#------------------------------------------------------------------------------ #$Date: 2020-02-06 04:02:28 +0200 (Thu, 06 Feb 2020) $ #$Revision: 247904 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557255.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_1557255 loop_ _publ_author_name 'Windorff, Cory J.' 'Celis-Barros, Cristian' 'Sperling, Joseph M.' 'McKinnon, Noah C.' 'Albrecht-Schmitt, Thomas' _publ_section_title ; Probing a variation of the inverse-trans-influence in americium and lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC05268B _journal_year 2020 _chemical_formula_moiety 'C54 H99 Br3 Ce O3 P3' _chemical_formula_sum 'C54 H99 Br3 Ce O3 P3' _chemical_formula_weight 1269.09 _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 2019-05-29 _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 28.920(5) _cell_length_b 11.434(2) _cell_length_c 18.209(3) _cell_measurement_reflns_used 9514 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.438 _cell_measurement_theta_min 2.531 _cell_volume 6021.2(18) _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 120(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _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 0.0685 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _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 -23 _diffrn_reflns_number 122286 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.511 _diffrn_reflns_theta_min 2.218 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.864 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6448 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0972 before and 0.0803 after correction. The Ratio of minimum to maximum transmission is 0.8648. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.400 _exptl_crystal_description block _exptl_crystal_F_000 2620 _exptl_crystal_preparation 'mixture of components in isopropyl alcohol' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: iPrOH' _exptl_crystal_size_max 0.268 _exptl_crystal_size_mid 0.156 _exptl_crystal_size_min 0.123 _refine_diff_density_max 0.956 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.095 _refine_ls_abs_structure_details ; Flack x determined using 5009 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.001(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 13805 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0353 _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^)+(0.0145P)^2^+11.2182P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.0726 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 11775 _reflns_number_total 13805 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05268b2.cif _cod_data_source_block 'save_b_CCDC1' _cod_database_code 1557255 _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 0.720 _shelx_estimated_absorpt_t_min 0.514 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.964(10) 0.036(10) 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: C25(H25), C19(H19), C7(H7), C1(H1), C13(H13), C31(H31), C37(H37), C43(H43), C49(H49) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C30(H30A,H30B), C44(H44A,H44B), C48(H48A,H48B), C36(H36A,H36B), C17(H17A,H17B), C3(H3A,H3B), C27(H27A,H27B), C26(H26A,H26B), C21(H21A,H21B), C32(H32A,H32B), C9(H9A,H9B), C8(H8A,H8B), C15(H15A,H15B), C14(H14A,H14B), C20(H20A,H20B), C28(H28A,H28B), C12(H12A,H12B), C29(H29A,H29B), C35(H35A,H35B), C46(H46A,H46B), C5(H5A,H5B), C22(H22A,H22B), C18(H18A,H18B), C10(H10A,H10B), C50(H50A,H50B), C4(H4A,H4B), C6(H6A,H6B), C16(H16A,H16B), C47(H47A,H47B), C0AA(H0AA,H0AB), C45(H45A,H45B), C23(H23A,H23B), C41(H41A,H41B), C42(H42A, H42B), C24(H24A,H24B), C11(H11A,H11B), C38(H38A,H38B), C52(H52A,H52B), C34(H34A,H34B), C39(H39A,H39B), C40(H40A,H40B), C51(H51A,H51B), C53(H53A,H53B), C33(H33A,H33B) ; _shelx_res_file ; TITL save_b.res in Pca2(1) save_b.res created by SHELXL-2016/6 at 14:27:11 on 29-May-2019 REM Old TITL save in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.110, Rweak 0.010, Alpha 0.019, Orientation as input REM Flack x = 0.093 ( 0.004 ) from Parsons' quotients REM Formula found by SHELXT: C50 O10 P3 Br3 Ce CELL 0.71073 28.9195 11.4343 18.209 90 90 90 ZERR 4 0.0052 0.002 0.003 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 Br Ce O P UNIT 216 396 12 4 12 12 L.S. 10 PLAN 10 SIZE 0.123 0.156 0.268 TEMP -153(2) BOND $H LIST 6 acta fmap 2 TWIN -1 0 0 0 1 0 0 0 -1 2 OMIT 26 0 -13 OMIT 26 0 13 REM REM REM WGHT 0.014500 11.218201 BASF 0.03608 FVAR 0.17668 CE1 4 0.626873 0.417103 0.480300 11.00000 0.01583 0.01837 = 0.01391 -0.00034 -0.00068 0.00156 BR1 3 0.684504 0.389935 0.349277 11.00000 0.03175 0.04379 = 0.02284 0.00013 0.01011 0.00305 BR3 3 0.567013 0.412745 0.609181 11.00000 0.03574 0.04439 = 0.02252 0.00337 0.01174 0.00889 BR2 3 0.627810 0.675119 0.479193 11.00000 0.03729 0.01907 = 0.06409 0.00105 -0.00911 0.00174 P1 6 0.734843 0.456930 0.598678 11.00000 0.02155 0.02282 = 0.01847 -0.00143 -0.00505 0.00274 P2 6 0.612754 0.080378 0.485174 11.00000 0.02711 0.01981 = 0.02723 0.00045 0.00297 0.00108 P3 6 0.521450 0.465650 0.358923 11.00000 0.02057 0.02398 = 0.02430 -0.00161 -0.00723 -0.00021 O1 5 0.692670 0.422333 0.554242 11.00000 0.02269 0.03117 = 0.01504 -0.00077 -0.00881 -0.00029 O2 5 0.622911 0.210389 0.485630 11.00000 0.02480 0.02951 = 0.02954 0.00529 0.00159 -0.00139 O3 5 0.561493 0.419860 0.405001 11.00000 0.02059 0.03045 = 0.02492 -0.00274 -0.00436 0.00214 C2 1 0.761718 0.610732 0.488708 11.00000 0.02522 0.02842 = 0.03006 0.00183 -0.00457 0.00247 AFIX 23 H2A 2 0.788885 0.562190 0.475852 11.00000 -1.20000 H2B 2 0.734658 0.580142 0.461505 11.00000 -1.20000 AFIX 0 C25 1 0.551408 0.056716 0.465091 11.00000 0.03072 0.02448 = 0.03415 0.00161 0.00164 -0.00060 AFIX 13 H25 2 0.545121 0.100863 0.418747 11.00000 -1.20000 AFIX 0 C19 1 0.646738 0.011303 0.412236 11.00000 0.03115 0.01800 = 0.02944 -0.00138 0.00384 0.00381 AFIX 13 H19 2 0.645401 -0.075489 0.418649 11.00000 -1.20000 AFIX 0 C30 1 0.537741 -0.070281 0.449009 11.00000 0.03195 0.02528 = 0.03919 0.00108 -0.00205 0.00321 AFIX 23 H30A 2 0.542068 -0.118413 0.493677 11.00000 -1.20000 H30B 2 0.557814 -0.102327 0.409834 11.00000 -1.20000 AFIX 0 C7 1 0.783002 0.355458 0.579020 11.00000 0.03078 0.02462 = 0.02379 0.00104 -0.00179 0.00604 AFIX 13 H7 2 0.804684 0.398810 0.546018 11.00000 -1.20000 AFIX 0 C44 1 0.487802 0.599854 0.472466 11.00000 0.04757 0.02261 = 0.03695 0.00288 0.01408 0.00305 AFIX 23 H44A 2 0.513694 0.570716 0.502965 11.00000 -1.20000 H44B 2 0.498760 0.669582 0.445339 11.00000 -1.20000 AFIX 0 C48 1 0.454327 0.398003 0.460027 11.00000 0.03692 0.02806 = 0.03924 0.00685 -0.00573 -0.00780 AFIX 23 H48A 2 0.442101 0.340011 0.424632 11.00000 -1.20000 H48B 2 0.479817 0.360573 0.487680 11.00000 -1.20000 AFIX 0 C1 1 0.752582 0.602632 0.571808 11.00000 0.02537 0.02789 = 0.02336 -0.00303 -0.00431 0.00521 AFIX 13 H1 2 0.725660 0.655047 0.582027 11.00000 -1.20000 AFIX 0 C13 1 0.720591 0.454346 0.695798 11.00000 0.02292 0.03513 = 0.01325 -0.00457 -0.00548 0.00046 AFIX 13 H13 2 0.749944 0.460222 0.724592 11.00000 -1.20000 AFIX 0 C36 1 0.670645 -0.046561 0.586182 11.00000 0.03166 0.03282 = 0.04410 0.00549 0.00034 0.00238 AFIX 23 H36A 2 0.675084 -0.107555 0.548244 11.00000 -1.20000 H36B 2 0.695783 0.011614 0.580928 11.00000 -1.20000 AFIX 0 C31 1 0.623667 0.013668 0.574634 11.00000 0.03284 0.02727 = 0.02937 0.00268 0.00024 0.00115 AFIX 13 H31 2 0.599510 -0.047950 0.581476 11.00000 -1.20000 AFIX 0 C17 1 0.685000 0.333329 0.798128 11.00000 0.03472 0.05439 = 0.03288 0.00299 0.00450 -0.00533 AFIX 23 H17A 2 0.668657 0.259266 0.809050 11.00000 -1.20000 H17B 2 0.713862 0.335127 0.827342 11.00000 -1.20000 AFIX 0 C3 1 0.770680 0.738232 0.466187 11.00000 0.03864 0.02621 = 0.03865 0.00632 0.00089 0.00669 AFIX 23 H3A 2 0.777904 0.741426 0.413080 11.00000 -1.20000 H3B 2 0.742390 0.785029 0.474774 11.00000 -1.20000 AFIX 0 C27 1 0.468362 0.100853 0.499383 11.00000 0.02704 0.03835 = 0.05333 -0.00611 0.00773 0.00019 AFIX 23 H27A 2 0.448297 0.131314 0.539063 11.00000 -1.20000 H27B 2 0.463394 0.149875 0.455268 11.00000 -1.20000 AFIX 0 C26 1 0.519058 0.110024 0.523223 11.00000 0.02702 0.03064 = 0.04241 -0.00388 0.00309 0.00106 AFIX 23 H26A 2 0.523320 0.068566 0.570471 11.00000 -1.20000 H26B 2 0.527187 0.193256 0.530812 11.00000 -1.20000 AFIX 0 C21 1 0.655902 -0.011142 0.274714 11.00000 0.04781 0.04184 = 0.02992 -0.00263 0.00772 0.00304 AFIX 23 H21A 2 0.654477 -0.097476 0.278150 11.00000 -1.20000 H21B 2 0.642983 0.012204 0.226547 11.00000 -1.20000 AFIX 0 C32 1 0.615572 0.105334 0.635083 11.00000 0.04349 0.03406 = 0.02878 0.00122 -0.00164 0.00087 AFIX 23 H32A 2 0.639040 0.167964 0.630602 11.00000 -1.20000 H32B 2 0.584715 0.141213 0.628247 11.00000 -1.20000 AFIX 0 C9 1 0.849360 0.231516 0.626835 11.00000 0.02165 0.03444 = 0.04811 0.00719 -0.00121 0.00674 AFIX 23 H9A 2 0.873147 0.270987 0.596596 11.00000 -1.20000 H9B 2 0.864446 0.203883 0.672451 11.00000 -1.20000 AFIX 0 C8 1 0.811362 0.320417 0.646851 11.00000 0.02587 0.02944 = 0.03379 0.00178 -0.00613 0.00515 AFIX 23 H8A 2 0.790564 0.285787 0.684160 11.00000 -1.20000 H8B 2 0.825771 0.391010 0.668465 11.00000 -1.20000 AFIX 0 C15 1 0.676735 0.551986 0.799304 11.00000 0.04221 0.05926 = 0.03038 -0.01625 0.00361 0.00273 AFIX 23 H15A 2 0.705151 0.562500 0.828895 11.00000 -1.20000 H15B 2 0.655203 0.616306 0.811762 11.00000 -1.20000 AFIX 0 C14 1 0.689238 0.559362 0.716496 11.00000 0.03677 0.03551 = 0.02701 -0.00827 -0.00165 0.00722 AFIX 23 H14A 2 0.660667 0.557688 0.686566 11.00000 -1.20000 H14B 2 0.705622 0.633649 0.706356 11.00000 -1.20000 AFIX 0 C20 1 0.626689 0.042867 0.336391 11.00000 0.03945 0.02922 = 0.03020 0.00169 0.00233 0.00506 AFIX 23 H20A 2 0.594528 0.013750 0.332818 11.00000 -1.20000 H20B 2 0.626055 0.128958 0.330703 11.00000 -1.20000 AFIX 0 C28 1 0.454721 -0.024641 0.482222 11.00000 0.03578 0.03451 = 0.05554 0.00115 -0.00068 -0.00585 AFIX 23 H28A 2 0.456334 -0.072297 0.527542 11.00000 -1.20000 H28B 2 0.422490 -0.026710 0.463946 11.00000 -1.20000 AFIX 0 C12 1 0.765862 0.251060 0.535121 11.00000 0.05191 0.03766 = 0.03624 -0.01488 -0.01080 0.01733 AFIX 23 H12A 2 0.751499 0.278871 0.488963 11.00000 -1.20000 H12B 2 0.741917 0.209199 0.563734 11.00000 -1.20000 AFIX 0 C29 1 0.486953 -0.075616 0.424547 11.00000 0.03617 0.02542 = 0.05200 0.00066 0.00001 -0.00388 AFIX 23 H29A 2 0.483291 -0.031624 0.378082 11.00000 -1.20000 H29B 2 0.478299 -0.158021 0.415095 11.00000 -1.20000 AFIX 0 C35 1 0.673009 -0.102246 0.662469 11.00000 0.03932 0.03491 = 0.04558 0.00796 -0.00505 0.00293 AFIX 23 H35A 2 0.703995 -0.137203 0.669699 11.00000 -1.20000 H35B 2 0.649864 -0.165836 0.665688 11.00000 -1.20000 AFIX 0 C37 1 0.539261 0.597955 0.312419 11.00000 0.02904 0.03376 = 0.03518 0.00893 -0.00183 0.00408 AFIX 13 H37 2 0.550743 0.649329 0.352950 11.00000 -1.20000 AFIX 0 C43 1 0.473474 0.504646 0.417421 11.00000 0.02378 0.02976 = 0.03233 0.00502 -0.00616 0.00506 AFIX 13 H43 2 0.448152 0.536573 0.385850 11.00000 -1.20000 AFIX 0 C46 1 0.430930 0.527900 0.565090 11.00000 0.04847 0.05797 = 0.04603 0.02146 0.01765 0.02494 AFIX 23 H46A 2 0.456106 0.498884 0.597110 11.00000 -1.20000 H46B 2 0.404565 0.550548 0.596717 11.00000 -1.20000 AFIX 0 C5 1 0.803615 0.779185 0.591493 11.00000 0.04051 0.02993 = 0.05715 -0.00484 -0.00843 -0.00378 AFIX 23 H5A 2 0.777521 0.829618 0.606838 11.00000 -1.20000 H5B 2 0.831780 0.807310 0.616851 11.00000 -1.20000 AFIX 0 C22 1 0.706106 0.028420 0.279666 11.00000 0.04394 0.04286 = 0.03975 0.00399 0.01252 0.00906 AFIX 23 H22A 2 0.724397 -0.010203 0.240629 11.00000 -1.20000 H22B 2 0.707875 0.113993 0.271882 11.00000 -1.20000 AFIX 0 C18 1 0.696718 0.339096 0.715658 11.00000 0.02426 0.04075 = 0.03306 0.00166 0.00227 -0.00236 AFIX 23 H18A 2 0.717248 0.272945 0.702726 11.00000 -1.20000 H18B 2 0.667926 0.331279 0.686658 11.00000 -1.20000 AFIX 0 C10 1 0.830800 0.127208 0.585079 11.00000 0.03418 0.03212 = 0.05728 -0.00183 -0.00008 0.00868 AFIX 23 H10A 2 0.809670 0.081957 0.617052 11.00000 -1.20000 H10B 2 0.856715 0.075508 0.570658 11.00000 -1.20000 AFIX 0 C50 1 0.459567 0.372306 0.255007 11.00000 0.03656 0.04518 = 0.04401 -0.01063 -0.02216 -0.00010 AFIX 23 H50A 2 0.465876 0.439366 0.222108 11.00000 -1.20000 H50B 2 0.434346 0.395507 0.288758 11.00000 -1.20000 AFIX 0 C4 1 0.810364 0.790554 0.509227 11.00000 0.04017 0.02362 = 0.05498 0.00753 0.00097 -0.00190 AFIX 23 H4A 2 0.813410 0.874333 0.496386 11.00000 -1.20000 H4B 2 0.839442 0.750835 0.495043 11.00000 -1.20000 AFIX 0 C6 1 0.793802 0.653444 0.615155 11.00000 0.02929 0.02894 = 0.03519 -0.00196 -0.00920 -0.00176 AFIX 23 H6A 2 0.786769 0.651631 0.668352 11.00000 -1.20000 H6B 2 0.821581 0.604747 0.606525 11.00000 -1.20000 AFIX 0 C16 1 0.654598 0.436446 0.819004 11.00000 0.03965 0.08290 = 0.02790 -0.00988 0.00676 -0.00344 AFIX 23 H16A 2 0.624527 0.429614 0.793379 11.00000 -1.20000 H16B 2 0.648581 0.434351 0.872510 11.00000 -1.20000 AFIX 0 C47 1 0.416146 0.432553 0.513195 11.00000 0.02661 0.07325 = 0.05452 0.03679 0.00226 -0.00244 AFIX 23 H47A 2 0.388910 0.459463 0.484924 11.00000 -1.20000 H47B 2 0.406757 0.363029 0.541964 11.00000 -1.20000 AFIX 0 C0AA 1 0.447727 0.634258 0.521935 11.00000 0.06096 0.04055 = 0.04411 0.00941 0.01802 0.02270 AFIX 23 H0AA 2 0.422096 0.665741 0.491802 11.00000 -1.20000 H0AB 2 0.457800 0.696161 0.556417 11.00000 -1.20000 AFIX 0 C45 1 0.537748 0.277617 0.264366 11.00000 0.05026 0.06097 = 0.10051 -0.04326 -0.03008 0.01281 AFIX 23 H45A 2 0.559389 0.249901 0.302728 11.00000 -1.20000 H45B 2 0.555433 0.328789 0.230683 11.00000 -1.20000 AFIX 0 C23 1 0.726284 -0.001919 0.354113 11.00000 0.03921 0.04774 = 0.03391 0.00303 0.00771 0.01434 AFIX 23 H23A 2 0.758309 0.028253 0.357296 11.00000 -1.20000 H23B 2 0.727413 -0.087989 0.359739 11.00000 -1.20000 AFIX 0 C41 1 0.519079 0.783959 0.244082 11.00000 0.05849 0.03315 = 0.05790 0.01059 -0.00019 0.00266 AFIX 23 H41A 2 0.494342 0.820918 0.214521 11.00000 -1.20000 H41B 2 0.526822 0.838058 0.284710 11.00000 -1.20000 AFIX 0 C42 1 0.500471 0.669781 0.276795 11.00000 0.03964 0.02869 = 0.03946 0.00583 -0.01295 0.00102 AFIX 23 H42A 2 0.485688 0.622971 0.237545 11.00000 -1.20000 H42B 2 0.476644 0.688034 0.314112 11.00000 -1.20000 AFIX 0 C24 1 0.697346 0.050581 0.415974 11.00000 0.03099 0.03441 = 0.03102 -0.00314 0.00553 0.00389 AFIX 23 H24A 2 0.698741 0.136956 0.412940 11.00000 -1.20000 H24B 2 0.710616 0.026801 0.463815 11.00000 -1.20000 AFIX 0 C11 1 0.805049 0.167311 0.517017 11.00000 0.05442 0.03686 = 0.04241 -0.01427 -0.00821 0.01810 AFIX 23 H11A 2 0.792299 0.098179 0.491299 11.00000 -1.20000 H11B 2 0.827013 0.206453 0.483327 11.00000 -1.20000 AFIX 0 C38 1 0.580438 0.582335 0.264135 11.00000 0.06593 0.07876 = 0.07712 0.04837 0.03895 0.03405 AFIX 23 H38A 2 0.572404 0.528418 0.223554 11.00000 -1.20000 H38B 2 0.605681 0.545976 0.292899 11.00000 -1.20000 AFIX 0 C52 1 0.477783 0.195461 0.178229 11.00000 0.06222 0.08054 = 0.07748 -0.03481 -0.01674 -0.01446 AFIX 23 H52A 2 0.487015 0.228897 0.130270 11.00000 -1.20000 H52B 2 0.463060 0.118938 0.168221 11.00000 -1.20000 AFIX 0 C34 1 0.663839 -0.013021 0.723476 11.00000 0.04972 0.05910 = 0.03368 0.00780 -0.01247 -0.00116 AFIX 23 H34A 2 0.662972 -0.053839 0.771405 11.00000 -1.20000 H34B 2 0.689497 0.044251 0.724893 11.00000 -1.20000 AFIX 0 C39 1 0.597317 0.696128 0.232342 11.00000 0.05736 0.06665 = 0.07379 0.03358 0.03625 0.01065 AFIX 23 H39A 2 0.611936 0.742394 0.272001 11.00000 -1.20000 H39B 2 0.621426 0.679020 0.195268 11.00000 -1.20000 AFIX 0 C49 1 0.502162 0.347091 0.299292 11.00000 0.03954 0.04165 = 0.07032 -0.02700 -0.02835 0.01261 AFIX 13 H49 2 0.489813 0.290284 0.336154 11.00000 -1.20000 AFIX 0 C40 1 0.560491 0.768728 0.197210 11.00000 0.09378 0.06023 = 0.04805 0.02833 0.02123 0.01019 AFIX 23 H40A 2 0.573403 0.846680 0.185408 11.00000 -1.20000 H40B 2 0.551099 0.731428 0.150468 11.00000 -1.20000 AFIX 0 C51 1 0.443524 0.270533 0.209455 11.00000 0.07357 0.08251 = 0.14379 -0.06972 -0.06778 0.01536 AFIX 23 H51A 2 0.422987 0.221920 0.240443 11.00000 -1.20000 H51B 2 0.424451 0.301774 0.168792 11.00000 -1.20000 AFIX 0 C53 1 0.520945 0.173330 0.221665 11.00000 0.04994 0.03595 = 0.05026 -0.01704 0.00078 -0.00202 AFIX 23 H53A 2 0.545704 0.148066 0.187635 11.00000 -1.20000 H53B 2 0.515110 0.108273 0.256324 11.00000 -1.20000 AFIX 0 C33 1 0.618392 0.051569 0.711816 11.00000 0.05585 0.04880 = 0.03493 0.00413 -0.00388 0.00228 AFIX 23 H33A 2 0.615417 0.114206 0.749053 11.00000 -1.20000 H33B 2 0.592346 -0.003550 0.718658 11.00000 -1.20000 AFIX 0 HKLF 4 REM save_b.res in Pca2(1) REM R1 = 0.0353 for 11775 Fo > 4sig(Fo) and 0.0499 for all 13805 data REM 578 parameters refined using 1 restraints END WGHT 0.0146 11.1991 REM Highest difference peak 0.956, deepest hole -0.784, 1-sigma level 0.095 Q1 1 0.7965 0.6697 0.8132 11.00000 0.05 0.96 Q2 1 0.6842 0.4698 0.3437 11.00000 0.05 0.88 Q3 1 0.5781 0.3377 0.6075 11.00000 0.05 0.77 Q4 1 0.5704 0.3245 0.5962 11.00000 0.05 0.68 Q5 1 0.6283 0.1569 0.4816 11.00000 0.05 0.60 Q6 1 0.6189 0.6028 0.4886 11.00000 0.05 0.59 Q7 1 0.6430 0.3519 0.4820 11.00000 0.05 0.56 Q8 1 0.6876 0.4382 0.6098 11.00000 0.05 0.56 Q9 1 0.6092 0.3551 0.4755 11.00000 0.05 0.55 Q10 1 0.5151 0.3803 0.2655 11.00000 0.05 0.54 ; _shelx_res_checksum 31 _olex2_exptl_crystal_mounting_method 'nylon lopp' _olex2_submission_original_sample_id cjw63 _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 Ce1 Ce 0.62687(2) 0.41710(2) 0.48030(2) 0.01604(6) Uani 1 1 d . Br1 Br 0.68450(2) 0.38994(6) 0.34928(4) 0.03279(15) Uani 1 1 d . Br3 Br 0.56701(2) 0.41275(6) 0.60918(3) 0.03422(16) Uani 1 1 d . Br2 Br 0.62781(2) 0.67512(4) 0.47919(7) 0.04015(15) Uani 1 1 d . P1 P 0.73484(5) 0.45693(14) 0.59868(9) 0.0209(3) Uani 1 1 d . P2 P 0.61275(5) 0.08038(12) 0.48517(11) 0.0247(3) Uani 1 1 d . P3 P 0.52145(5) 0.46565(14) 0.35892(9) 0.0229(3) Uani 1 1 d . O1 O 0.69267(14) 0.4223(4) 0.5542(2) 0.0230(9) Uani 1 1 d . O2 O 0.62291(14) 0.2104(3) 0.4856(3) 0.0280(8) Uani 1 1 d . O3 O 0.56149(14) 0.4199(4) 0.4050(2) 0.0253(9) Uani 1 1 d . C2 C 0.7617(2) 0.6107(5) 0.4887(4) 0.0279(14) Uani 1 1 d . H2A H 0.788885 0.562190 0.475852 0.033 Uiso 1 1 calc R H2B H 0.734658 0.580142 0.461505 0.033 Uiso 1 1 calc R C25 C 0.5514(2) 0.0567(5) 0.4651(4) 0.0298(15) Uani 1 1 d . H25 H 0.545121 0.100863 0.418747 0.036 Uiso 1 1 calc R C19 C 0.6467(2) 0.0113(5) 0.4122(4) 0.0262(14) Uani 1 1 d . H19 H 0.645401 -0.075489 0.418649 0.031 Uiso 1 1 calc R C30 C 0.5377(2) -0.0703(6) 0.4490(4) 0.0321(15) Uani 1 1 d . H30A H 0.542068 -0.118413 0.493677 0.039 Uiso 1 1 calc R H30B H 0.557814 -0.102327 0.409834 0.039 Uiso 1 1 calc R C7 C 0.7830(2) 0.3555(5) 0.5790(3) 0.0264(13) Uani 1 1 d . H7 H 0.804684 0.398810 0.546018 0.032 Uiso 1 1 calc R C44 C 0.4878(2) 0.5999(5) 0.4725(4) 0.0357(16) Uani 1 1 d . H44A H 0.513694 0.570716 0.502965 0.043 Uiso 1 1 calc R H44B H 0.498760 0.669582 0.445339 0.043 Uiso 1 1 calc R C48 C 0.4543(2) 0.3980(6) 0.4600(4) 0.0347(16) Uani 1 1 d . H48A H 0.442101 0.340011 0.424632 0.042 Uiso 1 1 calc R H48B H 0.479817 0.360573 0.487680 0.042 Uiso 1 1 calc R C1 C 0.7526(2) 0.6026(5) 0.5718(3) 0.0255(13) Uani 1 1 d . H1 H 0.725660 0.655047 0.582027 0.031 Uiso 1 1 calc R C13 C 0.7206(2) 0.4543(5) 0.6958(3) 0.0238(13) Uani 1 1 d . H13 H 0.749944 0.460222 0.724592 0.029 Uiso 1 1 calc R C36 C 0.6706(2) -0.0466(6) 0.5862(4) 0.0362(16) Uani 1 1 d . H36A H 0.675084 -0.107555 0.548244 0.043 Uiso 1 1 calc R H36B H 0.695783 0.011614 0.580928 0.043 Uiso 1 1 calc R C31 C 0.6237(2) 0.0137(6) 0.5746(4) 0.0298(15) Uani 1 1 d . H31 H 0.599510 -0.047950 0.581476 0.036 Uiso 1 1 calc R C17 C 0.6850(3) 0.3333(7) 0.7981(4) 0.0407(19) Uani 1 1 d . H17A H 0.668657 0.259266 0.809050 0.049 Uiso 1 1 calc R H17B H 0.713862 0.335127 0.827342 0.049 Uiso 1 1 calc R C3 C 0.7707(2) 0.7382(5) 0.4662(4) 0.0345(16) Uani 1 1 d . H3A H 0.777904 0.741426 0.413080 0.041 Uiso 1 1 calc R H3B H 0.742390 0.785029 0.474774 0.041 Uiso 1 1 calc R C27 C 0.4684(2) 0.1009(6) 0.4994(4) 0.0396(18) Uani 1 1 d . H27A H 0.448297 0.131314 0.539063 0.047 Uiso 1 1 calc R H27B H 0.463394 0.149875 0.455268 0.047 Uiso 1 1 calc R C26 C 0.5191(2) 0.1100(6) 0.5232(4) 0.0334(15) Uani 1 1 d . H26A H 0.523320 0.068566 0.570471 0.040 Uiso 1 1 calc R H26B H 0.527187 0.193256 0.530812 0.040 Uiso 1 1 calc R C21 C 0.6559(3) -0.0111(7) 0.2747(4) 0.0399(17) Uani 1 1 d . H21A H 0.654477 -0.097476 0.278150 0.048 Uiso 1 1 calc R H21B H 0.642983 0.012204 0.226547 0.048 Uiso 1 1 calc R C32 C 0.6156(3) 0.1053(6) 0.6351(4) 0.0354(16) Uani 1 1 d . H32A H 0.639040 0.167964 0.630602 0.043 Uiso 1 1 calc R H32B H 0.584715 0.141213 0.628247 0.043 Uiso 1 1 calc R C9 C 0.8494(2) 0.2315(6) 0.6268(4) 0.0347(16) Uani 1 1 d . H9A H 0.873147 0.270987 0.596596 0.042 Uiso 1 1 calc R H9B H 0.864446 0.203883 0.672451 0.042 Uiso 1 1 calc R C8 C 0.8114(2) 0.3204(6) 0.6469(4) 0.0297(15) Uani 1 1 d . H8A H 0.790564 0.285787 0.684160 0.036 Uiso 1 1 calc R H8B H 0.825771 0.391010 0.668465 0.036 Uiso 1 1 calc R C15 C 0.6767(3) 0.5520(7) 0.7993(4) 0.0439(19) Uani 1 1 d . H15A H 0.705151 0.562500 0.828895 0.053 Uiso 1 1 calc R H15B H 0.655203 0.616306 0.811762 0.053 Uiso 1 1 calc R C14 C 0.6892(2) 0.5594(6) 0.7165(4) 0.0331(15) Uani 1 1 d . H14A H 0.660667 0.557688 0.686566 0.040 Uiso 1 1 calc R H14B H 0.705622 0.633649 0.706356 0.040 Uiso 1 1 calc R C20 C 0.6267(2) 0.0429(6) 0.3364(4) 0.0330(15) Uani 1 1 d . H20A H 0.594528 0.013750 0.332818 0.040 Uiso 1 1 calc R H20B H 0.626055 0.128958 0.330703 0.040 Uiso 1 1 calc R C28 C 0.4547(2) -0.0246(5) 0.4822(5) 0.0419(15) Uani 1 1 d . H28A H 0.456334 -0.072297 0.527542 0.050 Uiso 1 1 calc R H28B H 0.422490 -0.026710 0.463946 0.050 Uiso 1 1 calc R C12 C 0.7659(3) 0.2511(6) 0.5351(4) 0.0419(19) Uani 1 1 d . H12A H 0.751499 0.278871 0.488963 0.050 Uiso 1 1 calc R H12B H 0.741917 0.209199 0.563734 0.050 Uiso 1 1 calc R C29 C 0.4870(2) -0.0756(6) 0.4245(4) 0.0379(16) Uani 1 1 d . H29A H 0.483291 -0.031624 0.378082 0.045 Uiso 1 1 calc R H29B H 0.478299 -0.158021 0.415095 0.045 Uiso 1 1 calc R C35 C 0.6730(3) -0.1022(6) 0.6625(4) 0.0399(17) Uani 1 1 d . H35A H 0.703995 -0.137203 0.669699 0.048 Uiso 1 1 calc R H35B H 0.649864 -0.165836 0.665688 0.048 Uiso 1 1 calc R C37 C 0.5393(2) 0.5980(6) 0.3124(4) 0.0327(15) Uani 1 1 d . H37 H 0.550743 0.649329 0.352950 0.039 Uiso 1 1 calc R C43 C 0.4735(2) 0.5046(6) 0.4174(4) 0.0286(14) Uani 1 1 d . H43 H 0.448152 0.536573 0.385850 0.034 Uiso 1 1 calc R C46 C 0.4309(3) 0.5279(7) 0.5651(4) 0.051(2) Uani 1 1 d . H46A H 0.456106 0.498884 0.597110 0.061 Uiso 1 1 calc R H46B H 0.404565 0.550548 0.596717 0.061 Uiso 1 1 calc R C5 C 0.8036(3) 0.7792(6) 0.5915(4) 0.0425(18) Uani 1 1 d . H5A H 0.777521 0.829618 0.606838 0.051 Uiso 1 1 calc R H5B H 0.831780 0.807310 0.616851 0.051 Uiso 1 1 calc R C22 C 0.7061(3) 0.0284(7) 0.2797(4) 0.0422(18) Uani 1 1 d . H22A H 0.724397 -0.010203 0.240629 0.051 Uiso 1 1 calc R H22B H 0.707875 0.113993 0.271882 0.051 Uiso 1 1 calc R C18 C 0.6967(2) 0.3391(6) 0.7157(4) 0.0327(15) Uani 1 1 d . H18A H 0.717248 0.272945 0.702726 0.039 Uiso 1 1 calc R H18B H 0.667926 0.331279 0.686658 0.039 Uiso 1 1 calc R C10 C 0.8308(2) 0.1272(6) 0.5851(4) 0.0412(18) Uani 1 1 d . H10A H 0.809670 0.081957 0.617052 0.049 Uiso 1 1 calc R H10B H 0.856715 0.075508 0.570658 0.049 Uiso 1 1 calc R C50 C 0.4596(2) 0.3723(7) 0.2550(4) 0.0419(18) Uani 1 1 d . H50A H 0.465876 0.439366 0.222108 0.050 Uiso 1 1 calc R H50B H 0.434346 0.395507 0.288758 0.050 Uiso 1 1 calc R C4 C 0.8104(2) 0.7906(6) 0.5092(4) 0.0396(17) Uani 1 1 d . H4A H 0.813410 0.874333 0.496386 0.048 Uiso 1 1 calc R H4B H 0.839442 0.750835 0.495043 0.048 Uiso 1 1 calc R C6 C 0.7938(2) 0.6534(5) 0.6152(4) 0.0311(14) Uani 1 1 d . H6A H 0.786769 0.651631 0.668352 0.037 Uiso 1 1 calc R H6B H 0.821581 0.604747 0.606525 0.037 Uiso 1 1 calc R C16 C 0.6546(3) 0.4364(8) 0.8190(4) 0.050(2) Uani 1 1 d . H16A H 0.624527 0.429614 0.793379 0.060 Uiso 1 1 calc R H16B H 0.648581 0.434351 0.872510 0.060 Uiso 1 1 calc R C47 C 0.4161(2) 0.4326(8) 0.5132(4) 0.051(2) Uani 1 1 d . H47A H 0.388910 0.459463 0.484924 0.062 Uiso 1 1 calc R H47B H 0.406757 0.363029 0.541964 0.062 Uiso 1 1 calc R C0AA C 0.4477(3) 0.6343(7) 0.5219(4) 0.049(2) Uani 1 1 d . H0AA H 0.422096 0.665741 0.491802 0.058 Uiso 1 1 calc R H0AB H 0.457800 0.696161 0.556417 0.058 Uiso 1 1 calc R C45 C 0.5377(3) 0.2776(9) 0.2644(6) 0.071(3) Uani 1 1 d . H45A H 0.559389 0.249901 0.302728 0.085 Uiso 1 1 calc R H45B H 0.555433 0.328789 0.230683 0.085 Uiso 1 1 calc R C23 C 0.7263(2) -0.0019(7) 0.3541(4) 0.0403(17) Uani 1 1 d . H23A H 0.758309 0.028253 0.357296 0.048 Uiso 1 1 calc R H23B H 0.727413 -0.087989 0.359739 0.048 Uiso 1 1 calc R C41 C 0.5191(3) 0.7840(7) 0.2441(5) 0.050(2) Uani 1 1 d . H41A H 0.494342 0.820918 0.214521 0.060 Uiso 1 1 calc R H41B H 0.526822 0.838058 0.284710 0.060 Uiso 1 1 calc R C42 C 0.5005(2) 0.6698(6) 0.2768(4) 0.0359(16) Uani 1 1 d . H42A H 0.485688 0.622971 0.237545 0.043 Uiso 1 1 calc R H42B H 0.476644 0.688034 0.314112 0.043 Uiso 1 1 calc R C24 C 0.6973(2) 0.0506(6) 0.4160(4) 0.0321(15) Uani 1 1 d . H24A H 0.698741 0.136956 0.412940 0.039 Uiso 1 1 calc R H24B H 0.710616 0.026801 0.463815 0.039 Uiso 1 1 calc R C11 C 0.8050(3) 0.1673(7) 0.5170(4) 0.0446(19) Uani 1 1 d . H11A H 0.792299 0.098179 0.491299 0.053 Uiso 1 1 calc R H11B H 0.827013 0.206453 0.483327 0.053 Uiso 1 1 calc R C38 C 0.5804(3) 0.5823(9) 0.2641(6) 0.074(3) Uani 1 1 d . H38A H 0.572404 0.528418 0.223554 0.089 Uiso 1 1 calc R H38B H 0.605681 0.545976 0.292899 0.089 Uiso 1 1 calc R C52 C 0.4778(3) 0.1955(10) 0.1782(6) 0.073(3) Uani 1 1 d . H52A H 0.487015 0.228897 0.130270 0.088 Uiso 1 1 calc R H52B H 0.463060 0.118938 0.168221 0.088 Uiso 1 1 calc R C34 C 0.6638(3) -0.0130(8) 0.7235(4) 0.047(2) Uani 1 1 d . H34A H 0.662972 -0.053839 0.771405 0.057 Uiso 1 1 calc R H34B H 0.689497 0.044251 0.724893 0.057 Uiso 1 1 calc R C39 C 0.5973(3) 0.6961(8) 0.2323(6) 0.066(3) Uani 1 1 d . H39A H 0.611936 0.742394 0.272001 0.079 Uiso 1 1 calc R H39B H 0.621426 0.679020 0.195268 0.079 Uiso 1 1 calc R C49 C 0.5022(3) 0.3471(7) 0.2993(5) 0.051(2) Uani 1 1 d . H49 H 0.489813 0.290284 0.336154 0.061 Uiso 1 1 calc R C40 C 0.5605(4) 0.7687(9) 0.1972(5) 0.067(3) Uani 1 1 d . H40A H 0.573403 0.846680 0.185408 0.081 Uiso 1 1 calc R H40B H 0.551099 0.731428 0.150468 0.081 Uiso 1 1 calc R C51 C 0.4435(4) 0.2705(10) 0.2095(8) 0.100(5) Uani 1 1 d . H51A H 0.422987 0.221920 0.240443 0.120 Uiso 1 1 calc R H51B H 0.424451 0.301774 0.168792 0.120 Uiso 1 1 calc R C53 C 0.5209(3) 0.1733(7) 0.2217(4) 0.0454(19) Uani 1 1 d . H53A H 0.545704 0.148066 0.187635 0.054 Uiso 1 1 calc R H53B H 0.515110 0.108273 0.256324 0.054 Uiso 1 1 calc R C33 C 0.6184(3) 0.0516(7) 0.7118(4) 0.0465(19) Uani 1 1 d . H33A H 0.615417 0.114206 0.749053 0.056 Uiso 1 1 calc R H33B H 0.592346 -0.003550 0.718658 0.056 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 Ce1 0.01583(12) 0.01837(13) 0.01391(12) -0.0003(2) -0.00068(12) 0.00156(12) Br1 0.0318(3) 0.0438(4) 0.0228(3) 0.0001(3) 0.0101(3) 0.0031(3) Br3 0.0357(4) 0.0444(4) 0.0225(3) 0.0034(3) 0.0117(3) 0.0089(3) Br2 0.0373(3) 0.0191(3) 0.0641(4) 0.0010(5) -0.0091(4) 0.0017(3) P1 0.0215(7) 0.0228(8) 0.0185(8) -0.0014(7) -0.0050(6) 0.0027(6) P2 0.0271(7) 0.0198(6) 0.0272(8) 0.0005(8) 0.0030(9) 0.0011(5) P3 0.0206(7) 0.0240(8) 0.0243(8) -0.0016(7) -0.0072(7) -0.0002(6) O1 0.023(2) 0.031(2) 0.015(2) -0.0008(17) -0.0088(16) -0.0003(18) O2 0.0248(19) 0.0295(19) 0.030(2) 0.005(3) 0.002(2) -0.0014(16) O3 0.021(2) 0.030(2) 0.025(2) -0.0027(19) -0.0044(17) 0.0021(19) C2 0.025(3) 0.028(3) 0.030(4) 0.002(3) -0.005(3) 0.002(2) C25 0.031(3) 0.024(3) 0.034(4) 0.002(3) 0.002(3) -0.001(2) C19 0.031(4) 0.018(3) 0.029(4) -0.001(3) 0.004(3) 0.004(3) C30 0.032(3) 0.025(4) 0.039(4) 0.001(3) -0.002(3) 0.003(3) C7 0.031(3) 0.025(3) 0.024(3) 0.001(2) -0.002(3) 0.006(3) C44 0.048(4) 0.023(3) 0.037(4) 0.003(3) 0.014(4) 0.003(3) C48 0.037(4) 0.028(4) 0.039(4) 0.007(3) -0.006(3) -0.008(3) C1 0.025(3) 0.028(3) 0.023(3) -0.003(2) -0.004(2) 0.005(3) C13 0.023(3) 0.035(3) 0.013(3) -0.005(2) -0.005(2) 0.000(3) C36 0.032(4) 0.033(4) 0.044(4) 0.005(3) 0.000(3) 0.002(3) C31 0.033(4) 0.027(4) 0.029(4) 0.003(3) 0.000(3) 0.001(3) C17 0.035(4) 0.054(5) 0.033(4) 0.003(3) 0.004(3) -0.005(4) C3 0.039(4) 0.026(3) 0.039(4) 0.006(3) 0.001(3) 0.007(3) C27 0.027(3) 0.038(4) 0.053(5) -0.006(3) 0.008(3) 0.000(3) C26 0.027(3) 0.031(4) 0.042(4) -0.004(3) 0.003(3) 0.001(3) C21 0.048(4) 0.042(4) 0.030(4) -0.003(3) 0.008(3) 0.003(3) C32 0.043(4) 0.034(4) 0.029(4) 0.001(3) -0.002(3) 0.001(3) C9 0.022(3) 0.034(4) 0.048(4) 0.007(3) -0.001(3) 0.007(3) C8 0.026(3) 0.029(4) 0.034(4) 0.002(3) -0.006(3) 0.005(3) C15 0.042(4) 0.059(5) 0.030(4) -0.016(3) 0.004(3) 0.003(4) C14 0.037(4) 0.036(4) 0.027(3) -0.008(3) -0.002(3) 0.007(3) C20 0.039(4) 0.029(4) 0.030(4) 0.002(3) 0.002(3) 0.005(3) C28 0.036(3) 0.035(4) 0.056(4) 0.001(5) -0.001(4) -0.006(3) C12 0.052(5) 0.038(4) 0.036(4) -0.015(3) -0.011(3) 0.017(3) C29 0.036(4) 0.025(4) 0.052(4) 0.001(3) 0.000(3) -0.004(3) C35 0.039(4) 0.035(4) 0.046(4) 0.008(3) -0.005(3) 0.003(3) C37 0.029(3) 0.034(4) 0.035(4) 0.009(3) -0.002(3) 0.004(3) C43 0.024(3) 0.030(4) 0.032(4) 0.005(3) -0.006(3) 0.005(3) C46 0.048(5) 0.058(5) 0.046(5) 0.021(4) 0.018(4) 0.025(4) C5 0.041(4) 0.030(4) 0.057(5) -0.005(3) -0.008(4) -0.004(3) C22 0.044(4) 0.043(4) 0.040(4) 0.004(3) 0.013(3) 0.009(3) C18 0.024(3) 0.041(4) 0.033(4) 0.002(3) 0.002(3) -0.002(3) C10 0.034(4) 0.032(4) 0.057(5) -0.002(3) 0.000(3) 0.009(3) C50 0.037(4) 0.045(4) 0.044(4) -0.011(3) -0.022(3) 0.000(3) C4 0.040(4) 0.024(4) 0.055(5) 0.008(3) 0.001(3) -0.002(3) C6 0.029(3) 0.029(3) 0.035(4) -0.002(3) -0.009(3) -0.002(3) C16 0.040(4) 0.083(7) 0.028(4) -0.010(4) 0.007(3) -0.003(4) C47 0.027(4) 0.073(6) 0.055(5) 0.037(4) 0.002(3) -0.002(4) C0AA 0.061(5) 0.041(4) 0.044(5) 0.009(4) 0.018(4) 0.023(4) C45 0.050(5) 0.061(6) 0.101(8) -0.043(6) -0.030(5) 0.013(4) C23 0.039(4) 0.048(4) 0.034(4) 0.003(4) 0.008(3) 0.014(3) C41 0.058(5) 0.033(4) 0.058(5) 0.011(4) 0.000(4) 0.003(4) C42 0.040(4) 0.029(4) 0.039(4) 0.006(3) -0.013(3) 0.001(3) C24 0.031(4) 0.034(4) 0.031(4) -0.003(3) 0.006(3) 0.004(3) C11 0.054(5) 0.037(4) 0.042(4) -0.014(3) -0.008(4) 0.018(4) C38 0.066(6) 0.079(7) 0.077(7) 0.048(6) 0.039(5) 0.034(5) C52 0.062(6) 0.081(7) 0.077(7) -0.035(6) -0.017(5) -0.014(5) C34 0.050(5) 0.059(5) 0.034(4) 0.008(4) -0.012(4) -0.001(4) C39 0.057(6) 0.067(6) 0.074(6) 0.034(5) 0.036(5) 0.011(5) C49 0.040(4) 0.042(5) 0.070(6) -0.027(4) -0.028(4) 0.013(4) C40 0.094(8) 0.060(6) 0.048(5) 0.028(4) 0.021(5) 0.010(5) C51 0.074(7) 0.083(8) 0.144(11) -0.070(8) -0.068(7) 0.015(6) C53 0.050(5) 0.036(4) 0.050(5) -0.017(4) 0.001(4) -0.002(4) C33 0.056(5) 0.049(5) 0.035(4) 0.004(3) -0.004(4) 0.002(4) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Br1 Ce1 Br2 95.47(3) Br3 Ce1 Br1 172.78(2) Br3 Ce1 Br2 91.61(3) O1 Ce1 Br1 90.50(10) O1 Ce1 Br3 91.16(10) O1 Ce1 Br2 88.33(11) O1 Ce1 O2 92.37(16) O1 Ce1 O3 177.66(14) O2 Ce1 Br1 87.42(13) O2 Ce1 Br3 85.48(13) O2 Ce1 Br2 177.02(12) O3 Ce1 Br1 89.08(11) O3 Ce1 Br3 89.55(11) O3 Ce1 Br2 89.42(11) O3 Ce1 O2 89.91(16) O1 P1 C7 109.8(3) O1 P1 C1 108.9(3) O1 P1 C13 109.4(3) C1 P1 C7 108.2(3) C1 P1 C13 110.0(3) C13 P1 C7 110.5(3) O2 P2 C25 109.5(3) O2 P2 C19 108.8(3) O2 P2 C31 111.8(3) C25 P2 C19 108.1(3) C31 P2 C25 106.5(3) C31 P2 C19 112.0(3) O3 P3 C37 109.2(3) O3 P3 C43 110.1(3) O3 P3 C49 107.8(3) C37 P3 C49 115.5(4) C43 P3 C37 106.8(3) C43 P3 C49 107.4(3) P1 O1 Ce1 166.2(3) P2 O2 Ce1 171.2(3) P3 O3 Ce1 160.7(3) H2A C2 H2B 108.1 C1 C2 H2A 109.6 C1 C2 H2B 109.6 C3 C2 H2A 109.6 C3 C2 H2B 109.6 C3 C2 C1 110.4(5) P2 C25 H25 105.7 C30 C25 P2 115.3(4) C30 C25 H25 105.7 C30 C25 C26 110.5(5) C26 C25 P2 113.1(4) C26 C25 H25 105.7 P2 C19 H19 108.8 C20 C19 P2 110.3(4) C20 C19 H19 108.8 C24 C19 P2 110.7(4) C24 C19 H19 108.8 C24 C19 C20 109.3(5) C25 C30 H30A 109.7 C25 C30 H30B 109.7 C25 C30 C29 109.8(5) H30A C30 H30B 108.2 C29 C30 H30A 109.7 C29 C30 H30B 109.7 P1 C7 H7 106.1 C8 C7 P1 114.2(4) C8 C7 H7 106.1 C12 C7 P1 110.4(5) C12 C7 H7 106.1 C12 C7 C8 113.1(5) H44A C44 H44B 108.0 C43 C44 H44A 109.4 C43 C44 H44B 109.4 C0AA C44 H44A 109.4 C0AA C44 H44B 109.4 C0AA C44 C43 111.4(6) H48A C48 H48B 107.9 C43 C48 H48A 109.2 C43 C48 H48B 109.2 C47 C48 H48A 109.2 C47 C48 H48B 109.2 C47 C48 C43 112.0(6) P1 C1 H1 106.3 C2 C1 P1 111.7(4) C2 C1 H1 106.3 C2 C1 C6 110.3(5) C6 C1 P1 115.3(4) C6 C1 H1 106.3 P1 C13 H13 108.5 C14 C13 P1 110.9(4) C14 C13 H13 108.5 C18 C13 P1 110.3(4) C18 C13 H13 108.5 C18 C13 C14 110.2(5) H36A C36 H36B 108.1 C31 C36 H36A 109.6 C31 C36 H36B 109.6 C35 C36 H36A 109.6 C35 C36 H36B 109.6 C35 C36 C31 110.5(6) P2 C31 H31 106.5 C36 C31 P2 117.5(5) C36 C31 H31 106.5 C36 C31 C32 110.0(6) C32 C31 P2 109.1(4) C32 C31 H31 106.5 H17A C17 H17B 108.2 C18 C17 H17A 109.7 C18 C17 H17B 109.7 C16 C17 H17A 109.7 C16 C17 H17B 109.7 C16 C17 C18 109.8(6) C2 C3 H3A 109.3 C2 C3 H3B 109.3 H3A C3 H3B 108.0 C4 C3 C2 111.4(5) C4 C3 H3A 109.3 C4 C3 H3B 109.3 H27A C27 H27B 107.9 C26 C27 H27A 109.3 C26 C27 H27B 109.3 C28 C27 H27A 109.3 C28 C27 H27B 109.3 C28 C27 C26 111.8(6) C25 C26 H26A 109.4 C25 C26 H26B 109.4 C27 C26 C25 111.1(6) C27 C26 H26A 109.4 C27 C26 H26B 109.4 H26A C26 H26B 108.0 H21A C21 H21B 108.0 C20 C21 H21A 109.4 C20 C21 H21B 109.4 C22 C21 H21A 109.4 C22 C21 H21B 109.4 C22 C21 C20 111.2(6) C31 C32 H32A 109.2 C31 C32 H32B 109.2 H32A C32 H32B 107.9 C33 C32 C31 111.8(6) C33 C32 H32A 109.2 C33 C32 H32B 109.2 H9A C9 H9B 107.8 C8 C9 H9A 109.1 C8 C9 H9B 109.1 C10 C9 H9A 109.1 C10 C9 H9B 109.1 C10 C9 C8 112.7(5) C7 C8 C9 111.3(6) C7 C8 H8A 109.4 C7 C8 H8B 109.4 C9 C8 H8A 109.4 C9 C8 H8B 109.4 H8A C8 H8B 108.0 H15A C15 H15B 107.9 C14 C15 H15A 109.2 C14 C15 H15B 109.2 C16 C15 H15A 109.2 C16 C15 H15B 109.2 C16 C15 C14 112.1(6) C13 C14 C15 109.3(6) C13 C14 H14A 109.8 C13 C14 H14B 109.8 C15 C14 H14A 109.8 C15 C14 H14B 109.8 H14A C14 H14B 108.3 C19 C20 H20A 109.5 C19 C20 H20B 109.5 C21 C20 C19 110.8(6) C21 C20 H20A 109.5 C21 C20 H20B 109.5 H20A C20 H20B 108.1 C27 C28 H28A 109.6 C27 C28 H28B 109.6 H28A C28 H28B 108.1 C29 C28 C27 110.2(6) C29 C28 H28A 109.6 C29 C28 H28B 109.6 C7 C12 H12A 109.3 C7 C12 H12B 109.3 C7 C12 C11 111.5(6) H12A C12 H12B 108.0 C11 C12 H12A 109.3 C11 C12 H12B 109.3 C30 C29 H29A 109.3 C30 C29 H29B 109.3 C28 C29 C30 111.8(6) C28 C29 H29A 109.3 C28 C29 H29B 109.3 H29A C29 H29B 107.9 C36 C35 H35A 109.2 C36 C35 H35B 109.2 C36 C35 C34 111.9(6) H35A C35 H35B 107.9 C34 C35 H35A 109.2 C34 C35 H35B 109.2 P3 C37 H37 103.9 C42 C37 P3 115.9(5) C42 C37 H37 103.9 C38 C37 P3 113.8(5) C38 C37 H37 103.9 C38 C37 C42 113.5(6) P3 C43 H43 108.3 C44 C43 P3 110.6(4) C44 C43 C48 109.1(5) C44 C43 H43 108.3 C48 C43 P3 112.1(5) C48 C43 H43 108.3 H46A C46 H46B 108.1 C47 C46 H46A 109.6 C47 C46 H46B 109.6 C47 C46 C0AA 110.1(7) C0AA C46 H46A 109.6 C0AA C46 H46B 109.6 H5A C5 H5B 107.8 C4 C5 H5A 109.1 C4 C5 H5B 109.1 C4 C5 C6 112.5(6) C6 C5 H5A 109.1 C6 C5 H5B 109.1 C21 C22 H22A 109.5 C21 C22 H22B 109.5 H22A C22 H22B 108.1 C23 C22 C21 110.6(6) C23 C22 H22A 109.5 C23 C22 H22B 109.5 C13 C18 C17 111.5(6) C13 C18 H18A 109.3 C13 C18 H18B 109.3 C17 C18 H18A 109.3 C17 C18 H18B 109.3 H18A C18 H18B 108.0 C9 C10 H10A 109.6 C9 C10 H10B 109.6 C9 C10 C11 110.3(6) H10A C10 H10B 108.1 C11 C10 H10A 109.6 C11 C10 H10B 109.6 H50A C50 H50B 107.7 C49 C50 H50A 108.8 C49 C50 H50B 108.8 C49 C50 C51 113.7(7) C51 C50 H50A 108.8 C51 C50 H50B 108.8 C3 C4 C5 112.3(6) C3 C4 H4A 109.1 C3 C4 H4B 109.1 C5 C4 H4A 109.1 C5 C4 H4B 109.1 H4A C4 H4B 107.9 C1 C6 H6A 109.5 C1 C6 H6B 109.5 C5 C6 C1 110.7(5) C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 108.1 C17 C16 H16A 109.2 C17 C16 H16B 109.2 C15 C16 C17 112.0(6) C15 C16 H16A 109.2 C15 C16 H16B 109.2 H16A C16 H16B 107.9 C48 C47 H47A 109.1 C48 C47 H47B 109.1 C46 C47 C48 112.4(6) C46 C47 H47A 109.1 C46 C47 H47B 109.1 H47A C47 H47B 107.8 C44 C0AA C46 110.0(6) C44 C0AA H0AA 109.7 C44 C0AA H0AB 109.7 C46 C0AA H0AA 109.7 C46 C0AA H0AB 109.7 H0AA C0AA H0AB 108.2 H45A C45 H45B 107.4 C49 C45 H45A 108.4 C49 C45 H45B 108.4 C49 C45 C53 115.6(7) C53 C45 H45A 108.4 C53 C45 H45B 108.4 C22 C23 H23A 109.4 C22 C23 H23B 109.4 C22 C23 C24 111.0(6) H23A C23 H23B 108.0 C24 C23 H23A 109.4 C24 C23 H23B 109.4 H41A C41 H41B 107.6 C42 C41 H41A 108.7 C42 C41 H41B 108.7 C40 C41 H41A 108.7 C40 C41 H41B 108.7 C40 C41 C42 114.1(7) C37 C42 H42A 109.4 C37 C42 H42B 109.4 C41 C42 C37 111.3(6) C41 C42 H42A 109.4 C41 C42 H42B 109.4 H42A C42 H42B 108.0 C19 C24 H24A 109.2 C19 C24 H24B 109.2 C23 C24 C19 112.1(6) C23 C24 H24A 109.2 C23 C24 H24B 109.2 H24A C24 H24B 107.9 C12 C11 H11A 109.1 C12 C11 H11B 109.1 C10 C11 C12 112.3(6) C10 C11 H11A 109.1 C10 C11 H11B 109.1 H11A C11 H11B 107.9 C37 C38 H38A 109.1 C37 C38 H38B 109.1 C37 C38 C39 112.5(7) H38A C38 H38B 107.8 C39 C38 H38A 109.1 C39 C38 H38B 109.1 H52A C52 H52B 107.2 C51 C52 H52A 107.8 C51 C52 H52B 107.8 C51 C52 C53 118.0(8) C53 C52 H52A 107.8 C53 C52 H52B 107.8 C35 C34 H34A 109.3 C35 C34 H34B 109.3 H34A C34 H34B 107.9 C33 C34 C35 111.8(6) C33 C34 H34A 109.3 C33 C34 H34B 109.3 C38 C39 H39A 108.7 C38 C39 H39B 108.7 H39A C39 H39B 107.6 C40 C39 C38 114.4(8) C40 C39 H39A 108.7 C40 C39 H39B 108.7 P3 C49 H49 101.1 C50 C49 P3 115.4(5) C50 C49 H49 101.1 C45 C49 P3 116.9(6) C45 C49 C50 116.9(7) C45 C49 H49 101.1 C41 C40 C39 113.3(7) C41 C40 H40A 108.9 C41 C40 H40B 108.9 C39 C40 H40A 108.9 C39 C40 H40B 108.9 H40A C40 H40B 107.7 C50 C51 H51A 107.8 C50 C51 H51B 107.8 C52 C51 C50 118.1(8) C52 C51 H51A 107.8 C52 C51 H51B 107.8 H51A C51 H51B 107.1 C45 C53 H53A 108.7 C45 C53 H53B 108.7 C52 C53 C45 114.1(7) C52 C53 H53A 108.7 C52 C53 H53B 108.7 H53A C53 H53B 107.6 C32 C33 H33A 109.3 C32 C33 H33B 109.3 C34 C33 C32 111.6(7) C34 C33 H33A 109.3 C34 C33 H33B 109.3 H33A C33 H33B 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ce1 Br1 2.9268(8) Ce1 Br3 2.9166(8) Ce1 Br2 2.9504(8) Ce1 O1 2.332(4) Ce1 O2 2.368(4) Ce1 O3 2.336(4) P1 O1 1.516(4) P1 C7 1.848(6) P1 C1 1.811(7) P1 C13 1.816(6) P2 O2 1.515(4) P2 C25 1.831(6) P2 C19 1.831(6) P2 C31 1.826(7) P3 O3 1.523(4) P3 C37 1.809(7) P3 C43 1.805(7) P3 C49 1.824(7) C2 H2A 0.9900 C2 H2B 0.9900 C2 C1 1.539(9) C2 C3 1.536(8) C25 H25 1.0000 C25 C30 1.533(9) C25 C26 1.539(9) C19 H19 1.0000 C19 C20 1.541(9) C19 C24 1.532(9) C30 H30A 0.9900 C30 H30B 0.9900 C30 C29 1.536(9) C7 H7 1.0000 C7 C8 1.536(8) C7 C12 1.520(9) C44 H44A 0.9900 C44 H44B 0.9900 C44 C43 1.537(10) C44 C0AA 1.520(10) C48 H48A 0.9900 C48 H48B 0.9900 C48 C43 1.548(9) C48 C47 1.521(10) C1 H1 1.0000 C1 C6 1.543(8) C13 H13 1.0000 C13 C14 1.551(9) C13 C18 1.531(9) C36 H36A 0.9900 C36 H36B 0.9900 C36 C31 1.538(9) C36 C35 1.530(10) C31 H31 1.0000 C31 C32 1.538(10) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.541(9) C17 C16 1.519(11) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.513(9) C27 H27A 0.9900 C27 H27B 0.9900 C27 C26 1.533(9) C27 C28 1.521(9) C26 H26A 0.9900 C26 H26B 0.9900 C21 H21A 0.9900 C21 H21B 0.9900 C21 C20 1.535(9) C21 C22 1.523(11) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.529(10) C9 H9A 0.9900 C9 H9B 0.9900 C9 C8 1.541(9) C9 C10 1.513(10) C8 H8A 0.9900 C8 H8B 0.9900 C15 H15A 0.9900 C15 H15B 0.9900 C15 C14 1.553(10) C15 C16 1.511(11) C14 H14A 0.9900 C14 H14B 0.9900 C20 H20A 0.9900 C20 H20B 0.9900 C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.520(10) C12 H12A 0.9900 C12 H12B 0.9900 C12 C11 1.520(9) C29 H29A 0.9900 C29 H29B 0.9900 C35 H35A 0.9900 C35 H35B 0.9900 C35 C34 1.531(11) C37 H37 1.0000 C37 C42 1.534(9) C37 C38 1.491(10) C43 H43 1.0000 C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.505(12) C46 C0AA 1.527(11) C5 H5A 0.9900 C5 H5B 0.9900 C5 C4 1.516(11) C5 C6 1.528(9) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.516(10) C18 H18A 0.9900 C18 H18B 0.9900 C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.517(10) C50 H50A 0.9900 C50 H50B 0.9900 C50 C49 1.500(9) C50 C51 1.502(11) C4 H4A 0.9900 C4 H4B 0.9900 C6 H6A 0.9900 C6 H6B 0.9900 C16 H16A 0.9900 C16 H16B 0.9900 C47 H47A 0.9900 C47 H47B 0.9900 C0AA H0AA 0.9900 C0AA H0AB 0.9900 C45 H45A 0.9900 C45 H45B 0.9900 C45 C49 1.447(11) C45 C53 1.504(10) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.526(9) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.533(10) C41 C40 1.481(12) C42 H42A 0.9900 C42 H42B 0.9900 C24 H24A 0.9900 C24 H24B 0.9900 C11 H11A 0.9900 C11 H11B 0.9900 C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.505(12) C52 H52A 0.9900 C52 H52B 0.9900 C52 C51 1.429(14) C52 C53 1.499(12) C34 H34A 0.9900 C34 H34B 0.9900 C34 C33 1.522(11) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.494(13) C49 H49 1.0000 C40 H40A 0.9900 C40 H40B 0.9900 C51 H51A 0.9900 C51 H51B 0.9900 C53 H53A 0.9900 C53 H53B 0.9900 C33 H33A 0.9900 C33 H33B 0.9900 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.964(10) 2 0.036(10)