#------------------------------------------------------------------------------ #$Date: 2024-10-20 01:10:19 +0300 (Sun, 20 Oct 2024) $ #$Revision: 295550 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572890.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_1572890 loop_ _publ_author_name 'Pedussaut, Lucie' 'Mahieu, Nolwenn' 'Chartier, Camille' 'Rajeshkumar, Thayalan' 'Tricoire, Maxime' 'Douair, Iskander' 'Casaretto, Nicolas' 'Maron, Laurent' 'Danoun, Gr\'egory' 'Nocton, Gr\'egory' _publ_section_title ; The photo-isomerization of the cyclononatetraenyl ligand and related rare earth complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04767B _journal_year 2024 _chemical_formula_moiety 'C17 H17 La' _chemical_formula_sum 'C17 H17 La' _chemical_formula_weight 360.21 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-01-17 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-07-13 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1385(7) _cell_length_b 12.7452(11) _cell_length_c 8.9543(11) _cell_measurement_reflns_used 10162 _cell_measurement_temperature 150 _cell_measurement_theta_max 29.14 _cell_measurement_theta_min 2.78 _cell_volume 1385.3(2) _computing_cell_refinement ; X-Area Recipe 1.37.0.0 (STOE, 2021) ; _computing_data_collection ; X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022) ; _computing_data_reduction ; X-Area Integrate 2.5.3.0 (STOE, 2021) X-Area LANA 2.7.5.0 (STOE, 2022) ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material ; STOE & Cie GmbH, X-Area, software package for collecting single-crystal or multi-domain crystal data on STOE area-detector diffractometers, for image processing, for the correction and scaling of reflection intensities and for outlier rejection, version 2.1, Darmstadt 2022 ; _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150 _diffrn_detector 'EIGER2 1M CDTE' _diffrn_detector_area_resol_mean 13.33 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_details ; 672 frames, detector distance = 60 mm ; _diffrn_measurement_device 'Eulerian 4-circle diffractometer' _diffrn_measurement_device_type 'STOE STADIVARI' _diffrn_measurement_method 'rotation method, \w scans' _diffrn_radiation_collimation '1.2 0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_polarisn_norm 270 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 14590 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.340 _diffrn_reflns_theta_min 2.780 _diffrn_source Axo_Mo _diffrn_source_current 1.00 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 3.062 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.236 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 1840 _refine_ls_number_restraints 124 _refine_ls_restrained_S_all 0.923 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0231 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.0554 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1221 _reflns_number_total 1840 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04767b3.cif _cod_data_source_block 2-La-trans _cod_database_code 1572890 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim C5A-C5A_$1 with sigma of 0.02 C1B-C2B \\sim C2B-C3B \\sim C3B-C4B \\sim C4B-C5B \\sim C5B-C5B_$1 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C1C: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C6B \\sim C7B \\sim C8B \\sim C9B \\sim C10B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A C6A \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A 4. Others 1*[Sof(C1A)+Sof(H1A)]+1*[Sof(C1C)+Sof(H1C)]+1*[Sof(C1B)+Sof(H1B)]=1 with esd of 0.001 1*[Sof(C2A)+Sof(H2A)+Sof(C3A)+Sof(H3A)+Sof(C4A)+Sof(H4A)+Sof(C5A)+Sof(H5A)]+1* [Sof(C2B)+Sof(H2B)+Sof(C3B)+Sof(H3B)+Sof(C4B)+Sof(H4B)+Sof(C5B)+Sof(H5B)]=1 with esd of 0.0001 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=FVAR(1) Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=1-FVAR(2) Sof(C6B)=Sof(H6B)=Sof(C10B)=Sof(H10B)=0.5*(1-FVAR(3)) Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=FVAR(2) Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=FVAR(3) Sof(C1A)=Sof(H1A)=0.5*FVAR(5) Sof(C1C)=Sof(H1C)=0.5*FVAR(6) Sof(C1B)=Sof(H1B)=0.5*FVAR(7) 5.a Aromatic/amide H refined with riding coordinates: C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B) ; _shelx_res_file ; TITL lp175_a.res in Pnma lp175.res created by SHELXL-2018/3 at 16:38:56 on 17-Jan-2024 REM Old TITL LP175 in Pnma #62 REM SHELXT solution in Pnma: R1 0.097, Rweak 0.001, Alpha 0.039 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: La C18 CELL 0.71073 12.1385 12.7452 8.9543 90 90 90 ZERR 4 0.0007 0.0011 0.0011 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H La UNIT 68 68 4 EQIV $1 +X,0.5-Y,+Z SADI C1A C2A C2A C3A C3A C4A C4A C5A C5A C5A_$1 SADI C1B C2B C2B C3B C3B C4B C4B C5B C5B C5B_$1 SIMU 0.004 0.008 2 C1A > C5A C1C SIMU 0.004 0.008 2 C1B > C5B SIMU 0.004 0.008 2 C6B > C10B SIMU 0.004 0.008 2 C6A > C9A SUMP 1 0.001 1 5 1 6 1 7 SUMP 1 0.0001 1 2 1 4 L.S. 20 PLAN 3 TEMP -123.14 CONF CONN 48 $La list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.035700 FVAR 0.32808 0.46278 0.68937 0.53722 0.26165 0.25580 0.48279 LA1 3 0.382583 0.250000 0.503497 10.50000 0.01785 0.02769 = 0.01721 0.00000 -0.00188 0.00000 PART 1 C1A 1 0.141780 0.250000 0.510257 50.50000 0.02338 0.03876 = 0.04641 0.00000 -0.01205 0.00000 AFIX 43 H1A 2 0.091571 0.250000 0.591641 50.50000 -1.20000 AFIX 0 C2A 1 0.167187 0.351045 0.469075 21.00000 0.02784 0.04079 = 0.04869 0.00304 -0.00850 0.00284 AFIX 43 H2A 2 0.121460 0.398426 0.522604 21.00000 -1.20000 AFIX 0 C3A 1 0.237616 0.408158 0.374947 21.00000 0.03235 0.04426 = 0.04644 0.01375 -0.00971 0.00061 AFIX 43 H3A 2 0.231813 0.481318 0.393671 21.00000 -1.20000 AFIX 0 C4A 1 0.311169 0.388701 0.265500 21.00000 0.03432 0.04751 = 0.03500 0.01662 -0.01190 -0.00549 AFIX 43 H4A 2 0.339393 0.452434 0.225965 21.00000 -1.20000 AFIX 0 C5A 1 0.357893 0.302920 0.193435 21.00000 0.03843 0.05237 = 0.02750 0.01768 -0.01523 -0.00732 AFIX 43 H5A 2 0.406722 0.327285 0.118124 21.00000 -1.20000 AFIX 0 PART 2 C1B 1 0.375083 0.250000 0.180132 70.50000 0.02837 0.03558 = 0.01670 0.00000 -0.00743 0.00000 AFIX 43 H1B 2 0.435128 0.250000 0.112085 70.50000 -1.20000 AFIX 0 C2B 1 0.345770 0.353286 0.213352 41.00000 0.03262 0.03673 = 0.02471 0.00361 -0.00916 0.00571 AFIX 43 H2B 2 0.387010 0.401266 0.154475 41.00000 -1.20000 AFIX 0 C3B 1 0.273991 0.406228 0.307257 41.00000 0.03076 0.04150 = 0.02740 0.00387 -0.00430 0.01006 AFIX 43 H3B 2 0.279566 0.479586 0.290036 41.00000 -1.20000 AFIX 0 C4B 1 0.197614 0.387489 0.416795 41.00000 0.03170 0.05426 = 0.03637 0.00756 0.00185 0.01525 AFIX 43 H4B 2 0.170360 0.452270 0.454063 41.00000 -1.20000 AFIX 0 C5B 1 0.146362 0.303987 0.492107 41.00000 0.02678 0.06529 = 0.03999 0.00458 0.00517 0.01210 AFIX 43 H5B 2 0.096617 0.329948 0.565204 41.00000 -1.20000 AFIX 0 PART 3 C1C 1 0.161600 0.250000 0.395524 60.50000 0.02779 0.05136 = 0.05342 0.00000 -0.01707 0.00000 PART 4 C6A 1 0.388349 0.306684 0.792312 31.00000 0.02159 0.03389 = 0.01587 -0.00714 0.00261 0.00147 AFIX 43 H6A 2 0.334756 0.335397 0.857945 31.00000 -1.20000 AFIX 0 C7A 1 0.449241 0.383991 0.717737 31.00000 0.02319 0.02547 = 0.02520 -0.00491 -0.00083 -0.00040 AFIX 43 H7A 2 0.427073 0.453037 0.744092 31.00000 -1.20000 AFIX 0 C8A 1 0.534017 0.383184 0.614798 31.00000 0.02037 0.02656 = 0.02912 0.00314 -0.00171 -0.00732 AFIX 43 H8A 2 0.556107 0.452086 0.587576 31.00000 -1.20000 AFIX 0 C9A 1 0.595497 0.306356 0.540587 31.00000 0.01706 0.03464 = 0.02926 0.00374 0.00017 -0.00827 AFIX 43 H9A 2 0.649385 0.335228 0.475543 31.00000 -1.20000 AFIX 0 PART 5 C6B 1 0.382696 0.250000 0.801623 -30.50000 0.02898 0.02741 = 0.02350 0.00000 0.00565 0.00000 AFIX 43 H6B 2 0.323856 0.250000 0.871578 -30.50000 -1.20000 AFIX 0 C7B 1 0.419286 0.353557 0.758123 -31.00000 0.02850 0.02380 = 0.02646 -0.00309 0.00398 0.00195 AFIX 43 H7B 2 0.380261 0.407593 0.808538 -31.00000 -1.20000 AFIX 0 C8B 1 0.494777 0.391359 0.664077 -31.00000 0.02778 0.02162 = 0.02921 -0.00126 0.00285 -0.00002 AFIX 43 H8B 2 0.495814 0.465879 0.665900 -31.00000 -1.20000 AFIX 0 C9B 1 0.569773 0.353681 0.567481 -31.00000 0.02633 0.02357 = 0.03221 0.00278 -0.00083 -0.00263 AFIX 43 H9B 2 0.609945 0.406972 0.517114 -31.00000 -1.20000 AFIX 0 C10B 1 0.601400 0.250000 0.525103 -30.50000 0.02257 0.02546 = 0.03356 0.00000 -0.00097 0.00000 AFIX 43 H10B 2 0.657060 0.250000 0.450518 -30.50000 -1.20000 AFIX 0 PART 0 H1C 2 0.186844 0.250000 0.277574 60.50000 -1.20000 HKLF 4 REM lp175_a.res in Pnma REM wR2 = 0.0554, GooF = S = 0.918, Restrained GooF = 0.923 for all data REM R1 = 0.0231 for 1221 Fo > 4sig(Fo) and 0.0378 for all 1840 data REM 180 parameters refined using 124 restraints END WGHT 0.0357 0.0000 REM Highest difference peak 1.236, deepest hole -0.407, 1-sigma level 0.100 Q1 1 0.3770 0.2500 0.4073 10.50000 0.05 1.24 Q2 1 0.3808 0.2500 0.6024 10.50000 0.05 1.07 Q3 1 0.3232 0.2500 0.4569 10.50000 0.05 0.97 ; _shelx_res_checksum 7509 _olex2_submission_special_instructions 'No special instructions were received' _stoe_detector_distance '60.0 mm' _stoe_detector_pixelsize_x '0.075 mm' _stoe_detector_pixelsize_y '0.075 mm' _stoe_detector_size_x '8.0 cm' _stoe_detector_size_y '7.7 cm' _stoe_evaluation_integration_a 14.5 _stoe_evaluation_integration_b 0.7 _stoe_evaluation_integration_ems 0.013 _stoe_evaluation_lana_bis_l_even_max - _stoe_evaluation_lana_bis_l_odd_max - _stoe_evaluation_lana_bos_l_even_max 6 _stoe_evaluation_lana_bos_l_odd_max 3 _stoe_evaluation_lana_completeness 92.6 _stoe_evaluation_lana_dxs_max_order 3 _stoe_evaluation_lana_dys_max_order 3 _stoe_evaluation_lana_fs_max_order 3 _stoe_evaluation_lana_max_2theta_available 58.7 _stoe_evaluation_lana_max_2theta_desired 58.7 _stoe_evaluation_lana_mean_redundancy 7.9 _stoe_evaluation_lana_number_refls_after_or 14590 _stoe_evaluation_lana_number_refls_outliers 627 _stoe_evaluation_lana_number_refls_total 15217 _stoe_evaluation_lana_number_refls_unique 1840 _stoe_evaluation_lana_number_refls_written 14590 _stoe_evaluation_lana_or_c1 0.050 _stoe_evaluation_lana_or_c2 0 _stoe_evaluation_lana_or_c3 0 _stoe_evaluation_lana_or_c4 1.0 _stoe_evaluation_lana_point_group mmm _stoe_evaluation_lana_table ; #---------------------------------------------------------------------------- 2Theta 6.8 13.0 19.2 25.4 31.6 37.8 44.0 50.2 56.4 #---------------------------------------------------------------------------- 5.29 3.08 2.15 1.59 1.30 1.09 0.95 0.84 0.77 N(total) 185 654 826 1293 2036 2702 3127 3340 1054 14.3 15.9 9.5 8.9 9.7 9.7 8.6 7.4 3.3 Complet. [%%] 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 68.1 151.4 54.8 56.0 28.8 20.3 11.5 8.2 5.1 2.9 R(int) 0.018 0.023 0.023 0.027 0.026 0.037 0.045 0.065 0.094 #---------------------------------------------------------------------------- ; _stoe_measurement_identifier LP175 _stoe_measurement_max_exposure_per_frame '10.0 s' _stoe_measurement_mean_exposure_per_frame '10.0 s' _stoe_measurement_min_exposure_per_frame '10.0 s' _stoe_measurement_total_exposure_time '112 min' _stoe_measurement_total_frame_number 672 _stoe_measurement_total_run_number 11 _stoe_measurement_tube_power '50.0 W' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.38258(2) 0.250000 0.50350(2) 0.02092(8) Uani 1 2 d S T P . . C1A C 0.1418(17) 0.250000 0.510(3) 0.036(3) Uani 0.262(11) 2 d DS TU P A 1 H1A H 0.091571 0.250000 0.591641 0.043 Uiso 0.262(11) 2 calc R U P A 1 C2A C 0.1672(7) 0.3510(7) 0.4691(10) 0.0391(19) Uani 0.463(3) 1 d D U P A 1 H2A H 0.121460 0.398426 0.522604 0.047 Uiso 0.463(3) 1 calc R U P A 1 C3A C 0.2376(7) 0.4082(7) 0.3749(10) 0.0410(18) Uani 0.463(3) 1 d D U P A 1 H3A H 0.231813 0.481318 0.393671 0.049 Uiso 0.463(3) 1 calc R U P A 1 C4A C 0.3112(7) 0.3887(7) 0.2655(9) 0.0389(18) Uani 0.463(3) 1 d D U P A 1 H4A H 0.339393 0.452434 0.225965 0.047 Uiso 0.463(3) 1 calc R U P A 1 C5A C 0.3579(8) 0.3029(5) 0.1934(9) 0.039(2) Uani 0.463(3) 1 d D U P A 1 H5A H 0.406722 0.327285 0.118124 0.047 Uiso 0.463(3) 1 calc R U P A 1 C1B C 0.3751(10) 0.250000 0.1801(12) 0.027(2) Uani 0.483(11) 2 d DS TU P A 2 H1B H 0.435128 0.250000 0.112085 0.032 Uiso 0.483(11) 2 calc R U P A 2 C2B C 0.3458(6) 0.3533(6) 0.2134(8) 0.0314(15) Uani 0.537(3) 1 d D U P A 2 H2B H 0.387010 0.401266 0.154475 0.038 Uiso 0.537(3) 1 calc R U P A 2 C3B C 0.2740(5) 0.4062(6) 0.3073(7) 0.0332(14) Uani 0.537(3) 1 d D U P A 2 H3B H 0.279566 0.479586 0.290036 0.040 Uiso 0.537(3) 1 calc R U P A 2 C4B C 0.1976(6) 0.3875(7) 0.4168(7) 0.0408(15) Uani 0.537(3) 1 d D U P A 2 H4B H 0.170360 0.452270 0.454063 0.049 Uiso 0.537(3) 1 calc R U P A 2 C5B C 0.1464(6) 0.3040(5) 0.4921(8) 0.0440(16) Uani 0.537(3) 1 d D U P A 2 H5B H 0.096617 0.329948 0.565204 0.053 Uiso 0.537(3) 1 calc R U P A 2 C1C C 0.1616(14) 0.250000 0.396(2) 0.044(3) Uani 0.256(9) 2 d S TU P A 3 C6A C 0.3883(4) 0.3067(4) 0.7923(4) 0.0238(13) Uani 0.689(11) 1 d . U P A 4 H6A H 0.334756 0.335397 0.857945 0.029 Uiso 0.689(11) 1 calc R U P A 4 C7A C 0.4492(4) 0.3840(4) 0.7177(6) 0.0246(13) Uani 0.689(11) 1 d . U P A 4 H7A H 0.427073 0.453037 0.744092 0.030 Uiso 0.689(11) 1 calc R U P A 4 C8A C 0.5340(4) 0.3832(4) 0.6148(5) 0.0253(13) Uani 0.689(11) 1 d . U P A 4 H8A H 0.556107 0.452086 0.587576 0.030 Uiso 0.689(11) 1 calc R U P A 4 C9A C 0.5955(4) 0.3064(5) 0.5406(5) 0.0270(13) Uani 0.689(11) 1 d . U P A 4 H9A H 0.649385 0.335228 0.475543 0.032 Uiso 0.689(11) 1 calc R U P A 4 C6B C 0.3827(16) 0.250000 0.8016(19) 0.027(3) Uani 0.311(11) 2 d S TU P A 5 H6B H 0.323856 0.250000 0.871578 0.032 Uiso 0.311(11) 2 calc R U P A 5 C7B C 0.4193(11) 0.3536(10) 0.7581(13) 0.026(2) Uani 0.311(11) 1 d . U P A 5 H7B H 0.380261 0.407593 0.808538 0.032 Uiso 0.311(11) 1 calc R U P A 5 C8B C 0.4948(10) 0.3914(8) 0.6641(12) 0.026(2) Uani 0.311(11) 1 d . U P A 5 H8B H 0.495814 0.465879 0.665900 0.031 Uiso 0.311(11) 1 calc R U P A 5 C9B C 0.5698(10) 0.3537(10) 0.5675(13) 0.027(2) Uani 0.311(11) 1 d . U P A 5 H9B H 0.609945 0.406972 0.517114 0.033 Uiso 0.311(11) 1 calc R U P A 5 C10B C 0.6014(13) 0.250000 0.5251(17) 0.027(3) Uani 0.311(11) 2 d S TU P A 5 H10B H 0.657060 0.250000 0.450518 0.033 Uiso 0.311(11) 2 calc R U P A 5 H1C H 0.187(10) 0.250000 0.278(13) 0.033 Uiso 0.256(9) 2 d S U P . . 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 La1 0.01785(12) 0.02769(13) 0.01721(11) 0.000 -0.00188(9) 0.000 C1A 0.023(4) 0.039(5) 0.046(5) 0.000 -0.012(4) 0.000 C2A 0.028(3) 0.041(4) 0.049(4) 0.003(2) -0.009(3) 0.003(2) C3A 0.032(4) 0.044(3) 0.046(4) 0.014(3) -0.010(3) 0.001(3) C4A 0.034(4) 0.048(4) 0.035(4) 0.017(3) -0.012(3) -0.005(3) C5A 0.038(4) 0.052(5) 0.028(3) 0.018(4) -0.015(3) -0.007(4) C1B 0.028(4) 0.036(5) 0.017(3) 0.000 -0.007(3) 0.000 C2B 0.033(3) 0.037(3) 0.025(2) 0.004(2) -0.009(2) 0.006(3) C3B 0.031(3) 0.042(3) 0.027(3) 0.004(2) -0.004(2) 0.010(2) C4B 0.032(3) 0.054(3) 0.036(3) 0.008(3) 0.002(2) 0.015(3) C5B 0.027(3) 0.065(4) 0.040(3) 0.005(4) 0.005(3) 0.012(4) C1C 0.028(6) 0.051(6) 0.053(6) 0.000 -0.017(5) 0.000 C6A 0.022(2) 0.034(3) 0.0159(17) -0.007(2) 0.0026(15) 0.001(2) C7A 0.023(2) 0.025(2) 0.025(2) -0.0049(17) -0.0008(19) -0.0004(18) C8A 0.020(2) 0.027(2) 0.029(2) 0.0031(18) -0.0017(19) -0.0073(19) C9A 0.017(2) 0.035(3) 0.029(2) 0.004(2) 0.0002(15) -0.008(2) C6B 0.029(5) 0.027(6) 0.024(5) 0.000 0.006(4) 0.000 C7B 0.029(5) 0.024(5) 0.026(4) -0.003(3) 0.004(3) 0.002(3) C8B 0.028(5) 0.022(4) 0.029(4) -0.001(3) 0.003(3) 0.000(3) C9B 0.026(4) 0.024(5) 0.032(4) 0.003(3) -0.001(3) -0.003(3) C10B 0.023(5) 0.025(6) 0.034(5) 0.000 -0.001(4) 0.000 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' La La -0.2871 2.4523 '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 C1A La1 C2A 27.16(19) . . ? C1A La1 C2A 27.16(19) . 7_565 ? C1A La1 C2B 82.3(4) . 7_565 ? C1A La1 C3B 64.4(3) . 7_565 ? C1A La1 C4B 41.0(2) . 7_565 ? C1A La1 C5B 13.86(15) . 7_565 ? C2A La1 C2A 52.1(3) . 7_565 ? C2A La1 C2B 64.9(2) 7_565 7_565 ? C2A La1 C2B 88.2(2) . 7_565 ? C2A La1 C3B 41.05(17) 7_565 7_565 ? C2A La1 C3B 80.6(2) . 7_565 ? C2A La1 C4B 63.6(2) . 7_565 ? C2A La1 C4B 14.76(14) 7_565 7_565 ? C2A La1 C5B 13.33(15) 7_565 7_565 ? C2A La1 C5B 39.8(2) . 7_565 ? C3A La1 C1A 53.4(3) 7_565 . ? C3A La1 C1A 53.4(3) . . ? C3A La1 C2A 74.0(2) . 7_565 ? C3A La1 C2A 27.80(15) 7_565 7_565 ? C3A La1 C2A 27.80(15) . . ? C3A La1 C2A 74.0(2) 7_565 . ? C3A La1 C3A 87.6(3) . 7_565 ? C3A La1 C2B 41.48(18) 7_565 7_565 ? C3A La1 C2B 82.5(2) . 7_565 ? C3A La1 C3B 14.63(14) 7_565 7_565 ? C3A La1 C3B 87.82(18) . 7_565 ? C3A La1 C4B 13.05(14) 7_565 7_565 ? C3A La1 C4B 81.2(2) . 7_565 ? C3A La1 C5B 40.35(18) 7_565 7_565 ? C3A La1 C5B 63.9(2) . 7_565 ? C4A La1 C1A 73.5(4) . . ? C4A La1 C1A 73.5(4) 7_565 . ? C4A La1 C2A 52.3(2) 7_565 7_565 ? C4A La1 C2A 85.6(2) . 7_565 ? C4A La1 C2A 52.3(2) . . ? C4A La1 C2A 85.6(2) 7_565 . ? C4A La1 C3A 26.83(16) . . ? C4A La1 C3A 26.83(16) 7_565 7_565 ? C4A La1 C3A 87.2(3) . 7_565 ? C4A La1 C3A 87.2(3) 7_565 . ? C4A La1 C4A 75.1(4) 7_565 . ? C4A La1 C2B 15.18(16) 7_565 7_565 ? C4A La1 C2B 65.1(3) . 7_565 ? C4A La1 C3B 80.85(18) . 7_565 ? C4A La1 C3B 12.21(15) 7_565 7_565 ? C4A La1 C4B 38.55(17) 7_565 7_565 ? C4A La1 C4B 86.6(2) . 7_565 ? C4A La1 C5B 80.0(2) . 7_565 ? C4A La1 C5B 62.8(2) 7_565 7_565 ? C5A La1 C1A 85.2(5) 7_565 . ? C5A La1 C1A 85.2(5) . . ? C5A La1 C2A 84.7(2) 7_565 . ? C5A La1 C2A 84.7(2) . 7_565 ? C5A La1 C2A 72.7(2) 7_565 7_565 ? C5A La1 C2A 72.7(2) . . ? C5A La1 C3A 52.6(2) 7_565 7_565 ? C5A La1 C3A 52.6(2) . . ? C5A La1 C3A 73.6(3) 7_565 . ? C5A La1 C3A 73.6(3) . 7_565 ? C5A La1 C4A 27.86(17) 7_565 7_565 ? C5A La1 C4A 53.3(3) . 7_565 ? C5A La1 C4A 53.3(3) 7_565 . ? C5A La1 C4A 27.86(17) . . ? C5A La1 C5A 27.2(3) 7_565 . ? C5A La1 C2B 13.39(15) 7_565 7_565 ? C5A La1 C2B 40.3(2) . 7_565 ? C5A La1 C3B 39.03(17) 7_565 7_565 ? C5A La1 C3B 62.5(2) . 7_565 ? C5A La1 C4B 61.8(2) 7_565 7_565 ? C5A La1 C4B 78.8(2) . 7_565 ? C5A La1 C5B 85.4(2) . 7_565 ? C5A La1 C5B 79.1(2) 7_565 7_565 ? C1B La1 C2B 27.62(15) . . ? C1B La1 C3B 52.67(18) . . ? C1B La1 C4B 73.3(2) . . ? C1B La1 C5B 86.3(3) . . ? C2B La1 C2B 53.1(3) 7_565 . ? C2B La1 C3B 73.1(2) 7_565 . ? C2B La1 C3B 27.12(13) . . ? C2B La1 C4B 52.24(17) . . ? C2B La1 C4B 85.3(2) 7_565 . ? C2B La1 C5B 85.8(2) 7_565 . ? C2B La1 C5B 73.6(2) . . ? C3B La1 C3B 84.4(3) 7_565 . ? C4B La1 C3B 84.5(2) 7_565 . ? C4B La1 C3B 26.79(13) . . ? C5B La1 C3B 72.8(2) 7_565 . ? C5B La1 C3B 52.47(17) . . ? C5B La1 C4B 27.54(16) . . ? C5B La1 C4B 52.4(2) 7_565 . ? C5B La1 C5B 27.0(3) 7_565 . ? C6A La1 C7A 58.5(2) 7_565 . ? C6A La1 C7A 30.20(12) . . ? C6A La1 C8A 78.20(16) 7_565 . ? C6A La1 C8A 57.07(13) . . ? C6A La1 C9A 85.89(13) 7_565 . ? C6A La1 C9A 77.60(13) . . ? C6A La1 C9B 69.0(3) 7_565 7_565 ? C6A La1 C9B 84.6(3) . 7_565 ? C7A La1 C8A 29.73(12) . . ? C7A La1 C8A 86.04(14) 7_565 . ? C7A La1 C9A 78.09(16) 7_565 . ? C7A La1 C9A 57.09(14) . . ? C8A La1 C8A 78.1(2) 7_565 . ? C8A La1 C9A 58.0(2) 7_565 . ? C8A La1 C9A 30.05(13) . . ? C9A La1 C9A 30.8(3) 7_565 . ? C6B La1 C7B 31.4(3) . . ? C6B La1 C8B 57.5(4) . . ? C6B La1 C9B 77.7(4) . . ? C6B La1 C9B 77.7(4) . 7_565 ? C7B La1 C7B 59.2(6) 7_565 . ? C7B La1 C8B 77.8(4) 7_565 . ? C7B La1 C8B 28.9(3) . . ? C7B La1 C9B 85.4(3) 7_565 . ? C7B La1 C9B 55.6(3) 7_565 7_565 ? C7B La1 C9B 85.4(3) . 7_565 ? C7B La1 C9B 55.6(3) . . ? C8B La1 C8B 84.6(4) 7_565 . ? C8B La1 C9B 77.7(4) . 7_565 ? C8B La1 C9B 29.0(3) 7_565 7_565 ? C8B La1 C9B 77.7(4) 7_565 . ? C8B La1 C9B 29.0(3) . . ? C9B La1 C9B 58.8(6) . 7_565 ? C10B La1 C6B 85.8(5) . . ? C10B La1 C7B 76.8(4) . . ? C10B La1 C8B 56.9(3) . . ? C10B La1 C9B 30.9(3) . 7_565 ? C10B La1 C9B 30.9(3) . . ? La1 C1A H1A 131.1 . . ? C2A C1A La1 76.7(10) 7_565 . ? C2A C1A La1 76.7(10) . . ? C2A C1A H1A 110.5 . . ? C2A C1A H1A 110.5 7_565 . ? C2A C1A C2A 139(2) . 7_565 ? La1 C2A H2A 138.4 . . ? C1A C2A La1 76.1(10) . . ? C1A C2A H2A 109.2 . . ? C1A C2A C3A 141.6(13) . . ? C3A C2A La1 75.4(4) . . ? C3A C2A H2A 109.2 . . ? La1 C3A H3A 130.9 . . ? C2A C3A La1 76.8(5) . . ? C2A C3A H3A 111.0 . . ? C4A C3A La1 76.1(5) . . ? C4A C3A C2A 138.1(9) . . ? C4A C3A H3A 111.0 . . ? La1 C4A H4A 133.4 . . ? C3A C4A La1 77.1(4) . . ? C3A C4A H4A 110.6 . . ? C3A C4A C5A 138.7(8) . . ? C5A C4A La1 74.9(4) . . ? C5A C4A H4A 110.6 . . ? La1 C5A H5A 134.2 . . ? C4A C5A La1 77.2(4) . . ? C4A C5A H5A 109.1 . . ? C5A C5A La1 76.42(14) 7_565 . ? C5A C5A C4A 141.8(5) 7_565 . ? C5A C5A H5A 109.1 7_565 . ? La1 C1B H1B 128.1 . . ? C2B C1B La1 78.2(6) 7_565 . ? C2B C1B La1 78.2(6) . . ? C2B C1B H1B 109.4 . . ? C2B C1B H1B 109.4 7_565 . ? C2B C1B C2B 141.2(12) 7_565 . ? La1 C2B H2B 134.2 . . ? C1B C2B La1 74.2(6) . . ? C1B C2B H2B 110.8 . . ? C3B C2B La1 77.2(4) . . ? C3B C2B C1B 138.5(9) . . ? C3B C2B H2B 110.8 . . ? La1 C3B H3B 136.5 . . ? C2B C3B La1 75.7(4) . . ? C2B C3B H3B 109.6 . . ? C4B C3B La1 76.1(4) . . ? C4B C3B C2B 140.8(7) . . ? C4B C3B H3B 109.6 . . ? La1 C4B H4B 133.5 . . ? C3B C4B La1 77.1(4) . . ? C3B C4B H4B 109.6 . . ? C3B C4B C5B 140.8(7) . . ? C5B C4B La1 76.2(4) . . ? C5B C4B H4B 109.6 . . ? La1 C5B H5B 132.5 . . ? C4B C5B La1 76.3(4) . . ? C4B C5B H5B 110.4 . . ? C5B C5B La1 76.51(13) 7_565 . ? C5B C5B C4B 139.2(4) 7_565 . ? C5B C5B H5B 110.4 7_565 . ? La1 C1C H1C 94(7) . . ? La1 C6A H6A 133.0 . . ? C6A C6A La1 74.40(12) 7_565 . ? C6A C6A H6A 112.7 7_565 . ? C7A C6A La1 75.2(2) . . ? C7A C6A H6A 112.7 . . ? La1 C7A H7A 132.8 . . ? C6A C7A La1 74.6(2) . . ? C6A C7A H7A 112.6 . . ? C8A C7A La1 75.2(3) . . ? C8A C7A C6A 134.9(5) . . ? C8A C7A H7A 112.6 . . ? La1 C8A H8A 132.9 . . ? C7A C8A La1 75.1(3) . . ? C7A C8A H8A 112.0 . . ? C7A C8A C9A 136.0(5) . . ? C9A C8A La1 75.4(3) . . ? C9A C8A H8A 112.0 . . ? La1 C9A H9A 133.3 . . ? C8A C9A La1 74.6(2) . . ? C8A C9A H9A 112.8 . . ? C9A C9A La1 74.59(13) 7_565 . ? C9A C9A H9A 112.8 7_565 . ? La1 C6B H6B 131.2 . . ? C7B C6B La1 74.4(8) . . ? C7B C6B La1 74.4(8) 7_565 . ? C7B C6B H6B 114.1 . . ? C7B C6B H6B 114.1 7_565 . ? La1 C7B H7B 132.9 . . ? C6B C7B La1 74.2(8) . . ? C6B C7B H7B 112.4 . . ? C8B C7B La1 75.8(6) . . ? C8B C7B C6B 135.3(13) . . ? C8B C7B H7B 112.4 . . ? La1 C8B H8B 133.5 . . ? C7B C8B La1 75.3(7) . . ? C7B C8B H8B 111.1 . . ? C7B C8B C9B 137.9(12) . . ? C9B C8B La1 76.0(6) . . ? C9B C8B H8B 111.1 . . ? La1 C9B H9B 133.1 . . ? C8B C9B La1 75.0(7) . . ? C8B C9B H9B 113.4 . . ? C8B C9B C10B 133.1(13) . . ? C10B C9B La1 73.5(8) . . ? C10B C9B H9B 113.4 . . ? La1 C10B H10B 131.2 . . ? C9B C10B La1 75.6(8) . . ? C9B C10B La1 75.6(8) 7_565 . ? C9B C10B C9B 135.6(16) . 7_565 ? C9B C10B H10B 112.2 . . ? C9B C10B H10B 112.2 7_565 . ? 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 La1 C1A 2.92(2) . ? La1 C2A 2.931(8) 7_565 ? La1 C2A 2.931(8) . ? La1 C3A 2.913(8) 7_565 ? La1 C3A 2.913(8) . ? La1 C4A 2.901(8) . ? La1 C4A 2.901(8) 7_565 ? La1 C5A 2.873(8) . ? La1 C5A 2.873(8) 7_565 ? La1 C1B 2.897(11) . ? La1 C2B 2.947(7) 7_565 ? La1 C2B 2.947(7) . ? La1 C3B 2.965(7) 7_565 ? La1 C3B 2.965(7) . ? La1 C4B 2.952(7) . ? La1 C4B 2.952(7) 7_565 ? La1 C5B 2.951(7) . ? La1 C5B 2.951(7) 7_565 ? La1 C1C 2.851(16) . ? La1 C6A 2.686(4) 7_565 ? La1 C6A 2.686(4) . ? La1 C7A 2.693(4) 7_565 ? La1 C7A 2.693(4) . ? La1 C8A 2.693(4) 7_565 ? La1 C8A 2.693(4) . ? La1 C9A 2.703(4) . ? La1 C9A 2.703(4) 7_565 ? La1 C6B 2.670(17) . ? La1 C7B 2.672(11) . ? La1 C7B 2.672(11) 7_565 ? La1 C8B 2.677(10) 7_565 ? La1 C8B 2.677(10) . ? La1 C9B 2.690(11) . ? La1 C9B 2.690(11) 7_565 ? La1 C10B 2.663(15) . ? C1A H1A 0.9500 . ? C1A C2A 1.375(10) . ? C1A C2A 1.375(10) 7_565 ? C2A H2A 0.9500 . ? C2A C3A 1.404(8) . ? C3A H3A 0.9500 . ? C3A C4A 1.349(8) . ? C4A H4A 0.9500 . ? C4A C5A 1.390(9) . ? C5A C5A 1.349(13) 7_565 ? C5A H5A 0.9500 . ? C1B H1B 0.9500 . ? C1B C2B 1.396(8) 7_565 ? C1B C2B 1.396(8) . ? C2B H2B 0.9500 . ? C2B C3B 1.386(7) . ? C3B H3B 0.9500 . ? C3B C4B 1.371(7) . ? C4B H4B 0.9500 . ? C4B C5B 1.405(8) . ? C5B C5B 1.376(13) 7_565 ? C5B H5B 0.9500 . ? C1C H1C 1.10(12) . ? C6A C6A 1.445(11) 7_565 ? C6A H6A 0.9500 . ? C6A C7A 1.401(6) . ? C7A H7A 0.9500 . ? C7A C8A 1.382(6) . ? C8A H8A 0.9500 . ? C8A C9A 1.399(6) . ? C9A C9A 1.437(12) 7_565 ? C9A H9A 0.9500 . ? C6B H6B 0.9500 . ? C6B C7B 1.446(15) . ? C6B C7B 1.446(15) 7_565 ? C7B H7B 0.9500 . ? C7B C8B 1.335(12) . ? C8B H8B 0.9500 . ? C8B C9B 1.344(12) . ? C9B H9B 0.9500 . ? C9B C10B 1.427(14) . ? C10B H10B 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag La1 C1A C2A C3A 43.2(17) . . . . ? La1 C2A C3A C4A 51.0(9) . . . . ? La1 C3A C4A C5A 48.2(10) . . . . ? La1 C4A C5A C5A 47.3(6) . . . 7_565 ? La1 C1B C2B C3B -48.1(10) . . . . ? La1 C2B C3B C4B -45.3(8) . . . . ? La1 C3B C4B C5B -48.1(9) . . . . ? La1 C4B C5B C5B -49.4(4) . . . 7_565 ? La1 C6A C7A C8A -49.6(5) . . . . ? La1 C7A C8A C9A -49.3(5) . . . . ? La1 C8A C9A C9A -49.0(2) . . . 7_565 ? La1 C6B C7B C8B -49.6(15) . . . . ? La1 C7B C8B C9B -48.5(14) . . . . ? La1 C8B C9B C10B -49.1(14) . . . . ? La1 C9B C10B C9B -51.0(18) . . . 7_565 ? C1A C2A C3A La1 -43.3(18) . . . . ? C1A C2A C3A C4A 8(2) . . . . ? C2A C1A C2A La1 -51(3) 7_565 . . . ? C2A C1A C2A C3A -8(4) 7_565 . . . ? C2A C3A C4A La1 -51.2(9) . . . . ? C2A C3A C4A C5A -3.0(17) . . . . ? C3A C4A C5A La1 -48.8(10) . . . . ? C3A C4A C5A C5A -1.5(15) . . . 7_565 ? C1B C2B C3B La1 47.3(10) . . . . ? C1B C2B C3B C4B 2.1(16) . . . . ? C2B C1B C2B La1 53.5(16) 7_565 . . . ? C2B C1B C2B C3B 5(2) 7_565 . . . ? C2B C3B C4B La1 45.2(8) . . . . ? C2B C3B C4B C5B -2.9(15) . . . . ? C3B C4B C5B La1 48.3(9) . . . . ? C3B C4B C5B C5B -1.1(13) . . . 7_565 ? C6A C6A C7A La1 49.2(2) 7_565 . . . ? C6A C6A C7A C8A -0.3(7) 7_565 . . . ? C6A C7A C8A La1 49.4(5) . . . . ? C6A C7A C8A C9A 0.1(8) . . . . ? C7A C8A C9A La1 49.2(5) . . . . ? C7A C8A C9A C9A 0.2(7) . . . 7_565 ? C6B C7B C8B La1 49.1(15) . . . . ? C6B C7B C8B C9B 1(3) . . . . ? C7B C6B C7B La1 51.4(18) 7_565 . . . ? C7B C6B C7B C8B 2(3) 7_565 . . . ? C7B C8B C9B La1 48.3(14) . . . . ? C7B C8B C9B C10B -1(2) . . . . ? C8B C9B C10B La1 49.6(14) . . . . ? C8B C9B C10B C9B -1(3) . . . 7_565 ?