#------------------------------------------------------------------------------ #$Date: 2017-04-22 05:10:45 +0300 (Sat, 22 Apr 2017) $ #$Revision: 195683 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042758.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_7042758 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 Nd O5 Si, 0.5 (C7 H8)' _chemical_formula_sum 'C55.5 H80 Al N2 Nd O5 Si' _chemical_formula_weight 1054.52 _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 67.054(1) _cell_angle_beta 77.662(1) _cell_angle_gamma 63.143(1) _cell_formula_units_Z 2 _cell_length_a 14.3004(6) _cell_length_b 14.3557(6) _cell_length_c 16.0951(6) _cell_measurement_reflns_used 9706 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.04 _cell_measurement_theta_min 2.62 _cell_volume 2711.71(19) _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 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_unetI/netI 0.0117 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 70954 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.038 _diffrn_reflns_theta_max 25.038 _diffrn_reflns_theta_min 1.689 _diffrn_source 'Fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.7022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2008/1' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.291 _exptl_crystal_description prism _exptl_crystal_F_000 1108 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.434 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 710 _refine_ls_number_reflns 9578 _refine_ls_number_restraints 432 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0171 _refine_ls_R_factor_gt 0.0164 _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^)+(0.0180P)^2^+1.6183P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0414 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9289 _reflns_number_total 9578 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00874k2.cif _cod_data_source_block Comp3 _cod_original_formula_sum 'C55.50 H80 Al N2 Nd O5 Si' _cod_database_code 7042758 _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 0.803 _shelx_estimated_absorpt_t_max 0.876 _shelx_res_file ; mo_025jav09_0m.res created by SHELXL-2014/7 TITL mo_025JAV09_0m in P-1 CELL 0.71073 14.3004 14.3557 16.0951 67.054 77.662 63.143 ZERR 2.00 0.0006 0.0006 0.0006 0.001 0.001 0.001 LATT 1 SFAC C H N O AL SI ND UNIT 111 160 4 10 2 2 2 LIST 4 TEMP -173 L.S. 15 BOND FMAP 2 PLAN 20 size 0.130 0.134 0.220 acta bind h2 o2 bind h5 o5 dfix 0.84 0.01 o2 h2 o5 h5 omit 1 0 0 omit 3 -1 4 omit -4 -2 2 htab o2 o5 WGHT 0.018000 1.618300 FVAR 0.11771 0.76550 ND1 7 0.566857 0.698197 0.124063 11.00000 0.01641 0.01378 = 0.01711 -0.00651 -0.00264 -0.00470 SI1 6 0.764911 0.393754 0.255902 11.00000 0.01424 0.01375 = 0.01393 -0.00442 -0.00257 -0.00641 AL1 5 0.707638 0.228656 0.225057 11.00000 0.01197 0.01217 = 0.01256 -0.00484 -0.00055 -0.00513 O1 4 0.762283 0.275585 0.277447 11.00000 0.01450 0.01438 = 0.01499 -0.00465 -0.00301 -0.00579 O2 4 0.662319 0.490839 0.193625 11.00000 0.01633 0.01475 = 0.01872 -0.00630 -0.00428 -0.00659 H2 2 0.642909 0.459669 0.171951 11.00000 -1.50000 O3 4 0.759206 0.423023 0.344570 11.00000 0.02698 0.02052 = 0.01577 -0.00677 -0.00189 -0.01329 O4 4 0.865384 0.409077 0.193157 11.00000 0.01475 0.02005 = 0.02001 -0.00490 -0.00276 -0.00881 O5 4 0.631078 0.349013 0.144918 11.00000 0.01694 0.01562 = 0.01549 -0.00461 -0.00517 -0.00630 H5 2 0.595319 0.351443 0.110853 11.00000 -1.50000 N1 3 0.625890 0.150919 0.298017 11.00000 0.01447 0.01460 = 0.01354 -0.00509 -0.00016 -0.00658 N2 3 0.805751 0.118020 0.177862 11.00000 0.01296 0.01526 = 0.01561 -0.00641 -0.00022 -0.00518 C1 1 0.528509 0.040826 0.310349 11.00000 0.02478 0.02444 = 0.02585 -0.01176 0.00466 -0.01640 AFIX 137 H1A 2 0.517801 0.031154 0.374884 11.00000 -1.50000 H1B 2 0.547227 -0.029916 0.302401 11.00000 -1.50000 H1C 2 0.463731 0.096415 0.279563 11.00000 -1.50000 AFIX 0 C2 1 0.615803 0.078997 0.270677 11.00000 0.01710 0.01419 = 0.01661 -0.00285 -0.00351 -0.00704 C3 1 0.684056 0.034842 0.206130 11.00000 0.01999 0.01466 = 0.01821 -0.00645 -0.00279 -0.00776 AFIX 43 H3 2 0.664913 -0.008161 0.186254 11.00000 -1.20000 AFIX 0 C4 1 0.776919 0.046480 0.167486 11.00000 0.01709 0.01365 = 0.01612 -0.00483 -0.00375 -0.00384 C5 1 0.847222 -0.027598 0.113649 11.00000 0.02227 0.02495 = 0.03164 -0.01866 0.00405 -0.00922 AFIX 137 H5A 2 0.810474 -0.066615 0.105460 11.00000 -1.50000 H5B 2 0.911314 -0.081772 0.146018 11.00000 -1.50000 H5C 2 0.865579 0.017437 0.054474 11.00000 -1.50000 AFIX 0 C6 1 0.560636 0.180416 0.374285 11.00000 0.01870 0.01692 = 0.01536 -0.00679 0.00297 -0.01210 C7 1 0.458811 0.264249 0.361508 11.00000 0.01765 0.01947 = 0.01789 -0.00780 0.00177 -0.01182 C8 1 0.401841 0.294101 0.436194 11.00000 0.01840 0.02394 = 0.02435 -0.01288 0.00340 -0.01049 AFIX 43 H8 2 0.333327 0.352062 0.428724 11.00000 -1.20000 AFIX 0 C9 1 0.443435 0.240851 0.520382 11.00000 0.02791 0.02998 = 0.01903 -0.01435 0.00723 -0.01809 AFIX 43 H9 2 0.403222 0.261535 0.570450 11.00000 -1.20000 AFIX 0 C10 1 0.543573 0.157403 0.532051 11.00000 0.02922 0.02531 = 0.01432 -0.00534 -0.00013 -0.01866 AFIX 43 H10 2 0.571388 0.121526 0.590386 11.00000 -1.20000 AFIX 0 C11 1 0.604695 0.124675 0.460165 11.00000 0.02058 0.01773 = 0.01799 -0.00498 -0.00011 -0.01276 C12 1 0.714651 0.031686 0.474800 11.00000 0.02372 0.02276 = 0.01716 -0.00235 -0.00241 -0.01061 AFIX 13 H12 2 0.762112 0.056497 0.424600 11.00000 -1.20000 AFIX 0 C13 1 0.759126 0.004706 0.564099 11.00000 0.03142 0.03335 = 0.02245 -0.00148 -0.00962 -0.01227 AFIX 137 H13A 2 0.721324 -0.031547 0.614604 11.00000 -1.50000 H13B 2 0.750659 0.073429 0.570218 11.00000 -1.50000 H13C 2 0.833800 -0.044995 0.564509 11.00000 -1.50000 AFIX 0 C14 1 0.719624 -0.076085 0.471689 11.00000 0.03684 0.01937 = 0.02758 -0.00421 -0.00731 -0.00575 AFIX 137 H14A 2 0.668008 -0.098048 0.515823 11.00000 -1.50000 H14B 2 0.790080 -0.134847 0.486220 11.00000 -1.50000 H14C 2 0.703954 -0.064100 0.411039 11.00000 -1.50000 AFIX 0 C15 1 0.405915 0.324175 0.271351 11.00000 0.01466 0.02385 = 0.01906 -0.00988 0.00089 -0.00683 AFIX 13 H15 2 0.453901 0.289220 0.226639 11.00000 -1.20000 AFIX 0 C16 1 0.385825 0.446898 0.235724 11.00000 0.02190 0.02286 = 0.02561 -0.00693 -0.00068 -0.00413 AFIX 137 H16A 2 0.452278 0.453708 0.229953 11.00000 -1.50000 H16B 2 0.337322 0.483112 0.277903 11.00000 -1.50000 H16C 2 0.355006 0.482485 0.176494 11.00000 -1.50000 AFIX 0 C17 1 0.301882 0.313646 0.279250 11.00000 0.01753 0.04248 = 0.02531 -0.01585 0.00083 -0.01298 AFIX 137 H17A 2 0.252522 0.350654 0.320638 11.00000 -1.50000 H17B 2 0.314564 0.235067 0.302564 11.00000 -1.50000 H17C 2 0.272189 0.348501 0.219589 11.00000 -1.50000 AFIX 0 C18 1 0.913154 0.106437 0.150630 11.00000 0.01370 0.01715 = 0.01999 -0.01061 0.00123 -0.00553 C19 1 0.992995 0.022645 0.209382 11.00000 0.01787 0.01797 = 0.02245 -0.00805 -0.00106 -0.00593 C20 1 1.096161 0.010700 0.182828 11.00000 0.01561 0.02099 = 0.03074 -0.00878 -0.00405 -0.00228 AFIX 43 H20 2 1.151377 -0.045852 0.221215 11.00000 -1.20000 AFIX 0 C21 1 1.119033 0.080127 0.101361 11.00000 0.01367 0.02648 = 0.03223 -0.01385 0.00389 -0.00790 AFIX 43 H21 2 1.189653 0.070987 0.084264 11.00000 -1.20000 AFIX 0 C22 1 1.039730 0.162665 0.044750 11.00000 0.02008 0.02222 = 0.02158 -0.00975 0.00457 -0.00980 AFIX 43 H22 2 1.056530 0.210254 -0.010716 11.00000 -1.20000 AFIX 0 C23 1 0.935156 0.177521 0.067526 11.00000 0.01730 0.01770 = 0.01902 -0.01004 0.00112 -0.00581 C24 1 0.851709 0.267152 0.000698 11.00000 0.01847 0.02311 = 0.01727 -0.00609 0.00024 -0.00711 AFIX 13 H24 2 0.782018 0.266876 0.027803 11.00000 -1.20000 AFIX 0 C25 1 0.847189 0.382042 -0.018312 11.00000 0.03428 0.02170 = 0.02482 -0.00416 -0.00689 -0.00662 AFIX 137 H25A 2 0.832473 0.397536 0.038385 11.00000 -1.50000 H25B 2 0.791497 0.438026 -0.060025 11.00000 -1.50000 H25C 2 0.914697 0.384219 -0.045482 11.00000 -1.50000 AFIX 0 C26 1 0.871465 0.244142 -0.088274 11.00000 0.03087 0.03428 = 0.02335 -0.01150 -0.00460 -0.00979 AFIX 137 H26A 2 0.872202 0.171422 -0.076194 11.00000 -1.50000 H26B 2 0.939268 0.244714 -0.116209 11.00000 -1.50000 H26C 2 0.815549 0.301583 -0.129281 11.00000 -1.50000 AFIX 0 C27 1 0.971612 -0.053505 0.301424 11.00000 0.02031 0.02154 = 0.02403 -0.00356 -0.00495 -0.00709 AFIX 13 H27 2 0.897276 -0.043729 0.304582 11.00000 -1.20000 AFIX 0 C28 1 0.983922 -0.020307 0.376845 11.00000 0.02349 0.02716 = 0.02487 -0.00658 -0.00311 -0.00789 AFIX 137 H28A 2 0.968487 -0.068598 0.435547 11.00000 -1.50000 H28B 2 0.935110 0.056910 0.368802 11.00000 -1.50000 H28C 2 1.056040 -0.028011 0.374402 11.00000 -1.50000 AFIX 0 C29 1 1.043084 -0.176132 0.315617 11.00000 0.04700 0.02099 = 0.03042 -0.00421 -0.00665 -0.01069 AFIX 137 H29A 2 1.023960 -0.222260 0.373775 11.00000 -1.50000 H29B 2 1.116324 -0.188311 0.315272 11.00000 -1.50000 H29C 2 1.034596 -0.196114 0.266865 11.00000 -1.50000 AFIX 0 C30 1 0.724265 0.383743 0.437797 11.00000 0.03781 0.02298 = 0.01270 -0.00579 -0.00338 -0.01391 C31 1 0.729438 0.457457 0.481897 11.00000 0.06363 0.03977 = 0.02346 -0.01604 -0.00223 -0.02798 AFIX 137 H31A 2 0.708671 0.433420 0.546171 11.00000 -1.50000 H31B 2 0.681694 0.534499 0.452600 11.00000 -1.50000 H31C 2 0.801285 0.452002 0.475368 11.00000 -1.50000 AFIX 0 C32 1 0.613405 0.394166 0.442900 11.00000 0.04385 0.04800 = 0.02875 -0.02063 0.01183 -0.02826 AFIX 137 H32A 2 0.590619 0.367208 0.506271 11.00000 -1.50000 H32B 2 0.611036 0.349940 0.410538 11.00000 -1.50000 H32C 2 0.566642 0.472114 0.415202 11.00000 -1.50000 AFIX 0 C33 1 0.799193 0.264371 0.480916 11.00000 0.07040 0.02711 = 0.02331 -0.00163 -0.01846 -0.00988 AFIX 137 H33A 2 0.778523 0.237922 0.544971 11.00000 -1.50000 H33B 2 0.870640 0.259775 0.475210 11.00000 -1.50000 H33C 2 0.796858 0.218244 0.450443 11.00000 -1.50000 AFIX 0 C34 1 0.974893 0.364975 0.213384 11.00000 0.01363 0.02587 = 0.03052 -0.00935 -0.00307 -0.00841 C35 1 1.012709 0.242753 0.268967 11.00000 0.01943 0.02746 = 0.03791 -0.00491 -0.00715 -0.00576 AFIX 137 H35A 2 0.974712 0.233605 0.327944 11.00000 -1.50000 H35B 2 1.088049 0.211832 0.277525 11.00000 -1.50000 H35C 2 0.999821 0.203788 0.237375 11.00000 -1.50000 AFIX 0 C36 1 1.034753 0.381438 0.122385 11.00000 0.01939 0.03506 = 0.03709 -0.01232 0.00327 -0.01437 AFIX 137 H36A 2 1.109179 0.355684 0.131567 11.00000 -1.50000 H36B 2 1.006508 0.460313 0.085818 11.00000 -1.50000 H36C 2 1.027161 0.338929 0.091106 11.00000 -1.50000 AFIX 0 C37 1 0.986303 0.429925 0.262927 11.00000 0.02073 0.04369 = 0.04780 -0.02314 -0.00441 -0.01440 AFIX 137 H37A 2 1.059977 0.400110 0.276665 11.00000 -1.50000 H37B 2 0.943062 0.423466 0.319289 11.00000 -1.50000 H37C 2 0.963236 0.508127 0.224808 11.00000 -1.50000 AFIX 0 C38 1 0.521786 0.788766 -0.056739 11.00000 0.05350 0.02360 = 0.01731 0.00112 -0.01233 -0.01527 AFIX 43 H38 2 0.520661 0.860945 -0.085585 11.00000 -1.20000 AFIX 0 C39 1 0.435998 0.764212 -0.012924 11.00000 0.03839 0.04086 = 0.02620 -0.00330 -0.01920 -0.01216 AFIX 43 H39 2 0.366342 0.816415 -0.007195 11.00000 -1.20000 AFIX 0 C40 1 0.471791 0.647616 0.021274 11.00000 0.05487 0.04670 = 0.02163 -0.00420 -0.01406 -0.03394 AFIX 43 H40 2 0.430625 0.607260 0.054881 11.00000 -1.20000 AFIX 0 C41 1 0.578364 0.602209 -0.003066 11.00000 0.06467 0.02579 = 0.01685 -0.00726 -0.00921 -0.01829 AFIX 43 H41 2 0.622080 0.525367 0.010624 11.00000 -1.20000 AFIX 0 C42 1 0.609970 0.688565 -0.050876 11.00000 0.04644 0.03560 = 0.01589 -0.00942 0.00149 -0.01733 AFIX 43 H42 2 0.678701 0.680982 -0.075091 11.00000 -1.20000 AFIX 0 C43 1 0.434174 0.824604 0.230212 11.00000 0.05632 0.04209 = 0.05644 -0.03873 0.02033 -0.01610 AFIX 43 H43 2 0.448935 0.884285 0.226713 11.00000 -1.20000 AFIX 0 C44 1 0.475532 0.715782 0.291495 11.00000 0.05252 0.05051 = 0.02735 -0.02559 0.00892 -0.02603 AFIX 43 H44 2 0.523981 0.688322 0.336384 11.00000 -1.20000 AFIX 0 C45 1 0.432312 0.655302 0.274308 11.00000 0.03219 0.04783 = 0.02736 -0.02162 0.01164 -0.02014 AFIX 43 H45 2 0.445996 0.579415 0.306110 11.00000 -1.20000 AFIX 0 C46 1 0.365899 0.724940 0.202802 11.00000 0.01827 0.06449 = 0.04710 -0.02923 0.00782 -0.01260 AFIX 43 H46 2 0.326511 0.705200 0.177169 11.00000 -1.20000 AFIX 0 C47 1 0.367773 0.829146 0.175644 11.00000 0.02908 0.04321 = 0.05872 -0.02298 0.00661 0.00934 AFIX 43 H47 2 0.329916 0.892657 0.127776 11.00000 -1.20000 AFIX 0 C48 1 0.747558 0.680871 0.178818 11.00000 0.03218 0.02714 = 0.04933 -0.00552 -0.01527 -0.01710 AFIX 43 H48 2 0.777925 0.618333 0.230291 11.00000 -1.20000 AFIX 0 C49 1 0.673096 0.785177 0.179670 11.00000 0.04523 0.02797 = 0.04716 -0.01214 -0.01456 -0.01972 AFIX 43 H49 2 0.644505 0.806328 0.231775 11.00000 -1.20000 AFIX 0 C50 1 0.647572 0.853983 0.089413 11.00000 0.04680 0.01994 = 0.05661 -0.00179 -0.02049 -0.01923 AFIX 43 H50 2 0.597892 0.928960 0.070075 11.00000 -1.20000 AFIX 0 C51 1 0.708938 0.791320 0.033864 11.00000 0.04724 0.04367 = 0.04088 -0.00348 -0.00088 -0.03578 AFIX 43 H51 2 0.709114 0.817179 -0.030208 11.00000 -1.20000 AFIX 0 C52 1 0.769894 0.684446 0.088233 11.00000 0.02422 0.03660 = 0.05816 -0.01461 0.00402 -0.02020 AFIX 43 H52 2 0.817814 0.624845 0.067840 11.00000 -1.20000 AFIX 0 part -1 same c54 > c58 c53 same c53 c58 < c54 c59 simu 0.01 c53 > c59a rigu 0.005 c53 > c59a isor 0.02 c53 > c59a C53 1 0.058472 0.395333 0.582919 20.50000 0.04707 0.06777 = 0.07180 -0.03512 0.00661 -0.04017 C54 1 0.101427 0.408459 0.496000 20.50000 0.03779 0.06127 = 0.06394 -0.03345 0.00954 -0.03026 AFIX 43 H54 2 0.168737 0.354982 0.486217 20.50000 -1.20000 AFIX 0 C55 1 0.049763 0.496727 0.422881 20.50000 0.04876 0.05908 = 0.05309 -0.04114 0.01481 -0.03227 AFIX 43 H55 2 0.080698 0.502035 0.363703 20.50000 -1.20000 AFIX 0 C56 1 -0.047832 0.578355 0.435432 20.50000 0.04650 0.05735 = 0.06027 -0.03533 0.00224 -0.03210 AFIX 43 H56 2 -0.084843 0.638917 0.385532 20.50000 -1.20000 AFIX 0 C57 1 -0.089260 0.568033 0.523791 20.50000 0.03711 0.05915 = 0.06043 -0.04123 0.01469 -0.02469 AFIX 43 H57 2 -0.153505 0.624541 0.534784 20.50000 -1.20000 AFIX 0 C58 1 -0.037059 0.475411 0.596035 20.50000 0.04653 0.06558 = 0.05690 -0.03636 0.00979 -0.03481 AFIX 43 H58 2 -0.068242 0.467691 0.655339 20.50000 -1.20000 AFIX 0 C59 1 0.115738 0.312878 0.649986 20.50000 0.07006 0.07746 = 0.09166 -0.03541 -0.01804 -0.03898 AFIX 137 H59A 2 0.139448 0.242823 0.639136 20.50000 -1.50000 H59B 2 0.073478 0.309867 0.706821 20.50000 -1.50000 H59C 2 0.176800 0.324730 0.653790 20.50000 -1.50000 AFIX 0 part -2 same 0.01 0.01 c53 > c59 C53A 1 0.035263 0.472656 0.518065 -20.50000 0.04621 0.05964 = 0.05955 -0.04001 0.00896 -0.03334 C54A 1 0.075185 0.495450 0.430095 -20.50000 0.04497 0.05956 = 0.05824 -0.03757 0.00904 -0.02938 AFIX 43 H54A 2 0.146031 0.450960 0.417696 -20.50000 -1.20000 AFIX 0 C55A 1 0.015635 0.580753 0.359460 -20.50000 0.05149 0.05803 = 0.06122 -0.03552 0.00529 -0.03125 AFIX 43 H55A 2 0.046301 0.595255 0.299874 -20.50000 -1.20000 AFIX 0 C56A 1 -0.089505 0.645886 0.375132 -20.50000 0.05104 0.05656 = 0.06140 -0.03103 0.00047 -0.03100 AFIX 43 H56A 2 -0.134064 0.698516 0.326704 -20.50000 -1.20000 AFIX 0 C57A 1 -0.126349 0.630325 0.465088 -20.50000 0.04498 0.06060 = 0.06401 -0.03537 0.00789 -0.03184 AFIX 43 H57A 2 -0.192390 0.682336 0.479009 -20.50000 -1.20000 AFIX 0 C58A 1 -0.066881 0.538831 0.534895 -20.50000 0.04621 0.06295 = 0.06094 -0.03500 0.00983 -0.02769 AFIX 43 H58A 2 -0.097418 0.522351 0.594425 -20.50000 -1.20000 AFIX 0 C59A 1 0.095670 0.384736 0.580871 -20.50000 0.05385 0.06781 = 0.07022 -0.03701 0.00482 -0.04008 AFIX 137 H59D 2 0.126662 0.320601 0.560282 -20.50000 -1.50000 H59E 2 0.053370 0.369132 0.636867 -20.50000 -1.50000 H59F 2 0.151674 0.399425 0.591935 -20.50000 -1.50000 AFIX 0 HKLF 4 REM mo_025JAV09_0m in P-1 REM R1 = 0.0164 for 9289 Fo > 4sig(Fo) and 0.0171 for all 9578 data REM 710 parameters refined using 432 restraints END WGHT 0.0180 1.6183 REM Highest difference peak 0.434, deepest hole -0.393, 1-sigma level 0.042 Q1 1 0.5597 0.7741 0.1110 11.00000 0.05 0.43 Q2 1 0.5764 0.6201 0.1337 11.00000 0.05 0.41 Q3 1 0.5489 0.7419 0.0733 11.00000 0.05 0.41 Q4 1 0.7625 0.3279 0.2669 11.00000 0.05 0.36 Q5 1 0.4359 0.2920 0.3158 11.00000 0.05 0.31 Q6 1 0.8958 0.2187 0.0363 11.00000 0.05 0.31 Q7 1 0.6601 0.0787 0.4686 11.00000 0.05 0.29 Q8 1 0.8627 0.2516 -0.0385 11.00000 0.05 0.29 Q9 1 0.8591 0.1161 0.1624 11.00000 0.05 0.29 Q10 1 0.5836 0.1524 0.4197 11.00000 0.05 0.29 Q11 1 1.0398 0.0279 0.2011 11.00000 0.05 0.29 Q12 1 0.5751 0.0574 0.2888 11.00000 0.05 0.28 Q13 1 0.9851 -0.0087 0.2575 11.00000 0.05 0.28 Q14 1 0.6583 0.0550 0.2374 11.00000 0.05 0.28 Q15 1 0.7219 0.4213 0.4589 11.00000 0.05 0.27 Q16 1 0.9212 0.1575 0.1161 11.00000 0.05 0.27 Q17 1 0.7184 -0.0176 0.4697 11.00000 0.05 0.27 Q18 1 0.5186 0.2364 0.3623 11.00000 0.05 0.27 Q19 1 0.3968 0.3815 0.2512 11.00000 0.05 0.26 Q20 1 0.5955 0.1612 0.3358 11.00000 0.05 0.26 ; _shelx_res_checksum 19351 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 Nd1 Nd 0.56686(2) 0.69820(2) 0.12406(2) 0.01560(3) Uani 1 1 d . . . . . Si1 Si 0.76491(3) 0.39375(3) 0.25590(3) 0.01345(8) Uani 1 1 d . . . . . Al1 Al 0.70764(3) 0.22866(3) 0.22506(3) 0.01193(8) Uani 1 1 d . . . . . O1 O 0.76228(7) 0.27559(8) 0.27745(6) 0.0144(2) Uani 1 1 d . . . . . O2 O 0.66232(8) 0.49084(8) 0.19363(7) 0.0157(2) Uani 1 1 d D . . . . H2 H 0.6429(13) 0.4597(13) 0.1720(11) 0.024 Uiso 1 1 d D U . . . O3 O 0.75921(8) 0.42302(8) 0.34457(7) 0.0193(2) Uani 1 1 d . . . . . O4 O 0.86538(8) 0.40908(8) 0.19316(7) 0.0179(2) Uani 1 1 d . . . . . O5 O 0.63108(8) 0.34901(8) 0.14492(7) 0.0156(2) Uani 1 1 d D . . . . H5 H 0.5953(12) 0.3514(15) 0.1109(10) 0.023 Uiso 1 1 d D U . . . N1 N 0.62589(9) 0.15092(10) 0.29802(8) 0.0139(2) Uani 1 1 d . . . . . N2 N 0.80575(9) 0.11802(10) 0.17786(8) 0.0145(2) Uani 1 1 d . . . . . C1 C 0.52851(12) 0.04083(13) 0.31035(11) 0.0224(3) Uani 1 1 d . . . . . H1A H 0.5178 0.0312 0.3749 0.034 Uiso 1 1 calc R U . . . H1B H 0.5472 -0.0299 0.3024 0.034 Uiso 1 1 calc R U . . . H1C H 0.4637 0.0964 0.2796 0.034 Uiso 1 1 calc R U . . . C2 C 0.61580(11) 0.07900(12) 0.27068(10) 0.0160(3) Uani 1 1 d . . . . . C3 C 0.68406(11) 0.03484(12) 0.20613(10) 0.0167(3) Uani 1 1 d . . . . . H3 H 0.6649 -0.0082 0.1863 0.020 Uiso 1 1 calc R U . . . C4 C 0.77692(11) 0.04648(12) 0.16749(9) 0.0161(3) Uani 1 1 d . . . . . C5 C 0.84722(12) -0.02760(13) 0.11365(11) 0.0243(3) Uani 1 1 d . . . . . H5A H 0.8105 -0.0666 0.1055 0.036 Uiso 1 1 calc R U . . . H5B H 0.9113 -0.0818 0.1460 0.036 Uiso 1 1 calc R U . . . H5C H 0.8656 0.0174 0.0545 0.036 Uiso 1 1 calc R U . . . C6 C 0.56064(11) 0.18042(12) 0.37429(9) 0.0152(3) Uani 1 1 d . . . . . C7 C 0.45881(11) 0.26425(12) 0.36151(10) 0.0166(3) Uani 1 1 d . . . . . C8 C 0.40184(12) 0.29410(13) 0.43619(10) 0.0207(3) Uani 1 1 d . . . . . H8 H 0.3333 0.3521 0.4287 0.025 Uiso 1 1 calc R U . . . C9 C 0.44344(13) 0.24085(13) 0.52038(10) 0.0225(3) Uani 1 1 d . . . . . H9 H 0.4032 0.2615 0.5704 0.027 Uiso 1 1 calc R U . . . C10 C 0.54357(12) 0.15740(13) 0.53205(10) 0.0205(3) Uani 1 1 d . . . . . H10 H 0.5714 0.1215 0.5904 0.025 Uiso 1 1 calc R U . . . C11 C 0.60470(12) 0.12467(12) 0.46016(10) 0.0173(3) Uani 1 1 d . . . . . C12 C 0.71465(12) 0.03169(13) 0.47480(10) 0.0220(3) Uani 1 1 d . . . . . H12 H 0.7621 0.0565 0.4246 0.026 Uiso 1 1 calc R U . . . C13 C 0.75913(14) 0.00471(15) 0.56410(11) 0.0307(4) Uani 1 1 d . . . . . H13A H 0.7213 -0.0315 0.6146 0.046 Uiso 1 1 calc R U . . . H13B H 0.7507 0.0734 0.5702 0.046 Uiso 1 1 calc R U . . . H13C H 0.8338 -0.0450 0.5645 0.046 Uiso 1 1 calc R U . . . C14 C 0.71962(14) -0.07609(13) 0.47169(12) 0.0305(4) Uani 1 1 d . . . . . H14A H 0.6680 -0.0980 0.5158 0.046 Uiso 1 1 calc R U . . . H14B H 0.7901 -0.1348 0.4862 0.046 Uiso 1 1 calc R U . . . H14C H 0.7040 -0.0641 0.4110 0.046 Uiso 1 1 calc R U . . . C15 C 0.40591(11) 0.32417(13) 0.27135(10) 0.0190(3) Uani 1 1 d . . . . . H15 H 0.4539 0.2892 0.2266 0.023 Uiso 1 1 calc R U . . . C16 C 0.38582(13) 0.44690(13) 0.23572(11) 0.0260(3) Uani 1 1 d . . . . . H16A H 0.4523 0.4537 0.2300 0.039 Uiso 1 1 calc R U . . . H16B H 0.3373 0.4831 0.2779 0.039 Uiso 1 1 calc R U . . . H16C H 0.3550 0.4825 0.1765 0.039 Uiso 1 1 calc R U . . . C17 C 0.30188(12) 0.31365(15) 0.27925(11) 0.0270(4) Uani 1 1 d . . . . . H17A H 0.2525 0.3507 0.3206 0.040 Uiso 1 1 calc R U . . . H17B H 0.3146 0.2351 0.3026 0.040 Uiso 1 1 calc R U . . . H17C H 0.2722 0.3485 0.2196 0.040 Uiso 1 1 calc R U . . . C18 C 0.91315(11) 0.10644(12) 0.15063(10) 0.0161(3) Uani 1 1 d . . . . . C19 C 0.99299(12) 0.02264(12) 0.20938(10) 0.0196(3) Uani 1 1 d . . . . . C20 C 1.09616(12) 0.01070(13) 0.18283(11) 0.0240(3) Uani 1 1 d . . . . . H20 H 1.1514 -0.0459 0.2212 0.029 Uiso 1 1 calc R U . . . C21 C 1.11903(12) 0.08013(13) 0.10136(11) 0.0238(3) Uani 1 1 d . . . . . H21 H 1.1897 0.0710 0.0843 0.029 Uiso 1 1 calc R U . . . C22 C 1.03973(12) 0.16266(13) 0.04475(10) 0.0210(3) Uani 1 1 d . . . . . H22 H 1.0565 0.2103 -0.0107 0.025 Uiso 1 1 calc R U . . . C23 C 0.93516(11) 0.17752(12) 0.06753(10) 0.0176(3) Uani 1 1 d . . . . . C24 C 0.85171(12) 0.26715(13) 0.00070(10) 0.0206(3) Uani 1 1 d . . . . . H24 H 0.7820 0.2669 0.0278 0.025 Uiso 1 1 calc R U . . . C25 C 0.84719(14) 0.38204(13) -0.01831(11) 0.0291(4) Uani 1 1 d . . . . . H25A H 0.8325 0.3975 0.0384 0.044 Uiso 1 1 calc R U . . . H25B H 0.7915 0.4380 -0.0600 0.044 Uiso 1 1 calc R U . . . H25C H 0.9147 0.3842 -0.0455 0.044 Uiso 1 1 calc R U . . . C26 C 0.87146(14) 0.24414(15) -0.08827(11) 0.0297(4) Uani 1 1 d . . . . . H26A H 0.8722 0.1714 -0.0762 0.045 Uiso 1 1 calc R U . . . H26B H 0.9393 0.2447 -0.1162 0.045 Uiso 1 1 calc R U . . . H26C H 0.8155 0.3016 -0.1293 0.045 Uiso 1 1 calc R U . . . C27 C 0.97161(12) -0.05350(13) 0.30142(11) 0.0233(3) Uani 1 1 d . . . . . H27 H 0.8973 -0.0437 0.3046 0.028 Uiso 1 1 calc R U . . . C28 C 0.98392(13) -0.02031(14) 0.37685(11) 0.0266(3) Uani 1 1 d . . . . . H28A H 0.9685 -0.0686 0.4355 0.040 Uiso 1 1 calc R U . . . H28B H 0.9351 0.0569 0.3688 0.040 Uiso 1 1 calc R U . . . H28C H 1.0560 -0.0280 0.3744 0.040 Uiso 1 1 calc R U . . . C29 C 1.04308(16) -0.17613(14) 0.31562(12) 0.0347(4) Uani 1 1 d . . . . . H29A H 1.0240 -0.2223 0.3738 0.052 Uiso 1 1 calc R U . . . H29B H 1.1163 -0.1883 0.3153 0.052 Uiso 1 1 calc R U . . . H29C H 1.0346 -0.1961 0.2669 0.052 Uiso 1 1 calc R U . . . C30 C 0.72427(13) 0.38374(13) 0.43780(10) 0.0236(3) Uani 1 1 d . . . . . C31 C 0.72944(17) 0.45746(16) 0.48190(12) 0.0377(4) Uani 1 1 d . . . . . H31A H 0.7087 0.4334 0.5462 0.057 Uiso 1 1 calc R U . . . H31B H 0.6817 0.5345 0.4526 0.057 Uiso 1 1 calc R U . . . H31C H 0.8013 0.4520 0.4754 0.057 Uiso 1 1 calc R U . . . C32 C 0.61341(15) 0.39417(17) 0.44290(12) 0.0362(4) Uani 1 1 d . . . . . H32A H 0.5906 0.3672 0.5063 0.054 Uiso 1 1 calc R U . . . H32B H 0.6110 0.3499 0.4105 0.054 Uiso 1 1 calc R U . . . H32C H 0.5666 0.4721 0.4152 0.054 Uiso 1 1 calc R U . . . C33 C 0.79919(18) 0.26437(15) 0.48092(12) 0.0438(5) Uani 1 1 d . . . . . H33A H 0.7785 0.2379 0.5450 0.066 Uiso 1 1 calc R U . . . H33B H 0.8706 0.2598 0.4752 0.066 Uiso 1 1 calc R U . . . H33C H 0.7969 0.2182 0.4504 0.066 Uiso 1 1 calc R U . . . C34 C 0.97489(12) 0.36498(13) 0.21338(11) 0.0229(3) Uani 1 1 d . . . . . C35 C 1.01271(13) 0.24275(14) 0.26897(12) 0.0308(4) Uani 1 1 d . . . . . H35A H 0.9747 0.2336 0.3279 0.046 Uiso 1 1 calc R U . . . H35B H 1.0880 0.2118 0.2775 0.046 Uiso 1 1 calc R U . . . H35C H 0.9998 0.2038 0.2374 0.046 Uiso 1 1 calc R U . . . C36 C 1.03475(13) 0.38144(15) 0.12239(12) 0.0299(4) Uani 1 1 d . . . . . H36A H 1.1092 0.3557 0.1316 0.045 Uiso 1 1 calc R U . . . H36B H 1.0065 0.4603 0.0858 0.045 Uiso 1 1 calc R U . . . H36C H 1.0272 0.3389 0.0911 0.045 Uiso 1 1 calc R U . . . C37 C 0.98630(13) 0.42992(16) 0.26293(13) 0.0338(4) Uani 1 1 d . . . . . H37A H 1.0600 0.4001 0.2767 0.051 Uiso 1 1 calc R U . . . H37B H 0.9431 0.4235 0.3193 0.051 Uiso 1 1 calc R U . . . H37C H 0.9632 0.5081 0.2248 0.051 Uiso 1 1 calc R U . . . C38 C 0.52179(15) 0.78877(14) -0.05674(11) 0.0325(4) Uani 1 1 d . . . . . H38 H 0.5207 0.8609 -0.0856 0.039 Uiso 1 1 calc R U . . . C39 C 0.43600(15) 0.76421(16) -0.01292(12) 0.0364(4) Uani 1 1 d . . . . . H39 H 0.3663 0.8164 -0.0072 0.044 Uiso 1 1 calc R U . . . C40 C 0.47179(16) 0.64762(16) 0.02127(12) 0.0361(4) Uani 1 1 d . . . . . H40 H 0.4306 0.6073 0.0549 0.043 Uiso 1 1 calc R U . . . C41 C 0.57836(17) 0.60221(15) -0.00307(11) 0.0346(4) Uani 1 1 d . . . . . H41 H 0.6221 0.5254 0.0106 0.041 Uiso 1 1 calc R U . . . C42 C 0.60997(16) 0.68857(15) -0.05088(11) 0.0327(4) Uani 1 1 d . . . . . H42 H 0.6787 0.6810 -0.0751 0.039 Uiso 1 1 calc R U . . . C43 C 0.43417(18) 0.82460(18) 0.23021(15) 0.0498(6) Uani 1 1 d . . . . . H43 H 0.4489 0.8843 0.2267 0.060 Uiso 1 1 calc R U . . . C44 C 0.47553(17) 0.71578(17) 0.29150(13) 0.0391(5) Uani 1 1 d . . . . . H44 H 0.5240 0.6883 0.3364 0.047 Uiso 1 1 calc R U . . . C45 C 0.43231(14) 0.65530(17) 0.27431(12) 0.0335(4) Uani 1 1 d . . . . . H45 H 0.4460 0.5794 0.3061 0.040 Uiso 1 1 calc R U . . . C46 C 0.36590(14) 0.72494(19) 0.20280(14) 0.0431(5) Uani 1 1 d . . . . . H46 H 0.3265 0.7052 0.1772 0.052 Uiso 1 1 calc R U . . . C47 C 0.36777(16) 0.82915(19) 0.17564(16) 0.0529(6) Uani 1 1 d . . . . . H47 H 0.3299 0.8927 0.1278 0.064 Uiso 1 1 calc R U . . . C48 C 0.74756(14) 0.68087(15) 0.17882(14) 0.0344(4) Uani 1 1 d . . . . . H48 H 0.7779 0.6183 0.2303 0.041 Uiso 1 1 calc R U . . . C49 C 0.67310(15) 0.78518(15) 0.17967(14) 0.0362(4) Uani 1 1 d . . . . . H49 H 0.6445 0.8063 0.2318 0.043 Uiso 1 1 calc R U . . . C50 C 0.64757(16) 0.85398(15) 0.08941(14) 0.0395(5) Uani 1 1 d . . . . . H50 H 0.5979 0.9290 0.0701 0.047 Uiso 1 1 calc R U . . . C51 C 0.70894(16) 0.79132(17) 0.03386(14) 0.0408(5) Uani 1 1 d . . . . . H51 H 0.7091 0.8172 -0.0302 0.049 Uiso 1 1 calc R U . . . C52 C 0.76989(14) 0.68445(16) 0.08823(14) 0.0380(4) Uani 1 1 d . . . . . H52 H 0.8178 0.6248 0.0678 0.046 Uiso 1 1 calc R U . . . C53 C 0.0585(12) 0.3953(14) 0.5829(11) 0.053(3) Uani 0.383(4) 1 d D U P A -1 C54 C 0.1014(12) 0.4085(12) 0.4960(9) 0.048(2) Uani 0.383(4) 1 d D U P A -1 H54 H 0.1687 0.3550 0.4862 0.058 Uiso 0.383(4) 1 calc R U P A -1 C55 C 0.0498(11) 0.4967(12) 0.4229(9) 0.045(3) Uani 0.383(4) 1 d D U P A -1 H55 H 0.0807 0.5020 0.3637 0.054 Uiso 0.383(4) 1 calc R U P A -1 C56 C -0.0478(11) 0.5784(11) 0.4354(8) 0.046(2) Uani 0.383(4) 1 d D U P A -1 H56 H -0.0848 0.6389 0.3855 0.055 Uiso 0.383(4) 1 calc R U P A -1 C57 C -0.0893(12) 0.5680(13) 0.5238(9) 0.046(2) Uani 0.383(4) 1 d D U P A -1 H57 H -0.1535 0.6245 0.5348 0.055 Uiso 0.383(4) 1 calc R U P A -1 C58 C -0.0371(11) 0.4754(12) 0.5960(9) 0.048(2) Uani 0.383(4) 1 d D U P A -1 H58 H -0.0682 0.4677 0.6553 0.058 Uiso 0.383(4) 1 calc R U P A -1 C59 C 0.1157(7) 0.3129(8) 0.6500(6) 0.071(2) Uani 0.383(4) 1 d D U P A -1 H59A H 0.1394 0.2428 0.6391 0.107 Uiso 0.383(4) 1 calc R U P A -1 H59B H 0.0735 0.3099 0.7068 0.107 Uiso 0.383(4) 1 calc R U P A -1 H59C H 0.1768 0.3247 0.6538 0.107 Uiso 0.383(4) 1 calc R U P A -1 C53A C 0.0353(12) 0.4727(16) 0.5181(11) 0.046(3) Uani 0.117(4) 1 d D U P A -2 C54A C 0.0752(14) 0.495(3) 0.4301(14) 0.047(4) Uani 0.117(4) 1 d D U P A -2 H54A H 0.1460 0.4510 0.4177 0.056 Uiso 0.117(4) 1 calc R U P A -2 C55A C 0.0156(14) 0.5808(18) 0.3595(11) 0.050(3) Uani 0.117(4) 1 d D U P A -2 H55A H 0.0463 0.5953 0.2999 0.059 Uiso 0.117(4) 1 calc R U P A -2 C56A C -0.0895(17) 0.646(2) 0.3751(13) 0.049(4) Uani 0.117(4) 1 d D U P A -2 H56A H -0.1341 0.6985 0.3267 0.059 Uiso 0.117(4) 1 calc R U P A -2 C57A C -0.1263(13) 0.6303(18) 0.4651(14) 0.049(3) Uani 0.117(4) 1 d D U P A -2 H57A H -0.1924 0.6823 0.4790 0.059 Uiso 0.117(4) 1 calc R U P A -2 C58A C -0.0669(19) 0.539(3) 0.5349(14) 0.052(4) Uani 0.117(4) 1 d D U P A -2 H58A H -0.0974 0.5224 0.5944 0.062 Uiso 0.117(4) 1 calc R U P A -2 C59A C 0.0957(18) 0.385(3) 0.5809(19) 0.055(5) Uani 0.117(4) 1 d D U P A -2 H59D H 0.1267 0.3206 0.5603 0.082 Uiso 0.117(4) 1 calc R U P A -2 H59E H 0.0534 0.3691 0.6369 0.082 Uiso 0.117(4) 1 calc R U P A -2 H59F H 0.1517 0.3994 0.5919 0.082 Uiso 0.117(4) 1 calc R U P A -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 Nd1 0.01641(5) 0.01378(4) 0.01711(5) -0.00651(3) -0.00264(3) -0.00470(3) Si1 0.01424(19) 0.01375(19) 0.01393(18) -0.00442(15) -0.00257(15) -0.00641(15) Al1 0.01197(19) 0.0122(2) 0.01256(19) -0.00484(16) -0.00055(15) -0.00513(16) O1 0.0145(5) 0.0144(5) 0.0150(5) -0.0047(4) -0.0030(4) -0.0058(4) O2 0.0163(5) 0.0148(5) 0.0187(5) -0.0063(4) -0.0043(4) -0.0066(4) O3 0.0270(6) 0.0205(5) 0.0158(5) -0.0068(4) -0.0019(4) -0.0133(5) O4 0.0147(5) 0.0200(5) 0.0200(5) -0.0049(4) -0.0028(4) -0.0088(4) O5 0.0169(5) 0.0156(5) 0.0155(5) -0.0046(4) -0.0052(4) -0.0063(4) N1 0.0145(6) 0.0146(6) 0.0135(6) -0.0051(5) -0.0002(5) -0.0066(5) N2 0.0130(6) 0.0153(6) 0.0156(6) -0.0064(5) -0.0002(5) -0.0052(5) C1 0.0248(8) 0.0244(8) 0.0258(8) -0.0118(7) 0.0047(6) -0.0164(7) C2 0.0171(7) 0.0142(7) 0.0166(7) -0.0029(6) -0.0035(6) -0.0070(6) C3 0.0200(7) 0.0147(7) 0.0182(7) -0.0065(6) -0.0028(6) -0.0078(6) C4 0.0171(7) 0.0136(7) 0.0161(7) -0.0048(6) -0.0037(6) -0.0038(6) C5 0.0223(8) 0.0249(8) 0.0316(9) -0.0187(7) 0.0041(7) -0.0092(7) C6 0.0187(7) 0.0169(7) 0.0154(7) -0.0068(6) 0.0030(6) -0.0121(6) C7 0.0176(7) 0.0195(7) 0.0179(7) -0.0078(6) 0.0018(6) -0.0118(6) C8 0.0184(7) 0.0239(8) 0.0244(8) -0.0129(7) 0.0034(6) -0.0105(6) C9 0.0279(8) 0.0300(9) 0.0190(8) -0.0144(7) 0.0072(6) -0.0181(7) C10 0.0292(8) 0.0253(8) 0.0143(7) -0.0053(6) -0.0001(6) -0.0187(7) C11 0.0206(7) 0.0177(7) 0.0180(7) -0.0050(6) -0.0001(6) -0.0128(6) C12 0.0237(8) 0.0228(8) 0.0172(7) -0.0023(6) -0.0024(6) -0.0106(7) C13 0.0314(9) 0.0333(9) 0.0224(8) -0.0015(7) -0.0096(7) -0.0123(8) C14 0.0368(10) 0.0194(8) 0.0276(9) -0.0042(7) -0.0073(7) -0.0057(7) C15 0.0147(7) 0.0238(8) 0.0191(7) -0.0099(6) 0.0009(6) -0.0068(6) C16 0.0219(8) 0.0229(8) 0.0256(8) -0.0069(7) -0.0007(6) -0.0041(7) C17 0.0175(8) 0.0425(10) 0.0253(8) -0.0158(8) 0.0008(6) -0.0130(7) C18 0.0137(7) 0.0172(7) 0.0200(7) -0.0106(6) 0.0012(6) -0.0055(6) C19 0.0179(7) 0.0180(7) 0.0225(8) -0.0081(6) -0.0011(6) -0.0059(6) C20 0.0156(7) 0.0210(8) 0.0307(9) -0.0088(7) -0.0041(6) -0.0023(6) C21 0.0137(7) 0.0265(8) 0.0322(9) -0.0139(7) 0.0039(6) -0.0079(6) C22 0.0201(8) 0.0222(8) 0.0216(8) -0.0097(6) 0.0046(6) -0.0098(6) C23 0.0173(7) 0.0177(7) 0.0190(7) -0.0100(6) 0.0011(6) -0.0058(6) C24 0.0185(7) 0.0231(8) 0.0173(7) -0.0061(6) 0.0002(6) -0.0071(6) C25 0.0343(9) 0.0217(8) 0.0248(8) -0.0042(7) -0.0069(7) -0.0066(7) C26 0.0309(9) 0.0343(9) 0.0233(8) -0.0115(7) -0.0046(7) -0.0098(8) C27 0.0203(8) 0.0215(8) 0.0240(8) -0.0036(6) -0.0049(6) -0.0071(7) C28 0.0235(8) 0.0272(9) 0.0249(8) -0.0066(7) -0.0031(7) -0.0079(7) C29 0.0470(11) 0.0210(9) 0.0304(9) -0.0042(7) -0.0066(8) -0.0107(8) C30 0.0378(9) 0.0230(8) 0.0127(7) -0.0058(6) -0.0034(6) -0.0139(7) C31 0.0636(13) 0.0398(11) 0.0235(9) -0.0160(8) -0.0022(8) -0.0280(10) C32 0.0439(11) 0.0480(11) 0.0288(9) -0.0206(9) 0.0118(8) -0.0283(9) C33 0.0704(14) 0.0271(10) 0.0233(9) -0.0016(8) -0.0185(9) -0.0099(10) C34 0.0136(7) 0.0259(8) 0.0305(9) -0.0094(7) -0.0031(6) -0.0084(6) C35 0.0194(8) 0.0275(9) 0.0379(10) -0.0049(8) -0.0072(7) -0.0058(7) C36 0.0194(8) 0.0351(10) 0.0371(10) -0.0123(8) 0.0033(7) -0.0144(7) C37 0.0207(8) 0.0437(11) 0.0478(11) -0.0231(9) -0.0044(8) -0.0144(8) C38 0.0535(12) 0.0236(9) 0.0173(8) 0.0011(7) -0.0123(8) -0.0153(8) C39 0.0384(10) 0.0409(11) 0.0262(9) -0.0033(8) -0.0192(8) -0.0122(9) C40 0.0549(12) 0.0467(11) 0.0216(8) -0.0042(8) -0.0141(8) -0.0339(10) C41 0.0647(13) 0.0258(9) 0.0168(8) -0.0073(7) -0.0092(8) -0.0183(9) C42 0.0464(11) 0.0356(10) 0.0159(8) -0.0094(7) 0.0015(7) -0.0173(9) C43 0.0563(14) 0.0421(12) 0.0564(13) -0.0387(11) 0.0203(11) -0.0161(10) C44 0.0525(12) 0.0505(12) 0.0274(9) -0.0256(9) 0.0089(8) -0.0260(10) C45 0.0322(9) 0.0478(11) 0.0274(9) -0.0216(8) 0.0116(7) -0.0201(9) C46 0.0183(9) 0.0645(14) 0.0471(12) -0.0292(11) 0.0078(8) -0.0126(9) C47 0.0291(11) 0.0432(12) 0.0587(14) -0.0230(11) 0.0066(10) 0.0093(9) C48 0.0322(10) 0.0271(9) 0.0493(11) -0.0055(8) -0.0153(8) -0.0171(8) C49 0.0452(11) 0.0280(9) 0.0472(11) -0.0121(8) -0.0146(9) -0.0197(8) C50 0.0468(11) 0.0199(9) 0.0566(12) -0.0018(8) -0.0205(10) -0.0192(8) C51 0.0472(12) 0.0437(11) 0.0409(11) -0.0035(9) -0.0009(9) -0.0358(10) C52 0.0242(9) 0.0366(10) 0.0582(13) -0.0146(9) 0.0040(8) -0.0202(8) C53 0.047(4) 0.068(5) 0.072(5) -0.035(4) 0.007(4) -0.040(4) C54 0.038(4) 0.061(5) 0.064(5) -0.033(4) 0.010(4) -0.030(4) C55 0.049(4) 0.059(5) 0.053(5) -0.041(4) 0.015(4) -0.032(4) C56 0.047(4) 0.057(5) 0.060(5) -0.035(4) 0.002(4) -0.032(4) C57 0.037(4) 0.059(6) 0.060(5) -0.041(4) 0.015(4) -0.025(4) C58 0.047(4) 0.066(6) 0.057(5) -0.036(4) 0.010(4) -0.035(4) C59 0.070(5) 0.077(5) 0.092(5) -0.035(4) -0.018(4) -0.039(4) C53A 0.046(4) 0.060(5) 0.060(5) -0.040(4) 0.009(4) -0.033(4) C54A 0.045(5) 0.060(6) 0.058(5) -0.038(4) 0.009(4) -0.029(5) C55A 0.051(5) 0.058(6) 0.061(6) -0.036(5) 0.005(4) -0.031(5) C56A 0.051(6) 0.057(7) 0.061(6) -0.031(5) 0.000(5) -0.031(5) C57A 0.045(5) 0.061(6) 0.064(6) -0.035(5) 0.008(5) -0.032(5) C58A 0.046(5) 0.063(6) 0.061(6) -0.035(5) 0.010(4) -0.028(5) C59A 0.054(8) 0.068(7) 0.070(7) -0.037(6) 0.005(6) -0.040(7) 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' Nd Nd -0.1943 3.0179 '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 Nd1 C52 81.86(5) O2 Nd1 C38 119.11(4) C52 Nd1 C38 93.60(6) O2 Nd1 C47 126.34(6) C52 Nd1 C47 141.59(7) C38 Nd1 C47 93.08(7) O2 Nd1 C51 110.12(5) C52 Nd1 C51 29.19(6) C38 Nd1 C51 73.82(6) C47 Nd1 C51 120.06(7) O2 Nd1 C50 126.21(5) C52 Nd1 C50 48.34(6) C38 Nd1 C50 87.37(6) C47 Nd1 C50 94.33(7) C51 Nd1 C50 29.17(6) O2 Nd1 C43 120.45(5) C52 Nd1 C43 117.46(7) C38 Nd1 C43 115.21(6) C47 Nd1 C43 28.99(7) C51 Nd1 C43 106.53(7) C50 Nd1 C43 77.40(7) O2 Nd1 C48 78.74(4) C52 Nd1 C48 29.44(6) C38 Nd1 C48 120.96(6) C47 Nd1 C48 122.00(7) C51 Nd1 C48 48.14(6) C50 Nd1 C48 48.27(5) C43 Nd1 C48 93.51(7) O2 Nd1 C44 91.21(5) C52 Nd1 C44 116.00(6) C38 Nd1 C44 140.97(6) C47 Nd1 C44 47.90(7) C51 Nd1 C44 120.71(6) C50 Nd1 C44 93.84(6) C43 Nd1 C44 29.26(6) C48 Nd1 C44 86.70(6) O2 Nd1 C39 113.98(5) C52 Nd1 C39 122.23(6) C38 Nd1 C39 29.11(6) C47 Nd1 C39 73.73(7) C51 Nd1 C39 102.35(6) C50 Nd1 C39 110.02(6) C43 Nd1 C39 101.60(7) C48 Nd1 C39 150.05(6) C44 Nd1 C39 118.53(6) O2 Nd1 C42 92.28(4) C52 Nd1 C42 77.84(6) C38 Nd1 C42 29.25(5) C47 Nd1 C42 120.51(7) C51 Nd1 C42 70.43(6) C50 Nd1 C42 94.94(6) C43 Nd1 C42 144.46(6) C48 Nd1 C42 107.19(6) C44 Nd1 C42 166.09(6) C39 Nd1 C42 48.03(6) O2 Nd1 C49 104.63(4) C52 Nd1 C49 48.13(6) C38 Nd1 C49 116.53(6) C47 Nd1 C49 95.66(7) C51 Nd1 C49 48.01(6) C50 Nd1 C49 29.37(6) C43 Nd1 C49 69.36(7) C48 Nd1 C49 28.94(5) C44 Nd1 C49 73.58(6) C39 Nd1 C49 138.52(6) C42 Nd1 C49 118.38(6) O1 Si1 O3 114.16(5) O1 Si1 O4 114.21(5) O3 Si1 O4 107.55(5) O1 Si1 O2 107.42(5) O3 Si1 O2 108.90(5) O4 Si1 O2 104.03(5) O1 Al1 O5 103.26(5) O1 Al1 N2 114.45(5) O5 Al1 N2 114.30(5) O1 Al1 N1 117.40(5) O5 Al1 N1 110.09(5) N2 Al1 N1 97.82(5) Si1 O1 Al1 133.32(6) H2 O2 Si1 107.4(12) H2 O2 Nd1 109.8(12) Si1 O2 Nd1 141.84(5) C30 O3 Si1 134.06(9) C34 O4 Si1 131.58(9) H5 O5 Al1 124.5(13) C2 N1 C6 119.23(12) C2 N1 Al1 118.70(10) C6 N1 Al1 121.29(9) C4 N2 C18 117.49(12) C4 N2 Al1 119.67(10) C18 N2 Al1 122.84(9) N1 C2 C3 123.12(13) N1 C2 C1 120.25(13) C3 C2 C1 116.62(13) C4 C3 C2 127.66(13) N2 C4 C3 122.94(13) N2 C4 C5 119.99(13) C3 C4 C5 117.05(13) C7 C6 C11 121.67(13) C7 C6 N1 120.40(12) C11 C6 N1 117.89(13) C8 C7 C6 118.02(13) C8 C7 C15 118.03(13) C6 C7 C15 123.94(13) C9 C8 C7 121.15(14) C8 C9 C10 120.09(14) C9 C10 C11 121.51(14) C10 C11 C6 117.54(14) C10 C11 C12 120.60(13) C6 C11 C12 121.87(13) C11 C12 C13 113.37(13) C11 C12 C14 112.43(13) C13 C12 C14 108.01(13) C7 C15 C16 111.21(12) C7 C15 C17 111.36(12) C16 C15 C17 109.40(13) C23 C18 C19 121.64(13) C23 C18 N2 120.18(13) C19 C18 N2 118.18(13) C20 C19 C18 118.19(14) C20 C19 C27 118.73(14) C18 C19 C27 123.06(13) C21 C20 C19 120.84(14) C22 C21 C20 120.31(14) C21 C22 C23 121.23(14) C22 C23 C18 117.77(14) C22 C23 C24 118.78(13) C18 C23 C24 123.42(13) C23 C24 C25 111.40(13) C23 C24 C26 111.11(13) C25 C24 C26 109.56(13) C19 C27 C28 110.13(13) C19 C27 C29 112.15(13) C28 C27 C29 110.36(13) O3 C30 C32 110.17(13) O3 C30 C33 108.63(14) C32 C30 C33 111.23(16) O3 C30 C31 105.42(13) C32 C30 C31 110.86(15) C33 C30 C31 110.35(15) O4 C34 C35 109.77(12) O4 C34 C37 109.49(13) C35 C34 C37 111.22(14) O4 C34 C36 105.66(12) C35 C34 C36 110.43(14) C37 C34 C36 110.12(14) C39 C38 C42 108.41(16) C39 C38 Nd1 76.33(9) C42 C38 Nd1 76.39(9) C38 C39 C40 107.49(17) C38 C39 Nd1 74.56(10) C40 C39 Nd1 76.17(9) C41 C40 C39 107.86(17) C41 C40 Nd1 76.08(10) C39 C40 Nd1 74.63(10) C42 C41 C40 108.58(17) C42 C41 Nd1 74.55(9) C40 C41 Nd1 75.23(10) C41 C42 C38 107.65(17) C41 C42 Nd1 76.68(9) C38 C42 Nd1 74.36(9) C47 C43 C44 107.7(2) C47 C43 Nd1 75.27(11) C44 C43 Nd1 75.56(10) C45 C44 C43 107.50(19) C45 C44 Nd1 76.14(10) C43 C44 Nd1 75.18(10) C46 C45 C44 108.58(19) C46 C45 Nd1 75.53(10) C44 C45 Nd1 74.86(10) C45 C46 C47 107.48(19) C45 C46 Nd1 75.69(10) C47 C46 Nd1 74.50(11) C43 C47 C46 108.8(2) C43 C47 Nd1 75.75(11) C46 C47 Nd1 76.48(11) C49 C48 C52 108.07(17) C49 C48 Nd1 76.22(10) C52 C48 Nd1 74.71(10) C48 C49 C50 108.08(18) C48 C49 Nd1 74.84(10) C50 C49 Nd1 74.57(10) C51 C50 C49 107.42(17) C51 C50 Nd1 75.23(10) C49 C50 Nd1 76.05(10) C52 C51 C50 108.68(18) C52 C51 Nd1 75.08(10) C50 C51 Nd1 75.60(11) C51 C52 C48 107.73(18) C51 C52 Nd1 75.74(10) C48 C52 Nd1 75.85(10) C59 C53 C58 123.1(10) C59 C53 C54 118.4(9) C58 C53 C54 118.1(8) C55 C54 C53 122.1(9) C54 C55 C56 120.3(8) C55 C56 C57 117.8(7) C58 C57 C56 120.5(8) C53 C58 C57 121.1(8) C59A C53A C58A 123.6(12) C59A C53A C54A 118.2(11) C58A C53A C54A 118.1(10) C53A C54A C55A 122.2(11) C54A C55A C56A 120.3(11) C55A C56A C57A 117.1(10) C56A C57A C58A 120.6(11) C53A C58A C57A 120.6(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Nd1 O2 2.5221(10) Nd1 C52 2.7672(17) Nd1 C38 2.7692(16) Nd1 C47 2.7748(18) Nd1 C51 2.7755(18) Nd1 C50 2.7802(17) Nd1 C43 2.7808(18) Nd1 C48 2.7817(17) Nd1 C44 2.7857(17) Nd1 C39 2.7916(16) Nd1 C42 2.7950(16) Nd1 C49 2.7991(17) Si1 O1 1.6102(10) Si1 O3 1.6145(10) Si1 O4 1.6202(10) Si1 O2 1.6707(10) Al1 O1 1.7250(10) Al1 O5 1.7333(10) Al1 N2 1.8815(12) Al1 N1 1.8871(12) O2 H2 0.821(9) O3 C30 1.4469(18) O4 C34 1.4562(17) O5 H5 0.808(9) N1 C2 1.3403(18) N1 C6 1.4545(18) N2 C4 1.3410(19) N2 C18 1.4550(18) C1 C2 1.507(2) C2 C3 1.398(2) C3 C4 1.395(2) C4 C5 1.508(2) C6 C7 1.401(2) C6 C11 1.415(2) C7 C8 1.400(2) C7 C15 1.525(2) C8 C9 1.378(2) C9 C10 1.382(2) C10 C11 1.394(2) C11 C12 1.525(2) C12 C13 1.534(2) C12 C14 1.536(2) C15 C16 1.530(2) C15 C17 1.536(2) C18 C23 1.405(2) C18 C19 1.407(2) C19 C20 1.396(2) C19 C27 1.526(2) C20 C21 1.383(2) C21 C22 1.381(2) C22 C23 1.398(2) C23 C24 1.523(2) C24 C25 1.529(2) C24 C26 1.533(2) C27 C28 1.533(2) C27 C29 1.535(2) C30 C32 1.511(2) C30 C33 1.516(2) C30 C31 1.519(2) C34 C35 1.516(2) C34 C37 1.518(2) C34 C36 1.520(2) C38 C39 1.398(3) C38 C42 1.405(3) C39 C40 1.412(3) C40 C41 1.395(3) C41 C42 1.395(3) C43 C47 1.390(3) C43 C44 1.406(3) C44 C45 1.399(3) C45 C46 1.392(3) C46 C47 1.397(3) C48 C49 1.395(3) C48 C52 1.410(3) C49 C50 1.415(3) C50 C51 1.399(3) C51 C52 1.397(3) C53 C59 1.320(19) C53 C58 1.371(10) C53 C54 1.379(10) C54 C55 1.378(10) C55 C56 1.396(10) C56 C57 1.397(10) C57 C58 1.395(10) C53A C59A 1.32(2) C53A C58A 1.374(13) C53A C54A 1.378(13) C54A C55A 1.380(13) C55A C56A 1.396(13) C56A C57A 1.397(13) C57A C58A 1.400(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 0.821(9) 1.885(10) 2.6787(14) 162.1(18)