.89(5) Si1 O1 Al1 133.16(6) H2 O2 Si1 110.1(12) H2 O2 Ce1 107.1(12) Si1 O2 Ce1 141.60(5) C30 O3 Si1 133.89(9) C34 O4 Si1 131.34(9) H5 O5 Al1 122.9(12) C2 N1 C6 119.17(10) C2 N1 Al1 118.72(9) C6 N1 Al1 121.32(8) C4 N2 C18 117.49(10) C4 N2 Al1 119.73(9) C18 N2 Al1 122.77(8) N1 C2 C3 123.16(12) N1 C2 C1 120.35(11) C3 C2 C1 116.49(11) C2 C3 C4 127.55(12) N2 C4 C3 122.93(12) N2 C4 C5 120.13(12) C3 C4 C5 116.93(12) C7 C6 C11 121.50(12) C7 C6 N1 120.55(11) C11 C6 N1 117.91(11) C8 C7 C6 118.18(12) C8 C7 C15 118.03(12) C6 C7 C15 123.79(11) C9 C8 C7 121.16(13) C8 C9 C10 119.97(13) C9 C10 C11 121.56(13) C10 C11 C6 117.62(12) C10 C11 C12 120.60(12) C6 C11 C12 121.77(12) C11 C12 C13 113.35(12) C11 C12 C14 112.27(12) C13 C12 C14 108.05(12) C7 C15 C17 111.40(11) C7 C15 C16 110.95(11) C17 C15 C16 109.50(12) C23 C18 C19 121.65(12) C23 C18 N2 120.16(11) C19 C18 N2 118.19(12) C20 C19 C18 118.06(13) C20 C19 C27 118.90(12) C18 C19 C27 123.02(12) C21 C20 C19 121.01(13) C22 C21 C20 120.28(13) C21 C22 C23 121.18(13) C22 C23 C18 117.81(12) C22 C23 C24 118.83(12) C18 C23 C24 123.34(12) C23 C24 C25 111.35(12) C23 C24 C26 111.09(12) C25 C24 C26 109.53(12) C19 C27 C28 110.17(12) C19 C27 C29 111.91(12) C28 C27 C29 110.42(12) O3 C30 C32 110.21(12) O3 C30 C33 108.59(13) C32 C30 C33 111.11(15) O3 C30 C31 105.38(12) C32 C30 C31 111.03(14) C33 C30 C31 110.35(14) O4 C34 C35 109.84(11) O4 C34 C37 109.46(12) C35 C34 C37 111.21(14) O4 C34 C36 105.65(12) C35 C34 C36 110.43(13) C37 C34 C36 110.10(13) C39 C38 C42 108.14(15) C39 C38 Ce1 76.35(9) C42 C38 Ce1 76.36(9) C38 C39 C40 107.90(17) C38 C39 Ce1 74.85(9) C40 C39 Ce1 76.56(9) C41 C40 C39 107.66(16) C41 C40 Ce1 76.17(9) C39 C40 Ce1 74.56(9) C42 C41 C40 108.63(16) C42 C41 Ce1 74.50(9) C40 C41 Ce1 75.44(9) C41 C42 C38 107.66(17) C41 C42 Ce1 77.00(9) C38 C42 Ce1 74.62(9) C47 C43 C44 108.0(3) C47 C43 Ce1 75.4(4) C44 C43 Ce1 77.9(4) C43 C44 C45 107.2(3) C43 C44 Ce1 73.3(4) C45 C44 Ce1 73.5(8) C46 C45 C44 108.3(3) C46 C45 Ce1 76.4(6) C44 C45 Ce1 77.7(7) C45 C46 C47 107.3(3) C45 C46 Ce1 75.0(6) C47 C46 Ce1 74.3(5) C43 C47 C46 109.0(3) C43 C47 Ce1 76.1(4) C46 C47 Ce1 76.7(5) C47A C43A C44A 108.0(4) C47A C43A Ce1 75.2(7) C44A C43A Ce1 72.2(7) C43A C44A C45A 106.5(5) C43A C44A Ce1 78.4(7) C45A C44A Ce1 80.4(13) C46A C45A C44A 108.2(5) C46A C45A Ce1 73.8(11) C44A C45A Ce1 70.4(12) C45A C46A C47A 107.0(4) C45A C46A Ce1 77.7(11) C47A C46A Ce1 75.0(8) C43A C47A C46A 109.3(4) C43A C47A Ce1 76.4(7) C46A C47A Ce1 76.1(8) C49 C48 C52 108.07(16) C49 C48 Ce1 76.35(9) C52 C48 Ce1 74.83(9) C48 C49 C50 107.96(18) C48 C49 Ce1 74.99(9) C50 C49 Ce1 74.71(9) C51 C50 C49 107.50(17) C51 C50 Ce1 75.36(9) C49 C50 Ce1 76.26(9) C52 C51 C50 108.69(18) C52 C51 Ce1 75.26(9) C50 C51 Ce1 75.84(10) C51 C52 C48 107.77(17) C51 C52 Ce1 75.86(10) C48 C52 Ce1 76.11(9) C59 C53 C58 124.8(11) C59 C53 C54 118.2(9) C58 C53 C54 116.4(9) C55 C54 C53 122.6(9) C54 C55 C56 120.2(9) C57 C56 C55 118.0(8) C56 C57 C58 120.6(8) C53 C58 C57 122.0(9) C59A C53A C58A 125.1(13) C59A C53A C54A 118.7(12) C58A C53A C54A 116.2(11) C55A C54A C53A 122.6(12) C54A C55A C56A 120.5(11) C57A C56A C55A 117.2(10) C56A C57A C58A 120.4(11) C53A C58A C57A 121.9(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ce1 O2 2.5499(9) Ce1 C44A 2.749(15) Ce1 C52 2.7998(16) Ce1 C38 2.8016(15) Ce1 C51 2.8073(17) Ce1 C47 2.808(8) Ce1 C47A 2.813(13) Ce1 C50 2.8133(16) Ce1 C48 2.8160(16) Ce1 C43 2.817(8) Ce1 C39 2.8204(15) Ce1 C45 2.822(15) Si1 O1 1.6106(9) Si1 O3 1.6149(10) Si1 O4 1.6221(10) Si1 O2 1.6686(9) Al1 O1 1.7269(9) Al1 O5 1.7334(10) Al1 N2 1.8814(11) Al1 N1 1.8862(11) O2 H2 0.832(9) O3 C30 1.4451(16) O4 C34 1.4533(16) O5 H5 0.818(9) N1 C2 1.3428(16) N1 C6 1.4521(16) N2 C4 1.3420(16) N2 C18 1.4524(16) C1 C2 1.5073(18) C2 C3 1.3979(18) C3 C4 1.3982(18) C4 C5 1.5051(18) C6 C7 1.4031(18) C6 C11 1.4174(18) C7 C8 1.4003(18) C7 C15 1.5253(18) C8 C9 1.382(2) C9 C10 1.384(2) C10 C11 1.3960(19) C11 C12 1.5256(19) C12 C13 1.532(2) C12 C14 1.540(2) C15 C17 1.5361(19) C15 C16 1.536(2) C18 C23 1.4061(19) C18 C19 1.4086(18) C19 C20 1.3954(19) C19 C27 1.5247(19) C20 C21 1.384(2) C21 C22 1.381(2) C22 C23 1.3997(18) C23 C24 1.5235(18) C24 C25 1.530(2) C24 C26 1.534(2) C27 C28 1.531(2) C27 C29 1.537(2) C30 C32 1.512(2) C30 C33 1.516(2) C30 C31 1.521(2) C34 C35 1.518(2) C34 C37 1.520(2) C34 C36 1.522(2) C38 C39 1.398(3) C38 C42 1.410(2) C39 C40 1.413(3) C40 C41 1.398(3) C41 C42 1.398(2) C43 C47 1.389(5) C43 C44 1.416(5) C44 C45 1.419(5) C45 C46 1.401(4) C46 C47 1.412(5) C43A C47A 1.386(7) C43A C44A 1.416(7) C44A C45A 1.423(7) C45A C46A 1.403(6) C46A C47A 1.406(7) C48 C49 1.399(2) C48 C52 1.409(3) C49 C50 1.415(3) C50 C51 1.398(3) C51 C52 1.398(3) C53 C59 1.275(18) C53 C58 1.378(10) C53 C54 1.392(11) C54 C55 1.389(10) C55 C56 1.393(10) C56 C57 1.384(10) C57 C58 1.404(10) C53A C59A 1.280(19) C53A C58A 1.379(13) C53A C54A 1.390(14) C54A C55A 1.390(13) C55A C56A 1.396(13) C56A C57A 1.385(13) C57A C58A 1.408(13) 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 O2 H2 O5 0.832(9) 1.882(11) 2.6723(13) 158.2(17)