#------------------------------------------------------------------------------ #$Date: 2020-04-05 13:25:03 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250212 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557256.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_1557256 loop_ _publ_author_name 'Windorff, Cory J.' 'Celis-Barros, Cristian' 'Sperling, Joseph M.' 'McKinnon, Noah C.' 'Albrecht-Schmitt, Thomas E.' _publ_section_title ; Probing a variation of the inverse-trans-influence in americium and lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes ; _journal_issue 10 _journal_name_full 'Chemical Science' _journal_page_first 2770 _journal_paper_doi 10.1039/C9SC05268B _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C54 H99 Br3 La O3 P3' _chemical_formula_sum 'C54 H99 Br3 La O3 P3' _chemical_formula_weight 1267.88 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-06-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-16 deposited with the CCDC. 2020-02-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 28.8790(16) _cell_length_b 11.4223(7) _cell_length_c 18.2083(10) _cell_measurement_reflns_used 9883 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 27.476 _cell_measurement_theta_min 2.534 _cell_volume 6006.3(6) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 130(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-III CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_unetI/netI 0.0436 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 109745 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 27.545 _diffrn_reflns_theta_min 2.220 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.824 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0828 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.8903. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.402 _exptl_crystal_description block _exptl_crystal_F_000 2616 _exptl_crystal_preparation 'combining reagents in iPrOH' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: iPrOH' _exptl_crystal_size_max 0.267 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.153 _refine_diff_density_max 0.757 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.088 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.018(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 13561 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0348 _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^)+(0.0056P)^2^+8.3987P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.0620 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 11489 _reflns_number_total 13561 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05268b2.cif _cod_data_source_block 'save_a' _cod_depositor_comments 'Adding full bibliography for 1557253--1557257.cif.' _cod_database_code 1557256 _shelx_shelxl_version_number 2016/6 _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_max 0.672 _shelx_estimated_absorpt_t_min 0.519 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.982(9) 0.018(9) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 3.a Ternary CH refined with riding coordinates: C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31), C37(H37), C43(H43), C49(H49) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A, H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A, H42B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B) ; _shelx_res_file ; TITL save_a.res in Pca2(1) save_a.res created by SHELXL-2016/6 at 17:21:43 on 08-Jun-2019 REM Old TITL save in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.099, Rweak 0.015, Alpha 0.019, Orientation as input REM Flack x = 0.053 ( 0.004 ) from Parsons' quotients REM Formula found by SHELXT: C52 O5 P2 Br1 La CELL 0.71073 28.879 11.4223 18.2083 90 90 90 ZERR 4 0.0016 0.0007 0.001 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H O P Br La UNIT 216 396 12 12 12 4 L.S. 20 PLAN 10 SIZE 0.153 0.157 0.267 TEMP -143(2) BOND $H LIST 6 fmap 2 acta 51 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.005600 8.398701 BASF 0.01767 FVAR 0.15848 LA1 6 0.372992 0.419351 0.483781 11.00000 0.01346 0.01583 = 0.01287 0.00001 0.00051 -0.00156 BR1 5 0.433181 0.414386 0.613728 11.00000 0.03592 0.04112 = 0.02236 0.00428 -0.01340 -0.01158 BR2 5 0.315398 0.391910 0.351591 11.00000 0.03046 0.04209 = 0.02274 0.00033 -0.01135 -0.00285 BR3 5 0.372093 0.678916 0.483827 11.00000 0.03602 0.01647 = 0.07036 0.00101 0.00751 -0.00228 P1 4 0.264284 0.457989 0.602358 11.00000 0.01873 0.02129 = 0.01600 -0.00164 0.00480 -0.00284 P2 4 0.479375 0.465461 0.362212 11.00000 0.01687 0.01974 = 0.02494 0.00003 0.00678 -0.00156 P3 4 0.386947 0.081225 0.488887 11.00000 0.02280 0.01606 = 0.02552 0.00236 -0.00402 -0.00033 O1 3 0.306533 0.424054 0.558252 11.00000 0.01950 0.02628 = 0.02170 -0.00207 0.00606 -0.00203 O2 3 0.439257 0.420811 0.407674 11.00000 0.01586 0.02435 = 0.02944 -0.00418 0.00820 -0.00290 O3 3 0.376810 0.211217 0.489708 11.00000 0.02434 0.02160 = 0.02781 0.00166 -0.00175 0.00046 C1 1 0.278405 0.456209 0.699529 11.00000 0.01681 0.02978 = 0.01353 -0.00057 0.00407 -0.00029 AFIX 13 H1 2 0.248988 0.461615 0.728303 11.00000 -1.20000 AFIX 0 C2 1 0.309618 0.559985 0.720688 11.00000 0.03723 0.03561 = 0.02743 -0.00787 0.00379 -0.00944 AFIX 23 H2A 2 0.338235 0.558329 0.690772 11.00000 -1.20000 H2B 2 0.293289 0.634475 0.710593 11.00000 -1.20000 AFIX 0 C3 1 0.322112 0.553048 0.802447 11.00000 0.03652 0.05925 = 0.02790 -0.01423 -0.00265 -0.00815 AFIX 23 H3A 2 0.343359 0.618118 0.814876 11.00000 -1.20000 H3B 2 0.293641 0.562580 0.832134 11.00000 -1.20000 AFIX 0 C4 1 0.344719 0.438964 0.821797 11.00000 0.03472 0.07568 = 0.02564 -0.00943 -0.00488 0.00370 AFIX 23 H4A 2 0.351016 0.436983 0.875229 11.00000 -1.20000 H4B 2 0.374710 0.432740 0.795752 11.00000 -1.20000 AFIX 0 C5 1 0.314424 0.335642 0.801248 11.00000 0.02276 0.05421 = 0.03053 0.00473 -0.00260 0.00551 AFIX 23 H5A 2 0.285522 0.337551 0.830462 11.00000 -1.20000 H5B 2 0.330849 0.261694 0.812458 11.00000 -1.20000 AFIX 0 C6 1 0.302687 0.340374 0.719068 11.00000 0.02232 0.03961 = 0.03014 0.00028 -0.00019 0.00268 AFIX 23 H6A 2 0.282219 0.273881 0.706323 11.00000 -1.20000 H6B 2 0.331489 0.332889 0.689959 11.00000 -1.20000 AFIX 0 C7 1 0.216618 0.356771 0.582876 11.00000 0.02819 0.02705 = 0.02163 0.00262 0.00126 -0.00429 AFIX 13 H7 2 0.194828 0.399638 0.549728 11.00000 -1.20000 AFIX 0 C8 1 0.234270 0.251778 0.539232 11.00000 0.04252 0.03858 = 0.03831 -0.01775 0.01567 -0.01761 AFIX 23 H8A 2 0.248970 0.279562 0.493310 11.00000 -1.20000 H8B 2 0.258072 0.210090 0.568339 11.00000 -1.20000 AFIX 0 C9 1 0.195212 0.167619 0.520486 11.00000 0.04662 0.04005 = 0.04187 -0.01398 0.00523 -0.01560 AFIX 23 H9A 2 0.173303 0.206626 0.486574 11.00000 -1.20000 H9B 2 0.208165 0.098459 0.494955 11.00000 -1.20000 AFIX 0 C10 1 0.169445 0.127857 0.588161 11.00000 0.02754 0.03059 = 0.05182 0.00048 -0.00257 -0.00695 AFIX 23 H10A 2 0.143762 0.075279 0.573701 11.00000 -1.20000 H10B 2 0.190664 0.083402 0.620501 11.00000 -1.20000 AFIX 0 C11 1 0.150326 0.231595 0.629274 11.00000 0.02234 0.02900 = 0.04486 0.00571 0.00331 -0.00567 AFIX 23 H11A 2 0.134968 0.204061 0.674711 11.00000 -1.20000 H11B 2 0.126715 0.271014 0.598576 11.00000 -1.20000 AFIX 0 C12 1 0.188484 0.319988 0.649457 11.00000 0.02552 0.02773 = 0.03018 0.00023 0.00600 -0.00552 AFIX 23 H12A 2 0.174122 0.390118 0.671861 11.00000 -1.20000 H12B 2 0.209372 0.284437 0.686353 11.00000 -1.20000 AFIX 0 C13 1 0.246553 0.603298 0.575858 11.00000 0.02226 0.02269 = 0.02305 -0.00463 0.00538 -0.00299 AFIX 13 H13 2 0.273350 0.655945 0.586772 11.00000 -1.20000 AFIX 0 C14 1 0.238048 0.611981 0.492757 11.00000 0.02829 0.02672 = 0.02492 0.00177 0.00107 -0.00250 AFIX 23 H14A 2 0.265449 0.582160 0.465973 11.00000 -1.20000 H14B 2 0.211093 0.562999 0.479180 11.00000 -1.20000 AFIX 0 C15 1 0.228920 0.738919 0.470727 11.00000 0.04016 0.02660 = 0.03307 0.00773 -0.00212 -0.01039 AFIX 23 H15A 2 0.257048 0.786181 0.480046 11.00000 -1.20000 H15B 2 0.222091 0.742525 0.417494 11.00000 -1.20000 AFIX 0 C16 1 0.188541 0.790441 0.513342 11.00000 0.03324 0.02600 = 0.05552 0.00693 -0.00117 -0.00151 AFIX 23 H16A 2 0.185121 0.874150 0.500333 11.00000 -1.20000 H16B 2 0.159687 0.749658 0.498940 11.00000 -1.20000 AFIX 0 C17 1 0.195083 0.779566 0.595369 11.00000 0.04100 0.02390 = 0.05717 -0.00519 0.00902 0.00188 AFIX 23 H17A 2 0.166739 0.807073 0.620620 11.00000 -1.20000 H17B 2 0.221069 0.830357 0.610935 11.00000 -1.20000 AFIX 0 C18 1 0.205220 0.652759 0.618455 11.00000 0.02916 0.02517 = 0.03786 -0.00357 0.00936 0.00085 AFIX 23 H18A 2 0.211939 0.650241 0.671748 11.00000 -1.20000 H18B 2 0.177575 0.603711 0.609132 11.00000 -1.20000 AFIX 0 C19 1 0.461745 0.596870 0.314704 11.00000 0.02829 0.04179 = 0.05107 0.01794 -0.00696 -0.00625 AFIX 13 H19 2 0.450417 0.648044 0.355482 11.00000 -1.20000 AFIX 0 C20 1 0.500097 0.669620 0.280612 11.00000 0.03396 0.02307 = 0.03602 0.00787 0.01036 0.00047 AFIX 23 H20A 2 0.515814 0.623071 0.242114 11.00000 -1.20000 H20B 2 0.523270 0.689205 0.318749 11.00000 -1.20000 AFIX 0 C21 1 0.481269 0.783557 0.246527 11.00000 0.05725 0.03838 = 0.07308 0.02200 -0.00794 -0.00917 AFIX 23 H21A 2 0.474720 0.839610 0.286675 11.00000 -1.20000 H21B 2 0.505802 0.818268 0.215413 11.00000 -1.20000 AFIX 0 C22 1 0.440254 0.770782 0.203033 11.00000 0.09043 0.06230 = 0.06666 0.03626 -0.01477 -0.00803 AFIX 23 H22A 2 0.449074 0.737589 0.154795 11.00000 -1.20000 H22B 2 0.427062 0.849494 0.194075 11.00000 -1.20000 AFIX 0 C23 1 0.403596 0.695520 0.235735 11.00000 0.05563 0.06400 = 0.06719 0.03592 -0.03315 -0.00967 AFIX 23 H23A 2 0.380714 0.676155 0.197116 11.00000 -1.20000 H23B 2 0.387299 0.740794 0.274225 11.00000 -1.20000 AFIX 0 C24 1 0.421024 0.583799 0.268846 11.00000 0.06462 0.09973 = 0.10073 0.07491 -0.05018 -0.04002 AFIX 23 H24A 2 0.395936 0.548773 0.298681 11.00000 -1.20000 H24B 2 0.428296 0.528330 0.228691 11.00000 -1.20000 AFIX 0 C25 1 0.498938 0.345740 0.304564 11.00000 0.03350 0.04541 = 0.04961 -0.02179 0.01938 -0.00731 AFIX 13 H25 2 0.510490 0.287820 0.341446 11.00000 -1.20000 AFIX 0 C26 1 0.541930 0.371083 0.259881 11.00000 0.02999 0.04504 = 0.03755 -0.01094 0.01463 -0.00151 AFIX 23 H26A 2 0.535513 0.436997 0.226074 11.00000 -1.20000 H26B 2 0.567141 0.395553 0.293372 11.00000 -1.20000 AFIX 0 C27 1 0.557763 0.267561 0.216075 11.00000 0.06790 0.07913 = 0.11801 -0.06030 0.05738 -0.01061 AFIX 23 H27A 2 0.578679 0.296426 0.176988 11.00000 -1.20000 H27B 2 0.576436 0.216986 0.248824 11.00000 -1.20000 AFIX 0 C28 1 0.523466 0.196500 0.182456 11.00000 0.06297 0.08114 = 0.06861 -0.03361 0.01153 0.01516 AFIX 23 H28A 2 0.537661 0.119850 0.170741 11.00000 -1.20000 H28B 2 0.514644 0.233459 0.135309 11.00000 -1.20000 AFIX 0 C29 1 0.479980 0.174340 0.225557 11.00000 0.04949 0.03240 = 0.05364 -0.01977 -0.00254 0.00257 AFIX 23 H29A 2 0.455320 0.148203 0.191534 11.00000 -1.20000 H29B 2 0.485717 0.110234 0.261000 11.00000 -1.20000 AFIX 0 C30 1 0.463470 0.279824 0.266419 11.00000 0.04116 0.05264 = 0.08996 -0.04140 0.02427 -0.01044 AFIX 23 H30A 2 0.447854 0.332753 0.231202 11.00000 -1.20000 H30B 2 0.440019 0.254482 0.302753 11.00000 -1.20000 AFIX 0 C31 1 0.527053 0.505887 0.420838 11.00000 0.02052 0.02426 = 0.03054 0.00166 0.00615 -0.00077 AFIX 13 H31 2 0.552524 0.538283 0.389672 11.00000 -1.20000 AFIX 0 C32 1 0.511829 0.600151 0.475651 11.00000 0.04092 0.01806 = 0.03585 -0.00005 -0.00950 0.00062 AFIX 23 H32A 2 0.500587 0.669572 0.448416 11.00000 -1.20000 H32B 2 0.485874 0.569820 0.505644 11.00000 -1.20000 AFIX 0 C33 1 0.551246 0.636205 0.525874 11.00000 0.05757 0.03118 = 0.04534 0.00173 -0.01017 -0.01824 AFIX 23 H33A 2 0.540627 0.698395 0.559794 11.00000 -1.20000 H33B 2 0.577179 0.667694 0.496305 11.00000 -1.20000 AFIX 0 C34 1 0.567652 0.530166 0.569813 11.00000 0.04608 0.04708 = 0.04058 0.01400 -0.01338 -0.02204 AFIX 23 H34A 2 0.593424 0.553260 0.602608 11.00000 -1.20000 H34B 2 0.541994 0.500309 0.600625 11.00000 -1.20000 AFIX 0 C35 1 0.583798 0.434891 0.517563 11.00000 0.02623 0.05883 = 0.05318 0.02884 -0.00660 -0.00084 AFIX 23 H35A 2 0.611081 0.463064 0.489787 11.00000 -1.20000 H35B 2 0.593329 0.365245 0.546179 11.00000 -1.20000 AFIX 0 C36 1 0.545878 0.400718 0.464208 11.00000 0.02989 0.02288 = 0.03907 0.00688 0.00539 0.00678 AFIX 23 H36A 2 0.520157 0.363899 0.491751 11.00000 -1.20000 H36B 2 0.558172 0.341966 0.429315 11.00000 -1.20000 AFIX 0 C37 1 0.448404 0.058153 0.469620 11.00000 0.02617 0.01907 = 0.03039 0.00094 -0.00344 -0.00099 AFIX 13 H37 2 0.454884 0.102113 0.423251 11.00000 -1.20000 AFIX 0 C38 1 0.480161 0.111482 0.527602 11.00000 0.02648 0.02926 = 0.03395 -0.00149 -0.00363 -0.00323 AFIX 23 H38A 2 0.475830 0.069982 0.574838 11.00000 -1.20000 H38B 2 0.471915 0.194763 0.535068 11.00000 -1.20000 AFIX 0 C39 1 0.531118 0.102349 0.503708 11.00000 0.02528 0.02992 = 0.05153 -0.00529 -0.00651 -0.00073 AFIX 23 H39A 2 0.536062 0.151114 0.459448 11.00000 -1.20000 H39B 2 0.551191 0.133211 0.543304 11.00000 -1.20000 AFIX 0 C40 1 0.544814 -0.023135 0.486950 11.00000 0.02668 0.03311 = 0.05167 0.00138 -0.00082 0.00472 AFIX 23 H40A 2 0.542857 -0.070751 0.532274 11.00000 -1.20000 H40B 2 0.577206 -0.025385 0.469209 11.00000 -1.20000 AFIX 0 C41 1 0.512789 -0.074088 0.428650 11.00000 0.03246 0.01890 = 0.04905 -0.00118 0.00329 0.00213 AFIX 23 H41A 2 0.521585 -0.156378 0.418813 11.00000 -1.20000 H41B 2 0.516312 -0.029360 0.382414 11.00000 -1.20000 AFIX 0 C42 1 0.461890 -0.069207 0.453901 11.00000 0.02697 0.01871 = 0.04086 0.00037 0.00055 -0.00006 AFIX 23 H42A 2 0.441585 -0.101717 0.415129 11.00000 -1.20000 H42B 2 0.457863 -0.116950 0.498827 11.00000 -1.20000 AFIX 0 C43 1 0.353663 0.012365 0.416037 11.00000 0.02718 0.01850 = 0.02445 0.00298 -0.00537 -0.00508 AFIX 13 H43 2 0.355019 -0.074480 0.422641 11.00000 -1.20000 AFIX 0 C44 1 0.373262 0.043043 0.340337 11.00000 0.02661 0.02287 = 0.03074 0.00322 -0.00222 -0.00266 AFIX 23 H44A 2 0.373889 0.129202 0.334514 11.00000 -1.20000 H44B 2 0.405485 0.014031 0.336724 11.00000 -1.20000 AFIX 0 C45 1 0.344348 -0.010667 0.278751 11.00000 0.04552 0.03715 = 0.02426 -0.00566 -0.00654 -0.00059 AFIX 23 H45A 2 0.357356 0.013047 0.230696 11.00000 -1.20000 H45B 2 0.345897 -0.097093 0.282029 11.00000 -1.20000 AFIX 0 C46 1 0.294217 0.028208 0.283423 11.00000 0.03974 0.03974 = 0.03304 0.00245 -0.01354 -0.00906 AFIX 23 H46A 2 0.292312 0.113733 0.275139 11.00000 -1.20000 H46B 2 0.276024 -0.011181 0.244524 11.00000 -1.20000 AFIX 0 C47 1 0.273937 -0.001069 0.357572 11.00000 0.03216 0.04090 = 0.03888 0.00373 -0.01187 -0.00967 AFIX 23 H47A 2 0.272680 -0.087171 0.363475 11.00000 -1.20000 H47B 2 0.241887 0.029357 0.360395 11.00000 -1.20000 AFIX 0 C48 1 0.302654 0.051606 0.419608 11.00000 0.02621 0.03395 = 0.02957 -0.00133 -0.00756 -0.00234 AFIX 23 H48A 2 0.289287 0.027614 0.467359 11.00000 -1.20000 H48B 2 0.301168 0.138066 0.416617 11.00000 -1.20000 AFIX 0 C49 1 0.375638 0.015097 0.578649 11.00000 0.02882 0.02210 = 0.02404 0.00320 0.00092 -0.00103 AFIX 13 H49 2 0.399678 -0.046909 0.585683 11.00000 -1.20000 AFIX 0 C50 1 0.328699 -0.044559 0.589644 11.00000 0.02484 0.03073 = 0.03617 0.00444 0.00071 0.00003 AFIX 23 H50A 2 0.303587 0.013794 0.584187 11.00000 -1.20000 H50B 2 0.324324 -0.105703 0.551739 11.00000 -1.20000 AFIX 0 C51 1 0.326252 -0.099856 0.665848 11.00000 0.02798 0.03118 = 0.04677 0.00822 0.00463 -0.00081 AFIX 23 H51A 2 0.295211 -0.134843 0.672965 11.00000 -1.20000 H51B 2 0.349402 -0.163564 0.669142 11.00000 -1.20000 AFIX 0 C52 1 0.335299 -0.011338 0.726738 11.00000 0.04576 0.05104 = 0.03389 0.00663 0.01403 -0.00326 AFIX 23 H52A 2 0.309721 0.046329 0.728059 11.00000 -1.20000 H52B 2 0.336026 -0.052289 0.774644 11.00000 -1.20000 AFIX 0 C53 1 0.380925 0.052413 0.715039 11.00000 0.04850 0.04448 = 0.03463 0.00534 0.00232 -0.00637 AFIX 23 H53A 2 0.384129 0.115041 0.752280 11.00000 -1.20000 H53B 2 0.406868 -0.003225 0.721745 11.00000 -1.20000 AFIX 0 C54 1 0.383667 0.105728 0.638914 11.00000 0.03474 0.02587 = 0.02757 -0.00149 0.00235 -0.00226 AFIX 23 H54A 2 0.414553 0.141733 0.632100 11.00000 -1.20000 H54B 2 0.360161 0.168429 0.634529 11.00000 -1.20000 AFIX 0 HKLF 4 REM save_a.res in Pca2(1) REM R1 = 0.0348 for 11489 Fo > 4sig(Fo) and 0.0510 for all 13561 data REM 578 parameters refined using 1 restraints END WGHT 0.0056 8.3993 REM Highest difference peak 0.757, deepest hole -0.569, 1-sigma level 0.088 Q1 1 0.3773 0.5368 0.4834 11.00000 0.05 0.76 Q2 1 0.3711 0.4326 0.4354 11.00000 0.05 0.59 Q3 1 0.4880 0.3854 0.2655 11.00000 0.05 0.58 Q4 1 0.3497 0.6073 0.4838 11.00000 0.05 0.56 Q5 1 0.4728 0.5697 0.2741 11.00000 0.05 0.54 Q6 1 0.4210 0.4838 0.6141 11.00000 0.05 0.54 Q7 1 0.3116 0.3822 0.4052 11.00000 0.05 0.51 Q8 1 0.3881 0.4263 0.4844 11.00000 0.05 0.47 Q9 1 0.3772 0.4400 0.5294 11.00000 0.05 0.47 Q10 1 0.4414 0.5362 0.6169 11.00000 0.05 0.47 ; _shelx_res_checksum 91597 _olex2_exptl_crystal_mounting_method 'nylon loop' _olex2_submission_original_sample_id cjw86 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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 La1 La 0.37299(2) 0.41935(2) 0.48378(2) 0.01405(6) Uani 1 1 d . Br1 Br 0.43318(2) 0.41439(6) 0.61373(3) 0.03313(15) Uani 1 1 d . Br2 Br 0.31540(2) 0.39191(6) 0.35159(3) 0.03176(15) Uani 1 1 d . Br3 Br 0.37209(2) 0.67892(4) 0.48383(7) 0.04095(14) Uani 1 1 d . P1 P 0.26428(5) 0.45799(13) 0.60236(8) 0.0187(3) Uani 1 1 d . P2 P 0.47938(5) 0.46546(13) 0.36221(9) 0.0205(3) Uani 1 1 d . P3 P 0.38695(4) 0.08122(11) 0.48889(11) 0.0215(3) Uani 1 1 d . O1 O 0.30653(13) 0.4241(3) 0.5583(2) 0.0225(9) Uani 1 1 d . O2 O 0.43926(12) 0.4208(3) 0.4077(2) 0.0232(9) Uani 1 1 d . O3 O 0.37681(13) 0.2112(3) 0.4897(3) 0.0246(8) Uani 1 1 d . C1 C 0.27840(18) 0.4562(5) 0.6995(3) 0.0200(11) Uani 1 1 d . H1 H 0.248988 0.461615 0.728303 0.024 Uiso 1 1 calc R C2 C 0.3096(2) 0.5600(6) 0.7207(3) 0.0334(15) Uani 1 1 d . H2A H 0.338235 0.558329 0.690772 0.040 Uiso 1 1 calc R H2B H 0.293289 0.634475 0.710593 0.040 Uiso 1 1 calc R C3 C 0.3221(2) 0.5530(6) 0.8024(4) 0.0412(17) Uani 1 1 d . H3A H 0.343359 0.618118 0.814876 0.049 Uiso 1 1 calc R H3B H 0.293641 0.562580 0.832134 0.049 Uiso 1 1 calc R C4 C 0.3447(2) 0.4390(7) 0.8218(4) 0.0453(19) Uani 1 1 d . H4A H 0.351016 0.436983 0.875229 0.054 Uiso 1 1 calc R H4B H 0.374710 0.432740 0.795752 0.054 Uiso 1 1 calc R C5 C 0.3144(2) 0.3356(7) 0.8012(3) 0.0358(17) Uani 1 1 d . H5A H 0.285522 0.337551 0.830462 0.043 Uiso 1 1 calc R H5B H 0.330849 0.261694 0.812458 0.043 Uiso 1 1 calc R C6 C 0.3027(2) 0.3404(5) 0.7191(3) 0.0307(14) Uani 1 1 d . H6A H 0.282219 0.273881 0.706323 0.037 Uiso 1 1 calc R H6B H 0.331489 0.332889 0.689959 0.037 Uiso 1 1 calc R C7 C 0.2166(2) 0.3568(5) 0.5829(3) 0.0256(13) Uani 1 1 d . H7 H 0.194828 0.399638 0.549728 0.031 Uiso 1 1 calc R C8 C 0.2343(2) 0.2518(6) 0.5392(4) 0.0398(17) Uani 1 1 d . H8A H 0.248970 0.279562 0.493310 0.048 Uiso 1 1 calc R H8B H 0.258072 0.210090 0.568339 0.048 Uiso 1 1 calc R C9 C 0.1952(2) 0.1676(6) 0.5205(4) 0.0428(17) Uani 1 1 d . H9A H 0.173303 0.206626 0.486574 0.051 Uiso 1 1 calc R H9B H 0.208165 0.098459 0.494955 0.051 Uiso 1 1 calc R C10 C 0.1694(2) 0.1279(5) 0.5882(4) 0.0366(16) Uani 1 1 d . H10A H 0.143762 0.075279 0.573701 0.044 Uiso 1 1 calc R H10B H 0.190664 0.083402 0.620501 0.044 Uiso 1 1 calc R C11 C 0.1503(2) 0.2316(5) 0.6293(4) 0.0321(15) Uani 1 1 d . H11A H 0.134968 0.204061 0.674711 0.038 Uiso 1 1 calc R H11B H 0.126715 0.271014 0.598576 0.038 Uiso 1 1 calc R C12 C 0.1885(2) 0.3200(6) 0.6495(3) 0.0278(14) Uani 1 1 d . H12A H 0.174122 0.390118 0.671861 0.033 Uiso 1 1 calc R H12B H 0.209372 0.284437 0.686353 0.033 Uiso 1 1 calc R C13 C 0.24655(19) 0.6033(5) 0.5759(3) 0.0227(12) Uani 1 1 d . H13 H 0.273350 0.655945 0.586772 0.027 Uiso 1 1 calc R C14 C 0.23805(19) 0.6120(4) 0.4928(4) 0.0266(13) Uani 1 1 d . H14A H 0.265449 0.582160 0.465973 0.032 Uiso 1 1 calc R H14B H 0.211093 0.562999 0.479180 0.032 Uiso 1 1 calc R C15 C 0.2289(2) 0.7389(5) 0.4707(3) 0.0333(15) Uani 1 1 d . H15A H 0.257048 0.786181 0.480046 0.040 Uiso 1 1 calc R H15B H 0.222091 0.742525 0.417494 0.040 Uiso 1 1 calc R C16 C 0.1885(2) 0.7904(5) 0.5133(4) 0.0383(17) Uani 1 1 d . H16A H 0.185121 0.874150 0.500333 0.046 Uiso 1 1 calc R H16B H 0.159687 0.749658 0.498940 0.046 Uiso 1 1 calc R C17 C 0.1951(2) 0.7796(5) 0.5954(4) 0.0407(17) Uani 1 1 d . H17A H 0.166739 0.807073 0.620620 0.049 Uiso 1 1 calc R H17B H 0.221069 0.830357 0.610935 0.049 Uiso 1 1 calc R C18 C 0.2052(2) 0.6528(5) 0.6185(4) 0.0307(14) Uani 1 1 d . H18A H 0.211939 0.650241 0.671748 0.037 Uiso 1 1 calc R H18B H 0.177575 0.603711 0.609132 0.037 Uiso 1 1 calc R C19 C 0.4617(2) 0.5969(6) 0.3147(4) 0.0404(17) Uani 1 1 d . H19 H 0.450417 0.648044 0.355482 0.048 Uiso 1 1 calc R C20 C 0.5001(2) 0.6696(5) 0.2806(4) 0.0310(14) Uani 1 1 d . H20A H 0.515814 0.623071 0.242114 0.037 Uiso 1 1 calc R H20B H 0.523270 0.689205 0.318749 0.037 Uiso 1 1 calc R C21 C 0.4813(3) 0.7836(7) 0.2465(5) 0.056(2) Uani 1 1 d . H21A H 0.474720 0.839610 0.286675 0.067 Uiso 1 1 calc R H21B H 0.505802 0.818268 0.215413 0.067 Uiso 1 1 calc R C22 C 0.4403(3) 0.7708(8) 0.2030(5) 0.073(3) Uani 1 1 d . H22A H 0.449074 0.737589 0.154795 0.088 Uiso 1 1 calc R H22B H 0.427062 0.849494 0.194075 0.088 Uiso 1 1 calc R C23 C 0.4036(3) 0.6955(7) 0.2357(5) 0.062(2) Uani 1 1 d . H23A H 0.380714 0.676155 0.197116 0.075 Uiso 1 1 calc R H23B H 0.387299 0.740794 0.274225 0.075 Uiso 1 1 calc R C24 C 0.4210(3) 0.5838(9) 0.2688(6) 0.088(4) Uani 1 1 d . H24A H 0.395936 0.548773 0.298681 0.106 Uiso 1 1 calc R H24B H 0.428296 0.528330 0.228691 0.106 Uiso 1 1 calc R C25 C 0.4989(2) 0.3457(6) 0.3046(4) 0.0428(18) Uani 1 1 d . H25 H 0.510490 0.287820 0.341446 0.051 Uiso 1 1 calc R C26 C 0.5419(2) 0.3711(6) 0.2599(4) 0.0375(16) Uani 1 1 d . H26A H 0.535513 0.436997 0.226074 0.045 Uiso 1 1 calc R H26B H 0.567141 0.395553 0.293372 0.045 Uiso 1 1 calc R C27 C 0.5578(3) 0.2676(9) 0.2161(6) 0.088(4) Uani 1 1 d . H27A H 0.578679 0.296426 0.176988 0.106 Uiso 1 1 calc R H27B H 0.576436 0.216986 0.248824 0.106 Uiso 1 1 calc R C28 C 0.5235(3) 0.1965(9) 0.1825(5) 0.071(3) Uani 1 1 d . H28A H 0.537661 0.119850 0.170741 0.085 Uiso 1 1 calc R H28B H 0.514644 0.233459 0.135309 0.085 Uiso 1 1 calc R C29 C 0.4800(2) 0.1743(6) 0.2256(4) 0.0452(18) Uani 1 1 d . H29A H 0.455320 0.148203 0.191534 0.054 Uiso 1 1 calc R H29B H 0.485717 0.110234 0.261000 0.054 Uiso 1 1 calc R C30 C 0.4635(3) 0.2798(7) 0.2664(5) 0.061(3) Uani 1 1 d . H30A H 0.447854 0.332753 0.231202 0.074 Uiso 1 1 calc R H30B H 0.440019 0.254482 0.302753 0.074 Uiso 1 1 calc R C31 C 0.52705(19) 0.5059(5) 0.4208(3) 0.0251(13) Uani 1 1 d . H31 H 0.552524 0.538283 0.389672 0.030 Uiso 1 1 calc R C32 C 0.5118(2) 0.6002(5) 0.4757(4) 0.0316(15) Uani 1 1 d . H32A H 0.500587 0.669572 0.448416 0.038 Uiso 1 1 calc R H32B H 0.485874 0.569820 0.505644 0.038 Uiso 1 1 calc R C33 C 0.5512(3) 0.6362(6) 0.5259(4) 0.0447(18) Uani 1 1 d . H33A H 0.540627 0.698395 0.559794 0.054 Uiso 1 1 calc R H33B H 0.577179 0.667694 0.496305 0.054 Uiso 1 1 calc R C34 C 0.5677(3) 0.5302(6) 0.5698(4) 0.0446(18) Uani 1 1 d . H34A H 0.593424 0.553260 0.602608 0.053 Uiso 1 1 calc R H34B H 0.541994 0.500309 0.600625 0.053 Uiso 1 1 calc R C35 C 0.5838(2) 0.4349(7) 0.5176(4) 0.0461(19) Uani 1 1 d . H35A H 0.611081 0.463064 0.489787 0.055 Uiso 1 1 calc R H35B H 0.593329 0.365245 0.546179 0.055 Uiso 1 1 calc R C36 C 0.5459(2) 0.4007(5) 0.4642(3) 0.0306(15) Uani 1 1 d . H36A H 0.520157 0.363899 0.491751 0.037 Uiso 1 1 calc R H36B H 0.558172 0.341966 0.429315 0.037 Uiso 1 1 calc R C37 C 0.44840(18) 0.0582(4) 0.4696(3) 0.0252(14) Uani 1 1 d . H37 H 0.454884 0.102113 0.423251 0.030 Uiso 1 1 calc R C38 C 0.48016(19) 0.1115(5) 0.5276(3) 0.0299(14) Uani 1 1 d . H38A H 0.475830 0.069982 0.574838 0.036 Uiso 1 1 calc R H38B H 0.471915 0.194763 0.535068 0.036 Uiso 1 1 calc R C39 C 0.5311(2) 0.1023(5) 0.5037(4) 0.0356(16) Uani 1 1 d . H39A H 0.536062 0.151114 0.459448 0.043 Uiso 1 1 calc R H39B H 0.551191 0.133211 0.543304 0.043 Uiso 1 1 calc R C40 C 0.54481(19) -0.0231(5) 0.4870(5) 0.0372(14) Uani 1 1 d . H40A H 0.542857 -0.070751 0.532274 0.045 Uiso 1 1 calc R H40B H 0.577206 -0.025385 0.469209 0.045 Uiso 1 1 calc R C41 C 0.5128(2) -0.0741(5) 0.4286(4) 0.0335(15) Uani 1 1 d . H41A H 0.521585 -0.156378 0.418813 0.040 Uiso 1 1 calc R H41B H 0.516312 -0.029360 0.382414 0.040 Uiso 1 1 calc R C42 C 0.46189(19) -0.0692(5) 0.4539(3) 0.0288(13) Uani 1 1 d . H42A H 0.441585 -0.101717 0.415129 0.035 Uiso 1 1 calc R H42B H 0.457863 -0.116950 0.498827 0.035 Uiso 1 1 calc R C43 C 0.3537(2) 0.0124(5) 0.4160(3) 0.0234(13) Uani 1 1 d . H43 H 0.355019 -0.074480 0.422641 0.028 Uiso 1 1 calc R C44 C 0.37326(19) 0.0430(5) 0.3403(3) 0.0267(13) Uani 1 1 d . H44A H 0.373889 0.129202 0.334514 0.032 Uiso 1 1 calc R H44B H 0.405485 0.014031 0.336724 0.032 Uiso 1 1 calc R C45 C 0.3443(2) -0.0107(6) 0.2788(4) 0.0356(16) Uani 1 1 d . H45A H 0.357356 0.013047 0.230696 0.043 Uiso 1 1 calc R H45B H 0.345897 -0.097093 0.282029 0.043 Uiso 1 1 calc R C46 C 0.2942(2) 0.0282(6) 0.2834(4) 0.0375(16) Uani 1 1 d . H46A H 0.292312 0.113733 0.275139 0.045 Uiso 1 1 calc R H46B H 0.276024 -0.011181 0.244524 0.045 Uiso 1 1 calc R C47 C 0.2739(2) -0.0011(6) 0.3576(4) 0.0373(16) Uani 1 1 d . H47A H 0.272680 -0.087171 0.363475 0.045 Uiso 1 1 calc R H47B H 0.241887 0.029357 0.360395 0.045 Uiso 1 1 calc R C48 C 0.3027(2) 0.0516(5) 0.4196(3) 0.0299(14) Uani 1 1 d . H48A H 0.289287 0.027614 0.467359 0.036 Uiso 1 1 calc R H48B H 0.301168 0.138066 0.416617 0.036 Uiso 1 1 calc R C49 C 0.3756(2) 0.0151(5) 0.5786(3) 0.0250(13) Uani 1 1 d . H49 H 0.399678 -0.046909 0.585683 0.030 Uiso 1 1 calc R C50 C 0.3287(2) -0.0446(5) 0.5896(3) 0.0306(14) Uani 1 1 d . H50A H 0.303587 0.013794 0.584187 0.037 Uiso 1 1 calc R H50B H 0.324324 -0.105703 0.551739 0.037 Uiso 1 1 calc R C51 C 0.3263(2) -0.0999(6) 0.6658(4) 0.0353(15) Uani 1 1 d . H51A H 0.295211 -0.134843 0.672965 0.042 Uiso 1 1 calc R H51B H 0.349402 -0.163564 0.669142 0.042 Uiso 1 1 calc R C52 C 0.3353(2) -0.0113(7) 0.7267(4) 0.0436(18) Uani 1 1 d . H52A H 0.309721 0.046329 0.728059 0.052 Uiso 1 1 calc R H52B H 0.336026 -0.052289 0.774644 0.052 Uiso 1 1 calc R C53 C 0.3809(2) 0.0524(6) 0.7150(4) 0.0425(17) Uani 1 1 d . H53A H 0.384129 0.115041 0.752280 0.051 Uiso 1 1 calc R H53B H 0.406868 -0.003225 0.721745 0.051 Uiso 1 1 calc R C54 C 0.3837(2) 0.1057(5) 0.6389(3) 0.0294(14) Uani 1 1 d . H54A H 0.414553 0.141733 0.632100 0.035 Uiso 1 1 calc R H54B H 0.360161 0.168429 0.634529 0.035 Uiso 1 1 calc R 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 0.01346(11) 0.01583(12) 0.01287(11) 0.0000(2) 0.00051(12) -0.00156(11) Br1 0.0359(3) 0.0411(4) 0.0224(3) 0.0043(3) -0.0134(3) -0.0116(3) Br2 0.0305(3) 0.0421(4) 0.0227(3) 0.0003(3) -0.0114(3) -0.0028(3) Br3 0.0360(3) 0.0165(2) 0.0704(4) 0.0010(5) 0.0075(4) -0.0023(2) P1 0.0187(7) 0.0213(7) 0.0160(7) -0.0016(6) 0.0048(6) -0.0028(6) P2 0.0169(7) 0.0197(7) 0.0249(8) 0.0000(7) 0.0068(6) -0.0016(6) P3 0.0228(6) 0.0161(5) 0.0255(7) 0.0024(8) -0.0040(8) -0.0003(5) O1 0.020(2) 0.026(2) 0.022(2) -0.0021(18) 0.0061(16) -0.0020(17) O2 0.0159(19) 0.024(2) 0.029(2) -0.0042(18) 0.0082(17) -0.0029(17) O3 0.0243(18) 0.0216(16) 0.028(2) 0.002(3) -0.0018(19) 0.0005(15) C1 0.017(3) 0.030(3) 0.014(3) -0.001(2) 0.004(2) 0.000(2) C2 0.037(4) 0.036(4) 0.027(3) -0.008(3) 0.004(3) -0.009(3) C3 0.037(4) 0.059(5) 0.028(4) -0.014(3) -0.003(3) -0.008(3) C4 0.035(4) 0.076(6) 0.026(3) -0.009(4) -0.005(3) 0.004(4) C5 0.023(3) 0.054(5) 0.031(4) 0.005(3) -0.003(3) 0.006(3) C6 0.022(3) 0.040(4) 0.030(4) 0.000(3) 0.000(3) 0.003(3) C7 0.028(3) 0.027(3) 0.022(3) 0.003(2) 0.001(2) -0.004(3) C8 0.043(4) 0.039(4) 0.038(4) -0.018(3) 0.016(3) -0.018(3) C9 0.047(4) 0.040(4) 0.042(4) -0.014(3) 0.005(3) -0.016(3) C10 0.028(3) 0.031(3) 0.052(4) 0.000(3) -0.003(3) -0.007(3) C11 0.022(3) 0.029(3) 0.045(4) 0.006(3) 0.003(3) -0.006(3) C12 0.026(3) 0.028(3) 0.030(3) 0.000(3) 0.006(3) -0.006(3) C13 0.022(3) 0.023(3) 0.023(3) -0.005(2) 0.005(2) -0.003(2) C14 0.028(3) 0.027(3) 0.025(3) 0.002(3) 0.001(3) -0.003(2) C15 0.040(3) 0.027(3) 0.033(4) 0.008(3) -0.002(3) -0.010(3) C16 0.033(4) 0.026(3) 0.056(5) 0.007(3) -0.001(3) -0.002(3) C17 0.041(4) 0.024(3) 0.057(5) -0.005(3) 0.009(3) 0.002(3) C18 0.029(3) 0.025(3) 0.038(4) -0.004(3) 0.009(3) 0.001(3) C19 0.028(3) 0.042(4) 0.051(4) 0.018(3) -0.007(3) -0.006(3) C20 0.034(3) 0.023(3) 0.036(4) 0.008(3) 0.010(3) 0.000(3) C21 0.057(5) 0.038(4) 0.073(6) 0.022(4) -0.008(4) -0.009(4) C22 0.090(7) 0.062(6) 0.067(6) 0.036(5) -0.015(5) -0.008(5) C23 0.056(5) 0.064(5) 0.067(6) 0.036(5) -0.033(4) -0.010(4) C24 0.065(6) 0.100(8) 0.101(8) 0.075(7) -0.050(6) -0.040(6) C25 0.033(4) 0.045(4) 0.050(4) -0.022(4) 0.019(3) -0.007(3) C26 0.030(3) 0.045(4) 0.038(4) -0.011(3) 0.015(3) -0.002(3) C27 0.068(6) 0.079(7) 0.118(9) -0.060(6) 0.057(6) -0.011(5) C28 0.063(6) 0.081(7) 0.069(6) -0.034(5) 0.012(5) 0.015(5) C29 0.049(4) 0.032(4) 0.054(5) -0.020(3) -0.003(4) 0.003(3) C30 0.041(5) 0.053(5) 0.090(7) -0.041(5) 0.024(4) -0.010(4) C31 0.021(3) 0.024(3) 0.031(3) 0.002(3) 0.006(3) -0.001(2) C32 0.041(3) 0.018(3) 0.036(4) 0.000(3) -0.009(3) 0.001(2) C33 0.058(5) 0.031(4) 0.045(4) 0.002(3) -0.010(4) -0.018(3) C34 0.046(4) 0.047(4) 0.041(4) 0.014(3) -0.013(3) -0.022(4) C35 0.026(3) 0.059(5) 0.053(4) 0.029(4) -0.007(3) -0.001(3) C36 0.030(3) 0.023(3) 0.039(4) 0.007(3) 0.005(3) 0.007(2) C37 0.026(3) 0.019(3) 0.030(4) 0.001(2) -0.003(2) -0.001(2) C38 0.026(3) 0.029(3) 0.034(4) -0.001(3) -0.004(3) -0.003(3) C39 0.025(3) 0.030(3) 0.052(5) -0.005(3) -0.007(3) -0.001(2) C40 0.027(3) 0.033(3) 0.052(4) 0.001(4) -0.001(4) 0.005(2) C41 0.032(3) 0.019(3) 0.049(4) -0.001(3) 0.003(3) 0.002(3) C42 0.027(3) 0.019(3) 0.041(3) 0.000(2) 0.001(3) 0.000(2) C43 0.027(4) 0.019(3) 0.024(3) 0.003(2) -0.005(3) -0.005(3) C44 0.027(3) 0.023(3) 0.031(4) 0.003(3) -0.002(3) -0.003(3) C45 0.046(4) 0.037(4) 0.024(4) -0.006(3) -0.007(3) -0.001(3) C46 0.040(4) 0.040(4) 0.033(4) 0.002(3) -0.014(3) -0.009(3) C47 0.032(3) 0.041(4) 0.039(4) 0.004(3) -0.012(3) -0.010(3) C48 0.026(3) 0.034(3) 0.030(3) -0.001(3) -0.008(3) -0.002(3) C49 0.029(3) 0.022(3) 0.024(3) 0.003(3) 0.001(3) -0.001(3) C50 0.025(3) 0.031(3) 0.036(4) 0.004(3) 0.001(3) 0.000(3) C51 0.028(3) 0.031(4) 0.047(4) 0.008(3) 0.005(3) -0.001(3) C52 0.046(4) 0.051(4) 0.034(4) 0.007(4) 0.014(3) -0.003(3) C53 0.048(4) 0.044(4) 0.035(4) 0.005(3) 0.002(3) -0.006(3) C54 0.035(3) 0.026(3) 0.028(3) -0.001(3) 0.002(3) -0.002(3) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Br1 La1 Br2 172.59(2) Br1 La1 Br3 91.39(3) Br2 La1 Br3 95.84(3) O1 La1 Br1 91.08(10) O1 La1 Br2 90.73(10) O1 La1 Br3 88.27(9) O1 La1 O2 178.16(13) O1 La1 O3 91.97(14) O2 La1 Br1 89.62(10) O2 La1 Br2 88.79(10) O2 La1 Br3 90.01(10) O2 La1 O3 89.78(14) O3 La1 Br1 85.23(12) O3 La1 Br2 87.53(12) O3 La1 Br3 176.61(12) O1 P1 C1 109.5(2) O1 P1 C7 110.0(2) O1 P1 C13 108.9(2) C1 P1 C7 110.5(3) C13 P1 C1 109.6(3) C13 P1 C7 108.4(3) O2 P2 C19 109.1(3) O2 P2 C25 107.5(3) O2 P2 C31 110.3(3) C19 P2 C25 115.9(4) C31 P2 C19 106.6(3) C31 P2 C25 107.3(3) O3 P3 C37 109.3(2) O3 P3 C43 109.2(3) O3 P3 C49 111.2(3) C37 P3 C49 106.6(3) C43 P3 C37 108.1(3) C43 P3 C49 112.3(3) P1 O1 La1 166.3(2) P2 O2 La1 160.7(2) P3 O3 La1 170.9(3) P1 C1 H1 108.6 C2 C1 P1 111.5(4) C2 C1 H1 108.6 C2 C1 C6 109.7(5) C6 C1 P1 109.7(4) C6 C1 H1 108.6 C1 C2 H2A 109.7 C1 C2 H2B 109.7 H2A C2 H2B 108.2 C3 C2 C1 109.9(5) C3 C2 H2A 109.7 C3 C2 H2B 109.7 C2 C3 H3A 109.2 C2 C3 H3B 109.2 H3A C3 H3B 107.9 C4 C3 C2 112.0(5) C4 C3 H3A 109.2 C4 C3 H3B 109.2 C3 C4 H4A 109.3 C3 C4 H4B 109.3 C3 C4 C5 111.5(6) H4A C4 H4B 108.0 C5 C4 H4A 109.3 C5 C4 H4B 109.3 C4 C5 H5A 109.7 C4 C5 H5B 109.7 C4 C5 C6 109.9(6) H5A C5 H5B 108.2 C6 C5 H5A 109.7 C6 C5 H5B 109.7 C1 C6 H6A 109.5 C1 C6 H6B 109.5 C5 C6 C1 110.9(5) C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 108.1 P1 C7 H7 106.3 C8 C7 P1 110.2(4) C8 C7 H7 106.3 C12 C7 P1 115.0(4) C12 C7 H7 106.3 C12 C7 C8 112.1(5) C7 C8 H8A 109.3 C7 C8 H8B 109.3 H8A C8 H8B 108.0 C9 C8 C7 111.5(5) C9 C8 H8A 109.3 C9 C8 H8B 109.3 C8 C9 H9A 109.2 C8 C9 H9B 109.2 H9A C9 H9B 107.9 C10 C9 C8 111.9(5) C10 C9 H9A 109.2 C10 C9 H9B 109.2 C9 C10 H10A 109.6 C9 C10 H10B 109.6 H10A C10 H10B 108.1 C11 C10 C9 110.5(5) C11 C10 H10A 109.6 C11 C10 H10B 109.6 C10 C11 H11A 109.2 C10 C11 H11B 109.2 C10 C11 C12 111.9(5) H11A C11 H11B 107.9 C12 C11 H11A 109.2 C12 C11 H11B 109.2 C7 C12 C11 112.0(5) C7 C12 H12A 109.2 C7 C12 H12B 109.2 C11 C12 H12A 109.2 C11 C12 H12B 109.2 H12A C12 H12B 107.9 P1 C13 H13 106.3 C14 C13 P1 111.6(4) C14 C13 H13 106.3 C18 C13 P1 115.2(4) C18 C13 H13 106.3 C18 C13 C14 110.5(5) C13 C14 H14A 109.6 C13 C14 H14B 109.6 H14A C14 H14B 108.1 C15 C14 C13 110.3(5) C15 C14 H14A 109.6 C15 C14 H14B 109.6 C14 C15 H15A 109.3 C14 C15 H15B 109.3 H15A C15 H15B 108.0 C16 C15 C14 111.5(5) C16 C15 H15A 109.3 C16 C15 H15B 109.3 C15 C16 H16A 109.2 C15 C16 H16B 109.2 H16A C16 H16B 107.9 C17 C16 C15 112.2(5) C17 C16 H16A 109.2 C17 C16 H16B 109.2 C16 C17 H17A 109.2 C16 C17 H17B 109.2 C16 C17 C18 111.8(5) H17A C17 H17B 107.9 C18 C17 H17A 109.2 C18 C17 H17B 109.2 C13 C18 C17 111.0(5) C13 C18 H18A 109.4 C13 C18 H18B 109.4 C17 C18 H18A 109.4 C17 C18 H18B 109.4 H18A C18 H18B 108.0 P2 C19 H19 102.9 C20 C19 P2 116.4(4) C20 C19 H19 102.9 C24 C19 P2 114.8(5) C24 C19 H19 102.9 C24 C19 C20 114.4(6) C19 C20 H20A 109.3 C19 C20 H20B 109.3 C19 C20 C21 111.7(6) H20A C20 H20B 107.9 C21 C20 H20A 109.3 C21 C20 H20B 109.3 C20 C21 H21A 108.4 C20 C21 H21B 108.4 H21A C21 H21B 107.5 C22 C21 C20 115.4(7) C22 C21 H21A 108.4 C22 C21 H21B 108.4 C21 C22 H22A 108.5 C21 C22 H22B 108.5 C21 C22 C23 115.2(7) H22A C22 H22B 107.5 C23 C22 H22A 108.5 C23 C22 H22B 108.5 C22 C23 H23A 108.6 C22 C23 H23B 108.6 C22 C23 C24 114.5(7) H23A C23 H23B 107.6 C24 C23 H23A 108.6 C24 C23 H23B 108.6 C19 C24 C23 114.6(7) C19 C24 H24A 108.6 C19 C24 H24B 108.6 C23 C24 H24A 108.6 C23 C24 H24B 108.6 H24A C24 H24B 107.6 P2 C25 H25 102.4 C26 C25 P2 115.0(5) C26 C25 H25 102.4 C30 C25 P2 116.7(5) C30 C25 H25 102.4 C30 C25 C26 115.0(6) C25 C26 H26A 109.1 C25 C26 H26B 109.1 H26A C26 H26B 107.8 C27 C26 C25 112.7(6) C27 C26 H26A 109.1 C27 C26 H26B 109.1 C26 C27 H27A 107.8 C26 C27 H27B 107.8 H27A C27 H27B 107.2 C28 C27 C26 117.9(8) C28 C27 H27A 107.8 C28 C27 H27B 107.8 C27 C28 H28A 108.0 C27 C28 H28B 108.0 C27 C28 C29 117.0(7) H28A C28 H28B 107.3 C29 C28 H28A 108.0 C29 C28 H28B 108.0 C28 C29 H29A 109.0 C28 C29 H29B 109.0 H29A C29 H29B 107.8 C30 C29 C28 113.0(7) C30 C29 H29A 109.0 C30 C29 H29B 109.0 C25 C30 C29 115.6(7) C25 C30 H30A 108.4 C25 C30 H30B 108.4 C29 C30 H30A 108.4 C29 C30 H30B 108.4 H30A C30 H30B 107.4 P2 C31 H31 108.7 C32 C31 P2 110.3(4) C32 C31 H31 108.7 C32 C31 C36 108.4(5) C36 C31 P2 112.0(4) C36 C31 H31 108.7 C31 C32 H32A 109.3 C31 C32 H32B 109.3 H32A C32 H32B 108.0 C33 C32 C31 111.6(5) C33 C32 H32A 109.3 C33 C32 H32B 109.3 C32 C33 H33A 109.8 C32 C33 H33B 109.8 C32 C33 C34 109.5(5) H33A C33 H33B 108.2 C34 C33 H33A 109.8 C34 C33 H33B 109.8 C33 C34 H34A 109.8 C33 C34 H34B 109.8 H34A C34 H34B 108.2 C35 C34 C33 109.6(6) C35 C34 H34A 109.8 C35 C34 H34B 109.8 C34 C35 H35A 109.4 C34 C35 H35B 109.4 H35A C35 H35B 108.0 C36 C35 C34 111.4(5) C36 C35 H35A 109.4 C36 C35 H35B 109.4 C31 C36 H36A 109.1 C31 C36 H36B 109.1 C35 C36 C31 112.6(5) C35 C36 H36A 109.1 C35 C36 H36B 109.1 H36A C36 H36B 107.8 P3 C37 H37 105.7 C38 C37 P3 113.2(4) C38 C37 H37 105.7 C38 C37 C42 110.8(5) C42 C37 P3 114.8(4) C42 C37 H37 105.7 C37 C38 H38A 109.5 C37 C38 H38B 109.5 C37 C38 C39 110.6(5) H38A C38 H38B 108.1 C39 C38 H38A 109.5 C39 C38 H38B 109.5 C38 C39 H39A 109.3 C38 C39 H39B 109.3 H39A C39 H39B 107.9 C40 C39 C38 111.7(5) C40 C39 H39A 109.3 C40 C39 H39B 109.3 C39 C40 H40A 109.7 C39 C40 H40B 109.7 C39 C40 C41 110.0(5) H40A C40 H40B 108.2 C41 C40 H40A 109.7 C41 C40 H40B 109.7 C40 C41 H41A 109.5 C40 C41 H41B 109.5 C40 C41 C42 110.9(5) H41A C41 H41B 108.0 C42 C41 H41A 109.5 C42 C41 H41B 109.5 C37 C42 C41 109.4(5) C37 C42 H42A 109.8 C37 C42 H42B 109.8 C41 C42 H42A 109.8 C41 C42 H42B 109.8 H42A C42 H42B 108.2 P3 C43 H43 108.7 C44 C43 P3 111.3(4) C44 C43 H43 108.7 C44 C43 C48 109.0(5) C48 C43 P3 110.4(4) C48 C43 H43 108.7 C43 C44 H44A 109.3 C43 C44 H44B 109.3 H44A C44 H44B 108.0 C45 C44 C43 111.5(5) C45 C44 H44A 109.3 C45 C44 H44B 109.3 C44 C45 H45A 109.4 C44 C45 H45B 109.4 H45A C45 H45B 108.0 C46 C45 C44 111.3(5) C46 C45 H45A 109.4 C46 C45 H45B 109.4 C45 C46 H46A 109.5 C45 C46 H46B 109.5 H46A C46 H46B 108.1 C47 C46 C45 110.8(5) C47 C46 H46A 109.5 C47 C46 H46B 109.5 C46 C47 H47A 109.4 C46 C47 H47B 109.4 C46 C47 C48 111.4(5) H47A C47 H47B 108.0 C48 C47 H47A 109.4 C48 C47 H47B 109.4 C43 C48 H48A 109.2 C43 C48 H48B 109.2 C47 C48 C43 112.0(5) C47 C48 H48A 109.2 C47 C48 H48B 109.2 H48A C48 H48B 107.9 P3 C49 H49 106.4 C50 C49 P3 117.3(4) C50 C49 H49 106.4 C54 C49 P3 109.6(4) C54 C49 H49 106.4 C54 C49 C50 110.0(5) C49 C50 H50A 109.6 C49 C50 H50B 109.6 H50A C50 H50B 108.1 C51 C50 C49 110.1(5) C51 C50 H50A 109.6 C51 C50 H50B 109.6 C50 C51 H51A 109.1 C50 C51 H51B 109.1 H51A C51 H51B 107.9 C52 C51 C50 112.3(5) C52 C51 H51A 109.1 C52 C51 H51B 109.1 C51 C52 H52A 109.4 C51 C52 H52B 109.4 H52A C52 H52B 108.0 C53 C52 C51 111.4(6) C53 C52 H52A 109.4 C53 C52 H52B 109.4 C52 C53 H53A 109.3 C52 C53 H53B 109.3 H53A C53 H53B 108.0 C54 C53 C52 111.5(6) C54 C53 H53A 109.3 C54 C53 H53B 109.3 C49 C54 H54A 109.2 C49 C54 H54B 109.2 C53 C54 C49 112.1(5) C53 C54 H54A 109.2 C53 C54 H54B 109.2 H54A C54 H54B 107.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance La1 Br1 2.9365(7) La1 Br2 2.9425(7) La1 Br3 2.9649(5) La1 O1 2.351(4) La1 O2 2.363(4) La1 O3 2.382(3) P1 O1 1.511(4) P1 C1 1.816(5) P1 C7 1.832(6) P1 C13 1.803(6) P2 O2 1.513(4) P2 C19 1.806(7) P2 C25 1.814(6) P2 C31 1.802(6) P3 O3 1.513(3) P3 C37 1.828(5) P3 C43 1.817(6) P3 C49 1.830(6) C1 H1 1.0000 C1 C2 1.538(8) C1 C6 1.539(8) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.534(9) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.499(10) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.516(10) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.535(8) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7 1.0000 C7 C8 1.526(8) C7 C12 1.519(8) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.521(8) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.509(9) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.506(9) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.539(8) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13 1.0000 C13 C14 1.536(8) C13 C18 1.532(7) C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.527(7) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.519(9) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.511(10) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.536(8) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19 1.0000 C19 C20 1.517(8) C19 C24 1.450(10) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.541(9) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.432(11) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.488(11) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.498(11) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25 1.0000 C25 C26 1.512(8) C25 C30 1.449(10) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.498(9) C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.419(12) C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.502(11) C29 H29A 0.9900 C29 H29B 0.9900 C29 C30 1.494(9) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31 1.0000 C31 C32 1.533(8) C31 C36 1.537(8) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.517(9) C33 H33A 0.9900 C33 H33B 0.9900 C33 C34 1.527(9) C34 H34A 0.9900 C34 H34B 0.9900 C34 C35 1.519(10) C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.515(9) C36 H36A 0.9900 C36 H36B 0.9900 C37 H37 1.0000 C37 C38 1.525(8) C37 C42 1.533(7) C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.538(8) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.518(8) C40 H40A 0.9900 C40 H40B 0.9900 C40 C41 1.523(9) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.541(8) C42 H42A 0.9900 C42 H42B 0.9900 C43 H43 1.0000 C43 C44 1.531(8) C43 C48 1.541(8) C44 H44A 0.9900 C44 H44B 0.9900 C44 C45 1.527(8) C45 H45A 0.9900 C45 H45B 0.9900 C45 C46 1.517(9) C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.509(9) C47 H47A 0.9900 C47 H47B 0.9900 C47 C48 1.525(8) C48 H48A 0.9900 C48 H48B 0.9900 C49 H49 1.0000 C49 C50 1.530(8) C49 C54 1.526(8) C50 H50A 0.9900 C50 H50B 0.9900 C50 C51 1.526(9) C51 H51A 0.9900 C51 H51B 0.9900 C51 C52 1.523(10) C52 H52A 0.9900 C52 H52B 0.9900 C52 C53 1.520(9) C53 H53A 0.9900 C53 H53B 0.9900 C53 C54 1.516(9) C54 H54A 0.9900 C54 H54B 0.9900 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.982(9) 2 0.018(9)